research papers
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 . 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
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768109013901/hw5003sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768109013901/hw5003Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768109013901/hw5003IIsup3.hkl |
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).
(I) top
Crystal data top
H3ClCu2O3 | Z = 8 |
Mr = 213.6 | F(000) = 816 |
Triclinic, P1 | Dx = 3.722 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.1646 (9) Å | Cell parameters from 47586 reflections |
b = 9.2029 (8) Å | θ = 2–35° |
c = 9.2102 (8) Å | µ = 11.69 mm−1 |
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 tube | 4581 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.045 |
φ scans, and ω scans with κ offsets | θmax = 35°, θmin = 2.2° |
Absorption correction: gaussian (Jana2000; Petricek, Dusek & Palatinus, 2000) | h = −14→14 |
Tmin = 0.148, Tmax = 0.708 | k = −14→14 |
47586 measured reflections | l = −14→14 |
Refinement top
Refinement on F2 | 1 constraint |
R[F2 > 2σ(F2)] = 0.041 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.191 | Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.01I2) |
S = 1.33 | (Δ/σ)max = −0.002 |
6622 reflections | Δρmax = 0.80 e Å−3 |
262 parameters | Δρmin = −1.49 e Å−3 |
24 restraints |
Crystal data top
H3ClCu2O3 | γ = 96.507 (2)° |
Mr = 213.6 | V = 761.97 (12) Å3 |
Triclinic, P1 | Z = 8 |
a = 9.1646 (9) Å | Mo Kα radiation |
b = 9.2029 (8) Å | µ = 11.69 mm−1 |
c = 9.2102 (8) Å | T = 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 = 0.708 | Rint = 0.045 |
47586 measured reflections |
Refinement top
R[F2 > 2σ(F2)] = 0.041 | 24 restraints |
wR(F2) = 0.191 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.33 | Δρmax = 0.80 e Å−3 |
6622 reflections | Δρmin = −1.49 e Å−3 |
262 parameters |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Cu1a | 0.5 | 0.5 | 0.5 | 0.0106 (3) | |
Cu2a | 0.5 | 0 | 0 | 0.0157 (4) | |
Cu2b | 0 | 0 | 0.5 | 0.0109 (3) | |
Cu2c | 0 | 0.5 | 0 | 0.0139 (4) | |
Cu3a | 0.74935 (8) | 0.24039 (8) | 1.00270 (8) | 0.0141 (3) | |
Cu3b | 0.25112 (13) | 0.00186 (9) | 0.73928 (8) | 0.0131 (2) | |
Cu3c | 1.00059 (9) | 0.75035 (15) | 0.24784 (8) | 0.0132 (3) | |
Cu4a | 0.49964 (9) | 0.24961 (15) | 0.25234 (9) | 0.0129 (3) | |
Cu4b | 0.24664 (8) | 0.26012 (8) | 0.49839 (6) | 0.0142 (3) | |
Cu4c | 0.25123 (12) | 0.50173 (9) | 0.23909 (8) | 0.0133 (2) | |
Cl1a | 0.19369 (17) | 0.19294 (19) | 0.19482 (18) | 0.0178 (5) | |
Cl2a | 0.80723 (17) | 0.30762 (19) | 0.3036 (2) | 0.0181 (5) | |
Cl2b | 0.30698 (16) | 0.30354 (18) | 0.80826 (17) | 0.0170 (5) | |
Cl2c | 0.30599 (16) | 0.80371 (18) | 0.30886 (19) | 0.0170 (5) | |
O1a | 0.5493 (5) | 0.0500 (6) | 0.2625 (5) | 0.0176 (13) | |
O1b | 0.0450 (6) | 0.2530 (7) | 0.5510 (5) | 0.0193 (14) | |
O1c | 0.2277 (5) | 0.5463 (6) | 0.0337 (5) | 0.0203 (14) | |
O2a | 0.9511 (6) | 0.2456 (7) | 0.9534 (6) | 0.0213 (14) | |
O2b | 0.2778 (5) | 0.9716 (5) | 0.9505 (5) | 0.0125 (11) | |
O2c | 0.9614 (5) | 0.9606 (6) | 0.2782 (6) | 0.0166 (13) | |
O3a | 0.5387 (6) | 0.2200 (6) | 0.0402 (6) | 0.0166 (13) | |
O3b | 0.2221 (5) | 0.0445 (5) | 0.5317 (5) | 0.0162 (12) | |
O3c | 0.0393 (5) | 0.5395 (6) | 0.2168 (5) | 0.0119 (11) | |
O4a | 0.4536 (5) | 0.4515 (6) | 0.2475 (6) | 0.0192 (14) | |
O4b | 0.4577 (6) | 0.2804 (6) | 0.4622 (6) | 0.0162 (13) | |
O4c | 0.2722 (5) | 0.4698 (5) | 0.4500 (5) | 0.0125 (11) | |
H4b | 0.510 (8) | 0.214 (7) | 0.524 (7) | 0.048 (10)* | |
H4a | 0.537 (6) | 0.531 (7) | 0.285 (6) | 0.048 (10)* | |
H4c | 0.231 (9) | 0.549 (6) | 0.502 (7) | 0.048 (10)* | |
H3a | 0.462 (8) | 0.266 (9) | −0.013 (7) | 0.048 (10)* | |
H1a | 0.497 (6) | −0.021 (6) | 0.320 (6) | 0.048 (10)* | |
H2b | 0.246 (11) | 1.069 (6) | 0.996 (7) | 0.048 (10)* | |
H2a | 1.040 (7) | 0.211 (10) | 1.001 (7) | 0.048 (10)* | |
H3c | −0.036 (6) | 0.458 (6) | 0.203 (7) | 0.048 (10)* | |
H1c | 0.246 (10) | 0.440 (4) | 0.006 (6) | 0.048 (10)* | |
H3b | 0.285 (7) | −0.012 (6) | 0.471 (7) | 0.048 (10)* | |
H2c | 1.062 (5) | 1.020 (7) | 0.286 (7) | 0.048 (10)* | |
H1b | −0.012 (8) | 0.315 (6) | 0.494 (7) | 0.048 (10)* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1a | 0.0098 (5) | 0.0099 (6) | 0.0137 (6) | 0.0058 (4) | 0.0023 (5) | 0.0032 (4) |
Cu2a | 0.0139 (5) | 0.0138 (7) | 0.0176 (7) | 0.0007 (5) | −0.0025 (7) | −0.0005 (5) |
Cu2b | 0.0075 (4) | 0.0153 (6) | 0.0117 (6) | 0.0060 (4) | 0.0013 (4) | 0.0048 (4) |
Cu2c | 0.0110 (5) | 0.0133 (6) | 0.0146 (7) | −0.0037 (5) | −0.0030 (5) | −0.0015 (4) |
Cu3a | 0.0134 (4) | 0.0163 (4) | 0.0145 (5) | 0.0052 (3) | 0.0032 (3) | 0.0055 (3) |
Cu3b | 0.0100 (3) | 0.0168 (5) | 0.0123 (3) | 0.0040 (3) | −0.0028 (3) | 0.0028 (3) |
Cu3c | 0.0141 (3) | 0.0171 (5) | 0.0096 (4) | 0.0048 (3) | 0.0038 (3) | 0.0021 (2) |
Cu4a | 0.0135 (3) | 0.0148 (5) | 0.0111 (5) | 0.0036 (3) | 0.0028 (3) | 0.0018 (2) |
Cu4b | 0.0128 (4) | 0.0157 (4) | 0.0171 (5) | 0.0091 (3) | 0.0040 (3) | 0.0062 (3) |
Cu4c | 0.0113 (3) | 0.0171 (5) | 0.0119 (3) | 0.0053 (3) | −0.0020 (3) | 0.0038 (3) |
Cl1a | 0.0164 (7) | 0.0174 (9) | 0.0188 (9) | 0.0032 (6) | −0.0014 (6) | 0.0010 (5) |
Cl2a | 0.0166 (6) | 0.0187 (9) | 0.0187 (10) | 0.0040 (7) | −0.0007 (6) | 0.0017 (5) |
Cl2b | 0.0153 (6) | 0.0161 (8) | 0.0191 (9) | 0.0047 (6) | −0.0023 (6) | 0.0021 (5) |
Cl2c | 0.0150 (6) | 0.0162 (8) | 0.0195 (9) | 0.0044 (7) | −0.0015 (6) | 0.0018 (5) |
O1a | 0.0124 (18) | 0.019 (2) | 0.027 (3) | 0.0091 (17) | 0.0129 (17) | 0.0110 (19) |
O1b | 0.016 (2) | 0.033 (3) | 0.0117 (18) | 0.012 (2) | −0.0005 (16) | 0.0102 (18) |
O1c | 0.018 (2) | 0.019 (2) | 0.023 (2) | 0.0064 (17) | 0.0027 (17) | −0.0040 (17) |
O2a | 0.019 (2) | 0.030 (3) | 0.019 (2) | 0.005 (2) | 0.0052 (19) | 0.0135 (19) |
O2b | 0.0125 (16) | 0.013 (2) | 0.0147 (18) | 0.0060 (14) | 0.0054 (14) | 0.0073 (13) |
O2c | 0.0063 (17) | 0.018 (2) | 0.027 (2) | 0.0013 (15) | 0.0057 (16) | 0.0022 (18) |
O3a | 0.021 (2) | 0.016 (2) | 0.0147 (19) | 0.0105 (17) | 0.0007 (16) | 0.0069 (16) |
O3b | 0.0122 (18) | 0.014 (2) | 0.022 (2) | 0.0008 (15) | 0.0038 (16) | 0.0014 (15) |
O3c | 0.0060 (15) | 0.020 (2) | 0.0100 (19) | 0.0021 (15) | −0.0003 (13) | 0.0054 (16) |
O4a | 0.0059 (17) | 0.018 (2) | 0.035 (3) | 0.0039 (15) | 0.0041 (16) | 0.007 (2) |
O4b | 0.0135 (19) | 0.021 (2) | 0.0149 (19) | 0.0032 (16) | 0.0009 (16) | 0.0071 (16) |
O4c | 0.0206 (19) | 0.0066 (18) | 0.0125 (17) | 0.0063 (14) | 0.0020 (14) | 0.0063 (12) |
Bond lengths (Å) top
Cu1a—Cu4a | 3.0719 (11) | Cl2b—O1b | 3.142 (5) |
Cu1a—Cu4ai | 3.0719 (11) | Cl2b—O1cxiv | 3.095 (5) |
Cu1a—Cu4b | 3.0148 (7) | Cl2b—O2bxvii | 3.439 (5) |
Cu1a—Cu4bi | 3.0148 (7) | Cl2b—O2ci | 3.227 (5) |
Cu1a—Cu4c | 3.1286 (9) | Cl2b—O3axiv | 3.062 (6) |
Cu1a—Cu4ci | 3.1286 (9) | Cl2b—O3b | 3.269 (5) |
Cu1a—O4a | 2.306 (5) | Cl2b—O4ai | 3.086 (5) |
Cu1a—O4ai | 2.306 (5) | Cl2b—H4b | 3.46 (7) |
Cu1a—O4b | 2.001 (5) | Cl2b—H4ai | 2.26 (6) |
Cu1a—O4bi | 2.001 (5) | Cl2b—H3axiv | 2.13 (7) |
Cu1a—O4c | 2.069 (5) | Cl2b—H2bxvii | 2.94 (6) |
Cu1a—O4ci | 2.069 (5) | Cl2b—H2aix | 3.26 (7) |
Cu1a—H4b | 2.68 (6) | Cl2b—H3cxix | 3.50 (6) |
Cu1a—H4bi | 2.68 (6) | Cl2b—H1cxiv | 2.27 (6) |
Cu1a—H4a | 2.09 (6) | Cl2c—O1axx | 3.091 (5) |
Cu1a—H4ai | 2.09 (6) | Cl2c—O1c | 3.247 (5) |
Cu1a—H4c | 2.55 (8) | Cl2c—O2ai | 3.143 (6) |
Cu1a—H4ci | 2.55 (8) | Cl2c—O3bxx | 3.085 (5) |
Cu2a—Cu3aii | 2.9912 (7) | Cl2c—O3c | 3.223 (5) |
Cu2a—Cu3aiii | 2.9912 (7) | Cl2c—O4bi | 3.074 (6) |
Cu2a—Cu3bii | 3.1283 (9) | Cl2c—O4c | 3.452 (5) |
Cu2a—Cu3biii | 3.1283 (9) | Cl2c—H4bi | 2.18 (7) |
Cu2a—Cu4a | 3.0971 (10) | Cl2c—H4a | 3.47 (6) |
Cu2a—Cu4aiv | 3.0971 (10) | Cl2c—H4c | 3.15 (6) |
Cu2a—O1a | 2.398 (5) | Cl2c—H1axx | 2.23 (5) |
Cu2a—O1aiv | 2.398 (5) | Cl2c—H3bxx | 2.19 (6) |
Cu2a—O2bv | 2.019 (4) | Cl2c—H2cix | 3.16 (6) |
Cu2a—O2bi | 2.019 (4) | O1a—O2bi | 2.660 (7) |
Cu2a—O3a | 2.004 (5) | O1a—O3a | 2.701 (8) |
Cu2a—O3aiv | 2.004 (5) | O1a—O3aiv | 3.498 (7) |
Cu2a—H3a | 2.53 (8) | O1a—O3biii | 2.935 (7) |
Cu2a—H3aiv | 2.53 (8) | O1a—O4b | 2.921 (7) |
Cu2a—H1a | 2.97 (6) | O1a—H4b | 2.79 (6) |
Cu2a—H1aiv | 2.97 (6) | O1a—H4biii | 3.31 (7) |
Cu2a—H2bv | 2.48 (10) | O1a—H3a | 3.46 (8) |
Cu2a—H2bi | 2.48 (10) | O1a—H1a | 0.99 (6) |
Cu2b—Cu3b | 3.0042 (9) | O1a—H2bi | 3.36 (8) |
Cu2b—Cu3bvi | 3.0042 (9) | O1a—H3b | 3.29 (7) |
Cu2b—Cu3cvii | 3.0965 (10) | O1a—H3biii | 2.82 (6) |
Cu2b—Cu3ci | 3.0965 (10) | O1b—O2cvii | 3.445 (7) |
Cu2b—Cu4b | 3.1029 (7) | O1b—O2ci | 2.640 (8) |
Cu2b—Cu4bvi | 3.1029 (7) | O1b—O3b | 2.655 (8) |
Cu2b—O1b | 2.308 (6) | O1b—O3bvi | 3.422 (7) |
Cu2b—O1bvi | 2.308 (6) | O1b—O3cxix | 2.946 (7) |
Cu2b—O2cvii | 2.023 (5) | O1b—O4c | 3.007 (8) |
Cu2b—O2ci | 2.023 (5) | O1b—H4c | 3.15 (6) |
Cu2b—O3b | 2.013 (4) | O1b—H4cxix | 3.31 (7) |
Cu2b—O3bvi | 2.013 (4) | O1b—H3cxix | 3.33 (5) |
Cu2b—H3b | 2.66 (6) | O1b—H2cvii | 3.11 (6) |
Cu2b—H3bvi | 2.66 (6) | O1b—H2ci | 3.17 (6) |
Cu2b—H2cvii | 2.13 (6) | O1b—H1b | 0.98 (7) |
Cu2b—H2ci | 2.13 (6) | O1c—O2aviii | 3.494 (7) |
Cu2b—H1b | 2.92 (6) | O1c—O2ai | 2.660 (9) |
Cu2b—H1bvi | 2.92 (6) | O1c—O3ax | 3.041 (7) |
Cu2c—Cu3aviii | 3.1251 (7) | O1c—O3c | 2.543 (7) |
Cu2c—Cu3ai | 3.1251 (7) | O1c—O3cxi | 3.144 (6) |
Cu2c—Cu3cix | 3.0724 (11) | O1c—O4a | 2.965 (7) |
Cu2c—Cu3cx | 3.0724 (11) | O1c—H4a | 3.48 (6) |
Cu2c—Cu4c | 3.0040 (9) | O1c—H3ax | 3.19 (7) |
Cu2c—Cu4cxi | 3.0040 (9) | O1c—H2aviii | 3.33 (8) |
Cu2c—O1c | 2.064 (5) | O1c—H3c | 3.09 (6) |
Cu2c—O1cxi | 2.064 (5) | O1c—H3cxi | 2.64 (6) |
Cu2c—O2aviii | 2.319 (6) | O1c—H1c | 1.02 (5) |
Cu2c—O2ai | 2.319 (6) | O2a—O2bxv | 3.000 (8) |
Cu2c—O3c | 1.979 (4) | O2a—O2cxiii | 2.948 (8) |
Cu2c—O3cxi | 1.979 (4) | O2a—O3cxvi | 3.404 (7) |
Cu2c—H2aviii | 2.73 (9) | O2a—O3ci | 2.646 (8) |
Cu2c—H2ai | 2.73 (9) | O2a—H2bxxi | 3.32 (9) |
Cu2c—H3c | 2.00 (6) | O2a—H2bxv | 3.34 (6) |
Cu2c—H3cxi | 2.00 (6) | O2a—H2a | 0.99 (7) |
Cu2c—H1c | 2.38 (9) | O2a—H3cxvi | 2.84 (5) |
Cu2c—H1cxi | 2.38 (9) | O2a—H3ci | 3.27 (6) |
Cu3a—Cu3bxii | 3.4204 (11) | O2a—H1cxvi | 3.03 (8) |
Cu3a—Cu3cxiii | 3.4262 (11) | O2a—H2cxiii | 3.10 (6) |
Cu3a—Cu4axiv | 3.4188 (11) | O2b—O2cxxii | 3.033 (7) |
Cu3a—Cu4ci | 3.4162 (11) | O2b—O3axxiii | 3.093 (7) |
Cu3a—Cl2axiv | 2.7563 (19) | O2b—O3ai | 2.572 (8) |
Cu3a—Cl2ci | 2.8378 (18) | O2b—H3axxiii | 2.99 (8) |
Cu3a—O1ci | 2.017 (5) | O2b—H3ai | 3.46 (8) |
Cu3a—O2a | 1.949 (6) | O2b—H1ai | 3.44 (6) |
Cu3a—O2bxv | 2.034 (5) | O2b—H2b | 1.03 (6) |
Cu3a—O3axiv | 1.990 (6) | O2b—H2axxiv | 3.30 (8) |
Cu3a—H3axiv | 2.67 (7) | O2b—H2axv | 3.29 (7) |
Cu3a—H2bxv | 2.85 (5) | O2c—O3bxxv | 3.122 (6) |
Cu3a—H2a | 2.71 (7) | O2c—O3bi | 2.557 (7) |
Cu3a—H3cxvi | 2.97 (5) | O2c—H2bxxii | 2.96 (7) |
Cu3a—H1ci | 2.94 (4) | O2c—H2axiii | 2.87 (7) |
Cu3b—Cu3ci | 3.4252 (16) | O2c—H3bxxv | 3.25 (6) |
Cu3b—Cu4aiii | 3.4315 (16) | O2c—H3bi | 3.43 (7) |
Cu3b—Cu4b | 3.4134 (11) | O2c—H2c | 1.01 (5) |
Cu3b—Cl2aiii | 2.8165 (19) | O2c—H1bi | 3.49 (6) |
Cu3b—Cl2b | 2.7604 (18) | O3a—O4a | 2.944 (8) |
Cu3b—O1aiii | 1.943 (5) | O3a—H4a | 3.46 (6) |
Cu3b—O2bxvii | 1.986 (5) | O3a—H3a | 0.98 (8) |
Cu3b—O2ci | 2.009 (5) | O3a—H2bv | 2.85 (9) |
Cu3b—O3b | 1.986 (5) | O3a—H2bi | 3.49 (8) |
Cu3b—H3axiv | 3.42 (7) | O3b—O4b | 3.051 (7) |
Cu3b—H1aiii | 2.42 (6) | O3b—H4b | 2.92 (7) |
Cu3b—H2bxvii | 2.39 (6) | O3b—H1a | 3.42 (6) |
Cu3b—H3b | 2.51 (7) | O3b—H1aiii | 2.83 (6) |
Cu3b—H2ci | 2.84 (4) | O3b—H3b | 0.99 (6) |
Cu3c—Cu4bi | 3.4297 (10) | O3b—H2cvii | 2.53 (6) |
Cu3c—Cu4cxviii | 3.4223 (16) | O3b—H2ci | 3.28 (5) |
Cu3c—Cl2bi | 2.7874 (16) | O3b—H1b | 3.49 (7) |
Cu3c—Cl2cxviii | 2.7709 (16) | O3c—O4c | 3.027 (6) |
Cu3c—O1bi | 1.946 (5) | O3c—H4c | 2.99 (6) |
Cu3c—O2axiii | 1.955 (6) | O3c—H2aviii | 3.45 (8) |
Cu3c—O2c | 2.005 (6) | O3c—H2ai | 3.29 (8) |
Cu3c—O3cxviii | 2.010 (5) | O3c—H3c | 0.95 (5) |
Cu3c—H2axiii | 2.35 (6) | O3c—H1c | 3.00 (8) |
Cu3c—H3cxviii | 2.66 (5) | O3c—H1cxi | 3.18 (8) |
Cu3c—H1cx | 3.28 (6) | O3c—H1b | 3.48 (6) |
Cu3c—H2c | 2.46 (6) | O3c—H1bxix | 2.90 (6) |
Cu3c—H1bi | 2.51 (6) | O4a—O4b | 2.650 (8) |
Cu4a—Cu4b | 3.4173 (11) | O4a—O4bi | 3.409 (7) |
Cu4a—Cu4c | 3.4316 (16) | O4a—O4c | 2.636 (7) |
Cu4a—Cl1a | 2.7751 (17) | O4a—O4ci | 3.500 (6) |
Cu4a—Cl2a | 2.7875 (17) | O4a—H4a | 1.00 (5) |
Cu4a—O1a | 1.951 (5) | O4a—H4c | 3.39 (7) |
Cu4a—O3a | 2.022 (5) | O4a—H4ci | 3.49 (7) |
Cu4a—O4a | 1.955 (6) | O4a—H3a | 2.81 (7) |
Cu4a—O4b | 2.010 (5) | O4a—H1c | 2.75 (7) |
Cu4a—H4b | 2.55 (7) | O4b—O4c | 2.571 (8) |
Cu4a—H4a | 2.56 (6) | O4b—O4ci | 3.156 (7) |
Cu4a—H4ci | 3.39 (6) | O4b—H4b | 1.01 (7) |
Cu4a—H3a | 2.45 (7) | O4b—H4a | 3.03 (6) |
Cu4a—H1a | 2.62 (5) | O4b—H4ai | 2.75 (6) |
Cu4a—H2bv | 3.30 (7) | O4b—H4c | 3.42 (7) |
Cu4b—Cu4c | 3.4255 (10) | O4b—H4ci | 3.06 (7) |
Cu4b—Cl1a | 2.7779 (17) | O4b—H1a | 3.02 (5) |
Cu4b—Cl2b | 2.8252 (17) | O4b—H1aiii | 3.31 (6) |
Cu4b—O1b | 1.957 (6) | O4b—H3b | 2.97 (6) |
Cu4b—O3b | 2.030 (5) | O4c—H4b | 3.46 (7) |
Cu4b—O4b | 1.990 (5) | O4c—H4bi | 3.31 (6) |
Cu4b—O4c | 2.018 (5) | O4c—H4a | 3.03 (6) |
Cu4b—H4b | 2.49 (7) | O4c—H4ai | 2.85 (6) |
Cu4b—H4ai | 3.01 (5) | O4c—H4c | 0.97 (7) |
Cu4b—H4c | 2.67 (6) | O4c—H3c | 3.41 (6) |
Cu4b—H3b | 2.55 (6) | O4c—H1b | 2.92 (7) |
Cu4b—H2cvii | 3.02 (5) | O4c—H1bxix | 3.31 (7) |
Cu4b—H1b | 2.48 (7) | H4b—H4ai | 2.89 (9) |
Cu4c—Cl1a | 2.8101 (19) | H4b—H4ci | 3.08 (9) |
Cu4c—Cl2c | 2.7635 (18) | H4b—H1a | 2.70 (8) |
Cu4c—O1c | 1.970 (5) | H4b—H1aiii | 2.39 (9) |
Cu4c—O3c | 2.004 (5) | H4b—H3b | 2.72 (8) |
Cu4c—O4a | 1.957 (5) | H4b—H3biii | 2.79 (9) |
Cu4c—O4c | 1.986 (5) | H4a—H4ci | 2.94 (9) |
Cu4c—H4a | 2.59 (6) | H4a—H3a | 3.43 (9) |
Cu4c—H4c | 2.45 (6) | H4a—H3ax | 3.27 (10) |
Cu4c—H3c | 2.60 (6) | H4a—H1c | 3.46 (9) |
Cu4c—H1c | 2.15 (6) | H4c—H3c | 3.45 (8) |
Cl1a—O2aviii | 3.082 (6) | H4c—H3cxix | 3.41 (9) |
Cl1a—O2bv | 3.099 (5) | H4c—H1b | 2.91 (9) |
Cl1a—O2cvii | 3.058 (5) | H4c—H1bxix | 2.48 (10) |
Cl1a—O4a | 3.130 (5) | H3a—H2bv | 2.54 (11) |
Cl1a—O4b | 3.227 (5) | H3a—H1c | 2.69 (11) |
Cl1a—O4c | 3.244 (4) | H1a—H1aiii | 3.30 (8) |
Cl1a—H3a | 3.32 (7) | H1a—H3b | 2.52 (9) |
Cl1a—H2bv | 2.19 (7) | H1a—H3biii | 2.59 (8) |
Cl1a—H2aviii | 2.18 (6) | H2b—H2axxiv | 2.41 (12) |
Cl1a—H3c | 3.39 (6) | H2b—H2axv | 3.47 (10) |
Cl1a—H1c | 3.03 (5) | H2b—H1cxxiii | 3.41 (7) |
Cl1a—H3b | 3.40 (6) | H2b—H2cxxvi | 3.36 (10) |
Cl1a—H2cvii | 2.18 (6) | H2a—H3cxvi | 2.98 (10) |
Cl2a—O1a | 3.115 (5) | H2a—H1cxvi | 2.66 (10) |
Cl2a—O1bxviii | 3.096 (6) | H2a—H2cxxvii | 3.31 (10) |
Cl2a—O2bi | 3.257 (5) | H2a—H2cxiii | 3.20 (9) |
Cl2a—O3a | 3.230 (5) | H3c—H1c | 3.32 (11) |
Cl2a—O3cxviii | 3.067 (5) | H3c—H1cxi | 2.88 (9) |
Cl2a—O4ci | 3.103 (5) | H3c—H1b | 3.10 (9) |
Cl2a—H4a | 3.40 (6) | H3c—H1bxix | 3.27 (8) |
Cl2a—H4ci | 2.20 (6) | H3b—H2cvii | 2.57 (8) |
Cl2a—H3cxviii | 2.22 (6) | H2c—H1bxxv | 3.34 (9) |
Cl2a—H1bxviii | 2.27 (6) | H1b—H1bxix | 3.37 (8) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y, z−1; (iii) −x+1, −y, −z+1; (iv) −x+1, −y, −z; (v) x, y−1, z−1; (vi) −x, −y, −z+1; (vii) x−1, y−1, z; (viii) x−1, y, z−1; (ix) x−1, 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, y−1, z; (xviii) x+1, y, z; (xix) −x, −y+1, −z+1; (xx) x, y+1, z; (xxi) x+1, y−1, z; (xxii) −x+1, −y+2, −z+1; (xxiii) x, y+1, z+1; (xxiv) x−1, y+1, z; (xxv) x+1, y+1, z; (xxvi) x−1, y, z+1; (xxvii) x, y−1, z+1. |
(II) top
Crystal data top
H3ClCu2O3 | F(000) = 408 |
Mr = 213.6 | Dx = 3.742 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yabc | Cell parameters from 1685 reflections |
a = 6.1226 (3) Å | θ = 3.7–35.6° |
b = 6.8346 (4) Å | µ = 11.76 mm−1 |
c = 9.1841 (6) Å | T = 294 K |
β = 99.577 (4)° | , green |
V = 378.96 (4) Å3 | 0.08 × 0.08 × 0.05 mm |
Z = 4 |
Data collection top
Nonius KappaCCD diffractometer | 1672 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 993 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.000 |
φ scans, and ω scans with κ offsets | θmax = 35.6°, θmin = 3.7° |
Absorption correction: multi-scan R.H. Blessing, Acta Cryst. (1995), A51, 33-38 | h = −9→9 |
Tmin = 0.350, Tmax = 0.540 | k = 0→10 |
1685 measured reflections | l = 0→14 |
Refinement top
Refinement on F2 | 1 constraint |
R[F2 > 2σ(F2)] = 0.040 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.122 | Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.0036I2) |
S = 1.08 | (Δ/σ)max = 0.0002 |
1672 reflections | Δρmax = 1.80 e Å−3 |
69 parameters | Δρmin = −1.92 e Å−3 |
3 restraints |
Crystal data top
H3ClCu2O3 | V = 378.96 (4) Å3 |
Mr = 213.6 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 6.1226 (3) Å | µ = 11.76 mm−1 |
b = 6.8346 (4) Å | T = 294 K |
c = 9.1841 (6) Å | 0.08 × 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 = 0.540 | Rint = 0.000 |
1685 measured reflections |
Refinement top
R[F2 > 2σ(F2)] = 0.040 | 3 restraints |
wR(F2) = 0.122 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | Δρmax = 1.80 e Å−3 |
1672 reflections | Δρmin = −1.92 e Å−3 |
69 parameters |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Cu1 | 0 | 0.5 | 0.5 | 0.01311 (16) | |
Cu2 | 0 | 0 | 0 | 0.01556 (17) | |
Cu3 | 0.25292 (8) | 0.24557 (5) | 0.74944 (6) | 0.01515 (14) | |
Cl1 | 0.11236 (15) | −0.00140 (13) | 0.30614 (10) | 0.0179 (2) | |
O1 | 0.2809 (6) | 0.3056 (4) | 0.5432 (3) | 0.0241 (9) | |
O2 | 0.4157 (5) | −0.0056 (4) | 0.7679 (4) | 0.0230 (9) | |
O3 | 0.2675 (5) | 0.6845 (4) | 0.5410 (3) | 0.0209 (9) | |
H1 | 0.22 (2) | 0.202 (12) | 0.473 (10) | 0.16 (3)* | |
H3 | 0.23 (3) | 0.793 (12) | 0.470 (10) | 0.16 (3)* | |
H2 | 0.580 (5) | −0.007 (8) | 0.779 (17) | 0.16 (3)* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0130 (3) | 0.0139 (3) | 0.0129 (3) | −0.0006 (2) | 0.0033 (2) | −0.0004 (3) |
Cu2 | 0.0161 (3) | 0.0164 (3) | 0.0156 (3) | −0.0001 (3) | 0.0067 (2) | −0.0003 (3) |
Cu3 | 0.0181 (2) | 0.0127 (2) | 0.0156 (2) | 0.00081 (14) | 0.00566 (18) | 0.00135 (14) |
Cl1 | 0.0181 (4) | 0.0187 (4) | 0.0173 (4) | 0.0002 (4) | 0.0039 (3) | 0.0008 (4) |
O1 | 0.0350 (16) | 0.0206 (15) | 0.0188 (14) | −0.0132 (14) | 0.0112 (14) | −0.0069 (12) |
O2 | 0.0169 (13) | 0.0155 (12) | 0.0401 (18) | 0.0016 (10) | 0.0153 (13) | −0.0019 (13) |
O3 | 0.0290 (15) | 0.0164 (14) | 0.0193 (14) | 0.0056 (12) | 0.0099 (14) | 0.0051 (11) |
Geometric parameters (Å, º) top
Cu1—O1 | 2.157 (3) | Cu3—Cl1ix | 2.7911 (10) |
Cu1—O1i | 2.157 (3) | Cu3—O1 | 1.973 (3) |
Cu1—O2ii | 2.108 (3) | Cu3—O2 | 1.978 (3) |
Cu1—O2iii | 2.108 (3) | Cu3—O2ii | 1.982 (3) |
Cu1—O3 | 2.052 (3) | Cu3—O3x | 1.993 (3) |
Cu1—O3i | 2.052 (3) | Cu3—H1 | 2.53 (10) |
Cu1—H1 | 2.49 (10) | Cu3—H3x | 2.59 (10) |
Cu1—H1i | 2.49 (10) | Cu3—H2 | 2.63 (4) |
Cu1—H3 | 2.49 (11) | Cu3—H2ii | 2.63 (4) |
Cu1—H3i | 2.49 (11) | Cl1—H1 | 2.09 (9) |
Cu1—H2ii | 2.17 (15) | Cl1—H3xi | 2.10 (9) |
Cu1—H2iii | 2.17 (15) | Cl1—H2vii | 2.15 (8) |
Cu2—Cl1 | 2.7812 (9) | O1—O2 | 2.983 (4) |
Cu2—Cl1iv | 2.7812 (9) | O1—O2ii | 2.611 (5) |
Cu2—O1v | 1.975 (3) | O1—O3 | 2.591 (4) |
Cu2—O1iii | 1.975 (3) | O1—O3xii | 2.993 (5) |
Cu2—O3v | 1.984 (3) | O1—H1 | 0.99 (9) |
Cu2—O3iii | 1.984 (3) | O2—O3x | 2.584 (5) |
Cu2—H1v | 2.64 (11) | O2—H2 | 1.00 (3) |
Cu2—H1iii | 2.64 (11) | O3—H3 | 0.99 (9) |
Cu2—H3v | 2.58 (11) | H1—H3xi | 2.80 (11) |
Cu2—H3iii | 2.58 (11) | H1—H3i | 2.9 (2) |
Cu2—H2vi | 3.00 (9) | H1—H2iii | 2.79 (13) |
Cu2—H2vii | 3.00 (9) | H3—H2iii | 2.69 (13) |
Cu3—Cl1viii | 2.7690 (10) | ||
O1—Cu1—O1i | 180 | Cu2—Cl1—H1 | 137 (2) |
O1—Cu1—O2ii | 75.48 (11) | Cu2—Cl1—H3xi | 136 (2) |
O1—Cu1—O2iii | 104.52 (11) | Cu2—Cl1—H2vii | 74 (4) |
O1—Cu1—O3 | 75.95 (12) | Cu3viii—Cl1—Cu3iii | 75.85 (3) |
O1—Cu1—O3i | 104.05 (12) | Cu3viii—Cl1—H1 | 133 (4) |
O1—Cu1—H1 | 23 (2) | Cu3viii—Cl1—H3xi | 84 (4) |
O1—Cu1—H1i | 157 (2) | Cu3viii—Cl1—H2vii | 133 (3) |
O1—Cu1—H3 | 94 (3) | Cu3iii—Cl1—Cu3viii | 75.85 (3) |
O1—Cu1—H3i | 86 (3) | Cu3iii—Cl1—H1 | 82 (3) |
O1—Cu1—H2ii | 96.4 (13) | Cu3iii—Cl1—H3xi | 136 (4) |
O1—Cu1—H2iii | 83.6 (13) | Cu3iii—Cl1—H2vii | 129 (2) |
O1i—Cu1—O1 | 180 | H1—Cl1—H3xi | 84 (3) |
O1i—Cu1—O2ii | 104.52 (11) | H1—Cl1—H2vii | 93 (5) |
O1i—Cu1—O2iii | 75.48 (11) | H3xi—Cl1—H2vii | 93 (5) |
O1i—Cu1—O3 | 104.05 (12) | Cu1—O1—Cu2xiii | 95.50 (12) |
O1i—Cu1—O3i | 75.95 (12) | Cu1—O1—Cu3 | 96.35 (14) |
O1i—Cu1—H1 | 157 (2) | Cu1—O1—O2 | 133.37 (16) |
O1i—Cu1—H1i | 23 (2) | Cu1—O1—O2ii | 51.41 (10) |
O1i—Cu1—H3 | 86 (3) | Cu1—O1—O3 | 50.18 (9) |
O1i—Cu1—H3i | 94 (3) | Cu1—O1—O3xii | 132.91 (14) |
O1i—Cu1—H2ii | 83.6 (13) | Cu1—O1—H1 | 97 (7) |
O1i—Cu1—H2iii | 96.4 (13) | Cu1—O1—H2iii | 48 (2) |
O2ii—Cu1—O2iii | 180 | Cu2xiii—O1—Cu3 | 120.20 (14) |
O2ii—Cu1—O3 | 76.80 (11) | Cu2xiii—O1—O2 | 119.98 (14) |
O2ii—Cu1—O3i | 103.20 (11) | Cu2xiii—O1—O2ii | 101.79 (13) |
O2ii—Cu1—H1 | 92 (2) | Cu2xiii—O1—O3 | 49.27 (10) |
O2ii—Cu1—H1i | 88 (2) | Cu2xiii—O1—H1 | 123 (7) |
O2ii—Cu1—H3 | 95 (2) | Cu2xiii—O1—H2iii | 73.6 (9) |
O2ii—Cu1—H3i | 85 (2) | Cu3—O1—O2ii | 48.84 (10) |
O2ii—Cu1—H2ii | 26.9 (12) | Cu3—O1—O3 | 101.97 (14) |
O2ii—Cu1—H2iii | 153.1 (12) | Cu3—O1—O3xii | 118.96 (14) |
O2iii—Cu1—O2ii | 180 | Cu3—O1—H1 | 113 (6) |
O2iii—Cu1—O3 | 103.20 (11) | Cu3—O1—H2iii | 144.6 (19) |
O2iii—Cu1—O3i | 76.80 (11) | O2—O1—O2ii | 89.87 (13) |
O2iii—Cu1—H1 | 88 (2) | O2—O1—O3 | 136.27 (14) |
O2iii—Cu1—H1i | 92 (2) | O2—O1—O3xii | 91.94 (12) |
O2iii—Cu1—H3 | 85 (2) | O2—O1—H1 | 88 (5) |
O2iii—Cu1—H3i | 95 (2) | O2—O1—H2iii | 162.5 (14) |
O2iii—Cu1—H2ii | 153.1 (12) | O2ii—O1—O2 | 89.87 (13) |
O2iii—Cu1—H2iii | 26.9 (12) | O2ii—O1—O3 | 59.56 (12) |
O3—Cu1—O3i | 180 | O2ii—O1—O3xii | 135.08 (14) |
O3—Cu1—H1 | 95 (3) | O2ii—O1—H1 | 129 (8) |
O3—Cu1—H1i | 85 (3) | O2ii—O1—H2iii | 98 (2) |
O3—Cu1—H3 | 23 (3) | O3—O1—O3xii | 90.27 (13) |
O3—Cu1—H3i | 157 (3) | O3—O1—H1 | 135 (5) |
O3—Cu1—H2ii | 98.0 (13) | O3—O1—H2iii | 60.5 (17) |
O3—Cu1—H2iii | 82.0 (13) | O3xii—O1—O3 | 90.27 (13) |
O3i—Cu1—O3 | 180 | O3xii—O1—H1 | 96 (8) |
O3i—Cu1—H1 | 85 (3) | O3xii—O1—H2iii | 93.1 (15) |
O3i—Cu1—H1i | 95 (3) | H1—O1—H2iii | 75 (5) |
O3i—Cu1—H3 | 157 (3) | Cu1x—O2—Cu3 | 96.11 (14) |
O3i—Cu1—H3i | 23 (3) | Cu1x—O2—Cu3x | 97.67 (14) |
O3i—Cu1—H2ii | 82.0 (13) | Cu1x—O2—O1 | 132.83 (13) |
O3i—Cu1—H2iii | 98.0 (13) | Cu1x—O2—O1x | 53.11 (10) |
H1—Cu1—H1i | 180 | Cu1x—O2—O3x | 50.62 (10) |
H1—Cu1—H3 | 108 (4) | Cu1x—O2—H2 | 80 (9) |
H1—Cu1—H3i | 72 (4) | Cu3—O2—Cu3x | 119.32 (15) |
H1—Cu1—H2ii | 107 (3) | Cu3—O2—O1x | 101.82 (15) |
H1—Cu1—H2iii | 73 (3) | Cu3—O2—O3x | 49.66 (10) |
H1i—Cu1—H1 | 180 | Cu3—O2—H2 | 120 (3) |
H1i—Cu1—H3 | 72 (4) | Cu3x—O2—Cu3 | 119.32 (15) |
H1i—Cu1—H3i | 108 (4) | Cu3x—O2—O1 | 118.40 (14) |
H1i—Cu1—H2ii | 73 (3) | Cu3x—O2—O1x | 48.54 (10) |
H1i—Cu1—H2iii | 107 (3) | Cu3x—O2—O3x | 101.95 (15) |
H3—Cu1—H3i | 180 | Cu3x—O2—H2 | 120 (3) |
H3—Cu1—H2ii | 110 (3) | O1—O2—O1x | 135.01 (15) |
H3—Cu1—H2iii | 70 (3) | O1—O2—O3x | 90.58 (12) |
H3i—Cu1—H3 | 180 | O1—O2—H2 | 104 (6) |
H3i—Cu1—H2ii | 70 (3) | O1x—O2—O1 | 135.01 (15) |
H3i—Cu1—H2iii | 110 (3) | O1x—O2—O3x | 59.83 (12) |
H2ii—Cu1—H2iii | 180 | O1x—O2—H2 | 120 (7) |
H2iii—Cu1—H2ii | 180 | O3x—O2—H2 | 119 (8) |
Cl1—Cu2—Cl1iv | 180 | Cu1—O3—Cu2xiii | 98.66 (12) |
Cl1—Cu2—O1v | 97.97 (8) | Cu1—O3—Cu3ii | 97.45 (13) |
Cl1—Cu2—O1iii | 82.03 (8) | Cu1—O3—O1 | 53.87 (10) |
Cl1—Cu2—O3v | 97.44 (8) | Cu1—O3—O1xii | 135.23 (14) |
Cl1—Cu2—O3iii | 82.56 (8) | Cu1—O3—O2ii | 52.58 (10) |
Cl1—Cu2—H1v | 82 (2) | Cu1—O3—H3 | 105 (8) |
Cl1—Cu2—H1iii | 98 (2) | Cu1—O3—H2iii | 51 (2) |
Cl1—Cu2—H3v | 81 (2) | Cu2xiii—O3—Cu3ii | 118.60 (13) |
Cl1—Cu2—H3iii | 99 (2) | Cu2xiii—O3—O1 | 48.96 (10) |
Cl1—Cu2—H2vi | 136 (3) | Cu2xiii—O3—O2ii | 102.45 (13) |
Cl1—Cu2—H2vii | 44 (3) | Cu2xiii—O3—H3 | 116 (8) |
Cl1iv—Cu2—Cl1 | 180 | Cu2xiii—O3—H2iii | 76.3 (9) |
Cl1iv—Cu2—O1v | 82.03 (8) | Cu3ii—O3—O1 | 102.06 (13) |
Cl1iv—Cu2—O1iii | 97.97 (8) | Cu3ii—O3—O1xii | 116.98 (13) |
Cl1iv—Cu2—O3v | 82.56 (8) | Cu3ii—O3—O2ii | 49.14 (9) |
Cl1iv—Cu2—O3iii | 97.44 (8) | Cu3ii—O3—H3 | 116 (6) |
Cl1iv—Cu2—H1v | 98 (2) | Cu3ii—O3—H2iii | 148.0 (19) |
Cl1iv—Cu2—H1iii | 82 (2) | O1—O3—O1xii | 89.73 (13) |
Cl1iv—Cu2—H3v | 99 (2) | O1—O3—O2ii | 60.60 (12) |
Cl1iv—Cu2—H3iii | 81 (2) | O1—O3—H3 | 139 (5) |
Cl1iv—Cu2—H2vi | 44 (3) | O1—O3—H2iii | 65.0 (16) |
Cl1iv—Cu2—H2vii | 136 (3) | O1xii—O3—O1 | 89.73 (13) |
O1v—Cu2—O1iii | 180 | O1xii—O3—O2ii | 135.29 (13) |
O1v—Cu2—O3v | 81.76 (13) | O1xii—O3—H3 | 86 (9) |
O1v—Cu2—O3iii | 98.24 (13) | O1xii—O3—H2iii | 92.9 (16) |
O1v—Cu2—H1v | 18 (2) | O2ii—O3—H3 | 139 (9) |
O1v—Cu2—H1iii | 162 (2) | O2ii—O3—H2iii | 102 (2) |
O1v—Cu2—H3v | 96 (3) | H3—O3—H2iii | 75 (5) |
O1v—Cu2—H3iii | 84 (3) | Cu1—H1—Cu2xiii | 73 (2) |
O1v—Cu2—H2vi | 112.8 (19) | Cu1—H1—Cl1 | 120 (5) |
O1v—Cu2—H2vii | 67.2 (19) | Cu1—H1—O1 | 59 (5) |
O1iii—Cu2—O1v | 180 | Cu1—H1—H3xi | 147 (6) |
O1iii—Cu2—O3v | 98.24 (13) | Cu1—H1—H3i | 54 (3) |
O1iii—Cu2—O3iii | 81.76 (13) | Cu1—H1—H2iii | 48 (3) |
O1iii—Cu2—H1v | 162 (2) | Cu2xiii—H1—Cu3 | 83 (3) |
O1iii—Cu2—H1iii | 18 (2) | Cu2xiii—H1—Cl1 | 135 (5) |
O1iii—Cu2—H3v | 84 (3) | Cu2xiii—H1—H3xi | 139 (6) |
O1iii—Cu2—H3iii | 96 (3) | Cu2xiii—H1—H3i | 126 (4) |
O1iii—Cu2—H2vi | 67.2 (19) | Cu2xiii—H1—H2iii | 67 (2) |
O1iii—Cu2—H2vii | 112.8 (19) | Cu3—H1—Cl1 | 141 (5) |
O3v—Cu2—O3iii | 180 | Cu3—H1—O1 | 46 (5) |
O3v—Cu2—H1v | 92 (3) | Cu3—H1—H3xi | 98 (3) |
O3v—Cu2—H1iii | 88 (3) | Cu3—H1—H3i | 74 (4) |
O3v—Cu2—H3v | 20 (3) | Cu3—H1—H2iii | 121 (4) |
O3v—Cu2—H3iii | 160 (3) | Cl1—H1—O1 | 174 (9) |
O3v—Cu2—H2vi | 116 (2) | Cl1—H1—H3xi | 48 (3) |
O3v—Cu2—H2vii | 64 (2) | Cl1—H1—H3i | 87 (4) |
O3iii—Cu2—O3v | 180 | Cl1—H1—H2iii | 90 (4) |
O3iii—Cu2—H1v | 88 (3) | O1—H1—H3xi | 136 (7) |
O3iii—Cu2—H1iii | 92 (3) | O1—H1—H3i | 97 (8) |
O3iii—Cu2—H3v | 160 (3) | O1—H1—H2iii | 85 (6) |
O3iii—Cu2—H3iii | 20 (3) | H3xi—H1—H3i | 92 (5) |
O3iii—Cu2—H2vi | 64 (2) | H3xi—H1—H2iii | 138 (5) |
O3iii—Cu2—H2vii | 116 (2) | H3i—H1—H3xi | 92 (5) |
H1v—Cu2—H1iii | 180 | H3i—H1—H2iii | 84 (4) |
H1v—Cu2—H3v | 102 (4) | Cu1—H3—Cu2xiii | 74 (2) |
H1v—Cu2—H3iii | 78 (4) | Cu1—H3—Cu3ii | 73 (3) |
H1v—Cu2—H2vi | 121 (3) | Cu1—H3—Cl1xiv | 119 (6) |
H1v—Cu2—H2vii | 59 (3) | Cu1—H3—O3 | 53 (6) |
H1iii—Cu2—H1v | 180 | Cu1—H3—H1xiv | 142 (7) |
H1iii—Cu2—H3v | 78 (4) | Cu1—H3—H1i | 54 (3) |
H1iii—Cu2—H3iii | 102 (4) | Cu1—H3—H2iii | 49 (3) |
H1iii—Cu2—H2vi | 59 (3) | Cu2xiii—H3—Cu3ii | 83 (3) |
H1iii—Cu2—H2vii | 121 (3) | Cu2xiii—H3—Cl1xiv | 138 (6) |
H3v—Cu2—H3iii | 180 | Cu2xiii—H3—H1xiv | 142 (6) |
H3v—Cu2—H2vi | 123 (3) | Cu2xiii—H3—H1i | 127 (4) |
H3v—Cu2—H2vii | 57 (3) | Cu2xiii—H3—H2iii | 69 (2) |
H3iii—Cu2—H3v | 180 | Cu3ii—H3—Cl1xiv | 138 (5) |
H3iii—Cu2—H2vi | 57 (3) | Cu3ii—H3—H1xiv | 96 (3) |
H3iii—Cu2—H2vii | 123 (3) | Cu3ii—H3—H1i | 72 (4) |
H2vi—Cu2—H2vii | 180 | Cu3ii—H3—H2iii | 121 (5) |
H2vii—Cu2—H2vi | 180 | Cl1xiv—H3—O3 | 171 (11) |
Cl1viii—Cu3—Cl1ix | 178.23 (3) | Cl1xiv—H3—H1xiv | 48 (3) |
Cl1viii—Cu3—O1 | 98.32 (10) | Cl1xiv—H3—H1i | 84 (5) |
Cl1viii—Cu3—O2 | 82.69 (8) | Cl1xiv—H3—H2iii | 89 (4) |
Cl1viii—Cu3—O2ii | 96.23 (8) | O3—H3—H1xiv | 138 (7) |
Cl1viii—Cu3—O3x | 82.72 (9) | O3—H3—H1i | 90 (9) |
Cl1viii—Cu3—H1 | 80 (3) | O3—H3—H2iii | 84 (6) |
Cl1viii—Cu3—H3x | 99 (3) | H1xiv—H3—H1i | 88 (5) |
Cl1viii—Cu3—H2 | 101.7 (10) | H1xiv—H3—H2iii | 137 (5) |
Cl1viii—Cu3—H2ii | 77.3 (11) | H1i—H3—H1xiv | 88 (5) |
Cl1ix—Cu3—Cl1viii | 178.23 (3) | H1i—H3—H2iii | 84 (4) |
Cl1ix—Cu3—O1 | 81.80 (9) | Cu1x—H2—Cu2xv | 71 (3) |
Cl1ix—Cu3—O2 | 99.05 (8) | Cu1x—H2—Cu3 | 78 (3) |
Cl1ix—Cu3—O2ii | 82.03 (8) | Cu1x—H2—Cu3x | 79 (3) |
Cl1ix—Cu3—O3x | 97.19 (9) | Cu1x—H2—Cl1vii | 133 (5) |
Cl1ix—Cu3—H1 | 101 (3) | Cu1x—H2—O1ix | 48 (3) |
Cl1ix—Cu3—H3x | 81 (3) | Cu1x—H2—O2 | 73 (8) |
Cl1ix—Cu3—H2 | 80.1 (10) | Cu1x—H2—O3ix | 47 (3) |
Cl1ix—Cu3—H2ii | 101.0 (11) | Cu1x—H2—H1ix | 59 (4) |
O1—Cu3—O2 | 98.04 (14) | Cu1x—H2—H3ix | 61 (4) |
O1—Cu3—O2ii | 82.62 (14) | Cu2xv—H2—Cu3 | 128 (4) |
O1—Cu3—O3x | 178.63 (13) | Cu2xv—H2—Cu3x | 130 (4) |
O1—Cu3—H1 | 21 (2) | Cu2xv—H2—Cl1vii | 62.8 (13) |
O1—Cu3—H3x | 160 (2) | Cu2xv—H2—O2 | 144 (11) |
O1—Cu3—H2 | 93 (3) | Cu2xv—H2—H1ix | 54 (3) |
O1—Cu3—H2ii | 88 (3) | Cu2xv—H2—H3ix | 54 (3) |
O2—Cu3—O2ii | 178.80 (13) | Cu3—H2—Cu3x | 81.1 (9) |
O2—Cu3—O3x | 81.20 (13) | Cu3—H2—Cl1vii | 130 (4) |
O2—Cu3—H1 | 86 (2) | Cu3—H2—O1ix | 89 (3) |
O2—Cu3—H3x | 95 (2) | Cu3—H2—O3ix | 125 (5) |
O2—Cu3—H2 | 19.1 (11) | Cu3—H2—H1ix | 74 (3) |
O2—Cu3—H2ii | 159.8 (11) | Cu3—H2—H3ix | 136 (6) |
O2ii—Cu3—O2 | 178.80 (13) | Cu3x—H2—Cu3 | 81.1 (9) |
O2ii—Cu3—O3x | 98.16 (14) | Cu3x—H2—Cl1vii | 134 (5) |
O2ii—Cu3—H1 | 94 (2) | Cu3x—H2—O1ix | 127 (5) |
O2ii—Cu3—H3x | 85 (2) | Cu3x—H2—O3ix | 90 (3) |
O2ii—Cu3—H2 | 162.0 (11) | Cu3x—H2—H1ix | 134 (6) |
O2ii—Cu3—H2ii | 19.1 (11) | Cu3x—H2—H3ix | 77 (4) |
O3x—Cu3—H1 | 160 (2) | Cl1vii—H2—O1ix | 91 (2) |
O3x—Cu3—H3x | 20 (2) | Cl1vii—H2—O2 | 153 (12) |
O3x—Cu3—H2 | 86 (3) | Cl1vii—H2—O3ix | 94 (2) |
O3x—Cu3—H2ii | 93 (3) | Cl1vii—H2—H1ix | 91 (3) |
H1—Cu3—H3x | 178 (5) | Cl1vii—H2—H3ix | 92 (4) |
H1—Cu3—H2 | 87 (4) | O1ix—H2—O2 | 111 (9) |
H1—Cu3—H2ii | 93 (4) | O1ix—H2—O3ix | 55 (3) |
H3x—Cu3—H2 | 95 (4) | O1ix—H2—H3ix | 75 (4) |
H3x—Cu3—H2ii | 85 (4) | O2—H2—O3ix | 111 (9) |
H2—Cu3—H2ii | 179 (2) | O2—H2—H1ix | 105 (7) |
H2ii—Cu3—H2 | 179 (2) | O2—H2—H3ix | 108 (8) |
Cu2—Cl1—Cu3viii | 76.08 (3) | O3ix—H2—H1ix | 74 (4) |
Cu2—Cl1—Cu3iii | 75.79 (2) | H1ix—H2—H3ix | 95 (5) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1/2, y+1/2, −z+3/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) −x, −y, −z; (v) −x+1/2, y−1/2, −z+1/2; (vi) x−1, y, z−1; (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, y−1/2, −z+3/2; (xi) x, y−1, 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 formula | H3ClCu2O3 | H3ClCu2O3 |
Mr | 213.6 | 213.6 |
Crystal system, space group | Triclinic, P1 | Monoclinic, P21/n |
Temperature (K) | 294 | 294 |
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 |
V (Å3) | 761.97 (12) | 378.96 (4) |
Z | 8 | 4 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 11.69 | 11.76 |
Crystal size (mm) | 0.19 × 0.12 × 0.03 | 0.08 × 0.08 × 0.05 |
Data collection | ||
Diffractometer | Nonius KappaCCD | Nonius KappaCCD |
Absorption correction | Gaussian (Jana2000; Petricek, Dusek & Palatinus, 2000) | Multi-scan R.H. Blessing, Acta Cryst. (1995), A51, 33-38 |
Tmin, Tmax | 0.148, 0.708 | 0.350, 0.540 |
No. of measured, independent and observed [I > 3σ(I)] reflections | 47586, 6622, 4581 | 1685, 1672, 993 |
Rint | 0.045 | 0.000 |
(sin θ/λ)max (Å−1) | 0.807 | 0.818 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.191, 1.33 | 0.040, 0.122, 1.08 |
No. of reflections | 6622 | 1672 |
No. of parameters | 262 | 69 |
No. of restraints | 24 | 3 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.80, −1.49 | 1.80, −1.92 |
Computer programs: Jana2000 (Petricek, Dusek & Palatinus, 2000).
Selected bond lengths (Å) for (I) top
Cu1a—Cu4a | 3.0719 (11) | Cl2b—O1b | 3.142 (5) |
Cu1a—Cu4ai | 3.0719 (11) | Cl2b—O1cxiv | 3.095 (5) |
Cu1a—Cu4b | 3.0148 (7) | Cl2b—O2bxvii | 3.439 (5) |
Cu1a—Cu4bi | 3.0148 (7) | Cl2b—O2ci | 3.227 (5) |
Cu1a—Cu4c | 3.1286 (9) | Cl2b—O3axiv | 3.062 (6) |
Cu1a—Cu4ci | 3.1286 (9) | Cl2b—O3b | 3.269 (5) |
Cu1a—O4a | 2.306 (5) | Cl2b—O4ai | 3.086 (5) |
Cu1a—O4ai | 2.306 (5) | Cl2b—H4b | 3.46 (7) |
Cu1a—O4b | 2.001 (5) | Cl2b—H4ai | 2.26 (6) |
Cu1a—O4bi | 2.001 (5) | Cl2b—H3axiv | 2.13 (7) |
Cu1a—O4c | 2.069 (5) | Cl2b—H2bxvii | 2.94 (6) |
Cu1a—O4ci | 2.069 (5) | Cl2b—H2aix | 3.26 (7) |
Cu1a—H4b | 2.68 (6) | Cl2b—H3cxix | 3.50 (6) |
Cu1a—H4bi | 2.68 (6) | Cl2b—H1cxiv | 2.27 (6) |
Cu1a—H4a | 2.09 (6) | Cl2c—O1axx | 3.091 (5) |
Cu1a—H4ai | 2.09 (6) | Cl2c—O1c | 3.247 (5) |
Cu1a—H4c | 2.55 (8) | Cl2c—O2ai | 3.143 (6) |
Cu1a—H4ci | 2.55 (8) | Cl2c—O3bxx | 3.085 (5) |
Cu2a—Cu3aii | 2.9912 (7) | Cl2c—O3c | 3.223 (5) |
Cu2a—Cu3aiii | 2.9912 (7) | Cl2c—O4bi | 3.074 (6) |
Cu2a—Cu3bii | 3.1283 (9) | Cl2c—O4c | 3.452 (5) |
Cu2a—Cu3biii | 3.1283 (9) | Cl2c—H4bi | 2.18 (7) |
Cu2a—Cu4a | 3.0971 (10) | Cl2c—H4a | 3.47 (6) |
Cu2a—Cu4aiv | 3.0971 (10) | Cl2c—H4c | 3.15 (6) |
Cu2a—O1a | 2.398 (5) | Cl2c—H1axx | 2.23 (5) |
Cu2a—O1aiv | 2.398 (5) | Cl2c—H3bxx | 2.19 (6) |
Cu2a—O2bv | 2.019 (4) | Cl2c—H2cix | 3.16 (6) |
Cu2a—O2bi | 2.019 (4) | O1a—O2bi | 2.660 (7) |
Cu2a—O3a | 2.004 (5) | O1a—O3a | 2.701 (8) |
Cu2a—O3aiv | 2.004 (5) | O1a—O3aiv | 3.498 (7) |
Cu2a—H3a | 2.53 (8) | O1a—O3biii | 2.935 (7) |
Cu2a—H3aiv | 2.53 (8) | O1a—O4b | 2.921 (7) |
Cu2a—H1a | 2.97 (6) | O1a—H4b | 2.79 (6) |
Cu2a—H1aiv | 2.97 (6) | O1a—H4biii | 3.31 (7) |
Cu2a—H2bv | 2.48 (10) | O1a—H3a | 3.46 (8) |
Cu2a—H2bi | 2.48 (10) | O1a—H1a | 0.99 (6) |
Cu2b—Cu3b | 3.0042 (9) | O1a—H2bi | 3.36 (8) |
Cu2b—Cu3bvi | 3.0042 (9) | O1a—H3b | 3.29 (7) |
Cu2b—Cu3cvii | 3.0965 (10) | O1a—H3biii | 2.82 (6) |
Cu2b—Cu3ci | 3.0965 (10) | O1b—O2cvii | 3.445 (7) |
Cu2b—Cu4b | 3.1029 (7) | O1b—O2ci | 2.640 (8) |
Cu2b—Cu4bvi | 3.1029 (7) | O1b—O3b | 2.655 (8) |
Cu2b—O1b | 2.308 (6) | O1b—O3bvi | 3.422 (7) |
Cu2b—O1bvi | 2.308 (6) | O1b—O3cxix | 2.946 (7) |
Cu2b—O2cvii | 2.023 (5) | O1b—O4c | 3.007 (8) |
Cu2b—O2ci | 2.023 (5) | O1b—H4c | 3.15 (6) |
Cu2b—O3b | 2.013 (4) | O1b—H4cxix | 3.31 (7) |
Cu2b—O3bvi | 2.013 (4) | O1b—H3cxix | 3.33 (5) |
Cu2b—H3b | 2.66 (6) | O1b—H2cvii | 3.11 (6) |
Cu2b—H3bvi | 2.66 (6) | O1b—H2ci | 3.17 (6) |
Cu2b—H2cvii | 2.13 (6) | O1b—H1b | 0.98 (7) |
Cu2b—H2ci | 2.13 (6) | O1c—O2aviii | 3.494 (7) |
Cu2b—H1b | 2.92 (6) | O1c—O2ai | 2.660 (9) |
Cu2b—H1bvi | 2.92 (6) | O1c—O3ax | 3.041 (7) |
Cu2c—Cu3aviii | 3.1251 (7) | O1c—O3c | 2.543 (7) |
Cu2c—Cu3ai | 3.1251 (7) | O1c—O3cxi | 3.144 (6) |
Cu2c—Cu3cix | 3.0724 (11) | O1c—O4a | 2.965 (7) |
Cu2c—Cu3cx | 3.0724 (11) | O1c—H4a | 3.48 (6) |
Cu2c—Cu4c | 3.0040 (9) | O1c—H3ax | 3.19 (7) |
Cu2c—Cu4cxi | 3.0040 (9) | O1c—H2aviii | 3.33 (8) |
Cu2c—O1c | 2.064 (5) | O1c—H3c | 3.09 (6) |
Cu2c—O1cxi | 2.064 (5) | O1c—H3cxi | 2.64 (6) |
Cu2c—O2aviii | 2.319 (6) | O1c—H1c | 1.02 (5) |
Cu2c—O2ai | 2.319 (6) | O2a—O2bxv | 3.000 (8) |
Cu2c—O3c | 1.979 (4) | O2a—O2cxiii | 2.948 (8) |
Cu2c—O3cxi | 1.979 (4) | O2a—O3cxvi | 3.404 (7) |
Cu2c—H2aviii | 2.73 (9) | O2a—O3ci | 2.646 (8) |
Cu2c—H2ai | 2.73 (9) | O2a—H2bxxi | 3.32 (9) |
Cu2c—H3c | 2.00 (6) | O2a—H2bxv | 3.34 (6) |
Cu2c—H3cxi | 2.00 (6) | O2a—H2a | 0.99 (7) |
Cu2c—H1c | 2.38 (9) | O2a—H3cxvi | 2.84 (5) |
Cu2c—H1cxi | 2.38 (9) | O2a—H3ci | 3.27 (6) |
Cu3a—Cu3bxii | 3.4204 (11) | O2a—H1cxvi | 3.03 (8) |
Cu3a—Cu3cxiii | 3.4262 (11) | O2a—H2cxiii | 3.10 (6) |
Cu3a—Cu4axiv | 3.4188 (11) | O2b—O2cxxii | 3.033 (7) |
Cu3a—Cu4ci | 3.4162 (11) | O2b—O3axxiii | 3.093 (7) |
Cu3a—Cl2axiv | 2.7563 (19) | O2b—O3ai | 2.572 (8) |
Cu3a—Cl2ci | 2.8378 (18) | O2b—H3axxiii | 2.99 (8) |
Cu3a—O1ci | 2.017 (5) | O2b—H3ai | 3.46 (8) |
Cu3a—O2a | 1.949 (6) | O2b—H1ai | 3.44 (6) |
Cu3a—O2bxv | 2.034 (5) | O2b—H2b | 1.03 (6) |
Cu3a—O3axiv | 1.990 (6) | O2b—H2axxiv | 3.30 (8) |
Cu3a—H3axiv | 2.67 (7) | O2b—H2axv | 3.29 (7) |
Cu3a—H2bxv | 2.85 (5) | O2c—O3bxxv | 3.122 (6) |
Cu3a—H2a | 2.71 (7) | O2c—O3bi | 2.557 (7) |
Cu3a—H3cxvi | 2.97 (5) | O2c—H2bxxii | 2.96 (7) |
Cu3a—H1ci | 2.94 (4) | O2c—H2axiii | 2.87 (7) |
Cu3b—Cu3ci | 3.4252 (16) | O2c—H3bxxv | 3.25 (6) |
Cu3b—Cu4aiii | 3.4315 (16) | O2c—H3bi | 3.43 (7) |
Cu3b—Cu4b | 3.4134 (11) | O2c—H2c | 1.01 (5) |
Cu3b—Cl2aiii | 2.8165 (19) | O2c—H1bi | 3.49 (6) |
Cu3b—Cl2b | 2.7604 (18) | O3a—O4a | 2.944 (8) |
Cu3b—O1aiii | 1.943 (5) | O3a—H4a | 3.46 (6) |
Cu3b—O2bxvii | 1.986 (5) | O3a—H3a | 0.98 (8) |
Cu3b—O2ci | 2.009 (5) | O3a—H2bv | 2.85 (9) |
Cu3b—O3b | 1.986 (5) | O3a—H2bi | 3.49 (8) |
Cu3b—H3axiv | 3.42 (7) | O3b—O4b | 3.051 (7) |
Cu3b—H1aiii | 2.42 (6) | O3b—H4b | 2.92 (7) |
Cu3b—H2bxvii | 2.39 (6) | O3b—H1a | 3.42 (6) |
Cu3b—H3b | 2.51 (7) | O3b—H1aiii | 2.83 (6) |
Cu3b—H2ci | 2.84 (4) | O3b—H3b | 0.99 (6) |
Cu3c—Cu4bi | 3.4297 (10) | O3b—H2cvii | 2.53 (6) |
Cu3c—Cu4cxviii | 3.4223 (16) | O3b—H2ci | 3.28 (5) |
Cu3c—Cl2bi | 2.7874 (16) | O3b—H1b | 3.49 (7) |
Cu3c—Cl2cxviii | 2.7709 (16) | O3c—O4c | 3.027 (6) |
Cu3c—O1bi | 1.946 (5) | O3c—H4c | 2.99 (6) |
Cu3c—O2axiii | 1.955 (6) | O3c—H2aviii | 3.45 (8) |
Cu3c—O2c | 2.005 (6) | O3c—H2ai | 3.29 (8) |
Cu3c—O3cxviii | 2.010 (5) | O3c—H3c | 0.95 (5) |
Cu3c—H2axiii | 2.35 (6) | O3c—H1c | 3.00 (8) |
Cu3c—H3cxviii | 2.66 (5) | O3c—H1cxi | 3.18 (8) |
Cu3c—H1cx | 3.28 (6) | O3c—H1b | 3.48 (6) |
Cu3c—H2c | 2.46 (6) | O3c—H1bxix | 2.90 (6) |
Cu3c—H1bi | 2.51 (6) | O4a—O4b | 2.650 (8) |
Cu4a—Cu4b | 3.4173 (11) | O4a—O4bi | 3.409 (7) |
Cu4a—Cu4c | 3.4316 (16) | O4a—O4c | 2.636 (7) |
Cu4a—Cl1a | 2.7751 (17) | O4a—O4ci | 3.500 (6) |
Cu4a—Cl2a | 2.7875 (17) | O4a—H4a | 1.00 (5) |
Cu4a—O1a | 1.951 (5) | O4a—H4c | 3.39 (7) |
Cu4a—O3a | 2.022 (5) | O4a—H4ci | 3.49 (7) |
Cu4a—O4a | 1.955 (6) | O4a—H3a | 2.81 (7) |
Cu4a—O4b | 2.010 (5) | O4a—H1c | 2.75 (7) |
Cu4a—H4b | 2.55 (7) | O4b—O4c | 2.571 (8) |
Cu4a—H4a | 2.56 (6) | O4b—O4ci | 3.156 (7) |
Cu4a—H4ci | 3.39 (6) | O4b—H4b | 1.01 (7) |
Cu4a—H3a | 2.45 (7) | O4b—H4a | 3.03 (6) |
Cu4a—H1a | 2.62 (5) | O4b—H4ai | 2.75 (6) |
Cu4a—H2bv | 3.30 (7) | O4b—H4c | 3.42 (7) |
Cu4b—Cu4c | 3.4255 (10) | O4b—H4ci | 3.06 (7) |
Cu4b—Cl1a | 2.7779 (17) | O4b—H1a | 3.02 (5) |
Cu4b—Cl2b | 2.8252 (17) | O4b—H1aiii | 3.31 (6) |
Cu4b—O1b | 1.957 (6) | O4b—H3b | 2.97 (6) |
Cu4b—O3b | 2.030 (5) | O4c—H4b | 3.46 (7) |
Cu4b—O4b | 1.990 (5) | O4c—H4bi | 3.31 (6) |
Cu4b—O4c | 2.018 (5) | O4c—H4a | 3.03 (6) |
Cu4b—H4b | 2.49 (7) | O4c—H4ai | 2.85 (6) |
Cu4b—H4ai | 3.01 (5) | O4c—H4c | 0.97 (7) |
Cu4b—H4c | 2.67 (6) | O4c—H3c | 3.41 (6) |
Cu4b—H3b | 2.55 (6) | O4c—H1b | 2.92 (7) |
Cu4b—H2cvii | 3.02 (5) | O4c—H1bxix | 3.31 (7) |
Cu4b—H1b | 2.48 (7) | H4b—H4ai | 2.89 (9) |
Cu4c—Cl1a | 2.8101 (19) | H4b—H4ci | 3.08 (9) |
Cu4c—Cl2c | 2.7635 (18) | H4b—H1a | 2.70 (8) |
Cu4c—O1c | 1.970 (5) | H4b—H1aiii | 2.39 (9) |
Cu4c—O3c | 2.004 (5) | H4b—H3b | 2.72 (8) |
Cu4c—O4a | 1.957 (5) | H4b—H3biii | 2.79 (9) |
Cu4c—O4c | 1.986 (5) | H4a—H4ci | 2.94 (9) |
Cu4c—H4a | 2.59 (6) | H4a—H3a | 3.43 (9) |
Cu4c—H4c | 2.45 (6) | H4a—H3ax | 3.27 (10) |
Cu4c—H3c | 2.60 (6) | H4a—H1c | 3.46 (9) |
Cu4c—H1c | 2.15 (6) | H4c—H3c | 3.45 (8) |
Cl1a—O2aviii | 3.082 (6) | H4c—H3cxix | 3.41 (9) |
Cl1a—O2bv | 3.099 (5) | H4c—H1b | 2.91 (9) |
Cl1a—O2cvii | 3.058 (5) | H4c—H1bxix | 2.48 (10) |
Cl1a—O4a | 3.130 (5) | H3a—H2bv | 2.54 (11) |
Cl1a—O4b | 3.227 (5) | H3a—H1c | 2.69 (11) |
Cl1a—O4c | 3.244 (4) | H1a—H1aiii | 3.30 (8) |
Cl1a—H3a | 3.32 (7) | H1a—H3b | 2.52 (9) |
Cl1a—H2bv | 2.19 (7) | H1a—H3biii | 2.59 (8) |
Cl1a—H2aviii | 2.18 (6) | H2b—H2axxiv | 2.41 (12) |
Cl1a—H3c | 3.39 (6) | H2b—H2axv | 3.47 (10) |
Cl1a—H1c | 3.03 (5) | H2b—H1cxxiii | 3.41 (7) |
Cl1a—H3b | 3.40 (6) | H2b—H2cxxvi | 3.36 (10) |
Cl1a—H2cvii | 2.18 (6) | H2a—H3cxvi | 2.98 (10) |
Cl2a—O1a | 3.115 (5) | H2a—H1cxvi | 2.66 (10) |
Cl2a—O1bxviii | 3.096 (6) | H2a—H2cxxvii | 3.31 (10) |
Cl2a—O2bi | 3.257 (5) | H2a—H2cxiii | 3.20 (9) |
Cl2a—O3a | 3.230 (5) | H3c—H1c | 3.32 (11) |
Cl2a—O3cxviii | 3.067 (5) | H3c—H1cxi | 2.88 (9) |
Cl2a—O4ci | 3.103 (5) | H3c—H1b | 3.10 (9) |
Cl2a—H4a | 3.40 (6) | H3c—H1bxix | 3.27 (8) |
Cl2a—H4ci | 2.20 (6) | H3b—H2cvii | 2.57 (8) |
Cl2a—H3cxviii | 2.22 (6) | H2c—H1bxxv | 3.34 (9) |
Cl2a—H1bxviii | 2.27 (6) | H1b—H1bxix | 3.37 (8) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y, z−1; (iii) −x+1, −y, −z+1; (iv) −x+1, −y, −z; (v) x, y−1, z−1; (vi) −x, −y, −z+1; (vii) x−1, y−1, z; (viii) x−1, y, z−1; (ix) x−1, 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, y−1, z; (xviii) x+1, y, z; (xix) −x, −y+1, −z+1; (xx) x, y+1, z; (xxi) x+1, y−1, z; (xxii) −x+1, −y+2, −z+1; (xxiii) x, y+1, z+1; (xxiv) x−1, y+1, z; (xxv) x+1, y+1, z; (xxvi) x−1, y, z+1; (xxvii) x, y−1, z+1. |
Selected geometric parameters (Å, º) for (II) top
Cu1—O1 | 2.157 (3) | Cu3—Cl1ix | 2.7911 (10) |
Cu1—O1i | 2.157 (3) | Cu3—O1 | 1.973 (3) |
Cu1—O2ii | 2.108 (3) | Cu3—O2 | 1.978 (3) |
Cu1—O2iii | 2.108 (3) | Cu3—O2ii | 1.982 (3) |
Cu1—O3 | 2.052 (3) | Cu3—O3x | 1.993 (3) |
Cu1—O3i | 2.052 (3) | Cu3—H1 | 2.53 (10) |
Cu1—H1 | 2.49 (10) | Cu3—H3x | 2.59 (10) |
Cu1—H1i | 2.49 (10) | Cu3—H2 | 2.63 (4) |
Cu1—H3 | 2.49 (11) | Cu3—H2ii | 2.63 (4) |
Cu1—H3i | 2.49 (11) | Cl1—H1 | 2.09 (9) |
Cu1—H2ii | 2.17 (15) | Cl1—H3xi | 2.10 (9) |
Cu1—H2iii | 2.17 (15) | Cl1—H2vii | 2.15 (8) |
Cu2—Cl1 | 2.7812 (9) | O1—O2 | 2.983 (4) |
Cu2—Cl1iv | 2.7812 (9) | O1—O2ii | 2.611 (5) |
Cu2—O1v | 1.975 (3) | O1—O3 | 2.591 (4) |
Cu2—O1iii | 1.975 (3) | O1—O3xii | 2.993 (5) |
Cu2—O3v | 1.984 (3) | O1—H1 | 0.99 (9) |
Cu2—O3iii | 1.984 (3) | O2—O3x | 2.584 (5) |
Cu2—H1v | 2.64 (11) | O2—H2 | 1.00 (3) |
Cu2—H1iii | 2.64 (11) | O3—H3 | 0.99 (9) |
Cu2—H3v | 2.58 (11) | H1—H3xi | 2.80 (11) |
Cu2—H3iii | 2.58 (11) | H1—H3i | 2.9 (2) |
Cu2—H2vi | 3.00 (9) | H1—H2iii | 2.79 (13) |
Cu2—H2vii | 3.00 (9) | H3—H2iii | 2.69 (13) |
Cu3—Cl1viii | 2.7690 (10) | ||
O1—Cu1—O1i | 180 | Cu2—Cl1—H1 | 137 (2) |
O1—Cu1—O2ii | 75.48 (11) | Cu2—Cl1—H3xi | 136 (2) |
O1—Cu1—O2iii | 104.52 (11) | Cu2—Cl1—H2vii | 74 (4) |
O1—Cu1—O3 | 75.95 (12) | Cu3viii—Cl1—Cu3iii | 75.85 (3) |
O1—Cu1—O3i | 104.05 (12) | Cu3viii—Cl1—H1 | 133 (4) |
O1—Cu1—H1 | 23 (2) | Cu3viii—Cl1—H3xi | 84 (4) |
O1—Cu1—H1i | 157 (2) | Cu3viii—Cl1—H2vii | 133 (3) |
O1—Cu1—H3 | 94 (3) | Cu3iii—Cl1—Cu3viii | 75.85 (3) |
O1—Cu1—H3i | 86 (3) | Cu3iii—Cl1—H1 | 82 (3) |
O1—Cu1—H2ii | 96.4 (13) | Cu3iii—Cl1—H3xi | 136 (4) |
O1—Cu1—H2iii | 83.6 (13) | Cu3iii—Cl1—H2vii | 129 (2) |
O1i—Cu1—O1 | 180 | H1—Cl1—H3xi | 84 (3) |
O1i—Cu1—O2ii | 104.52 (11) | H1—Cl1—H2vii | 93 (5) |
O1i—Cu1—O2iii | 75.48 (11) | H3xi—Cl1—H2vii | 93 (5) |
O1i—Cu1—O3 | 104.05 (12) | Cu1—O1—Cu2xiii | 95.50 (12) |
O1i—Cu1—O3i | 75.95 (12) | Cu1—O1—Cu3 | 96.35 (14) |
O1i—Cu1—H1 | 157 (2) | Cu1—O1—O2 | 133.37 (16) |
O1i—Cu1—H1i | 23 (2) | Cu1—O1—O2ii | 51.41 (10) |
O1i—Cu1—H3 | 86 (3) | Cu1—O1—O3 | 50.18 (9) |
O1i—Cu1—H3i | 94 (3) | Cu1—O1—O3xii | 132.91 (14) |
O1i—Cu1—H2ii | 83.6 (13) | Cu1—O1—H1 | 97 (7) |
O1i—Cu1—H2iii | 96.4 (13) | Cu1—O1—H2iii | 48 (2) |
O2ii—Cu1—O2iii | 180 | Cu2xiii—O1—Cu3 | 120.20 (14) |
O2ii—Cu1—O3 | 76.80 (11) | Cu2xiii—O1—O2 | 119.98 (14) |
O2ii—Cu1—O3i | 103.20 (11) | Cu2xiii—O1—O2ii | 101.79 (13) |
O2ii—Cu1—H1 | 92 (2) | Cu2xiii—O1—O3 | 49.27 (10) |
O2ii—Cu1—H1i | 88 (2) | Cu2xiii—O1—H1 | 123 (7) |
O2ii—Cu1—H3 | 95 (2) | Cu2xiii—O1—H2iii | 73.6 (9) |
O2ii—Cu1—H3i | 85 (2) | Cu3—O1—O2ii | 48.84 (10) |
O2ii—Cu1—H2ii | 26.9 (12) | Cu3—O1—O3 | 101.97 (14) |
O2ii—Cu1—H2iii | 153.1 (12) | Cu3—O1—O3xii | 118.96 (14) |
O2iii—Cu1—O2ii | 180 | Cu3—O1—H1 | 113 (6) |
O2iii—Cu1—O3 | 103.20 (11) | Cu3—O1—H2iii | 144.6 (19) |
O2iii—Cu1—O3i | 76.80 (11) | O2—O1—O2ii | 89.87 (13) |
O2iii—Cu1—H1 | 88 (2) | O2—O1—O3 | 136.27 (14) |
O2iii—Cu1—H1i | 92 (2) | O2—O1—O3xii | 91.94 (12) |
O2iii—Cu1—H3 | 85 (2) | O2—O1—H1 | 88 (5) |
O2iii—Cu1—H3i | 95 (2) | O2—O1—H2iii | 162.5 (14) |
O2iii—Cu1—H2ii | 153.1 (12) | O2ii—O1—O2 | 89.87 (13) |
O2iii—Cu1—H2iii | 26.9 (12) | O2ii—O1—O3 | 59.56 (12) |
O3—Cu1—O3i | 180 | O2ii—O1—O3xii | 135.08 (14) |
O3—Cu1—H1 | 95 (3) | O2ii—O1—H1 | 129 (8) |
O3—Cu1—H1i | 85 (3) | O2ii—O1—H2iii | 98 (2) |
O3—Cu1—H3 | 23 (3) | O3—O1—O3xii | 90.27 (13) |
O3—Cu1—H3i | 157 (3) | O3—O1—H1 | 135 (5) |
O3—Cu1—H2ii | 98.0 (13) | O3—O1—H2iii | 60.5 (17) |
O3—Cu1—H2iii | 82.0 (13) | O3xii—O1—O3 | 90.27 (13) |
O3i—Cu1—O3 | 180 | O3xii—O1—H1 | 96 (8) |
O3i—Cu1—H1 | 85 (3) | O3xii—O1—H2iii | 93.1 (15) |
O3i—Cu1—H1i | 95 (3) | H1—O1—H2iii | 75 (5) |
O3i—Cu1—H3 | 157 (3) | Cu1x—O2—Cu3 | 96.11 (14) |
O3i—Cu1—H3i | 23 (3) | Cu1x—O2—Cu3x | 97.67 (14) |
O3i—Cu1—H2ii | 82.0 (13) | Cu1x—O2—O1 | 132.83 (13) |
O3i—Cu1—H2iii | 98.0 (13) | Cu1x—O2—O1x | 53.11 (10) |
H1—Cu1—H1i | 180 | Cu1x—O2—O3x | 50.62 (10) |
H1—Cu1—H3 | 108 (4) | Cu1x—O2—H2 | 80 (9) |
H1—Cu1—H3i | 72 (4) | Cu3—O2—Cu3x | 119.32 (15) |
H1—Cu1—H2ii | 107 (3) | Cu3—O2—O1x | 101.82 (15) |
H1—Cu1—H2iii | 73 (3) | Cu3—O2—O3x | 49.66 (10) |
H1i—Cu1—H1 | 180 | Cu3—O2—H2 | 120 (3) |
H1i—Cu1—H3 | 72 (4) | Cu3x—O2—Cu3 | 119.32 (15) |
H1i—Cu1—H3i | 108 (4) | Cu3x—O2—O1 | 118.40 (14) |
H1i—Cu1—H2ii | 73 (3) | Cu3x—O2—O1x | 48.54 (10) |
H1i—Cu1—H2iii | 107 (3) | Cu3x—O2—O3x | 101.95 (15) |
H3—Cu1—H3i | 180 | Cu3x—O2—H2 | 120 (3) |
H3—Cu1—H2ii | 110 (3) | O1—O2—O1x | 135.01 (15) |
H3—Cu1—H2iii | 70 (3) | O1—O2—O3x | 90.58 (12) |
H3i—Cu1—H3 | 180 | O1—O2—H2 | 104 (6) |
H3i—Cu1—H2ii | 70 (3) | O1x—O2—O1 | 135.01 (15) |
H3i—Cu1—H2iii | 110 (3) | O1x—O2—O3x | 59.83 (12) |
H2ii—Cu1—H2iii | 180 | O1x—O2—H2 | 120 (7) |
H2iii—Cu1—H2ii | 180 | O3x—O2—H2 | 119 (8) |
Cl1—Cu2—Cl1iv | 180 | Cu1—O3—Cu2xiii | 98.66 (12) |
Cl1—Cu2—O1v | 97.97 (8) | Cu1—O3—Cu3ii | 97.45 (13) |
Cl1—Cu2—O1iii | 82.03 (8) | Cu1—O3—O1 | 53.87 (10) |
Cl1—Cu2—O3v | 97.44 (8) | Cu1—O3—O1xii | 135.23 (14) |
Cl1—Cu2—O3iii | 82.56 (8) | Cu1—O3—O2ii | 52.58 (10) |
Cl1—Cu2—H1v | 82 (2) | Cu1—O3—H3 | 105 (8) |
Cl1—Cu2—H1iii | 98 (2) | Cu1—O3—H2iii | 51 (2) |
Cl1—Cu2—H3v | 81 (2) | Cu2xiii—O3—Cu3ii | 118.60 (13) |
Cl1—Cu2—H3iii | 99 (2) | Cu2xiii—O3—O1 | 48.96 (10) |
Cl1—Cu2—H2vi | 136 (3) | Cu2xiii—O3—O2ii | 102.45 (13) |
Cl1—Cu2—H2vii | 44 (3) | Cu2xiii—O3—H3 | 116 (8) |
Cl1iv—Cu2—Cl1 | 180 | Cu2xiii—O3—H2iii | 76.3 (9) |
Cl1iv—Cu2—O1v | 82.03 (8) | Cu3ii—O3—O1 | 102.06 (13) |
Cl1iv—Cu2—O1iii | 97.97 (8) | Cu3ii—O3—O1xii | 116.98 (13) |
Cl1iv—Cu2—O3v | 82.56 (8) | Cu3ii—O3—O2ii | 49.14 (9) |
Cl1iv—Cu2—O3iii | 97.44 (8) | Cu3ii—O3—H3 | 116 (6) |
Cl1iv—Cu2—H1v | 98 (2) | Cu3ii—O3—H2iii | 148.0 (19) |
Cl1iv—Cu2—H1iii | 82 (2) | O1—O3—O1xii | 89.73 (13) |
Cl1iv—Cu2—H3v | 99 (2) | O1—O3—O2ii | 60.60 (12) |
Cl1iv—Cu2—H3iii | 81 (2) | O1—O3—H3 | 139 (5) |
Cl1iv—Cu2—H2vi | 44 (3) | O1—O3—H2iii | 65.0 (16) |
Cl1iv—Cu2—H2vii | 136 (3) | O1xii—O3—O1 | 89.73 (13) |
O1v—Cu2—O1iii | 180 | O1xii—O3—O2ii | 135.29 (13) |
O1v—Cu2—O3v | 81.76 (13) | O1xii—O3—H3 | 86 (9) |
O1v—Cu2—O3iii | 98.24 (13) | O1xii—O3—H2iii | 92.9 (16) |
O1v—Cu2—H1v | 18 (2) | O2ii—O3—H3 | 139 (9) |
O1v—Cu2—H1iii | 162 (2) | O2ii—O3—H2iii | 102 (2) |
O1v—Cu2—H3v | 96 (3) | H3—O3—H2iii | 75 (5) |
O1v—Cu2—H3iii | 84 (3) | Cu1—H1—Cu2xiii | 73 (2) |
O1v—Cu2—H2vi | 112.8 (19) | Cu1—H1—Cl1 | 120 (5) |
O1v—Cu2—H2vii | 67.2 (19) | Cu1—H1—O1 | 59 (5) |
O1iii—Cu2—O1v | 180 | Cu1—H1—H3xi | 147 (6) |
O1iii—Cu2—O3v | 98.24 (13) | Cu1—H1—H3i | 54 (3) |
O1iii—Cu2—O3iii | 81.76 (13) | Cu1—H1—H2iii | 48 (3) |
O1iii—Cu2—H1v | 162 (2) | Cu2xiii—H1—Cu3 | 83 (3) |
O1iii—Cu2—H1iii | 18 (2) | Cu2xiii—H1—Cl1 | 135 (5) |
O1iii—Cu2—H3v | 84 (3) | Cu2xiii—H1—H3xi | 139 (6) |
O1iii—Cu2—H3iii | 96 (3) | Cu2xiii—H1—H3i | 126 (4) |
O1iii—Cu2—H2vi | 67.2 (19) | Cu2xiii—H1—H2iii | 67 (2) |
O1iii—Cu2—H2vii | 112.8 (19) | Cu3—H1—Cl1 | 141 (5) |
O3v—Cu2—O3iii | 180 | Cu3—H1—O1 | 46 (5) |
O3v—Cu2—H1v | 92 (3) | Cu3—H1—H3xi | 98 (3) |
O3v—Cu2—H1iii | 88 (3) | Cu3—H1—H3i | 74 (4) |
O3v—Cu2—H3v | 20 (3) | Cu3—H1—H2iii | 121 (4) |
O3v—Cu2—H3iii | 160 (3) | Cl1—H1—O1 | 174 (9) |
O3v—Cu2—H2vi | 116 (2) | Cl1—H1—H3xi | 48 (3) |
O3v—Cu2—H2vii | 64 (2) | Cl1—H1—H3i | 87 (4) |
O3iii—Cu2—O3v | 180 | Cl1—H1—H2iii | 90 (4) |
O3iii—Cu2—H1v | 88 (3) | O1—H1—H3xi | 136 (7) |
O3iii—Cu2—H1iii | 92 (3) | O1—H1—H3i | 97 (8) |
O3iii—Cu2—H3v | 160 (3) | O1—H1—H2iii | 85 (6) |
O3iii—Cu2—H3iii | 20 (3) | H3xi—H1—H3i | 92 (5) |
O3iii—Cu2—H2vi | 64 (2) | H3xi—H1—H2iii | 138 (5) |
O3iii—Cu2—H2vii | 116 (2) | H3i—H1—H3xi | 92 (5) |
H1v—Cu2—H1iii | 180 | H3i—H1—H2iii | 84 (4) |
H1v—Cu2—H3v | 102 (4) | Cu1—H3—Cu2xiii | 74 (2) |
H1v—Cu2—H3iii | 78 (4) | Cu1—H3—Cu3ii | 73 (3) |
H1v—Cu2—H2vi | 121 (3) | Cu1—H3—Cl1xiv | 119 (6) |
H1v—Cu2—H2vii | 59 (3) | Cu1—H3—O3 | 53 (6) |
H1iii—Cu2—H1v | 180 | Cu1—H3—H1xiv | 142 (7) |
H1iii—Cu2—H3v | 78 (4) | Cu1—H3—H1i | 54 (3) |
H1iii—Cu2—H3iii | 102 (4) | Cu1—H3—H2iii | 49 (3) |
H1iii—Cu2—H2vi | 59 (3) | Cu2xiii—H3—Cu3ii | 83 (3) |
H1iii—Cu2—H2vii | 121 (3) | Cu2xiii—H3—Cl1xiv | 138 (6) |
H3v—Cu2—H3iii | 180 | Cu2xiii—H3—H1xiv | 142 (6) |
H3v—Cu2—H2vi | 123 (3) | Cu2xiii—H3—H1i | 127 (4) |
H3v—Cu2—H2vii | 57 (3) | Cu2xiii—H3—H2iii | 69 (2) |
H3iii—Cu2—H3v | 180 | Cu3ii—H3—Cl1xiv | 138 (5) |
H3iii—Cu2—H2vi | 57 (3) | Cu3ii—H3—H1xiv | 96 (3) |
H3iii—Cu2—H2vii | 123 (3) | Cu3ii—H3—H1i | 72 (4) |
H2vi—Cu2—H2vii | 180 | Cu3ii—H3—H2iii | 121 (5) |
H2vii—Cu2—H2vi | 180 | Cl1xiv—H3—O3 | 171 (11) |
Cl1viii—Cu3—Cl1ix | 178.23 (3) | Cl1xiv—H3—H1xiv | 48 (3) |
Cl1viii—Cu3—O1 | 98.32 (10) | Cl1xiv—H3—H1i | 84 (5) |
Cl1viii—Cu3—O2 | 82.69 (8) | Cl1xiv—H3—H2iii | 89 (4) |
Cl1viii—Cu3—O2ii | 96.23 (8) | O3—H3—H1xiv | 138 (7) |
Cl1viii—Cu3—O3x | 82.72 (9) | O3—H3—H1i | 90 (9) |
Cl1viii—Cu3—H1 | 80 (3) | O3—H3—H2iii | 84 (6) |
Cl1viii—Cu3—H3x | 99 (3) | H1xiv—H3—H1i | 88 (5) |
Cl1viii—Cu3—H2 | 101.7 (10) | H1xiv—H3—H2iii | 137 (5) |
Cl1viii—Cu3—H2ii | 77.3 (11) | H1i—H3—H1xiv | 88 (5) |
Cl1ix—Cu3—Cl1viii | 178.23 (3) | H1i—H3—H2iii | 84 (4) |
Cl1ix—Cu3—O1 | 81.80 (9) | Cu1x—H2—Cu2xv | 71 (3) |
Cl1ix—Cu3—O2 | 99.05 (8) | Cu1x—H2—Cu3 | 78 (3) |
Cl1ix—Cu3—O2ii | 82.03 (8) | Cu1x—H2—Cu3x | 79 (3) |
Cl1ix—Cu3—O3x | 97.19 (9) | Cu1x—H2—Cl1vii | 133 (5) |
Cl1ix—Cu3—H1 | 101 (3) | Cu1x—H2—O1ix | 48 (3) |
Cl1ix—Cu3—H3x | 81 (3) | Cu1x—H2—O2 | 73 (8) |
Cl1ix—Cu3—H2 | 80.1 (10) | Cu1x—H2—O3ix | 47 (3) |
Cl1ix—Cu3—H2ii | 101.0 (11) | Cu1x—H2—H1ix | 59 (4) |
O1—Cu3—O2 | 98.04 (14) | Cu1x—H2—H3ix | 61 (4) |
O1—Cu3—O2ii | 82.62 (14) | Cu2xv—H2—Cu3 | 128 (4) |
O1—Cu3—O3x | 178.63 (13) | Cu2xv—H2—Cu3x | 130 (4) |
O1—Cu3—H1 | 21 (2) | Cu2xv—H2—Cl1vii | 62.8 (13) |
O1—Cu3—H3x | 160 (2) | Cu2xv—H2—O2 | 144 (11) |
O1—Cu3—H2 | 93 (3) | Cu2xv—H2—H1ix | 54 (3) |
O1—Cu3—H2ii | 88 (3) | Cu2xv—H2—H3ix | 54 (3) |
O2—Cu3—O2ii | 178.80 (13) | Cu3—H2—Cu3x | 81.1 (9) |
O2—Cu3—O3x | 81.20 (13) | Cu3—H2—Cl1vii | 130 (4) |
O2—Cu3—H1 | 86 (2) | Cu3—H2—O1ix | 89 (3) |
O2—Cu3—H3x | 95 (2) | Cu3—H2—O3ix | 125 (5) |
O2—Cu3—H2 | 19.1 (11) | Cu3—H2—H1ix | 74 (3) |
O2—Cu3—H2ii | 159.8 (11) | Cu3—H2—H3ix | 136 (6) |
O2ii—Cu3—O2 | 178.80 (13) | Cu3x—H2—Cu3 | 81.1 (9) |
O2ii—Cu3—O3x | 98.16 (14) | Cu3x—H2—Cl1vii | 134 (5) |
O2ii—Cu3—H1 | 94 (2) | Cu3x—H2—O1ix | 127 (5) |
O2ii—Cu3—H3x | 85 (2) | Cu3x—H2—O3ix | 90 (3) |
O2ii—Cu3—H2 | 162.0 (11) | Cu3x—H2—H1ix | 134 (6) |
O2ii—Cu3—H2ii | 19.1 (11) | Cu3x—H2—H3ix | 77 (4) |
O3x—Cu3—H1 | 160 (2) | Cl1vii—H2—O1ix | 91 (2) |
O3x—Cu3—H3x | 20 (2) | Cl1vii—H2—O2 | 153 (12) |
O3x—Cu3—H2 | 86 (3) | Cl1vii—H2—O3ix | 94 (2) |
O3x—Cu3—H2ii | 93 (3) | Cl1vii—H2—H1ix | 91 (3) |
H1—Cu3—H3x | 178 (5) | Cl1vii—H2—H3ix | 92 (4) |
H1—Cu3—H2 | 87 (4) | O1ix—H2—O2 | 111 (9) |
H1—Cu3—H2ii | 93 (4) | O1ix—H2—O3ix | 55 (3) |
H3x—Cu3—H2 | 95 (4) | O1ix—H2—H3ix | 75 (4) |
H3x—Cu3—H2ii | 85 (4) | O2—H2—O3ix | 111 (9) |
H2—Cu3—H2ii | 179 (2) | O2—H2—H1ix | 105 (7) |
H2ii—Cu3—H2 | 179 (2) | O2—H2—H3ix | 108 (8) |
Cu2—Cl1—Cu3viii | 76.08 (3) | O3ix—H2—H1ix | 74 (4) |
Cu2—Cl1—Cu3iii | 75.79 (2) | H1ix—H2—H3ix | 95 (5) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1/2, y+1/2, −z+3/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) −x, −y, −z; (v) −x+1/2, y−1/2, −z+1/2; (vi) x−1, y, z−1; (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, y−1/2, −z+3/2; (xi) x, y−1, 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. |