Neutron and X-ray investigations of the Jahn–Teller switch in partially deuterated ammonium copper Tutton salt, (NH4)2[Cu(H2O)6](SO4)2

Jørgensen, M.R.V.; Piccoli, P.M.B.; Hathwar, V.R.; Wang, X.P.; Hoffmann, C.M.; Yakovenko, A.A.; Halder, G.J.; Schlueter, J.A.; Iversen, B.B.; Schultz, A.J.

doi:10.1107/S2052520616018412

Neutron and X-ray investigations of the Jahn-Teller switch in partially deuterated ammonium copper Tutton salt, (NH₄)₂[Cu(H₂O)₆](SO₄)₂

M. R. V. Jørgensen, P. M. B. Piccoli, V. R. Hathwar, X. P. Wang, C. M. Hoffmann, A. A. Yakovenko, G. J. Halder, J. A. Schlueter, B. B. Iversen and A. J. Schultz

The structural phase transition accompanied by a Jahn-Teller switch has been studied over a range of H/D ratios in (NH₄)₂[Cu(H₂O)₆](SO₄)₂ (ACTS). In particular, single-crystal neutron diffraction investigations of crystals with deuteration in the range 50 to 82% are shown to be consistent with previous electron paramagnetic resonance (EPR) experiments exhibiting a phase boundary at 50% deuteration under ambient pressure. Polycrystalline samples show that the two phases can co-exist. In addition, single-crystal neutron and polycrystalline X-ray diffraction pressure experiments show a shift to lower pressure at 60% deuteration versus previous measurements at 100% deuteration.

Keywords: single-crystal neutron diffraction; synchrotron powder diffraction; deuterium isotope phase transition; pressure-temperature phase transition.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520616018412/eb5054sup1.cif Contains datablocks D60H40_20K_publ, D60H40_20K_overall, IPNS_SCD_D60H40_20K_phase_1, D60H40_20K_s_01, D60H40_20K_s_02, D60H40_20K_s_03, D60H40_20K_s_04, D60H40_20K_s_05, D60H40_20K_s_06, D60H40_20K_s_07, D60H40_20K_s_08, D60H40_20K_s_09, D60H40_20K_s_10, D60H40_20K_s_11, D60H40_20K_s_12, D60H40_20K_s_13, D60H40_20K_s_14, D60H40_20K_s_15, D60H40_20K_s_16, D60H40_20K_s_17, D60H40_20K_s_18, D60H40_20K_s_19, D60H40_20K_s_20, D60H40_20K_s_21, D60H40_20K_s_22, D60H40_20K_s_23, D60H40_20K_s_24, D60H40_20K_s_25, D60H40_20K_s_26, D60H40_20K_s_27, D60H40_20K_s_28, D60H40_20K_s_29, D60H40_20K_s_30, D60H40_20K_s_31, D60H40_20K_s_32, D60H40_20K_s_33, D60H40_20K_s_34, D60H40_20K_s_35, D60H40_20K_s_36, D75_20K_publ, D75_20K_overall, IPNS_SCD_D75_20K_phase_1, D75_20K_s_01, D75_20K_s_02, D75_20K_s_03, D75_20K_s_04, D75_20K_s_05, D75_20K_s_06, D75_20K_s_07, D75_20K_s_08, D75_20K_s_09, D75_20K_s_10, D75_20K_s_11, D75_20K_s_12, D75_20K_s_13, D75_20K_s_14, D75_20K_s_15, D75_20K_s_16, D75_20K_s_17, D75_20K_s_18, D75_20K_s_19, D75_20K_s_20, D75_20K_s_21, D75_20K_s_22, D75_20K_s_23, D75_20K_s_24, D75_20K_s_25, D75_20K_s_26, D75_20K_s_27, D75_20K_s_28, D80_20K_publ, D80_20K_overall, IPNS_SCD_D80_20K_phase_1, D80_20K_s_01, D80_20K_s_02, D80_20K_s_03, D80_20K_s_04, D80_20K_s_05, D80_20K_s_06, D80_20K_s_07, D80_20K_s_08, D80_20K_s_09, D80_20K_s_10, D80_20K_s_11, D80_20K_s_12, D80_20K_s_13, D80_20K_s_14, D80_20K_s_15, D80_20K_s_16, CuTS_50D_100K, CuTS_54D_100K, CuTS_62D_100K, CuTS_62D_150K, CuTS_62D_200K, CuTS_62D_250K, CuTS_62D_295K, CuTS_62D_II_295K, CUTS_74D_295K, CuTS_78D_295K
	Text file https://doi.org/10.1107/S2052520616018412/eb5054sup2.txt X-ray file 60D_295K.flt
	Text file https://doi.org/10.1107/S2052520616018412/eb5054sup3.txt JANA2006 file 60D_295K_50bar_mixed-phase_step0.m40
	Text file https://doi.org/10.1107/S2052520616018412/eb5054sup4.txt JANA2006 file 60D_295K_50bar_mixed-phase_step0.m41
	Text file https://doi.org/10.1107/S2052520616018412/eb5054sup5.txt JANA2006 file 60D_295K_50bar_mixed-phase_step0.m50
	Text file https://doi.org/10.1107/S2052520616018412/eb5054sup6.txt JANA2006 file 60D_295K_50bar_mixed-phase_step0.m90
	Text file https://doi.org/10.1107/S2052520616018412/eb5054sup7.txt JANA2006 file 60D_295K_50bar_mixed-phase_step0.m91
	Text file https://doi.org/10.1107/S2052520616018412/eb5054sup8.txt JANA2006 file 60D_295K_50bar_mixed-phase_step0.prf
	Text file https://doi.org/10.1107/S2052520616018412/eb5054sup9.txt JANA2006 file 60D_295K_50bar_mixed-phase_step0.ref
	Portable Document Format (PDF) file https://doi.org/10.1107/S2052520616018412/eb5054sup10.pdf Descriptions of the X-ray powder analyses and the neutron single-crystal analyses. Additional plots of phase fractions versus pressure, temperature and H/D ratio, and temperature dependence of neutron structure

Computing details top

Data collection: CrystalPlan (Zikovsky, J. et al. 2011) for CuTS_50D_100K, CuTS_54D_100K, CuTS_62D_100K, CuTS_62D_150K, CuTS_62D_200K, CuTS_62D_250K, CuTS_62D_295K, CuTS_62D_II_295K, CUTS_74D_295K, CuTS_78D_295K. Cell refinement: MANTID (Taylor, J. et al. 2012) for CuTS_50D_100K, CuTS_54D_100K, CuTS_62D_100K, CuTS_62D_150K, CuTS_62D_200K, CuTS_62D_250K, CuTS_62D_295K, CuTS_62D_II_295K, CUTS_74D_295K, CuTS_78D_295K. Data reduction: MANTID (Taylor, J. et al. 2012) & ANVRED2X (local program) for CuTS_50D_100K, CuTS_54D_100K, CuTS_62D_100K, CuTS_62D_150K, CuTS_62D_200K, CuTS_62D_250K, CuTS_62D_295K, CuTS_62D_II_295K, CUTS_74D_295K, CuTS_78D_295K. Program(s) used to refine structure: GSAS (Larson & Von Dreele, 2004) for CuTS_50D_100K, CuTS_54D_100K, CuTS_62D_100K, CuTS_62D_150K, CuTS_62D_200K, CuTS_62D_250K, CuTS_62D_295K, CuTS_62D_II_295K, CUTS_74D_295K, CuTS_78D_295K.

(IPNS_SCD_D60H40_20K_phase_1) top

Crystal data top

(NH₄)₂[Cu(H2O)₆](SO₄)₂·43%H·57%D	β = 106.353 (14)°
M_r = 411.21	V = 674.7 (2) Å³
Monoclinic, P2₁/a	Z = 2
a = 9.068 (2) Å	D_x = 2.024 Mg m⁻³
b = 12.201 (2) Å	Neutron radiation
c = 6.355 (1) Å	T = 20 K

Data collection top

IPNS single crystal diffractometer	Not applicable to TOF Laue technique monochromator
Radiation source: Intense Pulsed Neutron Source

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.005
S2	0.4199 (3)	0.1348 (2)	0.7432 (4)	0.00423
O3	0.43017 (15)	0.22732 (11)	0.5958 (2)	0.00753
O4	0.55789 (15)	0.06696 (12)	0.7825 (2)	0.0085
O5	0.28435 (14)	0.06802 (12)	0.6320 (2)	0.00717
O6	0.40185 (15)	0.17927 (11)	0.9509 (2)	0.00747
O7	0.18736 (15)	0.11840 (12)	0.1780 (2)	0.00882
O8	0.84240 (14)	0.10942 (11)	0.0287 (2)	0.00754
O9	−0.00625 (15)	−0.06439 (12)	0.2828 (2)	0.00754
N10	0.14204 (10)	0.34148 (8)	0.35803 (14)	0.00897
H11	0.0798 (5)	0.3274 (4)	0.1996 (7)	0.03411	0.4340 (12)
D11	0.0798 (5)	0.3274 (4)	0.1996 (7)	0.02412	0.5660 (12)
H12	0.2398 (4)	0.2955 (3)	0.3993 (7)	0.02077	0.4340 (12)
D12	0.2398 (4)	0.2955 (3)	0.3993 (7)	0.01468	0.5660 (12)
H13	0.0742 (4)	0.3208 (4)	0.4585 (7)	0.02469	0.4340 (12)
D13	0.0742 (4)	0.3208 (4)	0.4585 (7)	0.01746	0.5660 (12)
H14	0.1695 (5)	0.4235 (4)	0.3749 (7)	0.03453	0.4340 (12)
D14	0.1695 (5)	0.4235 (4)	0.3749 (7)	0.02442	0.5660 (12)
H15	0.2310 (5)	0.0937 (4)	0.3302 (7)	0.03014	0.4340 (12)
D15	0.2310 (5)	0.0937 (4)	0.3302 (7)	0.02131	0.5660 (12)
H16	0.2692 (5)	0.1263 (4)	0.1104 (7)	0.03012	0.4340 (12)
D16	0.2692 (5)	0.1263 (4)	0.1104 (7)	0.0213	0.5660 (12)
H17	0.7389 (4)	0.0941 (4)	−0.0622 (7)	0.02942	0.4340 (12)
D17	0.7389 (4)	0.0941 (4)	−0.0622 (7)	0.0208	0.5660 (12)
H18	0.8651 (4)	0.1849 (3)	−0.0031 (7)	0.02408	0.4340 (12)
D18	0.8651 (4)	0.1849 (3)	−0.0031 (7)	0.01702	0.5660 (12)
H19	0.8946 (5)	−0.0569 (4)	0.3173 (8)	0.03754	0.4340 (12)
D19	0.8946 (5)	−0.0569 (4)	0.3173 (8)	0.02654	0.5660 (12)
H20	0.0199 (5)	0.8582 (3)	0.3103 (7)	0.02625	0.4340 (12)
D20	0.0199 (5)	0.8582 (3)	0.3103 (7)	0.01856	0.5660 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0048 (5)	0.0048 (5)	0.0054 (5)	0.0003 (4)	0.0014 (4)	0.0000 (4)
S2	0.0032 (8)	0.0027 (9)	0.0067 (10)	0.0005 (8)	0.0012 (8)	0.0007 (8)
O3	0.0093 (5)	0.0054 (5)	0.0081 (5)	−0.0010 (5)	0.0029 (4)	0.0014 (4)
O4	0.0070 (5)	0.0078 (5)	0.0101 (5)	0.0012 (5)	0.0015 (4)	−0.0014 (5)
O5	0.0059 (5)	0.0059 (5)	0.0092 (5)	−0.0013 (5)	0.0015 (4)	−0.0009 (4)
O6	0.0091 (5)	0.0073 (5)	0.0068 (5)	−0.0009 (5)	0.0035 (4)	−0.0009 (4)
O7	0.0094 (5)	0.0084 (6)	0.0086 (5)	−0.0006 (5)	0.0025 (5)	0.0006 (5)
O8	0.0077 (5)	0.0053 (5)	0.0101 (5)	0.0004 (5)	0.0031 (4)	−0.0002 (4)
O9	0.0078 (5)	0.0082 (5)	0.0077 (5)	−0.0005 (5)	0.0039 (4)	0.0002 (5)
N10	0.00993 (33	0.0076 (4)	0.0096 (4)	−0.00055 (31	0.00316 (29	−0.00064 (29
H11	0.041 (4)	0.034 (4)	0.024 (3)	−0.006 (3)	0.003 (3)	−0.002 (3)
D11	0.029 (2)	0.024 (3)	0.017 (2)	−0.004 (2)	0.002 (2)	−0.002 (2)
H12	0.010 (2)	0.017 (3)	0.036 (3)	0.005 (2)	0.007 (2)	0.007 (3)
D12	0.0068 (17)	0.012 (2)	0.025 (2)	0.0032 (17)	0.0048 (17)	0.0051 (18)
H13	0.023 (3)	0.026 (3)	0.033 (3)	0.000 (3)	0.019 (3)	0.001 (3)
D13	0.016 (2)	0.018 (2)	0.023 (2)	0.0003 (19)	0.0135 (18)	0.0010 (19)
H14	0.044 (4)	0.020 (3)	0.038 (4)	−0.006 (3)	0.008 (3)	−0.009 (3)
D14	0.031 (3)	0.014 (2)	0.027 (3)	−0.005 (2)	0.006 (2)	−0.007 (2)
H15	0.031 (3)	0.037 (4)	0.018 (3)	−0.001 (3)	−0.000 (3)	0.007 (3)
D15	0.022 (2)	0.026 (3)	0.013 (2)	−0.001 (2)	−0.0002 (18)	0.0046 (19)
H16	0.026 (3)	0.042 (4)	0.027 (3)	−0.008 (3)	0.015 (3)	−0.003 (3)
D16	0.019 (2)	0.030 (3)	0.019 (2)	−0.006 (2)	0.0103 (18)	−0.002 (2)
H17	0.018 (3)	0.036 (4)	0.031 (3)	0.002 (3)	0.003 (3)	0.002 (3)
D17	0.0129 (19)	0.025 (3)	0.022 (2)	0.001 (2)	0.0018 (18)	0.002 (2)
H18	0.025 (3)	0.014 (3)	0.031 (3)	−0.000 (3)	0.004 (3)	0.000 (3)
D18	0.018 (2)	0.010 (2)	0.022 (2)	−0.0003 (19)	0.0026 (18)	0.0002 (18)
H19	0.031 (3)	0.040 (4)	0.047 (4)	−0.001 (3)	0.020 (3)	−0.002 (3)
D19	0.022 (2)	0.028 (3)	0.033 (3)	−0.001 (2)	0.014 (2)	−0.001 (2)
H20	0.033 (3)	0.019 (3)	0.027 (3)	0.006 (3)	0.008 (3)	0.004 (3)
D20	0.023 (2)	0.013 (2)	0.019 (2)	0.004 (2)	0.0055 (19)	0.0025 (18)

Geometric parameters (Å, º) top

Cu1—O7	2.2739 (14)	H12—H14	1.677 (6)
Cu1—O7ⁱ	2.2739 (14)	H12—D14	1.677 (6)
Cu1—O8ⁱⁱ	2.0012 (14)	D12—O3	2.004 (4)
Cu1—O8ⁱⁱⁱ	2.0012 (14)	D12—N10	1.019 (4)
Cu1—O9	1.9769 (14)	D12—H11	1.683 (6)
Cu1—O9ⁱ	1.9769 (14)	D12—D11	1.683 (6)
Cu1—H17ⁱⁱ	2.560 (4)	D12—H13	1.676 (5)
Cu1—H17ⁱⁱⁱ	2.560 (4)	D12—D13	1.676 (5)
Cu1—D17ⁱⁱ	2.560 (4)	D12—H14	1.677 (6)
Cu1—D17ⁱⁱⁱ	2.560 (4)	D12—D14	1.677 (6)
Cu1—H18ⁱⁱ	2.564 (4)	H13—S2^xiv	2.636 (5)
Cu1—H18ⁱⁱⁱ	2.564 (4)	H13—O3^xiv	1.858 (4)
Cu1—D18ⁱⁱ	2.564 (4)	H13—N10	1.035 (4)
Cu1—D18ⁱⁱⁱ	2.564 (4)	H13—H11	1.662 (6)
Cu1—H19ⁱⁱ	2.559 (5)	H13—D11	1.662 (6)
Cu1—H19ⁱⁱⁱ	2.559 (5)	H13—H12	1.676 (5)
Cu1—D19ⁱⁱ	2.559 (5)	H13—D12	1.676 (5)
Cu1—D19ⁱⁱⁱ	2.559 (5)	H13—H14	1.690 (6)
Cu1—H20^iv	2.591 (4)	H13—D14	1.690 (6)
Cu1—H20^v	2.591 (4)	D13—S2^xiv	2.636 (5)
Cu1—D20^iv	2.591 (4)	D13—O3^xiv	1.858 (4)
Cu1—D20^v	2.591 (4)	D13—N10	1.035 (4)
S2—O3	1.486 (3)	D13—H11	1.662 (6)
S2—O4	1.462 (3)	D13—D11	1.662 (6)
S2—O5	1.478 (3)	D13—H12	1.676 (5)
S2—O6	1.478 (3)	D13—D12	1.676 (5)
S2—H13^vi	2.636 (5)	D13—H14	1.690 (6)
S2—D13^vi	2.636 (5)	D13—D14	1.690 (6)
O3—S2	1.486 (3)	H14—O5^xv	1.816 (5)
O3—O5	2.3981 (19)	H14—N10	1.029 (4)
O3—H12	2.004 (4)	H14—H11	1.663 (6)
O3—D12	2.004 (4)	H14—D11	1.663 (6)
O3—H13^vi	1.858 (4)	H14—H12	1.677 (6)
O3—D13^vi	1.858 (4)	H14—D12	1.677 (6)
O3—H20^vii	1.720 (4)	H14—H13	1.690 (6)
O3—D20^vii	1.720 (4)	H14—D13	1.690 (6)
O4—S2	1.462 (3)	D14—O5^xv	1.816 (5)
O4—O5	2.3940 (19)	D14—N10	1.029 (4)
O4—H17^viii	1.693 (4)	D14—H11	1.663 (6)
O4—D17^viii	1.693 (4)	D14—D11	1.663 (6)
O5—S2	1.478 (3)	D14—H12	1.677 (6)
O5—O3	2.3981 (19)	D14—D12	1.677 (6)
O5—O4	2.3940 (19)	D14—H13	1.690 (6)
O5—H14^vii	1.816 (5)	D14—D13	1.690 (6)
O5—D14^vii	1.816 (5)	H15—O5	1.868 (4)
O5—H15	1.868 (4)	H15—O7	0.984 (4)
O5—D15	1.868 (4)	H15—H16	1.581 (6)
O5—H19^ix	1.746 (4)	H15—D16	1.581 (6)
O5—D19^ix	1.746 (4)	D15—O5	1.868 (4)
O6—S2	1.478 (3)	D15—O7	0.984 (4)
O6—H11^x	1.916 (5)	D15—H16	1.581 (6)
O6—D11^x	1.916 (5)	D15—D16	1.581 (6)
O6—H16^viii	1.892 (4)	H16—O6^xvi	1.892 (4)
O6—D16^viii	1.892 (4)	H16—O7	0.961 (4)
O6—H18^xi	1.731 (4)	H16—H15	1.581 (6)
O6—D18^xi	1.731 (4)	H16—D15	1.581 (6)
O7—Cu1	2.2739 (14)	D16—O6^xvi	1.892 (4)
O7—H15	0.984 (4)	D16—O7	0.961 (4)
O7—D15	0.984 (4)	D16—H15	1.581 (6)
O7—H16	0.961 (4)	D16—D15	1.581 (6)
O7—D16	0.961 (4)	H17—Cu1^xii	2.560 (4)
O8—Cu1^xii	2.0012 (14)	H17—O4^xvi	1.693 (4)
O8—H17	0.972 (4)	H17—O8	0.972 (4)
O8—D17	0.972 (4)	H17—H18	1.561 (6)
O8—H18	0.978 (4)	H17—D18	1.561 (6)
O8—D18	0.978 (4)	D17—Cu1^xii	2.560 (4)
O9—Cu1	1.9769 (14)	D17—O4^xvi	1.693 (4)
O9—H19ⁱⁱ	0.988 (4)	D17—O8	0.972 (4)
O9—D19ⁱⁱ	0.988 (4)	D17—H18	1.561 (6)
O9—H20^iv	0.977 (4)	D17—D18	1.561 (6)
O9—D20^iv	0.977 (4)	H18—Cu1^xii	2.564 (4)
N10—H11	1.021 (4)	H18—O6^xvii	1.731 (4)
N10—D11	1.021 (4)	H18—O8	0.978 (4)
N10—H12	1.019 (4)	H18—H17	1.561 (6)
N10—D12	1.019 (4)	H18—D17	1.561 (6)
N10—H13	1.035 (4)	D18—Cu1^xii	2.564 (4)
N10—D13	1.035 (4)	D18—O6^xvii	1.731 (4)
N10—H14	1.029 (4)	D18—O8	0.978 (4)
N10—D14	1.029 (4)	D18—H17	1.561 (6)
H11—O6^xiii	1.916 (5)	D18—D17	1.561 (6)
H11—N10	1.021 (4)	H19—Cu1^xii	2.559 (5)
H11—H12	1.683 (6)	H19—O5^ix	1.746 (4)
H11—D12	1.683 (6)	H19—O9^xii	0.988 (4)
H11—H13	1.662 (6)	H19—H20^xviii	1.547 (6)
H11—D13	1.662 (6)	H19—D20^xviii	1.547 (6)
H11—H14	1.663 (6)	D19—Cu1^xii	2.559 (5)
H11—D14	1.663 (6)	D19—O5^ix	1.746 (4)
D11—O6^xiii	1.916 (5)	D19—O9^xii	0.988 (4)
D11—N10	1.021 (4)	D19—H20^xviii	1.547 (6)
D11—H12	1.683 (6)	D19—D20^xviii	1.547 (6)
D11—D12	1.683 (6)	H20—Cu1^xix	2.591 (4)
D11—H13	1.662 (6)	H20—O3^xv	1.720 (4)
D11—D13	1.662 (6)	H20—O9^xix	0.977 (4)
D11—H14	1.663 (6)	H20—H19^xx	1.547 (6)
D11—D14	1.663 (6)	H20—D19^xx	1.547 (6)
H12—O3	2.004 (4)	D20—Cu1^xix	2.591 (4)
H12—N10	1.019 (4)	D20—O3^xv	1.720 (4)
H12—H11	1.683 (6)	D20—O9^xix	0.977 (4)
H12—D11	1.683 (6)	D20—H19^xx	1.547 (6)
H12—H13	1.676 (5)	D20—D19^xx	1.547 (6)
H12—D13	1.676 (5)

O8ⁱⁱ—Cu1—O8ⁱⁱⁱ	180.0	H11—N10—H12	111.2 (4)
O8ⁱⁱ—Cu1—O9	88.76 (6)	H11—N10—D12	111.2 (4)
O8ⁱⁱ—Cu1—O9ⁱ	91.24 (6)	H11—N10—H13	107.9 (4)
O8ⁱⁱⁱ—Cu1—O9	91.24 (6)	H11—N10—D13	107.9 (4)
O8ⁱⁱⁱ—Cu1—O9ⁱ	88.76 (6)	H11—N10—H14	108.4 (4)
O9—Cu1—O9ⁱ	179.972	H11—N10—D14	108.4 (4)
O3—S2—O4	109.60 (17)	D11—N10—H12	111.2 (4)
O3—S2—O5	107.99 (17)	D11—N10—D12	111.2 (4)
O3—S2—O6	109.06 (18)	D11—N10—H13	107.9 (4)
O4—S2—O5	109.02 (18)	D11—N10—D13	107.9 (4)
O4—S2—O6	111.09 (17)	D11—N10—H14	108.4 (4)
O5—S2—O6	110.03 (16)	D11—N10—D14	108.4 (4)
H15—O7—D15	0.0	H12—N10—D12	0.0
H15—O7—H16	108.8 (4)	H12—N10—H13	109.4 (3)
H15—O7—D16	108.8 (4)	H12—N10—D13	109.4 (3)
D15—O7—H16	108.8 (4)	H12—N10—H14	110.0 (3)
D15—O7—D16	108.8 (4)	H12—N10—D14	110.0 (3)
H16—O7—D16	0.0	D12—N10—H13	109.4 (3)
Cu1^xii—O8—H17	114.4 (3)	D12—N10—D13	109.4 (3)
Cu1^xii—O8—D17	114.4 (3)	D12—N10—H14	110.0 (3)
Cu1^xii—O8—H18	114.4 (3)	D12—N10—D14	110.0 (3)
Cu1^xii—O8—D18	114.4 (3)	H13—N10—D13	0.0
H17—O8—D17	0.0	H13—N10—H14	109.9 (4)
H17—O8—H18	106.5 (4)	H13—N10—D14	109.9 (4)
H17—O8—D18	106.5 (4)	D13—N10—H14	109.9 (4)
D17—O8—H18	106.5 (4)	D13—N10—D14	109.9 (4)
D17—O8—D18	106.5 (4)	H14—N10—D14	0.0
H18—O8—D18	0.0	O9^xii—H19—H20^xviii	37.8 (3)
Cu1—O9—H19ⁱⁱ	115.2 (3)	O9^xii—H19—D20^xviii	37.8 (3)
Cu1—O9—D19ⁱⁱ	115.2 (3)	H20^xviii—H19—D20^xviii	0.0
Cu1—O9—H20^iv	118.6 (3)	O9^xii—D19—H20^xviii	37.8 (3)
Cu1—O9—D20^iv	118.6 (3)	O9^xii—D19—D20^xviii	37.8 (3)
H19ⁱⁱ—O9—D19ⁱⁱ	0.0	H20^xviii—D19—D20^xviii	0.0
H19ⁱⁱ—O9—H20^iv	103.9 (4)	O9^xix—H20—H19^xx	38.3 (3)
H19ⁱⁱ—O9—D20^iv	103.9 (4)	O9^xix—H20—D19^xx	38.3 (3)
D19ⁱⁱ—O9—H20^iv	103.9 (4)	H19^xx—H20—D19^xx	0.0
D19ⁱⁱ—O9—D20^iv	103.9 (4)	O9^xix—D20—H19^xx	38.3 (3)
H20^iv—O9—D20^iv	0.0	O9^xix—D20—D19^xx	38.3 (3)
H11—N10—D11	0.0	H19^xx—D20—D19^xx	0.0

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x, y−1, z; (v) −x, −y+1, −z; (vi) x+1/2, −y+1/2, z; (vii) −x+1/2, y−1/2, −z+1; (viii) x, y, z+1; (ix) −x+1, −y, −z+1; (x) x+1/2, −y+1/2, z+1; (xi) x−1/2, −y+1/2, z+1; (xii) x+1, y, z; (xiii) x−1/2, −y+1/2, z−1; (xiv) x−1/2, −y+1/2, z; (xv) −x+1/2, y+1/2, −z+1; (xvi) x, y, z−1; (xvii) x+1/2, −y+1/2, z−1; (xviii) x+1, y−1, z; (xix) x, y+1, z; (xx) x−1, y+1, z.

(IPNS_SCD_D75_20K_phase_1) top

Crystal data top

(NH₄)₂[Cu(H2O)₆](SO₄)₂·25%H·75%D	β = 106.53 (2)°
M_r = 415.03	V = 674.7 (3) Å³
Monoclinic, P2₁/a	Z = 2
a = 9.093 (2) Å	D_x = 2.043 Mg m⁻³
b = 12.201 (3) Å	Neutron radiation
c = 6.344 (1) Å	T = 20 K

Data collection top

IPNS single crystal diffractometer	Not applicable to TOF Laue technique monochromator
Radiation source: Intense Pulsed Neutron Source

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.00614
S2	0.4196 (7)	0.1334 (5)	0.7439 (8)	0.0006 (10)*
O3	0.4310 (4)	0.2270 (3)	0.5959 (5)	0.00859
O4	0.5577 (4)	0.0665 (3)	0.7821 (5)	0.00799
O5	0.2843 (4)	0.0682 (3)	0.6313 (5)	0.00578
O6	0.4021 (4)	0.1783 (3)	0.9496 (5)	0.00763
O7	0.1868 (4)	0.1189 (3)	0.1772 (5)	0.00791
O8	0.8435 (4)	0.1092 (3)	0.0291 (5)	0.00845
O9	−0.0063 (4)	−0.0646 (3)	0.2819 (5)	0.00685
N10	0.1422 (3)	0.34169 (19)	0.3578 (4)	0.00981
H11	0.0793 (7)	0.3269 (5)	0.1955 (8)	0.03286	0.2444 (33)
D11	0.0793 (7)	0.3269 (5)	0.1955 (8)	0.02323	0.7556 (33)
H12	0.2384 (6)	0.2951 (4)	0.3997 (9)	0.02582	0.2444 (33)
D12	0.2384 (6)	0.2951 (4)	0.3997 (9)	0.01825	0.7556 (33)
H13	0.0748 (6)	0.3205 (5)	0.4601 (8)	0.02635	0.2444 (33)
D13	0.0748 (6)	0.3205 (5)	0.4601 (8)	0.01863	0.7556 (33)
H14	0.1698 (7)	0.4239 (5)	0.3763 (9)	0.03239	0.2444 (33)
D14	0.1698 (7)	0.4239 (5)	0.3763 (9)	0.0229	0.7556 (33)
H15	0.2327 (6)	0.0958 (5)	0.3258 (8)	0.02592	0.2444 (33)
D15	0.2327 (6)	0.0958 (5)	0.3258 (8)	0.01832	0.7556 (33)
H16	0.2704 (6)	0.1256 (5)	0.1094 (8)	0.02842	0.2444 (33)
D16	0.2704 (6)	0.1256 (5)	0.1094 (8)	0.02009	0.7556 (33)
H17	0.7388 (7)	0.0945 (4)	−0.0609 (8)	0.02894	0.2444 (33)
D17	0.7388 (7)	0.0945 (4)	−0.0609 (8)	0.02046	0.7556 (33)
H18	0.8649 (6)	0.1842 (4)	−0.0001 (8)	0.0242	0.2444 (33)
D18	0.8649 (6)	0.1842 (4)	−0.0001 (8)	0.01711	0.7556 (33)
H19	0.8942 (6)	−0.0551 (5)	0.3168 (8)	0.02771	0.2444 (33)
D19	0.8942 (6)	−0.0551 (5)	0.3168 (8)	0.01959	0.7556 (33)
H20	0.0198 (6)	0.8566 (4)	0.3105 (8)	0.02628	0.2444 (33)
D20	0.0198 (6)	0.8566 (4)	0.3105 (8)	0.01858	0.7556 (33)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0036 (15)	0.0089 (15)	0.0058 (13)	−0.0007 (12)	0.0011 (11)	0.0016 (12)
O3	0.0165 (18)	0.0062 (14)	0.0034 (12)	0.0026 (12)	0.0034 (12)	0.0024 (11)
O4	0.0068 (15)	0.0078 (14)	0.0074 (12)	0.0031 (12)	−0.0012 (11)	0.0008 (12)
O5	0.0053 (13)	0.0033 (12)	0.0094 (12)	−0.0017 (11)	0.0031 (11)	−0.0001 (11)
O6	0.0082 (15)	0.0110 (15)	0.0047 (12)	−0.0018 (12)	0.0034 (11)	−0.0017 (11)
O7	0.0077 (15)	0.0086 (15)	0.0080 (13)	0.0001 (13)	0.0032 (12)	0.0016 (12)
O8	0.0108 (16)	0.0071 (14)	0.0070 (12)	−0.0012 (13)	0.0020 (12)	0.0015 (12)
O9	0.0074 (14)	0.0059 (14)	0.0085 (12)	0.0003 (12)	0.0043 (11)	−0.0002 (12)
N10	0.0121 (11)	0.0076 (10)	0.0101 (9)	−0.0013 (9)	0.0037 (8)	−0.0006 (8)
H11	0.031 (4)	0.050 (5)	0.015 (3)	−0.006 (4)	0.003 (3)	−0.003 (4)
D11	0.022 (3)	0.035 (4)	0.010 (2)	−0.004 (3)	0.002 (2)	−0.002 (3)
H12	0.016 (4)	0.023 (4)	0.042 (4)	0.007 (3)	0.013 (3)	0.002 (3)
D12	0.011 (3)	0.017 (3)	0.030 (3)	0.005 (2)	0.009 (2)	0.001 (2)
H13	0.019 (4)	0.038 (5)	0.028 (4)	0.001 (3)	0.018 (3)	0.004 (3)
D13	0.014 (3)	0.027 (3)	0.020 (3)	0.001 (2)	0.013 (2)	0.003 (2)
H14	0.039 (5)	0.024 (4)	0.033 (4)	−0.008 (4)	0.011 (4)	−0.006 (4)
D14	0.028 (4)	0.017 (3)	0.024 (3)	−0.006 (3)	0.008 (3)	−0.004 (3)
H15	0.023 (4)	0.030 (5)	0.023 (4)	−0.004 (3)	0.004 (3)	−0.001 (3)
D15	0.016 (3)	0.021 (3)	0.016 (3)	−0.003 (2)	0.003 (2)	−0.001 (2)
H16	0.025 (4)	0.036 (4)	0.029 (4)	−0.006 (4)	0.015 (3)	−0.006 (4)
D16	0.018 (3)	0.026 (3)	0.020 (3)	−0.004 (3)	0.011 (2)	−0.004 (2)
H17	0.037 (5)	0.028 (4)	0.024 (4)	−0.008 (4)	0.012 (4)	0.001 (3)
D17	0.026 (3)	0.020 (3)	0.017 (3)	−0.005 (3)	0.009 (3)	0.000 (2)
H18	0.030 (4)	0.016 (4)	0.029 (4)	−0.001 (3)	0.012 (3)	0.003 (3)
D18	0.021 (3)	0.011 (3)	0.020 (3)	−0.001 (2)	0.009 (2)	0.002 (2)
H19	0.031 (4)	0.029 (4)	0.029 (4)	−0.004 (4)	0.018 (3)	−0.004 (3)
D19	0.022 (3)	0.021 (3)	0.020 (3)	−0.003 (3)	0.013 (2)	−0.003 (2)
H20	0.034 (5)	0.022 (4)	0.024 (4)	0.005 (3)	0.011 (3)	0.006 (3)
D20	0.024 (3)	0.016 (3)	0.017 (3)	0.004 (2)	0.008 (2)	0.004 (2)

Geometric parameters (Å, º) top

Cu1—O7	2.273 (3)	D12—H13	1.667 (7)
Cu1—O7ⁱ	2.273 (3)	D12—D13	1.667 (7)
Cu1—O8ⁱⁱ	1.996 (4)	D12—H14	1.682 (8)
Cu1—O8ⁱⁱⁱ	1.996 (4)	D12—D14	1.682 (8)
Cu1—O9	1.970 (3)	H13—O3^xiii	1.852 (6)
Cu1—O9ⁱ	1.970 (3)	H13—N10	1.044 (5)
S2—O3	1.501 (6)	H13—H11	1.693 (7)
S2—O4	1.459 (7)	H13—D11	1.693 (7)
S2—O5	1.469 (6)	H13—H12	1.667 (7)
S2—O6	1.464 (6)	H13—D12	1.667 (7)
O3—S2	1.501 (6)	H13—H14	1.698 (8)
O3—H12	2.016 (6)	H13—D14	1.698 (8)
O3—D12	2.016 (6)	D13—O3^xiii	1.852 (6)
O3—H13^iv	1.852 (6)	D13—N10	1.044 (5)
O3—D13^iv	1.852 (6)	D13—H11	1.693 (7)
O3—H20^v	1.703 (6)	D13—D11	1.693 (7)
O3—D20^v	1.703 (6)	D13—H12	1.667 (7)
O4—S2	1.459 (7)	D13—D12	1.667 (7)
O4—H17^vi	1.699 (6)	D13—H14	1.698 (8)
O4—D17^vi	1.699 (6)	D13—D14	1.698 (8)
O5—S2	1.469 (6)	H14—O5^xiv	1.813 (7)
O5—H14^v	1.813 (7)	H14—N10	1.033 (6)
O5—D14^v	1.813 (7)	H14—H11	1.690 (8)
O5—H15	1.890 (6)	H14—D11	1.690 (8)
O5—D15	1.890 (6)	H14—H12	1.682 (8)
O5—H19^vii	1.753 (6)	H14—D12	1.682 (8)
O5—D19^vii	1.753 (6)	H14—H13	1.698 (8)
O6—S2	1.464 (6)	H14—D13	1.698 (8)
O6—H11^viii	1.898 (6)	D14—O5^xiv	1.813 (7)
O6—D11^viii	1.898 (6)	D14—N10	1.033 (6)
O6—H16^vi	1.889 (6)	D14—H11	1.690 (8)
O6—D16^vi	1.889 (6)	D14—D11	1.690 (8)
O6—H18^ix	1.759 (6)	D14—H12	1.682 (8)
O6—D18^ix	1.759 (6)	D14—D12	1.682 (8)
O7—Cu1	2.273 (3)	D14—H13	1.698 (8)
O7—H15	0.958 (5)	D14—D13	1.698 (8)
O7—D15	0.958 (5)	H15—O5	1.890 (6)
O7—H16	0.977 (6)	H15—O7	0.958 (5)
O7—D16	0.977 (6)	H15—H16	1.550 (7)
O8—Cu1^x	1.996 (4)	H15—D16	1.550 (7)
O8—H17	0.977 (6)	D15—O5	1.890 (6)
O8—D17	0.977 (6)	D15—O7	0.958 (5)
O8—H18	0.964 (6)	D15—H16	1.550 (7)
O8—D18	0.964 (6)	D15—D16	1.550 (7)
O9—Cu1	1.970 (3)	H16—O6^xv	1.889 (6)
O9—H19ⁱⁱ	0.997 (6)	H16—O7	0.977 (6)
O9—D19ⁱⁱ	0.997 (6)	H16—H15	1.550 (7)
O9—H20^xi	0.994 (6)	H16—D15	1.550 (7)
O9—D20^xi	0.994 (6)	D16—O6^xv	1.889 (6)
N10—H11	1.041 (5)	D16—O7	0.977 (6)
N10—D11	1.041 (5)	D16—H15	1.550 (7)
N10—H12	1.013 (5)	D16—D15	1.550 (7)
N10—D12	1.013 (5)	H17—O4^xv	1.699 (6)
N10—H13	1.044 (5)	H17—O8	0.977 (6)
N10—D13	1.044 (5)	H17—H18	1.552 (7)
N10—H14	1.033 (6)	H17—D18	1.552 (7)
N10—D14	1.033 (6)	D17—O4^xv	1.699 (6)
H11—O6^xii	1.898 (6)	D17—O8	0.977 (6)
H11—N10	1.041 (5)	D17—H18	1.552 (7)
H11—H12	1.690 (8)	D17—D18	1.552 (7)
H11—D12	1.690 (8)	H18—O6^xvi	1.759 (6)
H11—H13	1.693 (7)	H18—O8	0.964 (6)
H11—D13	1.693 (7)	H18—H17	1.552 (7)
H11—H14	1.690 (8)	H18—D17	1.552 (7)
H11—D14	1.690 (8)	D18—O6^xvi	1.759 (6)
D11—O6^xii	1.898 (6)	D18—O8	0.964 (6)
D11—N10	1.041 (5)	D18—H17	1.552 (7)
D11—H12	1.690 (8)	D18—D17	1.552 (7)
D11—D12	1.690 (8)	H19—O5^vii	1.753 (6)
D11—H13	1.693 (7)	H19—O9^x	0.997 (6)
D11—D13	1.693 (7)	H19—H20^xvii	1.578 (8)
D11—H14	1.690 (8)	H19—D20^xvii	1.578 (8)
D11—D14	1.690 (8)	D19—O5^vii	1.753 (6)
H12—O3	2.016 (6)	D19—O9^x	0.997 (6)
H12—N10	1.013 (5)	D19—H20^xvii	1.578 (8)
H12—H11	1.690 (8)	D19—D20^xvii	1.578 (8)
H12—D11	1.690 (8)	H20—O3^xiv	1.703 (6)
H12—H13	1.667 (7)	H20—O9^xviii	0.994 (6)
H12—D13	1.667 (7)	H20—H19^xix	1.578 (8)
H12—H14	1.682 (8)	H20—D19^xix	1.578 (8)
H12—D14	1.682 (8)	D20—O3^xiv	1.703 (6)
D12—O3	2.016 (6)	D20—O9^xviii	0.994 (6)
D12—N10	1.013 (5)	D20—H19^xix	1.578 (8)
D12—H11	1.690 (8)	D20—D19^xix	1.578 (8)
D12—D11	1.690 (8)

O8ⁱⁱ—Cu1—O8ⁱⁱⁱ	180.0	D11—N10—H12	110.7 (5)
O8ⁱⁱ—Cu1—O9	88.71 (14)	D11—N10—D12	110.7 (5)
O8ⁱⁱ—Cu1—O9ⁱ	91.29 (14)	D11—N10—H13	108.5 (5)
O8ⁱⁱⁱ—Cu1—O9	91.29 (14)	D11—N10—D13	108.5 (5)
O8ⁱⁱⁱ—Cu1—O9ⁱ	88.71 (14)	D11—N10—H14	109.1 (5)
O9—Cu1—O9ⁱ	179.9802	D11—N10—D14	109.1 (5)
O3—S2—O4	108.7 (4)	H12—N10—D12	0.0
O3—S2—O5	107.8 (4)	H12—N10—H13	108.3 (5)
O3—S2—O6	108.5 (4)	H12—N10—D13	108.3 (5)
O4—S2—O5	109.9 (4)	H12—N10—H14	110.6 (5)
O4—S2—O6	111.6 (4)	H12—N10—D14	110.6 (5)
O5—S2—O6	110.4 (4)	D12—N10—H13	108.3 (5)
H15—O7—D15	0.0	D12—N10—D13	108.3 (5)
H15—O7—H16	106.4 (6)	D12—N10—H14	110.6 (5)
H15—O7—D16	106.4 (6)	D12—N10—D14	110.6 (5)
D15—O7—H16	106.4 (6)	H13—N10—D13	0.0
D15—O7—D16	106.4 (6)	H13—N10—H14	109.7 (5)
H16—O7—D16	0.0	H13—N10—D14	109.7 (5)
Cu1^x—O8—H17	115.1 (4)	D13—N10—H14	109.7 (5)
Cu1^x—O8—D17	115.1 (4)	D13—N10—D14	109.7 (5)
Cu1^x—O8—H18	115.3 (4)	H14—N10—D14	0.0
Cu1^x—O8—D18	115.3 (4)	O7—H15—H16	37.2 (4)
H17—O8—D17	0.0	O7—H15—D16	37.2 (4)
H17—O8—H18	106.2 (6)	H16—H15—D16	0.0
H17—O8—D18	106.2 (6)	O7—D15—H16	37.2 (4)
D17—O8—H18	106.2 (6)	O7—D15—D16	37.2 (4)
D17—O8—D18	106.2 (6)	H16—D15—D16	0.0
H18—O8—D18	0.0	O7—H16—H15	36.4 (3)
Cu1—O9—H19ⁱⁱ	114.7 (4)	O7—H16—D15	36.4 (3)
Cu1—O9—D19ⁱⁱ	114.7 (4)	H15—H16—D15	0.0
Cu1—O9—H20^xi	119.0 (4)	O7—D16—H15	36.4 (3)
Cu1—O9—D20^xi	119.0 (4)	O7—D16—D15	36.4 (3)
H19ⁱⁱ—O9—D19ⁱⁱ	0.0	H15—D16—D15	0.0
H19ⁱⁱ—O9—H20^xi	104.8 (6)	O8—H17—H18	36.6 (3)
H19ⁱⁱ—O9—D20^xi	104.8 (6)	O8—H17—D18	36.6 (3)
D19ⁱⁱ—O9—H20^xi	104.8 (6)	H18—H17—D18	0.0
D19ⁱⁱ—O9—D20^xi	104.8 (6)	O8—D17—H18	36.6 (3)
H20^xi—O9—D20^xi	0.0	O8—D17—D18	36.6 (3)
H11—N10—D11	0.0	H18—D17—D18	0.0
H11—N10—H12	110.7 (5)	O8—H18—H17	37.2 (3)
H11—N10—D12	110.7 (5)	O8—H18—D17	37.2 (3)
H11—N10—H13	108.5 (5)	H17—H18—D17	0.0
H11—N10—D13	108.5 (5)	O8—D18—H17	37.2 (3)
H11—N10—H14	109.1 (5)	O8—D18—D17	37.2 (3)
H11—N10—D14	109.1 (5)	H17—D18—D17	0.0

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x+1/2, −y+1/2, z; (v) −x+1/2, y−1/2, −z+1; (vi) x, y, z+1; (vii) −x+1, −y, −z+1; (viii) x+1/2, −y+1/2, z+1; (ix) x−1/2, −y+1/2, z+1; (x) x+1, y, z; (xi) x, y−1, z; (xii) x−1/2, −y+1/2, z−1; (xiii) x−1/2, −y+1/2, z; (xiv) −x+1/2, y+1/2, −z+1; (xv) x, y, z−1; (xvi) x+1/2, −y+1/2, z−1; (xvii) x+1, y−1, z; (xviii) x, y+1, z; (xix) x−1, y+1, z.

(IPNS_SCD_D80_20K_phase_1) top

Crystal data top

(NH₄)₂[Cu(H2O)₆](SO₄)₂·20%H·80%D	β = 107.21 (3)°
M_r = 416.48	V = 689.0 (8) Å³
Monoclinic, P2₁/a	Z = 2
a = 9.394 (2) Å	D_x = 2.008 Mg m⁻³
b = 12.664 (3) Å	Neutron radiation
c = 6.063 (7) Å	T = 20 K

Data collection top

IPNS single crystal diffractometer	Not applicable to TOF Laue technique monochromator
Radiation source: Intense Pulsed Neutron Source

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.00408
S2	0.3868 (4)	0.1435 (3)	0.7490 (4)	0.00452
O3	0.38110 (19)	0.23899 (15)	0.6064 (2)	0.00682
O4	0.52741 (18)	0.08694 (16)	0.7755 (2)	0.00703
O5	0.26085 (18)	0.07326 (15)	0.6304 (2)	0.00648
O6	0.37305 (18)	0.17312 (15)	0.9783 (2)	0.00619
O7	0.15148 (19)	0.10765 (15)	0.1647 (2)	0.00726
O8	−0.1809 (2)	0.11218 (17)	0.0503 (2)	0.0084
O9	0.00982 (19)	−0.06613 (15)	0.2969 (2)	0.00621
N10	0.12577 (13)	0.36429 (10)	0.37774 (14)	0.00782
D11	0.0415 (3)	0.3464 (2)	0.2319 (3)	0.01798	0.8277 (18)
H11	0.0415 (3)	0.3464 (2)	0.2319 (3)	0.01898	0.1723 (18)
D12	0.2043 (3)	0.3051 (3)	0.4237 (4)	0.01849	0.8277 (18)
H12	0.2043 (3)	0.3051 (3)	0.4237 (4)	0.01879	0.1723 (18)
D13	0.0822 (3)	0.3776 (2)	0.5118 (3)	0.0175	0.8277 (18)
H13	0.0822 (3)	0.3776 (2)	0.5118 (3)	0.01975	0.1723 (18)
D14	0.1771 (3)	0.4334 (2)	0.3515 (3)	0.01939	0.8277 (18)
H14	0.1771 (3)	0.4334 (2)	0.3515 (3)	0.02004	0.1723 (18)
D15	0.1960 (3)	0.0932 (2)	0.3293 (3)	0.01598	0.8277 (18)
H15	0.1960 (3)	0.0932 (2)	0.3293 (3)	0.01756	0.1723 (18)
D16	0.2311 (3)	0.1258 (2)	0.0986 (3)	0.01655	0.8277 (18)
H16	0.2311 (3)	0.1258 (2)	0.0986 (3)	0.01794	0.1723 (18)
D17	−0.2838 (3)	0.1021 (2)	−0.0447 (3)	0.01616	0.8277 (18)
H17	−0.2838 (3)	0.1021 (2)	−0.0447 (3)	0.01649	0.1723 (18)
D18	−0.1579 (3)	0.1855 (2)	0.0292 (3)	0.01804	0.8277 (18)
H18	−0.1579 (3)	0.1855 (2)	0.0292 (3)	0.0184	0.1723 (18)
D19	−0.0849 (3)	−0.0637 (2)	0.3321 (3)	0.01612	0.8277 (18)
H19	−0.0849 (3)	−0.0637 (2)	0.3321 (3)	0.01734	0.1723 (18)
D20	0.0434 (3)	−0.1401 (2)	0.3172 (3)	0.01605	0.8277 (18)
H20	0.0434 (3)	−0.1401 (2)	0.3172 (3)	0.0171	0.1723 (18)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0021 (7)	0.0061 (9)	0.0038 (4)	0.0005 (6)	0.0005 (4)	0.0010 (4)
S2	0.0033 (14)	0.0063 (18)	0.0039 (8)	−0.0012 (11)	0.0009 (8)	−0.0002 (8)
O3	0.0069 (8)	0.0070 (10)	0.0066 (4)	0.0004 (6)	0.0020 (5)	0.0012 (4)
O4	0.0035 (7)	0.0094 (10)	0.0084 (4)	0.0019 (6)	0.0021 (5)	0.0003 (5)
O5	0.0036 (7)	0.0087 (10)	0.0069 (4)	−0.0007 (6)	0.0012 (5)	−0.0003 (4)
O6	0.0064 (8)	0.0068 (9)	0.0059 (4)	−0.0007 (6)	0.0025 (5)	−0.0009 (4)
O7	0.0046 (8)	0.0106 (11)	0.0063 (4)	−0.0026 (6)	0.0012 (5)	−0.0001 (5)
O8	0.0070 (8)	0.0101 (11)	0.0083 (5)	−0.0010 (6)	0.0026 (5)	−0.0005 (5)
O9	0.0052 (7)	0.0075 (10)	0.0062 (4)	0.0003 (6)	0.0022 (5)	0.0008 (4)
N10	0.0060 (5)	0.0094 (7)	0.00804 (30	−0.0007 (4)	0.00204 (32	0.00004 (31
D11	0.0144 (14)	0.023 (2)	0.0130 (7)	−0.0042 (11)	−0.0014 (8)	−0.0023 (8)
H11	0.014 (2)	0.026 (3)	0.0119 (10)	−0.0059 (16)	−0.0039 (11)	−0.0032 (11)
D12	0.0152 (15)	0.0180 (19)	0.0228 (9)	0.0063 (12)	0.0066 (10)	0.0033 (9)
H12	0.014 (2)	0.018 (3)	0.0249 (13)	0.0089 (17)	0.0072 (14)	0.0047 (13)
D13	0.0152 (13)	0.0265 (18)	0.0145 (7)	0.0026 (11)	0.0099 (8)	−0.0003 (8)
H13	0.0165 (18)	0.032 (3)	0.0154 (10)	0.0037 (16)	0.0125 (11)	−0.0004 (12)
D14	0.0205 (15)	0.0175 (19)	0.0204 (9)	−0.0052 (13)	0.0063 (9)	0.0020 (9)
H14	0.022 (2)	0.017 (3)	0.0214 (12)	−0.0073 (18)	0.0067 (13)	0.0028 (13)
D15	0.0131 (14)	0.0233 (17)	0.0095 (7)	−0.0003 (11)	0.0000 (7)	0.0013 (7)
H15	0.0135 (19)	0.028 (3)	0.0083 (9)	−0.0004 (15)	−0.0014 (10)	0.0019 (10)
D16	0.0134 (13)	0.0205 (18)	0.0185 (8)	−0.0047 (11)	0.0088 (9)	−0.0008 (8)
H16	0.0134 (18)	0.024 (3)	0.0207 (11)	−0.0066 (15)	0.0109 (12)	−0.0012 (11)
D17	0.0074 (12)	0.020 (2)	0.0181 (8)	−0.0030 (10)	−0.0008 (8)	−0.0020 (8)
H17	0.0041 (18)	0.022 (3)	0.0192 (11)	−0.0043 (14)	−0.0030 (12)	−0.0028 (11)
D18	0.0182 (15)	0.0155 (19)	0.0211 (9)	−0.0021 (12)	0.0069 (9)	0.0005 (9)
H18	0.019 (2)	0.015 (3)	0.0228 (12)	−0.0030 (17)	0.0076 (13)	0.0007 (12)
D19	0.0112 (12)	0.0207 (18)	0.0193 (8)	0.0032 (10)	0.0091 (9)	0.0020 (8)
H19	0.0104 (18)	0.024 (3)	0.0219 (11)	0.0045 (15)	0.0112 (12)	0.0029 (12)
D20	0.0172 (14)	0.0149 (17)	0.0170 (8)	0.0026 (11)	0.0065 (8)	0.0018 (8)
H20	0.019 (2)	0.015 (2)	0.0184 (11)	0.0036 (16)	0.0075 (12)	0.0025 (11)

Geometric parameters (Å, º) top

Cu1—O7	2.0099 (19)	H12—D13	1.675 (3)
Cu1—O7ⁱ	2.0099 (19)	H12—H13	1.675 (3)
Cu1—O8	2.3032 (19)	H12—D14	1.683 (4)
Cu1—O8ⁱ	2.3032 (19)	H12—H14	1.683 (4)
Cu1—O9	1.963 (2)	D13—O4^x	1.874 (3)
Cu1—O9ⁱ	1.963 (2)	D13—N10	1.0264 (19)
S2—O3	1.478 (4)	D13—D11	1.673 (3)
S2—O4	1.469 (4)	D13—H11	1.673 (3)
S2—O5	1.485 (4)	D13—D12	1.675 (3)
S2—O6	1.482 (3)	D13—H12	1.675 (3)
O3—S2	1.478 (4)	D13—D14	1.659 (3)
O3—D12	1.897 (3)	D13—H14	1.659 (3)
O3—H12	1.897 (3)	H13—O4^x	1.874 (3)
O3—D20ⁱⁱ	1.694 (3)	H13—N10	1.0264 (19)
O3—H20ⁱⁱ	1.694 (3)	H13—D11	1.673 (3)
O4—S2	1.469 (4)	H13—H11	1.673 (3)
O4—D13ⁱⁱⁱ	1.874 (3)	H13—D12	1.675 (3)
O4—H13ⁱⁱⁱ	1.874 (3)	H13—H12	1.675 (3)
O4—D17^iv	1.796 (3)	H13—D14	1.659 (3)
O4—H17^iv	1.796 (3)	H13—H14	1.659 (3)
O5—S2	1.485 (4)	D14—O5ⁱⁱ	1.857 (3)
O5—D14^v	1.857 (3)	D14—N10	1.034 (3)
O5—H14^v	1.857 (3)	D14—D11	1.679 (4)
O5—D15	1.764 (3)	D14—H11	1.679 (4)
O5—H15	1.764 (3)	D14—D12	1.683 (4)
O5—D19^vi	1.738 (3)	D14—H12	1.683 (4)
O5—H19^vi	1.738 (3)	D14—D13	1.659 (3)
O6—S2	1.482 (3)	D14—H13	1.659 (3)
O6—D11^vii	1.868 (3)	H14—O5ⁱⁱ	1.857 (3)
O6—H11^vii	1.868 (3)	H14—N10	1.034 (3)
O6—D16^viii	1.801 (3)	H14—D11	1.679 (4)
O6—H16^viii	1.801 (3)	H14—H11	1.679 (4)
O6—D18^vii	1.855 (4)	H14—D12	1.683 (4)
O6—H18^vii	1.855 (4)	H14—H12	1.683 (4)
O7—Cu1	2.0099 (19)	H14—D13	1.659 (3)
O7—D15	0.978 (3)	H14—H13	1.659 (3)
O7—H15	0.978 (3)	D15—O5	1.764 (3)
O7—D16	0.975 (2)	D15—O7	0.978 (3)
O7—H16	0.975 (2)	D15—D16	1.584 (3)
O8—Cu1	2.3032 (19)	D15—H16	1.584 (3)
O8—D17	0.977 (3)	H15—O5	1.764 (3)
O8—H17	0.977 (3)	H15—O7	0.978 (3)
O8—D18	0.970 (3)	H15—D16	1.584 (3)
O8—H18	0.970 (3)	H15—H16	1.584 (3)
O9—Cu1	1.963 (2)	D16—O6^xi	1.801 (3)
O9—D19	0.975 (3)	D16—O7	0.975 (2)
O9—H19	0.975 (3)	D16—D15	1.584 (3)
O9—D20	0.984 (3)	D16—H15	1.584 (3)
O9—H20	0.984 (3)	H16—O6^xi	1.801 (3)
N10—D11	1.023 (3)	H16—O7	0.975 (2)
N10—H11	1.023 (3)	H16—D15	1.584 (3)
N10—D12	1.030 (3)	H16—H15	1.584 (3)
N10—H12	1.030 (3)	D17—O4^xii	1.796 (3)
N10—D13	1.0264 (19)	D17—O8	0.977 (3)
N10—H13	1.0264 (19)	D17—D18	1.549 (4)
N10—D14	1.034 (3)	D17—H18	1.549 (4)
N10—H14	1.034 (3)	H17—O4^xii	1.796 (3)
D11—O6^ix	1.868 (3)	H17—O8	0.977 (3)
D11—N10	1.023 (3)	H17—D18	1.549 (4)
D11—D12	1.707 (4)	H17—H18	1.549 (4)
D11—H12	1.707 (4)	D18—O6^ix	1.855 (4)
D11—D13	1.673 (3)	D18—O8	0.970 (3)
D11—H13	1.673 (3)	D18—D17	1.549 (4)
D11—D14	1.679 (4)	D18—H17	1.549 (4)
D11—H14	1.679 (4)	H18—O6^ix	1.855 (4)
H11—O6^ix	1.868 (3)	H18—O8	0.970 (3)
H11—N10	1.023 (3)	H18—D17	1.549 (4)
H11—D12	1.707 (4)	H18—H17	1.549 (4)
H11—H12	1.707 (4)	D19—O5^vi	1.738 (3)
H11—D13	1.673 (3)	D19—O9	0.975 (3)
H11—H13	1.673 (3)	D19—D20	1.569 (4)
H11—D14	1.679 (4)	D19—H20	1.569 (4)
H11—H14	1.679 (4)	H19—O5^vi	1.738 (3)
D12—O3	1.897 (3)	H19—O9	0.975 (3)
D12—N10	1.030 (3)	H19—D20	1.569 (4)
D12—D11	1.707 (4)	H19—H20	1.569 (4)
D12—H11	1.707 (4)	D20—O3^v	1.694 (3)
D12—D13	1.675 (3)	D20—O9	0.984 (3)
D12—H13	1.675 (3)	D20—D19	1.569 (4)
D12—D14	1.683 (4)	D20—H19	1.569 (4)
D12—H14	1.683 (4)	H20—O3^v	1.694 (3)
H12—O3	1.897 (3)	H20—O9	0.984 (3)
H12—N10	1.030 (3)	H20—D19	1.569 (4)
H12—D11	1.707 (4)	H20—H19	1.569 (4)
H12—H11	1.707 (4)

O7—Cu1—O7ⁱ	180.0	D11—N10—D12	112.5 (3)
O7—Cu1—O9	89.97 (8)	D11—N10—H12	112.5 (3)
O7—Cu1—O9ⁱ	90.03 (8)	D11—N10—D13	109.4 (2)
O7ⁱ—Cu1—O9	90.03 (8)	D11—N10—H13	109.4 (2)
O7ⁱ—Cu1—O9ⁱ	89.97 (8)	D11—N10—D14	109.4 (2)
O9—Cu1—O9ⁱ	179.972	D11—N10—H14	109.4 (2)
O3—S2—O4	109.80 (19)	H11—N10—D12	112.5 (3)
O3—S2—O5	108.7 (2)	H11—N10—H12	112.5 (3)
O3—S2—O6	110.1 (2)	H11—N10—D13	109.4 (2)
O4—S2—O5	108.8 (3)	H11—N10—H13	109.4 (2)
O4—S2—O6	110.2 (2)	H11—N10—D14	109.4 (2)
O5—S2—O6	109.12 (19)	H11—N10—H14	109.4 (2)
Cu1—O7—D15	113.9 (2)	D12—N10—H12	0.0
Cu1—O7—H15	113.9 (2)	D12—N10—D13	109.03 (19)
Cu1—O7—D16	118.18 (19)	D12—N10—H13	109.03 (19)
Cu1—O7—H16	118.18 (19)	D12—N10—D14	109.2 (3)
D15—O7—H15	0.0	D12—N10—H14	109.2 (3)
D15—O7—D16	108.4 (3)	H12—N10—D13	109.03 (19)
D15—O7—H16	108.4 (3)	H12—N10—H13	109.03 (19)
H15—O7—D16	108.4 (3)	H12—N10—D14	109.2 (3)
H15—O7—H16	108.4 (3)	H12—N10—H14	109.2 (3)
D16—O7—H16	0.0	D13—N10—H13	0.0
D17—O8—H17	0.0	D13—N10—D14	107.3 (2)
D17—O8—D18	105.5 (3)	D13—N10—H14	107.3 (2)
D17—O8—H18	105.5 (3)	H13—N10—D14	107.3 (2)
H17—O8—D18	105.5 (3)	H13—N10—H14	107.3 (2)
H17—O8—H18	105.5 (3)	D14—N10—H14	0.0
D18—O8—H18	0.0	O8—D17—D18	37.09 (19)
Cu1—O9—D19	112.9 (2)	O8—D17—H18	37.09 (19)
Cu1—O9—H19	112.9 (2)	D18—D17—H18	0.0
Cu1—O9—D20	116.55 (14)	O8—H17—D18	37.09 (19)
Cu1—O9—H20	116.55 (14)	O8—H17—H18	37.09 (19)
D19—O9—H19	0.0	D18—H17—H18	0.0
D19—O9—D20	106.4 (3)	O8—D18—D17	37.40 (18)
D19—O9—H20	106.4 (3)	O8—D18—H17	37.40 (18)
H19—O9—D20	106.4 (3)	D17—D18—H17	0.0
H19—O9—H20	106.4 (3)	O8—H18—D17	37.40 (18)
D20—O9—H20	0.0	O8—H18—H17	37.40 (18)
D11—N10—H11	0.0	D17—H18—H17	0.0

Symmetry codes: (i) −x, −y, −z; (ii) −x+1/2, y+1/2, −z+1; (iii) x+1/2, −y+1/2, z; (iv) x+1, y, z+1; (v) −x+1/2, y−1/2, −z+1; (vi) −x, −y, −z+1; (vii) x+1/2, −y+1/2, z+1; (viii) x, y, z+1; (ix) x−1/2, −y+1/2, z−1; (x) x−1/2, −y+1/2, z; (xi) x, y, z−1; (xii) x−1, y, z−1.

(CuTS_50D_100K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.99D_2.01⁺)₂·CuH_6.28D_5.72O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 409.61	F(000) = 280
Monoclinic, P2₁/a	D_x = 2.005 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.0974 (3) Å	Cell parameters from 29899 reflections
b = 12.2272 (4) Å	µ = 0.17 mm⁻¹
c = 6.3523 (2) Å	T = 100 K
β = 106.251 (2)°	Block, blue
V = 678.37 (4) Å³	2.7 × 1.5 × 1.0 mm

Data collection top

TOPAZ Single Crystal Diffractometer	9578 measured reflections
Radiation source: spallation neutron source, SNS BL12	8053 independent reflections
Not applicable to TOF Laue technique monochromator	6949 reflections with > 3σ(I)
time–of–flight Laue scans	h = −17→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 1.110 + 0.588 * lambda [cm^-1] The value of 1.698(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −24→24
T_min = 0.608, T_max = 0.813	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.100	(Δ/σ)_max < 0.001
wR(F²) = 0.089	Δρ_max = 0.16E-12 cm Å^-3 e Å⁻³
S = 1.44	Δρ_min = −0.28E−12 cm Å⁻³ e Å⁻³
6949 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
194 parameters	Extinction coefficient: 8.3E-06 (3)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.00722
S2	0.41976 (13)	0.13485 (8)	0.74391 (19)	0.0073
O3	0.42940 (7)	0.22783 (4)	0.59727 (10)	0.01121
O4	0.55759 (7)	0.06790 (4)	0.78324 (11)	0.01404
O5	0.28468 (7)	0.06804 (4)	0.63280 (10)	0.01062
O6	0.40115 (8)	0.17908 (4)	0.95167 (10)	0.01183
O7	0.18682 (8)	0.11863 (4)	0.17838 (11)	0.01173
O8	−0.15743 (7)	0.10932 (4)	0.02885 (11)	0.01059
O9	−0.00698 (7)	−0.06459 (4)	0.28183 (10)	0.01039
N10	0.14119 (5)	0.341926 (27	0.35759 (7)	0.01214
D11	0.0785 (4)	0.3275 (2)	0.1999 (5)	0.03916	0.5024 (9)
D12	0.2376 (4)	0.29546 (19)	0.3978 (6)	0.03339	0.5024 (9)
D13	0.0746 (3)	0.3214 (2)	0.4565 (5)	0.02772	0.5024 (9)
D14	0.1688 (4)	0.42335 (19)	0.3731 (5)	0.0309	0.5024 (9)
D15	0.2317 (4)	0.0949 (2)	0.3277 (5)	0.02566	0.4768 (6)
D16	0.2680 (4)	0.1265 (2)	0.1095 (5)	0.02555	0.4768 (6)
D17	−0.2616 (4)	0.0947 (2)	−0.0611 (6)	0.02546	0.4768 (6)
D18	−0.1337 (4)	0.18474 (19)	−0.0022 (5)	0.02138	0.4768 (6)
D19	−0.1052 (4)	−0.0565 (2)	0.3135 (5)	0.02864	0.4768 (6)
D20	0.0201 (4)	−0.14168 (19)	0.3089 (5)	0.01991	0.4768 (6)
H11	0.0785 (4)	0.3275 (2)	0.1999 (5)	0.05537	0.4976 (9)
H12	0.2376 (4)	0.29546 (19)	0.3978 (6)	0.04721	0.4976 (9)
H13	0.0746 (3)	0.3214 (2)	0.4565 (5)	0.0392	0.4976 (9)
H14	0.1688 (4)	0.42335 (19)	0.3731 (5)	0.0437	0.4976 (9)
H15	0.2317 (4)	0.0949 (2)	0.3277 (5)	0.03629	0.5232 (6)
H16	0.2680 (4)	0.1265 (2)	0.1095 (5)	0.03613	0.5232 (6)
H17	−0.2616 (4)	0.0947 (2)	−0.0611 (6)	0.036	0.5232 (6)
H18	−0.1337 (4)	0.18474 (19)	−0.0022 (5)	0.03024	0.5232 (6)
H19	−0.1052 (4)	−0.0565 (2)	0.3135 (5)	0.0405	0.5232 (6)
H20	0.0201 (4)	−0.14168 (19)	0.3089 (5)	0.02816	0.5232 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.00675 (24	0.00737 (17	0.00738 (24	0.00015 (17	0.00173 (24	0.00064 (18
S2	0.0065 (5)	0.00739 (33	0.0074 (5)	0.00011 (32	0.0010 (5)	−0.00037 (33
O3	0.01424 (29	0.00923 (18	0.01051 (25	−0.00161 (18	0.00403 (26	0.00055 (19
O4	0.00931 (26	0.01331 (20	0.01810 (30	0.00269 (20	0.00156 (28	−0.00085 (22
O5	0.00933 (25	0.01065 (18	0.01153 (25	−0.00241 (18	0.00234 (25	−0.00151 (19
O6	0.01577 (30	0.01089 (19	0.00927 (25	−0.00038 (19	0.00424 (27	−0.00099 (18
O7	0.01137 (28	0.01218 (20	0.01082 (26	−0.00191 (19	0.00177 (27	−0.00064 (19
O8	0.00946 (26	0.00943 (18	0.01293 (28	0.00057 (18	0.00320 (27	0.00014 (19
O9	0.01136 (26	0.01040 (18	0.00989 (24	0.00104 (18	0.00376 (25	0.00177 (19
N10	0.01329 (18	0.01146 (13	0.01210 (18	0.00007 (12	0.00426 (18	−0.00027 (12
D11	0.048 (3)	0.0497 (19)	0.0203 (18)	−0.0193 (17)	0.010 (2)	−0.0058 (15)
D12	0.0265 (18)	0.0239 (13)	0.053 (2)	0.0092 (12)	0.017 (2)	0.0052 (15)
D13	0.0255 (18)	0.0366 (14)	0.0236 (17)	0.0019 (13)	0.0111 (17)	0.0061 (13)
D14	0.036 (2)	0.0195 (12)	0.035 (2)	−0.0017 (13)	0.006 (2)	0.0000 (13)
D15	0.028 (2)	0.0273 (16)	0.019 (2)	−0.0039 (15)	0.002 (2)	−0.0019 (15)
D16	0.025 (2)	0.0269 (15)	0.026 (2)	−0.0054 (15)	0.009 (2)	−0.0021 (15)
D17	0.022 (2)	0.0243 (15)	0.031 (2)	−0.0019 (14)	0.008 (2)	0.0002 (15)
D18	0.026 (2)	0.0157 (13)	0.0234 (19)	0.0015 (14)	0.008 (2)	−0.0007 (14)
D19	0.029 (2)	0.0293 (16)	0.030 (2)	0.0049 (16)	0.010 (2)	0.0032 (16)
D20	0.026 (2)	0.0167 (13)	0.0180 (18)	0.0028 (13)	0.0070 (19)	0.0018 (13)
H11	0.067 (4)	0.070 (3)	0.029 (3)	−0.027 (3)	0.014 (3)	−0.008 (2)
H12	0.038 (3)	0.0338 (18)	0.075 (3)	0.0130 (18)	0.024 (3)	0.007 (2)
H13	0.036 (3)	0.052 (2)	0.033 (2)	0.0027 (19)	0.016 (2)	0.0086 (19)
H14	0.051 (3)	0.0276 (17)	0.049 (3)	−0.0024 (18)	0.009 (3)	0.0000 (19)
H15	0.040 (3)	0.039 (2)	0.026 (3)	−0.006 (2)	0.002 (3)	−0.003 (2)
H16	0.035 (3)	0.038 (2)	0.037 (3)	−0.008 (2)	0.013 (3)	−0.003 (2)
H17	0.030 (3)	0.034 (2)	0.044 (3)	−0.003 (2)	0.011 (3)	0.000 (2)
H18	0.036 (3)	0.0223 (19)	0.033 (3)	0.0022 (19)	0.011 (3)	−0.001 (2)
H19	0.040 (3)	0.041 (2)	0.042 (3)	0.007 (2)	0.015 (3)	0.005 (2)
H20	0.036 (3)	0.0236 (19)	0.025 (3)	0.0040 (19)	0.010 (3)	0.0026 (19)

Geometric parameters (Å, º) top

Cu1—O7	2.2800 (7)	D13—N10	1.0188 (18)
Cu1—O7ⁱ	2.2800 (7)	D13—D11	1.642 (4)
Cu1—O8	2.0046 (5)	D13—D12	1.657 (3)
Cu1—O8ⁱ	2.0046 (5)	D13—D14	1.681 (3)
Cu1—O9	1.9739 (5)	D13—H11	1.642 (4)
Cu1—O9ⁱ	1.9739 (5)	D13—H12	1.657 (3)
Cu1—D17	2.577 (3)	D13—H14	1.681 (3)
Cu1—D17ⁱ	2.577 (3)	D14—S2^iv	2.748 (3)
Cu1—D18	2.564 (2)	D14—O5^iv	1.822 (2)
Cu1—D18ⁱ	2.564 (2)	D14—N10	1.025 (2)
Cu1—D19	2.535 (2)	D14—D11	1.659 (4)
Cu1—D19ⁱ	2.535 (2)	D14—D12	1.675 (3)
Cu1—D20	2.585 (2)	D14—D13	1.681 (3)
Cu1—D20ⁱ	2.585 (2)	D14—H11	1.659 (4)
Cu1—H17	2.577 (3)	D14—H12	1.675 (3)
Cu1—H17ⁱ	2.577 (3)	D14—H13	1.681 (3)
Cu1—H18	2.564 (2)	D15—O3	2.662 (3)
Cu1—H18ⁱ	2.564 (2)	D15—O5	1.890 (3)
Cu1—H19	2.535 (2)	D15—O7	0.966 (3)
Cu1—H19ⁱ	2.535 (2)	D15—D12	2.490 (4)
Cu1—H20	2.585 (2)	D15—D16	1.561 (4)
Cu1—H20ⁱ	2.585 (2)	D15—H12	2.490 (4)
S2—O3	1.4878 (11)	D15—H16	1.561 (4)
S2—O4	1.4592 (12)	D16—O6^xii	1.888 (2)
S2—O5	1.4799 (13)	D16—O7	0.963 (2)
S2—O6	1.4792 (11)	D16—D15	1.561 (4)
S2—D13ⁱⁱ	2.654 (2)	D16—H15	1.561 (4)
S2—D14ⁱⁱⁱ	2.748 (3)	D17—Cu1	2.577 (3)
S2—H13ⁱⁱ	2.654 (2)	D17—O4^ix	1.697 (4)
S2—H14ⁱⁱⁱ	2.748 (3)	D17—O8	0.976 (4)
O3—S2	1.4878 (11)	D17—D18	1.569 (4)
O3—O4	2.4101 (9)	D17—H18	1.569 (4)
O3—O5	2.4016 (7)	D18—Cu1	2.564 (2)
O3—O6	2.4111 (7)	D18—O6^x	1.735 (2)
O3—O9^iv	2.6883 (8)	D18—O8	0.980 (2)
O3—D12	2.024 (3)	D18—D17	1.569 (4)
O3—D13ⁱⁱ	1.8888 (19)	D18—D20ⁱ	2.503 (3)
O3—D15	2.662 (3)	D18—H17	1.569 (4)
O3—D20^iv	1.720 (3)	D18—H20ⁱ	2.503 (3)
O3—H12	2.024 (3)	D19—Cu1	2.535 (2)
O3—H13ⁱⁱ	1.8888 (19)	D19—O5^vi	1.764 (3)
O3—H15	2.662 (3)	D19—O8	2.669 (3)
O3—H20^iv	1.720 (3)	D19—O9	0.975 (3)
O4—S2	1.4592 (12)	D19—D20	1.551 (4)
O4—O3	2.4101 (9)	D19—H20	1.551 (4)
O4—O5	2.3978 (9)	D20—Cu1	2.585 (2)
O4—O6	2.4229 (7)	D20—O3ⁱⁱⁱ	1.720 (3)
O4—O8^v	2.6736 (10)	D20—O9	0.977 (2)
O4—D13ⁱⁱ	2.519 (2)	D20—D18ⁱ	2.503 (3)
O4—D17^v	1.697 (4)	D20—D19	1.551 (4)
O4—H13ⁱⁱ	2.519 (2)	D20—H18ⁱ	2.503 (3)
O4—H17^v	1.697 (4)	D20—H19	1.551 (4)
O5—S2	1.4799 (13)	H11—O6^x	1.916 (4)
O5—O3	2.4016 (7)	H11—N10	1.020 (3)
O5—O4	2.3978 (9)	H11—D12	1.677 (5)
O5—O6	2.4223 (9)	H11—D13	1.642 (4)
O5—O9^vi	2.7286 (7)	H11—D14	1.659 (4)
O5—D14ⁱⁱⁱ	1.822 (2)	H11—H12	1.677 (5)
O5—D15	1.890 (3)	H11—H13	1.642 (4)
O5—D19^vi	1.764 (3)	H11—H14	1.659 (4)
O5—H14ⁱⁱⁱ	1.822 (2)	H12—O3	2.024 (3)
O5—H15	1.890 (3)	H12—O7	2.544 (3)
O5—H19^vi	1.764 (3)	H12—N10	1.016 (3)
O6—S2	1.4792 (11)	H12—D11	1.677 (5)
O6—O3	2.4111 (7)	H12—D13	1.657 (3)
O6—O4	2.4229 (7)	H12—D14	1.675 (3)
O6—O5	2.4223 (9)	H12—D15	2.490 (4)
O6—O8^vii	2.7138 (7)	H12—H11	1.677 (5)
O6—D11^vii	1.916 (4)	H12—H13	1.657 (3)
O6—D16^viii	1.888 (2)	H12—H14	1.675 (3)
O6—D18^vii	1.735 (2)	H12—H15	2.490 (4)
O6—H11^vii	1.916 (4)	H13—S2^xi	2.654 (2)
O6—H16^viii	1.888 (2)	H13—O3^xi	1.8888 (19)
O6—H18^vii	1.735 (2)	H13—O4^xi	2.519 (2)
O7—Cu1	2.2800 (7)	H13—N10	1.0188 (18)
O7—D12	2.544 (3)	H13—D11	1.642 (4)
O7—D15	0.966 (3)	H13—D12	1.657 (3)
O7—D16	0.963 (2)	H13—D14	1.681 (3)
O7—H12	2.544 (3)	H13—H11	1.642 (4)
O7—H15	0.966 (3)	H13—H12	1.657 (3)
O7—H16	0.963 (2)	H13—H14	1.681 (3)
O8—Cu1	2.0046 (5)	H14—S2^iv	2.748 (3)
O8—O4^ix	2.6736 (10)	H14—O5^iv	1.822 (2)
O8—O6^x	2.7138 (7)	H14—N10	1.025 (2)
O8—D17	0.976 (4)	H14—D11	1.659 (4)
O8—D18	0.980 (2)	H14—D12	1.675 (3)
O8—D19	2.669 (3)	H14—D13	1.681 (3)
O8—H17	0.976 (4)	H14—H11	1.659 (4)
O8—H18	0.980 (2)	H14—H12	1.675 (3)
O8—H19	2.669 (3)	H14—H13	1.681 (3)
O9—Cu1	1.9739 (5)	H15—O3	2.662 (3)
O9—O3ⁱⁱⁱ	2.6883 (8)	H15—O5	1.890 (3)
O9—O5^vi	2.7286 (7)	H15—O7	0.966 (3)
O9—D19	0.975 (3)	H15—D12	2.490 (4)
O9—D20	0.977 (2)	H15—D16	1.561 (4)
O9—H19	0.975 (3)	H15—H12	2.490 (4)
O9—H20	0.977 (2)	H15—H16	1.561 (4)
N10—D11	1.020 (3)	H16—O6^xii	1.888 (2)
N10—D12	1.016 (3)	H16—O7	0.963 (2)
N10—D13	1.0188 (18)	H16—D15	1.561 (4)
N10—D14	1.025 (2)	H16—H15	1.561 (4)
N10—H11	1.020 (3)	H17—Cu1	2.577 (3)
N10—H12	1.016 (3)	H17—O4^ix	1.697 (4)
N10—H13	1.0188 (18)	H17—O8	0.976 (4)
N10—H14	1.025 (2)	H17—D18	1.569 (4)
D11—O6^x	1.916 (4)	H17—H18	1.569 (4)
D11—N10	1.020 (3)	H18—Cu1	2.564 (2)
D11—D12	1.677 (5)	H18—O6^x	1.735 (2)
D11—D13	1.642 (4)	H18—O8	0.980 (2)
D11—D14	1.659 (4)	H18—D17	1.569 (4)
D11—H12	1.677 (5)	H18—D20ⁱ	2.503 (3)
D11—H13	1.642 (4)	H18—H17	1.569 (4)
D11—H14	1.659 (4)	H18—H20ⁱ	2.503 (3)
D12—O3	2.024 (3)	H19—Cu1	2.535 (2)
D12—O7	2.544 (3)	H19—O5^vi	1.764 (3)
D12—N10	1.016 (3)	H19—O8	2.669 (3)
D12—D11	1.677 (5)	H19—O9	0.975 (3)
D12—D13	1.657 (3)	H19—D20	1.551 (4)
D12—D14	1.675 (3)	H19—H20	1.551 (4)
D12—D15	2.490 (4)	H20—Cu1	2.585 (2)
D12—H11	1.677 (5)	H20—O3ⁱⁱⁱ	1.720 (3)
D12—H13	1.657 (3)	H20—O9	0.977 (2)
D12—H14	1.675 (3)	H20—D18ⁱ	2.503 (3)
D12—H15	2.490 (4)	H20—D19	1.551 (4)
D13—S2^xi	2.654 (2)	H20—H18ⁱ	2.503 (3)
D13—O3^xi	1.8888 (19)	H20—H19	1.551 (4)
D13—O4^xi	2.519 (2)

D15—O7—D16	108.0 (3)	D11—N10—H13	107.3 (2)
D15—O7—H15	0.0	D11—N10—H14	108.5 (3)
D15—O7—H16	108.0 (3)	D12—N10—D13	109.1 (2)
D16—O7—H15	108.0 (3)	D12—N10—D14	110.4 (2)
D16—O7—H16	0.0	D12—N10—H11	110.9 (3)
H15—O7—H16	108.0 (3)	D12—N10—H12	0.0
D17—O8—D18	106.6 (3)	D12—N10—H13	109.1 (2)
D17—O8—H17	0.0	D12—N10—H14	110.4 (2)
D17—O8—H18	106.6 (3)	D13—N10—D14	110.65 (19)
D18—O8—H17	106.6 (3)	D13—N10—H11	107.3 (2)
D18—O8—H18	0.0	D13—N10—H12	109.1 (2)
H17—O8—H18	106.6 (3)	D13—N10—H13	0.0
D19—O9—D20	105.3 (2)	D13—N10—H14	110.65 (19)
D19—O9—H19	0.0	D14—N10—H11	108.5 (3)
D19—O9—H20	105.3 (2)	D14—N10—H12	110.4 (2)
D20—O9—H19	105.3 (2)	D14—N10—H13	110.65 (19)
D20—O9—H20	0.0	D14—N10—H14	0.0
H19—O9—H20	105.3 (2)	H11—N10—H12	110.9 (3)
D11—N10—D12	110.9 (3)	H11—N10—H13	107.3 (2)
D11—N10—D13	107.3 (2)	H11—N10—H14	108.5 (3)
D11—N10—D14	108.5 (3)	H12—N10—H13	109.1 (2)
D11—N10—H11	0.0	H12—N10—H14	110.4 (2)
D11—N10—H12	110.9 (3)	H13—N10—H14	110.65 (19)

Symmetry codes: (i) −x, −y, −z; (ii) x+1/2, −y+1/2, z; (iii) −x+1/2, y−1/2, −z+1; (iv) −x+1/2, y+1/2, −z+1; (v) x+1, y, z+1; (vi) −x, −y, −z+1; (vii) x+1/2, −y+1/2, z+1; (viii) x, y, z+1; (ix) x−1, y, z−1; (x) x−1/2, −y+1/2, z−1; (xi) x−1/2, −y+1/2, z; (xii) x, y, z−1.

(CuTS_54D_100K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.85D_2.15⁺)₂·CuH_5.86D_6.14O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 410.32	F(000) = 294.7
Monoclinic, P2₁/a	D_x = 2.007 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.0835 (5) Å	Cell parameters from 36284 reflections
b = 12.2186 (7) Å	µ = 0.16 mm⁻¹
c = 6.3612 (4) Å	T = 100 K
β = 105.933 (3)°	Block, blue
V = 678.89 (7) Å³	2.2 × 2.3 × 1.5 mm

Data collection top

TOPAZ Single Crystal Diffractometer	12715 measured reflections
Radiation source: spallation neutron source, SNS BL12	10700 independent reflections
Not applicable to TOF Laue technique monochromator	9605 reflections with > 3σ(I)
time–of–flight Laue scans	h = −17→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 1.084 + 0.550 * lambda [cm^-1] The value of 1.634(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −24→24
T_min = 0.599, T_max = 0.805	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.091	(Δ/σ)_max < 0.001
wR(F²) = 0.088	Δρ_max = 0.18E-12 cm Å^-3 e Å⁻³
S = 1.60	Δρ_min = −0.45E−12 cm Å⁻³ e Å⁻³
9605 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
197 parameters	Extinction coefficient: 1.47E-05 (4)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.00621
S2	0.41960 (7)	0.13495 (5)	0.74360 (12)	0.00649
O3	0.42941 (4)	0.227838 (30	0.59711 (6)	0.01038
O4	0.55759 (4)	0.067920 (32	0.78344 (7)	0.01317
O5	0.28458 (4)	0.067996 (30	0.63281 (6)	0.00959
O6	0.40131 (4)	0.179058 (30	0.95175 (6)	0.0107
O7	0.18678 (4)	0.118586 (31	0.17847 (7)	0.01092
O8	−0.15773 (4)	0.109190 (30	0.02863 (6)	0.00964
O9	−0.00691 (4)	−0.064525 (30	0.28185 (6)	0.00957
N10	0.141206 (27	0.341958 (19	0.35750 (4)	0.01126
D11	0.0782 (2)	0.32731 (14)	0.2003 (3)	0.03452	0.5385 (8)
D12	0.23794 (17)	0.29559 (12)	0.3991 (3)	0.03162	0.5385 (8)
D13	0.07424 (16)	0.32080 (13)	0.4571 (3)	0.02702	0.5385 (8)
D14	0.16961 (17)	0.42271 (12)	0.3732 (3)	0.02866	0.5385 (8)
D15	0.23167 (17)	0.09463 (13)	0.3289 (3)	0.02305	0.5115 (6)
D16	0.26874 (17)	0.12672 (13)	0.1104 (3)	0.02344	0.5115 (6)
D17	−0.26188 (15)	0.09456 (13)	−0.0622 (3)	0.02156	0.5115 (6)
D18	−0.13389 (16)	0.18432 (11)	−0.0019 (3)	0.01899	0.5115 (6)
D19	−0.10516 (18)	−0.05672 (13)	0.3142 (3)	0.02474	0.5115 (6)
D20	0.02042 (16)	−0.14138 (11)	0.3090 (3)	0.01834	0.5115 (6)
H11	0.0782 (2)	0.32731 (14)	0.2003 (3)	0.04881	0.4615 (8)
H12	0.23794 (17)	0.29559 (12)	0.3991 (3)	0.04471	0.4615 (8)
H13	0.07424 (16)	0.32080 (13)	0.4571 (3)	0.03821	0.4615 (8)
H14	0.16961 (17)	0.42271 (12)	0.3732 (3)	0.04053	0.4615 (8)
H15	0.23167 (17)	0.09463 (13)	0.3289 (3)	0.03259	0.4885 (6)
H16	0.26874 (17)	0.12672 (13)	0.1104 (3)	0.03315	0.4885 (6)
H17	−0.26188 (15)	0.09456 (13)	−0.0622 (3)	0.03049	0.4885 (6)
H18	−0.13389 (16)	0.18432 (11)	−0.0019 (3)	0.02685	0.4885 (6)
H19	−0.10516 (18)	−0.05672 (13)	0.3142 (3)	0.03499	0.4885 (6)
H20	0.02042 (16)	−0.14138 (11)	0.3090 (3)	0.02593	0.4885 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.00581 (12	0.00603 (12	0.00693 (14	0.00018 (9)	0.00198 (10	0.00054 (10
S2	0.00615 (22	0.00601 (23	0.00738 (27	−0.00025 (17	0.00195 (19	−0.00011 (20
O3	0.01344 (14	0.00836 (13	0.00986 (15	−0.00193 (10	0.00408 (12	0.00034 (11
O4	0.00791 (13	0.01221 (15	0.01808 (18	0.00267 (10	0.00135 (12	−0.00077 (13
O5	0.00763 (12	0.00973 (13	0.01112 (15	−0.00232 (10	0.00212 (11	−0.00156 (11
O6	0.01471 (15	0.00927 (13	0.00863 (15	−0.00050 (11	0.00408 (12	−0.00115 (11
O7	0.01047 (13	0.01103 (14	0.01066 (16	−0.00175 (10	0.00186 (11	−0.00065 (12
O8	0.00855 (12	0.00847 (13	0.01209 (16	0.00074 (9)	0.00316 (11	0.00028 (11
O9	0.01049 (13	0.00932 (13	0.00963 (15	0.00122 (10	0.00398 (11	0.00166 (11
N10	0.01226 (9)	0.01038 (9)	0.01191 (10	0.00021 (7)	0.00459 (8)	−0.00027 (7)
D11	0.0410 (9)	0.0438 (10)	0.0171 (8)	−0.0169 (8)	0.0053 (7)	−0.0057 (7)
D12	0.0262 (7)	0.0226 (8)	0.0503 (12)	0.0098 (6)	0.0177 (8)	0.0071 (7)
D13	0.0269 (7)	0.0342 (9)	0.0245 (8)	0.0010 (6)	0.0147 (6)	0.0045 (7)
D14	0.0330 (8)	0.0174 (7)	0.0341 (9)	−0.0027 (6)	0.0068 (7)	−0.0011 (6)
D15	0.0249 (8)	0.0250 (8)	0.0161 (8)	−0.0015 (6)	0.0004 (7)	0.0019 (7)
D16	0.0209 (8)	0.0262 (9)	0.0259 (9)	−0.0066 (6)	0.0108 (7)	−0.0034 (7)
D17	0.0138 (7)	0.0231 (8)	0.0267 (9)	0.0004 (6)	0.0036 (6)	−0.0008 (7)
D18	0.0217 (7)	0.0128 (7)	0.0230 (9)	−0.0013 (5)	0.0069 (6)	−0.0003 (6)
D19	0.0248 (8)	0.0256 (9)	0.0278 (10)	0.0054 (6)	0.0139 (7)	0.0041 (7)
D20	0.0221 (7)	0.0140 (7)	0.0196 (8)	0.0040 (5)	0.0067 (6)	0.0024 (6)
H11	0.0580 (13)	0.0620 (15)	0.0242 (11)	−0.0240 (11)	0.0075 (10)	−0.0080 (10)
H12	0.0371 (11)	0.0319 (11)	0.0711 (17)	0.0139 (8)	0.0250 (11)	0.0101 (10)
H13	0.0380 (11)	0.0483 (12)	0.0347 (12)	0.0014 (9)	0.0208 (9)	0.0064 (9)
H14	0.0467 (11)	0.0246 (10)	0.0482 (13)	−0.0038 (8)	0.0096 (10)	−0.0015 (9)
H15	0.0352 (11)	0.0353 (12)	0.0228 (12)	−0.0022 (9)	0.0005 (9)	0.0027 (9)
H16	0.0295 (11)	0.0371 (12)	0.0366 (13)	−0.0093 (9)	0.0153 (10)	−0.0049 (10)
H17	0.0195 (10)	0.0326 (11)	0.0378 (13)	0.0006 (8)	0.0051 (9)	−0.0011 (10)
H18	0.0306 (10)	0.0181 (10)	0.0325 (12)	−0.0019 (8)	0.0097 (9)	−0.0004 (9)
H19	0.0350 (11)	0.0363 (12)	0.0393 (14)	0.0076 (9)	0.0197 (10)	0.0057 (10)
H20	0.0312 (10)	0.0197 (10)	0.0277 (12)	0.0056 (8)	0.0095 (9)	0.0034 (8)

Geometric parameters (Å, º) top

Cu1—O7	2.2824 (4)	D13—N10	1.0244 (15)
Cu1—O7ⁱ	2.2824 (4)	D13—D11	1.646 (2)
Cu1—O8	2.0023 (4)	D13—D12	1.656 (2)
Cu1—O8ⁱ	2.0023 (4)	D13—D14	1.685 (2)
Cu1—O9	1.9753 (4)	D13—H11	1.646 (2)
Cu1—O9ⁱ	1.9753 (4)	D13—H12	1.656 (2)
Cu1—D17	2.5756 (14)	D13—H14	1.685 (2)
Cu1—D17ⁱ	2.5756 (14)	D14—O5ⁱⁱⁱ	1.8261 (15)
Cu1—D18	2.5581 (14)	D14—N10	1.0178 (14)
Cu1—D18ⁱ	2.5581 (14)	D14—D11	1.660 (2)
Cu1—D19	2.5367 (17)	D14—D12	1.664 (2)
Cu1—D19ⁱ	2.5367 (17)	D14—D13	1.685 (2)
Cu1—D20	2.5848 (15)	D14—H11	1.660 (2)
Cu1—D20ⁱ	2.5848 (15)	D14—H12	1.664 (2)
Cu1—H17	2.5756 (14)	D14—H13	1.685 (2)
Cu1—H17ⁱ	2.5756 (14)	D15—O3	2.6655 (15)
Cu1—H18	2.5581 (14)	D15—O5	1.8881 (17)
Cu1—H18ⁱ	2.5581 (14)	D15—O7	0.9762 (16)
Cu1—H19	2.5367 (17)	D15—D12	2.494 (2)
Cu1—H19ⁱ	2.5367 (17)	D15—D16	1.567 (2)
Cu1—H20	2.5848 (15)	D15—H12	2.494 (2)
Cu1—H20ⁱ	2.5848 (15)	D15—H16	1.567 (2)
S2—O3	1.4866 (8)	D16—O6^xii	1.8828 (17)
S2—O4	1.4600 (7)	D16—O7	0.9636 (16)
S2—O5	1.4818 (7)	D16—D15	1.567 (2)
S2—O6	1.4806 (8)	D16—H15	1.567 (2)
S2—D13ⁱⁱ	2.6445 (17)	D17—Cu1	2.5756 (14)
S2—H13ⁱⁱ	2.6445 (17)	D17—O4^ix	1.6957 (14)
O3—S2	1.4866 (8)	D17—O8	0.9801 (14)
O3—O4	2.4126 (5)	D17—D18	1.567 (2)
O3—O5	2.4002 (5)	D17—H18	1.567 (2)
O3—O6	2.4136 (6)	D18—Cu1	2.5581 (14)
O3—O9ⁱⁱⁱ	2.6884 (5)	D18—O6^x	1.7400 (15)
O3—D12	2.0235 (15)	D18—O8	0.9748 (14)
O3—D13ⁱⁱ	1.8765 (15)	D18—D17	1.567 (2)
O3—D15	2.6655 (15)	D18—D20ⁱ	2.502 (2)
O3—D20ⁱⁱⁱ	1.7229 (14)	D18—H17	1.567 (2)
O3—H12	2.0235 (15)	D18—H20ⁱ	2.502 (2)
O3—H13ⁱⁱ	1.8765 (15)	D19—Cu1	2.5367 (17)
O3—H15	2.6655 (15)	D19—O5^v	1.7580 (17)
O3—H20ⁱⁱⁱ	1.7229 (14)	D19—O9	0.9740 (16)
O4—S2	1.4600 (7)	D19—D20	1.547 (2)
O4—O3	2.4126 (5)	D19—H20	1.547 (2)
O4—O5	2.4007 (5)	D20—Cu1	2.5848 (15)
O4—O6	2.4166 (6)	D20—O3^vi	1.7229 (14)
O4—O8^iv	2.6757 (5)	D20—O9	0.9746 (14)
O4—D13ⁱⁱ	2.5208 (17)	D20—D18ⁱ	2.502 (2)
O4—D17^iv	1.6957 (14)	D20—D19	1.547 (2)
O4—H13ⁱⁱ	2.5208 (17)	D20—H18ⁱ	2.502 (2)
O4—H17^iv	1.6957 (14)	D20—H19	1.547 (2)
O5—S2	1.4818 (7)	H11—O6^x	1.9216 (16)
O5—O3	2.4002 (5)	H11—N10	1.0225 (15)
O5—O4	2.4007 (5)	H11—D12	1.687 (2)
O5—O6	2.4292 (5)	H11—D13	1.646 (2)
O5—O9^v	2.7221 (5)	H11—D14	1.660 (2)
O5—D14^vi	1.8261 (15)	H11—H12	1.687 (2)
O5—D15	1.8881 (17)	H11—H13	1.646 (2)
O5—D19^v	1.7580 (17)	H11—H14	1.660 (2)
O5—H14^vi	1.8261 (15)	H12—O3	2.0235 (15)
O5—H15	1.8881 (17)	H12—O7	2.5503 (17)
O5—H19^v	1.7580 (17)	H12—N10	1.0175 (14)
O6—S2	1.4806 (8)	H12—D11	1.687 (2)
O6—O3	2.4136 (6)	H12—D13	1.656 (2)
O6—O4	2.4166 (6)	H12—D14	1.664 (2)
O6—O5	2.4292 (5)	H12—D15	2.494 (2)
O6—O8^vii	2.7138 (5)	H12—H11	1.687 (2)
O6—D11^vii	1.9216 (16)	H12—H13	1.656 (2)
O6—D16^viii	1.8828 (17)	H12—H14	1.664 (2)
O6—D18^vii	1.7400 (15)	H12—H15	2.494 (2)
O6—H11^vii	1.9216 (16)	H13—S2^xi	2.6445 (17)
O6—H16^viii	1.8828 (17)	H13—O3^xi	1.8765 (15)
O6—H18^vii	1.7400 (15)	H13—O4^xi	2.5208 (17)
O7—Cu1	2.2824 (4)	H13—N10	1.0244 (15)
O7—D12	2.5503 (17)	H13—D11	1.646 (2)
O7—D15	0.9762 (16)	H13—D12	1.656 (2)
O7—D16	0.9636 (16)	H13—D14	1.685 (2)
O7—H12	2.5503 (17)	H13—H11	1.646 (2)
O7—H15	0.9762 (16)	H13—H12	1.656 (2)
O7—H16	0.9636 (16)	H13—H14	1.685 (2)
O8—Cu1	2.0023 (4)	H14—O5ⁱⁱⁱ	1.8261 (15)
O8—O4^ix	2.6757 (5)	H14—N10	1.0178 (14)
O8—O6^x	2.7138 (5)	H14—D11	1.660 (2)
O8—D17	0.9801 (14)	H14—D12	1.664 (2)
O8—D18	0.9748 (14)	H14—D13	1.685 (2)
O8—H17	0.9801 (14)	H14—H11	1.660 (2)
O8—H18	0.9748 (14)	H14—H12	1.664 (2)
O9—Cu1	1.9753 (4)	H14—H13	1.685 (2)
O9—O3^vi	2.6884 (5)	H15—O3	2.6655 (15)
O9—O5^v	2.7221 (5)	H15—O5	1.8881 (17)
O9—D19	0.9740 (16)	H15—O7	0.9762 (16)
O9—D20	0.9746 (14)	H15—D12	2.494 (2)
O9—H19	0.9740 (16)	H15—D16	1.567 (2)
O9—H20	0.9746 (14)	H15—H12	2.494 (2)
N10—D11	1.0225 (15)	H15—H16	1.567 (2)
N10—D12	1.0175 (14)	H16—O6^xii	1.8828 (17)
N10—D13	1.0244 (15)	H16—O7	0.9636 (16)
N10—D14	1.0178 (14)	H16—D15	1.567 (2)
N10—H11	1.0225 (15)	H16—H15	1.567 (2)
N10—H12	1.0175 (14)	H17—Cu1	2.5756 (14)
N10—H13	1.0244 (15)	H17—O4^ix	1.6957 (14)
N10—H14	1.0178 (14)	H17—O8	0.9801 (14)
D11—O6^x	1.9216 (16)	H17—D18	1.567 (2)
D11—N10	1.0225 (15)	H17—H18	1.567 (2)
D11—D12	1.687 (2)	H18—Cu1	2.5581 (14)
D11—D13	1.646 (2)	H18—O6^x	1.7400 (15)
D11—D14	1.660 (2)	H18—O8	0.9748 (14)
D11—H12	1.687 (2)	H18—D17	1.567 (2)
D11—H13	1.646 (2)	H18—D20ⁱ	2.502 (2)
D11—H14	1.660 (2)	H18—H17	1.567 (2)
D12—O3	2.0235 (15)	H18—H20ⁱ	2.502 (2)
D12—O7	2.5503 (17)	H19—Cu1	2.5367 (17)
D12—N10	1.0175 (14)	H19—O5^v	1.7580 (17)
D12—D11	1.687 (2)	H19—O9	0.9740 (16)
D12—D13	1.656 (2)	H19—D20	1.547 (2)
D12—D14	1.664 (2)	H19—H20	1.547 (2)
D12—D15	2.494 (2)	H20—Cu1	2.5848 (15)
D12—H11	1.687 (2)	H20—O3^vi	1.7229 (14)
D12—H13	1.656 (2)	H20—O9	0.9746 (14)
D12—H14	1.664 (2)	H20—D18ⁱ	2.502 (2)
D12—H15	2.494 (2)	H20—D19	1.547 (2)
D13—S2^xi	2.6445 (17)	H20—H18ⁱ	2.502 (2)
D13—O3^xi	1.8765 (15)	H20—H19	1.547 (2)
D13—O4^xi	2.5208 (17)

D15—O7—D16	107.75 (14)	D11—N10—H13	107.01 (13)
D15—O7—H15	0.0	D11—N10—H14	108.91 (14)
D15—O7—H16	107.75 (14)	D12—N10—D13	108.41 (13)
D16—O7—H15	107.75 (14)	D12—N10—D14	109.68 (12)
D16—O7—H16	0.0	D12—N10—H11	111.60 (15)
H15—O7—H16	107.75 (14)	D12—N10—H12	0.0
D17—O8—D18	106.60 (13)	D12—N10—H13	108.41 (13)
D17—O8—H17	0.0	D12—N10—H14	109.68 (12)
D17—O8—H18	106.60 (13)	D13—N10—D14	111.21 (14)
D18—O8—H17	106.60 (13)	D13—N10—H11	107.01 (13)
D18—O8—H18	0.0	D13—N10—H12	108.41 (13)
H17—O8—H18	106.60 (13)	D13—N10—H13	0.0
D19—O9—D20	105.11 (13)	D13—N10—H14	111.21 (14)
D19—O9—H19	0.0	D14—N10—H11	108.91 (14)
D19—O9—H20	105.11 (13)	D14—N10—H12	109.68 (12)
D20—O9—H19	105.11 (13)	D14—N10—H13	111.21 (14)
D20—O9—H20	0.0	D14—N10—H14	0.0
H19—O9—H20	105.11 (13)	H11—N10—H12	111.60 (15)
D11—N10—D12	111.60 (15)	H11—N10—H13	107.01 (13)
D11—N10—D13	107.01 (13)	H11—N10—H14	108.91 (14)
D11—N10—D14	108.91 (14)	H12—N10—H13	108.41 (13)
D11—N10—H11	0.0	H12—N10—H14	109.68 (12)
D11—N10—H12	111.60 (15)	H13—N10—H14	111.21 (14)

Symmetry codes: (i) −x, −y, −z; (ii) x+1/2, −y+1/2, z; (iii) −x+1/2, y+1/2, −z+1; (iv) x+1, y, z+1; (v) −x, −y, −z+1; (vi) −x+1/2, y−1/2, −z+1; (vii) x+1/2, −y+1/2, z+1; (viii) x, y, z+1; (ix) x−1, y, z−1; (x) x−1/2, −y+1/2, z−1; (xi) x−1/2, −y+1/2, z; (xii) x, y, z−1.

(CuTS_62D_100K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.53D_2.47⁺)₂·CuH_4.87D_7.13O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 411.97	F(000) = 243
Monoclinic, P2₁/a	D_x = 1.983 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.3925 (3) Å	Cell parameters from 21729 reflections
b = 12.6799 (5) Å	µ = 0.15 mm⁻¹
c = 6.0612 (2) Å	T = 100 K
β = 107.126 (2)°	Block, blue
V = 689.86 (1) Å³	1.5 × 1.2 × 1.1 mm

Data collection top

TOPAZ Single Crystal Diffractometer	7265 measured reflections
Radiation source: spallation neutron source, SNS BL12	6357 independent reflections
Not applicable to TOF Laue technique monochromator	5537 reflections with > 3σ(I)
time–of–flight Laue scans	h = −18→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 1.007 + 0.452 * lambda [cm^-1] The value of 1.459(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −25→25
T_min = 0.753, T_max = 0.884	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.100	(Δ/σ)_max < 0.001
wR(F²) = 0.089	Δρ_max = 0,235637E-12 cm Å^-3 e Å⁻³
S = 1.47	Δρ_min = −0.49E−12 cm Å⁻³ e Å⁻³
5537 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
190 parameters	Extinction coefficient: 2.48E-05 (9)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.0064
S2	0.38671 (11)	0.14378 (8)	0.74908 (16)	0.00625
O3	0.38056 (6)	0.23874 (4)	0.60637 (9)	0.01111
O4	0.52750 (6)	0.08748 (5)	0.77509 (9)	0.01135
O5	0.26129 (6)	0.07344 (4)	0.63017 (9)	0.00909
O6	0.37301 (6)	0.17330 (5)	0.97794 (9)	0.01007
O7	0.15210 (6)	0.10702 (5)	0.16499 (9)	0.01078
O8	0.81927 (6)	0.11216 (5)	0.05016 (9)	0.01114
O9	0.00949 (6)	−0.06631 (4)	0.29576 (9)	0.00879
N10	0.12589 (4)	0.364291 (29	0.37742 (6)	0.01081
D11	0.04180 (17)	0.34604 (13)	0.2312 (2)	0.02468	0.6175 (10)
D12	0.20436 (17)	0.30604 (12)	0.4220 (3)	0.0234	0.6175 (10)
D13	0.08260 (16)	0.37687 (13)	0.5117 (2)	0.02438	0.6175 (10)
D14	0.17631 (18)	0.43293 (12)	0.3510 (3)	0.0251	0.6175 (10)
D15	0.19619 (17)	0.09319 (13)	0.3292 (2)	0.0196	0.5940 (8)
D16	0.23106 (16)	0.12548 (13)	0.0982 (3)	0.02082	0.5940 (8)
D17	0.71754 (16)	0.10257 (13)	−0.0455 (3)	0.02016	0.5940 (8)
D18	0.84232 (18)	0.18531 (12)	0.0297 (3)	0.02151	0.5940 (8)
D19	−0.08542 (16)	−0.06328 (13)	0.3307 (3)	0.02015	0.5940 (8)
D20	0.04254 (17)	0.86059 (12)	0.3155 (3)	0.01839	0.5940 (8)
H11	0.04180 (17)	0.34603 (13)	0.2312 (2)	0.03491	0.3825 (10)
H12	0.20431 (17)	0.30600 (12)	0.4219 (3)	0.03309	0.3825 (10)
H13	0.08261 (16)	0.37683 (13)	0.5117 (2)	0.03447	0.3825 (10)
H14	0.17629 (18)	0.43296 (12)	0.3510 (3)	0.0355	0.3825 (10)
H15	0.19623 (17)	0.09319 (13)	0.3292 (2)	0.02772	0.4060 (8)
H16	0.23109 (16)	0.12548 (13)	0.0982 (3)	0.02945	0.4060 (8)
H17	0.71754 (16)	0.10257 (13)	−0.0455 (3)	0.0285	0.4060 (8)
H18	0.84233 (18)	0.18532 (12)	0.0298 (3)	0.03042	0.4060 (8)
H19	−0.08538 (16)	−0.06328 (13)	0.3307 (3)	0.0285	0.4060 (8)
H20	0.04256 (17)	0.86059 (12)	0.3155 (3)	0.02601	0.4060 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.00570 (18	0.00757 (21	0.00576 (17	−0.00115 (16	0.00142 (15	0.00041 (14
S2	0.00481 (33	0.0076 (4)	0.00624 (33	−0.00028 (30	0.00152 (28	−0.00021 (27
O3	0.01325 (22	0.00941 (22	0.00975 (20	−0.00169 (19	0.00198 (17	0.00187 (16
O4	0.00662 (20	0.01478 (26	0.01225 (21	0.00216 (18	0.00217 (17	0.00049 (17
O5	0.00698 (19	0.01041 (22	0.00954 (19	−0.00222 (17	0.00191 (15	−0.00144 (15
O6	0.01062 (21	0.01230 (23	0.00742 (18	−0.00112 (18	0.00285 (16	−0.00152 (15
O7	0.00966 (21	0.01367 (25	0.00842 (19	−0.00383 (18	0.00174 (16	−0.00012 (16
O8	0.00848 (20	0.01135 (24	0.01354 (21	0.00085 (18	0.00315 (17	0.00118 (17
O9	0.00888 (19	0.00960 (22	0.00845 (18	0.00038 (17	0.00343 (16	0.00076 (15
N10	0.00991 (13	0.01211 (15	0.01064 (13	0.00007 (11	0.00336 (11	0.00093 (10
D11	0.0219 (7)	0.0311 (9)	0.0179 (6)	−0.0035 (6)	0.0010 (5)	−0.0029 (5)
D12	0.0213 (7)	0.0191 (7)	0.0293 (8)	0.0074 (6)	0.0068 (6)	0.0032 (6)
D13	0.0220 (7)	0.0359 (9)	0.0184 (6)	0.0007 (7)	0.0109 (6)	−0.0013 (6)
D14	0.0266 (8)	0.0217 (8)	0.0280 (8)	−0.0054 (6)	0.0097 (6)	0.0051 (6)
D15	0.0188 (7)	0.0250 (8)	0.0135 (6)	−0.0033 (6)	0.0024 (5)	0.0004 (5)
D16	0.0191 (7)	0.0258 (9)	0.0193 (7)	−0.0074 (6)	0.0082 (6)	−0.0003 (6)
D17	0.0113 (6)	0.0263 (9)	0.0214 (7)	−0.0008 (6)	0.0026 (5)	−0.0002 (6)
D18	0.0247 (8)	0.0154 (8)	0.0259 (8)	−0.0018 (6)	0.0099 (7)	0.0012 (6)
D19	0.0174 (7)	0.0253 (9)	0.0205 (7)	0.0026 (6)	0.0097 (6)	0.0035 (6)
D20	0.0192 (7)	0.0156 (7)	0.0202 (7)	0.0025 (6)	0.0056 (6)	0.0023 (5)
H11	0.0310 (10)	0.0440 (13)	0.0254 (9)	−0.0049 (9)	0.0015 (8)	−0.0041 (8)
H12	0.0301 (10)	0.0271 (11)	0.0415 (11)	0.0105 (8)	0.0096 (8)	0.0045 (8)
H13	0.0311 (10)	0.0508 (13)	0.0260 (9)	0.0010 (9)	0.0154 (8)	−0.0018 (8)
H14	0.0377 (11)	0.0307 (11)	0.0397 (11)	−0.0076 (9)	0.0137 (9)	0.0071 (8)
H15	0.0266 (10)	0.0353 (12)	0.0191 (9)	−0.0047 (9)	0.0034 (8)	0.0006 (7)
H16	0.0270 (10)	0.0365 (12)	0.0272 (10)	−0.0105 (9)	0.0116 (8)	−0.0004 (8)
H17	0.0160 (9)	0.0372 (12)	0.0303 (10)	−0.0011 (8)	0.0036 (8)	−0.0003 (8)
H18	0.0350 (11)	0.0218 (11)	0.0367 (11)	−0.0026 (9)	0.0140 (9)	0.0017 (8)
H19	0.0246 (10)	0.0358 (12)	0.0289 (10)	0.0037 (9)	0.0137 (8)	0.0049 (8)
H20	0.0271 (10)	0.0221 (10)	0.0286 (10)	0.0035 (9)	0.0079 (8)	0.0033 (8)

Geometric parameters (Å, º) top

Cu1—O7	2.0102 (5)	D13—H11	1.676 (2)
Cu1—O7ⁱ	2.0102 (5)	D13—H12	1.667 (2)
Cu1—O8ⁱⁱ	2.3023 (6)	D13—H13	0.0006
Cu1—O8ⁱⁱⁱ	2.3023 (6)	D13—H14	1.653 (2)
Cu1—O9	1.9581 (5)	D14—O5^vii	1.8685 (16)
Cu1—O9ⁱ	1.9581 (5)	D14—O8^xvi	2.6261 (16)
Cu1—D15	2.5705 (14)	D14—N10	1.0258 (15)
Cu1—D15ⁱ	2.5705 (14)	D14—D11	1.672 (2)
Cu1—D16	2.6144 (15)	D14—D12	1.666 (2)
Cu1—D16ⁱ	2.6144 (15)	D14—D13	1.654 (2)
Cu1—D19	2.5006 (14)	D14—H11	1.673 (2)
Cu1—D19ⁱ	2.5006 (14)	D14—H12	1.667 (2)
Cu1—D20^iv	2.5477 (14)	D14—H13	1.654 (2)
Cu1—D20^v	2.5477 (14)	D14—H14	0.0005
Cu1—H15	2.5708 (14)	D15—Cu1	2.5705 (14)
Cu1—H15ⁱ	2.5708 (14)	D15—S2	2.7218 (17)
Cu1—H16	2.6146 (15)	D15—O5	1.7628 (15)
Cu1—H16ⁱ	2.6146 (15)	D15—O7	0.9747 (14)
Cu1—H19	2.5005 (14)	D15—O9	2.6451 (16)
Cu1—H19ⁱ	2.5005 (14)	D15—D16	1.583 (2)
Cu1—H20^iv	2.5478 (14)	D15—H15	0.0003
Cu1—H20^v	2.5478 (14)	D15—H16	1.583 (2)
S2—O3	1.4737 (12)	D16—Cu1	2.6144 (15)
S2—O4	1.4699 (11)	D16—O6^xiii	1.8023 (15)
S2—O5	1.4841 (11)	D16—O7	0.9726 (14)
S2—O6	1.4785 (11)	D16—D15	1.583 (2)
S2—D13^vi	2.6613 (16)	D16—H15	1.583 (2)
S2—D15	2.7218 (17)	D16—H16	0.0003
S2—H13^vi	2.6615 (16)	D17—O4^xiii	1.8060 (15)
S2—H15	2.7216 (17)	D17—O8	0.9684 (15)
O3—S2	1.4737 (12)	D17—D18	1.539 (2)
O3—O4	2.4079 (8)	D17—H17	0.0003
O3—O5	2.4009 (8)	D17—H18	1.539 (2)
O3—O6	2.4207 (7)	D18—O6^xvii	1.8572 (17)
O3—O9^vii	2.6774 (8)	D18—O8	0.9686 (16)
O3—D12	1.9045 (15)	D18—D17	1.539 (2)
O3—D13^vi	2.5923 (16)	D18—H17	1.539 (2)
O3—D20^viii	1.7122 (16)	D18—H18	0.0002
O3—H12	1.9047 (15)	D19—Cu1	2.5006 (14)
O3—H13^vi	2.5922 (16)	D19—O5^x	1.7413 (15)
O3—H20^viii	1.7122 (16)	D19—O9	0.9759 (14)
O4—S2	1.4699 (11)	D19—D20^iv	1.565 (2)
O4—O3	2.4079 (8)	D19—H19	0.0003
O4—O5	2.4004 (8)	D19—H20^iv	1.565 (2)
O4—O6	2.4191 (8)	D20—Cu1^xviii	2.5477 (14)
O4—O8^ix	2.7743 (8)	D20—O3^vii	1.7122 (16)
O4—D13^vi	1.8727 (14)	D20—O9^xviii	0.9736 (15)
O4—D17^ix	1.8060 (15)	D20—D12^vii	2.537 (2)
O4—H13^vi	1.8731 (14)	D20—D19^xviii	1.565 (2)
O4—H17^ix	1.8061 (15)	D20—H12^vii	2.537 (2)
O5—S2	1.4841 (11)	D20—H19^xviii	1.565 (2)
O5—O3	2.4009 (8)	D20—H20	0.0002
O5—O4	2.4004 (8)	H11—O6^xv	1.8697 (15)
O5—O6	2.4176 (7)	H11—N10	1.0252 (14)
O5—O7	2.7349 (7)	H11—D11	0.0003
O5—O9^x	2.7112 (7)	H11—D12	1.699 (2)
O5—D14^viii	1.8685 (16)	H11—D13	1.676 (2)
O5—D15	1.7628 (15)	H11—D14	1.673 (2)
O5—D19^x	1.7413 (15)	H11—H12	1.699 (2)
O5—H14^viii	1.8683 (16)	H11—H13	1.675 (2)
O5—H15	1.7626 (15)	H11—H14	1.673 (2)
O5—H19^x	1.7416 (15)	H12—O3	1.9047 (15)
O6—S2	1.4785 (11)	H12—N10	1.0220 (14)
O6—O3	2.4207 (7)	H12—D11	1.698 (2)
O6—O4	2.4191 (8)	H12—D12	0.0006
O6—O5	2.4176 (7)	H12—D13	1.667 (2)
O6—O7^ix	2.7717 (8)	H12—D14	1.667 (2)
O6—D11^xi	1.8700 (15)	H12—D20^viii	2.537 (2)
O6—D16^ix	1.8023 (15)	H12—H11	1.699 (2)
O6—D18^xii	1.8572 (17)	H12—H13	1.666 (2)
O6—H11^xi	1.8697 (15)	H12—H14	1.667 (2)
O6—H16^ix	1.8021 (15)	H12—H20^viii	2.537 (2)
O6—H18^xii	1.8571 (17)	H13—S2^xvi	2.6615 (16)
O7—Cu1	2.0102 (5)	H13—O3^xvi	2.5922 (16)
O7—O5	2.7349 (7)	H13—O4^xvi	1.8731 (14)
O7—O6^xiii	2.7717 (8)	H13—N10	1.0235 (13)
O7—D15	0.9747 (14)	H13—D11	1.675 (2)
O7—D16	0.9726 (14)	H13—D12	1.666 (2)
O7—H15	0.9750 (14)	H13—D13	0.0006
O7—H16	0.9728 (14)	H13—D14	1.654 (2)
O8—Cu1^xiv	2.3023 (6)	H13—H11	1.675 (2)
O8—O4^xiii	2.7743 (8)	H13—H12	1.666 (2)
O8—D14^vi	2.6261 (16)	H13—H14	1.653 (2)
O8—D17	0.9684 (15)	H14—O5^vii	1.8683 (16)
O8—D18	0.9686 (16)	H14—O8^xvi	2.6265 (16)
O8—H14^vi	2.6265 (16)	H14—N10	1.0259 (15)
O8—H17	0.9683 (15)	H14—D11	1.673 (2)
O8—H18	0.9687 (16)	H14—D12	1.667 (2)
O9—Cu1	1.9581 (5)	H14—D13	1.653 (2)
O9—O3^viii	2.6774 (8)	H14—D14	0.0005
O9—O5^x	2.7112 (7)	H14—H11	1.673 (2)
O9—D15	2.6451 (16)	H14—H12	1.667 (2)
O9—D19	0.9759 (14)	H14—H13	1.653 (2)
O9—D20^iv	0.9736 (15)	H15—Cu1	2.5708 (14)
O9—H15	2.6453 (16)	H15—S2	2.7216 (17)
O9—H19	0.9756 (14)	H15—O5	1.7626 (15)
O9—H20^iv	0.9737 (15)	H15—O7	0.9750 (14)
N10—D11	1.0250 (14)	H15—O9	2.6453 (16)
N10—D12	1.0220 (14)	H15—D15	0.0003
N10—D13	1.0239 (13)	H15—D16	1.583 (2)
N10—D14	1.0258 (15)	H15—H16	1.583 (2)
N10—H11	1.0252 (14)	H16—Cu1	2.6146 (15)
N10—H12	1.0220 (14)	H16—O6^xiii	1.8021 (15)
N10—H13	1.0235 (13)	H16—O7	0.9728 (14)
N10—H14	1.0259 (15)	H16—D15	1.583 (2)
D11—O6^xv	1.8700 (15)	H16—D16	0.0003
D11—N10	1.0250 (14)	H16—H15	1.583 (2)
D11—D12	1.699 (2)	H17—O4^xiii	1.8061 (15)
D11—D13	1.675 (2)	H17—O8	0.9683 (15)
D11—D14	1.672 (2)	H17—D17	0.0003
D11—H11	0.0003	H17—D18	1.539 (2)
D11—H12	1.698 (2)	H17—H18	1.539 (2)
D11—H13	1.675 (2)	H18—O6^xvii	1.8571 (17)
D11—H14	1.673 (2)	H18—O8	0.9687 (16)
D12—O3	1.9045 (15)	H18—D17	1.539 (2)
D12—N10	1.0220 (14)	H18—D18	0.0002
D12—D11	1.699 (2)	H18—H17	1.539 (2)
D12—D13	1.666 (2)	H19—Cu1	2.5005 (14)
D12—D14	1.666 (2)	H19—O5^x	1.7416 (15)
D12—D20^viii	2.537 (2)	H19—O9	0.9756 (14)
D12—H11	1.699 (2)	H19—D19	0.0003
D12—H12	0.0006	H19—D20^iv	1.565 (2)
D12—H13	1.666 (2)	H19—H20^iv	1.565 (2)
D12—H14	1.667 (2)	H20—Cu1^xviii	2.5478 (14)
D12—H20^viii	2.536 (2)	H20—O3^vii	1.7122 (16)
D13—S2^xvi	2.6613 (16)	H20—O9^xviii	0.9737 (15)
D13—O3^xvi	2.5923 (16)	H20—D12^vii	2.536 (2)
D13—O4^xvi	1.8727 (14)	H20—D19^xviii	1.565 (2)
D13—N10	1.0239 (13)	H20—D20	0.0002
D13—D11	1.675 (2)	H20—H12^vii	2.537 (2)
D13—D12	1.666 (2)	H20—H19^xviii	1.565 (2)
D13—D14	1.654 (2)

D15—O7—D16	108.77 (14)	D11—N10—H13	109.71 (12)
D15—O7—H15	0.0	D11—N10—H14	109.28 (13)
D15—O7—H16	108.76 (14)	D12—N10—D13	109.08 (13)
D16—O7—H15	108.75 (14)	D12—N10—D14	108.92 (13)
D16—O7—H16	0.0	D12—N10—H11	112.16 (13)
H15—O7—H16	108.74 (14)	D12—N10—H12	0.0
D17—O8—D18	105.19 (15)	D12—N10—H13	109.06 (13)
D17—O8—H17	0.0	D12—N10—H14	108.94 (13)
D17—O8—H18	105.20 (15)	D13—N10—D14	107.56 (13)
D18—O8—H17	105.19 (15)	D13—N10—H11	109.72 (12)
D18—O8—H18	0.0	D13—N10—H12	109.08 (13)
H17—O8—H18	105.20 (15)	D13—N10—H13	0.0
D19—O9—D20^iv	106.82 (14)	D13—N10—H14	107.54 (13)
D19—O9—H19	0.0	D14—N10—H11	109.27 (13)
D19—O9—H20^iv	106.83 (14)	D14—N10—H12	108.95 (13)
D20^iv—O9—H19	106.82 (14)	D14—N10—H13	107.59 (13)
D20^iv—O9—H20^iv	0.0	D14—N10—H14	0.0
H19—O9—H20^iv	106.83 (14)	H11—N10—H12	112.13 (13)
D11—N10—D12	112.17 (13)	H11—N10—H13	109.72 (12)
D11—N10—D13	109.71 (12)	H11—N10—H14	109.28 (13)
D11—N10—D14	109.28 (13)	H12—N10—H13	109.06 (13)
D11—N10—H11	0.0	H12—N10—H14	108.97 (13)
D11—N10—H12	112.14 (13)	H13—N10—H14	107.56 (13)

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x, y−1, z; (v) −x, −y+1, −z; (vi) x+1/2, −y+1/2, z; (vii) −x+1/2, y+1/2, −z+1; (viii) −x+1/2, y−1/2, −z+1; (ix) x, y, z+1; (x) −x, −y, −z+1; (xi) x+1/2, −y+1/2, z+1; (xii) x−1/2, −y+1/2, z+1; (xiii) x, y, z−1; (xiv) x+1, y, z; (xv) x−1/2, −y+1/2, z−1; (xvi) x−1/2, −y+1/2, z; (xvii) x+1/2, −y+1/2, z−1; (xviii) x, y+1, z.

(CuTS_62D_150K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.53D_2.47⁺)₂·CuH_4.87D_7.13O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 411.97	F(000) = 243
Monoclinic, P2₁/a	D_x = 1.984 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.3936 (3) Å	Cell parameters from 21815 reflections
b = 12.6772 (5) Å	µ = 0.15 mm⁻¹
c = 6.0723 (2) Å	T = 150 K
β = 107.086 (2)°	Block, blue
V = 691.20 (4) Å³	1.5 × 1.2 × 1.1 mm

Data collection top

TOPAZ Single Crystal Diffractometer	6830 measured reflections
Radiation source: spallation neutron source, SNS BL12	5848 independent reflections
Not applicable to TOF Laue technique monochromator	4985 reflections with > 3σ(I)
time–of–flight Laue scans	h = −18→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 1.005 + 0.451 * lambda [cm^-1] The value of 1.456(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −25→25
T_min = 0.753, T_max = 0.884	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.094	(Δ/σ)_max < 0.001
wR(F²) = 0.085	Δρ_max = 0.20E-12 cm Å^-3 e Å⁻³
S = 1.40	Δρ_min = −0.45E−12 cm Å⁻³ e Å⁻³
4985 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
188 parameters	Extinction coefficient: 2.26E-05 (8)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.0089
S2	0.38727 (11)	0.14377 (9)	0.74848 (17)	0.00873
O3	0.38130 (7)	0.23867 (5)	0.60636 (10)	0.01549
O4	0.52775 (6)	0.08755 (5)	0.77484 (10)	0.01577
O5	0.26171 (6)	0.07355 (5)	0.62964 (9)	0.01244
O6	0.37293 (7)	0.17315 (5)	0.97657 (9)	0.01374
O7	0.15250 (7)	0.10683 (5)	0.16515 (9)	0.01445
O8	0.81917 (6)	0.11227 (5)	0.04942 (10)	0.01484
O9	0.00882 (6)	−0.06641 (5)	0.29493 (9)	0.01141
N10	0.12582 (4)	0.363711 (31	0.37634 (6)	0.01456
D11	0.04232 (18)	0.34586 (15)	0.2302 (3)	0.03258	0.61757
D12	0.20444 (18)	0.30585 (13)	0.4206 (3)	0.03073	0.61757
D13	0.08249 (18)	0.37598 (15)	0.5099 (3)	0.03212	0.61757
D14	0.17588 (19)	0.43254 (13)	0.3509 (3)	0.03094	0.61757
D15	0.19672 (18)	0.09300 (13)	0.3288 (3)	0.02382	0.59399
D16	0.23120 (17)	0.12526 (14)	0.0976 (3)	0.02476	0.59399
D17	0.71780 (17)	0.10239 (13)	−0.0463 (3)	0.02351	0.59399
D18	0.84201 (19)	0.18537 (13)	0.0279 (3)	0.02657	0.59399
D19	−0.08605 (17)	−0.06341 (13)	0.3300 (3)	0.02433	0.59399
D20	0.04214 (17)	0.86072 (13)	0.3152 (3)	0.02159	0.59399
H11	0.04231 (18)	0.34585 (15)	0.2301 (3)	0.04608	0.38243
H12	0.20439 (18)	0.30582 (13)	0.4206 (3)	0.04346	0.38243
H13	0.08251 (18)	0.37594 (15)	0.5099 (3)	0.04543	0.38243
H14	0.17585 (19)	0.43256 (13)	0.3509 (3)	0.04375	0.38243
H15	0.19676 (18)	0.09300 (13)	0.3289 (3)	0.03368	0.40601
H16	0.23123 (17)	0.12526 (14)	0.0976 (3)	0.03501	0.40601
H17	0.71780 (17)	0.10239 (13)	−0.0462 (3)	0.03324	0.40601
H18	0.84203 (19)	0.18538 (13)	0.0279 (3)	0.03757	0.40601
H19	−0.08602 (17)	−0.06341 (13)	0.3300 (3)	0.03441	0.40601
H20	0.04216 (17)	0.86072 (13)	0.3152 (3)	0.03052	0.40601

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.00804 (20	0.01023 (23	0.00810 (19	−0.00180 (18	0.00187 (16	0.00052 (16
S2	0.0069 (4)	0.0104 (4)	0.0086 (4)	−0.00116 (34	0.00196 (30	−0.00002 (30
O3	0.01905 (27	0.01212 (25	0.01392 (23	−0.00328 (22	0.00271 (20	0.00248 (18
O4	0.00932 (22	0.02000 (31	0.01756 (25	0.00284 (20	0.00326 (19	0.00020 (20
O5	0.01005 (21	0.01407 (25	0.01300 (21	−0.00377 (19	0.00307 (17	−0.00197 (18
O6	0.01503 (24	0.01610 (27	0.01031 (21	−0.00150 (20	0.00406 (18	−0.00203 (18
O7	0.01304 (23	0.01836 (28	0.01115 (21	−0.00549 (21	0.00231 (18	0.00001 (19
O8	0.01137 (23	0.01489 (27	0.01822 (24	0.00129 (20	0.00432 (20	0.00167 (19
O9	0.01175 (21	0.01229 (24	0.01091 (20	0.00089 (19	0.00446 (17	0.00133 (17
N10	0.01337 (15	0.01656 (18	0.01420 (15	0.00018 (13	0.00475 (12	0.00128 (12
D11	0.0281 (8)	0.0428 (11)	0.0235 (8)	−0.0041 (8)	0.0024 (6)	−0.0027 (7)
D12	0.0283 (8)	0.0251 (8)	0.0389 (9)	0.0090 (7)	0.0099 (7)	0.0053 (7)
D13	0.0281 (8)	0.0476 (11)	0.0242 (7)	0.0007 (8)	0.0131 (7)	−0.0007 (7)
D14	0.0325 (9)	0.0262 (9)	0.0344 (8)	−0.0074 (7)	0.0103 (7)	0.0064 (7)
D15	0.0232 (8)	0.0300 (9)	0.0165 (7)	−0.0042 (7)	0.0030 (6)	0.0009 (6)
D16	0.0231 (8)	0.0288 (9)	0.0238 (7)	−0.0091 (7)	0.0091 (6)	−0.0001 (6)
D17	0.0150 (7)	0.0291 (9)	0.0255 (7)	−0.0008 (7)	0.0045 (6)	−0.0006 (6)
D18	0.0279 (9)	0.0212 (8)	0.0326 (9)	−0.0020 (7)	0.0119 (7)	0.0009 (7)
D19	0.0216 (8)	0.0288 (9)	0.0258 (8)	0.0033 (7)	0.0119 (7)	0.0031 (7)
D20	0.0231 (8)	0.0182 (8)	0.0229 (7)	0.0023 (7)	0.0060 (6)	0.0021 (6)
H11	0.0397 (12)	0.0606 (15)	0.0333 (11)	−0.0058 (11)	0.0034 (9)	−0.0038 (9)
H12	0.0400 (12)	0.0354 (12)	0.0550 (13)	0.0127 (10)	0.0141 (10)	0.0075 (10)
H13	0.0398 (11)	0.0673 (16)	0.0342 (10)	0.0009 (11)	0.0185 (9)	−0.0010 (10)
H14	0.0460 (12)	0.0371 (12)	0.0486 (12)	−0.0105 (10)	0.0146 (10)	0.0091 (9)
H15	0.0329 (11)	0.0424 (13)	0.0233 (9)	−0.0059 (10)	0.0043 (8)	0.0012 (8)
H16	0.0327 (11)	0.0408 (13)	0.0336 (11)	−0.0128 (10)	0.0129 (9)	−0.0002 (9)
H17	0.0212 (9)	0.0411 (13)	0.0360 (11)	−0.0011 (9)	0.0063 (8)	−0.0009 (9)
H18	0.0395 (12)	0.0300 (12)	0.0460 (12)	−0.0029 (10)	0.0169 (10)	0.0013 (10)
H19	0.0305 (11)	0.0407 (13)	0.0365 (11)	0.0047 (10)	0.0168 (9)	0.0043 (9)
H20	0.0327 (11)	0.0257 (11)	0.0324 (10)	0.0033 (9)	0.0085 (8)	0.0029 (8)

Geometric parameters (Å, º) top

Cu1—O7	2.0119 (6)	D13—H11	1.673 (2)
Cu1—O7ⁱ	2.0119 (6)	D13—H12	1.662 (2)
Cu1—O8ⁱⁱ	2.3024 (6)	D13—H13	0.0006
Cu1—O8ⁱⁱⁱ	2.3024 (6)	D13—H14	1.647 (2)
Cu1—O9	1.9585 (5)	D14—O5^vii	1.8742 (17)
Cu1—O9ⁱ	1.9585 (5)	D14—O8^xvi	2.6331 (18)
Cu1—D15	2.5736 (15)	D14—N10	1.0242 (16)
Cu1—D15ⁱ	2.5736 (15)	D14—D11	1.667 (2)
Cu1—D16	2.6140 (15)	D14—D12	1.663 (2)
Cu1—D16ⁱ	2.6140 (15)	D14—D13	1.647 (2)
Cu1—D19	2.5035 (15)	D14—H11	1.667 (2)
Cu1—D19ⁱ	2.5035 (15)	D14—H12	1.663 (2)
Cu1—D20^iv	2.5480 (15)	D14—H13	1.647 (2)
Cu1—D20^v	2.5480 (15)	D14—H14	0.0005
Cu1—H15	2.5739 (15)	D15—Cu1	2.5736 (15)
Cu1—H15ⁱ	2.5739 (15)	D15—S2	2.7261 (18)
Cu1—H16	2.6142 (15)	D15—O5	1.7649 (16)
Cu1—H16ⁱ	2.6142 (15)	D15—O7	0.9739 (15)
Cu1—H19	2.5034 (15)	D15—O9	2.6511 (17)
Cu1—H19ⁱ	2.5034 (15)	D15—D16	1.584 (2)
Cu1—H20^iv	2.5480 (15)	D15—H15	0.0003
Cu1—H20^v	2.5480 (15)	D15—H16	1.585 (2)
S2—O3	1.4720 (12)	D16—Cu1	2.6140 (15)
S2—O4	1.4666 (12)	D16—O6^xiii	1.8046 (16)
S2—O5	1.4846 (12)	D16—O7	0.9733 (15)
S2—O6	1.4781 (11)	D16—D15	1.584 (2)
S2—D13^vi	2.6620 (18)	D16—H15	1.584 (2)
S2—D15	2.7261 (18)	D16—H16	0.0003
S2—H13^vi	2.6622 (18)	D17—O4^xiii	1.8063 (16)
S2—H15	2.7258 (18)	D17—O8	0.9669 (16)
O3—S2	1.4720 (12)	D17—D18	1.537 (2)
O3—O4	2.4047 (9)	D17—H17	0.0003
O3—O5	2.3994 (8)	D17—H18	1.537 (2)
O3—O6	2.4194 (8)	D18—O6^xvii	1.8578 (18)
O3—O9^vii	2.6772 (9)	D18—O8	0.9687 (17)
O3—D12	1.9123 (17)	D18—D17	1.537 (2)
O3—D13^vi	2.5842 (18)	D18—H17	1.537 (2)
O3—D20^viii	1.7138 (17)	D18—H18	0.0002
O3—H12	1.9124 (17)	D19—Cu1	2.5035 (15)
O3—H13^vi	2.5841 (18)	D19—O5^x	1.7426 (16)
O3—H20^viii	1.7137 (17)	D19—O9	0.9761 (15)
O4—S2	1.4666 (12)	D19—D20^iv	1.564 (2)
O4—O3	2.4047 (9)	D19—H19	0.0003
O4—O5	2.3999 (8)	D19—H20^iv	1.564 (2)
O4—O6	2.4166 (8)	D20—Cu1^xviii	2.5480 (15)
O4—O8^ix	2.7731 (8)	D20—O3^vii	1.7138 (17)
O4—D13^vi	1.8849 (16)	D20—O9^xviii	0.9715 (16)
O4—D17^ix	1.8063 (16)	D20—D12^vii	2.546 (2)
O4—H13^vi	1.8853 (16)	D20—D19^xviii	1.564 (2)
O4—H17^ix	1.8064 (16)	D20—H12^vii	2.546 (2)
O5—S2	1.4846 (12)	D20—H19^xviii	1.564 (2)
O5—O3	2.3994 (8)	D20—H20	0.0002
O5—O4	2.3999 (8)	H11—O6^xv	1.8763 (17)
O5—O6	2.4147 (8)	H11—N10	1.0226 (16)
O5—O7	2.7360 (8)	H11—D11	0.0003
O5—O9^x	2.7129 (8)	H11—D12	1.697 (2)
O5—D14^viii	1.8742 (17)	H11—D13	1.673 (2)
O5—D15	1.7649 (16)	H11—D14	1.667 (2)
O5—D19^x	1.7426 (16)	H11—H12	1.697 (2)
O5—H14^viii	1.8740 (17)	H11—H13	1.672 (2)
O5—H15	1.7647 (16)	H11—H14	1.667 (2)
O5—H19^x	1.7429 (16)	H12—O3	1.9124 (17)
O6—S2	1.4781 (11)	H12—N10	1.0193 (16)
O6—O3	2.4194 (8)	H12—D11	1.696 (2)
O6—O4	2.4166 (8)	H12—D12	0.0006
O6—O5	2.4147 (8)	H12—D13	1.662 (2)
O6—O7^ix	2.7748 (8)	H12—D14	1.663 (2)
O6—D11^xi	1.8765 (17)	H12—D20^viii	2.546 (2)
O6—D16^ix	1.8046 (16)	H12—H11	1.697 (2)
O6—D18^xii	1.8578 (18)	H12—H13	1.661 (2)
O6—H11^xi	1.8763 (17)	H12—H14	1.663 (2)
O6—H16^ix	1.8044 (16)	H12—H20^viii	2.546 (2)
O6—H18^xii	1.8578 (18)	H13—S2^xvi	2.6622 (18)
O7—Cu1	2.0119 (6)	H13—O3^xvi	2.5841 (18)
O7—O5	2.7360 (8)	H13—O4^xvi	1.8853 (16)
O7—O6^xiii	2.7748 (8)	H13—N10	1.0201 (14)
O7—D15	0.9739 (15)	H13—D11	1.672 (2)
O7—D16	0.9733 (15)	H13—D12	1.661 (2)
O7—H15	0.9741 (15)	H13—D13	0.0006
O7—H16	0.9736 (15)	H13—D14	1.647 (2)
O8—Cu1^xiv	2.3024 (6)	H13—H11	1.672 (2)
O8—O4^xiii	2.7731 (8)	H13—H12	1.661 (2)
O8—D14^vi	2.6331 (18)	H13—H14	1.647 (2)
O8—D17	0.9669 (16)	H14—O5^vii	1.8740 (17)
O8—D18	0.9687 (17)	H14—O8^xvi	2.6335 (18)
O8—H14^vi	2.6335 (18)	H14—N10	1.0243 (16)
O8—H17	0.9668 (16)	H14—D11	1.667 (2)
O8—H18	0.9688 (17)	H14—D12	1.663 (2)
O9—Cu1	1.9585 (5)	H14—D13	1.647 (2)
O9—O3^viii	2.6772 (9)	H14—D14	0.0005
O9—O5^x	2.7129 (8)	H14—H11	1.667 (2)
O9—D15	2.6511 (17)	H14—H12	1.663 (2)
O9—D19	0.9761 (15)	H14—H13	1.647 (2)
O9—D20^iv	0.9715 (16)	H15—Cu1	2.5739 (15)
O9—H15	2.6513 (17)	H15—S2	2.7258 (18)
O9—H19	0.9758 (15)	H15—O5	1.7647 (16)
O9—H20^iv	0.9716 (16)	H15—O7	0.9741 (15)
N10—D11	1.0223 (16)	H15—O9	2.6513 (17)
N10—D12	1.0193 (16)	H15—D15	0.0003
N10—D13	1.0205 (14)	H15—D16	1.584 (2)
N10—D14	1.0242 (16)	H15—H16	1.585 (2)
N10—H11	1.0226 (16)	H16—Cu1	2.6142 (15)
N10—H12	1.0193 (16)	H16—O6^xiii	1.8044 (16)
N10—H13	1.0201 (14)	H16—O7	0.9736 (15)
N10—H14	1.0243 (16)	H16—D15	1.585 (2)
D11—O6^xv	1.8765 (17)	H16—D16	0.0003
D11—N10	1.0223 (16)	H16—H15	1.585 (2)
D11—D12	1.697 (2)	H17—O4^xiii	1.8064 (16)
D11—D13	1.672 (2)	H17—O8	0.9668 (16)
D11—D14	1.667 (2)	H17—D17	0.0003
D11—H11	0.0003	H17—D18	1.537 (2)
D11—H12	1.696 (2)	H17—H18	1.537 (2)
D11—H13	1.672 (2)	H18—O6^xvii	1.8578 (18)
D11—H14	1.667 (2)	H18—O8	0.9688 (17)
D12—O3	1.9123 (17)	H18—D17	1.537 (2)
D12—N10	1.0193 (16)	H18—D18	0.0002
D12—D11	1.697 (2)	H18—H17	1.537 (2)
D12—D13	1.662 (2)	H19—Cu1	2.5034 (15)
D12—D14	1.663 (2)	H19—O5^x	1.7429 (16)
D12—D20^viii	2.546 (2)	H19—O9	0.9758 (15)
D12—H11	1.697 (2)	H19—D19	0.0003
D12—H12	0.0006	H19—D20^iv	1.564 (2)
D12—H13	1.661 (2)	H19—H20^iv	1.564 (2)
D12—H14	1.663 (2)	H20—Cu1^xviii	2.5480 (15)
D12—H20^viii	2.546 (2)	H20—O3^vii	1.7137 (17)
D13—S2^xvi	2.6620 (18)	H20—O9^xviii	0.9716 (16)
D13—O3^xvi	2.5842 (18)	H20—D12^vii	2.546 (2)
D13—O4^xvi	1.8849 (16)	H20—D19^xviii	1.564 (2)
D13—N10	1.0205 (14)	H20—D20	0.0002
D13—D11	1.672 (2)	H20—H12^vii	2.546 (2)
D13—D12	1.662 (2)	H20—H19^xviii	1.564 (2)
D13—D14	1.647 (2)

D15—O7—D16	108.91 (15)	D11—N10—H13	109.89 (13)
D15—O7—H15	0.0	D11—N10—H14	109.07 (14)
D15—O7—H16	108.90 (15)	D12—N10—D13	109.11 (14)
D16—O7—H15	108.89 (15)	D12—N10—D14	108.88 (14)
D16—O7—H16	0.0	D12—N10—H11	112.41 (15)
H15—O7—H16	108.88 (15)	D12—N10—H12	0.0
D17—O8—D18	105.12 (16)	D12—N10—H13	109.09 (14)
D17—O8—H17	0.0	D12—N10—H14	108.90 (14)
D17—O8—H18	105.13 (16)	D13—N10—D14	107.34 (15)
D18—O8—H17	105.13 (16)	D13—N10—H11	109.90 (13)
D18—O8—H18	0.0	D13—N10—H12	109.11 (14)
H17—O8—H18	105.14 (16)	D13—N10—H13	0.0
D19—O9—D20^iv	106.87 (15)	D13—N10—H14	107.32 (15)
D19—O9—H19	0.0	D14—N10—H11	109.06 (14)
D19—O9—H20^iv	106.88 (15)	D14—N10—H12	108.91 (14)
D20^iv—O9—H19	106.87 (15)	D14—N10—H13	107.37 (15)
D20^iv—O9—H20^iv	0.0	D14—N10—H14	0.0
H19—O9—H20^iv	106.88 (15)	H11—N10—H12	112.38 (15)
D11—N10—D12	112.41 (15)	H11—N10—H13	109.90 (13)
D11—N10—D13	109.89 (13)	H11—N10—H14	109.07 (14)
D11—N10—D14	109.07 (14)	H12—N10—H13	109.09 (14)
D11—N10—H11	0.0	H12—N10—H14	108.93 (14)
D11—N10—H12	112.38 (15)	H13—N10—H14	107.34 (15)

(CuTS_62D_200K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.53D_2.47⁺)₂·CuH_4.87D_7.13O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 411.97	F(000) = 243
Monoclinic, P2₁/a	D_x = 1.984 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.3834 (3) Å	Cell parameters from 21861 reflections
b = 12.6608 (5) Å	µ = 0.15 mm⁻¹
c = 6.0905 (2) Å	T = 200 K
β = 106.983 (2)°	Block, blue
V = 692.00 (3) Å³	1.5 × 1.2 × 1.1 mm

Data collection top

TOPAZ Single Crystal Diffractometer	6293 measured reflections
Radiation source: spallation neutron source, SNS BL12	5241 independent reflections
Not applicable to TOF Laue technique monochromator	4361 reflections with > 3σ(I)
time–of–flight Laue scans	h = −18→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 1.005 + 0.453 * lambda [cm^-1] The value of 1.458(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −25→25
T_min = 0.753, T_max = 0.883	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.090	(Δ/σ)_max < 0.001
wR(F²) = 0.082	Δρ_max = 0.15E-12 cm Å^-3 e Å⁻³
S = 1.35	Δρ_min = −0.31E−12 cm Å⁻³ e Å⁻³
4361 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
188 parameters	Extinction coefficient: 2.00E-05 (8)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.01152
S2	0.38804 (12)	0.14359 (9)	0.74757 (18)	0.01141
O3	0.38298 (8)	0.23831 (5)	0.60561 (11)	0.02068
O4	0.52834 (7)	0.08705 (6)	0.77412 (12)	0.02164
O5	0.26269 (7)	0.07342 (5)	0.62858 (10)	0.0162
O6	0.37305 (7)	0.17318 (5)	0.97404 (10)	0.01818
O7	0.15316 (7)	0.10690 (6)	0.16508 (10)	0.01903
O8	0.81909 (7)	0.11230 (6)	0.04789 (11)	0.01935
O9	0.00769 (7)	−0.06631 (5)	0.29367 (10)	0.01464
N10	0.12570 (5)	0.36224 (4)	0.37409 (7)	0.01913
D11	0.0430 (2)	0.34532 (16)	0.2281 (3)	0.04066	0.61757
D12	0.2048 (2)	0.30527 (15)	0.4176 (3)	0.039	0.61757
D13	0.0822 (2)	0.37363 (18)	0.5066 (3)	0.04429	0.61757
D14	0.1753 (2)	0.43160 (15)	0.3512 (3)	0.04116	0.61757
D15	0.19772 (19)	0.09284 (14)	0.3281 (3)	0.02842	0.59399
D16	0.23199 (19)	0.12490 (15)	0.0978 (3)	0.02997	0.59399
D17	0.71803 (18)	0.10184 (15)	−0.0474 (3)	0.02968	0.59399
D18	0.8419 (2)	0.18529 (14)	0.0254 (3)	0.03077	0.59399
D19	−0.08739 (18)	−0.06336 (14)	0.3287 (3)	0.02853	0.59399
D20	0.04096 (18)	0.86074 (14)	0.3150 (3)	0.02559	0.59399
H11	0.0430 (2)	0.34531 (16)	0.2280 (3)	0.05749	0.38243
H12	0.2047 (2)	0.30523 (15)	0.4176 (3)	0.05516	0.38243
H13	0.0822 (2)	0.37359 (18)	0.5066 (3)	0.06264	0.38243
H14	0.1752 (2)	0.43163 (15)	0.3512 (3)	0.0582	0.38243
H15	0.19776 (19)	0.09284 (14)	0.3281 (3)	0.04019	0.40601
H16	0.23202 (19)	0.12490 (15)	0.0978 (3)	0.04238	0.40601
H17	0.71803 (18)	0.10184 (15)	−0.0474 (3)	0.04197	0.40601
H18	0.8419 (2)	0.18529 (14)	0.0254 (3)	0.04352	0.40601
H19	−0.08736 (18)	−0.06336 (14)	0.3287 (3)	0.04034	0.40601
H20	0.04098 (18)	0.86074 (14)	0.3150 (3)	0.03619	0.40601

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.01043 (23	0.01317 (26	0.01063 (21	−0.00226 (20	0.00253 (18	0.00079 (18
S2	0.0097 (4)	0.0130 (5)	0.0115 (4)	−0.0016 (4)	0.00300 (34	−0.00077 (34
O3	0.02588 (33	0.01645 (29	0.01818 (27	−0.00441 (26	0.00406 (24	0.00322 (21
O4	0.01205 (26	0.0276 (4)	0.02437 (30	0.00359 (24	0.00389 (23	−0.00065 (25
O5	0.01316 (24	0.01814 (29	0.01697 (25	−0.00491 (22	0.00387 (20	−0.00228 (20
O6	0.02042 (29	0.02107 (31	0.01367 (24	−0.00201 (24	0.00598 (21	−0.00286 (20
O7	0.01716 (27	0.02425 (34	0.01475 (25	−0.00699 (24	0.00321 (21	0.00016 (22
O8	0.01517 (27	0.01915 (32	0.02367 (29	0.00143 (24	0.00556 (24	0.00224 (23
O9	0.01499 (24	0.01585 (28	0.01389 (23	0.00084 (22	0.00550 (19	0.00169 (19
N10	0.01802 (18	0.02185 (21	0.01844 (18	0.00033 (16	0.00675 (15	0.00201 (14
D11	0.0347 (10)	0.0536 (13)	0.0300 (9)	−0.0065 (9)	0.0037 (8)	−0.0020 (8)
D12	0.0361 (10)	0.0316 (10)	0.0492 (11)	0.0117 (8)	0.0124 (9)	0.0054 (8)
D13	0.0375 (10)	0.0696 (15)	0.0309 (9)	0.0053 (10)	0.0180 (8)	0.0031 (9)
D14	0.0439 (11)	0.0335 (10)	0.0453 (11)	−0.0082 (9)	0.0118 (9)	0.0093 (8)
D15	0.0287 (9)	0.0338 (10)	0.0209 (8)	−0.0055 (8)	0.0044 (7)	0.0001 (7)
D16	0.0282 (9)	0.0351 (11)	0.0277 (8)	−0.0105 (8)	0.0099 (7)	−0.0001 (7)
D17	0.0192 (8)	0.0364 (11)	0.0327 (9)	0.0000 (8)	0.0065 (7)	0.0000 (7)
D18	0.0321 (10)	0.0241 (9)	0.0388 (10)	−0.0017 (8)	0.0145 (8)	0.0012 (8)
D19	0.0257 (8)	0.0357 (11)	0.0280 (8)	0.0039 (8)	0.0139 (7)	0.0033 (7)
D20	0.0269 (8)	0.0229 (9)	0.0268 (8)	0.0039 (7)	0.0077 (7)	0.0040 (7)
H11	0.0491 (14)	0.0758 (19)	0.0424 (13)	−0.0092 (13)	0.0052 (11)	−0.0028 (11)
H12	0.0511 (14)	0.0447 (14)	0.0696 (16)	0.0166 (12)	0.0176 (12)	0.0076 (11)
H13	0.0530 (14)	0.098 (2)	0.0437 (13)	0.0075 (14)	0.0255 (11)	0.0044 (13)
H14	0.0621 (15)	0.0474 (15)	0.0640 (15)	−0.0116 (13)	0.0167 (12)	0.0131 (12)
H15	0.0406 (13)	0.0479 (14)	0.0296 (11)	−0.0078 (11)	0.0063 (9)	0.0001 (9)
H16	0.0399 (13)	0.0497 (15)	0.0392 (12)	−0.0148 (11)	0.0140 (10)	−0.0001 (10)
H17	0.0272 (11)	0.0514 (15)	0.0463 (12)	0.0001 (11)	0.0091 (10)	0.0000 (11)
H18	0.0453 (13)	0.0341 (13)	0.0549 (14)	−0.0024 (11)	0.0206 (12)	0.0017 (11)
H19	0.0364 (12)	0.0505 (15)	0.0396 (12)	0.0055 (11)	0.0197 (10)	0.0047 (10)
H20	0.0381 (12)	0.0324 (12)	0.0379 (11)	0.0055 (11)	0.0108 (9)	0.0056 (9)

Geometric parameters (Å, º) top

Cu1—O7	2.0159 (6)	D13—D12	1.652 (3)
Cu1—O7ⁱ	2.0159 (6)	D13—D14	1.637 (3)
Cu1—O8ⁱⁱ	2.2973 (7)	D13—H11	1.667 (3)
Cu1—O8ⁱⁱⁱ	2.2973 (7)	D13—H12	1.652 (3)
Cu1—O9	1.9580 (6)	D13—H13	0.0006
Cu1—O9ⁱ	1.9580 (6)	D13—H14	1.637 (3)
Cu1—D15	2.5790 (16)	D14—O5^vii	1.881 (2)
Cu1—D15ⁱ	2.5790 (16)	D14—O8^xvi	2.646 (2)
Cu1—D16	2.6147 (16)	D14—N10	1.0221 (18)
Cu1—D16ⁱ	2.6147 (16)	D14—D11	1.659 (3)
Cu1—D19	2.5063 (16)	D14—D12	1.653 (3)
Cu1—D19ⁱ	2.5063 (16)	D14—D13	1.637 (3)
Cu1—D20^iv	2.5506 (16)	D14—H11	1.659 (3)
Cu1—D20^v	2.5506 (16)	D14—H12	1.654 (3)
Cu1—H15	2.5793 (16)	D14—H13	1.637 (3)
Cu1—H15ⁱ	2.5793 (16)	D14—H14	0.0005
Cu1—H16	2.6150 (16)	D15—Cu1	2.5790 (16)
Cu1—H16ⁱ	2.6150 (16)	D15—S2	2.7320 (19)
Cu1—H19	2.5061 (16)	D15—O5	1.7690 (17)
Cu1—H19ⁱ	2.5061 (16)	D15—O7	0.9746 (16)
Cu1—H20^iv	2.5506 (16)	D15—O9	2.6581 (18)
Cu1—H20^v	2.5506 (16)	D15—D16	1.581 (2)
S2—O3	1.4711 (13)	D15—H15	0.0003
S2—O4	1.4654 (13)	D15—H16	1.581 (2)
S2—O5	1.4833 (12)	D16—Cu1	2.6147 (16)
S2—O6	1.4751 (12)	D16—O6^xiii	1.8101 (18)
S2—D13^vi	2.662 (2)	D16—O7	0.9717 (16)
S2—D15	2.7320 (19)	D16—D15	1.581 (2)
S2—H13^vi	2.662 (2)	D16—H15	1.581 (2)
S2—H15	2.7317 (19)	D16—H16	0.0003
O3—S2	1.4711 (13)	D17—O4^xiii	1.8039 (18)
O3—O4	2.4007 (10)	D17—O8	0.9656 (17)
O3—O5	2.3967 (9)	D17—D18	1.537 (3)
O3—O6	2.4178 (9)	D17—H17	0.0003
O3—O9^vii	2.6795 (9)	D17—H18	1.537 (3)
O3—D12	1.9255 (19)	D18—O6^xvii	1.8568 (19)
O3—D13^vi	2.555 (2)	D18—O8	0.9672 (18)
O3—D20^viii	1.7159 (18)	D18—D17	1.537 (3)
O3—H12	1.9256 (19)	D18—H17	1.537 (3)
O3—H13^vi	2.555 (2)	D18—H18	0.0002
O3—H20^viii	1.7159 (18)	D19—Cu1	2.5063 (16)
O4—S2	1.4654 (13)	D19—O5^x	1.7435 (17)
O4—O3	2.4007 (10)	D19—O9	0.9767 (16)
O4—O5	2.3955 (9)	D19—D20^iv	1.562 (2)
O4—O6	2.4148 (9)	D19—H19	0.0003
O4—O8^ix	2.7691 (9)	D19—H20^iv	1.562 (2)
O4—D13^vi	1.9078 (18)	D20—Cu1^xviii	2.5506 (16)
O4—D17^ix	1.8039 (18)	D20—O3^vii	1.7159 (18)
O4—H13^vi	1.9082 (18)	D20—O9^xviii	0.9714 (17)
O4—H17^ix	1.8040 (18)	D20—D19^xviii	1.562 (2)
O5—S2	1.4833 (12)	D20—H19^xviii	1.562 (2)
O5—O3	2.3967 (9)	D20—H20	0.0002
O5—O4	2.3955 (9)	H11—O6^xv	1.8838 (19)
O5—O6	2.4129 (9)	H11—N10	1.0182 (17)
O5—O7	2.7404 (9)	H11—D11	0.0003
O5—O9^x	2.7150 (9)	H11—D12	1.695 (3)
O5—D14^viii	1.881 (2)	H11—D13	1.667 (3)
O5—D15	1.7690 (17)	H11—D14	1.659 (3)
O5—D19^x	1.7435 (17)	H11—H12	1.694 (3)
O5—H14^viii	1.880 (2)	H11—H13	1.666 (3)
O5—H15	1.7688 (17)	H11—H14	1.659 (3)
O5—H19^x	1.7439 (17)	H12—O3	1.9256 (19)
O6—S2	1.4751 (12)	H12—N10	1.0130 (17)
O6—O3	2.4178 (9)	H12—D11	1.694 (3)
O6—O4	2.4148 (9)	H12—D12	0.0006
O6—O5	2.4129 (9)	H12—D13	1.652 (3)
O6—O7^ix	2.7781 (9)	H12—D14	1.654 (3)
O6—D11^xi	1.8840 (19)	H12—H11	1.694 (3)
O6—D16^ix	1.8101 (18)	H12—H13	1.652 (3)
O6—D18^xii	1.8568 (19)	H12—H14	1.654 (3)
O6—H11^xi	1.8838 (19)	H13—S2^xvi	2.662 (2)
O6—H16^ix	1.8099 (18)	H13—O3^xvi	2.555 (2)
O6—H18^xii	1.8567 (19)	H13—O4^xvi	1.9082 (18)
O7—Cu1	2.0159 (6)	H13—N10	1.0150 (16)
O7—O5	2.7404 (9)	H13—D11	1.666 (3)
O7—O6^xiii	2.7781 (9)	H13—D12	1.652 (3)
O7—D15	0.9746 (16)	H13—D13	0.0006
O7—D16	0.9717 (16)	H13—D14	1.637 (3)
O7—H15	0.9748 (16)	H13—H11	1.666 (3)
O7—H16	0.9719 (16)	H13—H12	1.652 (3)
O8—Cu1^xiv	2.2973 (7)	H13—H14	1.637 (3)
O8—O4^xiii	2.7691 (9)	H14—O5^vii	1.880 (2)
O8—D14^vi	2.646 (2)	H14—O8^xvi	2.646 (2)
O8—D17	0.9656 (17)	H14—N10	1.0222 (18)
O8—D18	0.9672 (18)	H14—D11	1.659 (3)
O8—H14^vi	2.646 (2)	H14—D12	1.654 (3)
O8—H17	0.9655 (17)	H14—D13	1.637 (3)
O8—H18	0.9673 (18)	H14—D14	0.0005
O9—Cu1	1.9580 (6)	H14—H11	1.659 (3)
O9—O3^viii	2.6795 (9)	H14—H12	1.654 (3)
O9—O5^x	2.7150 (9)	H14—H13	1.637 (3)
O9—D15	2.6581 (18)	H15—Cu1	2.5793 (16)
O9—D19	0.9767 (16)	H15—S2	2.7317 (19)
O9—D20^iv	0.9714 (17)	H15—O5	1.7688 (17)
O9—H15	2.6583 (18)	H15—O7	0.9748 (16)
O9—H19	0.9764 (16)	H15—O9	2.6583 (18)
O9—H20^iv	0.9714 (17)	H15—D15	0.0003
N10—D11	1.0180 (17)	H15—D16	1.581 (2)
N10—D12	1.0130 (17)	H15—H16	1.581 (2)
N10—D13	1.0153 (16)	H16—Cu1	2.6150 (16)
N10—D14	1.0221 (18)	H16—O6^xiii	1.8099 (18)
N10—H11	1.0182 (17)	H16—O7	0.9719 (16)
N10—H12	1.0130 (17)	H16—D15	1.581 (2)
N10—H13	1.0150 (16)	H16—D16	0.0003
N10—H14	1.0222 (18)	H16—H15	1.581 (2)
D11—O6^xv	1.8840 (19)	H17—O4^xiii	1.8040 (18)
D11—N10	1.0180 (17)	H17—O8	0.9655 (17)
D11—D12	1.695 (3)	H17—D17	0.0003
D11—D13	1.666 (3)	H17—D18	1.537 (3)
D11—D14	1.659 (3)	H17—H18	1.537 (3)
D11—H11	0.0003	H18—O6^xvii	1.8567 (19)
D11—H12	1.694 (3)	H18—O8	0.9673 (18)
D11—H13	1.666 (3)	H18—D17	1.537 (3)
D11—H14	1.659 (3)	H18—D18	0.0002
D12—O3	1.9255 (19)	H18—H17	1.537 (3)
D12—N10	1.0130 (17)	H19—Cu1	2.5061 (16)
D12—D11	1.695 (3)	H19—O5^x	1.7439 (17)
D12—D13	1.652 (3)	H19—O9	0.9764 (16)
D12—D14	1.653 (3)	H19—D19	0.0003
D12—H11	1.695 (3)	H19—D20^iv	1.562 (2)
D12—H12	0.0006	H19—H20^iv	1.562 (2)
D12—H13	1.652 (3)	H20—Cu1^xviii	2.5506 (16)
D12—H14	1.654 (3)	H20—O3^vii	1.7159 (18)
D13—S2^xvi	2.662 (2)	H20—O9^xviii	0.9714 (17)
D13—O3^xvi	2.555 (2)	H20—D19^xviii	1.562 (2)
D13—O4^xvi	1.9078 (18)	H20—D20	0.0002
D13—N10	1.0153 (16)	H20—H19^xviii	1.562 (2)
D13—D11	1.666 (3)

D15—O7—D16	108.64 (16)	D11—N10—H13	110.07 (15)
D15—O7—H15	0.0	D11—N10—H14	108.83 (16)
D15—O7—H16	108.63 (16)	D12—N10—D13	109.08 (16)
D16—O7—H15	108.62 (16)	D12—N10—D14	108.66 (17)
D16—O7—H16	0.0	D12—N10—H11	113.08 (17)
H15—O7—H16	108.61 (16)	D12—N10—H12	0.0
D17—O8—D18	105.34 (17)	D12—N10—H13	109.06 (16)
D17—O8—H17	0.0	D12—N10—H14	108.68 (17)
D17—O8—H18	105.35 (17)	D13—N10—D14	106.92 (18)
D18—O8—H17	105.35 (17)	D13—N10—H11	110.08 (15)
D18—O8—H18	0.0	D13—N10—H12	109.08 (16)
H17—O8—H18	105.35 (17)	D13—N10—H13	0.0
D19—O9—D20^iv	106.60 (16)	D13—N10—H14	106.89 (18)
D19—O9—H19	0.0	D14—N10—H11	108.83 (16)
D19—O9—H20^iv	106.61 (16)	D14—N10—H12	108.69 (17)
D20^iv—O9—H19	106.60 (16)	D14—N10—H13	106.94 (18)
D20^iv—O9—H20^iv	0.0	D14—N10—H14	0.0
H19—O9—H20^iv	106.61 (16)	H11—N10—H12	113.05 (17)
D11—N10—D12	113.09 (17)	H11—N10—H13	110.08 (15)
D11—N10—D13	110.07 (15)	H11—N10—H14	108.83 (16)
D11—N10—D14	108.83 (16)	H12—N10—H13	109.06 (16)
D11—N10—H11	0.0	H12—N10—H14	108.71 (17)
D11—N10—H12	113.06 (17)	H13—N10—H14	106.92 (18)

(CuTS_62D_250K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.53D_2.47⁺)₂·CuH_4.87D_7.13O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 411.97	F(000) = 243
Monoclinic, P2₁/a	D_x = 1.957 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.3561 (3) Å	Cell parameters from 21844 reflections
b = 12.6163 (5) Å	µ = 0.15 mm⁻¹
c = 6.1226 (2) Å	T = 250 K
β = 106.762 (2)°	Block, blue
V = 692.00 (4) Å³	1.5 × 1.2 × 1.1 mm

Data collection top

TOPAZ Single Crystal Diffractometer	5546 measured reflections
Radiation source: spallation neutron source, SNS BL12	4438 independent reflections
Not applicable to TOF Laue technique monochromator	3622 reflections with > 3σ(I)
time–of–flight Laue scans	h = −18→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 1.007 + 0.456 * lambda [cm^-1] The value of 1.461(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −25→25
T_min = 0.752, T_max = 0.883	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.090	(Δ/σ)_max < 0.001
wR(F²) = 0.083	Δρ_max = 0.14E-12 cm Å^-3 e Å⁻³
S = 1.39	Δρ_min = −0.15E−12 cm Å⁻³ e Å⁻³
3622 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
188 parameters	Extinction coefficient: 1.93E-05 (9)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.01431
S2	0.39003 (15)	0.14279 (11)	0.7450 (2)	0.01536
O3	0.38724 (10)	0.23747 (7)	0.60369 (13)	0.0276
O4	0.53016 (9)	0.08554 (7)	0.77277 (15)	0.02997
O5	0.26438 (8)	0.07309 (6)	0.62625 (12)	0.02122
O6	0.37365 (9)	0.17347 (6)	0.96874 (12)	0.02425
O7	0.15498 (9)	0.10765 (7)	0.16528 (13)	0.02444
O8	0.81968 (9)	0.11249 (7)	0.04504 (14)	0.02503
O9	0.00561 (8)	−0.06601 (6)	0.29150 (12)	0.01823
N10	0.12541 (6)	0.35928 (5)	0.36938 (8)	0.02489
D11	0.0451 (3)	0.3440 (2)	0.2234 (4)	0.05529	0.61757
D12	0.2060 (3)	0.30390 (19)	0.4117 (4)	0.05317	0.61757
D13	0.0814 (3)	0.3681 (3)	0.4993 (4)	0.06687	0.61757
D14	0.1738 (3)	0.42979 (19)	0.3519 (4)	0.05913	0.61757
D15	0.2001 (2)	0.09264 (17)	0.3262 (3)	0.03604	0.59399
D16	0.2337 (2)	0.12498 (18)	0.0973 (3)	0.03735	0.59399
D17	0.7190 (2)	0.10138 (17)	−0.0502 (4)	0.03654	0.59399
D18	0.8420 (2)	0.18539 (17)	0.0199 (4)	0.0379	0.59399
D19	−0.0891 (2)	−0.06264 (17)	0.3275 (3)	0.0347	0.59399
D20	0.0385 (2)	0.86071 (16)	0.3138 (3)	0.03047	0.59399
H11	0.0451 (3)	0.3440 (2)	0.2234 (4)	0.07818	0.38243
H12	0.2060 (3)	0.30387 (19)	0.4117 (4)	0.0752	0.38243
H13	0.0814 (3)	0.3680 (3)	0.4993 (4)	0.09457	0.38243
H14	0.1738 (3)	0.42981 (19)	0.3520 (4)	0.08361	0.38243
H15	0.2001 (2)	0.09264 (17)	0.3263 (3)	0.05097	0.40601
H16	0.2337 (2)	0.12498 (18)	0.0973 (3)	0.05281	0.40601
H17	0.7190 (2)	0.10138 (17)	−0.0502 (4)	0.05167	0.40601
H18	0.8420 (2)	0.18540 (17)	0.0199 (4)	0.0536	0.40601
H19	−0.0891 (2)	−0.06264 (17)	0.3275 (3)	0.04907	0.40601
H20	0.0385 (2)	0.86071 (16)	0.3138 (3)	0.04309	0.40601

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.01315 (28	0.01628 (33	0.01311 (26	−0.00226 (25	0.00315 (22	0.00108 (23
S2	0.0133 (5)	0.0167 (6)	0.0157 (5)	−0.0023 (5)	0.0035 (4)	−0.0009 (5)
O3	0.0358 (4)	0.0218 (4)	0.0236 (4)	−0.00695 (34	0.00603 (32	0.00349 (28
O4	0.01600 (34	0.0389 (5)	0.0338 (4)	0.00500 (33	0.00513 (31	−0.0021 (4)
O5	0.01749 (31	0.0241 (4)	0.02167 (32	−0.00668 (28	0.00505 (26	−0.00292 (26
O6	0.0279 (4)	0.0276 (4)	0.01810 (31	−0.00261 (31	0.00803 (28	−0.00389 (26
O7	0.0217 (4)	0.0320 (4)	0.01881 (32	−0.00832 (31	0.00458 (28	0.00068 (29
O8	0.0201 (4)	0.0250 (4)	0.0295 (4)	0.00103 (31	0.00648 (31	0.00359 (30
O9	0.01932 (31	0.0195 (4)	0.01727 (29	0.00078 (27	0.00744 (25	0.00221 (24
N10	0.02363 (24	0.02860 (28	0.02396 (23	0.00072 (21	0.00929 (20	0.00268 (19
D11	0.0468 (14)	0.0755 (19)	0.0392 (12)	−0.0114 (13)	0.0054 (11)	−0.0026 (11)
D12	0.0496 (14)	0.0443 (14)	0.0671 (15)	0.0142 (12)	0.0191 (12)	0.0072 (12)
D13	0.0530 (15)	0.113 (2)	0.0427 (13)	0.0148 (16)	0.0266 (12)	0.0103 (14)
D14	0.0632 (16)	0.0447 (14)	0.0635 (16)	−0.0123 (13)	0.0086 (13)	0.0110 (12)
D15	0.0348 (11)	0.0445 (13)	0.0258 (10)	−0.0073 (10)	0.0039 (8)	−0.0003 (9)
D16	0.0354 (11)	0.0444 (14)	0.0332 (10)	−0.0137 (10)	0.0115 (9)	0.0003 (9)
D17	0.0249 (10)	0.0463 (14)	0.0385 (11)	0.0000 (10)	0.0093 (9)	0.0002 (10)
D18	0.0407 (12)	0.0302 (12)	0.0461 (13)	−0.0016 (10)	0.0179 (10)	0.0028 (10)
D19	0.0327 (11)	0.0421 (13)	0.0342 (10)	0.0040 (10)	0.0174 (9)	0.0050 (9)
D20	0.0326 (10)	0.0279 (11)	0.0316 (10)	0.0014 (9)	0.0105 (8)	0.0031 (8)
H11	0.0661 (19)	0.107 (3)	0.0554 (17)	−0.0161 (19)	0.0076 (15)	−0.0037 (16)
H12	0.070 (2)	0.063 (2)	0.095 (2)	0.0201 (17)	0.0270 (17)	0.0101 (16)
H13	0.075 (2)	0.160 (3)	0.0603 (18)	0.021 (2)	0.0376 (17)	0.015 (2)
H14	0.089 (2)	0.063 (2)	0.090 (2)	−0.0174 (19)	0.0122 (18)	0.0155 (17)
H15	0.0493 (16)	0.0629 (19)	0.0365 (14)	−0.0104 (14)	0.0056 (12)	−0.0004 (12)
H16	0.0501 (16)	0.0628 (19)	0.0469 (15)	−0.0193 (14)	0.0163 (13)	0.0005 (13)
H17	0.0352 (14)	0.066 (2)	0.0544 (15)	−0.0001 (14)	0.0131 (13)	0.0003 (14)
H18	0.0576 (18)	0.0427 (17)	0.0652 (18)	−0.0023 (15)	0.0253 (15)	0.0039 (14)
H19	0.0462 (15)	0.0595 (18)	0.0484 (15)	0.0057 (14)	0.0246 (13)	0.0070 (13)
H20	0.0461 (15)	0.0395 (15)	0.0448 (14)	0.0019 (13)	0.0148 (12)	0.0044 (12)

Geometric parameters (Å, º) top

Cu1—O7	2.0309 (8)	D13—D14	1.618 (4)
Cu1—O7ⁱ	2.0309 (8)	D13—H11	1.653 (3)
Cu1—O8ⁱⁱ	2.2813 (8)	D13—H12	1.632 (3)
Cu1—O8ⁱⁱⁱ	2.2813 (8)	D13—H13	0.0006
Cu1—O9	1.9564 (7)	D13—H14	1.618 (4)
Cu1—O9ⁱ	1.9564 (7)	D14—O5^vii	1.891 (3)
Cu1—D15	2.5891 (19)	D14—N10	1.018 (2)
Cu1—D15ⁱ	2.5891 (19)	D14—D11	1.641 (4)
Cu1—D16	2.621 (2)	D14—D12	1.638 (3)
Cu1—D16ⁱ	2.621 (2)	D14—D13	1.618 (4)
Cu1—D19	2.5110 (18)	D14—H11	1.642 (4)
Cu1—D19ⁱ	2.5110 (18)	D14—H12	1.639 (3)
Cu1—D20^iv	2.5517 (19)	D14—H13	1.618 (4)
Cu1—D20^v	2.5517 (19)	D14—H14	0.0005
Cu1—H15	2.5894 (19)	D15—Cu1	2.5891 (19)
Cu1—H15ⁱ	2.5894 (19)	D15—S2	2.740 (2)
Cu1—H16	2.621 (2)	D15—O5	1.777 (2)
Cu1—H16ⁱ	2.621 (2)	D15—O7	0.972 (2)
Cu1—H19	2.5108 (18)	D15—D16	1.576 (3)
Cu1—H19ⁱ	2.5108 (18)	D15—H15	0.0003
Cu1—H20^iv	2.5517 (19)	D15—H16	1.576 (3)
Cu1—H20^v	2.5517 (19)	D16—Cu1	2.621 (2)
S2—O3	1.4708 (16)	D16—O6^xiv	1.818 (2)
S2—O4	1.4632 (16)	D16—O7	0.9692 (19)
S2—O5	1.4802 (15)	D16—D15	1.576 (3)
S2—O6	1.4732 (15)	D16—H15	1.576 (3)
S2—D13^vi	2.653 (3)	D16—H16	0.0003
S2—D15	2.740 (2)	D17—O4^xiv	1.798 (2)
S2—H13^vi	2.654 (3)	D17—O8	0.965 (2)
S2—H15	2.739 (2)	D17—D18	1.532 (3)
O3—S2	1.4708 (16)	D17—H17	0.0003
O3—O4	2.3948 (12)	D17—H18	1.532 (3)
O3—O5	2.3943 (11)	D18—O6^xvii	1.847 (2)
O3—O6	2.4140 (10)	D18—O8	0.965 (2)
O3—O9^vii	2.6820 (11)	D18—D17	1.532 (3)
O3—D12	1.952 (3)	D18—H17	1.532 (3)
O3—D13^vi	2.480 (3)	D18—H18	0.0002
O3—D20^viii	1.719 (2)	D19—Cu1	2.5110 (18)
O3—H12	1.952 (3)	D19—O5^x	1.748 (2)
O3—H13^vi	2.480 (3)	D19—O9	0.9740 (19)
O3—H20^viii	1.719 (2)	D19—D20^iv	1.557 (3)
O4—S2	1.4632 (16)	D19—H19	0.0003
O4—O3	2.3948 (12)	D19—H20^iv	1.557 (3)
O4—O5	2.3930 (11)	D20—Cu1^xviii	2.5517 (19)
O4—O6	2.4141 (11)	D20—O3^vii	1.719 (2)
O4—O8^ix	2.7618 (12)	D20—O9^xviii	0.972 (2)
O4—D13^vi	1.959 (2)	D20—D19^xviii	1.557 (3)
O4—D17^ix	1.798 (2)	D20—H19^xviii	1.557 (3)
O4—H13^vi	1.959 (2)	D20—H20	0.0002
O4—H17^ix	1.798 (2)	H11—O6^xv	1.900 (2)
O5—S2	1.4802 (15)	H11—N10	1.007 (2)
O5—O3	2.3943 (11)	H11—D11	0.0003
O5—O4	2.3930 (11)	H11—D12	1.688 (3)
O5—O6	2.4103 (10)	H11—D13	1.653 (3)
O5—O7	2.7453 (10)	H11—D14	1.642 (4)
O5—O9^x	2.7159 (10)	H11—H12	1.688 (3)
O5—D14^viii	1.891 (3)	H11—H13	1.652 (3)
O5—D15	1.777 (2)	H11—H14	1.642 (4)
O5—D19^x	1.748 (2)	H12—O3	1.952 (3)
O5—H14^viii	1.891 (3)	H12—N10	1.006 (2)
O5—H15	1.777 (2)	H12—D11	1.688 (3)
O5—H19^x	1.748 (2)	H12—D12	0.0006
O6—S2	1.4732 (15)	H12—D13	1.632 (3)
O6—O3	2.4140 (10)	H12—D14	1.639 (3)
O6—O4	2.4141 (11)	H12—H11	1.688 (3)
O6—O5	2.4103 (10)	H12—H13	1.632 (3)
O6—D11^xi	1.900 (2)	H12—H14	1.639 (3)
O6—D16^ix	1.818 (2)	H13—S2^xvi	2.654 (3)
O6—D18^xii	1.847 (2)	H13—O3^xvi	2.480 (3)
O6—H11^xi	1.900 (2)	H13—O4^xvi	1.959 (2)
O6—H16^ix	1.818 (2)	H13—N10	1.002 (2)
O6—H18^xii	1.847 (2)	H13—D11	1.652 (3)
O7—Cu1	2.0309 (8)	H13—D12	1.632 (3)
O7—O5	2.7453 (10)	H13—D13	0.0006
O7—D15	0.972 (2)	H13—D14	1.618 (4)
O7—D16	0.9692 (19)	H13—H11	1.652 (3)
O7—H15	0.972 (2)	H13—H12	1.632 (3)
O7—H16	0.9695 (19)	H13—H14	1.618 (4)
O8—Cu1^xiii	2.2813 (8)	H14—O5^vii	1.891 (3)
O8—O4^xiv	2.7618 (12)	H14—N10	1.018 (2)
O8—D17	0.965 (2)	H14—D11	1.642 (4)
O8—D18	0.965 (2)	H14—D12	1.639 (3)
O8—H17	0.965 (2)	H14—D13	1.618 (4)
O8—H18	0.966 (2)	H14—D14	0.0005
O9—Cu1	1.9564 (7)	H14—H11	1.642 (4)
O9—O3^viii	2.6820 (11)	H14—H12	1.639 (3)
O9—O5^x	2.7159 (10)	H14—H13	1.618 (4)
O9—D19	0.9740 (19)	H15—Cu1	2.5894 (19)
O9—D20^iv	0.972 (2)	H15—S2	2.739 (2)
O9—H19	0.9736 (19)	H15—O5	1.777 (2)
O9—H20^iv	0.972 (2)	H15—O7	0.972 (2)
N10—D11	1.006 (2)	H15—D15	0.0003
N10—D12	1.006 (2)	H15—D16	1.576 (3)
N10—D13	1.002 (2)	H15—H16	1.576 (3)
N10—D14	1.018 (2)	H16—Cu1	2.621 (2)
N10—H11	1.007 (2)	H16—O6^xiv	1.818 (2)
N10—H12	1.006 (2)	H16—O7	0.9695 (19)
N10—H13	1.002 (2)	H16—D15	1.576 (3)
N10—H14	1.018 (2)	H16—D16	0.0003
D11—O6^xv	1.900 (2)	H16—H15	1.576 (3)
D11—N10	1.006 (2)	H17—O4^xiv	1.798 (2)
D11—D12	1.688 (3)	H17—O8	0.965 (2)
D11—D13	1.652 (3)	H17—D17	0.0003
D11—D14	1.641 (4)	H17—D18	1.532 (3)
D11—H11	0.0003	H17—H18	1.532 (3)
D11—H12	1.688 (3)	H18—O6^xvii	1.847 (2)
D11—H13	1.652 (3)	H18—O8	0.966 (2)
D11—H14	1.642 (4)	H18—D17	1.532 (3)
D12—O3	1.952 (3)	H18—D18	0.0002
D12—N10	1.006 (2)	H18—H17	1.532 (3)
D12—D11	1.688 (3)	H19—Cu1	2.5108 (18)
D12—D13	1.632 (3)	H19—O5^x	1.748 (2)
D12—D14	1.638 (3)	H19—O9	0.9736 (19)
D12—H11	1.688 (3)	H19—D19	0.0003
D12—H12	0.0006	H19—D20^iv	1.557 (3)
D12—H13	1.632 (3)	H19—H20^iv	1.557 (3)
D12—H14	1.639 (3)	H20—Cu1^xviii	2.5517 (19)
D13—S2^xvi	2.653 (3)	H20—O3^vii	1.719 (2)
D13—O3^xvi	2.480 (3)	H20—O9^xviii	0.972 (2)
D13—O4^xvi	1.959 (2)	H20—D19^xviii	1.557 (3)
D13—N10	1.002 (2)	H20—D20	0.0002
D13—D11	1.652 (3)	H20—H19^xviii	1.557 (3)
D13—D12	1.632 (3)

D15—O7—D16	108.52 (19)	D11—N10—H13	110.7 (2)
D15—O7—H15	0.0	D11—N10—H14	108.4 (2)
D15—O7—H16	108.51 (19)	D12—N10—D13	108.8 (2)
D16—O7—H15	108.50 (19)	D12—N10—D14	108.1 (2)
D16—O7—H16	0.0	D12—N10—H11	114.0 (2)
H15—O7—H16	108.49 (19)	D12—N10—H12	0.0
D17—O8—D18	105.1 (2)	D12—N10—H13	108.8 (2)
D17—O8—H17	0.0	D12—N10—H14	108.2 (2)
D17—O8—H18	105.1 (2)	D13—N10—D14	106.5 (3)
D18—O8—H17	105.1 (2)	D13—N10—H11	110.7 (2)
D18—O8—H18	0.0	D13—N10—H12	108.8 (2)
H17—O8—H18	105.1 (2)	D13—N10—H13	0.0
D19—O9—D20^iv	106.33 (19)	D13—N10—H14	106.5 (3)
D19—O9—H19	0.0	D14—N10—H11	108.4 (2)
D19—O9—H20^iv	106.33 (19)	D14—N10—H12	108.2 (2)
D20^iv—O9—H19	106.33 (19)	D14—N10—H13	106.5 (3)
D20^iv—O9—H20^iv	0.0	D14—N10—H14	0.0
H19—O9—H20^iv	106.34 (19)	H11—N10—H12	114.0 (2)
D11—N10—D12	114.1 (2)	H11—N10—H13	110.7 (2)
D11—N10—D13	110.7 (2)	H11—N10—H14	108.4 (2)
D11—N10—D14	108.4 (2)	H12—N10—H13	108.8 (2)
D11—N10—H11	0.0	H12—N10—H14	108.2 (2)
D11—N10—H12	114.0 (2)	H13—N10—H14	106.5 (3)

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x, y−1, z; (v) −x, −y+1, −z; (vi) x+1/2, −y+1/2, z; (vii) −x+1/2, y+1/2, −z+1; (viii) −x+1/2, y−1/2, −z+1; (ix) x, y, z+1; (x) −x, −y, −z+1; (xi) x+1/2, −y+1/2, z+1; (xii) x−1/2, −y+1/2, z+1; (xiii) x+1, y, z; (xiv) x, y, z−1; (xv) x−1/2, −y+1/2, z−1; (xvi) x−1/2, −y+1/2, z; (xvii) x+1/2, −y+1/2, z−1; (xviii) x, y+1, z.

(CuTS_62D_295K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.53D_2.47⁺)₂·CuH_4.87D_7.13O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 411.97	F(000) = 243
Monoclinic, P2₁/a	D_x = 1.960 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.3046 (3) Å	Cell parameters from 19587 reflections
b = 12.5166 (5) Å	µ = 0.15 mm⁻¹
c = 6.1831 (2) Å	T = 295 K
β = 106.453 (2)°	Block, blue
V = 690.61 (4) Å³	1.5 × 1.2 × 1.2 mm

Data collection top

TOPAZ Single Crystal Diffractometer	4055 measured reflections
Radiation source: spallation neutron source, SNS BL12	3119 independent reflections
Not applicable to TOF Laue technique monochromator	2545 reflections with > 3σ(I)
time–of–flight Laue scans	h = −18→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 1.011 + 0.460 * lambda [cm^-1] The value of 1.471(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −24→23
T_min = 0.750, T_max = 0.882	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.088	(Δ/σ)_max < 0.001
wR(F²) = 0.081	Δρ_max = 0.10E-12 cm Å^-3 e Å⁻³
S = 1.37	Δρ_min = −0.12E−12 cm Å⁻³ e Å⁻³
2545 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
187 parameters	Extinction coefficient: 1.47E-05 (8)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.01709
S2	0.39531 (19)	0.14133 (16)	0.7425 (3)	0.02057
O3	0.39650 (13)	0.23579 (9)	0.60104 (17)	0.03529
O4	0.53483 (12)	0.08217 (10)	0.7731 (2)	0.04077
O5	0.26904 (10)	0.07230 (8)	0.62506 (16)	0.02713
O6	0.37696 (12)	0.17444 (9)	0.96160 (15)	0.03196
O7	0.16020 (12)	0.10982 (9)	0.16723 (17)	0.03158
O8	0.82298 (12)	0.11210 (10)	0.03934 (18)	0.03182
O9	0.00169 (10)	−0.06546 (8)	0.28810 (15)	0.02247
N10	0.12663 (8)	0.35445 (7)	0.36345 (12)	0.03127
D11	0.0508 (4)	0.3409 (3)	0.2179 (5)	0.07475	0.61757
D12	0.2101 (4)	0.3020 (3)	0.4041 (6)	0.07311	0.61757
D13	0.0791 (4)	0.3549 (4)	0.4874 (5)	0.10133	0.61757
D14	0.1706 (5)	0.4259 (3)	0.3558 (7)	0.08677	0.61757
D15	0.2055 (3)	0.0931 (2)	0.3244 (4)	0.04518	0.59399
D16	0.2386 (3)	0.1254 (3)	0.0988 (4)	0.04692	0.59399
D17	0.7229 (3)	0.0991 (2)	−0.0544 (4)	0.04563	0.59399
D18	0.8450 (3)	0.1854 (2)	0.0112 (4)	0.04508	0.59399
D19	−0.0936 (3)	−0.0613 (2)	0.3239 (4)	0.0411	0.59399
D20	0.0342 (3)	0.8609 (2)	0.3127 (4)	0.03669	0.59399
H11	0.0508 (4)	0.3409 (3)	0.2179 (5)	0.10571	0.38243
H12	0.2100 (4)	0.3020 (3)	0.4041 (6)	0.1034	0.38243
H13	0.0792 (4)	0.3549 (4)	0.4874 (5)	0.1433	0.38243
H14	0.1706 (5)	0.4259 (3)	0.3558 (7)	0.1227	0.38243
H15	0.2055 (3)	0.0931 (2)	0.3245 (4)	0.06389	0.40601
H16	0.2387 (3)	0.1254 (3)	0.0988 (4)	0.06635	0.40601
H17	0.7229 (3)	0.0991 (2)	−0.0544 (4)	0.06453	0.40601
H18	0.8450 (3)	0.1854 (2)	0.0112 (4)	0.06375	0.40601
H19	−0.0936 (3)	−0.0613 (2)	0.3239 (4)	0.05812	0.40601
H20	0.0342 (3)	0.8609 (2)	0.3127 (4)	0.05189	0.40601

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0155 (4)	0.0191 (4)	0.0164 (4)	−0.00247 (34	0.00412 (30	0.00200 (32
S2	0.0183 (7)	0.0229 (9)	0.0206 (7)	−0.0031 (7)	0.0058 (6)	−0.0017 (7)
O3	0.0470 (6)	0.0281 (5)	0.0300 (5)	−0.0105 (5)	0.0097 (5)	0.0021 (4)
O4	0.0207 (5)	0.0488 (8)	0.0503 (7)	0.0050 (5)	0.0060 (5)	−0.0050 (6)
O5	0.0230 (4)	0.0303 (5)	0.0281 (5)	−0.0095 (4)	0.0071 (4)	−0.0041 (4)
O6	0.0392 (6)	0.0346 (6)	0.0236 (4)	−0.0038 (5)	0.0115 (4)	−0.0058 (4)
O7	0.0281 (5)	0.0423 (7)	0.0241 (5)	−0.0069 (5)	0.0070 (4)	0.0028 (4)
O8	0.0259 (5)	0.0320 (6)	0.0362 (5)	−0.0020 (5)	0.0065 (4)	0.0056 (5)
O9	0.0245 (4)	0.0225 (5)	0.0222 (4)	0.0011 (4)	0.0097 (4)	0.0030 (4)
N10	0.0303 (4)	0.0351 (4)	0.03064 (35	0.00098 (33	0.01221 (29	0.00244 (30
D11	0.065 (2)	0.105 (3)	0.0494 (18)	−0.025 (2)	0.0079 (16)	−0.0070 (18)
D12	0.068 (2)	0.056 (2)	0.101 (3)	0.0196 (19)	0.034 (2)	0.0091 (19)
D13	0.082 (3)	0.175 (5)	0.062 (2)	0.050 (3)	0.046 (2)	0.041 (3)
D14	0.101 (3)	0.059 (2)	0.087 (3)	−0.021 (2)	0.004 (2)	0.0087 (19)
D15	0.0430 (15)	0.058 (2)	0.0323 (14)	−0.0033 (14)	0.0063 (12)	0.0004 (13)
D16	0.0450 (16)	0.054 (2)	0.0427 (15)	−0.0131 (15)	0.0143 (14)	0.0017 (13)
D17	0.0330 (14)	0.057 (2)	0.0471 (15)	−0.0023 (14)	0.0119 (13)	0.0028 (14)
D18	0.0488 (16)	0.0364 (17)	0.0537 (17)	−0.0017 (14)	0.0204 (14)	0.0048 (14)
D19	0.0367 (14)	0.0531 (19)	0.0388 (14)	0.0063 (13)	0.0192 (12)	0.0066 (13)
D20	0.0392 (14)	0.0389 (16)	0.0343 (13)	0.0020 (13)	0.0142 (11)	0.0037 (12)
H11	0.092 (3)	0.148 (4)	0.070 (3)	−0.036 (3)	0.011 (2)	−0.010 (3)
H12	0.097 (3)	0.079 (3)	0.143 (4)	0.028 (3)	0.048 (3)	0.013 (3)
H13	0.117 (4)	0.248 (7)	0.088 (3)	0.071 (4)	0.065 (3)	0.057 (4)
H14	0.142 (4)	0.084 (3)	0.123 (4)	−0.030 (3)	0.005 (3)	0.012 (3)
H15	0.061 (2)	0.081 (3)	0.0456 (19)	−0.005 (2)	0.0089 (17)	0.0005 (18)
H16	0.064 (2)	0.077 (3)	0.060 (2)	−0.019 (2)	0.0203 (19)	0.0024 (19)
H17	0.047 (2)	0.081 (3)	0.067 (2)	−0.003 (2)	0.0168 (19)	0.004 (2)
H18	0.069 (2)	0.051 (2)	0.076 (2)	−0.003 (2)	0.029 (2)	0.0068 (19)
H19	0.052 (2)	0.075 (3)	0.0549 (19)	0.0089 (19)	0.0272 (17)	0.0093 (18)
H20	0.055 (2)	0.055 (2)	0.0485 (18)	0.0028 (19)	0.0200 (16)	0.0053 (17)

Geometric parameters (Å, º) top

Cu1—O7	2.0754 (11)	D13—D12	1.595 (5)
Cu1—O7ⁱ	2.0754 (11)	D13—D14	1.603 (6)
Cu1—O8ⁱⁱ	2.2288 (11)	D13—H11	1.621 (4)
Cu1—O8ⁱⁱⁱ	2.2288 (11)	D13—H12	1.595 (5)
Cu1—O9	1.9568 (9)	D13—H13	0.0006
Cu1—O9ⁱ	1.9568 (9)	D13—H14	1.603 (6)
Cu1—D15	2.620 (3)	D14—O5^vii	1.910 (4)
Cu1—D15ⁱ	2.620 (3)	D14—N10	0.990 (4)
Cu1—D16	2.646 (3)	D14—D11	1.601 (5)
Cu1—D16ⁱ	2.646 (3)	D14—D12	1.602 (5)
Cu1—D18ⁱⁱ	2.743 (3)	D14—D13	1.603 (6)
Cu1—D18ⁱⁱⁱ	2.743 (3)	D14—H11	1.601 (5)
Cu1—D19	2.519 (2)	D14—H12	1.602 (5)
Cu1—D19ⁱ	2.519 (2)	D14—H13	1.603 (6)
Cu1—D20^iv	2.554 (3)	D14—H14	0.0005
Cu1—D20^v	2.554 (3)	D15—Cu1	2.620 (3)
Cu1—H15	2.621 (3)	D15—O5	1.803 (3)
Cu1—H15ⁱ	2.621 (3)	D15—O7	0.966 (3)
Cu1—H16	2.646 (3)	D15—D16	1.565 (4)
Cu1—H16ⁱ	2.646 (3)	D15—H15	0.0003
Cu1—H18ⁱⁱ	2.743 (3)	D15—H16	1.565 (4)
Cu1—H18ⁱⁱⁱ	2.743 (3)	D16—Cu1	2.646 (3)
Cu1—H19	2.519 (2)	D16—O6^xiv	1.836 (3)
Cu1—H19ⁱ	2.519 (2)	D16—O7	0.961 (3)
Cu1—H20^iv	2.554 (3)	D16—D15	1.565 (4)
Cu1—H20^v	2.554 (3)	D16—H15	1.565 (4)
S2—O3	1.473 (2)	D16—H16	0.0003
S2—O4	1.460 (2)	D17—O4^xiv	1.785 (3)
S2—O5	1.473 (2)	D17—O8	0.961 (3)
S2—O6	1.4723 (19)	D17—D18	1.536 (4)
S2—D13^vi	2.635 (4)	D17—H17	0.0003
S2—H13^vi	2.635 (4)	D17—H18	1.536 (4)
O3—S2	1.473 (2)	D18—Cu1^xiii	2.743 (3)
O3—O4	2.3896 (17)	D18—O6^xvii	1.820 (3)
O3—O5	2.3908 (14)	D18—O8	0.966 (3)
O3—O6	2.4130 (14)	D18—D17	1.536 (4)
O3—O9^vii	2.6810 (15)	D18—H17	1.536 (4)
O3—D12	1.995 (4)	D18—H18	0.0002
O3—D13^vi	2.312 (4)	D19—Cu1	2.519 (2)
O3—D20^viii	1.720 (3)	D19—O5^x	1.753 (3)
O3—H12	1.996 (4)	D19—O9	0.974 (2)
O3—H13^vi	2.312 (4)	D19—D20^iv	1.554 (4)
O3—H20^viii	1.720 (3)	D19—H19	0.0003
O4—S2	1.460 (2)	D19—H20^iv	1.554 (4)
O4—O3	2.3896 (17)	D20—Cu1^xviii	2.554 (3)
O4—O5	2.3847 (14)	D20—O3^vii	1.720 (3)
O4—O6	2.4123 (16)	D20—O9^xviii	0.969 (3)
O4—O8^ix	2.7456 (15)	D20—D19^xviii	1.554 (4)
O4—D13^vi	2.079 (4)	D20—H19^xviii	1.553 (4)
O4—D17^ix	1.785 (3)	D20—H20	0.0002
O4—H13^vi	2.080 (4)	H11—O6^xv	1.927 (3)
O4—H17^ix	1.785 (3)	H11—N10	0.988 (3)
O5—S2	1.473 (2)	H11—D11	0.0003
O5—O3	2.3908 (14)	H11—D12	1.671 (5)
O5—O4	2.3847 (14)	H11—D13	1.621 (4)
O5—O6	2.4060 (13)	H11—D14	1.601 (5)
O5—O7	2.7633 (14)	H11—H12	1.671 (5)
O5—O9^x	2.7217 (13)	H11—H13	1.621 (4)
O5—D14^viii	1.910 (4)	H11—H14	1.601 (5)
O5—D15	1.803 (3)	H12—O3	1.996 (4)
O5—D19^x	1.753 (3)	H12—N10	0.993 (3)
O5—H14^viii	1.910 (4)	H12—D11	1.671 (5)
O5—H15	1.803 (3)	H12—D12	0.0006
O5—H19^x	1.754 (3)	H12—D13	1.595 (5)
O6—S2	1.4723 (19)	H12—D14	1.602 (5)
O6—O3	2.4130 (14)	H12—H11	1.671 (5)
O6—O4	2.4123 (16)	H12—H13	1.594 (5)
O6—O5	2.4060 (13)	H12—H14	1.603 (5)
O6—D11^xi	1.927 (3)	H13—S2^xvi	2.635 (4)
O6—D16^ix	1.836 (3)	H13—O3^xvi	2.312 (4)
O6—D18^xii	1.820 (3)	H13—O4^xvi	2.080 (4)
O6—H11^xi	1.927 (3)	H13—N10	0.987 (3)
O6—H16^ix	1.836 (3)	H13—D11	1.621 (4)
O6—H18^xii	1.820 (3)	H13—D12	1.594 (5)
O7—Cu1	2.0754 (11)	H13—D13	0.0006
O7—O5	2.7633 (14)	H13—D14	1.603 (6)
O7—D15	0.966 (3)	H13—H11	1.621 (4)
O7—D16	0.961 (3)	H13—H12	1.594 (5)
O7—H15	0.967 (3)	H13—H14	1.603 (6)
O7—H16	0.962 (3)	H14—O5^vii	1.910 (4)
O8—Cu1^xiii	2.2288 (11)	H14—N10	0.990 (4)
O8—O4^xiv	2.7456 (15)	H14—D11	1.601 (5)
O8—D17	0.961 (3)	H14—D12	1.602 (5)
O8—D18	0.966 (3)	H14—D13	1.603 (6)
O8—H17	0.961 (3)	H14—D14	0.0005
O8—H18	0.966 (3)	H14—H11	1.601 (5)
O9—Cu1	1.9568 (9)	H14—H12	1.603 (5)
O9—O3^viii	2.6810 (15)	H14—H13	1.603 (6)
O9—O5^x	2.7217 (13)	H15—Cu1	2.621 (3)
O9—D19	0.974 (2)	H15—O5	1.803 (3)
O9—D20^iv	0.969 (3)	H15—O7	0.967 (3)
O9—H19	0.974 (2)	H15—D15	0.0003
O9—H20^iv	0.969 (3)	H15—D16	1.565 (4)
N10—D11	0.988 (3)	H15—H16	1.565 (4)
N10—D12	0.993 (3)	H16—Cu1	2.646 (3)
N10—D13	0.987 (3)	H16—O6^xiv	1.836 (3)
N10—D14	0.990 (4)	H16—O7	0.962 (3)
N10—H11	0.988 (3)	H16—D15	1.565 (4)
N10—H12	0.993 (3)	H16—D16	0.0003
N10—H13	0.987 (3)	H16—H15	1.565 (4)
N10—H14	0.990 (4)	H17—O4^xiv	1.785 (3)
D11—O6^xv	1.927 (3)	H17—O8	0.961 (3)
D11—N10	0.988 (3)	H17—D17	0.0003
D11—D12	1.671 (5)	H17—D18	1.536 (4)
D11—D13	1.621 (4)	H17—H18	1.536 (4)
D11—D14	1.601 (5)	H18—Cu1^xiii	2.743 (3)
D11—H11	0.0003	H18—O6^xvii	1.820 (3)
D11—H12	1.671 (5)	H18—O8	0.966 (3)
D11—H13	1.621 (4)	H18—D17	1.536 (4)
D11—H14	1.601 (5)	H18—D18	0.0002
D12—O3	1.995 (4)	H18—H17	1.536 (4)
D12—N10	0.993 (3)	H19—Cu1	2.519 (2)
D12—D11	1.671 (5)	H19—O5^x	1.754 (3)
D12—D13	1.595 (5)	H19—O9	0.974 (2)
D12—D14	1.602 (5)	H19—D19	0.0003
D12—H11	1.671 (5)	H19—D20^iv	1.553 (4)
D12—H12	0.0006	H19—H20^iv	1.553 (4)
D12—H13	1.594 (5)	H20—Cu1^xviii	2.554 (3)
D12—H14	1.602 (5)	H20—O3^vii	1.720 (3)
D13—S2^xvi	2.635 (4)	H20—O9^xviii	0.969 (3)
D13—O3^xvi	2.312 (4)	H20—D19^xviii	1.554 (4)
D13—O4^xvi	2.079 (4)	H20—D20	0.0002
D13—N10	0.987 (3)	H20—H19^xviii	1.553 (4)
D13—D11	1.621 (4)

D15—O7—D16	108.5 (3)	D11—N10—H13	110.3 (3)
D15—O7—H15	0.0	D11—N10—H14	108.0 (3)
D15—O7—H16	108.5 (3)	D12—N10—D13	107.3 (3)
D16—O7—H15	108.5 (3)	D12—N10—D14	107.8 (3)
D16—O7—H16	0.0	D12—N10—H11	115.0 (3)
H15—O7—H16	108.5 (3)	D12—N10—H12	0.0
D17—O8—D18	105.7 (3)	D12—N10—H13	107.3 (3)
D17—O8—H17	0.0	D12—N10—H14	107.8 (3)
D17—O8—H18	105.7 (3)	D13—N10—D14	108.3 (4)
D18—O8—H17	105.7 (3)	D13—N10—H11	110.3 (3)
D18—O8—H18	0.0	D13—N10—H12	107.3 (3)
H17—O8—H18	105.7 (3)	D13—N10—H13	0.0
D19—O9—D20^iv	106.2 (3)	D13—N10—H14	108.3 (4)
D19—O9—H19	0.0	D14—N10—H11	108.0 (3)
D19—O9—H20^iv	106.2 (3)	D14—N10—H12	107.8 (3)
D20^iv—O9—H19	106.2 (3)	D14—N10—H13	108.3 (4)
D20^iv—O9—H20^iv	0.0	D14—N10—H14	0.0
H19—O9—H20^iv	106.2 (3)	H11—N10—H12	115.0 (3)
D11—N10—D12	115.0 (3)	H11—N10—H13	110.3 (3)
D11—N10—D13	110.3 (3)	H11—N10—H14	108.0 (3)
D11—N10—D14	108.0 (3)	H12—N10—H13	107.2 (3)
D11—N10—H11	0.0	H12—N10—H14	107.8 (3)
D11—N10—H12	115.0 (3)	H13—N10—H14	108.3 (4)

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x, y−1, z; (v) −x, −y+1, −z; (vi) x+1/2, −y+1/2, z; (vii) −x+1/2, y+1/2, −z+1; (viii) −x+1/2, y−1/2, −z+1; (ix) x, y, z+1; (x) −x, −y, −z+1; (xi) x+1/2, −y+1/2, z+1; (xii) x−1/2, −y+1/2, z+1; (xiii) x+1, y, z; (xiv) x, y, z−1; (xv) x−1/2, −y+1/2, z−1; (xvi) x−1/2, −y+1/2, z; (xvii) x+1/2, −y+1/2, z−1; (xviii) x, y+1, z.

(CuTS_62D_II_295K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.53D_2.47⁺)₂·CuH_4.87D_7.13O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 411.97	F(000) = 243
Monoclinic, P2₁/a	D_x = 1.957 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.3067 (3) Å	Cell parameters from 19462 reflections
b = 12.5071 (4) Å	µ = 0.15 mm⁻¹
c = 6.1856 (2) Å	T = 295 K
β = 106.346 (2)°	Block, blue
V = 690.89 (4) Å³	1.50 × 1.00 × 1.00 mm

Data collection top

TOPAZ Single Crystal Diffractometer	4121 measured reflections
Radiation source: spallation neutron source, SNS BL12	3128 independent reflections
Not applicable to TOF Laue technique monochromator	2472 reflections with > 3σ(I)
time–of–flight Laue scans	h = −18→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 1.011 + 0.460 * lambda [cm^-1] The value of 1.471(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −25→25
T_min = 0.770, T_max = 0.892	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.091	(Δ/σ)_max < 0.001
wR(F²) = 0.083	Δρ_max = 0.14E-12 cm Å^-3 e Å⁻³
S = 1.40	Δρ_min = −0.12E−12 cm Å⁻³ e Å⁻³
2472 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
187 parameters	Extinction coefficient: 6.8E-05 (2)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.01643
S2	0.3956 (2)	0.14132 (14)	0.7426 (3)	0.01994
O3	0.39659 (16)	0.23552 (9)	0.60090 (18)	0.03489
O4	0.53497 (16)	0.08183 (10)	0.7739 (2)	0.04002
O5	0.26894 (13)	0.07230 (8)	0.62498 (17)	0.02645
O6	0.37729 (15)	0.17461 (9)	0.96161 (18)	0.0315
O7	0.16012 (15)	0.10979 (10)	0.16774 (19)	0.03172
O8	0.82287 (15)	0.11209 (9)	0.0395 (2)	0.03167
O9	0.00195 (13)	−0.06551 (8)	0.28815 (16)	0.02214
N10	0.12668 (10)	0.35458 (6)	0.36347 (13)	0.03102
D11	0.0503 (5)	0.3398 (3)	0.2184 (6)	0.07703	0.61757
D12	0.2094 (5)	0.3023 (3)	0.4055 (7)	0.07524	0.61757
D13	0.0797 (5)	0.3546 (4)	0.4871 (6)	0.1035	0.61757
D14	0.1694 (5)	0.4262 (3)	0.3561 (7)	0.08689	0.61757
D15	0.2060 (4)	0.0931 (2)	0.3244 (5)	0.04402	0.59399
D16	0.2382 (4)	0.1265 (3)	0.0993 (5)	0.04599	0.59399
D17	0.7215 (4)	0.0993 (2)	−0.0556 (5)	0.04517	0.59399
D18	0.8451 (4)	0.1853 (2)	0.0126 (5)	0.04618	0.59399
D19	−0.0927 (4)	−0.0614 (2)	0.3243 (4)	0.03938	0.59399
D20	0.0349 (3)	0.8607 (2)	0.3131 (4)	0.03671	0.59399
H11	0.0503 (5)	0.3398 (3)	0.2184 (6)	0.10893	0.38243
H12	0.2093 (5)	0.3022 (3)	0.4055 (7)	0.1064	0.38243
H13	0.0797 (5)	0.3546 (4)	0.4870 (6)	0.14636	0.38243
H14	0.1693 (5)	0.4263 (3)	0.3562 (7)	0.12288	0.38243
H15	0.2060 (4)	0.0931 (2)	0.3244 (5)	0.06225	0.40601
H16	0.2383 (4)	0.1265 (3)	0.0993 (5)	0.06504	0.40601
H17	0.7215 (4)	0.0993 (2)	−0.0555 (5)	0.06387	0.40601
H18	0.8451 (4)	0.1853 (2)	0.0126 (5)	0.0653	0.40601
H19	−0.0927 (4)	−0.0614 (2)	0.3243 (4)	0.05569	0.40601
H20	0.0350 (3)	0.8607 (2)	0.3132 (4)	0.05191	0.40601

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0150 (5)	0.0185 (4)	0.0155 (4)	−0.00293 (34	0.0039 (4)	0.00108 (32
S2	0.0185 (11)	0.0213 (8)	0.0200 (8)	−0.0027 (7)	0.0054 (7)	−0.0012 (7)
O3	0.0482 (9)	0.0274 (5)	0.0285 (5)	−0.0120 (5)	0.0098 (5)	0.0018 (4)
O4	0.0200 (7)	0.0487 (7)	0.0497 (7)	0.0052 (5)	0.0071 (6)	−0.0057 (6)
O5	0.0218 (6)	0.0301 (5)	0.0271 (5)	−0.0091 (4)	0.0061 (4)	−0.0041 (4)
O6	0.0383 (8)	0.0343 (5)	0.0230 (5)	−0.0035 (5)	0.0105 (5)	−0.0045 (4)
O7	0.0280 (7)	0.0429 (6)	0.0236 (5)	−0.0057 (5)	0.0063 (5)	0.0040 (5)
O8	0.0264 (7)	0.0307 (6)	0.0366 (6)	−0.0012 (5)	0.0068 (5)	0.0060 (5)
O9	0.0234 (6)	0.0232 (5)	0.0213 (4)	0.0005 (4)	0.0088 (4)	0.0033 (4)
N10	0.0307 (5)	0.0340 (4)	0.0304 (4)	0.00181 (34	0.01188 (34	0.00317 (32
D11	0.066 (3)	0.108 (3)	0.054 (2)	−0.026 (2)	0.0103 (19)	−0.010 (2)
D12	0.070 (3)	0.063 (2)	0.099 (3)	0.022 (2)	0.034 (2)	0.014 (2)
D13	0.082 (4)	0.184 (5)	0.059 (2)	0.056 (3)	0.044 (2)	0.043 (3)
D14	0.104 (4)	0.055 (2)	0.083 (3)	−0.019 (2)	−0.004 (3)	0.016 (2)
D15	0.040 (2)	0.0567 (18)	0.0316 (14)	−0.0035 (14)	0.0042 (14)	0.0000 (14)
D16	0.041 (2)	0.0554 (18)	0.0440 (17)	−0.0104 (15)	0.0165 (16)	0.0032 (15)
D17	0.031 (2)	0.0577 (19)	0.0482 (17)	−0.0005 (15)	0.0126 (16)	0.0019 (16)
D18	0.050 (2)	0.0386 (16)	0.0539 (19)	−0.0055 (14)	0.0204 (17)	−0.0001 (14)
D19	0.042 (2)	0.0442 (16)	0.0362 (15)	0.0055 (13)	0.0186 (15)	0.0042 (13)
D20	0.039 (2)	0.0358 (14)	0.0356 (14)	0.0047 (13)	0.0118 (13)	0.0037 (13)
H11	0.093 (4)	0.153 (5)	0.076 (3)	−0.037 (3)	0.015 (3)	−0.014 (3)
H12	0.100 (4)	0.089 (3)	0.140 (4)	0.031 (3)	0.048 (3)	0.019 (3)
H13	0.116 (5)	0.261 (7)	0.083 (3)	0.079 (5)	0.062 (3)	0.061 (4)
H14	0.147 (6)	0.078 (3)	0.118 (4)	−0.027 (3)	−0.005 (4)	0.023 (3)
H15	0.057 (3)	0.080 (3)	0.045 (2)	−0.005 (2)	0.0059 (19)	−0.000 (2)
H16	0.058 (3)	0.078 (3)	0.062 (2)	−0.015 (2)	0.023 (2)	0.005 (2)
H17	0.043 (3)	0.082 (3)	0.068 (2)	−0.001 (2)	0.018 (2)	0.003 (2)
H18	0.070 (3)	0.055 (2)	0.076 (3)	−0.008 (2)	0.029 (2)	−0.000 (2)
H19	0.060 (3)	0.063 (2)	0.051 (2)	0.0077 (19)	0.026 (2)	0.0060 (18)
H20	0.056 (3)	0.051 (2)	0.050 (2)	0.0066 (18)	0.0166 (18)	0.0052 (18)

Geometric parameters (Å, º) top

Cu1—O7	2.0767 (12)	D13—D12	1.576 (5)
Cu1—O7ⁱ	2.0767 (12)	D13—D14	1.592 (6)
Cu1—O8ⁱⁱ	2.2291 (13)	D13—H11	1.617 (5)
Cu1—O8ⁱⁱⁱ	2.2291 (13)	D13—H12	1.576 (5)
Cu1—O9	1.9571 (9)	D13—H13	0.0006
Cu1—O9ⁱ	1.9571 (9)	D13—H14	1.592 (6)
Cu1—D15	2.625 (3)	D14—O5^vii	1.909 (4)
Cu1—D15ⁱ	2.625 (3)	D14—N10	0.986 (3)
Cu1—D16	2.652 (3)	D14—D11	1.609 (5)
Cu1—D16ⁱ	2.652 (3)	D14—D12	1.604 (5)
Cu1—D18ⁱⁱ	2.742 (3)	D14—D13	1.592 (6)
Cu1—D18ⁱⁱⁱ	2.742 (3)	D14—H11	1.609 (5)
Cu1—D19	2.516 (3)	D14—H12	1.604 (5)
Cu1—D19ⁱ	2.516 (3)	D14—H13	1.592 (6)
Cu1—D20^iv	2.557 (3)	D14—H14	0.0005
Cu1—D20^v	2.557 (3)	D15—Cu1	2.625 (3)
Cu1—H15	2.625 (3)	D15—O5	1.804 (3)
Cu1—H15ⁱ	2.625 (3)	D15—O7	0.965 (3)
Cu1—H16	2.652 (3)	D15—D16	1.561 (4)
Cu1—H16ⁱ	2.652 (3)	D15—H15	0.0003
Cu1—H18ⁱⁱ	2.742 (3)	D15—H16	1.562 (4)
Cu1—H18ⁱⁱⁱ	2.742 (3)	D16—Cu1	2.652 (3)
Cu1—H19	2.516 (3)	D16—O6^xiv	1.839 (3)
Cu1—H19ⁱ	2.516 (3)	D16—O7	0.962 (3)
Cu1—H20^iv	2.557 (3)	D16—D15	1.561 (4)
Cu1—H20^v	2.557 (3)	D16—H15	1.561 (4)
S2—O3	1.470 (2)	D16—H16	0.0003
S2—O4	1.461 (2)	D17—O4^xiv	1.773 (4)
S2—O5	1.477 (2)	D17—O8	0.974 (3)
S2—O6	1.472 (2)	D17—D18	1.544 (4)
S2—D13^vi	2.638 (4)	D17—H17	0.0003
S2—H13^vi	2.639 (4)	D17—H18	1.544 (4)
O3—S2	1.470 (2)	D18—Cu1^xiii	2.742 (3)
O3—O4	2.3922 (18)	D18—O6^xvii	1.820 (3)
O3—O5	2.3876 (14)	D18—O8	0.964 (3)
O3—O6	2.4117 (15)	D18—D17	1.544 (4)
O3—O9^vii	2.6816 (14)	D18—H17	1.544 (4)
O3—D12	2.002 (4)	D18—H18	0.0002
O3—D13^vi	2.312 (5)	D19—Cu1	2.516 (3)
O3—D20^viii	1.717 (3)	D19—O5^x	1.760 (3)
O3—H12	2.002 (4)	D19—O9	0.970 (3)
O3—H13^vi	2.312 (5)	D19—D20^iv	1.553 (4)
O3—H20^viii	1.717 (3)	D19—H19	0.0003
O4—S2	1.461 (2)	D19—H20^iv	1.553 (4)
O4—O3	2.3922 (18)	D20—Cu1^xviii	2.557 (3)
O4—O5	2.3893 (19)	D20—O3^vii	1.717 (3)
O4—O6	2.4099 (17)	D20—O9^xviii	0.971 (3)
O4—O8^ix	2.747 (2)	D20—D19^xviii	1.553 (4)
O4—D13^vi	2.090 (4)	D20—H19^xviii	1.553 (4)
O4—D17^ix	1.773 (4)	D20—H20	0.0002
O4—H13^vi	2.090 (4)	H11—O6^xv	1.926 (4)
O4—H17^ix	1.773 (4)	H11—N10	0.993 (4)
O5—S2	1.477 (2)	H11—D11	0.0003
O5—O3	2.3876 (14)	H11—D12	1.669 (5)
O5—O4	2.3893 (19)	H11—D13	1.617 (5)
O5—O6	2.4100 (15)	H11—D14	1.609 (5)
O5—O7	2.7627 (16)	H11—H12	1.669 (5)
O5—O9^x	2.7230 (16)	H11—H13	1.617 (5)
O5—D14^viii	1.909 (4)	H11—H14	1.610 (5)
O5—D15	1.804 (3)	H12—O3	2.002 (4)
O5—D19^x	1.760 (3)	H12—N10	0.988 (4)
O5—H14^viii	1.909 (4)	H12—D11	1.669 (5)
O5—H15	1.804 (3)	H12—D12	0.0006
O5—H19^x	1.760 (3)	H12—D13	1.576 (5)
O6—S2	1.472 (2)	H12—D14	1.604 (5)
O6—O3	2.4117 (15)	H12—H11	1.669 (5)
O6—O4	2.4099 (17)	H12—H13	1.575 (5)
O6—O5	2.4100 (15)	H12—H14	1.604 (5)
O6—D11^xi	1.926 (4)	H13—S2^xvi	2.639 (4)
O6—D16^ix	1.839 (3)	H13—O3^xvi	2.312 (5)
O6—D18^xii	1.820 (3)	H13—O4^xvi	2.090 (4)
O6—H11^xi	1.926 (4)	H13—N10	0.982 (3)
O6—H16^ix	1.839 (3)	H13—D11	1.617 (5)
O6—H18^xii	1.820 (3)	H13—D12	1.575 (5)
O7—Cu1	2.0767 (12)	H13—D13	0.0006
O7—O5	2.7627 (16)	H13—D14	1.592 (6)
O7—D15	0.965 (3)	H13—H11	1.617 (5)
O7—D16	0.962 (3)	H13—H12	1.575 (5)
O7—H15	0.966 (3)	H13—H14	1.592 (6)
O7—H16	0.962 (3)	H14—O5^vii	1.909 (4)
O8—Cu1^xiii	2.2291 (13)	H14—N10	0.987 (3)
O8—O4^xiv	2.747 (2)	H14—D11	1.609 (5)
O8—D17	0.974 (3)	H14—D12	1.604 (5)
O8—D18	0.964 (3)	H14—D13	1.592 (6)
O8—H17	0.974 (3)	H14—D14	0.0005
O8—H18	0.964 (3)	H14—H11	1.610 (5)
O9—Cu1	1.9571 (9)	H14—H12	1.604 (5)
O9—O3^viii	2.6816 (14)	H14—H13	1.592 (6)
O9—O5^x	2.7230 (16)	H15—Cu1	2.625 (3)
O9—D19	0.970 (3)	H15—O5	1.804 (3)
O9—D20^iv	0.971 (3)	H15—O7	0.966 (3)
O9—H19	0.969 (3)	H15—D15	0.0003
O9—H20^iv	0.971 (3)	H15—D16	1.561 (4)
N10—D11	0.993 (4)	H15—H16	1.562 (4)
N10—D12	0.988 (4)	H16—Cu1	2.652 (3)
N10—D13	0.982 (3)	H16—O6^xiv	1.839 (3)
N10—D14	0.986 (3)	H16—O7	0.962 (3)
N10—H11	0.993 (4)	H16—D15	1.562 (4)
N10—H12	0.988 (4)	H16—D16	0.0003
N10—H13	0.982 (3)	H16—H15	1.562 (4)
N10—H14	0.987 (3)	H17—O4^xiv	1.773 (4)
D11—O6^xv	1.926 (4)	H17—O8	0.974 (3)
D11—N10	0.993 (4)	H17—D17	0.0003
D11—D12	1.669 (5)	H17—D18	1.544 (4)
D11—D13	1.617 (5)	H17—H18	1.544 (4)
D11—D14	1.609 (5)	H18—Cu1^xiii	2.742 (3)
D11—H11	0.0003	H18—O6^xvii	1.820 (3)
D11—H12	1.669 (5)	H18—O8	0.964 (3)
D11—H13	1.617 (5)	H18—D17	1.544 (4)
D11—H14	1.609 (5)	H18—D18	0.0002
D12—O3	2.002 (4)	H18—H17	1.544 (4)
D12—N10	0.988 (4)	H19—Cu1	2.516 (3)
D12—D11	1.669 (5)	H19—O5^x	1.760 (3)
D12—D13	1.576 (5)	H19—O9	0.969 (3)
D12—D14	1.604 (5)	H19—D19	0.0003
D12—H11	1.669 (5)	H19—D20^iv	1.553 (4)
D12—H12	0.0006	H19—H20^iv	1.553 (4)
D12—H13	1.575 (5)	H20—Cu1^xviii	2.557 (3)
D12—H14	1.604 (5)	H20—O3^vii	1.717 (3)
D13—S2^xvi	2.638 (4)	H20—O9^xviii	0.971 (3)
D13—O3^xvi	2.312 (5)	H20—D19^xviii	1.553 (4)
D13—O4^xvi	2.090 (4)	H20—D20	0.0002
D13—N10	0.982 (3)	H20—H19^xviii	1.553 (4)
D13—D11	1.617 (5)

D15—O7—D16	108.3 (3)	D11—N10—H13	110.0 (4)
D15—O7—H15	0.0	D11—N10—H14	108.8 (3)
D15—O7—H16	108.2 (3)	D12—N10—D13	106.3 (3)
D16—O7—H15	108.2 (3)	D12—N10—D14	108.7 (4)
D16—O7—H16	0.0	D12—N10—H11	114.9 (4)
H15—O7—H16	108.2 (3)	D12—N10—H12	0.0
D17—O8—D18	105.7 (3)	D12—N10—H13	106.3 (3)
D17—O8—H17	0.0	D12—N10—H14	108.7 (4)
D17—O8—H18	105.7 (3)	D13—N10—D14	108.0 (4)
D18—O8—H17	105.7 (3)	D13—N10—H11	110.0 (4)
D18—O8—H18	0.0	D13—N10—H12	106.3 (3)
H17—O8—H18	105.7 (3)	D13—N10—H13	0.0
D19—O9—D20^iv	106.3 (3)	D13—N10—H14	108.0 (4)
D19—O9—H19	0.0	D14—N10—H11	108.8 (3)
D19—O9—H20^iv	106.3 (3)	D14—N10—H12	108.7 (4)
D20^iv—O9—H19	106.3 (3)	D14—N10—H13	108.0 (4)
D20^iv—O9—H20^iv	0.0	D14—N10—H14	0.0
H19—O9—H20^iv	106.3 (3)	H11—N10—H12	114.9 (4)
D11—N10—D12	114.9 (4)	H11—N10—H13	110.0 (4)
D11—N10—D13	110.0 (4)	H11—N10—H14	108.8 (3)
D11—N10—D14	108.8 (3)	H12—N10—H13	106.3 (3)
D11—N10—H11	0.0	H12—N10—H14	108.7 (4)
D11—N10—H12	114.9 (4)	H13—N10—H14	108.0 (4)

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x, y−1, z; (v) −x, −y+1, −z; (vi) x+1/2, −y+1/2, z; (vii) −x+1/2, y+1/2, −z+1; (viii) −x+1/2, y−1/2, −z+1; (ix) x, y, z+1; (x) −x, −y, −z+1; (xi) x+1/2, −y+1/2, z+1; (xii) x−1/2, −y+1/2, z+1; (xiii) x+1, y, z; (xiv) x, y, z−1; (xv) x−1/2, −y+1/2, z−1; (xvi) x−1/2, −y+1/2, z; (xvii) x+1/2, −y+1/2, z−1; (xviii) x, y+1, z.

(CUTS_74D_295K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.24D_2.76⁺)₂·CuH_3.64D_8.36O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 413.80	F(000) = 204
Monoclinic, P2₁/a	D_x = 1.952 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.2969 (3) Å	Cell parameters from 32724 reflections
b = 12.5314 (4) Å	µ = 0.13 mm⁻¹
c = 6.1815 (2) Å	T = 295 K
β = 106.444 (2)°	Block, blue
V = 690.70 (4) Å³	1.4 × 1.4 × 1.4 mm

Data collection top

TOPAZ Single Crystal Diffractometer	8212 measured reflections
Radiation source: spallation neutron source, SNS BL12	6166 independent reflections
Not applicable to TOF Laue technique monochromator	5081 reflections with > 3σ(I)
time–of–flight Laue scans	h = −17→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 0.936 + 0.348 * lambda [cm^-1] The value of 1.284(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −24→22
T_min = 0.767, T_max = 0.882	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.085	(Δ/σ)_max < 0.001
wR(F²) = 0.084	Δρ_max = 0.13E-12 cm Å^-3 e Å⁻³
S = 1.54	Δρ_min = −0.14E−12 cm Å⁻³ e Å⁻³
5081 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
195 parameters	Extinction coefficient: 4.5E-05 (1)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.01693
S2	0.39546 (13)	0.14135 (10)	0.74274 (19)	0.02026
O3	0.39662 (9)	0.23557 (6)	0.60093 (12)	0.03502
O4	0.53509 (8)	0.08223 (7)	0.77334 (14)	0.03976
O5	0.26917 (7)	0.07220 (5)	0.62496 (11)	0.02692
O6	0.37698 (8)	0.17448 (6)	0.96152 (11)	0.0315
O7	0.15997 (8)	0.10988 (6)	0.16697 (12)	0.03136
O8	0.82300 (8)	0.11197 (6)	0.03977 (12)	0.03188
O9	0.00177 (7)	−0.06567 (5)	0.28814 (10)	0.02218
N10	0.12659 (5)	0.35462 (4)	0.36341 (8)	0.03164
D11	0.04987 (19)	0.34058 (15)	0.2160 (3)	0.06477	0.6908 (18)
D12	0.2118 (2)	0.30224 (14)	0.4060 (3)	0.06416	0.6908 (18)
D13	0.0786 (2)	0.3556 (2)	0.4877 (3)	0.08656	0.6908 (18)
D14	0.1715 (2)	0.42744 (14)	0.3560 (3)	0.07215	0.6908 (18)
D15	0.20558 (15)	0.09323 (11)	0.3256 (2)	0.04072	0.6970 (10)
D16	0.23825 (14)	0.12614 (11)	0.0982 (2)	0.04275	0.6970 (10)
D17	0.72185 (14)	0.09913 (11)	−0.0546 (2)	0.04152	0.6970 (10)
D18	0.84489 (15)	0.18507 (11)	0.0120 (2)	0.04282	0.6970 (10)
D19	−0.09340 (13)	−0.06100 (10)	0.3243 (2)	0.03745	0.6970 (10)
D20	0.03423 (13)	0.86046 (10)	0.31291 (19)	0.03421	0.6970 (10)
H11	0.04986 (19)	0.34058 (15)	0.2159 (3)	0.09159	0.3092 (18)
H12	0.2117 (2)	0.30220 (14)	0.4060 (3)	0.09073	0.3092 (18)
H13	0.0787 (2)	0.3555 (2)	0.4877 (3)	0.12241	0.3092 (18)
H14	0.1715 (2)	0.42747 (14)	0.3560 (3)	0.10203	0.3092 (18)
H15	0.20562 (15)	0.09323 (11)	0.3257 (2)	0.05759	0.3030 (10)
H16	0.23828 (14)	0.12614 (11)	0.0982 (2)	0.06045	0.3030 (10)
H17	0.72185 (14)	0.09912 (11)	−0.0546 (2)	0.05871	0.3030 (10)
H18	0.84490 (15)	0.18508 (11)	0.0121 (2)	0.06055	0.3030 (10)
H19	−0.09336 (13)	−0.06100 (10)	0.3243 (2)	0.05296	0.3030 (10)
H20	0.03425 (13)	0.86046 (10)	0.31292 (19)	0.04837	0.3030 (10)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.01537 (23	0.01947 (27	0.01555 (23	−0.00220 (20	0.00374 (18	0.00079 (19
S2	0.0187 (5)	0.0217 (5)	0.0201 (5)	−0.0043 (4)	0.0050 (4)	−0.0020 (4)
O3	0.0469 (4)	0.02786 (34	0.02949 (32	−0.01183 (31	0.00949 (30	0.00230 (26
O4	0.02158 (31	0.0472 (5)	0.0486 (4)	0.00612 (29	0.00675 (29	−0.00502 (35
O5	0.02221 (27	0.03023 (34	0.02836 (31	−0.00907 (24	0.00720 (23	−0.00422 (24
O6	0.0383 (4)	0.0346 (4)	0.02287 (30	−0.00363 (29	0.01072 (26	−0.00454 (25
O7	0.02735 (32	0.0420 (4)	0.02418 (31	−0.00602 (28	0.00643 (25	0.00309 (27
O8	0.02650 (33	0.0318 (4)	0.0361 (4)	−0.00131 (28	0.00697 (28	0.00536 (29
O9	0.02343 (27	0.02410 (32	0.02049 (25	0.00038 (23	0.00864 (21	0.00289 (21
N10	0.03017 (22	0.03659 (26	0.03040 (22	0.00164 (19	0.01225 (18	0.00328 (18
D11	0.0576 (10)	0.0893 (14)	0.0412 (9)	−0.0208 (9)	0.0038 (7)	−0.0053 (8)
D12	0.0583 (11)	0.0526 (10)	0.0859 (13)	0.0196 (8)	0.0273 (9)	0.0073 (9)
D13	0.0663 (12)	0.153 (2)	0.0539 (10)	0.0439 (13)	0.0392 (9)	0.0348 (12)
D14	0.0833 (13)	0.0442 (10)	0.0759 (13)	−0.0168 (9)	0.0013 (10)	0.0100 (8)
D15	0.0410 (7)	0.0490 (8)	0.0296 (6)	−0.0037 (6)	0.0059 (5)	0.0004 (5)
D16	0.0394 (7)	0.0533 (9)	0.0383 (7)	−0.0119 (6)	0.0156 (5)	0.0005 (6)
D17	0.0294 (6)	0.0516 (8)	0.0429 (7)	−0.0015 (6)	0.0092 (5)	−0.0004 (6)
D18	0.0458 (7)	0.0350 (7)	0.0501 (8)	−0.0009 (6)	0.0177 (6)	0.0018 (6)
D19	0.0359 (6)	0.0447 (7)	0.0373 (6)	0.0062 (5)	0.0194 (5)	0.0061 (5)
D20	0.0381 (6)	0.0314 (6)	0.0338 (6)	0.0057 (5)	0.0114 (5)	0.0044 (5)
H11	0.0814 (15)	0.126 (2)	0.0583 (13)	−0.0294 (13)	0.0054 (11)	−0.0075 (11)
H12	0.0824 (15)	0.0743 (15)	0.1215 (18)	0.0277 (12)	0.0386 (13)	0.0103 (12)
H13	0.0937 (16)	0.217 (3)	0.0762 (14)	0.0621 (18)	0.0555 (13)	0.0492 (16)
H14	0.1178 (19)	0.0624 (14)	0.1074 (18)	−0.0237 (13)	0.0019 (14)	0.0141 (12)
H15	0.0580 (10)	0.0693 (11)	0.0419 (9)	−0.0052 (8)	0.0084 (7)	0.0006 (7)
H16	0.0557 (10)	0.0754 (12)	0.0542 (9)	−0.0169 (9)	0.0220 (8)	0.0007 (8)
H17	0.0416 (9)	0.0730 (12)	0.0606 (10)	−0.0021 (8)	0.0130 (7)	−0.0005 (8)
H18	0.0648 (11)	0.0495 (10)	0.0709 (11)	−0.0013 (8)	0.0250 (9)	0.0026 (8)
H19	0.0508 (9)	0.0632 (11)	0.0528 (9)	0.0088 (8)	0.0275 (7)	0.0087 (7)
H20	0.0539 (9)	0.0444 (9)	0.0479 (8)	0.0081 (7)	0.0161 (7)	0.0062 (7)

Geometric parameters (Å, º) top

Cu1—O7	2.0747 (7)	D13—D12	1.609 (2)
Cu1—O7ⁱ	2.0747 (7)	D13—D14	1.618 (3)
Cu1—O8ⁱⁱ	2.2285 (8)	D13—H11	1.636 (2)
Cu1—O8ⁱⁱⁱ	2.2285 (8)	D13—H12	1.609 (2)
Cu1—O9	1.9579 (6)	D13—H13	0.0006
Cu1—O9ⁱ	1.9579 (6)	D13—H14	1.618 (3)
Cu1—D15	2.6252 (13)	D14—O5^vii	1.8899 (19)
Cu1—D15ⁱ	2.6252 (13)	D14—N10	1.0100 (17)
Cu1—D16	2.6480 (12)	D14—D11	1.631 (3)
Cu1—D16ⁱ	2.6480 (12)	D14—D12	1.622 (3)
Cu1—D18ⁱⁱ	2.7431 (14)	D14—D13	1.618 (3)
Cu1—D18ⁱⁱⁱ	2.7431 (14)	D14—H11	1.631 (3)
Cu1—D19	2.5182 (11)	D14—H12	1.623 (3)
Cu1—D19ⁱ	2.5182 (11)	D14—H13	1.618 (3)
Cu1—D20^iv	2.5596 (12)	D14—H14	0.0005
Cu1—D20^v	2.5596 (12)	D15—Cu1	2.6252 (13)
Cu1—H15	2.6254 (13)	D15—S2	2.7478 (17)
Cu1—H15ⁱ	2.6254 (13)	D15—O5	1.7953 (14)
Cu1—H16	2.6482 (12)	D15—O7	0.9746 (13)
Cu1—H16ⁱ	2.6482 (12)	D15—D16	1.5753 (17)
Cu1—H18ⁱⁱ	2.7431 (14)	D15—H15	0.0003
Cu1—H18ⁱⁱⁱ	2.7431 (14)	D15—H16	1.5754 (17)
Cu1—H19	2.5180 (11)	D16—Cu1	2.6480 (12)
Cu1—H19ⁱ	2.5180 (11)	D16—O6^xiv	1.8332 (14)
Cu1—H20^iv	2.5596 (12)	D16—O7	0.9630 (12)
Cu1—H20^v	2.5596 (12)	D16—D15	1.5753 (17)
S2—O3	1.4724 (14)	D16—H15	1.5753 (17)
S2—O4	1.4598 (14)	D16—H16	0.0003
S2—O5	1.4750 (13)	D17—O4^xiv	1.7735 (15)
S2—O6	1.4704 (13)	D17—O8	0.9695 (14)
S2—D13^vi	2.6281 (18)	D17—D18	1.5399 (19)
S2—D15	2.7478 (17)	D17—H17	0.0003
S2—H13^vi	2.6283 (18)	D17—H18	1.5400 (19)
S2—H15	2.7476 (17)	D18—Cu1^xiii	2.7431 (14)
O3—S2	1.4724 (14)	D18—O6^xvii	1.8267 (16)
O3—O4	2.3893 (11)	D18—O8	0.9642 (14)
O3—O5	2.3911 (9)	D18—D17	1.5399 (19)
O3—O6	2.4121 (9)	D18—H17	1.5399 (19)
O3—O9^vii	2.6832 (10)	D18—H18	0.0002
O3—D12	1.983 (2)	D19—Cu1	2.5182 (11)
O3—D13^vi	2.308 (2)	D19—O5^x	1.7547 (13)
O3—D20^viii	1.7183 (14)	D19—O9	0.9736 (12)
O3—H12	1.983 (2)	D19—D20^iv	1.5584 (17)
O3—H13^vi	2.308 (2)	D19—H19	0.0003
O3—H20^viii	1.7183 (14)	D19—H20^iv	1.5585 (17)
O4—S2	1.4598 (14)	D20—Cu1^xviii	2.5596 (12)
O4—O3	2.3893 (11)	D20—O3^vii	1.7183 (14)
O4—O5	2.3844 (9)	D20—O9^xviii	0.9722 (12)
O4—O6	2.4121 (10)	D20—D19^xviii	1.5584 (17)
O4—O8^ix	2.7422 (11)	D20—H19^xviii	1.5582 (17)
O4—D13^vi	2.072 (2)	D20—H20	0.0002
O4—D17^ix	1.7735 (15)	H11—O6^xv	1.9133 (18)
O4—H13^vi	2.073 (2)	H11—N10	1.0015 (16)
O4—H17^ix	1.7736 (15)	H11—D11	0.0003
O5—S2	1.4750 (13)	H11—D12	1.696 (3)
O5—O3	2.3911 (9)	H11—D13	1.636 (2)
O5—O4	2.3844 (9)	H11—D14	1.631 (3)
O5—O6	2.4073 (9)	H11—H12	1.696 (3)
O5—O7	2.7643 (10)	H11—H13	1.636 (2)
O5—O9^x	2.7214 (8)	H11—H14	1.631 (3)
O5—D14^viii	1.8899 (19)	H12—O3	1.983 (2)
O5—D15	1.7953 (14)	H12—N10	1.0045 (16)
O5—D19^x	1.7547 (13)	H12—D11	1.696 (3)
O5—H14^viii	1.8897 (19)	H12—D12	0.0006
O5—H15	1.7951 (14)	H12—D13	1.609 (2)
O5—H19^x	1.7550 (13)	H12—D14	1.623 (3)
O6—S2	1.4704 (13)	H12—H11	1.696 (3)
O6—O3	2.4121 (9)	H12—H13	1.608 (2)
O6—O4	2.4121 (10)	H12—H14	1.623 (3)
O6—O5	2.4073 (9)	H13—S2^xvi	2.6283 (18)
O6—D11^xi	1.9135 (18)	H13—O3^xvi	2.308 (2)
O6—D16^ix	1.8332 (14)	H13—O4^xvi	2.073 (2)
O6—D18^xii	1.8268 (16)	H13—N10	0.9914 (15)
O6—H11^xi	1.9133 (18)	H13—D11	1.635 (2)
O6—H16^ix	1.8330 (14)	H13—D12	1.608 (2)
O6—H18^xii	1.8267 (16)	H13—D13	0.0006
O7—Cu1	2.0747 (7)	H13—D14	1.618 (3)
O7—O5	2.7643 (10)	H13—H11	1.636 (2)
O7—D15	0.9746 (13)	H13—H12	1.608 (2)
O7—D16	0.9630 (12)	H13—H14	1.618 (3)
O7—H15	0.9748 (13)	H14—O5^vii	1.8897 (19)
O7—H16	0.9632 (12)	H14—N10	1.0102 (17)
O8—Cu1^xiii	2.2285 (8)	H14—D11	1.631 (3)
O8—O4^xiv	2.7422 (11)	H14—D12	1.623 (3)
O8—D17	0.9695 (14)	H14—D13	1.618 (3)
O8—D18	0.9642 (14)	H14—D14	0.0005
O8—H17	0.9694 (14)	H14—H11	1.631 (3)
O8—H18	0.9643 (14)	H14—H12	1.623 (3)
O9—Cu1	1.9579 (6)	H14—H13	1.618 (3)
O9—O3^viii	2.6832 (10)	H15—Cu1	2.6254 (13)
O9—O5^x	2.7214 (8)	H15—S2	2.7476 (17)
O9—D19	0.9736 (12)	H15—O5	1.7951 (14)
O9—D20^iv	0.9722 (12)	H15—O7	0.9748 (13)
O9—H19	0.9733 (12)	H15—D15	0.0003
O9—H20^iv	0.9723 (12)	H15—D16	1.5753 (17)
N10—D11	1.0012 (16)	H15—H16	1.5754 (17)
N10—D12	1.0045 (16)	H16—Cu1	2.6482 (12)
N10—D13	0.9917 (15)	H16—O6^xiv	1.8330 (14)
N10—D14	1.0100 (17)	H16—O7	0.9632 (12)
N10—H11	1.0015 (16)	H16—D15	1.5754 (17)
N10—H12	1.0045 (16)	H16—D16	0.0003
N10—H13	0.9914 (15)	H16—H15	1.5754 (17)
N10—H14	1.0102 (17)	H17—O4^xiv	1.7736 (15)
D11—O6^xv	1.9135 (18)	H17—O8	0.9694 (14)
D11—N10	1.0012 (16)	H17—D17	0.0003
D11—D12	1.696 (3)	H17—D18	1.5399 (19)
D11—D13	1.635 (2)	H17—H18	1.5400 (19)
D11—D14	1.631 (3)	H18—Cu1^xiii	2.7431 (14)
D11—H11	0.0003	H18—O6^xvii	1.8267 (16)
D11—H12	1.696 (3)	H18—O8	0.9643 (14)
D11—H13	1.635 (2)	H18—D17	1.5400 (19)
D11—H14	1.631 (3)	H18—D18	0.0002
D12—O3	1.983 (2)	H18—H17	1.5400 (19)
D12—N10	1.0045 (16)	H19—Cu1	2.5180 (11)
D12—D11	1.696 (3)	H19—O5^x	1.7550 (13)
D12—D13	1.609 (2)	H19—O9	0.9733 (12)
D12—D14	1.622 (3)	H19—D19	0.0003
D12—H11	1.696 (3)	H19—D20^iv	1.5582 (17)
D12—H12	0.0006	H19—H20^iv	1.5583 (17)
D12—H13	1.608 (2)	H20—Cu1^xviii	2.5596 (12)
D12—H14	1.623 (3)	H20—O3^vii	1.7183 (14)
D13—S2^xvi	2.6281 (18)	H20—O9^xviii	0.9723 (12)
D13—O3^xvi	2.308 (2)	H20—D19^xviii	1.5585 (17)
D13—O4^xvi	2.072 (2)	H20—D20	0.0002
D13—N10	0.9917 (15)	H20—H19^xviii	1.5583 (17)
D13—D11	1.635 (2)

D15—O7—D16	108.78 (13)	D11—N10—H13	110.29 (16)
D15—O7—H15	0.0	D11—N10—H14	108.33 (16)
D15—O7—H16	108.77 (13)	D12—N10—D13	107.37 (15)
D16—O7—H15	108.77 (13)	D12—N10—D14	107.28 (17)
D16—O7—H16	0.0	D12—N10—H11	115.43 (16)
H15—O7—H16	108.76 (13)	D12—N10—H12	0.0
D17—O8—D18	105.57 (14)	D12—N10—H13	107.35 (15)
D17—O8—H17	0.0	D12—N10—H14	107.30 (17)
D17—O8—H18	105.58 (14)	D13—N10—D14	107.9 (2)
D18—O8—H17	105.57 (14)	D13—N10—H11	110.30 (16)
D18—O8—H18	0.0	D13—N10—H12	107.37 (15)
H17—O8—H18	105.58 (14)	D13—N10—H13	0.0
D19—O9—D20^iv	106.43 (12)	D13—N10—H14	107.8 (2)
D19—O9—H19	0.0	D14—N10—H11	108.33 (16)
D19—O9—H20^iv	106.44 (12)	D14—N10—H12	107.31 (17)
D20^iv—O9—H19	106.43 (12)	D14—N10—H13	107.9 (2)
D20^iv—O9—H20^iv	0.0	D14—N10—H14	0.0
H19—O9—H20^iv	106.44 (12)	H11—N10—H12	115.40 (16)
D11—N10—D12	115.44 (16)	H11—N10—H13	110.30 (16)
D11—N10—D13	110.29 (16)	H11—N10—H14	108.33 (16)
D11—N10—D14	108.33 (16)	H12—N10—H13	107.35 (15)
D11—N10—H11	0.0	H12—N10—H14	107.33 (17)
D11—N10—H12	115.41 (16)	H13—N10—H14	107.9 (2)

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x, y−1, z; (v) −x, −y+1, −z; (vi) x+1/2, −y+1/2, z; (vii) −x+1/2, y+1/2, −z+1; (viii) −x+1/2, y−1/2, −z+1; (ix) x, y, z+1; (x) −x, −y, −z+1; (xi) x+1/2, −y+1/2, z+1; (xii) x−1/2, −y+1/2, z+1; (xiii) x+1, y, z; (xiv) x, y, z−1; (xv) x−1/2, −y+1/2, z−1; (xvi) x−1/2, −y+1/2, z; (xvii) x+1/2, −y+1/2, z−1; (xviii) x, y+1, z.

(CuTS_78D_295K) perdeuterated diammonium hexaaquacopper(II) bis(sulfate) top

Crystal data top

(NH_1.15D_2.85⁺)₂·CuH_3.16D_8.84O₆²⁺·(SO₄²⁻)₂	Z = 2
M_r = 414.45	F(000) = 191
Monoclinic, P2₁/a	D_x = 1.949 Mg m⁻³
Hall symbol: -P 2yab	Neutron radiation, λ = 0.4-3.4 Å
a = 9.3067 (3) Å	Cell parameters from 23735 reflections
b = 12.5152 (4) Å	µ = 0.12 mm⁻¹
c = 6.1802 (2) Å	T = 295 K
β = 106.358 (2)°	Block, blue
V = 690.70 (4) Å³	2.5 × 2.0 × 1.5 mm

Data collection top

TOPAZ Single Crystal Diffractometer	6149 measured reflections
Radiation source: spallation neutron source, SNS BL12	4566 independent reflections
Not applicable to TOF Laue technique monochromator	3784 reflections with > 3σ(I)
time–of–flight Laue scans	h = −17→18
Absorption correction: analytical The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 0.904 + 0.302 * lambda [cm^-1] The value of 1.206(cm^-1)given in _exptl_absorpt_coefficient_mu is the value at 1 Å	k = −24→24
T_min = 0.720, T_max = 0.846	l = −12→12

Refinement top

Refinement on F²	All H-atom parameters refined
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F² > 2σ(F²)] = 0.091	(Δ/σ)_max < 0.001
wR(F²) = 0.091	Δρ_max = 0.13E-12 cm Å^-3 e Å⁻³
S = 1.54	Δρ_min = −0.13E−12 cm Å⁻³ e Å⁻³
3784 reflections	Extinction correction: B-C Secondary type 1 Lorenzian
195 parameters	Extinction coefficient: 1.1E-04 (3)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	0.0	0.0	0.0	0.01715
S2	0.39544 (15)	0.14113 (11)	0.7422 (2)	0.01998
O3	0.39691 (11)	0.23568 (7)	0.60131 (15)	0.0351
O4	0.53502 (10)	0.08221 (8)	0.77275 (18)	0.03951
O5	0.26901 (9)	0.07210 (6)	0.62491 (14)	0.02704
O6	0.37688 (10)	0.17454 (7)	0.96152 (14)	0.03173
O7	0.16015 (10)	0.10967 (7)	0.16683 (15)	0.0321
O8	0.82286 (10)	0.11212 (7)	0.03993 (15)	0.03196
O9	0.00177 (8)	−0.06560 (6)	0.28831 (13)	0.02246
N10	0.12638 (6)	0.35451 (5)	0.36341 (10)	0.03166
D11	0.0491 (2)	0.34084 (19)	0.2151 (3)	0.06327	0.7119 (24)
D12	0.2116 (2)	0.30162 (15)	0.4068 (4)	0.06201	0.7119 (24)
D13	0.0794 (2)	0.3559 (3)	0.4886 (4)	0.0847	0.7119 (24)
D14	0.1712 (3)	0.42759 (15)	0.3569 (4)	0.06968	0.7119 (24)
D15	0.20509 (16)	0.09327 (12)	0.3246 (2)	0.03989	0.7368 (14)
D16	0.23829 (17)	0.12613 (12)	0.0974 (3)	0.04288	0.7368 (14)
D17	0.72191 (16)	0.09945 (12)	−0.0544 (3)	0.04171	0.7368 (14)
D18	0.84455 (17)	0.18514 (11)	0.0118 (3)	0.0419	0.7368 (14)
D19	−0.09365 (15)	−0.06147 (10)	0.3237 (2)	0.03721	0.7368 (14)
D20	0.03424 (15)	0.86025 (10)	0.3128 (2)	0.03463	0.7368 (14)
H11	0.0491 (2)	0.34084 (19)	0.2151 (3)	0.08948	0.2881 (24)
H12	0.2116 (2)	0.30158 (15)	0.4068 (4)	0.08769	0.2881 (24)
H13	0.0795 (2)	0.3559 (3)	0.4885 (4)	0.11978	0.2881 (24)
H14	0.1712 (3)	0.42761 (15)	0.3570 (4)	0.09853	0.2881 (24)
H15	0.20513 (16)	0.09327 (12)	0.3246 (2)	0.05642	0.2632 (14)
H16	0.23832 (17)	0.12613 (12)	0.0974 (3)	0.06064	0.2632 (14)
H17	0.72191 (16)	0.09945 (12)	−0.0544 (3)	0.05899	0.2632 (14)
H18	0.84456 (17)	0.18515 (11)	0.0119 (3)	0.05925	0.2632 (14)
H19	−0.09362 (15)	−0.06146 (10)	0.3237 (2)	0.05262	0.2632 (14)
H20	0.03426 (15)	0.86025 (10)	0.3128 (2)	0.04898	0.2632 (14)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.01606 (28	0.01831 (29	0.01706 (29	−0.00254 (24	0.00463 (24	0.00090 (23
S2	0.0175 (5)	0.0213 (6)	0.0205 (6)	−0.0021 (5)	0.0043 (5)	−0.0001 (5)
O3	0.0475 (5)	0.0273 (4)	0.0298 (4)	−0.0107 (4)	0.0096 (4)	0.00337 (31
O4	0.0223 (4)	0.0462 (5)	0.0481 (6)	0.0055 (4)	0.0067 (4)	−0.0042 (4)
O5	0.02290 (34	0.0297 (4)	0.0283 (4)	−0.00862 (28	0.00680 (30	−0.00397 (28
O6	0.0393 (5)	0.0342 (4)	0.0231 (4)	−0.00459 (34	0.01117 (35	−0.00471 (30
O7	0.0290 (4)	0.0424 (5)	0.0242 (4)	−0.00605 (34	0.00641 (34	0.00309 (33
O8	0.0271 (4)	0.0321 (4)	0.0351 (4)	−0.00171 (33	0.0062 (4)	0.00538 (34
O9	0.02465 (34	0.02357 (34	0.02073 (31	0.00043 (27	0.00899 (28	0.00281 (25
N10	0.03071 (27	0.03541 (29	0.03100 (28	0.00116 (23	0.01218 (23	0.00260 (21
D11	0.0545 (12)	0.0870 (15)	0.0415 (10)	−0.0249 (11)	0.0025 (9)	−0.0059 (9)
D12	0.0547 (12)	0.0504 (11)	0.0842 (15)	0.0187 (9)	0.0250 (11)	0.0067 (9)
D13	0.0636 (13)	0.155 (2)	0.0476 (12)	0.0407 (15)	0.0357 (11)	0.0313 (13)
D14	0.0815 (16)	0.0432 (10)	0.0718 (14)	−0.0122 (10)	0.0011 (12)	0.0070 (9)
D15	0.0407 (7)	0.0475 (8)	0.0293 (6)	−0.0032 (6)	0.0061 (6)	0.0008 (6)
D16	0.0419 (8)	0.0503 (8)	0.0394 (7)	−0.0105 (6)	0.0161 (6)	0.0007 (6)
D17	0.0308 (7)	0.0498 (8)	0.0450 (8)	−0.0010 (6)	0.0114 (6)	0.0001 (6)
D18	0.0435 (8)	0.0356 (7)	0.0488 (8)	−0.0021 (6)	0.0165 (7)	0.0014 (6)
D19	0.0373 (7)	0.0422 (7)	0.0376 (7)	0.0062 (6)	0.0194 (6)	0.0058 (5)
D20	0.0388 (7)	0.0315 (6)	0.0347 (7)	0.0047 (5)	0.0122 (6)	0.0036 (5)
H11	0.0771 (16)	0.123 (2)	0.0587 (14)	−0.0353 (15)	0.0035 (13)	−0.0084 (13)
H12	0.0774 (17)	0.0712 (15)	0.119 (2)	0.0265 (13)	0.0354 (15)	0.0095 (13)
H13	0.0899 (18)	0.219 (3)	0.0673 (16)	0.058 (2)	0.0504 (15)	0.0443 (18)
H14	0.115 (2)	0.0611 (15)	0.102 (2)	−0.0173 (14)	0.0015 (17)	0.0099 (13)
H15	0.0575 (11)	0.0671 (11)	0.0414 (9)	−0.0046 (9)	0.0086 (8)	0.0012 (8)
H16	0.0592 (11)	0.0711 (12)	0.0557 (10)	−0.0148 (9)	0.0228 (9)	0.0011 (9)
H17	0.0435 (10)	0.0704 (12)	0.0637 (11)	−0.0015 (9)	0.0161 (9)	0.0001 (9)
H18	0.0614 (11)	0.0503 (10)	0.0690 (12)	−0.0029 (8)	0.0233 (10)	0.0020 (8)
H19	0.0527 (10)	0.0596 (10)	0.0531 (10)	0.0088 (8)	0.0274 (9)	0.0082 (8)
H20	0.0549 (10)	0.0446 (9)	0.0491 (9)	0.0067 (8)	0.0173 (8)	0.0051 (7)

Geometric parameters (Å, º) top

Cu1—O7	2.0744 (9)	D13—D12	1.606 (3)
Cu1—O7ⁱ	2.0744 (9)	D13—D14	1.608 (3)
Cu1—O8ⁱⁱ	2.2309 (9)	D13—H11	1.644 (3)
Cu1—O8ⁱⁱⁱ	2.2309 (9)	D13—H12	1.606 (3)
Cu1—O9	1.9577 (7)	D13—H13	0.0006
Cu1—O9ⁱ	1.9577 (7)	D13—H14	1.608 (3)
Cu1—D15	2.6217 (14)	D14—O5^vii	1.886 (2)
Cu1—D15ⁱ	2.6217 (14)	D14—N10	1.0106 (19)
Cu1—D16	2.6496 (14)	D14—D11	1.636 (3)
Cu1—D16ⁱ	2.6496 (14)	D14—D12	1.630 (3)
Cu1—D18ⁱⁱ	2.7435 (14)	D14—D13	1.608 (3)
Cu1—D18ⁱⁱⁱ	2.7435 (14)	D14—H11	1.636 (3)
Cu1—D19	2.5172 (12)	D14—H12	1.630 (3)
Cu1—D19ⁱ	2.5172 (12)	D14—H13	1.608 (3)
Cu1—D20^iv	2.5594 (13)	D14—H14	0.0005
Cu1—D20^v	2.5594 (13)	D15—Cu1	2.6217 (14)
Cu1—H15	2.6219 (14)	D15—O5	1.8020 (16)
Cu1—H15ⁱ	2.6219 (14)	D15—O7	0.9684 (16)
Cu1—H16	2.6498 (14)	D15—D16	1.575 (2)
Cu1—H16ⁱ	2.6498 (14)	D15—H15	0.0003
Cu1—H18ⁱⁱ	2.7435 (14)	D15—H16	1.575 (2)
Cu1—H18ⁱⁱⁱ	2.7435 (14)	D16—Cu1	2.6496 (14)
Cu1—H19	2.5170 (12)	D16—O6^xiv	1.8291 (16)
Cu1—H19ⁱ	2.5170 (12)	D16—O7	0.9650 (15)
Cu1—H20^iv	2.5594 (13)	D16—D15	1.575 (2)
Cu1—H20^v	2.5594 (13)	D16—H15	1.575 (2)
S2—O3	1.4714 (16)	D16—H16	0.0003
S2—O4	1.4590 (17)	D17—O4^xiv	1.7795 (18)
S2—O5	1.4750 (16)	D17—O8	0.9691 (16)
S2—O6	1.4745 (16)	D17—D18	1.535 (2)
S2—D13^vi	2.627 (2)	D17—H17	0.0003
S2—H13^vi	2.628 (2)	D17—H18	1.536 (2)
O3—S2	1.4714 (16)	D18—Cu1^xiii	2.7435 (14)
O3—O4	2.3867 (14)	D18—O6^xvii	1.8231 (17)
O3—O5	2.3931 (11)	D18—O8	0.9622 (15)
O3—O6	2.4104 (12)	D18—D17	1.535 (2)
O3—O9^vii	2.6791 (11)	D18—H17	1.535 (2)
O3—D12	1.983 (2)	D18—H18	0.0002
O3—D13^vi	2.313 (3)	D19—Cu1	2.5172 (12)
O3—D20^viii	1.7122 (16)	D19—O5^x	1.7532 (15)
O3—H12	1.983 (2)	D19—O9	0.9740 (14)
O3—H13^vi	2.313 (3)	D19—D20^iv	1.5577 (18)
O3—H20^viii	1.7121 (16)	D19—H19	0.0003
O4—S2	1.4590 (17)	D19—H20^iv	1.5578 (18)
O4—O3	2.3867 (14)	D20—Cu1^xviii	2.5594 (13)
O4—O5	2.3887 (12)	D20—O3^vii	1.7122 (16)
O4—O6	2.4145 (12)	D20—O9^xviii	0.9744 (14)
O4—O8^ix	2.7480 (13)	D20—D19^xviii	1.5577 (18)
O4—D13^vi	2.065 (3)	D20—H19^xviii	1.5574 (18)
O4—D17^ix	1.7795 (18)	D20—H20	0.0002
O4—H13^vi	2.065 (3)	H11—O6^xv	1.910 (2)
O4—H17^ix	1.7795 (18)	H11—N10	1.0077 (19)
O5—S2	1.4750 (16)	H11—D11	0.0003
O5—O3	2.3931 (11)	H11—D12	1.710 (3)
O5—O4	2.3887 (12)	H11—D13	1.644 (3)
O5—O6	2.4089 (11)	H11—D14	1.636 (3)
O5—O7	2.7652 (12)	H11—H12	1.709 (3)
O5—O9^x	2.7214 (10)	H11—H13	1.644 (3)
O5—D14^viii	1.886 (2)	H11—H14	1.636 (3)
O5—D15	1.8020 (16)	H12—O3	1.983 (2)
O5—D19^x	1.7532 (15)	H12—N10	1.0098 (18)
O5—H14^viii	1.886 (2)	H12—D11	1.709 (3)
O5—H15	1.8018 (16)	H12—D12	0.0006
O5—H19^x	1.7535 (15)	H12—D13	1.606 (3)
O6—S2	1.4745 (16)	H12—D14	1.630 (3)
O6—O3	2.4104 (12)	H12—H11	1.709 (3)
O6—O4	2.4145 (12)	H12—H13	1.606 (3)
O6—O5	2.4089 (11)	H12—H14	1.631 (3)
O6—D11^xi	1.910 (2)	H13—S2^xvi	2.628 (2)
O6—D16^ix	1.8291 (16)	H13—O3^xvi	2.313 (3)
O6—D18^xii	1.8231 (17)	H13—O4^xvi	2.065 (3)
O6—H11^xi	1.910 (2)	H13—N10	0.9895 (18)
O6—H16^ix	1.8289 (16)	H13—D11	1.644 (3)
O6—H18^xii	1.8231 (17)	H13—D12	1.606 (3)
O7—Cu1	2.0744 (9)	H13—D13	0.0006
O7—O5	2.7652 (12)	H13—D14	1.608 (3)
O7—D15	0.9684 (16)	H13—H11	1.644 (3)
O7—D16	0.9650 (15)	H13—H12	1.606 (3)
O7—H15	0.9686 (16)	H13—H14	1.608 (3)
O7—H16	0.9652 (15)	H14—O5^vii	1.886 (2)
O8—Cu1^xiii	2.2309 (9)	H14—N10	1.0108 (19)
O8—O4^xiv	2.7480 (13)	H14—D11	1.636 (3)
O8—D17	0.9691 (16)	H14—D12	1.630 (3)
O8—D18	0.9622 (15)	H14—D13	1.608 (3)
O8—H17	0.9690 (16)	H14—D14	0.0005
O8—H18	0.9622 (15)	H14—H11	1.636 (3)
O9—Cu1	1.9577 (7)	H14—H12	1.631 (3)
O9—O3^viii	2.6791 (11)	H14—H13	1.608 (3)
O9—O5^x	2.7214 (10)	H15—Cu1	2.6219 (14)
O9—D19	0.9740 (14)	H15—O5	1.8018 (16)
O9—D20^iv	0.9744 (14)	H15—O7	0.9686 (16)
O9—H19	0.9737 (14)	H15—D15	0.0003
O9—H20^iv	0.9745 (14)	H15—D16	1.575 (2)
N10—D11	1.0075 (19)	H15—H16	1.575 (2)
N10—D12	1.0098 (18)	H16—Cu1	2.6498 (14)
N10—D13	0.9898 (18)	H16—O6^xiv	1.8289 (16)
N10—D14	1.0106 (19)	H16—O7	0.9652 (15)
N10—H11	1.0077 (19)	H16—D15	1.575 (2)
N10—H12	1.0098 (18)	H16—D16	0.0003
N10—H13	0.9895 (18)	H16—H15	1.575 (2)
N10—H14	1.0108 (19)	H17—O4^xiv	1.7795 (18)
D11—O6^xv	1.910 (2)	H17—O8	0.9690 (16)
D11—N10	1.0075 (19)	H17—D17	0.0003
D11—D12	1.710 (3)	H17—D18	1.535 (2)
D11—D13	1.644 (3)	H17—H18	1.536 (2)
D11—D14	1.636 (3)	H18—Cu1^xiii	2.7435 (14)
D11—H11	0.0003	H18—O6^xvii	1.8231 (17)
D11—H12	1.709 (3)	H18—O8	0.9622 (15)
D11—H13	1.644 (3)	H18—D17	1.536 (2)
D11—H14	1.636 (3)	H18—D18	0.0002
D12—O3	1.983 (2)	H18—H17	1.536 (2)
D12—N10	1.0098 (18)	H19—Cu1	2.5170 (12)
D12—D11	1.710 (3)	H19—O5^x	1.7535 (15)
D12—D13	1.606 (3)	H19—O9	0.9737 (14)
D12—D14	1.630 (3)	H19—D19	0.0003
D12—H11	1.710 (3)	H19—D20^iv	1.5574 (18)
D12—H12	0.0006	H19—H20^iv	1.5576 (18)
D12—H13	1.606 (3)	H20—Cu1^xviii	2.5594 (13)
D12—H14	1.630 (3)	H20—O3^vii	1.7121 (16)
D13—S2^xvi	2.627 (2)	H20—O9^xviii	0.9745 (14)
D13—O3^xvi	2.313 (3)	H20—D19^xviii	1.5578 (18)
D13—O4^xvi	2.065 (3)	H20—D20	0.0002
D13—N10	0.9898 (18)	H20—H19^xviii	1.5576 (18)
D13—D11	1.644 (3)

D15—O7—D16	109.09 (16)	D11—N10—H13	110.8 (2)
D15—O7—H15	0.0	D11—N10—H14	108.32 (19)
D15—O7—H16	109.08 (16)	D12—N10—D13	106.89 (18)
D16—O7—H15	109.07 (16)	D12—N10—D14	107.56 (19)
D16—O7—H16	0.0	D12—N10—H11	115.86 (19)
H15—O7—H16	109.06 (16)	D12—N10—H12	0.0
D17—O8—D18	105.31 (16)	D12—N10—H13	106.87 (18)
D17—O8—H17	0.0	D12—N10—H14	107.58 (19)
D17—O8—H18	105.32 (16)	D13—N10—D14	107.0 (3)
D18—O8—H17	105.32 (16)	D13—N10—H11	110.8 (2)
D18—O8—H18	0.0	D13—N10—H12	106.89 (18)
H17—O8—H18	105.32 (16)	D13—N10—H13	0.0
D19—O9—D20^iv	106.16 (13)	D13—N10—H14	107.0 (3)
D19—O9—H19	0.0	D14—N10—H11	108.32 (19)
D19—O9—H20^iv	106.17 (13)	D14—N10—H12	107.59 (19)
D20^iv—O9—H19	106.16 (13)	D14—N10—H13	107.1 (3)
D20^iv—O9—H20^iv	0.0	D14—N10—H14	0.0
H19—O9—H20^iv	106.17 (13)	H11—N10—H12	115.83 (19)
D11—N10—D12	115.87 (19)	H11—N10—H13	110.8 (2)
D11—N10—D13	110.8 (2)	H11—N10—H14	108.32 (19)
D11—N10—D14	108.32 (19)	H12—N10—H13	106.87 (18)
D11—N10—H11	0.0	H12—N10—H14	107.61 (19)
D11—N10—H12	115.84 (19)	H13—N10—H14	107.0 (3)

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x, y−1, z; (v) −x, −y+1, −z; (vi) x+1/2, −y+1/2, z; (vii) −x+1/2, y+1/2, −z+1; (viii) −x+1/2, y−1/2, −z+1; (ix) x, y, z+1; (x) −x, −y, −z+1; (xi) x+1/2, −y+1/2, z+1; (xii) x−1/2, −y+1/2, z+1; (xiii) x+1, y, z; (xiv) x, y, z−1; (xv) x−1/2, −y+1/2, z−1; (xvi) x−1/2, −y+1/2, z; (xvii) x+1/2, −y+1/2, z−1; (xviii) x, y+1, z.

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Neutron and X-ray investigations of the Jahn-Teller switch in partially deuterated ammonium copper Tutton salt, (NH4)2[Cu(H2O)6](SO4)2

Supporting information

Neutron and X-ray investigations of the Jahn-Teller switch in partially deuterated ammonium copper Tutton salt, (NH₄)₂[Cu(H₂O)₆](SO₄)₂