Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614019921/ry5062sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520614019921/ry5062Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052520614019921/ry5062sup3.pdf |
CCDC reference: 1022754
Data collection: APEX2 v2013.4-1 (Bruker AXS, 2013); cell refinement: APEX2 v2013.4-1 (Bruker AXS, 2013); data reduction: APEX2 v2013.4-1 (Bruker AXS, 2013); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND for Windows (Klaus, 2004); software used to prepare material for publication: enCIFer 1.3 (Allen et al., 2004)).
Co(C6H8N2)3Cr(C2O4)3.6H2O | F(000) = 1668 |
Mr = 807.52 | Dx = 1.612 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.1923 (8) Å | θ = 2.3–31.6° |
b = 18.0299 (10) Å | µ = 0.91 mm−1 |
c = 14.1801 (9) Å | T = 100 K |
β = 99.357 (2)° | Prismatic, brown |
V = 3327.9 (3) Å3 | 0.18 × 0.12 × 0.10 mm |
Z = 4 |
D8 Venture Photon, Bruker AXS diffractometer | 10353 independent reflections |
Radiation source: fine-focus sealed tube | 8042 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.054 |
ω–scans | θmax = 31.6°, θmin = 2.3° |
Absorption correction: multi-scan APEX2 v2013.4-1 (Bruker AXS, 2013) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. | h = −18→19 |
Tmin = 0.693, Tmax = 0.746 | k = −26→26 |
100946 measured reflections | l = −19→20 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0376P)2 + 3.4133P] where P = (Fo2 + 2Fc2)/3 |
10353 reflections | (Δ/σ)max = 0.005 |
505 parameters | Δρmax = 0.70 e Å−3 |
18 restraints | Δρmin = −0.56 e Å−3 |
Co(C6H8N2)3Cr(C2O4)3.6H2O | V = 3327.9 (3) Å3 |
Mr = 807.52 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.1923 (8) Å | µ = 0.91 mm−1 |
b = 18.0299 (10) Å | T = 100 K |
c = 14.1801 (9) Å | 0.18 × 0.12 × 0.10 mm |
β = 99.357 (2)° |
D8 Venture Photon, Bruker AXS diffractometer | 10353 independent reflections |
Absorption correction: multi-scan APEX2 v2013.4-1 (Bruker AXS, 2013) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. | 8042 reflections with I > 2σ(I) |
Tmin = 0.693, Tmax = 0.746 | Rint = 0.054 |
100946 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 18 restraints |
wR(F2) = 0.094 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | Δρmax = 0.70 e Å−3 |
10353 reflections | Δρmin = −0.56 e Å−3 |
505 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Co | 0.221891 (17) | 0.211154 (13) | 0.417512 (16) | 0.01164 (6) | |
Cr | 0.20036 (2) | 0.148639 (15) | 0.896164 (19) | 0.01152 (6) | |
O3 | 0.15148 (10) | 0.09276 (7) | 0.99868 (9) | 0.0174 (3) | |
O11 | 0.49965 (10) | 0.11928 (8) | 0.89630 (10) | 0.0205 (3) | |
O6 | 0.26803 (9) | 0.20883 (7) | 0.80730 (9) | 0.0153 (2) | |
O12 | 0.42345 (10) | 0.22937 (8) | 0.76808 (10) | 0.0207 (3) | |
O2 | 0.15075 (10) | 0.07367 (7) | 0.79948 (9) | 0.0183 (3) | |
O4 | 0.22995 (10) | 0.22388 (7) | 0.99741 (9) | 0.0201 (3) | |
O1 | 0.06500 (10) | 0.19200 (7) | 0.85587 (9) | 0.0177 (3) | |
O5 | 0.33972 (9) | 0.10337 (7) | 0.92644 (9) | 0.0172 (3) | |
N4 | 0.15445 (12) | 0.27904 (8) | 0.32060 (11) | 0.0141 (3) | |
N5 | 0.28725 (11) | 0.29973 (8) | 0.47583 (10) | 0.0140 (3) | |
O10 | 0.21405 (14) | 0.24494 (10) | 1.14837 (12) | 0.0427 (5) | |
O7 | −0.08746 (10) | 0.16494 (8) | 0.77116 (10) | 0.0235 (3) | |
O8 | 0.00560 (13) | 0.04289 (9) | 0.70042 (12) | 0.0358 (4) | |
N1 | 0.29683 (11) | 0.14262 (8) | 0.51120 (10) | 0.0144 (3) | |
N6 | 0.34045 (12) | 0.19734 (9) | 0.35248 (11) | 0.0161 (3) | |
N3 | 0.14964 (12) | 0.12764 (9) | 0.35107 (11) | 0.0157 (3) | |
N2 | 0.10514 (11) | 0.21718 (8) | 0.48382 (10) | 0.0149 (3) | |
O9 | 0.13700 (11) | 0.10025 (9) | 1.15293 (10) | 0.0285 (3) | |
C12 | 0.20497 (13) | 0.35287 (10) | 0.32656 (12) | 0.0148 (3) | |
H12A | 0.1521 | 0.3923 | 0.3200 | 0.018* | |
H12B | 0.2451 | 0.3583 | 0.2737 | 0.018* | |
C1 | 0.36526 (13) | 0.19708 (9) | 0.81295 (12) | 0.0139 (3) | |
C11 | 0.27467 (13) | 0.36086 (10) | 0.42036 (12) | 0.0148 (3) | |
C14 | 0.31662 (15) | 0.05566 (10) | 0.64058 (14) | 0.0210 (4) | |
H14A | 0.2878 | 0.0301 | 0.6885 | 0.025* | |
C7 | 0.34713 (14) | 0.30352 (10) | 0.56295 (13) | 0.0187 (4) | |
H7A | 0.3537 | 0.2610 | 0.6031 | 0.022* | |
C2 | 0.40790 (13) | 0.13491 (10) | 0.88434 (12) | 0.0147 (3) | |
C17 | 0.39554 (14) | 0.13095 (10) | 0.50074 (13) | 0.0166 (3) | |
C19 | 0.09717 (15) | 0.26067 (11) | 0.55960 (13) | 0.0200 (4) | |
H19A | 0.1506 | 0.2948 | 0.5817 | 0.024* | |
C10 | 0.32543 (15) | 0.42658 (10) | 0.44855 (14) | 0.0199 (4) | |
H10A | 0.3165 | 0.4689 | 0.4082 | 0.024* | |
C22 | −0.05850 (15) | 0.16395 (12) | 0.49476 (15) | 0.0256 (4) | |
H22A | −0.1120 | 0.1304 | 0.4708 | 0.031* | |
C3 | 0.20480 (14) | 0.20502 (11) | 1.07769 (14) | 0.0216 (4) | |
C6 | 0.00405 (14) | 0.15158 (10) | 0.79811 (12) | 0.0172 (3) | |
C24 | 0.03988 (14) | 0.12762 (11) | 0.36308 (15) | 0.0226 (4) | |
H24A | 0.0159 | 0.0760 | 0.3685 | 0.027* | |
H24B | −0.0024 | 0.1507 | 0.3066 | 0.027* | |
C9 | 0.38924 (16) | 0.42961 (11) | 0.53621 (14) | 0.0231 (4) | |
H9A | 0.4261 | 0.4737 | 0.5561 | 0.028* | |
C16 | 0.45803 (14) | 0.08212 (11) | 0.55956 (14) | 0.0209 (4) | |
H16A | 0.5275 | 0.0750 | 0.5516 | 0.025* | |
C18 | 0.43160 (14) | 0.17573 (11) | 0.42348 (13) | 0.0184 (4) | |
H18A | 0.4681 | 0.2206 | 0.4512 | 0.022* | |
H18B | 0.4797 | 0.1461 | 0.3919 | 0.022* | |
C13 | 0.25810 (14) | 0.10527 (10) | 0.57998 (13) | 0.0171 (3) | |
H13A | 0.1885 | 0.1133 | 0.5870 | 0.021* | |
C15 | 0.41839 (16) | 0.04396 (11) | 0.62985 (14) | 0.0228 (4) | |
H15A | 0.4601 | 0.0101 | 0.6704 | 0.027* | |
C8 | 0.39850 (15) | 0.36745 (11) | 0.59453 (14) | 0.0225 (4) | |
H8A | 0.4400 | 0.3690 | 0.6559 | 0.027* | |
C4 | 0.16032 (13) | 0.12603 (11) | 1.07948 (13) | 0.0188 (4) | |
C21 | −0.06553 (15) | 0.20721 (13) | 0.57318 (14) | 0.0270 (4) | |
H21A | −0.1236 | 0.2033 | 0.6047 | 0.032* | |
C23 | 0.02786 (14) | 0.16998 (10) | 0.45100 (13) | 0.0179 (3) | |
C5 | 0.05497 (15) | 0.08235 (11) | 0.76112 (13) | 0.0200 (4) | |
C20 | 0.01265 (16) | 0.25652 (12) | 0.60590 (14) | 0.0253 (4) | |
H20A | 0.0084 | 0.2872 | 0.6596 | 0.030* | |
O1W | 0.34866 (14) | −0.06415 (9) | 0.85997 (13) | 0.0372 (4) | |
O2W | 0.43457 (12) | 0.02806 (8) | 1.09685 (10) | 0.0255 (3) | |
O5W | 0.18874 (12) | 0.38509 (8) | 0.99724 (12) | 0.0299 (3) | |
O6W | 0.2190 (3) | 0.36554 (11) | 0.81306 (15) | 0.0793 (9) | |
O4W | 0.28792 (11) | 0.47485 (8) | 1.14099 (11) | 0.0263 (3) | |
O3W | 0.36046 (11) | 0.05199 (8) | 0.27300 (11) | 0.0267 (3) | |
H4A | 0.158 (2) | 0.2611 (14) | 0.2656 (19) | 0.032* | |
H4B | 0.089 (2) | 0.2844 (14) | 0.3257 (19) | 0.032* | |
H6B | 0.358 (2) | 0.2389 (15) | 0.3224 (19) | 0.032* | |
H6A | 0.332 (2) | 0.1599 (15) | 0.3138 (19) | 0.032* | |
H3B | 0.179 (2) | 0.0863 (15) | 0.3736 (19) | 0.032* | |
H3A | 0.152 (2) | 0.1308 (14) | 0.289 (2) | 0.032* | |
H1W | 0.4196 (8) | −0.0532 (13) | 0.8783 (19) | 0.040* | |
H2W | 0.3110 (16) | −0.0219 (10) | 0.8719 (19) | 0.040* | |
H3W | 0.3973 (18) | 0.0499 (12) | 1.0412 (12) | 0.040* | |
H4W | 0.448 (2) | −0.0221 (7) | 1.0836 (17) | 0.040* | |
H9W | 0.201 (2) | 0.3356 (7) | 1.0183 (16) | 0.040* | |
H10W | 0.195 (2) | 0.3862 (14) | 0.9315 (8) | 0.040* | |
H11W | 0.197 (2) | 0.3872 (12) | 0.7522 (10) | 0.040* | |
H12W | 0.234 (2) | 0.3153 (7) | 0.8007 (17) | 0.040* | |
H7W | 0.3542 (11) | 0.4559 (13) | 1.1651 (17) | 0.040* | |
H8W | 0.2610 (17) | 0.4439 (12) | 1.0883 (13) | 0.040* | |
H5W | 0.3099 (16) | 0.0206 (12) | 0.2906 (17) | 0.040* | |
H6W | 0.369 (2) | 0.0428 (14) | 0.2099 (9) | 0.040* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co | 0.01124 (11) | 0.01325 (11) | 0.01088 (11) | 0.00200 (8) | 0.00311 (8) | 0.00023 (8) |
Cr | 0.01049 (12) | 0.01193 (12) | 0.01229 (13) | 0.00021 (9) | 0.00230 (9) | −0.00001 (10) |
O3 | 0.0188 (6) | 0.0188 (6) | 0.0159 (6) | −0.0011 (5) | 0.0064 (5) | 0.0012 (5) |
O11 | 0.0132 (6) | 0.0232 (7) | 0.0255 (7) | 0.0029 (5) | 0.0044 (5) | 0.0056 (5) |
O6 | 0.0143 (6) | 0.0151 (6) | 0.0167 (6) | 0.0002 (5) | 0.0026 (5) | 0.0036 (5) |
O12 | 0.0182 (6) | 0.0230 (7) | 0.0213 (7) | −0.0024 (5) | 0.0045 (5) | 0.0068 (5) |
O2 | 0.0209 (6) | 0.0158 (6) | 0.0194 (6) | −0.0020 (5) | 0.0070 (5) | −0.0041 (5) |
O4 | 0.0217 (7) | 0.0195 (6) | 0.0192 (6) | −0.0040 (5) | 0.0037 (5) | −0.0049 (5) |
O1 | 0.0129 (6) | 0.0196 (6) | 0.0200 (6) | 0.0022 (5) | 0.0011 (5) | −0.0003 (5) |
O5 | 0.0130 (6) | 0.0204 (6) | 0.0188 (6) | 0.0023 (5) | 0.0040 (5) | 0.0069 (5) |
N4 | 0.0124 (7) | 0.0172 (7) | 0.0129 (7) | 0.0012 (5) | 0.0029 (5) | −0.0001 (6) |
N5 | 0.0137 (7) | 0.0158 (7) | 0.0127 (7) | 0.0024 (5) | 0.0028 (5) | 0.0004 (5) |
O10 | 0.0421 (10) | 0.0567 (11) | 0.0348 (9) | −0.0245 (9) | 0.0231 (8) | −0.0292 (8) |
O7 | 0.0134 (6) | 0.0357 (8) | 0.0214 (7) | −0.0010 (6) | 0.0025 (5) | 0.0051 (6) |
O8 | 0.0337 (9) | 0.0313 (8) | 0.0389 (9) | −0.0052 (7) | −0.0049 (7) | −0.0154 (7) |
N1 | 0.0149 (7) | 0.0146 (7) | 0.0139 (7) | 0.0017 (5) | 0.0026 (5) | 0.0000 (5) |
N6 | 0.0149 (7) | 0.0187 (7) | 0.0154 (7) | 0.0030 (6) | 0.0044 (6) | 0.0011 (6) |
N3 | 0.0169 (7) | 0.0152 (7) | 0.0149 (7) | 0.0015 (6) | 0.0021 (6) | −0.0013 (6) |
N2 | 0.0148 (7) | 0.0172 (7) | 0.0134 (7) | 0.0042 (6) | 0.0043 (5) | 0.0026 (6) |
O9 | 0.0270 (8) | 0.0431 (9) | 0.0168 (7) | 0.0012 (7) | 0.0079 (6) | 0.0050 (6) |
C12 | 0.0141 (8) | 0.0161 (8) | 0.0143 (8) | 0.0022 (6) | 0.0032 (6) | 0.0026 (6) |
C1 | 0.0151 (8) | 0.0121 (7) | 0.0140 (8) | −0.0021 (6) | 0.0012 (6) | −0.0004 (6) |
C11 | 0.0140 (8) | 0.0166 (8) | 0.0148 (8) | 0.0040 (6) | 0.0050 (6) | 0.0001 (6) |
C14 | 0.0255 (10) | 0.0183 (9) | 0.0193 (9) | 0.0030 (7) | 0.0040 (7) | 0.0038 (7) |
C7 | 0.0201 (9) | 0.0196 (9) | 0.0158 (8) | 0.0021 (7) | 0.0014 (7) | 0.0009 (7) |
C2 | 0.0144 (8) | 0.0160 (8) | 0.0137 (8) | −0.0007 (6) | 0.0026 (6) | 0.0002 (6) |
C17 | 0.0157 (8) | 0.0155 (8) | 0.0184 (8) | 0.0009 (6) | 0.0027 (7) | −0.0020 (7) |
C19 | 0.0224 (9) | 0.0218 (9) | 0.0168 (8) | 0.0048 (7) | 0.0063 (7) | 0.0005 (7) |
C10 | 0.0214 (9) | 0.0169 (8) | 0.0215 (9) | 0.0003 (7) | 0.0040 (7) | −0.0010 (7) |
C22 | 0.0147 (9) | 0.0360 (11) | 0.0261 (10) | 0.0000 (8) | 0.0035 (7) | 0.0096 (8) |
C3 | 0.0137 (8) | 0.0305 (10) | 0.0214 (9) | −0.0026 (7) | 0.0049 (7) | −0.0085 (8) |
C6 | 0.0159 (8) | 0.0218 (9) | 0.0146 (8) | −0.0030 (7) | 0.0046 (6) | 0.0046 (7) |
C24 | 0.0161 (9) | 0.0236 (9) | 0.0276 (10) | −0.0008 (7) | 0.0018 (7) | −0.0055 (8) |
C9 | 0.0249 (10) | 0.0193 (9) | 0.0244 (10) | −0.0022 (7) | 0.0017 (8) | −0.0052 (7) |
C16 | 0.0157 (8) | 0.0215 (9) | 0.0252 (9) | 0.0054 (7) | 0.0023 (7) | 0.0003 (7) |
C18 | 0.0133 (8) | 0.0220 (9) | 0.0202 (9) | 0.0033 (7) | 0.0033 (7) | 0.0033 (7) |
C13 | 0.0178 (8) | 0.0169 (8) | 0.0172 (8) | 0.0019 (7) | 0.0043 (7) | 0.0013 (7) |
C15 | 0.0259 (10) | 0.0191 (9) | 0.0220 (9) | 0.0077 (7) | −0.0005 (8) | 0.0040 (7) |
C8 | 0.0218 (9) | 0.0260 (10) | 0.0181 (9) | −0.0006 (8) | −0.0015 (7) | −0.0027 (7) |
C4 | 0.0111 (8) | 0.0275 (9) | 0.0179 (8) | 0.0028 (7) | 0.0028 (6) | 0.0010 (7) |
C21 | 0.0163 (9) | 0.0451 (13) | 0.0210 (9) | 0.0092 (9) | 0.0069 (7) | 0.0142 (9) |
C23 | 0.0141 (8) | 0.0205 (9) | 0.0188 (8) | 0.0025 (7) | 0.0017 (7) | 0.0060 (7) |
C5 | 0.0223 (9) | 0.0200 (9) | 0.0176 (8) | −0.0062 (7) | 0.0027 (7) | 0.0002 (7) |
C20 | 0.0276 (10) | 0.0347 (11) | 0.0157 (9) | 0.0120 (9) | 0.0096 (8) | 0.0051 (8) |
O1W | 0.0396 (10) | 0.0257 (8) | 0.0451 (10) | −0.0026 (7) | 0.0035 (8) | −0.0066 (7) |
O2W | 0.0350 (8) | 0.0221 (7) | 0.0194 (7) | 0.0036 (6) | 0.0040 (6) | 0.0037 (5) |
O5W | 0.0242 (7) | 0.0249 (7) | 0.0407 (9) | 0.0018 (6) | 0.0052 (7) | 0.0007 (7) |
O6W | 0.172 (3) | 0.0289 (10) | 0.0341 (11) | 0.0403 (14) | 0.0080 (14) | −0.0004 (8) |
O4W | 0.0221 (7) | 0.0228 (7) | 0.0328 (8) | 0.0012 (6) | 0.0005 (6) | 0.0012 (6) |
O3W | 0.0241 (7) | 0.0281 (8) | 0.0282 (8) | 0.0010 (6) | 0.0054 (6) | −0.0067 (6) |
Co—N2 | 1.9336 (14) | N1—C17 | 1.351 (2) |
Co—N5 | 1.9355 (15) | N1—C13 | 1.352 (2) |
Co—N3 | 1.9420 (15) | N6—C18 | 1.489 (2) |
Co—N4 | 1.9444 (15) | N3—C24 | 1.485 (2) |
Co—N6 | 1.9564 (15) | N2—C19 | 1.348 (2) |
Co—N1 | 1.9601 (15) | N2—C23 | 1.351 (2) |
Cr—O1 | 1.9480 (13) | O9—C4 | 1.225 (2) |
Cr—O2 | 1.9604 (13) | C12—C11 | 1.496 (2) |
Cr—O3 | 1.9619 (13) | C1—C2 | 1.553 (2) |
Cr—O4 | 1.9677 (13) | C11—C10 | 1.388 (3) |
Cr—O6 | 1.9819 (12) | C14—C13 | 1.385 (3) |
Cr—O5 | 1.9933 (13) | C14—C15 | 1.392 (3) |
O3—C4 | 1.282 (2) | C7—C8 | 1.375 (3) |
O11—C2 | 1.227 (2) | C17—C16 | 1.388 (3) |
O6—C1 | 1.290 (2) | C17—C18 | 1.499 (3) |
O12—C1 | 1.221 (2) | C19—C20 | 1.385 (3) |
O2—C5 | 1.301 (2) | C10—C9 | 1.384 (3) |
O4—C3 | 1.282 (2) | C22—C21 | 1.374 (3) |
O1—C6 | 1.278 (2) | C22—C23 | 1.387 (3) |
O5—C2 | 1.290 (2) | C3—C4 | 1.542 (3) |
N4—C12 | 1.485 (2) | C6—C5 | 1.549 (3) |
N5—C11 | 1.348 (2) | C24—C23 | 1.492 (3) |
N5—C7 | 1.356 (2) | C9—C8 | 1.386 (3) |
O10—C3 | 1.224 (2) | C16—C15 | 1.382 (3) |
O7—C6 | 1.229 (2) | C21—C20 | 1.383 (3) |
O8—C5 | 1.220 (2) | ||
N2—Co—N5 | 94.62 (6) | C19—N2—C23 | 119.25 (16) |
N2—Co—N3 | 84.99 (6) | C19—N2—Co | 126.29 (13) |
N5—Co—N3 | 175.19 (7) | C23—N2—Co | 114.40 (12) |
N2—Co—N4 | 89.95 (6) | N4—C12—C11 | 110.01 (14) |
N5—Co—N4 | 84.46 (6) | O12—C1—O6 | 126.32 (16) |
N3—Co—N4 | 90.75 (7) | O12—C1—C2 | 119.46 (15) |
N2—Co—N6 | 175.84 (7) | O6—C1—C2 | 114.22 (14) |
N5—Co—N6 | 88.38 (7) | N5—C11—C10 | 121.47 (17) |
N3—Co—N6 | 92.27 (7) | N5—C11—C12 | 116.07 (15) |
N4—Co—N6 | 93.21 (6) | C10—C11—C12 | 122.45 (16) |
N2—Co—N1 | 93.42 (6) | C13—C14—C15 | 118.71 (18) |
N5—Co—N1 | 95.17 (6) | N5—C7—C8 | 121.49 (17) |
N3—Co—N1 | 89.64 (7) | O11—C2—O5 | 125.53 (16) |
N4—Co—N1 | 176.62 (6) | O11—C2—C1 | 120.02 (15) |
N6—Co—N1 | 83.42 (6) | O5—C2—C1 | 114.45 (15) |
O1—Cr—O2 | 83.44 (6) | N1—C17—C16 | 121.44 (17) |
O1—Cr—O3 | 91.56 (6) | N1—C17—C18 | 114.99 (15) |
O2—Cr—O3 | 92.95 (5) | C16—C17—C18 | 123.55 (16) |
O1—Cr—O4 | 90.05 (6) | N2—C19—C20 | 121.31 (19) |
O2—Cr—O4 | 171.77 (6) | C9—C10—C11 | 119.14 (18) |
O3—Cr—O4 | 82.16 (6) | C21—C22—C23 | 119.1 (2) |
O1—Cr—O6 | 94.58 (5) | O10—C3—O4 | 124.4 (2) |
O2—Cr—O6 | 93.82 (5) | O10—C3—C4 | 121.14 (18) |
O3—Cr—O6 | 171.33 (6) | O4—C3—C4 | 114.43 (16) |
O4—Cr—O6 | 91.72 (5) | O7—C6—O1 | 124.82 (18) |
O1—Cr—O5 | 175.45 (5) | O7—C6—C5 | 120.71 (17) |
O2—Cr—O5 | 93.42 (6) | O1—C6—C5 | 114.46 (15) |
O3—Cr—O5 | 91.89 (5) | N3—C24—C23 | 109.49 (15) |
O4—Cr—O5 | 93.36 (6) | C10—C9—C8 | 119.04 (18) |
O6—Cr—O5 | 82.31 (5) | C15—C16—C17 | 119.46 (17) |
C4—O3—Cr | 115.40 (12) | N6—C18—C17 | 108.52 (15) |
C1—O6—Cr | 114.63 (11) | N1—C13—C14 | 122.09 (17) |
C5—O2—Cr | 113.61 (12) | C16—C15—C14 | 119.23 (17) |
C3—O4—Cr | 114.56 (12) | C7—C8—C9 | 119.51 (18) |
C6—O1—Cr | 114.22 (12) | O9—C4—O3 | 125.72 (19) |
C2—O5—Cr | 114.08 (11) | O9—C4—C3 | 120.89 (18) |
C12—N4—Co | 112.00 (11) | O3—C4—C3 | 113.39 (16) |
C11—N5—C7 | 119.25 (16) | C22—C21—C20 | 119.44 (18) |
C11—N5—Co | 114.91 (12) | N2—C23—C22 | 121.58 (18) |
C7—N5—Co | 125.73 (12) | N2—C23—C24 | 115.68 (16) |
C17—N1—C13 | 119.07 (15) | C22—C23—C24 | 122.69 (18) |
C17—N1—Co | 114.37 (12) | O8—C5—O2 | 126.54 (19) |
C13—N1—Co | 126.50 (12) | O8—C5—C6 | 119.84 (18) |
C18—N6—Co | 109.53 (11) | O2—C5—C6 | 113.61 (15) |
C24—N3—Co | 110.81 (11) | C21—C20—C19 | 119.32 (19) |
O1—Cr—O3—C4 | −90.54 (13) | N3—Co—N2—C23 | −5.77 (13) |
O2—Cr—O3—C4 | −174.04 (13) | N4—Co—N2—C23 | 84.99 (13) |
O4—Cr—O3—C4 | −0.70 (12) | N6—Co—N2—C23 | −54.5 (9) |
O6—Cr—O3—C4 | 44.7 (4) | N1—Co—N2—C23 | −95.10 (13) |
O5—Cr—O3—C4 | 92.43 (13) | Co—N4—C12—C11 | −15.27 (17) |
O1—Cr—O6—C1 | 178.82 (12) | Cr—O6—C1—O12 | −177.16 (15) |
O2—Cr—O6—C1 | −97.47 (12) | Cr—O6—C1—C2 | 3.25 (18) |
O3—Cr—O6—C1 | 43.8 (4) | C7—N5—C11—C10 | 3.0 (3) |
O4—Cr—O6—C1 | 88.63 (12) | Co—N5—C11—C10 | −173.43 (13) |
O5—Cr—O6—C1 | −4.53 (12) | C7—N5—C11—C12 | −178.20 (15) |
O1—Cr—O2—C5 | −5.18 (12) | Co—N5—C11—C12 | 5.32 (19) |
O3—Cr—O2—C5 | 86.05 (13) | N4—C12—C11—N5 | 6.6 (2) |
O4—Cr—O2—C5 | 32.8 (5) | N4—C12—C11—C10 | −174.63 (16) |
O6—Cr—O2—C5 | −99.37 (12) | C11—N5—C7—C8 | −2.5 (3) |
O5—Cr—O2—C5 | 178.12 (12) | Co—N5—C7—C8 | 173.52 (14) |
O1—Cr—O4—C3 | 90.58 (13) | Cr—O5—C2—O11 | 175.71 (15) |
O2—Cr—O4—C3 | 52.9 (5) | Cr—O5—C2—C1 | −4.70 (18) |
O3—Cr—O4—C3 | −0.99 (13) | O12—C1—C2—O11 | 1.0 (3) |
O6—Cr—O4—C3 | −174.83 (13) | O6—C1—C2—O11 | −179.38 (16) |
O5—Cr—O4—C3 | −92.43 (13) | O12—C1—C2—O5 | −178.61 (16) |
O2—Cr—O1—C6 | 7.67 (12) | O6—C1—C2—O5 | 1.0 (2) |
O3—Cr—O1—C6 | −85.12 (12) | C13—N1—C17—C16 | −0.6 (3) |
O4—Cr—O1—C6 | −167.28 (12) | Co—N1—C17—C16 | −177.97 (14) |
O6—Cr—O1—C6 | 101.00 (12) | C13—N1—C17—C18 | −179.19 (16) |
O5—Cr—O1—C6 | 54.2 (7) | Co—N1—C17—C18 | 3.5 (2) |
O1—Cr—O5—C2 | 52.3 (7) | C23—N2—C19—C20 | 1.7 (3) |
O2—Cr—O5—C2 | 98.50 (12) | Co—N2—C19—C20 | −175.22 (14) |
O3—Cr—O5—C2 | −168.43 (12) | N5—C11—C10—C9 | −0.9 (3) |
O4—Cr—O5—C2 | −86.18 (12) | C12—C11—C10—C9 | −179.60 (17) |
O6—Cr—O5—C2 | 5.10 (12) | Cr—O4—C3—O10 | −177.64 (18) |
N2—Co—N4—C12 | 109.39 (12) | Cr—O4—C3—C4 | 2.2 (2) |
N5—Co—N4—C12 | 14.74 (11) | Cr—O1—C6—O7 | 172.68 (14) |
N3—Co—N4—C12 | −165.62 (12) | Cr—O1—C6—C5 | −8.33 (18) |
N6—Co—N4—C12 | −73.31 (12) | Co—N3—C24—C23 | −23.15 (19) |
N1—Co—N4—C12 | −69.0 (11) | C11—C10—C9—C8 | −1.7 (3) |
N2—Co—N5—C11 | −100.94 (12) | N1—C17—C16—C15 | 0.6 (3) |
N3—Co—N5—C11 | −15.8 (8) | C18—C17—C16—C15 | 179.07 (18) |
N4—Co—N5—C11 | −11.44 (12) | Co—N6—C18—C17 | 32.35 (17) |
N6—Co—N5—C11 | 81.95 (13) | N1—C17—C18—N6 | −23.6 (2) |
N1—Co—N5—C11 | 165.19 (12) | C16—C17—C18—N6 | 157.86 (17) |
N2—Co—N5—C7 | 82.84 (15) | C17—N1—C13—C14 | 0.4 (3) |
N3—Co—N5—C7 | 168.0 (7) | Co—N1—C13—C14 | 177.39 (14) |
N4—Co—N5—C7 | 172.35 (15) | C15—C14—C13—N1 | −0.2 (3) |
N6—Co—N5—C7 | −94.27 (15) | C17—C16—C15—C14 | −0.4 (3) |
N1—Co—N5—C7 | −11.03 (15) | C13—C14—C15—C16 | 0.2 (3) |
N2—Co—N1—C17 | −170.13 (13) | N5—C7—C8—C9 | −0.1 (3) |
N5—Co—N1—C17 | −75.17 (13) | C10—C9—C8—C7 | 2.2 (3) |
N3—Co—N1—C17 | 104.91 (13) | Cr—O3—C4—O9 | −178.01 (15) |
N4—Co—N1—C17 | 8.3 (11) | Cr—O3—C4—C3 | 1.96 (19) |
N6—Co—N1—C17 | 12.59 (13) | O10—C3—C4—O9 | −3.0 (3) |
N2—Co—N1—C13 | 12.75 (15) | O4—C3—C4—O9 | 177.17 (17) |
N5—Co—N1—C13 | 107.71 (15) | O10—C3—C4—O3 | 177.06 (19) |
N3—Co—N1—C13 | −72.21 (15) | O4—C3—C4—O3 | −2.8 (2) |
N4—Co—N1—C13 | −168.9 (10) | C23—C22—C21—C20 | 1.0 (3) |
N6—Co—N1—C13 | −164.53 (16) | C19—N2—C23—C22 | −1.5 (3) |
N2—Co—N6—C18 | −65.9 (9) | Co—N2—C23—C22 | 175.77 (14) |
N5—Co—N6—C18 | 70.27 (13) | C19—N2—C23—C24 | 176.11 (16) |
N3—Co—N6—C18 | −114.50 (13) | Co—N2—C23—C24 | −6.6 (2) |
N4—Co—N6—C18 | 154.62 (12) | C21—C22—C23—N2 | 0.2 (3) |
N1—Co—N6—C18 | −25.12 (12) | C21—C22—C23—C24 | −177.27 (18) |
N2—Co—N3—C24 | 16.43 (13) | N3—C24—C23—N2 | 19.6 (2) |
N5—Co—N3—C24 | −69.1 (8) | N3—C24—C23—C22 | −162.81 (17) |
N4—Co—N3—C24 | −73.46 (13) | Cr—O2—C5—O8 | −179.02 (17) |
N6—Co—N3—C24 | −166.70 (13) | Cr—O2—C5—C6 | 2.22 (19) |
N1—Co—N3—C24 | 109.89 (13) | O7—C6—C5—O8 | 4.3 (3) |
N5—Co—N2—C19 | −13.53 (16) | O1—C6—C5—O8 | −174.76 (18) |
N3—Co—N2—C19 | 171.28 (16) | O7—C6—C5—O2 | −176.86 (16) |
N4—Co—N2—C19 | −97.96 (15) | O1—C6—C5—O2 | 4.1 (2) |
N6—Co—N2—C19 | 122.5 (9) | C22—C21—C20—C19 | −0.8 (3) |
N1—Co—N2—C19 | 81.94 (15) | N2—C19—C20—C21 | −0.6 (3) |
N5—Co—N2—C23 | 169.43 (12) |
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4A···O10i | 0.85 (3) | 1.95 (3) | 2.754 (2) | 158 (2) |
N4—H4B···O12ii | 0.89 (3) | 2.21 (3) | 3.021 (2) | 151 (2) |
N4—H4B···O11ii | 0.89 (3) | 2.40 (3) | 3.065 (2) | 132 (2) |
N6—H6B···O7iii | 0.91 (3) | 2.06 (3) | 2.959 (2) | 172 (2) |
N3—H3A···O9i | 0.89 (3) | 1.98 (3) | 2.831 (2) | 158 (2) |
N3—H3B···O4Wiv | 0.88 (3) | 2.07 (3) | 2.872 (2) | 151 (2) |
O1W—H1W···O2Wv | 0.95 (1) | 1.95 (1) | 2.899 (2) | 174 (3) |
N6—H6A···O3W | 0.87 (3) | 2.08 (3) | 2.882 (2) | 153 (2) |
O1W—H2W···O5 | 0.94 (1) | 2.40 (2) | 3.172 (2) | 140 (2) |
O2W—H3W···O5 | 0.95 (1) | 1.94 (1) | 2.8751 (19) | 171 (2) |
O2W—H4W···O11v | 0.94 (1) | 1.89 (1) | 2.791 (2) | 159 (2) |
O5W—H9W···O4 | 0.95 (1) | 2.08 (2) | 2.957 (2) | 153 (2) |
O5W—H9W···O10 | 0.95 (1) | 2.45 (1) | 3.295 (3) | 149 (2) |
O5W—H10W···O6W | 0.95 (1) | 1.80 (1) | 2.728 (3) | 166 (2) |
O6W—H11W···O1Wvi | 0.95 (1) | 1.83 (1) | 2.777 (3) | 175 (2) |
O6W—H12W···O6 | 0.95 (1) | 1.97 (1) | 2.903 (2) | 167 (2) |
O4W—H7W···O8vii | 0.95 (1) | 1.98 (1) | 2.876 (2) | 157 (2) |
O4W—H8W···O5W | 0.95 (1) | 1.82 (1) | 2.760 (2) | 170 (2) |
O3W—H5W···O4Wiv | 0.94 (1) | 1.92 (1) | 2.834 (2) | 163 (2) |
O3W—H6W···O2Wi | 0.94 (1) | 1.96 (1) | 2.859 (2) | 161 (2) |
C7—H7A···O12 | 0.95 | 2.44 | 3.211 (2) | 138 |
C9—H9A···O3vi | 0.95 | 2.45 | 3.017 (2) | 118 |
C10—H10A···O3vi | 0.95 | 2.59 | 3.091 (2) | 113 |
C16—H16A···O5Wiii | 0.95 | 2.48 | 3.357 (2) | 153 |
C21—H21A···O10ii | 0.95 | 2.50 | 3.368 (3) | 151 |
C21—H21A···O7 | 0.95 | 2.43 | 2.968 (2) | 116 |
Symmetry codes: (i) x, y, z−1; (ii) x−1/2, −y+1/2, z−1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) −x+1/2, y−1/2, −z+3/2; (v) −x+1, −y, −z+2; (vi) −x+1/2, y+1/2, −z+3/2; (vii) x+1/2, −y+1/2, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | Co(C6H8N2)3Cr(C2O4)3.6H2O |
Mr | 807.52 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 100 |
a, b, c (Å) | 13.1923 (8), 18.0299 (10), 14.1801 (9) |
β (°) | 99.357 (2) |
V (Å3) | 3327.9 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.91 |
Crystal size (mm) | 0.18 × 0.12 × 0.10 |
Data collection | |
Diffractometer | D8 Venture Photon, Bruker AXS diffractometer |
Absorption correction | Multi-scan APEX2 v2013.4-1 (Bruker AXS, 2013) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. |
Tmin, Tmax | 0.693, 0.746 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 100946, 10353, 8042 |
Rint | 0.054 |
(sin θ/λ)max (Å−1) | 0.738 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.094, 1.05 |
No. of reflections | 10353 |
No. of parameters | 505 |
No. of restraints | 18 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.70, −0.56 |
Computer programs: APEX2 v2013.4-1 (Bruker AXS, 2013), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND for Windows (Klaus, 2004), enCIFer 1.3 (Allen et al., 2004)).
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4A···O10i | 0.85 (3) | 1.95 (3) | 2.754 (2) | 158 (2) |
N4—H4B···O12ii | 0.89 (3) | 2.21 (3) | 3.021 (2) | 151 (2) |
N4—H4B···O11ii | 0.89 (3) | 2.40 (3) | 3.065 (2) | 132 (2) |
N6—H6B···O7iii | 0.91 (3) | 2.06 (3) | 2.959 (2) | 172 (2) |
N3—H3A···O9i | 0.89 (3) | 1.98 (3) | 2.831 (2) | 158 (2) |
N3—H3B···O4Wiv | 0.88 (3) | 2.07 (3) | 2.872 (2) | 151 (2) |
O1W—H1W···O2Wv | 0.950 (9) | 1.952 (10) | 2.899 (2) | 174 (3) |
N6—H6A···O3W | 0.87 (3) | 2.08 (3) | 2.882 (2) | 153 (2) |
O1W—H2W···O5 | 0.939 (9) | 2.397 (18) | 3.172 (2) | 139.6 (19) |
O2W—H3W···O5 | 0.945 (9) | 1.938 (10) | 2.8751 (19) | 171 (2) |
O2W—H4W···O11v | 0.944 (9) | 1.891 (12) | 2.791 (2) | 159 (2) |
O5W—H9W···O4 | 0.945 (9) | 2.082 (15) | 2.957 (2) | 153 (2) |
O5W—H9W···O10 | 0.945 (9) | 2.450 (14) | 3.295 (3) | 149 (2) |
O5W—H10W···O6W | 0.950 (9) | 1.797 (12) | 2.728 (3) | 166 (2) |
O6W—H11W···O1Wvi | 0.950 (9) | 1.829 (10) | 2.777 (3) | 175 (2) |
O6W—H12W···O6 | 0.949 (9) | 1.970 (10) | 2.903 (2) | 167 (2) |
O4W—H7W···O8vii | 0.949 (9) | 1.978 (13) | 2.876 (2) | 157 (2) |
O4W—H8W···O5W | 0.954 (9) | 1.816 (10) | 2.760 (2) | 170 (2) |
O3W—H5W···O4Wiv | 0.939 (9) | 1.922 (11) | 2.834 (2) | 163 (2) |
O3W—H6W···O2Wi | 0.936 (9) | 1.957 (12) | 2.859 (2) | 161 (2) |
C7—H7A···O12 | 0.95 | 2.44 | 3.211 (2) | 138.4 |
C9—H9A···O3vi | 0.95 | 2.45 | 3.017 (2) | 118.1 |
C10—H10A···O3vi | 0.95 | 2.59 | 3.091 (2) | 113.1 |
C16—H16A···O5Wiii | 0.95 | 2.48 | 3.357 (2) | 152.7 |
C21—H21A···O10ii | 0.95 | 2.50 | 3.368 (3) | 151.2 |
C21—H21A···O7 | 0.95 | 2.43 | 2.968 (2) | 115.6 |
Symmetry codes: (i) x, y, z−1; (ii) x−1/2, −y+1/2, z−1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) −x+1/2, y−1/2, −z+3/2; (v) −x+1, −y, −z+2; (vi) −x+1/2, y+1/2, −z+3/2; (vii) x+1/2, −y+1/2, z+1/2. |