Determination of the cation distribution in Fe₂Ni(PO₄)₂ using isotopic substitution and powder neutron diffraction

The distribution of divalent iron and nickel over the two metal sites with differing coordination geometry in Fe₂Ni(PO₄)₂, sarcopside, has been investigated using time-of-flight powder neutron diffraction of nickel isotopically substituted materials. Data from four separate samples were collected using HRPD at ISIS, containing ^natNi, ⁵⁸Ni, ⁶⁰Ni and ⁶²Ni, under identical conditions. The occupancy of iron on the M(1) site was found to be 0.290 (1) from a combined-data-set Rietveld refinement of the three isotopically substituted samples, compared with 0.26 (4) and 0.26 (15) respectively from this and a previous time-of-flight powder neutron diffraction study using natural-abundance nickel, and 0.366 (6) and 0.376 (3) using anomalous X-ray scattering techniques. A critical comparison of isotope substitution neutron diffraction and anomalous X-ray scattering methods for distinguishing nickel and iron from powder data is presented.

Computing details

(58NI_phase_1)

Crystal data

Fe1.00Ni0.50O4P	c = 10.35700 (8) Å
Mr = 180.17	β = 90.8913 (3)°
Monoclinic, P21/c	V = 292.65 Å^3
a = 5.98709 (4) Å	Z = 4
b = 4.72008 (4) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
FE1	0.5	0.0	0.0	0.00917	0.356 (8)
NI2	0.5	0.0	0.0	0.00917	0.644 (8)
FE3	0.23773 (11)	−0.0189 (2)	0.28158 (8)	0.01544	0.822 (4)
NI4	0.23773 (11)	−0.0189 (2)	0.28159 (8)	0.01544	0.178 (4)
O5	0.2770 (2)	0.7466 (3)	0.10199 (14)	0.01179
O6	0.2539 (3)	0.1896 (3)	0.46032 (14)	0.01254
O7	0.0676 (2)	0.3185 (3)	0.17842 (15)	0.01296
O8	0.4698 (3)	0.2775 (3)	0.15973 (16)	0.01405
P9	0.2596 (3)	0.4306 (3)	0.09730 (15)	0.00857

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
FE1	0.0110 (7)	0.0069 (7)	0.0096 (7)	0.0019 (5)	0.0011 (5)	−0.0008 (6)
NI2	0.0110 (7)	0.0069 (7)	0.0096 (7)	0.0019 (5)	0.0011 (5)	−0.0008 (6)
FE3	0.0160 (6)	0.0164 (6)	0.0140 (5)	0.0002 (5)	0.0021 (4)	0.0018 (5)
NI4	0.0160 (6)	0.0164 (6)	0.0140 (5)	0.0002 (5)	0.0021 (4)	0.0018 (5)
O5	0.0158 (10)	0.0037 (11)	0.0159 (10)	−0.0027 (9)	−0.0003 (8)	−0.0037 (8)
O6	0.0171 (10)	0.0111 (9)	0.0095 (10)	0.0021 (8)	0.0035 (8)	−0.0007 (7)
O7	0.0176 (11)	0.0122 (9)	0.0092 (9)	−0.0013 (7)	0.0038 (8)	0.0069 (8)
O8	0.0154 (9)	0.0120 (10)	0.0147 (9)	0.0037 (8)	0.0005 (7)	0.0083 (9)
P9	0.0127 (10)	0.0019 (10)	0.0112 (11)	0.0000 (8)	0.0033 (8)	0.0063 (8)

Geometric parameters (Å, º)

FE1—O5^i	2.0911 (14)	O5—FE1^vii	2.0911 (14)
FE1—O5^ii	2.0911 (14)	O5—NI2^vii	2.0911 (14)
FE1—O6^iii	2.1135 (14)	O5—FE3^vii	2.1804 (17)
FE1—O6^iv	2.1135 (14)	O5—NI4^vii	2.1804 (17)
FE1—O8	2.1201 (16)	O5—P9	1.496 (2)
FE1—O8^v	2.1201 (16)	O6—FE1^viii	2.1135 (14)
FE1—P9	2.6950 (16)	O6—NI2^viii	2.1135 (14)
FE1—P9^v	2.6950 (16)	O6—FE3	2.0974 (17)
NI2—O5^i	2.0911 (14)	O6—NI4	2.0973 (17)
NI2—O5^ii	2.0911 (14)	O6—P9^ix	1.5277 (19)
NI2—O6^iii	2.1135 (14)	O7—FE3	2.1637 (16)
NI2—O6^iv	2.1135 (14)	O7—FE3^x	2.0312 (16)
NI2—O8	2.1201 (16)	O7—NI4	2.1637 (16)
NI2—O8^v	2.1201 (16)	O7—NI4^x	2.0312 (16)
NI2—P9	2.6950 (16)	O7—P9	1.529 (2)
NI2—P9^v	2.6950 (16)	O8—FE1	2.1201 (16)
FE3—O5^i	2.1804 (17)	O8—NI2	2.1201 (16)
FE3—O6	2.0974 (17)	O8—FE3	2.3526 (17)
FE3—O7	2.1637 (16)	O8—FE3^viii	2.0800 (18)
FE3—O7^vi	2.0312 (16)	O8—NI4	2.3527 (17)
FE3—O8	2.3526 (17)	O8—NI4^viii	2.0800 (18)
FE3—O8^iii	2.0800 (18)	O8—P9	1.581 (2)
FE3—P9	2.8579 (17)	P9—FE1	2.6950 (16)
NI4—O5^i	2.1804 (17)	P9—NI2	2.6950 (16)
NI4—O6	2.0973 (17)	P9—FE3	2.8579 (17)
NI4—O7	2.1637 (16)	P9—NI4	2.8580 (17)
NI4—O7^vi	2.0312 (16)	P9—O5	1.496 (2)
NI4—O8	2.3527 (17)	P9—O6^iv	1.5277 (19)
NI4—O8^iii	2.0800 (18)	P9—O7	1.529 (2)
NI4—P9	2.8580 (17)	P9—O8	1.581 (2)
O5^i—FE1—O5^ii	180.0	O6—NI4—O8^iii	86.08 (6)
O5^i—FE1—O6^iii	87.36 (5)	O7^vi—NI4—O8^iii	121.47 (6)
O5^i—FE1—O6^iv	92.64 (5)	FE1^vii—O5—NI2^vii	0.0
O5^i—FE1—O8	84.05 (6)	FE1^vii—O5—P9	126.77 (11)
O5^i—FE1—O8^v	95.95 (6)	NI2^vii—O5—P9	126.77 (11)
O5^ii—FE1—O6^iii	92.64 (5)	FE1^viii—O6—NI2^viii	0.0
O5^ii—FE1—O6^iv	87.36 (5)	FE1^viii—O6—FE3	121.29 (8)
O5^ii—FE1—O8	95.95 (6)	FE1^viii—O6—NI4	121.29 (8)
O5^ii—FE1—O8^v	84.05 (6)	FE1^viii—O6—P9^ix	94.10 (9)
O6^iii—FE1—O6^iv	180.0	NI2^viii—O6—FE3	121.29 (8)
O6^iii—FE1—O8	110.14 (5)	NI2^viii—O6—NI4	121.29 (8)
O6^iii—FE1—O8^v	69.86 (5)	NI2^viii—O6—P9^ix	94.10 (9)
O6^iv—FE1—O8	69.86 (5)	FE3—O6—NI4	0.0
O6^iv—FE1—O8^v	110.14 (5)	FE3—O6—P9^ix	130.20 (9)
O8—FE1—O8^v	180.0	NI4—O6—P9^ix	130.20 (9)
O5^i—NI2—O5^ii	180.0	FE3^x—O7—NI4^x	0.0
O5^i—NI2—O6^iii	87.36 (5)	FE3^x—O7—P9	131.93 (9)
O5^i—NI2—O6^iv	92.64 (5)	NI4^x—O7—P9	131.93 (9)
O5^i—NI2—O8	84.05 (6)	FE1—O8—NI2	0.0
O5^i—NI2—O8^v	95.95 (6)	FE1—O8—FE3^viii	115.58 (7)
O5^ii—NI2—O6^iii	92.64 (5)	FE1—O8—NI4^viii	115.58 (7)
O5^ii—NI2—O6^iv	87.36 (5)	FE1—O8—P9	92.31 (10)
O5^ii—NI2—O8	95.95 (6)	NI2—O8—FE3^viii	115.58 (7)
O5^ii—NI2—O8^v	84.05 (6)	NI2—O8—NI4^viii	115.58 (7)
O6^iii—NI2—O6^iv	180.0	NI2—O8—P9	92.31 (10)
O6^iii—NI2—O8	110.14 (5)	FE3^viii—O8—NI4^viii	0.0
O6^iii—NI2—O8^v	69.86 (5)	FE3^viii—O8—P9	124.73 (9)
O6^iv—NI2—O8	69.86 (5)	NI4^viii—O8—P9	124.73 (9)
O6^iv—NI2—O8^v	110.14 (5)	O5—P9—O6^iv	113.63 (12)
O8—NI2—O8^v	180.0	O5—P9—O7	112.31 (13)
O6—FE3—O7^vi	91.53 (6)	O5—P9—O8	112.82 (13)
O6—FE3—O8^iii	86.08 (6)	O6^iv—P9—O7	112.08 (11)
O7^vi—FE3—O8^iii	121.47 (6)	O6^iv—P9—O8	102.49 (12)
O6—NI4—O7^vi	91.53 (6)	O7—P9—O8	102.58 (11)

Symmetry codes: (i) x, y−1, z; (ii) −x+1, −y+1, −z; (iii) −x+1, y−1/2, −z+1/2; (iv) x, −y+3/2, z+1/2; (v) −x+1, −y, −z; (vi) −x, y−1/2, −z+1/2; (vii) x, y+1, z; (viii) −x+1, y+1/2, −z+1/2; (ix) x, −y+3/2, z+3/2; (x) −x, y+1/2, −z+1/2.

(60NI_phase_1)

Crystal data

Fe1.00Ni0.50O4P	c = 10.35681 (3) Å
Mr = 180.17	β = 90.8902 (3)°
Monoclinic, P21/c	V = 292.67 Å^3
a = 5.987146 (18) Å	Z = 4
b = 4.720383 (16) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
FE1	0.5	0.0	0.0	0.00979	0.259 (4)
NI2	0.5	0.0	0.0	0.00979	0.741 (4)
FE3	0.23707 (12)	−0.02107 (17)	0.28182 (7)	0.01499	0.8706 (22)
NI4	0.23707 (12)	−0.02107 (17)	0.28183 (7)	0.01499	0.1294 (22)
O5	0.27751 (17)	0.7475 (2)	0.10199 (11)	0.01321
O6	0.2545 (2)	0.1906 (2)	0.46012 (11)	0.0139
O7	0.06711 (18)	0.3171 (2)	0.17862 (12)	0.01365
O8	0.4700 (2)	0.2761 (2)	0.15984 (11)	0.01331
P9	0.2594 (2)	0.4286 (3)	0.09761 (12)	0.00961

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
FE1	0.0137 (14)	0.0057 (15)	0.0100 (14)	0.0023 (11)	0.0007 (10)	−0.0022 (11)
NI2	0.0137 (14)	0.0057 (15)	0.0100 (14)	0.0023 (11)	0.0007 (10)	−0.0022 (11)
FE3	0.0141 (5)	0.0167 (5)	0.0142 (5)	−0.0003 (4)	0.0017 (4)	0.0019 (4)
NI4	0.0141 (5)	0.0167 (5)	0.0142 (5)	−0.0003 (4)	0.0017 (4)	0.0019 (4)
O5	0.0142 (8)	0.0096 (8)	0.0159 (7)	−0.0011 (7)	0.0006 (6)	−0.0017 (6)
O6	0.0167 (7)	0.0124 (7)	0.0127 (8)	0.0003 (6)	0.0038 (6)	0.0009 (6)
O7	0.0169 (8)	0.0120 (8)	0.0122 (7)	−0.0006 (5)	0.0050 (6)	0.0055 (6)
O8	0.0166 (7)	0.0100 (8)	0.0133 (7)	0.0014 (6)	0.0002 (6)	0.0058 (6)
P9	0.0112 (8)	0.0077 (7)	0.0100 (8)	−0.0005 (7)	0.0014 (7)	0.0066 (7)

Geometric parameters (Å, º)

FE1—O5^i	2.0866 (11)	O5—FE1^vii	2.0866 (11)
FE1—O5^ii	2.0866 (11)	O5—NI2^vii	2.0866 (11)
FE1—O6^iii	2.1083 (11)	O5—FE3^vii	2.1760 (14)
FE1—O6^iv	2.1083 (11)	O5—NI4^vii	2.1760 (14)
FE1—O8	2.1166 (12)	O5—P9	1.5099 (15)
FE1—O8^v	2.1166 (12)	O6—FE1^viii	2.1083 (11)
FE1—P9	2.6901 (13)	O6—NI2^viii	2.1083 (11)
FE1—P9^v	2.6901 (13)	O6—FE3	2.1007 (14)
NI2—O5^i	2.0866 (11)	O6—NI4	2.1006 (14)
NI2—O5^ii	2.0866 (11)	O6—P9^ix	1.5309 (16)
NI2—O6^iii	2.1083 (11)	O7—FE3	2.1661 (14)
NI2—O6^iv	2.1083 (11)	O7—FE3^x	2.0227 (12)
NI2—O8	2.1166 (12)	O7—NI4	2.1661 (14)
NI2—O8^v	2.1166 (12)	O7—NI4^x	2.0227 (12)
NI2—P9	2.6901 (13)	O7—P9	1.5285 (17)
NI2—P9^v	2.6901 (13)	O8—FE1	2.1166 (12)
FE3—O5^i	2.1760 (14)	O8—NI2	2.1166 (12)
FE3—O6	2.1007 (14)	O8—FE3	2.3587 (13)
FE3—O7	2.1661 (14)	O8—FE3^viii	2.0795 (15)
FE3—O7^vi	2.0227 (12)	O8—NI4	2.3588 (13)
FE3—O8	2.3587 (13)	O8—NI4^viii	2.0794 (15)
FE3—O8^iii	2.0795 (15)	O8—P9	1.5810 (17)
FE3—P9	2.8586 (15)	P9—FE1	2.6901 (13)
NI4—O5^i	2.1760 (14)	P9—NI2	2.6901 (13)
NI4—O6	2.1006 (14)	P9—FE3	2.8586 (15)
NI4—O7	2.1661 (14)	P9—NI4	2.8587 (15)
NI4—O7^vi	2.0227 (12)	P9—O5	1.5099 (15)
NI4—O8	2.3588 (13)	P9—O6^iv	1.5309 (16)
NI4—O8^iii	2.0794 (15)	P9—O7	1.5285 (17)
NI4—P9	2.8587 (15)	P9—O8	1.5810 (17)
O5^i—FE1—O5^ii	180.0	O6—NI4—O8^iii	86.18 (5)
O5^i—FE1—O6^iii	87.34 (4)	O7^vi—NI4—O8^iii	121.68 (5)
O5^i—FE1—O6^iv	92.66 (4)	FE1^vii—O5—NI2^vii	0.0
O5^i—FE1—O8	83.87 (4)	FE1^vii—O5—P9	126.90 (8)
O5^i—FE1—O8^v	96.13 (4)	NI2^vii—O5—P9	126.90 (8)
O5^ii—FE1—O6^iii	92.66 (4)	FE1^viii—O6—NI2^viii	0.0
O5^ii—FE1—O6^iv	87.34 (4)	FE1^viii—O6—FE3	121.78 (6)
O5^ii—FE1—O8	96.13 (4)	FE1^viii—O6—NI4	121.78 (6)
O5^ii—FE1—O8^v	83.87 (4)	FE1^viii—O6—P9^ix	93.98 (7)
O6^iii—FE1—O6^iv	179.9802	NI2^viii—O6—FE3	121.78 (6)
O6^iii—FE1—O8	109.91 (4)	NI2^viii—O6—NI4	121.78 (6)
O6^iii—FE1—O8^v	70.09 (4)	NI2^viii—O6—P9^ix	93.98 (7)
O6^iv—FE1—O8	70.09 (4)	FE3—O6—NI4	0.0
O6^iv—FE1—O8^v	109.91 (4)	FE3—O6—P9^ix	130.00 (8)
O8—FE1—O8^v	180.0	NI4—O6—P9^ix	130.00 (8)
O5^i—NI2—O5^ii	180.0	FE3^x—O7—NI4^x	0.0
O5^i—NI2—O6^iii	87.34 (4)	FE3^x—O7—P9	132.00 (7)
O5^i—NI2—O6^iv	92.66 (4)	NI4^x—O7—P9	132.00 (7)
O5^i—NI2—O8	83.87 (4)	FE1—O8—NI2	0.0
O5^i—NI2—O8^v	96.13 (4)	FE1—O8—FE3^viii	115.43 (5)
O5^ii—NI2—O6^iii	92.66 (4)	FE1—O8—NI4^viii	115.43 (5)
O5^ii—NI2—O6^iv	87.34 (4)	FE1—O8—P9	92.20 (8)
O5^ii—NI2—O8	96.13 (4)	NI2—O8—FE3^viii	115.43 (5)
O5^ii—NI2—O8^v	83.87 (4)	NI2—O8—NI4^viii	115.43 (5)
O6^iii—NI2—O6^iv	179.9802	NI2—O8—P9	92.20 (8)
O6^iii—NI2—O8	109.91 (4)	FE3^viii—O8—NI4^viii	0.0
O6^iii—NI2—O8^v	70.09 (4)	FE3^viii—O8—P9	124.92 (7)
O6^iv—NI2—O8	70.09 (4)	NI4^viii—O8—P9	124.92 (7)
O6^iv—NI2—O8^v	109.91 (4)	O5—P9—O6^iv	113.25 (10)
O8—NI2—O8^v	180.0	O5—P9—O7	112.42 (10)
O6—FE3—O7^vi	91.96 (5)	O5—P9—O8	112.66 (10)
O6—FE3—O8^iii	86.18 (5)	O6^iv—P9—O7	112.36 (9)
O7^vi—FE3—O8^iii	121.67 (5)	O6^iv—P9—O8	102.43 (9)
O6—NI4—O7^vi	91.96 (5)	O7—P9—O8	102.84 (8)

Symmetry codes: (i) x, y−1, z; (ii) −x+1, −y+1, −z; (iii) −x+1, y−1/2, −z+1/2; (iv) x, −y+3/2, z+1/2; (v) −x+1, −y, −z; (vi) −x, y−1/2, −z+1/2; (vii) x, y+1, z; (viii) −x+1, y+1/2, −z+1/2; (ix) x, −y+3/2, z+3/2; (x) −x, y+1/2, −z+1/2.

(62NI_phase_1)

Crystal data

Fe1.00Ni0.50O4P	c = 10.35671 (8) Å
Mr = 180.17	β = 90.8886 (4)°
Monoclinic, P21/c	V = 292.60 Å^3
a = 5.98729 (5) Å	Z = 4
b = 4.71923 (4) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
FE1	0.5	0.0	0.0	0.02056	0.2921 (22)
NI2	0.5	0.0	0.0	0.02056	0.7079 (22)
FE3	0.23621 (19)	−0.0235 (3)	0.28215 (10)	0.00916	0.8539 (11)
NI4	0.23621 (19)	−0.0235 (3)	0.28215 (10)	0.00916	0.1461 (11)
O5	0.2771 (2)	0.7475 (3)	0.10226 (14)	0.0145
O6	0.2547 (3)	0.1910 (3)	0.46042 (15)	0.01434
O7	0.0672 (2)	0.3168 (3)	0.17874 (16)	0.01504
O8	0.4698 (2)	0.2752 (3)	0.15971 (14)	0.01407
P9	0.2598 (3)	0.4265 (3)	0.09766 (16)	0.01038

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
FE1	0.016 (3)	0.027 (3)	0.018 (3)	−0.004 (3)	0.0020 (19)	−0.003 (3)
NI2	0.016 (3)	0.027 (3)	0.018 (3)	−0.004 (3)	0.0020 (19)	−0.003 (3)
FE3	0.0090 (7)	0.0092 (8)	0.0093 (8)	0.0005 (7)	0.0015 (5)	0.0003 (6)
NI4	0.0090 (7)	0.0092 (8)	0.0093 (8)	0.0005 (7)	0.0015 (5)	0.0003 (6)
O5	0.0154 (10)	0.0133 (10)	0.0148 (9)	−0.0004 (10)	0.0020 (8)	−0.0004 (9)
O6	0.0186 (9)	0.0121 (11)	0.0124 (11)	−0.0025 (9)	0.0032 (7)	0.0008 (8)
O7	0.0165 (11)	0.0150 (11)	0.0138 (10)	0.0014 (8)	0.0049 (8)	0.0036 (7)
O8	0.0170 (9)	0.0134 (10)	0.0118 (9)	0.0004 (8)	−0.0008 (7)	0.0036 (9)
P9	0.0131 (10)	0.0054 (9)	0.0126 (11)	−0.0020 (9)	0.0017 (9)	0.0087 (9)

Geometric parameters (Å, º)

FE1—O5^i	2.0898 (15)	O5—FE1^vii	2.0898 (15)
FE1—O5^ii	2.0898 (15)	O5—NI2^vii	2.0898 (15)
FE1—O6^iii	2.1055 (14)	O5—FE3^vii	2.1710 (18)
FE1—O6^iv	2.1055 (14)	O5—NI4^vii	2.1710 (18)
FE1—O8	2.1131 (15)	O5—P9	1.519 (2)
FE1—O8^v	2.1131 (15)	O6—FE1^viii	2.1055 (14)
FE1—P9	2.6810 (17)	O6—NI2^viii	2.1055 (14)
FE1—P9^v	2.6810 (17)	O6—FE3	2.1069 (18)
NI2—O5^i	2.0898 (15)	O6—NI4	2.1069 (18)
NI2—O5^ii	2.0898 (15)	O6—P9^ix	1.526 (2)
NI2—O6^iii	2.1055 (14)	O7—FE3	2.172 (2)
NI2—O6^iv	2.1055 (14)	O7—FE3^x	2.0138 (17)
NI2—O8	2.1131 (15)	O7—NI4	2.172 (2)
NI2—O8^v	2.1131 (15)	O7—NI4^x	2.0138 (17)
NI2—P9	2.6810 (17)	O7—P9	1.527 (2)
NI2—P9^v	2.6810 (17)	O8—FE1	2.1131 (15)
FE3—O5^i	2.1710 (18)	O8—NI2	2.1131 (15)
FE3—O6	2.1069 (18)	O8—FE3	2.3679 (19)
FE3—O7	2.172 (2)	O8—FE3^viii	2.0808 (19)
FE3—O7^vi	2.0138 (17)	O8—NI4	2.3679 (19)
FE3—O8	2.3679 (19)	O8—NI4^viii	2.0808 (19)
FE3—O8^iii	2.0808 (19)	O8—P9	1.575 (2)
FE3—P9	2.862 (2)	P9—FE1	2.6810 (17)
NI4—O5^i	2.1710 (18)	P9—NI2	2.6810 (17)
NI4—O6	2.1069 (18)	P9—FE3	2.862 (2)
NI4—O7	2.172 (2)	P9—NI4	2.862 (2)
NI4—O7^vi	2.0138 (17)	P9—O5	1.519 (2)
NI4—O8	2.3679 (19)	P9—O6^iv	1.526 (2)
NI4—O8^iii	2.0808 (19)	P9—O7	1.527 (2)
NI4—P9	2.862 (2)	P9—O8	1.575 (2)
O5^i—FE1—O5^ii	180.0	O6—NI4—O8^iii	86.16 (7)
O5^i—FE1—O6^iii	87.45 (6)	O7^vi—NI4—O8^iii	122.18 (7)
O5^i—FE1—O6^iv	92.55 (6)	FE1^vii—O5—NI2^vii	0.0
O5^i—FE1—O8	83.73 (6)	FE1^vii—O5—P9	126.62 (11)
O5^i—FE1—O8^v	96.27 (6)	NI2^vii—O5—P9	126.62 (11)
O5^ii—FE1—O6^iii	92.55 (6)	FE1^viii—O6—NI2^viii	0.0
O5^ii—FE1—O6^iv	87.45 (6)	FE1^viii—O6—FE3	122.03 (8)
O5^ii—FE1—O8	96.27 (6)	FE1^viii—O6—NI4	122.03 (8)
O5^ii—FE1—O8^v	83.73 (6)	FE1^viii—O6—P9^ix	93.82 (9)
O6^iii—FE1—O6^iv	179.9802	NI2^viii—O6—FE3	122.03 (8)
O6^iii—FE1—O8	109.95 (5)	NI2^viii—O6—NI4	122.03 (8)
O6^iii—FE1—O8^v	70.05 (5)	NI2^viii—O6—P9^ix	93.82 (9)
O6^iv—FE1—O8	70.05 (5)	FE3—O6—NI4	0.0
O6^iv—FE1—O8^v	109.95 (5)	FE3—O6—P9^ix	129.93 (10)
O8—FE1—O8^v	179.9657	NI4—O6—P9^ix	129.93 (10)
O5^i—NI2—O5^ii	180.0	FE3^x—O7—NI4^x	0.0
O5^i—NI2—O6^iii	87.45 (6)	FE3^x—O7—P9	132.44 (9)
O5^i—NI2—O6^iv	92.55 (6)	NI4^x—O7—P9	132.44 (9)
O5^i—NI2—O8	83.73 (6)	FE1—O8—NI2	0.0
O5^i—NI2—O8^v	96.27 (6)	FE1—O8—FE3^viii	115.15 (7)
O5^ii—NI2—O6^iii	92.55 (6)	FE1—O8—NI4^viii	115.15 (7)
O5^ii—NI2—O6^iv	87.45 (6)	FE1—O8—P9	92.10 (10)
O5^ii—NI2—O8	96.27 (6)	NI2—O8—FE3^viii	115.15 (7)
O5^ii—NI2—O8^v	83.73 (6)	NI2—O8—NI4^viii	115.15 (7)
O6^iii—NI2—O6^iv	179.9802	NI2—O8—P9	92.10 (10)
O6^iii—NI2—O8	109.95 (5)	FE3^viii—O8—NI4^viii	0.0
O6^iii—NI2—O8^v	70.05 (5)	FE3^viii—O8—P9	125.30 (10)
O6^iv—NI2—O8	70.05 (5)	NI4^viii—O8—P9	125.30 (10)
O6^iv—NI2—O8^v	109.95 (5)	O5—P9—O6^iv	113.08 (12)
O8—NI2—O8^v	179.9657	O5—P9—O7	111.87 (15)
O6—FE3—O7^vi	92.23 (7)	O5—P9—O8	112.68 (14)
O6—FE3—O8^iii	86.16 (7)	O6^iv—P9—O7	112.64 (13)
O7^vi—FE3—O8^iii	122.18 (7)	O6^iv—P9—O8	102.69 (12)
O6—NI4—O7^vi	92.23 (7)	O7—P9—O8	103.12 (10)

Symmetry codes: (i) x, y−1, z; (ii) −x+1, −y+1, −z; (iii) −x+1, y−1/2, −z+1/2; (iv) x, −y+3/2, z+1/2; (v) −x+1, −y, −z; (vi) −x, y−1/2, −z+1/2; (vii) x, y+1, z; (viii) −x+1, y+1/2, −z+1/2; (ix) x, −y+3/2, z+3/2; (x) −x, y+1/2, −z+1/2.

Fe3(PO4)2_phase_1

Crystal data

Fe3O8P2	c = 6.14402 (18) Å
Mr = 357.48	β = 99.348 (3)°
Monoclinic, P21/c	V = 601.72 Å^3
a = 8.8828 (3) Å	Z = 4
b = 11.1738 (3) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
FE1	0.9276 (9)	0.1168 (6)	0.8692 (12)	0.03344
FE2	0.7235 (9)	0.0811 (6)	0.3308 (14)	0.0464
FE3	0.3631 (8)	0.1939 (7)	0.1221 (13)	0.03901
P4	0.0946 (15)	0.1360 (11)	0.389 (2)	0.037 (3)*
P5	0.6047 (16)	0.0889 (11)	0.803 (3)	0.037 (3)*
O6	0.076 (3)	0.065 (2)	0.174 (3)	0.021 (3)*
O7	0.481 (2)	0.1806 (19)	0.826 (4)	0.021 (3)*
O8	0.9463 (19)	0.2035 (19)	0.396 (4)	0.021 (3)*
O9	0.698 (2)	0.122 (2)	0.625 (3)	0.021 (3)*
O10	0.226 (2)	0.2233 (17)	0.381 (4)	0.021 (3)*
O11	0.720 (2)	0.090 (2)	0.017 (3)	0.021 (3)*
O12	0.131 (3)	0.0600 (19)	0.598 (3)	0.021 (3)*
O13	0.530 (3)	−0.0337 (14)	0.760 (4)	0.021 (3)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
FE1	0.028 (6)	0.019 (5)	0.049 (7)	0.003 (5)	−0.010 (5)	−0.001 (5)
FE2	0.051 (8)	0.030 (6)	0.058 (8)	0.019 (5)	0.008 (6)	−0.009 (6)
FE3	0.037 (6)	0.030 (6)	0.048 (7)	0.000 (6)	0.000 (5)	0.004 (6)

Geometric parameters (Å, º)

FE1—P5	2.848 (17)	P5—O13	1.525 (2)
FE1—O6^i	2.19 (2)	O6—FE1^viii	2.19 (2)
FE1—O6^ii	2.05 (2)	O6—FE1^ii	2.05 (2)
FE1—O8^iii	2.02 (2)	O6—P4	1.526 (2)
FE1—O9	2.33 (2)	O7—FE3^iv	2.25 (2)
FE1—O11^iv	2.21 (3)	O7—FE3^iii	2.05 (2)
FE2—O8	2.39 (2)	O7—P5	1.525 (2)
FE2—O9	1.91 (2)	O8—FE1^vi	2.02 (2)
FE2—O11	1.93 (2)	O8—FE2	2.39 (2)
FE2—O12^ii	2.04 (2)	O8—P4^ix	1.525 (2)
FE2—O13^ii	2.29 (2)	O9—FE1	2.33 (2)
FE3—O7^v	2.25 (2)	O9—FE2	1.91 (2)
FE3—O7^vi	2.05 (2)	O9—P5	1.525 (2)
FE3—O10	2.18 (2)	O10—FE3	2.18 (2)
FE3—O10^vi	1.99 (2)	O10—FE3^iii	1.99 (2)
FE3—O13^ii	2.10 (2)	O10—P4	1.525 (2)
P4—O6	1.526 (2)	O11—FE1^v	2.21 (3)
P4—O8^vii	1.525 (2)	O11—FE2	1.93 (2)
P4—O10	1.525 (2)	O11—P5^v	1.525 (2)
P4—O12	1.526 (2)	O12—FE2^ii	2.04 (2)
P5—FE1	2.848 (17)	O12—P4	1.526 (2)
P5—O7	1.525 (2)	O13—FE2^ii	2.29 (2)
P5—O9	1.525 (2)	O13—FE3^ii	2.10 (2)
P5—O11^iv	1.525 (2)	O13—P5	1.525 (2)
O6^ii—FE1—O8^iii	175.0 (9)	O7—P5—O11^iv	107.9 (16)
O9—FE2—O11	161.4 (11)	O7—P5—O13	108.7 (15)
O9—FE2—O12^ii	98.5 (10)	O9—P5—O11^iv	104.5 (16)
O11—FE2—O12^ii	99.5 (10)	O9—P5—O13	111.4 (16)
O7^vi—FE3—O10^vi	109.1 (9)	O11^iv—P5—O13	111.5 (17)
O7^vi—FE3—O13^ii	102.5 (9)	FE1^ii—O6—P4	128.4 (15)
O10^vi—FE3—O13^ii	147.4 (9)	FE3^iii—O7—P5	135.0 (16)
O6—P4—O8^vii	108.0 (15)	FE1^vi—O8—P4^ix	123.4 (14)
O6—P4—O10	106.0 (16)	FE2—O9—P5	141.5 (16)
O6—P4—O12	114.7 (15)	FE3^iii—O10—P4	130.7 (16)
O8^vii—P4—O10	110.6 (14)	FE2—O11—P5^v	139.6 (17)
O8^vii—P4—O12	108.6 (16)	FE2^ii—O12—P4	130.7 (15)
O10—P4—O12	108.9 (15)	FE3^ii—O13—P5	123.2 (15)
O7—P5—O9	112.8 (16)

Symmetry codes: (i) x+1, y, z+1; (ii) −x+1, −y, −z+1; (iii) x, −y+3/2, z+3/2; (iv) x, y, z+1; (v) x, y, z−1; (vi) x, −y+3/2, z+1/2; (vii) x−1, y, z; (viii) x−1, y, z−1; (ix) x+1, y, z.

(ISO191A_phase_2)

Crystal data

Fe2O7P2	α = 90.43 (4)°
Mr = 285.64	β = 103.80 (4)°
Triclinic, C1	γ = 92.49 (6)°
a = 6.643 (3) Å	V = 244.66 Å^3
b = 8.447 (5) Å	Z = 2
c = 4.495 (3) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
FE1	0.0096	0.3101	0.483	0.015*
P2	0.7884	−0.0006	0.0899	0.015*
O3	0.0	0.0	0.0	0.015*
O4	0.3748	0.0047	0.2148	0.015*
O5	0.7892	0.1487	0.2741	0.015*
O6	0.2745	0.3527	0.2782	0.015*

(MULTI_phase_1)

Crystal data

Fe1.00Ni0.50O4P	c = 10.35657 (4) Å
Mr = 180.17	β = 90.8909 (2)°
Monoclinic, P21/c	V = 292.62 Å^3
a = 5.98701 (2) Å	Z = 4
b = 4.719891 (17) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
FE1	0.5	0.0	0.0	0.0096	0.2903 (14)
NI2	0.5	0.0	0.0	0.0096	0.7097 (14)
FE3	0.23720 (10)	−0.02072 (13)	0.28149 (6)	0.00865	0.8548 (7)
NI4	0.23720 (10)	−0.02072 (13)	0.28149 (6)	0.00865	0.1452 (7)
O5	0.27786 (15)	0.74901 (18)	0.10184 (9)	0.01102
O6	0.25519 (16)	0.19028 (19)	0.46003 (9)	0.01087
O7	0.06694 (14)	0.31659 (18)	0.17867 (9)	0.01059
O8	0.46974 (15)	0.27493 (19)	0.15953 (9)	0.00951
P9	0.25937 (17)	0.4263 (2)	0.09766 (9)	0.0079

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
FE1	0.0121 (5)	0.0071 (5)	0.0096 (5)	0.0011 (5)	0.0013 (4)	0.0006 (5)
NI2	0.0121 (5)	0.0071 (5)	0.0096 (5)	0.0011 (5)	0.0013 (4)	0.0006 (5)
FE3	0.0082 (3)	0.0098 (4)	0.0080 (3)	0.0008 (3)	0.0013 (3)	0.0005 (3)
NI4	0.0082 (3)	0.0098 (4)	0.0080 (3)	0.0008 (3)	0.0013 (3)	0.0005 (3)
O5	0.0147 (6)	0.0071 (5)	0.0113 (5)	−0.0003 (5)	0.0013 (4)	0.0000 (5)
O6	0.0144 (5)	0.0102 (6)	0.0080 (5)	−0.0003 (4)	0.0004 (4)	0.0001 (4)
O7	0.0095 (6)	0.0095 (5)	0.0129 (5)	0.0003 (4)	0.0056 (4)	0.0030 (4)
O8	0.0092 (5)	0.0092 (5)	0.0101 (5)	0.0008 (4)	−0.0006 (4)	0.0020 (4)
P9	0.0104 (5)	0.0052 (5)	0.0081 (6)	−0.0003 (4)	0.0007 (4)	0.0012 (5)

Geometric parameters (Å, º)

FE1—O5^i	2.0804 (9)	O5—FE1^vii	2.0804 (9)
FE1—O5^ii	2.0804 (9)	O5—NI2^vii	2.0804 (9)
FE1—O6^iii	2.1066 (9)	O5—FE3^vii	2.1717 (11)
FE1—O6^iv	2.1066 (9)	O5—NI4^vii	2.1718 (11)
FE1—O8	2.1109 (9)	O5—P9	1.5276 (14)
FE1—O8^v	2.1109 (9)	O6—FE1^viii	2.1066 (9)
FE1—P9	2.6819 (10)	O6—NI2^viii	2.1066 (9)
FE1—P9^v	2.6819 (10)	O6—FE3	2.1015 (11)
NI2—O5^i	2.0804 (9)	O6—NI4	2.1015 (11)
NI2—O5^ii	2.0804 (9)	O6—P9^ix	1.5277 (14)
NI2—O6^iii	2.1066 (9)	O7—FE3	2.1619 (11)
NI2—O6^iv	2.1066 (9)	O7—FE3^x	2.0246 (10)
NI2—O8	2.1109 (9)	O7—NI4	2.1619 (11)
NI2—O8^v	2.1109 (9)	O7—NI4^x	2.0246 (10)
NI2—P9	2.6819 (10)	O7—P9	1.5263 (14)
NI2—P9^v	2.6819 (10)	O8—FE1	2.1109 (9)
FE3—O5^i	2.1717 (11)	O8—NI2	2.1109 (9)
FE3—O6	2.1015 (11)	O8—FE3	2.3528 (11)
FE3—O7	2.1619 (11)	O8—FE3^viii	2.0853 (11)
FE3—O7^vi	2.0246 (10)	O8—NI4	2.3528 (11)
FE3—O8	2.3528 (11)	O8—NI4^viii	2.0853 (11)
FE3—O8^iii	2.0853 (11)	O8—P9	1.5756 (14)
FE3—P9	2.8465 (11)	P9—FE1	2.6819 (10)
NI4—O5^i	2.1718 (11)	P9—NI2	2.6819 (10)
NI4—O6	2.1015 (11)	P9—FE3	2.8465 (11)
NI4—O7	2.1619 (11)	P9—NI4	2.8465 (11)
NI4—O7^vi	2.0246 (10)	P9—O5	1.5276 (14)
NI4—O8	2.3528 (11)	P9—O6^iv	1.5277 (14)
NI4—O8^iii	2.0853 (11)	P9—O7	1.5263 (14)
NI4—P9	2.8465 (11)	P9—O8	1.5756 (14)
O5^i—FE1—O5^ii	180.0	O6—NI4—O8^iii	85.99 (4)
O5^i—FE1—O6^iii	87.34 (4)	O7^vi—NI4—O8^iii	121.35 (4)
O5^i—FE1—O6^iv	92.66 (4)	FE1^vii—O5—NI2^vii	0.0
O5^i—FE1—O8	83.68 (4)	FE1^vii—O5—P9	126.87 (7)
O5^i—FE1—O8^v	96.32 (4)	NI2^vii—O5—P9	126.87 (7)
O5^ii—FE1—O6^iii	92.66 (4)	FE1^viii—O6—NI2^viii	0.0
O5^ii—FE1—O6^iv	87.34 (4)	FE1^viii—O6—FE3	121.85 (5)
O5^ii—FE1—O8	96.32 (4)	FE1^viii—O6—NI4	121.85 (5)
O5^ii—FE1—O8^v	83.68 (4)	FE1^viii—O6—P9^ix	93.75 (5)
O6^iii—FE1—O6^iv	180.0	NI2^viii—O6—FE3	121.85 (5)
O6^iii—FE1—O8	109.92 (3)	NI2^viii—O6—NI4	121.85 (5)
O6^iii—FE1—O8^v	70.08 (3)	NI2^viii—O6—P9^ix	93.75 (5)
O6^iv—FE1—O8	70.08 (3)	FE3—O6—NI4	0.0
O6^iv—FE1—O8^v	109.92 (3)	FE3—O6—P9^ix	130.54 (6)
O8—FE1—O8^v	180.0	NI4—O6—P9^ix	130.54 (6)
O5^i—NI2—O5^ii	180.0	FE3^x—O7—NI4^x	0.0
O5^i—NI2—O6^iii	87.34 (4)	FE3^x—O7—P9	132.24 (6)
O5^i—NI2—O6^iv	92.66 (4)	NI4^x—O7—P9	132.24 (6)
O5^i—NI2—O8	83.68 (4)	FE1—O8—NI2	0.0
O5^i—NI2—O8^v	96.32 (4)	FE1—O8—FE3^viii	115.56 (4)
O5^ii—NI2—O6^iii	92.66 (4)	FE1—O8—NI4^viii	115.56 (4)
O5^ii—NI2—O6^iv	87.34 (4)	FE1—O8—P9	92.19 (5)
O5^ii—NI2—O8	96.32 (4)	NI2—O8—FE3^viii	115.56 (4)
O5^ii—NI2—O8^v	83.68 (4)	NI2—O8—NI4^viii	115.56 (4)
O6^iii—NI2—O6^iv	180.0	NI2—O8—P9	92.19 (5)
O6^iii—NI2—O8	109.92 (3)	FE3^viii—O8—NI4^viii	0.0
O6^iii—NI2—O8^v	70.08 (3)	FE3^viii—O8—P9	124.96 (6)
O6^iv—NI2—O8	70.08 (3)	NI4^viii—O8—P9	124.96 (6)
O6^iv—NI2—O8^v	109.92 (3)	O5—P9—O6^iv	112.69 (7)
O8—NI2—O8^v	180.0	O5—P9—O7	112.19 (8)
O6—FE3—O7^vi	91.97 (4)	O5—P9—O8	112.55 (8)
O6—FE3—O8^iii	85.99 (4)	O6^iv—P9—O7	112.89 (7)
O7^vi—FE3—O8^iii	121.35 (4)	O6^iv—P9—O8	102.56 (7)
O6—NI4—O7^vi	91.97 (4)	O7—P9—O8	103.18 (7)

Symmetry codes: (i) x, y−1, z; (ii) −x+1, −y+1, −z; (iii) −x+1, y−1/2, −z+1/2; (iv) x, −y+3/2, z+1/2; (v) −x+1, −y, −z; (vi) −x, y−1/2, −z+1/2; (vii) x, y+1, z; (viii) −x+1, y+1/2, −z+1/2; (ix) x, −y+3/2, z+3/2; (x) −x, y+1/2, −z+1/2.

(MULTI_phase_2)

Crystal data

Co0.50Fe1.00O4P	c = 10.35657 (4) Å
Mr = 180.28	β = 90.8909 (2)°
Monoclinic, P21/c	V = 292.62 Å^3
a = 5.98701 (2) Å	Z = 4
b = 4.719891 (17) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
FE1	0.5	0.0	0.0	0.0096	0.2903 (14)
NI2	0.5	0.0	0.0	0.0096	0.7097 (14)
FE3	0.23720 (10)	−0.02072 (13)	0.28149 (6)	0.00865	0.8548 (7)
NI4	0.23720 (10)	−0.02072 (13)	0.28149 (6)	0.00865	0.1452 (7)
O5	0.27786 (15)	0.74901 (18)	0.10184 (9)	0.01102
O6	0.25519 (16)	0.19028 (19)	0.46003 (9)	0.01087
O7	0.06694 (14)	0.31659 (18)	0.17867 (9)	0.01059
O8	0.46974 (15)	0.27493 (19)	0.15953 (9)	0.00951
P9	0.25937 (17)	0.4263 (2)	0.09766 (9)	0.0079

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
FE1	0.0121 (5)	0.0071 (5)	0.0096 (5)	0.0011 (5)	0.0013 (4)	0.0006 (5)
NI2	0.0121 (5)	0.0071 (5)	0.0096 (5)	0.0011 (5)	0.0013 (4)	0.0006 (5)
FE3	0.0082 (3)	0.0098 (4)	0.0080 (3)	0.0008 (3)	0.0013 (3)	0.0005 (3)
NI4	0.0082 (3)	0.0098 (4)	0.0080 (3)	0.0008 (3)	0.0013 (3)	0.0005 (3)
O5	0.0147 (6)	0.0071 (5)	0.0113 (5)	−0.0003 (5)	0.0013 (4)	0.0000 (5)
O6	0.0144 (5)	0.0102 (6)	0.0080 (5)	−0.0003 (4)	0.0004 (4)	0.0001 (4)
O7	0.0095 (6)	0.0095 (5)	0.0129 (5)	0.0003 (4)	0.0056 (4)	0.0030 (4)
O8	0.0092 (5)	0.0092 (5)	0.0101 (5)	0.0008 (4)	−0.0006 (4)	0.0020 (4)
P9	0.0104 (5)	0.0052 (5)	0.0081 (6)	−0.0003 (4)	0.0007 (4)	0.0012 (5)

(MULTI_phase_3)

Crystal data

Cu0.50Fe1.00O4P	c = 10.35657 (4) Å
Mr = 182.59	β = 90.8909 (2)°
Monoclinic, P21/c	V = 292.62 Å^3
a = 5.98701 (2) Å	Z = 4
b = 4.719891 (17) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
FE1	0.5	0.0	0.0	0.0096	0.2903 (14)
NI2	0.5	0.0	0.0	0.0096	0.7097 (14)
FE3	0.23720 (10)	−0.02072 (13)	0.28149 (6)	0.00865	0.8548 (7)
NI4	0.23720 (10)	−0.02072 (13)	0.28149 (6)	0.00865	0.1452 (7)
O5	0.27786 (15)	0.74901 (18)	0.10184 (9)	0.01102
O6	0.25519 (16)	0.19028 (19)	0.46003 (9)	0.01087
O7	0.06694 (14)	0.31659 (18)	0.17867 (9)	0.01059
O8	0.46974 (15)	0.27493 (19)	0.15953 (9)	0.00951
P9	0.25937 (17)	0.4263 (2)	0.09766 (9)	0.0079

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
FE1	0.0121 (5)	0.0071 (5)	0.0096 (5)	0.0011 (5)	0.0013 (4)	0.0006 (5)
NI2	0.0121 (5)	0.0071 (5)	0.0096 (5)	0.0011 (5)	0.0013 (4)	0.0006 (5)
FE3	0.0082 (3)	0.0098 (4)	0.0080 (3)	0.0008 (3)	0.0013 (3)	0.0005 (3)
NI4	0.0082 (3)	0.0098 (4)	0.0080 (3)	0.0008 (3)	0.0013 (3)	0.0005 (3)
O5	0.0147 (6)	0.0071 (5)	0.0113 (5)	−0.0003 (5)	0.0013 (4)	0.0000 (5)
O6	0.0144 (5)	0.0102 (6)	0.0080 (5)	−0.0003 (4)	0.0004 (4)	0.0001 (4)
O7	0.0095 (6)	0.0095 (5)	0.0129 (5)	0.0003 (4)	0.0056 (4)	0.0030 (4)
O8	0.0092 (5)	0.0092 (5)	0.0101 (5)	0.0008 (4)	−0.0006 (4)	0.0020 (4)
P9	0.0104 (5)	0.0052 (5)	0.0081 (6)	−0.0003 (4)	0.0007 (4)	0.0012 (5)

(ISO192C_phase_1)

Crystal data

Ni3O8P2	c = 10.1098 (3) Å
Mr = 366.07	β = 91.1288 (16)°
Monoclinic, P21/c	V = 276.88 Å^3
a = 5.83104 (15) Å	Z = 2
b = 4.69778 (13) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
NI1	0.5	0.0	0.0	0.01862
NI2	0.2382 (4)	−0.0133 (7)	0.2749 (3)	0.01382
P3	0.2396 (9)	0.4232 (10)	0.0945 (5)	0.0154 (17)*
O4	0.2464 (18)	0.7483 (11)	0.0971 (11)	0.0089 (16)*
O5	0.2403 (19)	0.1996 (19)	0.4541 (6)	0.0089 (16)*
O6	0.0410 (13)	0.296 (2)	0.1715 (9)	0.0089 (16)*
O7	0.4489 (13)	0.2705 (19)	0.1538 (10)	0.0089 (16)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
NI1	0.041 (4)	0.007 (3)	0.009 (3)	0.006 (4)	0.006 (3)	0.006 (3)
NI2	0.008 (2)	0.018 (3)	0.016 (3)	−0.006 (2)	0.0009 (16)	−0.006 (3)

Geometric parameters (Å, º)

NI1—P3	2.689 (5)	P3—O4	1.528 (3)
NI1—P3^i	2.689 (5)	P3—O5^v	1.532 (3)
NI1—O4^ii	2.146 (9)	P3—O6	1.530 (3)
NI1—O4^iii	2.146 (9)	P3—O7	1.528 (3)
NI1—O5^iv	2.115 (10)	O4—NI1^vii	2.146 (9)
NI1—O5^v	2.115 (10)	O4—NI2^vii	2.119 (10)
NI1—O7	2.034 (10)	O4—P3	1.528 (3)
NI1—O7^i	2.034 (10)	O5—NI1^viii	2.115 (10)
NI2—P3	2.744 (5)	O5—NI2	2.069 (8)
NI2—O4^ii	2.119 (10)	O5—P3^ix	1.532 (3)
NI2—O5	2.069 (8)	O6—NI2	2.116 (10)
NI2—O6	2.116 (10)	O6—NI2^x	1.945 (9)
NI2—O6^vi	1.945 (9)	O6—P3	1.530 (3)
NI2—O7	2.201 (10)	O7—NI1	2.034 (10)
NI2—O7^iv	2.197 (9)	O7—NI2	2.201 (10)
P3—NI1	2.689 (5)	O7—NI2^viii	2.197 (9)
P3—NI2	2.744 (5)	O7—P3	1.528 (3)
O5^iv—NI1—O5^v	179.972	O4—P3—O6	113.7 (7)
O5^iv—NI1—O7	111.4 (2)	O4—P3—O7	116.3 (7)
O5^iv—NI1—O7^i	68.6 (2)	O5^v—P3—O6	109.9 (6)
O5^v—NI1—O7	68.6 (2)	O5^v—P3—O7	99.8 (6)
O5^v—NI1—O7^i	111.4 (2)	O6—P3—O7	102.9 (6)
O7—NI1—O7^i	180.0	NI2^vii—O4—P3	122.8 (6)
O4^ii—NI2—O5	176.6 (3)	NI1^viii—O5—NI2	120.4 (4)
O4^ii—NI2—O6	88.0 (4)	NI1^viii—O5—P3^ix	93.6 (5)
O4^ii—NI2—O6^vi	91.5 (4)	NI2—O5—P3^ix	129.0 (6)
O5—NI2—O6	95.4 (4)	NI2—O6—NI2^x	128.9 (4)
O5—NI2—O6^vi	88.2 (4)	NI2—O6—P3	96.3 (5)
O6—NI2—O6^vi	90.3 (3)	NI2^x—O6—P3	127.4 (6)
O4—P3—O5^v	113.0 (7)	NI1—O7—P3	97.0 (5)

Symmetry codes: (i) −x+1, −y, −z; (ii) x, y−1, z; (iii) −x+1, −y+1, −z; (iv) −x+1, y−1/2, −z+1/2; (v) x, −y+3/2, z+1/2; (vi) −x, y−1/2, −z+1/2; (vii) x, y+1, z; (viii) −x+1, y+1/2, −z+1/2; (ix) x, −y+3/2, z+3/2; (x) −x, y+1/2, −z+1/2.

(ISO192C_phase_2)

Crystal data

Ni2O7P2	c = 8.9714 (11) Å
Mr = 291.36	β = 104.949 (9)°
Monoclinic, B121/c1	V = 942.45 Å^3
a = 13.1459 (16) Å	Z = 8
b = 8.2711 (11) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
NI1	0.35256	0.07453	0.02695	0.027 (6)*
NI2	0.11614	0.92621	−0.00027	0.027 (6)*
P3	0.47678	0.7379	0.20844	0.026 (9)*
P4	0.21345	0.27121	0.19917	0.026 (9)*
O5	0.11981	0.3445	0.25335	−0.002 (9)*
O6	0.19421	0.71279	0.15698	−0.002 (9)*
O7	0.43667	0.27553	0.1447	−0.002 (9)*
O8	0.20975	0.11397	0.1072	−0.002 (9)*
O9	0.50919	0.60492	0.11089	−0.002 (9)*
O10	0.25663	0.40816	0.11784	−0.002 (9)*
O11	0.43818	0.89372	0.11792	−0.002 (9)*

(NAT_phase_1)

Crystal data

Fe1.00Ni0.50O4P	c = 10.369383 (18) Å
Mr = 180.17	β = 90.8910 (1)°
Monoclinic, P21/c	V = 293.66 Å^3
a = 5.994351 (10) Å	Z = 4
b = 4.724935 (9) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
FE1	0.5	0.0	0.0	0.01042	0.257 (14)
NI2	0.5	0.0	0.0	0.01042	0.743 (14)
FE3	0.237381 (31	−0.02058 (5)	0.280994 (23	0.01084	0.871 (7)
NI4	0.237381 (31	−0.02058 (5)	0.280998 (23	0.01084	0.129 (7)
O5	0.27781 (6)	0.74823 (9)	0.10252 (4)	0.01558
O6	0.25542 (7)	0.19207 (8)	0.46020 (4)	0.01418
O7	0.06751 (6)	0.31584 (8)	0.17846 (4)	0.01454
O8	0.47010 (7)	0.27457 (9)	0.15950 (4)	0.01348
P9	0.25969 (7)	0.42521 (10)	0.09724 (5)	0.01281

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
FE1	0.0143 (3)	0.0061 (3)	0.0108 (3)	0.0023 (2)	0.00020 (18)	0.0012 (2)
NI2	0.0143 (3)	0.0061 (3)	0.0108 (3)	0.0023 (2)	0.00020 (18)	0.0012 (2)
FE3	0.0104 (3)	0.0110 (3)	0.0111 (2)	−0.00040 (15)	−0.00006 (13)	−0.00225 (16)
NI4	0.0104 (3)	0.0110 (3)	0.0111 (2)	−0.00040 (15)	−0.00006 (13)	−0.00225 (16)
O5	0.0158 (3)	0.0187 (4)	0.0123 (4)	−0.0015 (3)	0.0010 (2)	−0.0023 (2)
O6	0.0178 (3)	0.0161 (3)	0.0087 (4)	−0.0025 (2)	0.0003 (2)	−0.0008 (2)
O7	0.0104 (4)	0.0169 (3)	0.0164 (3)	0.0023 (2)	0.0022 (2)	0.0032 (3)
O8	0.0156 (3)	0.0092 (4)	0.0156 (3)	0.0016 (3)	−0.0019 (2)	0.0027 (3)
P9	0.0151 (4)	0.0119 (4)	0.0116 (4)	−0.0028 (3)	0.0037 (3)	−0.0004 (3)

Geometric parameters (Å, º)

FE1—O5^i	2.0889 (4)	O5—FE1^vii	2.0889 (4)
FE1—O5^ii	2.0889 (4)	O5—NI2^vii	2.0889 (4)
FE1—O6^iii	2.1019 (4)	O5—FE3^vii	2.1658 (5)
FE1—O6^iv	2.1019 (4)	O5—NI4^vii	2.1659 (5)
FE1—O8	2.1118 (5)	O5—P9	1.5310 (6)
FE1—O8^v	2.1118 (5)	O6—FE1^viii	2.1019 (4)
FE1—P9	2.6783 (5)	O6—NI2^viii	2.1019 (4)
FE1—P9^v	2.6783 (5)	O6—FE3	2.1138 (5)
NI2—O5^i	2.0889 (4)	O6—NI4	2.1138 (5)
NI2—O5^ii	2.0889 (4)	O6—P9^ix	1.5250 (5)
NI2—O6^iii	2.1019 (4)	O7—FE3	2.1587 (5)
NI2—O6^iv	2.1019 (4)	O7—FE3^x	2.0343 (4)
NI2—O8	2.1118 (5)	O7—NI4	2.1588 (5)
NI2—O8^v	2.1118 (5)	O7—NI4^x	2.0343 (4)
NI2—P9	2.6783 (5)	O7—P9	1.5277 (6)
NI2—P9^v	2.6783 (5)	O8—FE1	2.1118 (5)
FE3—O5^i	2.1658 (5)	O8—NI2	2.1118 (5)
FE3—O6	2.1138 (5)	O8—FE3	2.3521 (4)
FE3—O7	2.1587 (5)	O8—FE3^viii	2.0877 (5)
FE3—O7^vi	2.0343 (4)	O8—NI4	2.3522 (4)
FE3—O8	2.3521 (4)	O8—NI4^viii	2.0877 (5)
FE3—O8^iii	2.0877 (5)	O8—P9	1.5777 (6)
FE3—P9	2.8449 (6)	P9—FE1	2.6783 (5)
NI4—O5^i	2.1659 (5)	P9—NI2	2.6783 (5)
NI4—O6	2.1138 (5)	P9—FE3	2.8449 (6)
NI4—O7	2.1588 (5)	P9—NI4	2.8449 (6)
NI4—O7^vi	2.0343 (4)	P9—O5	1.5310 (6)
NI4—O8	2.3522 (4)	P9—O6^iv	1.5250 (5)
NI4—O8^iii	2.0877 (5)	P9—O7	1.5277 (6)
NI4—P9	2.8449 (6)	P9—O8	1.5777 (6)
O5^i—FE1—O5^ii	180.0	O6—NI4—O8^iii	85.947 (18)
O5^i—FE1—O6^iii	87.375 (15)	O7^vi—NI4—O8^iii	121.059 (18)
O5^i—FE1—O6^iv	92.625 (15)	FE1^vii—O5—NI2^vii	0.0
O5^i—FE1—O8	83.611 (16)	FE1^vii—O5—P9	126.51 (3)
O5^i—FE1—O8^v	96.389 (16)	NI2^vii—O5—P9	126.51 (3)
O5^ii—FE1—O6^iii	92.625 (15)	FE1^viii—O6—NI2^viii	0.0
O5^ii—FE1—O6^iv	87.375 (15)	FE1^viii—O6—FE3	121.84 (2)
O5^ii—FE1—O8	96.389 (16)	FE1^viii—O6—NI4	121.84 (2)
O5^ii—FE1—O8^v	83.611 (16)	FE1^viii—O6—P9^ix	93.84 (3)
O6^iii—FE1—O6^iv	180.0	NI2^viii—O6—FE3	121.84 (2)
O6^iii—FE1—O8	109.810 (14)	NI2^viii—O6—NI4	121.84 (2)
O6^iii—FE1—O8^v	70.190 (14)	NI2^viii—O6—P9^ix	93.84 (3)
O6^iv—FE1—O8	70.190 (14)	FE3—O6—NI4	0.0
O6^iv—FE1—O8^v	109.810 (14)	FE3—O6—P9^ix	130.26 (3)
O8—FE1—O8^v	179.972	NI4—O6—P9^ix	130.26 (3)
O5^i—NI2—O5^ii	180.0	FE3—O7—FE3^x	126.61 (2)
O5^i—NI2—O6^iii	87.375 (15)	FE3—O7—NI4^x	126.61 (2)
O5^i—NI2—O6^iv	92.625 (15)	FE3—O7—P9	99.59 (3)
O5^i—NI2—O8	83.611 (16)	FE3^x—O7—NI4^x	0.0
O5^i—NI2—O8^v	96.389 (16)	FE3^x—O7—P9	132.30 (3)
O5^ii—NI2—O6^iii	92.625 (15)	NI4^x—O7—P9	132.30 (3)
O5^ii—NI2—O6^iv	87.375 (15)	FE1—O8—NI2	0.0
O5^ii—NI2—O8	96.389 (16)	FE1—O8—FE3^viii	115.797 (18)
O5^ii—NI2—O8^v	83.611 (16)	FE1—O8—NI4^viii	115.796 (18)
O6^iii—NI2—O6^iv	180.0	FE1—O8—P9	91.93 (3)
O6^iii—NI2—O8	109.810 (14)	NI2—O8—FE3^viii	115.797 (18)
O6^iii—NI2—O8^v	70.190 (14)	NI2—O8—NI4^viii	115.796 (18)
O6^iv—NI2—O8	70.190 (14)	NI2—O8—P9	91.93 (3)
O6^iv—NI2—O8^v	109.810 (14)	FE3^viii—O8—NI4^viii	0.0
O8—NI2—O8^v	179.972	FE3^viii—O8—P9	125.05 (3)
O6—FE3—O7	95.754 (17)	NI4^viii—O8—P9	125.05 (3)
O6—FE3—O7^vi	91.878 (17)	O5—P9—O6^iv	113.31 (4)
O6—FE3—O8^iii	85.946 (18)	O5—P9—O7	111.79 (4)
O7—FE3—O7^vi	87.887 (13)	O5—P9—O8	112.29 (4)
O7—FE3—O8^iii	150.988 (17)	O6^iv—P9—O7	112.89 (3)
O7^vi—FE3—O8^iii	121.058 (18)	O6^iv—P9—O8	102.66 (3)
O6—NI4—O7^vi	91.879 (17)	O7—P9—O8	103.10 (3)

Symmetry codes: (i) x, y−1, z; (ii) −x+1, −y+1, −z; (iii) −x+1, y−1/2, −z+1/2; (iv) x, −y+3/2, z+1/2; (v) −x+1, −y, −z; (vi) −x, y−1/2, −z+1/2; (vii) x, y+1, z; (viii) −x+1, y+1/2, −z+1/2; (ix) x, −y+3/2, z+3/2; (x) −x, y+1/2, −z+1/2.