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The crystal structure of Cu2(OH)3Cl has been determined using two natural samples with almost ideal stoichiometry. While one of the samples exhibits a twinned clinoatacamite structure, the other sample is characterized by the appearance of additional weak diffraction maxima at half integer positions of h and k. Structure refinement was carried out with the space group P\bar 1. The relationship between the triclinic phase, clinoatacamite, paratacamite and the herbertsmithite structure is discussed in terms of symmetry as a function of Cu concentration.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768109013901/hw5003sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768109013901/hw5003Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768109013901/hw5003IIsup3.hkl
Contains datablock II

Computing details top

For both compounds, program(s) used to refine structure: Jana2000 (Petricek, Dusek & Palatinus, 2000); software used to prepare material for publication: Jana2000 (Petricek, Dusek & Palatinus, 2000).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
(I) top
Crystal data top
H3ClCu2O3Z = 8
Mr = 213.6F(000) = 816
Triclinic, P1Dx = 3.722 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.1646 (9) ÅCell parameters from 47586 reflections
b = 9.2029 (8) Åθ = 2–35°
c = 9.2102 (8) ŵ = 11.69 mm1
α = 95.858 (6)°T = 294 K
β = 96.290 (7)°Tabular, green
γ = 96.507 (2)°0.19 × 0.12 × 0.03 mm
V = 761.97 (12) Å3
Data collection top
Nonius KappaCCD
diffractometer
6622 independent reflections
Radiation source: fine-focus sealed X-ray tube4581 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.045
φ scans, and ω scans with κ offsetsθmax = 35°, θmin = 2.2°
Absorption correction: gaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
h = 1414
Tmin = 0.148, Tmax = 0.708k = 1414
47586 measured reflectionsl = 1414
Refinement top
Refinement on F21 constraint
R[F2 > 2σ(F2)] = 0.041H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.191Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.01I2)
S = 1.33(Δ/σ)max = 0.002
6622 reflectionsΔρmax = 0.80 e Å3
262 parametersΔρmin = 1.49 e Å3
24 restraints
Crystal data top
H3ClCu2O3γ = 96.507 (2)°
Mr = 213.6V = 761.97 (12) Å3
Triclinic, P1Z = 8
a = 9.1646 (9) ÅMo Kα radiation
b = 9.2029 (8) ŵ = 11.69 mm1
c = 9.2102 (8) ÅT = 294 K
α = 95.858 (6)°0.19 × 0.12 × 0.03 mm
β = 96.290 (7)°
Data collection top
Nonius KappaCCD
diffractometer
6622 independent reflections
Absorption correction: gaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
4581 reflections with I > 3σ(I)
Tmin = 0.148, Tmax = 0.708Rint = 0.045
47586 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04124 restraints
wR(F2) = 0.191H atoms treated by a mixture of independent and constrained refinement
S = 1.33Δρmax = 0.80 e Å3
6622 reflectionsΔρmin = 1.49 e Å3
262 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu1a0.50.50.50.0106 (3)
Cu2a0.5000.0157 (4)
Cu2b000.50.0109 (3)
Cu2c00.500.0139 (4)
Cu3a0.74935 (8)0.24039 (8)1.00270 (8)0.0141 (3)
Cu3b0.25112 (13)0.00186 (9)0.73928 (8)0.0131 (2)
Cu3c1.00059 (9)0.75035 (15)0.24784 (8)0.0132 (3)
Cu4a0.49964 (9)0.24961 (15)0.25234 (9)0.0129 (3)
Cu4b0.24664 (8)0.26012 (8)0.49839 (6)0.0142 (3)
Cu4c0.25123 (12)0.50173 (9)0.23909 (8)0.0133 (2)
Cl1a0.19369 (17)0.19294 (19)0.19482 (18)0.0178 (5)
Cl2a0.80723 (17)0.30762 (19)0.3036 (2)0.0181 (5)
Cl2b0.30698 (16)0.30354 (18)0.80826 (17)0.0170 (5)
Cl2c0.30599 (16)0.80371 (18)0.30886 (19)0.0170 (5)
O1a0.5493 (5)0.0500 (6)0.2625 (5)0.0176 (13)
O1b0.0450 (6)0.2530 (7)0.5510 (5)0.0193 (14)
O1c0.2277 (5)0.5463 (6)0.0337 (5)0.0203 (14)
O2a0.9511 (6)0.2456 (7)0.9534 (6)0.0213 (14)
O2b0.2778 (5)0.9716 (5)0.9505 (5)0.0125 (11)
O2c0.9614 (5)0.9606 (6)0.2782 (6)0.0166 (13)
O3a0.5387 (6)0.2200 (6)0.0402 (6)0.0166 (13)
O3b0.2221 (5)0.0445 (5)0.5317 (5)0.0162 (12)
O3c0.0393 (5)0.5395 (6)0.2168 (5)0.0119 (11)
O4a0.4536 (5)0.4515 (6)0.2475 (6)0.0192 (14)
O4b0.4577 (6)0.2804 (6)0.4622 (6)0.0162 (13)
O4c0.2722 (5)0.4698 (5)0.4500 (5)0.0125 (11)
H4b0.510 (8)0.214 (7)0.524 (7)0.048 (10)*
H4a0.537 (6)0.531 (7)0.285 (6)0.048 (10)*
H4c0.231 (9)0.549 (6)0.502 (7)0.048 (10)*
H3a0.462 (8)0.266 (9)0.013 (7)0.048 (10)*
H1a0.497 (6)0.021 (6)0.320 (6)0.048 (10)*
H2b0.246 (11)1.069 (6)0.996 (7)0.048 (10)*
H2a1.040 (7)0.211 (10)1.001 (7)0.048 (10)*
H3c0.036 (6)0.458 (6)0.203 (7)0.048 (10)*
H1c0.246 (10)0.440 (4)0.006 (6)0.048 (10)*
H3b0.285 (7)0.012 (6)0.471 (7)0.048 (10)*
H2c1.062 (5)1.020 (7)0.286 (7)0.048 (10)*
H1b0.012 (8)0.315 (6)0.494 (7)0.048 (10)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu1a0.0098 (5)0.0099 (6)0.0137 (6)0.0058 (4)0.0023 (5)0.0032 (4)
Cu2a0.0139 (5)0.0138 (7)0.0176 (7)0.0007 (5)0.0025 (7)0.0005 (5)
Cu2b0.0075 (4)0.0153 (6)0.0117 (6)0.0060 (4)0.0013 (4)0.0048 (4)
Cu2c0.0110 (5)0.0133 (6)0.0146 (7)0.0037 (5)0.0030 (5)0.0015 (4)
Cu3a0.0134 (4)0.0163 (4)0.0145 (5)0.0052 (3)0.0032 (3)0.0055 (3)
Cu3b0.0100 (3)0.0168 (5)0.0123 (3)0.0040 (3)0.0028 (3)0.0028 (3)
Cu3c0.0141 (3)0.0171 (5)0.0096 (4)0.0048 (3)0.0038 (3)0.0021 (2)
Cu4a0.0135 (3)0.0148 (5)0.0111 (5)0.0036 (3)0.0028 (3)0.0018 (2)
Cu4b0.0128 (4)0.0157 (4)0.0171 (5)0.0091 (3)0.0040 (3)0.0062 (3)
Cu4c0.0113 (3)0.0171 (5)0.0119 (3)0.0053 (3)0.0020 (3)0.0038 (3)
Cl1a0.0164 (7)0.0174 (9)0.0188 (9)0.0032 (6)0.0014 (6)0.0010 (5)
Cl2a0.0166 (6)0.0187 (9)0.0187 (10)0.0040 (7)0.0007 (6)0.0017 (5)
Cl2b0.0153 (6)0.0161 (8)0.0191 (9)0.0047 (6)0.0023 (6)0.0021 (5)
Cl2c0.0150 (6)0.0162 (8)0.0195 (9)0.0044 (7)0.0015 (6)0.0018 (5)
O1a0.0124 (18)0.019 (2)0.027 (3)0.0091 (17)0.0129 (17)0.0110 (19)
O1b0.016 (2)0.033 (3)0.0117 (18)0.012 (2)0.0005 (16)0.0102 (18)
O1c0.018 (2)0.019 (2)0.023 (2)0.0064 (17)0.0027 (17)0.0040 (17)
O2a0.019 (2)0.030 (3)0.019 (2)0.005 (2)0.0052 (19)0.0135 (19)
O2b0.0125 (16)0.013 (2)0.0147 (18)0.0060 (14)0.0054 (14)0.0073 (13)
O2c0.0063 (17)0.018 (2)0.027 (2)0.0013 (15)0.0057 (16)0.0022 (18)
O3a0.021 (2)0.016 (2)0.0147 (19)0.0105 (17)0.0007 (16)0.0069 (16)
O3b0.0122 (18)0.014 (2)0.022 (2)0.0008 (15)0.0038 (16)0.0014 (15)
O3c0.0060 (15)0.020 (2)0.0100 (19)0.0021 (15)0.0003 (13)0.0054 (16)
O4a0.0059 (17)0.018 (2)0.035 (3)0.0039 (15)0.0041 (16)0.007 (2)
O4b0.0135 (19)0.021 (2)0.0149 (19)0.0032 (16)0.0009 (16)0.0071 (16)
O4c0.0206 (19)0.0066 (18)0.0125 (17)0.0063 (14)0.0020 (14)0.0063 (12)
Bond lengths (Å) top
Cu1a—Cu4a3.0719 (11)Cl2b—O1b3.142 (5)
Cu1a—Cu4ai3.0719 (11)Cl2b—O1cxiv3.095 (5)
Cu1a—Cu4b3.0148 (7)Cl2b—O2bxvii3.439 (5)
Cu1a—Cu4bi3.0148 (7)Cl2b—O2ci3.227 (5)
Cu1a—Cu4c3.1286 (9)Cl2b—O3axiv3.062 (6)
Cu1a—Cu4ci3.1286 (9)Cl2b—O3b3.269 (5)
Cu1a—O4a2.306 (5)Cl2b—O4ai3.086 (5)
Cu1a—O4ai2.306 (5)Cl2b—H4b3.46 (7)
Cu1a—O4b2.001 (5)Cl2b—H4ai2.26 (6)
Cu1a—O4bi2.001 (5)Cl2b—H3axiv2.13 (7)
Cu1a—O4c2.069 (5)Cl2b—H2bxvii2.94 (6)
Cu1a—O4ci2.069 (5)Cl2b—H2aix3.26 (7)
Cu1a—H4b2.68 (6)Cl2b—H3cxix3.50 (6)
Cu1a—H4bi2.68 (6)Cl2b—H1cxiv2.27 (6)
Cu1a—H4a2.09 (6)Cl2c—O1axx3.091 (5)
Cu1a—H4ai2.09 (6)Cl2c—O1c3.247 (5)
Cu1a—H4c2.55 (8)Cl2c—O2ai3.143 (6)
Cu1a—H4ci2.55 (8)Cl2c—O3bxx3.085 (5)
Cu2a—Cu3aii2.9912 (7)Cl2c—O3c3.223 (5)
Cu2a—Cu3aiii2.9912 (7)Cl2c—O4bi3.074 (6)
Cu2a—Cu3bii3.1283 (9)Cl2c—O4c3.452 (5)
Cu2a—Cu3biii3.1283 (9)Cl2c—H4bi2.18 (7)
Cu2a—Cu4a3.0971 (10)Cl2c—H4a3.47 (6)
Cu2a—Cu4aiv3.0971 (10)Cl2c—H4c3.15 (6)
Cu2a—O1a2.398 (5)Cl2c—H1axx2.23 (5)
Cu2a—O1aiv2.398 (5)Cl2c—H3bxx2.19 (6)
Cu2a—O2bv2.019 (4)Cl2c—H2cix3.16 (6)
Cu2a—O2bi2.019 (4)O1a—O2bi2.660 (7)
Cu2a—O3a2.004 (5)O1a—O3a2.701 (8)
Cu2a—O3aiv2.004 (5)O1a—O3aiv3.498 (7)
Cu2a—H3a2.53 (8)O1a—O3biii2.935 (7)
Cu2a—H3aiv2.53 (8)O1a—O4b2.921 (7)
Cu2a—H1a2.97 (6)O1a—H4b2.79 (6)
Cu2a—H1aiv2.97 (6)O1a—H4biii3.31 (7)
Cu2a—H2bv2.48 (10)O1a—H3a3.46 (8)
Cu2a—H2bi2.48 (10)O1a—H1a0.99 (6)
Cu2b—Cu3b3.0042 (9)O1a—H2bi3.36 (8)
Cu2b—Cu3bvi3.0042 (9)O1a—H3b3.29 (7)
Cu2b—Cu3cvii3.0965 (10)O1a—H3biii2.82 (6)
Cu2b—Cu3ci3.0965 (10)O1b—O2cvii3.445 (7)
Cu2b—Cu4b3.1029 (7)O1b—O2ci2.640 (8)
Cu2b—Cu4bvi3.1029 (7)O1b—O3b2.655 (8)
Cu2b—O1b2.308 (6)O1b—O3bvi3.422 (7)
Cu2b—O1bvi2.308 (6)O1b—O3cxix2.946 (7)
Cu2b—O2cvii2.023 (5)O1b—O4c3.007 (8)
Cu2b—O2ci2.023 (5)O1b—H4c3.15 (6)
Cu2b—O3b2.013 (4)O1b—H4cxix3.31 (7)
Cu2b—O3bvi2.013 (4)O1b—H3cxix3.33 (5)
Cu2b—H3b2.66 (6)O1b—H2cvii3.11 (6)
Cu2b—H3bvi2.66 (6)O1b—H2ci3.17 (6)
Cu2b—H2cvii2.13 (6)O1b—H1b0.98 (7)
Cu2b—H2ci2.13 (6)O1c—O2aviii3.494 (7)
Cu2b—H1b2.92 (6)O1c—O2ai2.660 (9)
Cu2b—H1bvi2.92 (6)O1c—O3ax3.041 (7)
Cu2c—Cu3aviii3.1251 (7)O1c—O3c2.543 (7)
Cu2c—Cu3ai3.1251 (7)O1c—O3cxi3.144 (6)
Cu2c—Cu3cix3.0724 (11)O1c—O4a2.965 (7)
Cu2c—Cu3cx3.0724 (11)O1c—H4a3.48 (6)
Cu2c—Cu4c3.0040 (9)O1c—H3ax3.19 (7)
Cu2c—Cu4cxi3.0040 (9)O1c—H2aviii3.33 (8)
Cu2c—O1c2.064 (5)O1c—H3c3.09 (6)
Cu2c—O1cxi2.064 (5)O1c—H3cxi2.64 (6)
Cu2c—O2aviii2.319 (6)O1c—H1c1.02 (5)
Cu2c—O2ai2.319 (6)O2a—O2bxv3.000 (8)
Cu2c—O3c1.979 (4)O2a—O2cxiii2.948 (8)
Cu2c—O3cxi1.979 (4)O2a—O3cxvi3.404 (7)
Cu2c—H2aviii2.73 (9)O2a—O3ci2.646 (8)
Cu2c—H2ai2.73 (9)O2a—H2bxxi3.32 (9)
Cu2c—H3c2.00 (6)O2a—H2bxv3.34 (6)
Cu2c—H3cxi2.00 (6)O2a—H2a0.99 (7)
Cu2c—H1c2.38 (9)O2a—H3cxvi2.84 (5)
Cu2c—H1cxi2.38 (9)O2a—H3ci3.27 (6)
Cu3a—Cu3bxii3.4204 (11)O2a—H1cxvi3.03 (8)
Cu3a—Cu3cxiii3.4262 (11)O2a—H2cxiii3.10 (6)
Cu3a—Cu4axiv3.4188 (11)O2b—O2cxxii3.033 (7)
Cu3a—Cu4ci3.4162 (11)O2b—O3axxiii3.093 (7)
Cu3a—Cl2axiv2.7563 (19)O2b—O3ai2.572 (8)
Cu3a—Cl2ci2.8378 (18)O2b—H3axxiii2.99 (8)
Cu3a—O1ci2.017 (5)O2b—H3ai3.46 (8)
Cu3a—O2a1.949 (6)O2b—H1ai3.44 (6)
Cu3a—O2bxv2.034 (5)O2b—H2b1.03 (6)
Cu3a—O3axiv1.990 (6)O2b—H2axxiv3.30 (8)
Cu3a—H3axiv2.67 (7)O2b—H2axv3.29 (7)
Cu3a—H2bxv2.85 (5)O2c—O3bxxv3.122 (6)
Cu3a—H2a2.71 (7)O2c—O3bi2.557 (7)
Cu3a—H3cxvi2.97 (5)O2c—H2bxxii2.96 (7)
Cu3a—H1ci2.94 (4)O2c—H2axiii2.87 (7)
Cu3b—Cu3ci3.4252 (16)O2c—H3bxxv3.25 (6)
Cu3b—Cu4aiii3.4315 (16)O2c—H3bi3.43 (7)
Cu3b—Cu4b3.4134 (11)O2c—H2c1.01 (5)
Cu3b—Cl2aiii2.8165 (19)O2c—H1bi3.49 (6)
Cu3b—Cl2b2.7604 (18)O3a—O4a2.944 (8)
Cu3b—O1aiii1.943 (5)O3a—H4a3.46 (6)
Cu3b—O2bxvii1.986 (5)O3a—H3a0.98 (8)
Cu3b—O2ci2.009 (5)O3a—H2bv2.85 (9)
Cu3b—O3b1.986 (5)O3a—H2bi3.49 (8)
Cu3b—H3axiv3.42 (7)O3b—O4b3.051 (7)
Cu3b—H1aiii2.42 (6)O3b—H4b2.92 (7)
Cu3b—H2bxvii2.39 (6)O3b—H1a3.42 (6)
Cu3b—H3b2.51 (7)O3b—H1aiii2.83 (6)
Cu3b—H2ci2.84 (4)O3b—H3b0.99 (6)
Cu3c—Cu4bi3.4297 (10)O3b—H2cvii2.53 (6)
Cu3c—Cu4cxviii3.4223 (16)O3b—H2ci3.28 (5)
Cu3c—Cl2bi2.7874 (16)O3b—H1b3.49 (7)
Cu3c—Cl2cxviii2.7709 (16)O3c—O4c3.027 (6)
Cu3c—O1bi1.946 (5)O3c—H4c2.99 (6)
Cu3c—O2axiii1.955 (6)O3c—H2aviii3.45 (8)
Cu3c—O2c2.005 (6)O3c—H2ai3.29 (8)
Cu3c—O3cxviii2.010 (5)O3c—H3c0.95 (5)
Cu3c—H2axiii2.35 (6)O3c—H1c3.00 (8)
Cu3c—H3cxviii2.66 (5)O3c—H1cxi3.18 (8)
Cu3c—H1cx3.28 (6)O3c—H1b3.48 (6)
Cu3c—H2c2.46 (6)O3c—H1bxix2.90 (6)
Cu3c—H1bi2.51 (6)O4a—O4b2.650 (8)
Cu4a—Cu4b3.4173 (11)O4a—O4bi3.409 (7)
Cu4a—Cu4c3.4316 (16)O4a—O4c2.636 (7)
Cu4a—Cl1a2.7751 (17)O4a—O4ci3.500 (6)
Cu4a—Cl2a2.7875 (17)O4a—H4a1.00 (5)
Cu4a—O1a1.951 (5)O4a—H4c3.39 (7)
Cu4a—O3a2.022 (5)O4a—H4ci3.49 (7)
Cu4a—O4a1.955 (6)O4a—H3a2.81 (7)
Cu4a—O4b2.010 (5)O4a—H1c2.75 (7)
Cu4a—H4b2.55 (7)O4b—O4c2.571 (8)
Cu4a—H4a2.56 (6)O4b—O4ci3.156 (7)
Cu4a—H4ci3.39 (6)O4b—H4b1.01 (7)
Cu4a—H3a2.45 (7)O4b—H4a3.03 (6)
Cu4a—H1a2.62 (5)O4b—H4ai2.75 (6)
Cu4a—H2bv3.30 (7)O4b—H4c3.42 (7)
Cu4b—Cu4c3.4255 (10)O4b—H4ci3.06 (7)
Cu4b—Cl1a2.7779 (17)O4b—H1a3.02 (5)
Cu4b—Cl2b2.8252 (17)O4b—H1aiii3.31 (6)
Cu4b—O1b1.957 (6)O4b—H3b2.97 (6)
Cu4b—O3b2.030 (5)O4c—H4b3.46 (7)
Cu4b—O4b1.990 (5)O4c—H4bi3.31 (6)
Cu4b—O4c2.018 (5)O4c—H4a3.03 (6)
Cu4b—H4b2.49 (7)O4c—H4ai2.85 (6)
Cu4b—H4ai3.01 (5)O4c—H4c0.97 (7)
Cu4b—H4c2.67 (6)O4c—H3c3.41 (6)
Cu4b—H3b2.55 (6)O4c—H1b2.92 (7)
Cu4b—H2cvii3.02 (5)O4c—H1bxix3.31 (7)
Cu4b—H1b2.48 (7)H4b—H4ai2.89 (9)
Cu4c—Cl1a2.8101 (19)H4b—H4ci3.08 (9)
Cu4c—Cl2c2.7635 (18)H4b—H1a2.70 (8)
Cu4c—O1c1.970 (5)H4b—H1aiii2.39 (9)
Cu4c—O3c2.004 (5)H4b—H3b2.72 (8)
Cu4c—O4a1.957 (5)H4b—H3biii2.79 (9)
Cu4c—O4c1.986 (5)H4a—H4ci2.94 (9)
Cu4c—H4a2.59 (6)H4a—H3a3.43 (9)
Cu4c—H4c2.45 (6)H4a—H3ax3.27 (10)
Cu4c—H3c2.60 (6)H4a—H1c3.46 (9)
Cu4c—H1c2.15 (6)H4c—H3c3.45 (8)
Cl1a—O2aviii3.082 (6)H4c—H3cxix3.41 (9)
Cl1a—O2bv3.099 (5)H4c—H1b2.91 (9)
Cl1a—O2cvii3.058 (5)H4c—H1bxix2.48 (10)
Cl1a—O4a3.130 (5)H3a—H2bv2.54 (11)
Cl1a—O4b3.227 (5)H3a—H1c2.69 (11)
Cl1a—O4c3.244 (4)H1a—H1aiii3.30 (8)
Cl1a—H3a3.32 (7)H1a—H3b2.52 (9)
Cl1a—H2bv2.19 (7)H1a—H3biii2.59 (8)
Cl1a—H2aviii2.18 (6)H2b—H2axxiv2.41 (12)
Cl1a—H3c3.39 (6)H2b—H2axv3.47 (10)
Cl1a—H1c3.03 (5)H2b—H1cxxiii3.41 (7)
Cl1a—H3b3.40 (6)H2b—H2cxxvi3.36 (10)
Cl1a—H2cvii2.18 (6)H2a—H3cxvi2.98 (10)
Cl2a—O1a3.115 (5)H2a—H1cxvi2.66 (10)
Cl2a—O1bxviii3.096 (6)H2a—H2cxxvii3.31 (10)
Cl2a—O2bi3.257 (5)H2a—H2cxiii3.20 (9)
Cl2a—O3a3.230 (5)H3c—H1c3.32 (11)
Cl2a—O3cxviii3.067 (5)H3c—H1cxi2.88 (9)
Cl2a—O4ci3.103 (5)H3c—H1b3.10 (9)
Cl2a—H4a3.40 (6)H3c—H1bxix3.27 (8)
Cl2a—H4ci2.20 (6)H3b—H2cvii2.57 (8)
Cl2a—H3cxviii2.22 (6)H2c—H1bxxv3.34 (9)
Cl2a—H1bxviii2.27 (6)H1b—H1bxix3.37 (8)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y, z1; (iii) x+1, y, z+1; (iv) x+1, y, z; (v) x, y1, z1; (vi) x, y, z+1; (vii) x1, y1, z; (viii) x1, y, z1; (ix) x1, y, z; (x) x+1, y+1, z; (xi) x, y+1, z; (xii) x+1, y, z+2; (xiii) x+2, y+1, z+1; (xiv) x, y, z+1; (xv) x+1, y+1, z+2; (xvi) x+1, y, z+1; (xvii) x, y1, z; (xviii) x+1, y, z; (xix) x, y+1, z+1; (xx) x, y+1, z; (xxi) x+1, y1, z; (xxii) x+1, y+2, z+1; (xxiii) x, y+1, z+1; (xxiv) x1, y+1, z; (xxv) x+1, y+1, z; (xxvi) x1, y, z+1; (xxvii) x, y1, z+1.
(II) top
Crystal data top
H3ClCu2O3F(000) = 408
Mr = 213.6Dx = 3.742 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yabcCell parameters from 1685 reflections
a = 6.1226 (3) Åθ = 3.7–35.6°
b = 6.8346 (4) ŵ = 11.76 mm1
c = 9.1841 (6) ÅT = 294 K
β = 99.577 (4)°, green
V = 378.96 (4) Å30.08 × 0.08 × 0.05 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
1672 independent reflections
Radiation source: fine-focus sealed X-ray tube993 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.000
φ scans, and ω scans with κ offsetsθmax = 35.6°, θmin = 3.7°
Absorption correction: multi-scan
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
h = 99
Tmin = 0.350, Tmax = 0.540k = 010
1685 measured reflectionsl = 014
Refinement top
Refinement on F21 constraint
R[F2 > 2σ(F2)] = 0.040H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.122Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.0036I2)
S = 1.08(Δ/σ)max = 0.0002
1672 reflectionsΔρmax = 1.80 e Å3
69 parametersΔρmin = 1.92 e Å3
3 restraints
Crystal data top
H3ClCu2O3V = 378.96 (4) Å3
Mr = 213.6Z = 4
Monoclinic, P21/nMo Kα radiation
a = 6.1226 (3) ŵ = 11.76 mm1
b = 6.8346 (4) ÅT = 294 K
c = 9.1841 (6) Å0.08 × 0.08 × 0.05 mm
β = 99.577 (4)°
Data collection top
Nonius KappaCCD
diffractometer
1672 independent reflections
Absorption correction: multi-scan
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
993 reflections with I > 3σ(I)
Tmin = 0.350, Tmax = 0.540Rint = 0.000
1685 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0403 restraints
wR(F2) = 0.122H atoms treated by a mixture of independent and constrained refinement
S = 1.08Δρmax = 1.80 e Å3
1672 reflectionsΔρmin = 1.92 e Å3
69 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu100.50.50.01311 (16)
Cu20000.01556 (17)
Cu30.25292 (8)0.24557 (5)0.74944 (6)0.01515 (14)
Cl10.11236 (15)0.00140 (13)0.30614 (10)0.0179 (2)
O10.2809 (6)0.3056 (4)0.5432 (3)0.0241 (9)
O20.4157 (5)0.0056 (4)0.7679 (4)0.0230 (9)
O30.2675 (5)0.6845 (4)0.5410 (3)0.0209 (9)
H10.22 (2)0.202 (12)0.473 (10)0.16 (3)*
H30.23 (3)0.793 (12)0.470 (10)0.16 (3)*
H20.580 (5)0.007 (8)0.779 (17)0.16 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0130 (3)0.0139 (3)0.0129 (3)0.0006 (2)0.0033 (2)0.0004 (3)
Cu20.0161 (3)0.0164 (3)0.0156 (3)0.0001 (3)0.0067 (2)0.0003 (3)
Cu30.0181 (2)0.0127 (2)0.0156 (2)0.00081 (14)0.00566 (18)0.00135 (14)
Cl10.0181 (4)0.0187 (4)0.0173 (4)0.0002 (4)0.0039 (3)0.0008 (4)
O10.0350 (16)0.0206 (15)0.0188 (14)0.0132 (14)0.0112 (14)0.0069 (12)
O20.0169 (13)0.0155 (12)0.0401 (18)0.0016 (10)0.0153 (13)0.0019 (13)
O30.0290 (15)0.0164 (14)0.0193 (14)0.0056 (12)0.0099 (14)0.0051 (11)
Geometric parameters (Å, º) top
Cu1—O12.157 (3)Cu3—Cl1ix2.7911 (10)
Cu1—O1i2.157 (3)Cu3—O11.973 (3)
Cu1—O2ii2.108 (3)Cu3—O21.978 (3)
Cu1—O2iii2.108 (3)Cu3—O2ii1.982 (3)
Cu1—O32.052 (3)Cu3—O3x1.993 (3)
Cu1—O3i2.052 (3)Cu3—H12.53 (10)
Cu1—H12.49 (10)Cu3—H3x2.59 (10)
Cu1—H1i2.49 (10)Cu3—H22.63 (4)
Cu1—H32.49 (11)Cu3—H2ii2.63 (4)
Cu1—H3i2.49 (11)Cl1—H12.09 (9)
Cu1—H2ii2.17 (15)Cl1—H3xi2.10 (9)
Cu1—H2iii2.17 (15)Cl1—H2vii2.15 (8)
Cu2—Cl12.7812 (9)O1—O22.983 (4)
Cu2—Cl1iv2.7812 (9)O1—O2ii2.611 (5)
Cu2—O1v1.975 (3)O1—O32.591 (4)
Cu2—O1iii1.975 (3)O1—O3xii2.993 (5)
Cu2—O3v1.984 (3)O1—H10.99 (9)
Cu2—O3iii1.984 (3)O2—O3x2.584 (5)
Cu2—H1v2.64 (11)O2—H21.00 (3)
Cu2—H1iii2.64 (11)O3—H30.99 (9)
Cu2—H3v2.58 (11)H1—H3xi2.80 (11)
Cu2—H3iii2.58 (11)H1—H3i2.9 (2)
Cu2—H2vi3.00 (9)H1—H2iii2.79 (13)
Cu2—H2vii3.00 (9)H3—H2iii2.69 (13)
Cu3—Cl1viii2.7690 (10)
O1—Cu1—O1i180Cu2—Cl1—H1137 (2)
O1—Cu1—O2ii75.48 (11)Cu2—Cl1—H3xi136 (2)
O1—Cu1—O2iii104.52 (11)Cu2—Cl1—H2vii74 (4)
O1—Cu1—O375.95 (12)Cu3viii—Cl1—Cu3iii75.85 (3)
O1—Cu1—O3i104.05 (12)Cu3viii—Cl1—H1133 (4)
O1—Cu1—H123 (2)Cu3viii—Cl1—H3xi84 (4)
O1—Cu1—H1i157 (2)Cu3viii—Cl1—H2vii133 (3)
O1—Cu1—H394 (3)Cu3iii—Cl1—Cu3viii75.85 (3)
O1—Cu1—H3i86 (3)Cu3iii—Cl1—H182 (3)
O1—Cu1—H2ii96.4 (13)Cu3iii—Cl1—H3xi136 (4)
O1—Cu1—H2iii83.6 (13)Cu3iii—Cl1—H2vii129 (2)
O1i—Cu1—O1180H1—Cl1—H3xi84 (3)
O1i—Cu1—O2ii104.52 (11)H1—Cl1—H2vii93 (5)
O1i—Cu1—O2iii75.48 (11)H3xi—Cl1—H2vii93 (5)
O1i—Cu1—O3104.05 (12)Cu1—O1—Cu2xiii95.50 (12)
O1i—Cu1—O3i75.95 (12)Cu1—O1—Cu396.35 (14)
O1i—Cu1—H1157 (2)Cu1—O1—O2133.37 (16)
O1i—Cu1—H1i23 (2)Cu1—O1—O2ii51.41 (10)
O1i—Cu1—H386 (3)Cu1—O1—O350.18 (9)
O1i—Cu1—H3i94 (3)Cu1—O1—O3xii132.91 (14)
O1i—Cu1—H2ii83.6 (13)Cu1—O1—H197 (7)
O1i—Cu1—H2iii96.4 (13)Cu1—O1—H2iii48 (2)
O2ii—Cu1—O2iii180Cu2xiii—O1—Cu3120.20 (14)
O2ii—Cu1—O376.80 (11)Cu2xiii—O1—O2119.98 (14)
O2ii—Cu1—O3i103.20 (11)Cu2xiii—O1—O2ii101.79 (13)
O2ii—Cu1—H192 (2)Cu2xiii—O1—O349.27 (10)
O2ii—Cu1—H1i88 (2)Cu2xiii—O1—H1123 (7)
O2ii—Cu1—H395 (2)Cu2xiii—O1—H2iii73.6 (9)
O2ii—Cu1—H3i85 (2)Cu3—O1—O2ii48.84 (10)
O2ii—Cu1—H2ii26.9 (12)Cu3—O1—O3101.97 (14)
O2ii—Cu1—H2iii153.1 (12)Cu3—O1—O3xii118.96 (14)
O2iii—Cu1—O2ii180Cu3—O1—H1113 (6)
O2iii—Cu1—O3103.20 (11)Cu3—O1—H2iii144.6 (19)
O2iii—Cu1—O3i76.80 (11)O2—O1—O2ii89.87 (13)
O2iii—Cu1—H188 (2)O2—O1—O3136.27 (14)
O2iii—Cu1—H1i92 (2)O2—O1—O3xii91.94 (12)
O2iii—Cu1—H385 (2)O2—O1—H188 (5)
O2iii—Cu1—H3i95 (2)O2—O1—H2iii162.5 (14)
O2iii—Cu1—H2ii153.1 (12)O2ii—O1—O289.87 (13)
O2iii—Cu1—H2iii26.9 (12)O2ii—O1—O359.56 (12)
O3—Cu1—O3i180O2ii—O1—O3xii135.08 (14)
O3—Cu1—H195 (3)O2ii—O1—H1129 (8)
O3—Cu1—H1i85 (3)O2ii—O1—H2iii98 (2)
O3—Cu1—H323 (3)O3—O1—O3xii90.27 (13)
O3—Cu1—H3i157 (3)O3—O1—H1135 (5)
O3—Cu1—H2ii98.0 (13)O3—O1—H2iii60.5 (17)
O3—Cu1—H2iii82.0 (13)O3xii—O1—O390.27 (13)
O3i—Cu1—O3180O3xii—O1—H196 (8)
O3i—Cu1—H185 (3)O3xii—O1—H2iii93.1 (15)
O3i—Cu1—H1i95 (3)H1—O1—H2iii75 (5)
O3i—Cu1—H3157 (3)Cu1x—O2—Cu396.11 (14)
O3i—Cu1—H3i23 (3)Cu1x—O2—Cu3x97.67 (14)
O3i—Cu1—H2ii82.0 (13)Cu1x—O2—O1132.83 (13)
O3i—Cu1—H2iii98.0 (13)Cu1x—O2—O1x53.11 (10)
H1—Cu1—H1i180Cu1x—O2—O3x50.62 (10)
H1—Cu1—H3108 (4)Cu1x—O2—H280 (9)
H1—Cu1—H3i72 (4)Cu3—O2—Cu3x119.32 (15)
H1—Cu1—H2ii107 (3)Cu3—O2—O1x101.82 (15)
H1—Cu1—H2iii73 (3)Cu3—O2—O3x49.66 (10)
H1i—Cu1—H1180Cu3—O2—H2120 (3)
H1i—Cu1—H372 (4)Cu3x—O2—Cu3119.32 (15)
H1i—Cu1—H3i108 (4)Cu3x—O2—O1118.40 (14)
H1i—Cu1—H2ii73 (3)Cu3x—O2—O1x48.54 (10)
H1i—Cu1—H2iii107 (3)Cu3x—O2—O3x101.95 (15)
H3—Cu1—H3i180Cu3x—O2—H2120 (3)
H3—Cu1—H2ii110 (3)O1—O2—O1x135.01 (15)
H3—Cu1—H2iii70 (3)O1—O2—O3x90.58 (12)
H3i—Cu1—H3180O1—O2—H2104 (6)
H3i—Cu1—H2ii70 (3)O1x—O2—O1135.01 (15)
H3i—Cu1—H2iii110 (3)O1x—O2—O3x59.83 (12)
H2ii—Cu1—H2iii180O1x—O2—H2120 (7)
H2iii—Cu1—H2ii180O3x—O2—H2119 (8)
Cl1—Cu2—Cl1iv180Cu1—O3—Cu2xiii98.66 (12)
Cl1—Cu2—O1v97.97 (8)Cu1—O3—Cu3ii97.45 (13)
Cl1—Cu2—O1iii82.03 (8)Cu1—O3—O153.87 (10)
Cl1—Cu2—O3v97.44 (8)Cu1—O3—O1xii135.23 (14)
Cl1—Cu2—O3iii82.56 (8)Cu1—O3—O2ii52.58 (10)
Cl1—Cu2—H1v82 (2)Cu1—O3—H3105 (8)
Cl1—Cu2—H1iii98 (2)Cu1—O3—H2iii51 (2)
Cl1—Cu2—H3v81 (2)Cu2xiii—O3—Cu3ii118.60 (13)
Cl1—Cu2—H3iii99 (2)Cu2xiii—O3—O148.96 (10)
Cl1—Cu2—H2vi136 (3)Cu2xiii—O3—O2ii102.45 (13)
Cl1—Cu2—H2vii44 (3)Cu2xiii—O3—H3116 (8)
Cl1iv—Cu2—Cl1180Cu2xiii—O3—H2iii76.3 (9)
Cl1iv—Cu2—O1v82.03 (8)Cu3ii—O3—O1102.06 (13)
Cl1iv—Cu2—O1iii97.97 (8)Cu3ii—O3—O1xii116.98 (13)
Cl1iv—Cu2—O3v82.56 (8)Cu3ii—O3—O2ii49.14 (9)
Cl1iv—Cu2—O3iii97.44 (8)Cu3ii—O3—H3116 (6)
Cl1iv—Cu2—H1v98 (2)Cu3ii—O3—H2iii148.0 (19)
Cl1iv—Cu2—H1iii82 (2)O1—O3—O1xii89.73 (13)
Cl1iv—Cu2—H3v99 (2)O1—O3—O2ii60.60 (12)
Cl1iv—Cu2—H3iii81 (2)O1—O3—H3139 (5)
Cl1iv—Cu2—H2vi44 (3)O1—O3—H2iii65.0 (16)
Cl1iv—Cu2—H2vii136 (3)O1xii—O3—O189.73 (13)
O1v—Cu2—O1iii180O1xii—O3—O2ii135.29 (13)
O1v—Cu2—O3v81.76 (13)O1xii—O3—H386 (9)
O1v—Cu2—O3iii98.24 (13)O1xii—O3—H2iii92.9 (16)
O1v—Cu2—H1v18 (2)O2ii—O3—H3139 (9)
O1v—Cu2—H1iii162 (2)O2ii—O3—H2iii102 (2)
O1v—Cu2—H3v96 (3)H3—O3—H2iii75 (5)
O1v—Cu2—H3iii84 (3)Cu1—H1—Cu2xiii73 (2)
O1v—Cu2—H2vi112.8 (19)Cu1—H1—Cl1120 (5)
O1v—Cu2—H2vii67.2 (19)Cu1—H1—O159 (5)
O1iii—Cu2—O1v180Cu1—H1—H3xi147 (6)
O1iii—Cu2—O3v98.24 (13)Cu1—H1—H3i54 (3)
O1iii—Cu2—O3iii81.76 (13)Cu1—H1—H2iii48 (3)
O1iii—Cu2—H1v162 (2)Cu2xiii—H1—Cu383 (3)
O1iii—Cu2—H1iii18 (2)Cu2xiii—H1—Cl1135 (5)
O1iii—Cu2—H3v84 (3)Cu2xiii—H1—H3xi139 (6)
O1iii—Cu2—H3iii96 (3)Cu2xiii—H1—H3i126 (4)
O1iii—Cu2—H2vi67.2 (19)Cu2xiii—H1—H2iii67 (2)
O1iii—Cu2—H2vii112.8 (19)Cu3—H1—Cl1141 (5)
O3v—Cu2—O3iii180Cu3—H1—O146 (5)
O3v—Cu2—H1v92 (3)Cu3—H1—H3xi98 (3)
O3v—Cu2—H1iii88 (3)Cu3—H1—H3i74 (4)
O3v—Cu2—H3v20 (3)Cu3—H1—H2iii121 (4)
O3v—Cu2—H3iii160 (3)Cl1—H1—O1174 (9)
O3v—Cu2—H2vi116 (2)Cl1—H1—H3xi48 (3)
O3v—Cu2—H2vii64 (2)Cl1—H1—H3i87 (4)
O3iii—Cu2—O3v180Cl1—H1—H2iii90 (4)
O3iii—Cu2—H1v88 (3)O1—H1—H3xi136 (7)
O3iii—Cu2—H1iii92 (3)O1—H1—H3i97 (8)
O3iii—Cu2—H3v160 (3)O1—H1—H2iii85 (6)
O3iii—Cu2—H3iii20 (3)H3xi—H1—H3i92 (5)
O3iii—Cu2—H2vi64 (2)H3xi—H1—H2iii138 (5)
O3iii—Cu2—H2vii116 (2)H3i—H1—H3xi92 (5)
H1v—Cu2—H1iii180H3i—H1—H2iii84 (4)
H1v—Cu2—H3v102 (4)Cu1—H3—Cu2xiii74 (2)
H1v—Cu2—H3iii78 (4)Cu1—H3—Cu3ii73 (3)
H1v—Cu2—H2vi121 (3)Cu1—H3—Cl1xiv119 (6)
H1v—Cu2—H2vii59 (3)Cu1—H3—O353 (6)
H1iii—Cu2—H1v180Cu1—H3—H1xiv142 (7)
H1iii—Cu2—H3v78 (4)Cu1—H3—H1i54 (3)
H1iii—Cu2—H3iii102 (4)Cu1—H3—H2iii49 (3)
H1iii—Cu2—H2vi59 (3)Cu2xiii—H3—Cu3ii83 (3)
H1iii—Cu2—H2vii121 (3)Cu2xiii—H3—Cl1xiv138 (6)
H3v—Cu2—H3iii180Cu2xiii—H3—H1xiv142 (6)
H3v—Cu2—H2vi123 (3)Cu2xiii—H3—H1i127 (4)
H3v—Cu2—H2vii57 (3)Cu2xiii—H3—H2iii69 (2)
H3iii—Cu2—H3v180Cu3ii—H3—Cl1xiv138 (5)
H3iii—Cu2—H2vi57 (3)Cu3ii—H3—H1xiv96 (3)
H3iii—Cu2—H2vii123 (3)Cu3ii—H3—H1i72 (4)
H2vi—Cu2—H2vii180Cu3ii—H3—H2iii121 (5)
H2vii—Cu2—H2vi180Cl1xiv—H3—O3171 (11)
Cl1viii—Cu3—Cl1ix178.23 (3)Cl1xiv—H3—H1xiv48 (3)
Cl1viii—Cu3—O198.32 (10)Cl1xiv—H3—H1i84 (5)
Cl1viii—Cu3—O282.69 (8)Cl1xiv—H3—H2iii89 (4)
Cl1viii—Cu3—O2ii96.23 (8)O3—H3—H1xiv138 (7)
Cl1viii—Cu3—O3x82.72 (9)O3—H3—H1i90 (9)
Cl1viii—Cu3—H180 (3)O3—H3—H2iii84 (6)
Cl1viii—Cu3—H3x99 (3)H1xiv—H3—H1i88 (5)
Cl1viii—Cu3—H2101.7 (10)H1xiv—H3—H2iii137 (5)
Cl1viii—Cu3—H2ii77.3 (11)H1i—H3—H1xiv88 (5)
Cl1ix—Cu3—Cl1viii178.23 (3)H1i—H3—H2iii84 (4)
Cl1ix—Cu3—O181.80 (9)Cu1x—H2—Cu2xv71 (3)
Cl1ix—Cu3—O299.05 (8)Cu1x—H2—Cu378 (3)
Cl1ix—Cu3—O2ii82.03 (8)Cu1x—H2—Cu3x79 (3)
Cl1ix—Cu3—O3x97.19 (9)Cu1x—H2—Cl1vii133 (5)
Cl1ix—Cu3—H1101 (3)Cu1x—H2—O1ix48 (3)
Cl1ix—Cu3—H3x81 (3)Cu1x—H2—O273 (8)
Cl1ix—Cu3—H280.1 (10)Cu1x—H2—O3ix47 (3)
Cl1ix—Cu3—H2ii101.0 (11)Cu1x—H2—H1ix59 (4)
O1—Cu3—O298.04 (14)Cu1x—H2—H3ix61 (4)
O1—Cu3—O2ii82.62 (14)Cu2xv—H2—Cu3128 (4)
O1—Cu3—O3x178.63 (13)Cu2xv—H2—Cu3x130 (4)
O1—Cu3—H121 (2)Cu2xv—H2—Cl1vii62.8 (13)
O1—Cu3—H3x160 (2)Cu2xv—H2—O2144 (11)
O1—Cu3—H293 (3)Cu2xv—H2—H1ix54 (3)
O1—Cu3—H2ii88 (3)Cu2xv—H2—H3ix54 (3)
O2—Cu3—O2ii178.80 (13)Cu3—H2—Cu3x81.1 (9)
O2—Cu3—O3x81.20 (13)Cu3—H2—Cl1vii130 (4)
O2—Cu3—H186 (2)Cu3—H2—O1ix89 (3)
O2—Cu3—H3x95 (2)Cu3—H2—O3ix125 (5)
O2—Cu3—H219.1 (11)Cu3—H2—H1ix74 (3)
O2—Cu3—H2ii159.8 (11)Cu3—H2—H3ix136 (6)
O2ii—Cu3—O2178.80 (13)Cu3x—H2—Cu381.1 (9)
O2ii—Cu3—O3x98.16 (14)Cu3x—H2—Cl1vii134 (5)
O2ii—Cu3—H194 (2)Cu3x—H2—O1ix127 (5)
O2ii—Cu3—H3x85 (2)Cu3x—H2—O3ix90 (3)
O2ii—Cu3—H2162.0 (11)Cu3x—H2—H1ix134 (6)
O2ii—Cu3—H2ii19.1 (11)Cu3x—H2—H3ix77 (4)
O3x—Cu3—H1160 (2)Cl1vii—H2—O1ix91 (2)
O3x—Cu3—H3x20 (2)Cl1vii—H2—O2153 (12)
O3x—Cu3—H286 (3)Cl1vii—H2—O3ix94 (2)
O3x—Cu3—H2ii93 (3)Cl1vii—H2—H1ix91 (3)
H1—Cu3—H3x178 (5)Cl1vii—H2—H3ix92 (4)
H1—Cu3—H287 (4)O1ix—H2—O2111 (9)
H1—Cu3—H2ii93 (4)O1ix—H2—O3ix55 (3)
H3x—Cu3—H295 (4)O1ix—H2—H3ix75 (4)
H3x—Cu3—H2ii85 (4)O2—H2—O3ix111 (9)
H2—Cu3—H2ii179 (2)O2—H2—H1ix105 (7)
H2ii—Cu3—H2179 (2)O2—H2—H3ix108 (8)
Cu2—Cl1—Cu3viii76.08 (3)O3ix—H2—H1ix74 (4)
Cu2—Cl1—Cu3iii75.79 (2)H1ix—H2—H3ix95 (5)
Symmetry codes: (i) x, y+1, z+1; (ii) x+1/2, y+1/2, z+3/2; (iii) x1/2, y+1/2, z1/2; (iv) x, y, z; (v) x+1/2, y1/2, z+1/2; (vi) x1, y, z1; (vii) x+1, y, z+1; (viii) x, y, z+1; (ix) x+1/2, y+1/2, z+1/2; (x) x+1/2, y1/2, z+3/2; (xi) x, y1, z; (xii) x+1, y+1, z+1; (xiii) x+1/2, y+1/2, z+1/2; (xiv) x, y+1, z; (xv) x+1, y, z+1.

Experimental details

(I)(II)
Crystal data
Chemical formulaH3ClCu2O3H3ClCu2O3
Mr213.6213.6
Crystal system, space groupTriclinic, P1Monoclinic, P21/n
Temperature (K)294294
a, b, c (Å)9.1646 (9), 9.2029 (8), 9.2102 (8)6.1226 (3), 6.8346 (4), 9.1841 (6)
α, β, γ (°)95.858 (6), 96.290 (7), 96.507 (2)90, 99.577 (4), 90
V3)761.97 (12)378.96 (4)
Z84
Radiation typeMo KαMo Kα
µ (mm1)11.6911.76
Crystal size (mm)0.19 × 0.12 × 0.030.08 × 0.08 × 0.05
Data collection
DiffractometerNonius KappaCCDNonius KappaCCD
Absorption correctionGaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
Multi-scan
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
Tmin, Tmax0.148, 0.7080.350, 0.540
No. of measured, independent and
observed [I > 3σ(I)] reflections
47586, 6622, 4581 1685, 1672, 993
Rint0.0450.000
(sin θ/λ)max1)0.8070.818
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.191, 1.33 0.040, 0.122, 1.08
No. of reflections66221672
No. of parameters26269
No. of restraints243
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.80, 1.491.80, 1.92

Computer programs: Jana2000 (Petricek, Dusek & Palatinus, 2000).

Selected bond lengths (Å) for (I) top
Cu1a—Cu4a3.0719 (11)Cl2b—O1b3.142 (5)
Cu1a—Cu4ai3.0719 (11)Cl2b—O1cxiv3.095 (5)
Cu1a—Cu4b3.0148 (7)Cl2b—O2bxvii3.439 (5)
Cu1a—Cu4bi3.0148 (7)Cl2b—O2ci3.227 (5)
Cu1a—Cu4c3.1286 (9)Cl2b—O3axiv3.062 (6)
Cu1a—Cu4ci3.1286 (9)Cl2b—O3b3.269 (5)
Cu1a—O4a2.306 (5)Cl2b—O4ai3.086 (5)
Cu1a—O4ai2.306 (5)Cl2b—H4b3.46 (7)
Cu1a—O4b2.001 (5)Cl2b—H4ai2.26 (6)
Cu1a—O4bi2.001 (5)Cl2b—H3axiv2.13 (7)
Cu1a—O4c2.069 (5)Cl2b—H2bxvii2.94 (6)
Cu1a—O4ci2.069 (5)Cl2b—H2aix3.26 (7)
Cu1a—H4b2.68 (6)Cl2b—H3cxix3.50 (6)
Cu1a—H4bi2.68 (6)Cl2b—H1cxiv2.27 (6)
Cu1a—H4a2.09 (6)Cl2c—O1axx3.091 (5)
Cu1a—H4ai2.09 (6)Cl2c—O1c3.247 (5)
Cu1a—H4c2.55 (8)Cl2c—O2ai3.143 (6)
Cu1a—H4ci2.55 (8)Cl2c—O3bxx3.085 (5)
Cu2a—Cu3aii2.9912 (7)Cl2c—O3c3.223 (5)
Cu2a—Cu3aiii2.9912 (7)Cl2c—O4bi3.074 (6)
Cu2a—Cu3bii3.1283 (9)Cl2c—O4c3.452 (5)
Cu2a—Cu3biii3.1283 (9)Cl2c—H4bi2.18 (7)
Cu2a—Cu4a3.0971 (10)Cl2c—H4a3.47 (6)
Cu2a—Cu4aiv3.0971 (10)Cl2c—H4c3.15 (6)
Cu2a—O1a2.398 (5)Cl2c—H1axx2.23 (5)
Cu2a—O1aiv2.398 (5)Cl2c—H3bxx2.19 (6)
Cu2a—O2bv2.019 (4)Cl2c—H2cix3.16 (6)
Cu2a—O2bi2.019 (4)O1a—O2bi2.660 (7)
Cu2a—O3a2.004 (5)O1a—O3a2.701 (8)
Cu2a—O3aiv2.004 (5)O1a—O3aiv3.498 (7)
Cu2a—H3a2.53 (8)O1a—O3biii2.935 (7)
Cu2a—H3aiv2.53 (8)O1a—O4b2.921 (7)
Cu2a—H1a2.97 (6)O1a—H4b2.79 (6)
Cu2a—H1aiv2.97 (6)O1a—H4biii3.31 (7)
Cu2a—H2bv2.48 (10)O1a—H3a3.46 (8)
Cu2a—H2bi2.48 (10)O1a—H1a0.99 (6)
Cu2b—Cu3b3.0042 (9)O1a—H2bi3.36 (8)
Cu2b—Cu3bvi3.0042 (9)O1a—H3b3.29 (7)
Cu2b—Cu3cvii3.0965 (10)O1a—H3biii2.82 (6)
Cu2b—Cu3ci3.0965 (10)O1b—O2cvii3.445 (7)
Cu2b—Cu4b3.1029 (7)O1b—O2ci2.640 (8)
Cu2b—Cu4bvi3.1029 (7)O1b—O3b2.655 (8)
Cu2b—O1b2.308 (6)O1b—O3bvi3.422 (7)
Cu2b—O1bvi2.308 (6)O1b—O3cxix2.946 (7)
Cu2b—O2cvii2.023 (5)O1b—O4c3.007 (8)
Cu2b—O2ci2.023 (5)O1b—H4c3.15 (6)
Cu2b—O3b2.013 (4)O1b—H4cxix3.31 (7)
Cu2b—O3bvi2.013 (4)O1b—H3cxix3.33 (5)
Cu2b—H3b2.66 (6)O1b—H2cvii3.11 (6)
Cu2b—H3bvi2.66 (6)O1b—H2ci3.17 (6)
Cu2b—H2cvii2.13 (6)O1b—H1b0.98 (7)
Cu2b—H2ci2.13 (6)O1c—O2aviii3.494 (7)
Cu2b—H1b2.92 (6)O1c—O2ai2.660 (9)
Cu2b—H1bvi2.92 (6)O1c—O3ax3.041 (7)
Cu2c—Cu3aviii3.1251 (7)O1c—O3c2.543 (7)
Cu2c—Cu3ai3.1251 (7)O1c—O3cxi3.144 (6)
Cu2c—Cu3cix3.0724 (11)O1c—O4a2.965 (7)
Cu2c—Cu3cx3.0724 (11)O1c—H4a3.48 (6)
Cu2c—Cu4c3.0040 (9)O1c—H3ax3.19 (7)
Cu2c—Cu4cxi3.0040 (9)O1c—H2aviii3.33 (8)
Cu2c—O1c2.064 (5)O1c—H3c3.09 (6)
Cu2c—O1cxi2.064 (5)O1c—H3cxi2.64 (6)
Cu2c—O2aviii2.319 (6)O1c—H1c1.02 (5)
Cu2c—O2ai2.319 (6)O2a—O2bxv3.000 (8)
Cu2c—O3c1.979 (4)O2a—O2cxiii2.948 (8)
Cu2c—O3cxi1.979 (4)O2a—O3cxvi3.404 (7)
Cu2c—H2aviii2.73 (9)O2a—O3ci2.646 (8)
Cu2c—H2ai2.73 (9)O2a—H2bxxi3.32 (9)
Cu2c—H3c2.00 (6)O2a—H2bxv3.34 (6)
Cu2c—H3cxi2.00 (6)O2a—H2a0.99 (7)
Cu2c—H1c2.38 (9)O2a—H3cxvi2.84 (5)
Cu2c—H1cxi2.38 (9)O2a—H3ci3.27 (6)
Cu3a—Cu3bxii3.4204 (11)O2a—H1cxvi3.03 (8)
Cu3a—Cu3cxiii3.4262 (11)O2a—H2cxiii3.10 (6)
Cu3a—Cu4axiv3.4188 (11)O2b—O2cxxii3.033 (7)
Cu3a—Cu4ci3.4162 (11)O2b—O3axxiii3.093 (7)
Cu3a—Cl2axiv2.7563 (19)O2b—O3ai2.572 (8)
Cu3a—Cl2ci2.8378 (18)O2b—H3axxiii2.99 (8)
Cu3a—O1ci2.017 (5)O2b—H3ai3.46 (8)
Cu3a—O2a1.949 (6)O2b—H1ai3.44 (6)
Cu3a—O2bxv2.034 (5)O2b—H2b1.03 (6)
Cu3a—O3axiv1.990 (6)O2b—H2axxiv3.30 (8)
Cu3a—H3axiv2.67 (7)O2b—H2axv3.29 (7)
Cu3a—H2bxv2.85 (5)O2c—O3bxxv3.122 (6)
Cu3a—H2a2.71 (7)O2c—O3bi2.557 (7)
Cu3a—H3cxvi2.97 (5)O2c—H2bxxii2.96 (7)
Cu3a—H1ci2.94 (4)O2c—H2axiii2.87 (7)
Cu3b—Cu3ci3.4252 (16)O2c—H3bxxv3.25 (6)
Cu3b—Cu4aiii3.4315 (16)O2c—H3bi3.43 (7)
Cu3b—Cu4b3.4134 (11)O2c—H2c1.01 (5)
Cu3b—Cl2aiii2.8165 (19)O2c—H1bi3.49 (6)
Cu3b—Cl2b2.7604 (18)O3a—O4a2.944 (8)
Cu3b—O1aiii1.943 (5)O3a—H4a3.46 (6)
Cu3b—O2bxvii1.986 (5)O3a—H3a0.98 (8)
Cu3b—O2ci2.009 (5)O3a—H2bv2.85 (9)
Cu3b—O3b1.986 (5)O3a—H2bi3.49 (8)
Cu3b—H3axiv3.42 (7)O3b—O4b3.051 (7)
Cu3b—H1aiii2.42 (6)O3b—H4b2.92 (7)
Cu3b—H2bxvii2.39 (6)O3b—H1a3.42 (6)
Cu3b—H3b2.51 (7)O3b—H1aiii2.83 (6)
Cu3b—H2ci2.84 (4)O3b—H3b0.99 (6)
Cu3c—Cu4bi3.4297 (10)O3b—H2cvii2.53 (6)
Cu3c—Cu4cxviii3.4223 (16)O3b—H2ci3.28 (5)
Cu3c—Cl2bi2.7874 (16)O3b—H1b3.49 (7)
Cu3c—Cl2cxviii2.7709 (16)O3c—O4c3.027 (6)
Cu3c—O1bi1.946 (5)O3c—H4c2.99 (6)
Cu3c—O2axiii1.955 (6)O3c—H2aviii3.45 (8)
Cu3c—O2c2.005 (6)O3c—H2ai3.29 (8)
Cu3c—O3cxviii2.010 (5)O3c—H3c0.95 (5)
Cu3c—H2axiii2.35 (6)O3c—H1c3.00 (8)
Cu3c—H3cxviii2.66 (5)O3c—H1cxi3.18 (8)
Cu3c—H1cx3.28 (6)O3c—H1b3.48 (6)
Cu3c—H2c2.46 (6)O3c—H1bxix2.90 (6)
Cu3c—H1bi2.51 (6)O4a—O4b2.650 (8)
Cu4a—Cu4b3.4173 (11)O4a—O4bi3.409 (7)
Cu4a—Cu4c3.4316 (16)O4a—O4c2.636 (7)
Cu4a—Cl1a2.7751 (17)O4a—O4ci3.500 (6)
Cu4a—Cl2a2.7875 (17)O4a—H4a1.00 (5)
Cu4a—O1a1.951 (5)O4a—H4c3.39 (7)
Cu4a—O3a2.022 (5)O4a—H4ci3.49 (7)
Cu4a—O4a1.955 (6)O4a—H3a2.81 (7)
Cu4a—O4b2.010 (5)O4a—H1c2.75 (7)
Cu4a—H4b2.55 (7)O4b—O4c2.571 (8)
Cu4a—H4a2.56 (6)O4b—O4ci3.156 (7)
Cu4a—H4ci3.39 (6)O4b—H4b1.01 (7)
Cu4a—H3a2.45 (7)O4b—H4a3.03 (6)
Cu4a—H1a2.62 (5)O4b—H4ai2.75 (6)
Cu4a—H2bv3.30 (7)O4b—H4c3.42 (7)
Cu4b—Cu4c3.4255 (10)O4b—H4ci3.06 (7)
Cu4b—Cl1a2.7779 (17)O4b—H1a3.02 (5)
Cu4b—Cl2b2.8252 (17)O4b—H1aiii3.31 (6)
Cu4b—O1b1.957 (6)O4b—H3b2.97 (6)
Cu4b—O3b2.030 (5)O4c—H4b3.46 (7)
Cu4b—O4b1.990 (5)O4c—H4bi3.31 (6)
Cu4b—O4c2.018 (5)O4c—H4a3.03 (6)
Cu4b—H4b2.49 (7)O4c—H4ai2.85 (6)
Cu4b—H4ai3.01 (5)O4c—H4c0.97 (7)
Cu4b—H4c2.67 (6)O4c—H3c3.41 (6)
Cu4b—H3b2.55 (6)O4c—H1b2.92 (7)
Cu4b—H2cvii3.02 (5)O4c—H1bxix3.31 (7)
Cu4b—H1b2.48 (7)H4b—H4ai2.89 (9)
Cu4c—Cl1a2.8101 (19)H4b—H4ci3.08 (9)
Cu4c—Cl2c2.7635 (18)H4b—H1a2.70 (8)
Cu4c—O1c1.970 (5)H4b—H1aiii2.39 (9)
Cu4c—O3c2.004 (5)H4b—H3b2.72 (8)
Cu4c—O4a1.957 (5)H4b—H3biii2.79 (9)
Cu4c—O4c1.986 (5)H4a—H4ci2.94 (9)
Cu4c—H4a2.59 (6)H4a—H3a3.43 (9)
Cu4c—H4c2.45 (6)H4a—H3ax3.27 (10)
Cu4c—H3c2.60 (6)H4a—H1c3.46 (9)
Cu4c—H1c2.15 (6)H4c—H3c3.45 (8)
Cl1a—O2aviii3.082 (6)H4c—H3cxix3.41 (9)
Cl1a—O2bv3.099 (5)H4c—H1b2.91 (9)
Cl1a—O2cvii3.058 (5)H4c—H1bxix2.48 (10)
Cl1a—O4a3.130 (5)H3a—H2bv2.54 (11)
Cl1a—O4b3.227 (5)H3a—H1c2.69 (11)
Cl1a—O4c3.244 (4)H1a—H1aiii3.30 (8)
Cl1a—H3a3.32 (7)H1a—H3b2.52 (9)
Cl1a—H2bv2.19 (7)H1a—H3biii2.59 (8)
Cl1a—H2aviii2.18 (6)H2b—H2axxiv2.41 (12)
Cl1a—H3c3.39 (6)H2b—H2axv3.47 (10)
Cl1a—H1c3.03 (5)H2b—H1cxxiii3.41 (7)
Cl1a—H3b3.40 (6)H2b—H2cxxvi3.36 (10)
Cl1a—H2cvii2.18 (6)H2a—H3cxvi2.98 (10)
Cl2a—O1a3.115 (5)H2a—H1cxvi2.66 (10)
Cl2a—O1bxviii3.096 (6)H2a—H2cxxvii3.31 (10)
Cl2a—O2bi3.257 (5)H2a—H2cxiii3.20 (9)
Cl2a—O3a3.230 (5)H3c—H1c3.32 (11)
Cl2a—O3cxviii3.067 (5)H3c—H1cxi2.88 (9)
Cl2a—O4ci3.103 (5)H3c—H1b3.10 (9)
Cl2a—H4a3.40 (6)H3c—H1bxix3.27 (8)
Cl2a—H4ci2.20 (6)H3b—H2cvii2.57 (8)
Cl2a—H3cxviii2.22 (6)H2c—H1bxxv3.34 (9)
Cl2a—H1bxviii2.27 (6)H1b—H1bxix3.37 (8)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y, z1; (iii) x+1, y, z+1; (iv) x+1, y, z; (v) x, y1, z1; (vi) x, y, z+1; (vii) x1, y1, z; (viii) x1, y, z1; (ix) x1, y, z; (x) x+1, y+1, z; (xi) x, y+1, z; (xii) x+1, y, z+2; (xiii) x+2, y+1, z+1; (xiv) x, y, z+1; (xv) x+1, y+1, z+2; (xvi) x+1, y, z+1; (xvii) x, y1, z; (xviii) x+1, y, z; (xix) x, y+1, z+1; (xx) x, y+1, z; (xxi) x+1, y1, z; (xxii) x+1, y+2, z+1; (xxiii) x, y+1, z+1; (xxiv) x1, y+1, z; (xxv) x+1, y+1, z; (xxvi) x1, y, z+1; (xxvii) x, y1, z+1.
Selected geometric parameters (Å, º) for (II) top
Cu1—O12.157 (3)Cu3—Cl1ix2.7911 (10)
Cu1—O1i2.157 (3)Cu3—O11.973 (3)
Cu1—O2ii2.108 (3)Cu3—O21.978 (3)
Cu1—O2iii2.108 (3)Cu3—O2ii1.982 (3)
Cu1—O32.052 (3)Cu3—O3x1.993 (3)
Cu1—O3i2.052 (3)Cu3—H12.53 (10)
Cu1—H12.49 (10)Cu3—H3x2.59 (10)
Cu1—H1i2.49 (10)Cu3—H22.63 (4)
Cu1—H32.49 (11)Cu3—H2ii2.63 (4)
Cu1—H3i2.49 (11)Cl1—H12.09 (9)
Cu1—H2ii2.17 (15)Cl1—H3xi2.10 (9)
Cu1—H2iii2.17 (15)Cl1—H2vii2.15 (8)
Cu2—Cl12.7812 (9)O1—O22.983 (4)
Cu2—Cl1iv2.7812 (9)O1—O2ii2.611 (5)
Cu2—O1v1.975 (3)O1—O32.591 (4)
Cu2—O1iii1.975 (3)O1—O3xii2.993 (5)
Cu2—O3v1.984 (3)O1—H10.99 (9)
Cu2—O3iii1.984 (3)O2—O3x2.584 (5)
Cu2—H1v2.64 (11)O2—H21.00 (3)
Cu2—H1iii2.64 (11)O3—H30.99 (9)
Cu2—H3v2.58 (11)H1—H3xi2.80 (11)
Cu2—H3iii2.58 (11)H1—H3i2.9 (2)
Cu2—H2vi3.00 (9)H1—H2iii2.79 (13)
Cu2—H2vii3.00 (9)H3—H2iii2.69 (13)
Cu3—Cl1viii2.7690 (10)
O1—Cu1—O1i180Cu2—Cl1—H1137 (2)
O1—Cu1—O2ii75.48 (11)Cu2—Cl1—H3xi136 (2)
O1—Cu1—O2iii104.52 (11)Cu2—Cl1—H2vii74 (4)
O1—Cu1—O375.95 (12)Cu3viii—Cl1—Cu3iii75.85 (3)
O1—Cu1—O3i104.05 (12)Cu3viii—Cl1—H1133 (4)
O1—Cu1—H123 (2)Cu3viii—Cl1—H3xi84 (4)
O1—Cu1—H1i157 (2)Cu3viii—Cl1—H2vii133 (3)
O1—Cu1—H394 (3)Cu3iii—Cl1—Cu3viii75.85 (3)
O1—Cu1—H3i86 (3)Cu3iii—Cl1—H182 (3)
O1—Cu1—H2ii96.4 (13)Cu3iii—Cl1—H3xi136 (4)
O1—Cu1—H2iii83.6 (13)Cu3iii—Cl1—H2vii129 (2)
O1i—Cu1—O1180H1—Cl1—H3xi84 (3)
O1i—Cu1—O2ii104.52 (11)H1—Cl1—H2vii93 (5)
O1i—Cu1—O2iii75.48 (11)H3xi—Cl1—H2vii93 (5)
O1i—Cu1—O3104.05 (12)Cu1—O1—Cu2xiii95.50 (12)
O1i—Cu1—O3i75.95 (12)Cu1—O1—Cu396.35 (14)
O1i—Cu1—H1157 (2)Cu1—O1—O2133.37 (16)
O1i—Cu1—H1i23 (2)Cu1—O1—O2ii51.41 (10)
O1i—Cu1—H386 (3)Cu1—O1—O350.18 (9)
O1i—Cu1—H3i94 (3)Cu1—O1—O3xii132.91 (14)
O1i—Cu1—H2ii83.6 (13)Cu1—O1—H197 (7)
O1i—Cu1—H2iii96.4 (13)Cu1—O1—H2iii48 (2)
O2ii—Cu1—O2iii180Cu2xiii—O1—Cu3120.20 (14)
O2ii—Cu1—O376.80 (11)Cu2xiii—O1—O2119.98 (14)
O2ii—Cu1—O3i103.20 (11)Cu2xiii—O1—O2ii101.79 (13)
O2ii—Cu1—H192 (2)Cu2xiii—O1—O349.27 (10)
O2ii—Cu1—H1i88 (2)Cu2xiii—O1—H1123 (7)
O2ii—Cu1—H395 (2)Cu2xiii—O1—H2iii73.6 (9)
O2ii—Cu1—H3i85 (2)Cu3—O1—O2ii48.84 (10)
O2ii—Cu1—H2ii26.9 (12)Cu3—O1—O3101.97 (14)
O2ii—Cu1—H2iii153.1 (12)Cu3—O1—O3xii118.96 (14)
O2iii—Cu1—O2ii180Cu3—O1—H1113 (6)
O2iii—Cu1—O3103.20 (11)Cu3—O1—H2iii144.6 (19)
O2iii—Cu1—O3i76.80 (11)O2—O1—O2ii89.87 (13)
O2iii—Cu1—H188 (2)O2—O1—O3136.27 (14)
O2iii—Cu1—H1i92 (2)O2—O1—O3xii91.94 (12)
O2iii—Cu1—H385 (2)O2—O1—H188 (5)
O2iii—Cu1—H3i95 (2)O2—O1—H2iii162.5 (14)
O2iii—Cu1—H2ii153.1 (12)O2ii—O1—O289.87 (13)
O2iii—Cu1—H2iii26.9 (12)O2ii—O1—O359.56 (12)
O3—Cu1—O3i180O2ii—O1—O3xii135.08 (14)
O3—Cu1—H195 (3)O2ii—O1—H1129 (8)
O3—Cu1—H1i85 (3)O2ii—O1—H2iii98 (2)
O3—Cu1—H323 (3)O3—O1—O3xii90.27 (13)
O3—Cu1—H3i157 (3)O3—O1—H1135 (5)
O3—Cu1—H2ii98.0 (13)O3—O1—H2iii60.5 (17)
O3—Cu1—H2iii82.0 (13)O3xii—O1—O390.27 (13)
O3i—Cu1—O3180O3xii—O1—H196 (8)
O3i—Cu1—H185 (3)O3xii—O1—H2iii93.1 (15)
O3i—Cu1—H1i95 (3)H1—O1—H2iii75 (5)
O3i—Cu1—H3157 (3)Cu1x—O2—Cu396.11 (14)
O3i—Cu1—H3i23 (3)Cu1x—O2—Cu3x97.67 (14)
O3i—Cu1—H2ii82.0 (13)Cu1x—O2—O1132.83 (13)
O3i—Cu1—H2iii98.0 (13)Cu1x—O2—O1x53.11 (10)
H1—Cu1—H1i180Cu1x—O2—O3x50.62 (10)
H1—Cu1—H3108 (4)Cu1x—O2—H280 (9)
H1—Cu1—H3i72 (4)Cu3—O2—Cu3x119.32 (15)
H1—Cu1—H2ii107 (3)Cu3—O2—O1x101.82 (15)
H1—Cu1—H2iii73 (3)Cu3—O2—O3x49.66 (10)
H1i—Cu1—H1180Cu3—O2—H2120 (3)
H1i—Cu1—H372 (4)Cu3x—O2—Cu3119.32 (15)
H1i—Cu1—H3i108 (4)Cu3x—O2—O1118.40 (14)
H1i—Cu1—H2ii73 (3)Cu3x—O2—O1x48.54 (10)
H1i—Cu1—H2iii107 (3)Cu3x—O2—O3x101.95 (15)
H3—Cu1—H3i180Cu3x—O2—H2120 (3)
H3—Cu1—H2ii110 (3)O1—O2—O1x135.01 (15)
H3—Cu1—H2iii70 (3)O1—O2—O3x90.58 (12)
H3i—Cu1—H3180O1—O2—H2104 (6)
H3i—Cu1—H2ii70 (3)O1x—O2—O1135.01 (15)
H3i—Cu1—H2iii110 (3)O1x—O2—O3x59.83 (12)
H2ii—Cu1—H2iii180O1x—O2—H2120 (7)
H2iii—Cu1—H2ii180O3x—O2—H2119 (8)
Cl1—Cu2—Cl1iv180Cu1—O3—Cu2xiii98.66 (12)
Cl1—Cu2—O1v97.97 (8)Cu1—O3—Cu3ii97.45 (13)
Cl1—Cu2—O1iii82.03 (8)Cu1—O3—O153.87 (10)
Cl1—Cu2—O3v97.44 (8)Cu1—O3—O1xii135.23 (14)
Cl1—Cu2—O3iii82.56 (8)Cu1—O3—O2ii52.58 (10)
Cl1—Cu2—H1v82 (2)Cu1—O3—H3105 (8)
Cl1—Cu2—H1iii98 (2)Cu1—O3—H2iii51 (2)
Cl1—Cu2—H3v81 (2)Cu2xiii—O3—Cu3ii118.60 (13)
Cl1—Cu2—H3iii99 (2)Cu2xiii—O3—O148.96 (10)
Cl1—Cu2—H2vi136 (3)Cu2xiii—O3—O2ii102.45 (13)
Cl1—Cu2—H2vii44 (3)Cu2xiii—O3—H3116 (8)
Cl1iv—Cu2—Cl1180Cu2xiii—O3—H2iii76.3 (9)
Cl1iv—Cu2—O1v82.03 (8)Cu3ii—O3—O1102.06 (13)
Cl1iv—Cu2—O1iii97.97 (8)Cu3ii—O3—O1xii116.98 (13)
Cl1iv—Cu2—O3v82.56 (8)Cu3ii—O3—O2ii49.14 (9)
Cl1iv—Cu2—O3iii97.44 (8)Cu3ii—O3—H3116 (6)
Cl1iv—Cu2—H1v98 (2)Cu3ii—O3—H2iii148.0 (19)
Cl1iv—Cu2—H1iii82 (2)O1—O3—O1xii89.73 (13)
Cl1iv—Cu2—H3v99 (2)O1—O3—O2ii60.60 (12)
Cl1iv—Cu2—H3iii81 (2)O1—O3—H3139 (5)
Cl1iv—Cu2—H2vi44 (3)O1—O3—H2iii65.0 (16)
Cl1iv—Cu2—H2vii136 (3)O1xii—O3—O189.73 (13)
O1v—Cu2—O1iii180O1xii—O3—O2ii135.29 (13)
O1v—Cu2—O3v81.76 (13)O1xii—O3—H386 (9)
O1v—Cu2—O3iii98.24 (13)O1xii—O3—H2iii92.9 (16)
O1v—Cu2—H1v18 (2)O2ii—O3—H3139 (9)
O1v—Cu2—H1iii162 (2)O2ii—O3—H2iii102 (2)
O1v—Cu2—H3v96 (3)H3—O3—H2iii75 (5)
O1v—Cu2—H3iii84 (3)Cu1—H1—Cu2xiii73 (2)
O1v—Cu2—H2vi112.8 (19)Cu1—H1—Cl1120 (5)
O1v—Cu2—H2vii67.2 (19)Cu1—H1—O159 (5)
O1iii—Cu2—O1v180Cu1—H1—H3xi147 (6)
O1iii—Cu2—O3v98.24 (13)Cu1—H1—H3i54 (3)
O1iii—Cu2—O3iii81.76 (13)Cu1—H1—H2iii48 (3)
O1iii—Cu2—H1v162 (2)Cu2xiii—H1—Cu383 (3)
O1iii—Cu2—H1iii18 (2)Cu2xiii—H1—Cl1135 (5)
O1iii—Cu2—H3v84 (3)Cu2xiii—H1—H3xi139 (6)
O1iii—Cu2—H3iii96 (3)Cu2xiii—H1—H3i126 (4)
O1iii—Cu2—H2vi67.2 (19)Cu2xiii—H1—H2iii67 (2)
O1iii—Cu2—H2vii112.8 (19)Cu3—H1—Cl1141 (5)
O3v—Cu2—O3iii180Cu3—H1—O146 (5)
O3v—Cu2—H1v92 (3)Cu3—H1—H3xi98 (3)
O3v—Cu2—H1iii88 (3)Cu3—H1—H3i74 (4)
O3v—Cu2—H3v20 (3)Cu3—H1—H2iii121 (4)
O3v—Cu2—H3iii160 (3)Cl1—H1—O1174 (9)
O3v—Cu2—H2vi116 (2)Cl1—H1—H3xi48 (3)
O3v—Cu2—H2vii64 (2)Cl1—H1—H3i87 (4)
O3iii—Cu2—O3v180Cl1—H1—H2iii90 (4)
O3iii—Cu2—H1v88 (3)O1—H1—H3xi136 (7)
O3iii—Cu2—H1iii92 (3)O1—H1—H3i97 (8)
O3iii—Cu2—H3v160 (3)O1—H1—H2iii85 (6)
O3iii—Cu2—H3iii20 (3)H3xi—H1—H3i92 (5)
O3iii—Cu2—H2vi64 (2)H3xi—H1—H2iii138 (5)
O3iii—Cu2—H2vii116 (2)H3i—H1—H3xi92 (5)
H1v—Cu2—H1iii180H3i—H1—H2iii84 (4)
H1v—Cu2—H3v102 (4)Cu1—H3—Cu2xiii74 (2)
H1v—Cu2—H3iii78 (4)Cu1—H3—Cu3ii73 (3)
H1v—Cu2—H2vi121 (3)Cu1—H3—Cl1xiv119 (6)
H1v—Cu2—H2vii59 (3)Cu1—H3—O353 (6)
H1iii—Cu2—H1v180Cu1—H3—H1xiv142 (7)
H1iii—Cu2—H3v78 (4)Cu1—H3—H1i54 (3)
H1iii—Cu2—H3iii102 (4)Cu1—H3—H2iii49 (3)
H1iii—Cu2—H2vi59 (3)Cu2xiii—H3—Cu3ii83 (3)
H1iii—Cu2—H2vii121 (3)Cu2xiii—H3—Cl1xiv138 (6)
H3v—Cu2—H3iii180Cu2xiii—H3—H1xiv142 (6)
H3v—Cu2—H2vi123 (3)Cu2xiii—H3—H1i127 (4)
H3v—Cu2—H2vii57 (3)Cu2xiii—H3—H2iii69 (2)
H3iii—Cu2—H3v180Cu3ii—H3—Cl1xiv138 (5)
H3iii—Cu2—H2vi57 (3)Cu3ii—H3—H1xiv96 (3)
H3iii—Cu2—H2vii123 (3)Cu3ii—H3—H1i72 (4)
H2vi—Cu2—H2vii180Cu3ii—H3—H2iii121 (5)
H2vii—Cu2—H2vi180Cl1xiv—H3—O3171 (11)
Cl1viii—Cu3—Cl1ix178.23 (3)Cl1xiv—H3—H1xiv48 (3)
Cl1viii—Cu3—O198.32 (10)Cl1xiv—H3—H1i84 (5)
Cl1viii—Cu3—O282.69 (8)Cl1xiv—H3—H2iii89 (4)
Cl1viii—Cu3—O2ii96.23 (8)O3—H3—H1xiv138 (7)
Cl1viii—Cu3—O3x82.72 (9)O3—H3—H1i90 (9)
Cl1viii—Cu3—H180 (3)O3—H3—H2iii84 (6)
Cl1viii—Cu3—H3x99 (3)H1xiv—H3—H1i88 (5)
Cl1viii—Cu3—H2101.7 (10)H1xiv—H3—H2iii137 (5)
Cl1viii—Cu3—H2ii77.3 (11)H1i—H3—H1xiv88 (5)
Cl1ix—Cu3—Cl1viii178.23 (3)H1i—H3—H2iii84 (4)
Cl1ix—Cu3—O181.80 (9)Cu1x—H2—Cu2xv71 (3)
Cl1ix—Cu3—O299.05 (8)Cu1x—H2—Cu378 (3)
Cl1ix—Cu3—O2ii82.03 (8)Cu1x—H2—Cu3x79 (3)
Cl1ix—Cu3—O3x97.19 (9)Cu1x—H2—Cl1vii133 (5)
Cl1ix—Cu3—H1101 (3)Cu1x—H2—O1ix48 (3)
Cl1ix—Cu3—H3x81 (3)Cu1x—H2—O273 (8)
Cl1ix—Cu3—H280.1 (10)Cu1x—H2—O3ix47 (3)
Cl1ix—Cu3—H2ii101.0 (11)Cu1x—H2—H1ix59 (4)
O1—Cu3—O298.04 (14)Cu1x—H2—H3ix61 (4)
O1—Cu3—O2ii82.62 (14)Cu2xv—H2—Cu3128 (4)
O1—Cu3—O3x178.63 (13)Cu2xv—H2—Cu3x130 (4)
O1—Cu3—H121 (2)Cu2xv—H2—Cl1vii62.8 (13)
O1—Cu3—H3x160 (2)Cu2xv—H2—O2144 (11)
O1—Cu3—H293 (3)Cu2xv—H2—H1ix54 (3)
O1—Cu3—H2ii88 (3)Cu2xv—H2—H3ix54 (3)
O2—Cu3—O2ii178.80 (13)Cu3—H2—Cu3x81.1 (9)
O2—Cu3—O3x81.20 (13)Cu3—H2—Cl1vii130 (4)
O2—Cu3—H186 (2)Cu3—H2—O1ix89 (3)
O2—Cu3—H3x95 (2)Cu3—H2—O3ix125 (5)
O2—Cu3—H219.1 (11)Cu3—H2—H1ix74 (3)
O2—Cu3—H2ii159.8 (11)Cu3—H2—H3ix136 (6)
O2ii—Cu3—O2178.80 (13)Cu3x—H2—Cu381.1 (9)
O2ii—Cu3—O3x98.16 (14)Cu3x—H2—Cl1vii134 (5)
O2ii—Cu3—H194 (2)Cu3x—H2—O1ix127 (5)
O2ii—Cu3—H3x85 (2)Cu3x—H2—O3ix90 (3)
O2ii—Cu3—H2162.0 (11)Cu3x—H2—H1ix134 (6)
O2ii—Cu3—H2ii19.1 (11)Cu3x—H2—H3ix77 (4)
O3x—Cu3—H1160 (2)Cl1vii—H2—O1ix91 (2)
O3x—Cu3—H3x20 (2)Cl1vii—H2—O2153 (12)
O3x—Cu3—H286 (3)Cl1vii—H2—O3ix94 (2)
O3x—Cu3—H2ii93 (3)Cl1vii—H2—H1ix91 (3)
H1—Cu3—H3x178 (5)Cl1vii—H2—H3ix92 (4)
H1—Cu3—H287 (4)O1ix—H2—O2111 (9)
H1—Cu3—H2ii93 (4)O1ix—H2—O3ix55 (3)
H3x—Cu3—H295 (4)O1ix—H2—H3ix75 (4)
H3x—Cu3—H2ii85 (4)O2—H2—O3ix111 (9)
H2—Cu3—H2ii179 (2)O2—H2—H1ix105 (7)
H2ii—Cu3—H2179 (2)O2—H2—H3ix108 (8)
Cu2—Cl1—Cu3viii76.08 (3)O3ix—H2—H1ix74 (4)
Cu2—Cl1—Cu3iii75.79 (2)H1ix—H2—H3ix95 (5)
Symmetry codes: (i) x, y+1, z+1; (ii) x+1/2, y+1/2, z+3/2; (iii) x1/2, y+1/2, z1/2; (iv) x, y, z; (v) x+1/2, y1/2, z+1/2; (vi) x1, y, z1; (vii) x+1, y, z+1; (viii) x, y, z+1; (ix) x+1/2, y+1/2, z+1/2; (x) x+1/2, y1/2, z+3/2; (xi) x, y1, z; (xii) x+1, y+1, z+1; (xiii) x+1/2, y+1/2, z+1/2; (xiv) x, y+1, z; (xv) x+1, y, z+1.
 

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