Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229615010761/ov3064sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229615010761/ov3064Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229615010761/ov3064IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229615010761/ov3064IIIsup4.hkl |
CCDC references: 898180; 898181; 898179
Data collection: SMART (Bruker, 1998) for (I); SMART (Bruker, 2007) for (II), (III). Cell refinement: SAINT-Plus (Bruker, 1998) for (I); SAINT (Bruker, 2007) for (II), (III). Data reduction: SAINT-Plus (Bruker, 1998) for (I); SAINT (Bruker, 2007) for (II), (III). Program(s) used to solve structure: SHELXTL (Sheldrick, 2008) for (I); SHELXS97 (Sheldrick, 2008) for (II), (III). For all compounds, program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).
C4H12N22+·C6H2N2O42−·4.5H2O | Z = 2 |
Mr = 335.32 | F(000) = 358 |
Triclinic, P1 | Dx = 1.428 Mg m−3 |
a = 6.8024 (11) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.218 (2) Å | Cell parameters from 3169 reflections |
c = 12.926 (2) Å | θ = 3–29° |
α = 67.584 (3)° | µ = 0.12 mm−1 |
β = 87.521 (4)° | T = 120 K |
γ = 70.632 (3)° | Prism, colorless |
V = 780.0 (2) Å3 | 0.21 × 0.19 × 0.18 mm |
Bruker SMART 1000 diffractometer | 4156 independent reflections |
Radiation source: fine-focus sealed tube | 3240 reflections with I > 2σ(I) |
Detector resolution: 8.3 pixels mm-1 | Rint = 0.023 |
φ and ω scans | θmax = 29.1°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −9→9 |
Tmin = 0.819, Tmax = 0.862 | k = −13→13 |
8529 measured reflections | l = −17→17 |
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)] = 0.052 | Hydrogen site location: mixed |
wR(F2) = 0.150 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0786P)2 + 0.4842P] where P = (Fo2 + 2Fc2)/3 |
4156 reflections | (Δ/σ)max < 0.001 |
276 parameters | Δρmax = 0.59 e Å−3 |
23 restraints | Δρmin = −0.48 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
O1 | 0.29044 (19) | 0.36731 (13) | 0.78902 (9) | 0.0227 (3) | |
O2 | −0.01780 (19) | 0.35818 (14) | 0.74566 (10) | 0.0263 (3) | |
O3 | 0.3000 (2) | 0.08288 (13) | 0.73336 (9) | 0.0240 (3) | |
O4 | 0.3470 (2) | −0.15686 (13) | 0.84321 (10) | 0.0242 (3) | |
N1 | 0.1474 (2) | 0.20942 (15) | 1.00631 (11) | 0.0199 (3) | |
N2 | 0.2818 (2) | −0.08993 (15) | 1.02746 (11) | 0.0193 (3) | |
C1 | 0.1844 (2) | 0.17323 (17) | 0.91595 (12) | 0.0164 (3) | |
C2 | 0.2536 (2) | 0.02269 (17) | 0.92686 (12) | 0.0168 (3) | |
C3 | 0.2437 (3) | −0.05349 (18) | 1.11717 (13) | 0.0209 (3) | |
H3 | 0.2625 | −0.1312 | 1.1898 | 0.025* | |
C4 | 0.1774 (3) | 0.09551 (18) | 1.10639 (13) | 0.0204 (3) | |
H4 | 0.1527 | 0.1171 | 1.1720 | 0.024* | |
C5 | 0.1485 (2) | 0.30846 (17) | 0.80588 (12) | 0.0184 (3) | |
C6 | 0.3035 (2) | −0.02002 (17) | 0.82579 (13) | 0.0180 (3) | |
N3 | 0.3437 (2) | 0.51734 (17) | 0.57659 (12) | 0.0240 (3) | |
H3A | 0.305 (4) | 0.480 (3) | 0.647 (2) | 0.029 (5)* | |
H3B | 0.245 (4) | 0.604 (3) | 0.5290 (19) | 0.026 (5)* | |
C7 | 0.5385 (3) | 0.5511 (2) | 0.58464 (14) | 0.0257 (3) | |
H7A | 0.6462 | 0.4602 | 0.6382 | 0.031* | |
H7B | 0.5085 | 0.6321 | 0.6133 | 0.031* | |
C8 | 0.3795 (3) | 0.4001 (2) | 0.52978 (15) | 0.0270 (4) | |
H8A | 0.2466 | 0.3830 | 0.5228 | 0.032* | |
H8B | 0.4819 | 0.3042 | 0.5815 | 0.032* | |
N4 | 0.4590 (2) | 0.39449 (15) | 0.96457 (11) | 0.0182 (3) | |
H4A | 0.526 (3) | 0.306 (3) | 1.0241 (18) | 0.024 (5)* | |
H4B | 0.397 (4) | 0.377 (2) | 0.9105 (19) | 0.026 (5)* | |
C9 | 0.2902 (2) | 0.49275 (18) | 1.00684 (13) | 0.0197 (3) | |
H9A | 0.1928 | 0.4395 | 1.0443 | 0.024* | |
H9B | 0.2099 | 0.5858 | 0.9430 | 0.024* | |
C10 | 0.6145 (3) | 0.46729 (17) | 0.91069 (13) | 0.0191 (3) | |
H10A | 0.5448 | 0.5596 | 0.8437 | 0.023* | |
H10B | 0.7261 | 0.3977 | 0.8858 | 0.023* | |
O1W | 0.0973 (4) | −0.0068 (3) | 0.4924 (2) | 0.0324 (6) | 0.5 |
H1A | 0.128 (7) | −0.079 (4) | 0.556 (2) | 0.035 (12)* | 0.5 |
H1B | 0.211 (4) | 0.000 (6) | 0.467 (4) | 0.063 (18)* | 0.5 |
O2W | −0.1324 (3) | 0.66382 (18) | 0.73400 (17) | 0.0572 (5) | |
H2A | −0.118 (4) | 0.5861 (19) | 0.722 (2) | 0.047 (7)* | |
H2B | −0.207 (9) | 0.739 (3) | 0.680 (3) | 0.07 (2)* | 0.5 |
H2C | −0.038 (5) | 0.696 (4) | 0.704 (3) | 0.024 (10)* | 0.5 |
O3W | 0.5802 (3) | −0.05810 (19) | 0.61225 (14) | 0.0513 (5) | |
H3C | 0.493 (4) | −0.018 (3) | 0.648 (2) | 0.069 (10)* | |
H3D | 0.552 (6) | −0.019 (4) | 0.5433 (9) | 0.028 (11)* | 0.5 |
H3E | 0.609 (6) | −0.1503 (12) | 0.643 (3) | 0.022 (10)* | 0.5 |
O4W | −0.0684 (3) | 0.22655 (19) | 0.57863 (15) | 0.0509 (5) | |
H4C | −0.033 (6) | 0.149 (3) | 0.564 (3) | 0.089 (12)* | |
H4D | 0.019 (5) | 0.213 (4) | 0.629 (2) | 0.095 (13)* | |
O5W | 0.2034 (3) | −0.23609 (15) | 0.68828 (11) | 0.0337 (3) | |
H5A | 0.253 (4) | −0.206 (3) | 0.7301 (17) | 0.042 (7)* | |
H5B | 0.108 (5) | −0.265 (5) | 0.723 (3) | 0.061 (18)* | 0.5 |
H5C | 0.148 (5) | −0.158 (3) | 0.6305 (19) | 0.022 (10)* | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.0291 (6) | 0.0220 (6) | 0.0192 (5) | −0.0115 (5) | 0.0034 (4) | −0.0081 (4) |
O2 | 0.0229 (6) | 0.0257 (6) | 0.0253 (6) | −0.0023 (5) | −0.0036 (5) | −0.0091 (5) |
O3 | 0.0301 (6) | 0.0208 (6) | 0.0195 (5) | −0.0056 (5) | 0.0032 (4) | −0.0087 (5) |
O4 | 0.0331 (7) | 0.0188 (6) | 0.0226 (6) | −0.0066 (5) | 0.0006 (5) | −0.0115 (5) |
N1 | 0.0208 (6) | 0.0206 (6) | 0.0214 (6) | −0.0071 (5) | 0.0031 (5) | −0.0114 (5) |
N2 | 0.0194 (6) | 0.0184 (6) | 0.0204 (6) | −0.0058 (5) | 0.0026 (5) | −0.0084 (5) |
C1 | 0.0144 (7) | 0.0179 (7) | 0.0184 (7) | −0.0059 (5) | 0.0014 (5) | −0.0083 (5) |
C2 | 0.0154 (7) | 0.0177 (7) | 0.0188 (7) | −0.0055 (5) | 0.0021 (5) | −0.0091 (6) |
C3 | 0.0229 (8) | 0.0213 (7) | 0.0181 (7) | −0.0078 (6) | 0.0029 (6) | −0.0070 (6) |
C4 | 0.0217 (7) | 0.0235 (8) | 0.0180 (7) | −0.0077 (6) | 0.0042 (5) | −0.0103 (6) |
C5 | 0.0212 (7) | 0.0166 (7) | 0.0177 (7) | −0.0039 (6) | 0.0026 (5) | −0.0092 (6) |
C6 | 0.0166 (7) | 0.0197 (7) | 0.0193 (7) | −0.0042 (5) | 0.0005 (5) | −0.0107 (6) |
N3 | 0.0238 (7) | 0.0263 (7) | 0.0180 (6) | −0.0072 (6) | 0.0042 (5) | −0.0061 (6) |
C7 | 0.0267 (8) | 0.0298 (9) | 0.0223 (8) | −0.0092 (7) | 0.0020 (6) | −0.0123 (7) |
C8 | 0.0289 (9) | 0.0279 (8) | 0.0265 (8) | −0.0140 (7) | 0.0052 (6) | −0.0096 (7) |
N4 | 0.0208 (6) | 0.0162 (6) | 0.0205 (6) | −0.0069 (5) | 0.0026 (5) | −0.0097 (5) |
C9 | 0.0175 (7) | 0.0193 (7) | 0.0249 (7) | −0.0060 (6) | 0.0045 (6) | −0.0118 (6) |
C10 | 0.0212 (7) | 0.0179 (7) | 0.0203 (7) | −0.0071 (6) | 0.0055 (6) | −0.0098 (6) |
O1W | 0.0327 (14) | 0.0285 (13) | 0.0279 (13) | −0.0081 (11) | 0.0031 (11) | −0.0044 (11) |
O2W | 0.0565 (11) | 0.0221 (8) | 0.0709 (12) | −0.0029 (7) | 0.0320 (10) | −0.0066 (8) |
O3W | 0.0654 (12) | 0.0392 (9) | 0.0357 (9) | −0.0042 (8) | 0.0238 (8) | −0.0140 (7) |
O4W | 0.0564 (11) | 0.0378 (9) | 0.0478 (9) | 0.0071 (7) | −0.0293 (8) | −0.0217 (7) |
O5W | 0.0530 (9) | 0.0270 (7) | 0.0247 (6) | −0.0166 (6) | 0.0003 (6) | −0.0108 (5) |
O1—C5 | 1.268 (2) | N4—C10 | 1.490 (2) |
O2—C5 | 1.240 (2) | N4—C9 | 1.491 (2) |
O3—C6 | 1.2495 (19) | N4—H4A | 0.92 (2) |
O4—C6 | 1.2588 (19) | N4—H4B | 0.93 (2) |
N1—C4 | 1.337 (2) | C9—C10ii | 1.514 (2) |
N1—C1 | 1.3441 (19) | C9—H9A | 0.9900 |
N2—C2 | 1.336 (2) | C9—H9B | 0.9900 |
N2—C3 | 1.338 (2) | C10—C9ii | 1.514 (2) |
C1—C2 | 1.403 (2) | C10—H10A | 0.9900 |
C1—C5 | 1.517 (2) | C10—H10B | 0.9900 |
C2—C6 | 1.520 (2) | O1W—H1A | 0.840 (10) |
C3—C4 | 1.389 (2) | O1W—H1B | 0.841 (10) |
C3—H3 | 0.9500 | O2W—H2A | 0.837 (10) |
C4—H4 | 0.9500 | O2W—H2B | 0.834 (10) |
N3—C8 | 1.486 (2) | O2W—H2C | 0.834 (10) |
N3—C7 | 1.492 (2) | O3W—H3C | 0.831 (10) |
N3—H3A | 0.91 (2) | O3W—H3D | 0.827 (10) |
N3—H3B | 0.91 (2) | O3W—H3E | 0.826 (10) |
C7—C8i | 1.516 (2) | O4W—H4C | 0.843 (10) |
C7—H7A | 0.9900 | O4W—H4D | 0.837 (10) |
C7—H7B | 0.9900 | O5W—H5A | 0.843 (10) |
C8—C7i | 1.516 (2) | O5W—H5B | 0.841 (10) |
C8—H8A | 0.9900 | O5W—H5C | 0.839 (10) |
C8—H8B | 0.9900 | ||
C4—N1—C1 | 116.86 (13) | N3—C8—C7i | 110.30 (14) |
C2—N2—C3 | 117.42 (13) | N3—C8—H8A | 109.6 |
N1—C1—C2 | 121.30 (14) | C7i—C8—H8A | 109.6 |
N1—C1—C5 | 113.62 (13) | N3—C8—H8B | 109.6 |
C2—C1—C5 | 125.07 (13) | C7i—C8—H8B | 109.6 |
N2—C2—C1 | 121.13 (13) | H8A—C8—H8B | 108.1 |
N2—C2—C6 | 117.05 (13) | C10—N4—C9 | 111.96 (12) |
C1—C2—C6 | 121.81 (13) | C10—N4—H4A | 109.4 (13) |
N2—C3—C4 | 121.40 (15) | C9—N4—H4A | 108.4 (13) |
N2—C3—H3 | 119.3 | C10—N4—H4B | 108.0 (13) |
C4—C3—H3 | 119.3 | C9—N4—H4B | 108.1 (14) |
N1—C4—C3 | 121.89 (14) | H4A—N4—H4B | 111.0 (19) |
N1—C4—H4 | 119.1 | N4—C9—C10ii | 109.79 (13) |
C3—C4—H4 | 119.1 | N4—C9—H9A | 109.7 |
O2—C5—O1 | 125.93 (15) | C10ii—C9—H9A | 109.7 |
O2—C5—C1 | 119.23 (14) | N4—C9—H9B | 109.7 |
O1—C5—C1 | 114.61 (13) | C10ii—C9—H9B | 109.7 |
O3—C6—O4 | 125.81 (14) | H9A—C9—H9B | 108.2 |
O3—C6—C2 | 117.41 (13) | N4—C10—C9ii | 110.06 (12) |
O4—C6—C2 | 116.77 (13) | N4—C10—H10A | 109.6 |
C8—N3—C7 | 111.49 (14) | C9ii—C10—H10A | 109.6 |
C8—N3—H3A | 107.2 (14) | N4—C10—H10B | 109.6 |
C7—N3—H3A | 108.3 (15) | C9ii—C10—H10B | 109.6 |
C8—N3—H3B | 108.1 (14) | H10A—C10—H10B | 108.2 |
C7—N3—H3B | 108.1 (14) | H1A—O1W—H1B | 107 (3) |
H3A—N3—H3B | 114 (2) | H2A—O2W—H2B | 109 (3) |
N3—C7—C8i | 110.27 (14) | H2A—O2W—H2C | 107 (3) |
N3—C7—H7A | 109.6 | H3C—O3W—H3D | 115 (3) |
C8i—C7—H7A | 109.6 | H3C—O3W—H3E | 109 (3) |
N3—C7—H7B | 109.6 | H4C—O4W—H4D | 108 (3) |
C8i—C7—H7B | 109.6 | H5A—O5W—H5B | 105 (3) |
H7A—C7—H7B | 108.1 | H5A—O5W—H5C | 105 (2) |
C4—N1—C1—C2 | −0.7 (2) | C2—C1—C5—O2 | 81.59 (19) |
C4—N1—C1—C5 | −179.52 (13) | N1—C1—C5—O1 | 75.09 (17) |
C3—N2—C2—C1 | −0.7 (2) | C2—C1—C5—O1 | −103.67 (17) |
C3—N2—C2—C6 | 178.21 (14) | N2—C2—C6—O3 | −172.27 (14) |
N1—C1—C2—N2 | 1.1 (2) | C1—C2—C6—O3 | 6.7 (2) |
C5—C1—C2—N2 | 179.79 (14) | N2—C2—C6—O4 | 7.0 (2) |
N1—C1—C2—C6 | −177.78 (14) | C1—C2—C6—O4 | −174.06 (14) |
C5—C1—C2—C6 | 0.9 (2) | C8—N3—C7—C8i | 57.1 (2) |
C2—N2—C3—C4 | 0.0 (2) | C7—N3—C8—C7i | −57.1 (2) |
C1—N1—C4—C3 | 0.0 (2) | C10—N4—C9—C10ii | −57.44 (18) |
N2—C3—C4—N1 | 0.4 (3) | C9—N4—C10—C9ii | 57.60 (18) |
N1—C1—C5—O2 | −99.66 (17) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+1, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
N3—H3A···O1 | 0.91 (2) | 1.77 (2) | 2.6633 (18) | 165 (2) |
N3—H3B···O4Wiii | 0.91 (2) | 1.82 (2) | 2.730 (2) | 173 (2) |
N4—H4A···O4iv | 0.92 (2) | 1.81 (2) | 2.7145 (18) | 168 (2) |
N4—H4B···O1 | 0.93 (2) | 1.81 (2) | 2.7308 (18) | 170 (2) |
O1W—H1A···O5W | 0.84 (1) | 1.79 (1) | 2.633 (3) | 178 (5) |
O1W—H1B···O3Wv | 0.84 (1) | 1.84 (2) | 2.666 (3) | 166 (5) |
O2W—H2A···O2 | 0.84 (1) | 2.10 (1) | 2.902 (2) | 160 (3) |
O2W—H2B···O3Wvi | 0.83 (1) | 1.97 (3) | 2.747 (2) | 154 (5) |
O2W—H2C···O5Wvii | 0.83 (1) | 1.96 (2) | 2.754 (3) | 160 (4) |
O3W—H3C···O3 | 0.83 (1) | 1.96 (1) | 2.793 (2) | 177 (3) |
O3W—H3D···O3Wv | 0.83 (1) | 1.99 (2) | 2.794 (4) | 165 (4) |
O3W—H3E···O2Wviii | 0.83 (1) | 2.08 (3) | 2.747 (2) | 137 (4) |
O4W—H4C···O1W | 0.84 (1) | 2.07 (2) | 2.887 (3) | 164 (4) |
O4W—H4C···O1Wix | 0.84 (1) | 2.02 (2) | 2.793 (4) | 152 (4) |
O4W—H4D···O3 | 0.84 (1) | 2.10 (2) | 2.862 (2) | 151 (3) |
O5W—H5A···O4 | 0.84 (1) | 1.91 (1) | 2.7476 (18) | 171 (2) |
O5W—H5B···O2Wx | 0.84 (1) | 1.98 (2) | 2.754 (3) | 152 (4) |
Symmetry codes: (iii) −x, −y+1, −z+1; (iv) −x+1, −y, −z+2; (v) −x+1, −y, −z+1; (vi) x−1, y+1, z; (vii) x, y+1, z; (viii) x+1, y−1, z; (ix) −x, −y, −z+1; (x) x, y−1, z. |
(C4H12N2)2[Zn2(C6H2N2O4)4(H2O)2]·10H2O | Z = 2 |
Mr = 1187.62 | F(000) = 1232 |
Triclinic, P1 | Dx = 1.665 Mg m−3 |
a = 10.2828 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.7110 (7) Å | Cell parameters from 8797 reflections |
c = 20.2387 (10) Å | θ = 2.2–31.3° |
α = 96.671 (3)° | µ = 1.12 mm−1 |
β = 98.200 (3)° | T = 90 K |
γ = 112.923 (4)° | Plate, pink |
V = 2368.3 (2) Å3 | 0.55 × 0.29 × 0.22 mm |
Bruker SMART 1000 diffractometer | 11694 independent reflections |
Radiation source: fine-focus sealed tube | 9431 reflections with I > 2σ(I) |
Detector resolution: 8.3 pixels mm-1 | Rint = 0.016 |
ω scans | θmax = 28.3°, θmin = 1.0° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −13→13 |
Tmin = 0.578, Tmax = 0.791 | k = −16→16 |
31671 measured reflections | l = −26→26 |
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)] = 0.024 | Hydrogen site location: mixed |
wR(F2) = 0.076 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0406P)2 + 0.5808P] where P = (Fo2 + 2Fc2)/3 |
11694 reflections | (Δ/σ)max = 0.003 |
803 parameters | Δρmax = 0.56 e Å−3 |
10 restraints | Δρmin = −0.27 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Zn1 | 0.36001 (2) | 0.32198 (2) | 0.10937 (2) | 0.00928 (4) | |
Zn2 | 0.63884 (2) | 0.17939 (2) | 0.39223 (2) | 0.00936 (4) | |
O1 | 0.25764 (9) | 0.20454 (7) | 0.02012 (4) | 0.01321 (16) | |
O2 | 0.05456 (9) | 0.12863 (8) | −0.06032 (4) | 0.01929 (18) | |
O3 | −0.00726 (9) | 0.30883 (8) | −0.12502 (4) | 0.01646 (17) | |
O4 | −0.22197 (9) | 0.20074 (7) | −0.10368 (4) | 0.01592 (17) | |
O5 | 0.43296 (9) | 0.42570 (7) | 0.20590 (4) | 0.01194 (15) | |
O6 | 0.48052 (9) | 0.42090 (7) | 0.31699 (4) | 0.01292 (16) | |
O7 | 0.45189 (8) | 0.20790 (7) | 0.39968 (4) | 0.01220 (15) | |
O8 | 0.27078 (8) | 0.26330 (7) | 0.38967 (4) | 0.01264 (16) | |
O9 | 0.56406 (9) | 0.07468 (7) | 0.29594 (4) | 0.01197 (15) | |
O10 | 0.51404 (9) | 0.07829 (7) | 0.18478 (4) | 0.01297 (16) | |
O11 | 0.54420 (8) | 0.29043 (7) | 0.10115 (4) | 0.01210 (15) | |
O12 | 0.72442 (9) | 0.23380 (7) | 0.11160 (4) | 0.01266 (16) | |
O13 | 0.73926 (9) | 0.29918 (7) | 0.48091 (4) | 0.01361 (16) | |
O14 | 0.94340 (9) | 0.38125 (7) | 0.56047 (4) | 0.01753 (17) | |
O15 | 1.00814 (9) | 0.20770 (8) | 0.63034 (4) | 0.01694 (17) | |
O16 | 1.22328 (8) | 0.30824 (7) | 0.60649 (4) | 0.01458 (16) | |
O17 | 0.45720 (10) | 0.46702 (7) | 0.06812 (4) | 0.01450 (16) | |
H17A | 0.418 (2) | 0.5098 (17) | 0.0527 (10) | 0.039 (5)* | |
H17B | 0.542 (2) | 0.5084 (15) | 0.0872 (8) | 0.024 (4)* | |
O18 | 0.54465 (10) | 0.03455 (8) | 0.43415 (4) | 0.01582 (17) | |
H18A | 0.583 (2) | −0.0090 (18) | 0.4472 (10) | 0.043 (5)* | |
H18B | 0.460 (2) | −0.0040 (15) | 0.4179 (9) | 0.024 (4)* | |
N1 | 0.15686 (10) | 0.34256 (8) | 0.08613 (5) | 0.01156 (18) | |
N2 | −0.07644 (10) | 0.37796 (8) | 0.02283 (5) | 0.01292 (18) | |
N3 | 0.28575 (10) | 0.19637 (8) | 0.17362 (5) | 0.00985 (17) | |
N4 | 0.23147 (10) | 0.05783 (8) | 0.27159 (5) | 0.01168 (18) | |
N5 | 0.71090 (10) | 0.30377 (8) | 0.32734 (5) | 0.00990 (17) | |
N6 | 0.76470 (10) | 0.44117 (8) | 0.22873 (5) | 0.01140 (18) | |
N7 | 0.84157 (10) | 0.16037 (8) | 0.41759 (5) | 0.01163 (18) | |
N8 | 1.07438 (10) | 0.12673 (8) | 0.48293 (5) | 0.01335 (19) | |
C1 | 0.08820 (11) | 0.28795 (9) | 0.02253 (5) | 0.0106 (2) | |
C2 | −0.02554 (11) | 0.30984 (9) | −0.01052 (5) | 0.0108 (2) | |
C3 | −0.01152 (12) | 0.42706 (10) | 0.08783 (6) | 0.0140 (2) | |
H3 | −0.0481 | 0.4731 | 0.1131 | 0.017* | |
C4 | 0.10800 (12) | 0.41216 (10) | 0.11915 (6) | 0.0133 (2) | |
H4 | 0.1553 | 0.4518 | 0.1644 | 0.016* | |
C5 | 0.13750 (12) | 0.19941 (9) | −0.00951 (5) | 0.0121 (2) | |
C6 | −0.09123 (12) | 0.26683 (9) | −0.08617 (5) | 0.0116 (2) | |
C7 | 0.33480 (11) | 0.24383 (9) | 0.24015 (5) | 0.00929 (19) | |
C8 | 0.30621 (11) | 0.17441 (9) | 0.28928 (5) | 0.00965 (19) | |
C9 | 0.18231 (12) | 0.01257 (9) | 0.20531 (6) | 0.0125 (2) | |
H9 | 0.1283 | −0.0690 | 0.1915 | 0.015* | |
C10 | 0.20820 (12) | 0.08192 (9) | 0.15585 (6) | 0.0117 (2) | |
H10 | 0.1702 | 0.0473 | 0.1092 | 0.014* | |
C11 | 0.42373 (11) | 0.37480 (9) | 0.25730 (5) | 0.00985 (19) | |
C12 | 0.34901 (11) | 0.22119 (9) | 0.36525 (5) | 0.00971 (19) | |
C13 | 0.66174 (11) | 0.25576 (9) | 0.26089 (5) | 0.00937 (19) | |
C14 | 0.68997 (11) | 0.32452 (9) | 0.21149 (5) | 0.00952 (19) | |
C15 | 0.81350 (12) | 0.48700 (9) | 0.29487 (6) | 0.0123 (2) | |
H15 | 0.8671 | 0.5687 | 0.3084 | 0.015* | |
C16 | 0.78810 (11) | 0.41836 (9) | 0.34471 (5) | 0.0116 (2) | |
H16 | 0.8261 | 0.4536 | 0.3913 | 0.014* | |
C17 | 0.57234 (11) | 0.12511 (9) | 0.24416 (5) | 0.00972 (19) | |
C18 | 0.64680 (11) | 0.27700 (9) | 0.13573 (5) | 0.00951 (19) | |
C19 | 0.91068 (11) | 0.21770 (9) | 0.48071 (5) | 0.0105 (2) | |
C20 | 1.02447 (11) | 0.19724 (9) | 0.51482 (6) | 0.0111 (2) | |
C21 | 1.00796 (12) | 0.07386 (10) | 0.41878 (6) | 0.0145 (2) | |
H21 | 1.0433 | 0.0254 | 0.3948 | 0.017* | |
C22 | 0.88872 (12) | 0.08775 (10) | 0.38622 (6) | 0.0136 (2) | |
H22 | 0.8406 | 0.0455 | 0.3416 | 0.016* | |
C23 | 0.86063 (12) | 0.30710 (9) | 0.51069 (5) | 0.0117 (2) | |
C24 | 1.09164 (12) | 0.24428 (9) | 0.59013 (6) | 0.0120 (2) | |
N9 | 0.60807 (10) | 0.09967 (8) | −0.01664 (5) | 0.01136 (18) | |
H9A | 0.6386 (17) | 0.1450 (14) | 0.0223 (8) | 0.018 (4)* | |
H9B | 0.6597 (18) | 0.1350 (14) | −0.0457 (8) | 0.022 (4)* | |
C25 | 0.63331 (12) | −0.00707 (10) | −0.00926 (6) | 0.0126 (2) | |
H25A | 0.7375 | 0.0151 | 0.0073 | 0.015* | |
H25B | 0.6030 | −0.0594 | −0.0541 | 0.015* | |
C26 | 0.45115 (12) | 0.07024 (10) | −0.04026 (6) | 0.0127 (2) | |
H26A | 0.4159 | 0.0203 | −0.0860 | 0.015* | |
H26B | 0.4370 | 0.1424 | −0.0433 | 0.015* | |
N10 | 0.39241 (10) | 0.40094 (8) | 0.51753 (5) | 0.01088 (18) | |
H10A | 0.3408 (17) | 0.3671 (14) | 0.5472 (8) | 0.020 (4)* | |
H10B | 0.3608 (17) | 0.3550 (14) | 0.4786 (8) | 0.017 (4)* | |
C27 | 0.36726 (12) | 0.50759 (9) | 0.50979 (6) | 0.0119 (2) | |
H27A | 0.3986 | 0.5606 | 0.5544 | 0.014* | |
H27B | 0.2630 | 0.4855 | 0.4937 | 0.014* | |
C28 | 0.54952 (12) | 0.43052 (10) | 0.54050 (6) | 0.0122 (2) | |
H28A | 0.5638 | 0.3585 | 0.5439 | 0.015* | |
H28B | 0.5858 | 0.4813 | 0.5860 | 0.015* | |
N11 | 0.55355 (11) | 0.66652 (9) | 0.23906 (5) | 0.01346 (19) | |
H11A | 0.5344 (17) | 0.5939 (15) | 0.2268 (8) | 0.021 (4)* | |
H11B | 0.6500 (18) | 0.7150 (14) | 0.2523 (8) | 0.022 (4)* | |
N12 | 0.43762 (11) | 0.83754 (9) | 0.26127 (5) | 0.01438 (19) | |
H12A | 0.3431 (18) | 0.7959 (14) | 0.2500 (8) | 0.022 (4)* | |
H12B | 0.4619 (17) | 0.9108 (14) | 0.2731 (8) | 0.018 (4)* | |
C29 | 0.49190 (14) | 0.70546 (10) | 0.18043 (6) | 0.0175 (2) | |
H29A | 0.3890 | 0.6522 | 0.1635 | 0.021* | |
H29B | 0.5437 | 0.7030 | 0.1430 | 0.021* | |
C30 | 0.50543 (13) | 0.82825 (10) | 0.20181 (6) | 0.0153 (2) | |
H30A | 0.6087 | 0.8826 | 0.2137 | 0.018* | |
H30B | 0.4583 | 0.8510 | 0.1633 | 0.018* | |
C31 | 0.48271 (12) | 0.67315 (10) | 0.29758 (6) | 0.0144 (2) | |
H31A | 0.5280 | 0.6490 | 0.3360 | 0.017* | |
H31B | 0.3794 | 0.6190 | 0.2845 | 0.017* | |
C32 | 0.49636 (13) | 0.79573 (10) | 0.31967 (6) | 0.0150 (2) | |
H32A | 0.4429 | 0.7972 | 0.3565 | 0.018* | |
H32B | 0.5991 | 0.8484 | 0.3376 | 0.018* | |
O1W | 1.18115 (9) | 0.15367 (8) | 0.72431 (5) | 0.01885 (18) | |
H1A | 1.108 (2) | 0.1726 (16) | 0.7046 (10) | 0.044 (5)* | |
H1B | 1.154 (3) | 0.138 (2) | 0.7615 (13) | 0.087 (8)* | |
O2W | −0.13775 (10) | 0.29719 (8) | −0.25026 (5) | 0.0226 (2) | |
H2A | −0.088 (2) | 0.3034 (17) | −0.2089 (11) | 0.049 (6)* | |
H2B | −0.115 (3) | 0.261 (2) | −0.2771 (13) | 0.092 (9)* | |
O3W | 0.72995 (10) | 0.08575 (9) | 0.63463 (5) | 0.0242 (2) | |
H3A | 0.803 (2) | 0.1169 (15) | 0.6230 (9) | 0.026 (4)* | |
H3B | 0.743 (2) | 0.0414 (17) | 0.6592 (10) | 0.034 (5)* | |
O4W | 0.27545 (10) | 0.40370 (8) | −0.14273 (5) | 0.01873 (18) | |
H4A | 0.205 (2) | 0.3743 (16) | −0.1284 (9) | 0.029 (5)* | |
H4B | 0.262 (2) | 0.4507 (17) | −0.1636 (10) | 0.033 (5)* | |
O5W | 0.17206 (11) | 0.06342 (10) | −0.16305 (5) | 0.0220 (2) | |
H5A | 0.141 (2) | 0.0815 (16) | −0.1318 (10) | 0.030 (5)* | |
H5B | 0.144 (2) | 0.0012 (16) | −0.1691 (9) | 0.037 (6)* | |
O6W | 0.83275 (11) | 0.45113 (9) | 0.66338 (6) | 0.0228 (2) | |
H6A | 0.860 (2) | 0.4329 (16) | 0.6315 (10) | 0.035 (5)* | |
H6B | 0.851 (2) | 0.4196 (17) | 0.6876 (10) | 0.046 (6)* | |
O7W | −0.35828 (10) | 0.37966 (8) | −0.01897 (5) | 0.01772 (18) | |
H7A | −0.395 (2) | 0.3580 (16) | 0.0133 (10) | 0.033 (5)* | |
H7B | −0.278 (2) | 0.3823 (17) | −0.0095 (10) | 0.042 (5)* | |
O8WA | 0.05498 (15) | 0.30744 (12) | 0.31076 (8) | 0.0274 (3) | 0.8 |
O8WB | 0.1036 (7) | 0.3259 (6) | 0.2919 (3) | 0.0277 (14)* | 0.2 |
H8A | 0.1260 (17) | 0.2970 (19) | 0.3262 (9) | 0.072 (8)* | |
H8B | 0.0909 (19) | 0.3797 (8) | 0.3143 (9) | 0.061 (7)* | |
O9WA | 0.93562 (15) | 0.17518 (12) | 0.18230 (7) | 0.0244 (3) | 0.8 |
O9WB | 0.8832 (7) | 0.1529 (6) | 0.2009 (4) | 0.0358 (15)* | 0.2 |
H9C | 0.8635 (16) | 0.1871 (19) | 0.1690 (9) | 0.070 (8)* | |
H9D | 0.9627 (14) | 0.2115 (12) | 0.2213 (6) | 0.047 (6)* | |
O10W | 1.35708 (10) | 0.12306 (8) | 0.52120 (5) | 0.01814 (18) | |
H10C | 1.387 (2) | 0.1424 (16) | 0.4866 (10) | 0.034 (5)* | |
H10D | 1.278 (2) | 0.1217 (17) | 0.5143 (10) | 0.040 (5)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.01032 (7) | 0.00978 (7) | 0.00743 (7) | 0.00421 (5) | 0.00072 (5) | 0.00156 (5) |
Zn2 | 0.01055 (7) | 0.01044 (7) | 0.00738 (7) | 0.00492 (5) | 0.00103 (5) | 0.00171 (5) |
O1 | 0.0141 (4) | 0.0151 (4) | 0.0109 (4) | 0.0084 (3) | −0.0005 (3) | −0.0004 (3) |
O2 | 0.0183 (4) | 0.0199 (4) | 0.0158 (4) | 0.0095 (4) | −0.0049 (3) | −0.0067 (3) |
O3 | 0.0127 (4) | 0.0227 (4) | 0.0120 (4) | 0.0044 (3) | 0.0033 (3) | 0.0055 (3) |
O4 | 0.0115 (4) | 0.0202 (4) | 0.0124 (4) | 0.0031 (3) | 0.0013 (3) | 0.0029 (3) |
O5 | 0.0156 (4) | 0.0092 (4) | 0.0095 (4) | 0.0038 (3) | 0.0017 (3) | 0.0021 (3) |
O6 | 0.0159 (4) | 0.0109 (4) | 0.0095 (4) | 0.0042 (3) | 0.0004 (3) | 0.0001 (3) |
O7 | 0.0126 (4) | 0.0151 (4) | 0.0102 (4) | 0.0070 (3) | 0.0017 (3) | 0.0033 (3) |
O8 | 0.0133 (4) | 0.0149 (4) | 0.0111 (4) | 0.0075 (3) | 0.0025 (3) | 0.0016 (3) |
O9 | 0.0154 (4) | 0.0099 (4) | 0.0094 (4) | 0.0043 (3) | 0.0017 (3) | 0.0021 (3) |
O10 | 0.0157 (4) | 0.0112 (4) | 0.0094 (4) | 0.0042 (3) | 0.0002 (3) | 0.0001 (3) |
O11 | 0.0122 (4) | 0.0144 (4) | 0.0104 (4) | 0.0064 (3) | 0.0013 (3) | 0.0030 (3) |
O12 | 0.0135 (4) | 0.0149 (4) | 0.0109 (4) | 0.0076 (3) | 0.0025 (3) | 0.0014 (3) |
O13 | 0.0154 (4) | 0.0165 (4) | 0.0103 (4) | 0.0100 (3) | −0.0006 (3) | −0.0004 (3) |
O14 | 0.0177 (4) | 0.0175 (4) | 0.0144 (4) | 0.0082 (3) | −0.0026 (3) | −0.0046 (3) |
O15 | 0.0121 (4) | 0.0225 (4) | 0.0137 (4) | 0.0035 (3) | 0.0022 (3) | 0.0076 (3) |
O16 | 0.0105 (4) | 0.0166 (4) | 0.0135 (4) | 0.0028 (3) | 0.0010 (3) | 0.0029 (3) |
O17 | 0.0135 (4) | 0.0142 (4) | 0.0165 (4) | 0.0056 (3) | 0.0021 (3) | 0.0070 (3) |
O18 | 0.0156 (4) | 0.0174 (4) | 0.0188 (4) | 0.0088 (4) | 0.0056 (3) | 0.0103 (3) |
N1 | 0.0118 (4) | 0.0116 (4) | 0.0104 (4) | 0.0043 (4) | 0.0014 (3) | 0.0016 (3) |
N2 | 0.0126 (4) | 0.0132 (4) | 0.0141 (4) | 0.0060 (4) | 0.0036 (4) | 0.0037 (4) |
N3 | 0.0096 (4) | 0.0113 (4) | 0.0087 (4) | 0.0048 (4) | 0.0013 (3) | 0.0010 (3) |
N4 | 0.0123 (4) | 0.0101 (4) | 0.0121 (4) | 0.0041 (4) | 0.0025 (3) | 0.0020 (3) |
N5 | 0.0093 (4) | 0.0116 (4) | 0.0091 (4) | 0.0048 (4) | 0.0015 (3) | 0.0013 (3) |
N6 | 0.0121 (4) | 0.0101 (4) | 0.0112 (4) | 0.0038 (4) | 0.0024 (3) | 0.0017 (3) |
N7 | 0.0114 (4) | 0.0115 (4) | 0.0111 (4) | 0.0042 (4) | 0.0010 (3) | 0.0019 (3) |
N8 | 0.0121 (4) | 0.0124 (4) | 0.0161 (5) | 0.0054 (4) | 0.0032 (4) | 0.0036 (4) |
C1 | 0.0104 (5) | 0.0102 (5) | 0.0105 (5) | 0.0039 (4) | 0.0016 (4) | 0.0017 (4) |
C2 | 0.0098 (5) | 0.0109 (5) | 0.0112 (5) | 0.0031 (4) | 0.0025 (4) | 0.0038 (4) |
C3 | 0.0146 (5) | 0.0129 (5) | 0.0153 (5) | 0.0063 (4) | 0.0050 (4) | 0.0016 (4) |
C4 | 0.0141 (5) | 0.0129 (5) | 0.0104 (5) | 0.0040 (4) | 0.0015 (4) | −0.0002 (4) |
C5 | 0.0139 (5) | 0.0121 (5) | 0.0113 (5) | 0.0066 (4) | 0.0021 (4) | 0.0017 (4) |
C6 | 0.0115 (5) | 0.0130 (5) | 0.0112 (5) | 0.0060 (4) | 0.0015 (4) | 0.0030 (4) |
C7 | 0.0089 (5) | 0.0090 (5) | 0.0093 (5) | 0.0037 (4) | 0.0008 (4) | 0.0005 (4) |
C8 | 0.0093 (5) | 0.0098 (5) | 0.0101 (5) | 0.0045 (4) | 0.0013 (4) | 0.0011 (4) |
C9 | 0.0125 (5) | 0.0096 (5) | 0.0131 (5) | 0.0031 (4) | 0.0014 (4) | 0.0006 (4) |
C10 | 0.0113 (5) | 0.0119 (5) | 0.0100 (5) | 0.0040 (4) | 0.0002 (4) | −0.0002 (4) |
C11 | 0.0097 (5) | 0.0090 (5) | 0.0112 (5) | 0.0043 (4) | 0.0020 (4) | 0.0018 (4) |
C12 | 0.0108 (5) | 0.0074 (5) | 0.0097 (5) | 0.0021 (4) | 0.0023 (4) | 0.0026 (4) |
C13 | 0.0091 (5) | 0.0099 (5) | 0.0090 (5) | 0.0044 (4) | 0.0012 (4) | 0.0007 (4) |
C14 | 0.0090 (5) | 0.0105 (5) | 0.0094 (5) | 0.0047 (4) | 0.0013 (4) | 0.0015 (4) |
C15 | 0.0122 (5) | 0.0100 (5) | 0.0127 (5) | 0.0030 (4) | 0.0022 (4) | 0.0003 (4) |
C16 | 0.0110 (5) | 0.0123 (5) | 0.0096 (5) | 0.0040 (4) | 0.0011 (4) | −0.0004 (4) |
C17 | 0.0096 (5) | 0.0089 (5) | 0.0112 (5) | 0.0043 (4) | 0.0022 (4) | 0.0018 (4) |
C18 | 0.0103 (5) | 0.0076 (5) | 0.0085 (5) | 0.0012 (4) | 0.0019 (4) | 0.0022 (4) |
C19 | 0.0108 (5) | 0.0098 (5) | 0.0104 (5) | 0.0040 (4) | 0.0017 (4) | 0.0018 (4) |
C20 | 0.0095 (5) | 0.0102 (5) | 0.0124 (5) | 0.0026 (4) | 0.0016 (4) | 0.0037 (4) |
C21 | 0.0143 (5) | 0.0123 (5) | 0.0176 (5) | 0.0060 (4) | 0.0046 (4) | 0.0018 (4) |
C22 | 0.0147 (5) | 0.0125 (5) | 0.0122 (5) | 0.0049 (4) | 0.0024 (4) | −0.0003 (4) |
C23 | 0.0141 (5) | 0.0117 (5) | 0.0104 (5) | 0.0062 (4) | 0.0027 (4) | 0.0020 (4) |
C24 | 0.0123 (5) | 0.0118 (5) | 0.0121 (5) | 0.0054 (4) | 0.0006 (4) | 0.0041 (4) |
N9 | 0.0129 (4) | 0.0109 (4) | 0.0092 (4) | 0.0039 (4) | 0.0024 (4) | 0.0012 (4) |
C25 | 0.0143 (5) | 0.0120 (5) | 0.0131 (5) | 0.0068 (4) | 0.0043 (4) | 0.0022 (4) |
C26 | 0.0128 (5) | 0.0134 (5) | 0.0125 (5) | 0.0058 (4) | 0.0021 (4) | 0.0037 (4) |
N10 | 0.0124 (4) | 0.0102 (4) | 0.0098 (4) | 0.0042 (4) | 0.0031 (4) | 0.0017 (3) |
C27 | 0.0136 (5) | 0.0115 (5) | 0.0123 (5) | 0.0062 (4) | 0.0042 (4) | 0.0025 (4) |
C28 | 0.0127 (5) | 0.0131 (5) | 0.0119 (5) | 0.0059 (4) | 0.0024 (4) | 0.0042 (4) |
N11 | 0.0153 (5) | 0.0098 (4) | 0.0150 (5) | 0.0049 (4) | 0.0029 (4) | 0.0028 (4) |
N12 | 0.0134 (5) | 0.0097 (5) | 0.0185 (5) | 0.0042 (4) | 0.0003 (4) | 0.0030 (4) |
C29 | 0.0233 (6) | 0.0141 (5) | 0.0128 (5) | 0.0074 (5) | −0.0017 (4) | 0.0011 (4) |
C30 | 0.0188 (6) | 0.0132 (5) | 0.0137 (5) | 0.0066 (5) | 0.0005 (4) | 0.0051 (4) |
C31 | 0.0159 (5) | 0.0125 (5) | 0.0169 (5) | 0.0063 (4) | 0.0054 (4) | 0.0065 (4) |
C32 | 0.0184 (6) | 0.0144 (5) | 0.0129 (5) | 0.0075 (5) | 0.0022 (4) | 0.0028 (4) |
O1W | 0.0167 (4) | 0.0223 (4) | 0.0167 (4) | 0.0073 (4) | 0.0013 (3) | 0.0060 (3) |
O2W | 0.0227 (5) | 0.0248 (5) | 0.0142 (4) | 0.0050 (4) | −0.0012 (4) | 0.0046 (4) |
O3W | 0.0173 (5) | 0.0269 (5) | 0.0360 (6) | 0.0108 (4) | 0.0118 (4) | 0.0205 (4) |
O4W | 0.0140 (4) | 0.0191 (4) | 0.0244 (5) | 0.0060 (4) | 0.0050 (4) | 0.0107 (4) |
O5W | 0.0260 (5) | 0.0247 (5) | 0.0188 (5) | 0.0116 (4) | 0.0092 (4) | 0.0068 (4) |
O6W | 0.0258 (5) | 0.0267 (5) | 0.0239 (5) | 0.0159 (4) | 0.0117 (4) | 0.0089 (4) |
O7W | 0.0178 (4) | 0.0262 (5) | 0.0161 (4) | 0.0140 (4) | 0.0062 (4) | 0.0094 (4) |
O8WA | 0.0238 (7) | 0.0218 (7) | 0.0335 (7) | 0.0118 (6) | −0.0087 (6) | 0.0029 (6) |
O9WA | 0.0255 (7) | 0.0240 (6) | 0.0264 (7) | 0.0162 (6) | −0.0022 (6) | 0.0029 (5) |
O10W | 0.0194 (4) | 0.0270 (5) | 0.0164 (4) | 0.0155 (4) | 0.0070 (4) | 0.0102 (4) |
Zn1—O1 | 2.0510 (8) | C19—C23 | 1.5194 (14) |
Zn1—O17 | 2.0629 (8) | C20—C24 | 1.5245 (15) |
Zn1—O5 | 2.0810 (8) | C21—C22 | 1.3907 (16) |
Zn1—O11 | 2.1075 (8) | C21—H21 | 0.9500 |
Zn1—N3 | 2.1537 (9) | C22—H22 | 0.9500 |
Zn1—N1 | 2.1972 (9) | N9—C26 | 1.4967 (14) |
Zn2—O13 | 2.0537 (8) | N9—C25 | 1.4969 (14) |
Zn2—O18 | 2.0629 (9) | N9—H9A | 0.857 (17) |
Zn2—O9 | 2.0816 (8) | N9—H9B | 0.891 (17) |
Zn2—O7 | 2.1124 (8) | C25—C26i | 1.5152 (15) |
Zn2—N5 | 2.1496 (9) | C25—H25A | 0.9900 |
Zn2—N7 | 2.1872 (9) | C25—H25B | 0.9900 |
O1—C5 | 1.2676 (13) | C26—C25i | 1.5152 (15) |
O2—C5 | 1.2374 (13) | C26—H26A | 0.9900 |
O3—C6 | 1.2573 (13) | C26—H26B | 0.9900 |
O4—C6 | 1.2465 (14) | N10—C28 | 1.4965 (14) |
O5—C11 | 1.2832 (13) | N10—C27 | 1.4967 (14) |
O6—C11 | 1.2295 (13) | N10—H10A | 0.894 (16) |
O7—C12 | 1.2608 (13) | N10—H10B | 0.861 (16) |
O8—C12 | 1.2511 (13) | C27—C28ii | 1.5155 (15) |
O9—C17 | 1.2867 (13) | C27—H27A | 0.9900 |
O10—C17 | 1.2281 (13) | C27—H27B | 0.9900 |
O11—C18 | 1.2608 (13) | C28—C27ii | 1.5155 (15) |
O12—C18 | 1.2520 (13) | C28—H28A | 0.9900 |
O13—C23 | 1.2667 (13) | C28—H28B | 0.9900 |
O14—C23 | 1.2401 (13) | N11—C31 | 1.4869 (15) |
O15—C24 | 1.2617 (14) | N11—C29 | 1.4904 (15) |
O16—C24 | 1.2471 (14) | N11—H11A | 0.862 (17) |
O17—H17A | 0.85 (2) | N11—H11B | 0.919 (17) |
O17—H17B | 0.829 (18) | N12—C30 | 1.4896 (15) |
O18—H18A | 0.84 (2) | N12—C32 | 1.4956 (14) |
O18—H18B | 0.813 (19) | N12—H12A | 0.886 (17) |
N1—C4 | 1.3365 (14) | N12—H12B | 0.858 (16) |
N1—C1 | 1.3373 (14) | C29—C30 | 1.5164 (16) |
N2—C2 | 1.3406 (14) | C29—H29A | 0.9900 |
N2—C3 | 1.3416 (15) | C29—H29B | 0.9900 |
N3—C10 | 1.3321 (14) | C30—H30A | 0.9900 |
N3—C7 | 1.3461 (13) | C30—H30B | 0.9900 |
N4—C9 | 1.3367 (14) | C31—C32 | 1.5157 (15) |
N4—C8 | 1.3512 (14) | C31—H31A | 0.9900 |
N5—C16 | 1.3327 (14) | C31—H31B | 0.9900 |
N5—C13 | 1.3460 (13) | C32—H32A | 0.9900 |
N6—C15 | 1.3350 (14) | C32—H32B | 0.9900 |
N6—C14 | 1.3515 (14) | O1W—H1A | 0.92 (2) |
N7—C19 | 1.3378 (14) | O1W—H1B | 0.86 (3) |
N7—C22 | 1.3381 (14) | O2W—H2A | 0.90 (2) |
N8—C21 | 1.3382 (15) | O2W—H2B | 0.79 (3) |
N8—C20 | 1.3422 (14) | O3W—H3A | 0.782 (19) |
C1—C2 | 1.4023 (15) | O3W—H3B | 0.83 (2) |
C1—C5 | 1.5209 (15) | O4W—H4A | 0.790 (19) |
C2—C6 | 1.5239 (15) | O4W—H4B | 0.81 (2) |
C3—C4 | 1.3911 (16) | O5W—H5A | 0.800 (19) |
C3—H3 | 0.9500 | O5W—H5B | 0.717 (19) |
C4—H4 | 0.9500 | O6W—H6A | 0.78 (2) |
C7—C8 | 1.3924 (14) | O6W—H6B | 0.72 (2) |
C7—C11 | 1.5223 (14) | O7W—H7A | 0.82 (2) |
C8—C12 | 1.5173 (14) | O7W—H7B | 0.81 (2) |
C9—C10 | 1.3958 (15) | O8WA—H8A | 0.818 (9) |
C9—H9 | 0.9500 | O8WA—H8B | 0.836 (9) |
C10—H10 | 0.9500 | O8WB—H8A | 0.866 (9) |
C13—C14 | 1.3914 (14) | O8WB—H8B | 0.838 (9) |
C13—C17 | 1.5195 (14) | O9WA—H9C | 0.828 (9) |
C14—C18 | 1.5148 (14) | O9WA—H9D | 0.817 (9) |
C15—C16 | 1.3960 (15) | O9WB—H9C | 0.861 (9) |
C15—H15 | 0.9500 | O9WB—H9D | 0.867 (9) |
C16—H16 | 0.9500 | O10W—H10C | 0.83 (2) |
C19—C20 | 1.4005 (15) | O10W—H10D | 0.80 (2) |
O1—Zn1—O17 | 97.94 (3) | O10—C17—C13 | 118.97 (9) |
O1—Zn1—O5 | 170.37 (3) | O9—C17—C13 | 114.59 (9) |
O17—Zn1—O5 | 89.76 (3) | O12—C18—O11 | 124.83 (10) |
O1—Zn1—O11 | 87.45 (3) | O12—C18—C14 | 115.97 (9) |
O17—Zn1—O11 | 85.58 (3) | O11—C18—C14 | 119.01 (9) |
O5—Zn1—O11 | 98.95 (3) | N7—C19—C20 | 120.85 (10) |
O1—Zn1—N3 | 94.82 (3) | N7—C19—C23 | 115.69 (9) |
O17—Zn1—N3 | 167.18 (4) | C20—C19—C23 | 123.43 (10) |
O5—Zn1—N3 | 77.66 (3) | N8—C20—C19 | 120.64 (10) |
O11—Zn1—N3 | 93.84 (3) | N8—C20—C24 | 115.72 (9) |
O1—Zn1—N1 | 78.28 (3) | C19—C20—C24 | 123.49 (10) |
O17—Zn1—N1 | 88.36 (4) | N8—C21—C22 | 121.93 (10) |
O5—Zn1—N1 | 96.28 (3) | N8—C21—H21 | 119.0 |
O11—Zn1—N1 | 163.58 (3) | C22—C21—H21 | 119.0 |
N3—Zn1—N1 | 95.41 (3) | N7—C22—C21 | 120.21 (10) |
O13—Zn2—O18 | 98.27 (4) | N7—C22—H22 | 119.9 |
O13—Zn2—O9 | 170.87 (3) | C21—C22—H22 | 119.9 |
O18—Zn2—O9 | 89.65 (3) | O14—C23—O13 | 126.87 (10) |
O13—Zn2—O7 | 87.36 (3) | O14—C23—C19 | 117.07 (10) |
O18—Zn2—O7 | 85.65 (3) | O13—C23—C19 | 116.04 (9) |
O9—Zn2—O7 | 97.83 (3) | O16—C24—O15 | 126.21 (10) |
O13—Zn2—N5 | 94.59 (3) | O16—C24—C20 | 118.18 (10) |
O18—Zn2—N5 | 167.11 (4) | O15—C24—C20 | 115.45 (10) |
O9—Zn2—N5 | 77.62 (3) | C26—N9—C25 | 111.32 (8) |
O7—Zn2—N5 | 94.03 (3) | C26—N9—H9A | 109.2 (11) |
O13—Zn2—N7 | 78.22 (3) | C25—N9—H9A | 108.0 (10) |
O18—Zn2—N7 | 87.24 (4) | C26—N9—H9B | 111.2 (10) |
O9—Zn2—N7 | 97.73 (3) | C25—N9—H9B | 108.1 (10) |
O7—Zn2—N7 | 162.83 (3) | H9A—N9—H9B | 108.9 (14) |
N5—Zn2—N7 | 96.35 (3) | N9—C25—C26i | 110.37 (9) |
C5—O1—Zn1 | 117.73 (7) | N9—C25—H25A | 109.6 |
C11—O5—Zn1 | 117.87 (7) | C26i—C25—H25A | 109.6 |
C12—O7—Zn2 | 142.88 (7) | N9—C25—H25B | 109.6 |
C17—O9—Zn2 | 117.86 (7) | C26i—C25—H25B | 109.6 |
C18—O11—Zn1 | 142.43 (7) | H25A—C25—H25B | 108.1 |
C23—O13—Zn2 | 117.65 (7) | N9—C26—C25i | 109.63 (9) |
Zn1—O17—H17A | 127.0 (13) | N9—C26—H26A | 109.7 |
Zn1—O17—H17B | 114.4 (11) | C25i—C26—H26A | 109.7 |
H17A—O17—H17B | 109.0 (17) | N9—C26—H26B | 109.7 |
Zn2—O18—H18A | 126.5 (14) | C25i—C26—H26B | 109.7 |
Zn2—O18—H18B | 114.6 (12) | H26A—C26—H26B | 108.2 |
H18A—O18—H18B | 109.6 (18) | C28—N10—C27 | 111.18 (8) |
C4—N1—C1 | 118.44 (9) | C28—N10—H10A | 111.8 (10) |
C4—N1—Zn1 | 131.11 (8) | C27—N10—H10A | 107.1 (10) |
C1—N1—Zn1 | 109.40 (7) | C28—N10—H10B | 109.4 (10) |
C2—N2—C3 | 117.62 (10) | C27—N10—H10B | 107.8 (10) |
C10—N3—C7 | 118.63 (9) | H10A—N10—H10B | 109.4 (14) |
C10—N3—Zn1 | 128.78 (7) | N10—C27—C28ii | 110.33 (9) |
C7—N3—Zn1 | 112.46 (7) | N10—C27—H27A | 109.6 |
C9—N4—C8 | 117.34 (9) | C28ii—C27—H27A | 109.6 |
C16—N5—C13 | 118.55 (9) | N10—C27—H27B | 109.6 |
C16—N5—Zn2 | 128.66 (7) | C28ii—C27—H27B | 109.6 |
C13—N5—Zn2 | 112.67 (7) | H27A—C27—H27B | 108.1 |
C15—N6—C14 | 117.26 (9) | N10—C28—C27ii | 109.70 (9) |
C19—N7—C22 | 118.51 (9) | N10—C28—H28A | 109.7 |
C19—N7—Zn2 | 109.92 (7) | C27ii—C28—H28A | 109.7 |
C22—N7—Zn2 | 130.32 (8) | N10—C28—H28B | 109.7 |
C21—N8—C20 | 117.61 (10) | C27ii—C28—H28B | 109.7 |
N1—C1—C2 | 120.77 (10) | H28A—C28—H28B | 108.2 |
N1—C1—C5 | 116.04 (9) | C31—N11—C29 | 111.53 (9) |
C2—C1—C5 | 123.15 (9) | C31—N11—H11A | 105.7 (11) |
N2—C2—C1 | 120.74 (10) | C29—N11—H11A | 108.0 (11) |
N2—C2—C6 | 115.80 (9) | C31—N11—H11B | 108.7 (10) |
C1—C2—C6 | 123.31 (10) | C29—N11—H11B | 107.8 (10) |
N2—C3—C4 | 121.63 (10) | H11A—N11—H11B | 115.2 (14) |
N2—C3—H3 | 119.2 | C30—N12—C32 | 112.10 (9) |
C4—C3—H3 | 119.2 | C30—N12—H12A | 110.6 (10) |
N1—C4—C3 | 120.51 (10) | C32—N12—H12A | 108.0 (10) |
N1—C4—H4 | 119.7 | C30—N12—H12B | 104.2 (10) |
C3—C4—H4 | 119.7 | C32—N12—H12B | 108.3 (10) |
O2—C5—O1 | 127.26 (10) | H12A—N12—H12B | 113.7 (14) |
O2—C5—C1 | 116.65 (10) | N11—C29—C30 | 110.25 (9) |
O1—C5—C1 | 116.06 (9) | N11—C29—H29A | 109.6 |
O4—C6—O3 | 126.42 (10) | C30—C29—H29A | 109.6 |
O4—C6—C2 | 118.38 (10) | N11—C29—H29B | 109.6 |
O3—C6—C2 | 115.04 (9) | C30—C29—H29B | 109.6 |
N3—C7—C8 | 120.60 (10) | H29A—C29—H29B | 108.1 |
N3—C7—C11 | 116.23 (9) | N12—C30—C29 | 111.30 (9) |
C8—C7—C11 | 123.17 (9) | N12—C30—H30A | 109.4 |
N4—C8—C7 | 121.12 (10) | C29—C30—H30A | 109.4 |
N4—C8—C12 | 114.72 (9) | N12—C30—H30B | 109.4 |
C7—C8—C12 | 124.12 (9) | C29—C30—H30B | 109.4 |
N4—C9—C10 | 121.82 (10) | H30A—C30—H30B | 108.0 |
N4—C9—H9 | 119.1 | N11—C31—C32 | 110.80 (9) |
C10—C9—H9 | 119.1 | N11—C31—H31A | 109.5 |
N3—C10—C9 | 120.46 (10) | C32—C31—H31A | 109.5 |
N3—C10—H10 | 119.8 | N11—C31—H31B | 109.5 |
C9—C10—H10 | 119.8 | C32—C31—H31B | 109.5 |
O6—C11—O5 | 126.60 (10) | H31A—C31—H31B | 108.1 |
O6—C11—C7 | 118.66 (9) | N12—C32—C31 | 110.69 (9) |
O5—C11—C7 | 114.72 (9) | N12—C32—H32A | 109.5 |
O8—C12—O7 | 124.73 (10) | C31—C32—H32A | 109.5 |
O8—C12—C8 | 116.08 (9) | N12—C32—H32B | 109.5 |
O7—C12—C8 | 118.98 (9) | C31—C32—H32B | 109.5 |
N5—C13—C14 | 120.65 (10) | H32A—C32—H32B | 108.1 |
N5—C13—C17 | 116.23 (9) | H1A—O1W—H1B | 100.0 (19) |
C14—C13—C17 | 123.10 (9) | H2A—O2W—H2B | 108 (2) |
N6—C14—C13 | 121.16 (10) | H3A—O3W—H3B | 106.3 (17) |
N6—C14—C18 | 114.71 (9) | H4A—O4W—H4B | 105.4 (18) |
C13—C14—C18 | 124.09 (9) | H5A—O5W—H5B | 106.0 (19) |
N6—C15—C16 | 121.93 (10) | H6A—O6W—H6B | 103 (2) |
N6—C15—H15 | 119.0 | H7A—O7W—H7B | 104.5 (18) |
C16—C15—H15 | 119.0 | H8A—O8WA—H8B | 100.8 (18) |
N5—C16—C15 | 120.41 (10) | H8A—O8WB—H8B | 96.8 (17) |
N5—C16—H16 | 119.8 | H9C—O9WA—H9D | 101.7 (18) |
C15—C16—H16 | 119.8 | H9C—O9WB—H9D | 95.1 (17) |
O10—C17—O9 | 126.43 (10) | H10C—O10W—H10D | 102.8 (18) |
C4—N1—C1—C2 | 4.69 (15) | C15—N6—C14—C18 | −175.83 (9) |
Zn1—N1—C1—C2 | −164.87 (8) | N5—C13—C14—N6 | −1.33 (16) |
C4—N1—C1—C5 | −173.16 (10) | C17—C13—C14—N6 | 177.06 (9) |
Zn1—N1—C1—C5 | 17.27 (11) | N5—C13—C14—C18 | 176.08 (10) |
C3—N2—C2—C1 | 2.20 (15) | C17—C13—C14—C18 | −5.53 (16) |
C3—N2—C2—C6 | −173.48 (10) | C14—N6—C15—C16 | −0.53 (16) |
N1—C1—C2—N2 | −5.99 (16) | C13—N5—C16—C15 | 1.81 (15) |
C5—C1—C2—N2 | 171.71 (10) | Zn2—N5—C16—C15 | −173.99 (8) |
N1—C1—C2—C6 | 169.35 (10) | N6—C15—C16—N5 | −1.32 (17) |
C5—C1—C2—C6 | −12.95 (16) | Zn2—O9—C17—O10 | −167.84 (9) |
C2—N2—C3—C4 | 2.53 (16) | Zn2—O9—C17—C13 | 10.86 (11) |
C1—N1—C4—C3 | 0.01 (16) | N5—C13—C17—O10 | 173.57 (9) |
Zn1—N1—C4—C3 | 166.91 (8) | C14—C13—C17—O10 | −4.88 (15) |
N2—C3—C4—N1 | −3.78 (17) | N5—C13—C17—O9 | −5.23 (13) |
Zn1—O1—C5—O2 | −173.71 (10) | C14—C13—C17—O9 | 176.31 (10) |
Zn1—O1—C5—C1 | 4.18 (12) | Zn1—O11—C18—O12 | 163.47 (8) |
N1—C1—C5—O2 | 162.69 (10) | Zn1—O11—C18—C14 | −21.82 (17) |
C2—C1—C5—O2 | −15.11 (16) | N6—C14—C18—O12 | 99.92 (11) |
N1—C1—C5—O1 | −15.43 (14) | C13—C14—C18—O12 | −77.65 (13) |
C2—C1—C5—O1 | 166.77 (10) | N6—C14—C18—O11 | −75.25 (13) |
N2—C2—C6—O4 | −64.52 (14) | C13—C14—C18—O11 | 107.18 (12) |
C1—C2—C6—O4 | 119.93 (12) | C22—N7—C19—C20 | −3.70 (16) |
N2—C2—C6—O3 | 111.17 (11) | Zn2—N7—C19—C20 | 164.84 (8) |
C1—C2—C6—O3 | −64.38 (14) | C22—N7—C19—C23 | 174.38 (9) |
C10—N3—C7—C8 | 0.66 (15) | Zn2—N7—C19—C23 | −17.07 (11) |
Zn1—N3—C7—C8 | −175.51 (8) | C21—N8—C20—C19 | −2.52 (15) |
C10—N3—C7—C11 | 179.53 (9) | C21—N8—C20—C24 | 173.12 (10) |
Zn1—N3—C7—C11 | 3.36 (11) | N7—C19—C20—N8 | 5.47 (16) |
C9—N4—C8—C7 | −2.12 (15) | C23—C19—C20—N8 | −172.46 (10) |
C9—N4—C8—C12 | 175.51 (9) | N7—C19—C20—C24 | −169.82 (10) |
N3—C7—C8—N4 | 1.41 (16) | C23—C19—C20—C24 | 12.25 (16) |
C11—C7—C8—N4 | −177.38 (9) | C20—N8—C21—C22 | −1.88 (16) |
N3—C7—C8—C12 | −175.99 (9) | C19—N7—C22—C21 | −0.67 (16) |
C11—C7—C8—C12 | 5.22 (16) | Zn2—N7—C22—C21 | −166.50 (8) |
C8—N4—C9—C10 | 0.87 (16) | N8—C21—C22—N7 | 3.61 (17) |
C7—N3—C10—C9 | −1.90 (15) | Zn2—O13—C23—O14 | 172.31 (9) |
Zn1—N3—C10—C9 | 173.56 (8) | Zn2—O13—C23—C19 | −6.03 (12) |
N4—C9—C10—N3 | 1.17 (17) | N7—C19—C23—O14 | −162.11 (10) |
Zn1—O5—C11—O6 | 168.07 (9) | C20—C19—C23—O14 | 15.92 (16) |
Zn1—O5—C11—C7 | −10.71 (11) | N7—C19—C23—O13 | 16.39 (14) |
N3—C7—C11—O6 | −174.30 (9) | C20—C19—C23—O13 | −165.58 (10) |
C8—C7—C11—O6 | 4.54 (15) | N8—C20—C24—O16 | 63.10 (13) |
N3—C7—C11—O5 | 4.58 (13) | C19—C20—C24—O16 | −121.39 (12) |
C8—C7—C11—O5 | −176.58 (10) | N8—C20—C24—O15 | −112.57 (11) |
Zn2—O7—C12—O8 | −162.68 (8) | C19—C20—C24—O15 | 62.94 (14) |
Zn2—O7—C12—C8 | 22.81 (17) | C26—N9—C25—C26i | −58.03 (12) |
N4—C8—C12—O8 | −99.38 (11) | C25—N9—C26—C25i | 57.61 (12) |
C7—C8—C12—O8 | 78.18 (13) | C28—N10—C27—C28ii | 58.05 (12) |
N4—C8—C12—O7 | 75.61 (13) | C27—N10—C28—C27ii | −57.69 (12) |
C7—C8—C12—O7 | −106.84 (12) | C31—N11—C29—C30 | 57.06 (13) |
C16—N5—C13—C14 | −0.53 (15) | C32—N12—C30—C29 | 54.72 (13) |
Zn2—N5—C13—C14 | 175.91 (8) | N11—C29—C30—N12 | −55.28 (13) |
C16—N5—C13—C17 | −179.03 (9) | C29—N11—C31—C32 | −57.45 (13) |
Zn2—N5—C13—C17 | −2.59 (11) | C30—N12—C32—C31 | −54.46 (13) |
C15—N6—C14—C13 | 1.81 (15) | N11—C31—C32—N12 | 55.35 (13) |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O17—H17A···O7Wiii | 0.85 (2) | 1.90 (2) | 2.7437 (12) | 172.1 (19) |
O17—H17B···O4Wiv | 0.829 (18) | 1.872 (19) | 2.6941 (13) | 171.1 (16) |
O18—H18A···O10Wv | 0.84 (2) | 1.92 (2) | 2.7547 (12) | 171 (2) |
O18—H18B···O3Wvi | 0.813 (19) | 1.893 (19) | 2.6963 (14) | 169.6 (17) |
N9—H9A···O12 | 0.857 (17) | 1.901 (17) | 2.7517 (13) | 171.4 (15) |
N9—H9B···O4vii | 0.891 (17) | 1.844 (17) | 2.7318 (13) | 174.3 (15) |
N10—H10A···O16viii | 0.894 (16) | 1.838 (17) | 2.7283 (13) | 173.3 (15) |
N10—H10B···O8 | 0.861 (16) | 1.910 (17) | 2.7644 (13) | 171.5 (15) |
N11—H11A···O5 | 0.862 (17) | 1.941 (17) | 2.7725 (13) | 161.8 (15) |
N11—H11B···O1Wix | 0.919 (17) | 1.830 (17) | 2.7180 (14) | 161.7 (15) |
N12—H12A···O2Wiii | 0.886 (17) | 1.979 (17) | 2.8447 (14) | 165.3 (14) |
N12—H12B···O9x | 0.858 (16) | 1.895 (17) | 2.7320 (13) | 164.7 (15) |
O1W—H1A···O15 | 0.92 (2) | 1.90 (2) | 2.7466 (12) | 152.1 (17) |
O1W—H1B···O5Wxi | 0.86 (3) | 1.91 (3) | 2.6658 (13) | 146 (2) |
O2W—H2A···O3 | 0.90 (2) | 1.76 (2) | 2.6524 (12) | 173.9 (19) |
O2W—H2B···O15xii | 0.79 (3) | 2.57 (3) | 3.3329 (14) | 162 (2) |
O2W—H2B···O3Wxii | 0.79 (3) | 2.49 (3) | 3.0486 (15) | 129 (2) |
O3W—H3A···O15 | 0.782 (19) | 1.947 (19) | 2.6909 (13) | 158.7 (17) |
O3W—H3B···N4vi | 0.83 (2) | 2.05 (2) | 2.8713 (14) | 173.2 (18) |
O4W—H4A···O3 | 0.790 (19) | 2.02 (2) | 2.7750 (12) | 158.5 (18) |
O4W—H4B···N6iv | 0.81 (2) | 2.08 (2) | 2.8835 (13) | 171.3 (18) |
O5W—H5A···O2 | 0.800 (19) | 1.95 (2) | 2.7507 (14) | 175.8 (18) |
O5W—H5B···O9WAi | 0.717 (19) | 2.033 (19) | 2.7499 (18) | 178 (2) |
O5W—H5B···O9WBi | 0.717 (19) | 1.89 (2) | 2.577 (7) | 162 (2) |
O6W—H6A···O14 | 0.78 (2) | 1.95 (2) | 2.7304 (13) | 172.5 (19) |
O6W—H6B···O2Wxi | 0.72 (2) | 2.14 (2) | 2.8428 (14) | 168 (2) |
O7W—H7A···O11viii | 0.82 (2) | 2.13 (2) | 2.9414 (12) | 168.3 (18) |
O7W—H7B···N2 | 0.81 (2) | 2.11 (2) | 2.9102 (13) | 174 (2) |
O8WA—H8A···O8 | 0.82 (1) | 2.03 (1) | 2.8208 (15) | 162 (2) |
O8WB—H8A···O8 | 0.87 (1) | 2.03 (1) | 2.822 (6) | 151 (2) |
O8WA—H8B···O6Wii | 0.84 (1) | 1.95 (1) | 2.7782 (17) | 171 (2) |
O8WB—H8B···O6Wii | 0.84 (1) | 1.95 (1) | 2.658 (6) | 142 (2) |
O9WA—H9C···O12 | 0.83 (1) | 2.02 (1) | 2.8180 (14) | 161 (2) |
O9WB—H9C···O12 | 0.86 (1) | 2.02 (1) | 2.807 (7) | 151 (2) |
O9WA—H9D···O8WAvii | 0.82 (1) | 1.94 (1) | 2.749 (2) | 172 (2) |
O9WB—H9D···O8WBvii | 0.87 (1) | 1.88 (1) | 2.712 (10) | 160 (2) |
O10W—H10C···O7vii | 0.83 (2) | 2.12 (2) | 2.9399 (12) | 172.9 (18) |
O10W—H10D···N8 | 0.80 (2) | 2.12 (2) | 2.9196 (13) | 171.7 (19) |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x+1, −y+1, −z+1; (iii) −x, −y+1, −z; (iv) −x+1, −y+1, −z; (v) −x+2, −y, −z+1; (vi) −x+1, −y, −z+1; (vii) x+1, y, z; (viii) x−1, y, z; (ix) −x+2, −y+1, −z+1; (x) x, y+1, z; (xi) x+1, y, z+1; (xii) x−1, y, z−1. |
(C4H12N2)[Co(C6H2N2O4)2]·6H2O | F(000) = 610 |
Mr = 587.37 | Dx = 1.642 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 6.5238 (2) Å | Cell parameters from 9483 reflections |
b = 17.3808 (5) Å | θ = 3.0–31.5° |
c = 10.6599 (3) Å | µ = 0.81 mm−1 |
β = 100.656 (3)° | T = 90 K |
V = 1187.87 (6) Å3 | Lath, gold |
Z = 2 | 0.44 × 0.11 × 0.04 mm |
Bruker SMART APEXII diffractometer | 3297 independent reflections |
Radiation source: fine-focus sealed tube | 3037 reflections with I > 2σ(I) |
Detector resolution: 8.3 pixels mm-1 | Rint = 0.016 |
ω scans | θmax = 29.6°, θmin = 3.1° |
Absorption correction: multi-scan SADABS (Krause et al., 2015) | h = −9→9 |
Tmin = 0.688, Tmax = 0.746 | k = −24→24 |
15886 measured reflections | l = −14→14 |
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)] = 0.026 | Hydrogen site location: mixed |
wR(F2) = 0.068 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0323P)2 + 0.6413P] where P = (Fo2 + 2Fc2)/3 |
3297 reflections | (Δ/σ)max < 0.001 |
198 parameters | Δρmax = 0.50 e Å−3 |
9 restraints | Δρmin = −0.28 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.0000 | 0.0000 | 0.0000 | 0.01014 (6) | |
O1 | 0.23666 (12) | −0.04985 (5) | 0.12825 (7) | 0.01235 (15) | |
O2 | 0.55067 (13) | −0.02475 (5) | 0.24765 (8) | 0.01507 (16) | |
O3 | 0.80158 (13) | 0.13153 (5) | 0.30239 (8) | 0.01490 (16) | |
O4 | 0.92673 (12) | 0.06019 (5) | 0.15954 (8) | 0.01394 (16) | |
N1 | 0.23817 (14) | 0.08169 (5) | 0.00078 (9) | 0.01114 (17) | |
N2 | 0.57931 (15) | 0.17953 (6) | 0.03747 (9) | 0.01342 (18) | |
C1 | 0.41064 (16) | 0.06441 (6) | 0.08623 (10) | 0.01035 (19) | |
C2 | 0.58346 (16) | 0.11325 (6) | 0.10262 (10) | 0.01112 (19) | |
C3 | 0.40667 (18) | 0.19561 (7) | −0.04732 (11) | 0.0145 (2) | |
H3 | 0.4006 | 0.2419 | −0.0953 | 0.017* | |
C4 | 0.23572 (17) | 0.14636 (7) | −0.06702 (11) | 0.0138 (2) | |
H4 | 0.1163 | 0.1588 | −0.1292 | 0.017* | |
C5 | 0.40230 (17) | −0.00927 (6) | 0.16184 (10) | 0.01062 (19) | |
C6 | 0.78639 (17) | 0.09878 (6) | 0.19544 (10) | 0.0117 (2) | |
N3 | 0.09950 (16) | 0.07302 (6) | 0.49606 (10) | 0.0166 (2) | |
H3A | 0.019 (3) | 0.0943 (10) | 0.4241 (16) | 0.020* | |
H3B | 0.194 (3) | 0.1075 (10) | 0.5287 (16) | 0.020* | |
C7 | 0.20088 (19) | 0.00148 (7) | 0.46019 (12) | 0.0176 (2) | |
H7A | 0.2946 | −0.0197 | 0.5360 | 0.021* | |
H7B | 0.2858 | 0.0135 | 0.3947 | 0.021* | |
C8 | −0.03635 (19) | 0.05733 (7) | 0.59170 (11) | 0.0171 (2) | |
H8A | −0.1043 | 0.1056 | 0.6115 | 0.021* | |
H8B | 0.0498 | 0.0379 | 0.6717 | 0.021* | |
O1W | 0.22510 (15) | 0.31043 (6) | 0.23296 (9) | 0.0230 (2) | |
H1A | 0.285 (3) | 0.2712 (8) | 0.2771 (16) | 0.034 (5)* | |
H1B | 0.232 (3) | 0.3492 (8) | 0.2872 (16) | 0.044 (6)* | |
O2W | 0.35034 (15) | 0.19415 (6) | 0.59026 (10) | 0.0245 (2) | |
H2A | 0.471 (2) | 0.1953 (13) | 0.6459 (17) | 0.050 (6)* | |
H2B | 0.288 (3) | 0.2389 (8) | 0.591 (2) | 0.048 (6)* | |
O3W | 0.41755 (17) | 0.18273 (7) | 0.34547 (11) | 0.0301 (2) | |
H3C | 0.427 (3) | 0.1796 (11) | 0.4310 (9) | 0.036* | |
H3D | 0.5462 (19) | 0.1699 (13) | 0.3368 (19) | 0.048 (6)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.00694 (10) | 0.01250 (11) | 0.01014 (10) | −0.00044 (7) | −0.00061 (7) | 0.00097 (7) |
O1 | 0.0094 (3) | 0.0135 (4) | 0.0131 (4) | −0.0011 (3) | −0.0006 (3) | 0.0016 (3) |
O2 | 0.0121 (4) | 0.0182 (4) | 0.0132 (4) | −0.0005 (3) | −0.0021 (3) | 0.0033 (3) |
O3 | 0.0137 (4) | 0.0170 (4) | 0.0127 (4) | 0.0006 (3) | −0.0011 (3) | −0.0024 (3) |
O4 | 0.0099 (4) | 0.0181 (4) | 0.0133 (4) | 0.0007 (3) | 0.0008 (3) | −0.0005 (3) |
N1 | 0.0094 (4) | 0.0131 (4) | 0.0105 (4) | 0.0006 (3) | 0.0007 (3) | −0.0001 (3) |
N2 | 0.0119 (4) | 0.0136 (4) | 0.0141 (4) | −0.0005 (3) | 0.0007 (3) | 0.0008 (3) |
C1 | 0.0090 (5) | 0.0125 (5) | 0.0093 (4) | 0.0004 (4) | 0.0012 (3) | −0.0004 (4) |
C2 | 0.0092 (5) | 0.0134 (5) | 0.0104 (4) | 0.0003 (4) | 0.0010 (4) | −0.0006 (4) |
C3 | 0.0135 (5) | 0.0141 (5) | 0.0149 (5) | 0.0005 (4) | 0.0006 (4) | 0.0027 (4) |
C4 | 0.0113 (5) | 0.0155 (5) | 0.0135 (5) | 0.0009 (4) | −0.0008 (4) | 0.0021 (4) |
C5 | 0.0102 (5) | 0.0124 (5) | 0.0095 (4) | 0.0007 (4) | 0.0026 (4) | −0.0007 (4) |
C6 | 0.0097 (5) | 0.0127 (5) | 0.0120 (5) | −0.0019 (4) | −0.0004 (4) | 0.0018 (4) |
N3 | 0.0141 (5) | 0.0189 (5) | 0.0152 (5) | −0.0019 (4) | −0.0017 (4) | 0.0009 (4) |
C7 | 0.0120 (5) | 0.0260 (6) | 0.0147 (5) | 0.0029 (4) | 0.0026 (4) | −0.0001 (4) |
C8 | 0.0171 (5) | 0.0208 (6) | 0.0126 (5) | 0.0033 (4) | 0.0005 (4) | −0.0028 (4) |
O1W | 0.0223 (5) | 0.0210 (5) | 0.0252 (5) | −0.0014 (4) | 0.0032 (4) | −0.0049 (4) |
O2W | 0.0208 (5) | 0.0186 (4) | 0.0304 (5) | 0.0039 (4) | −0.0045 (4) | −0.0031 (4) |
O3W | 0.0228 (5) | 0.0381 (6) | 0.0288 (5) | 0.0095 (4) | 0.0035 (4) | −0.0044 (4) |
Co1—O1i | 2.0550 (8) | C3—H3 | 0.9500 |
Co1—O1 | 2.0550 (8) | C4—H4 | 0.9500 |
Co1—N1i | 2.1037 (9) | N3—C7 | 1.4910 (16) |
Co1—N1 | 2.1037 (9) | N3—C8 | 1.4945 (16) |
Co1—O4ii | 2.1251 (8) | N3—H3A | 0.924 (17) |
Co1—O4iii | 2.1251 (8) | N3—H3B | 0.884 (18) |
O1—C5 | 1.2846 (13) | C7—C8v | 1.5111 (17) |
O2—C5 | 1.2323 (14) | C7—H7A | 0.9900 |
O3—C6 | 1.2616 (13) | C7—H7B | 0.9900 |
O4—C6 | 1.2507 (13) | C8—C7v | 1.5111 (17) |
O4—Co1iv | 2.1251 (8) | C8—H8A | 0.9900 |
N1—C4 | 1.3348 (14) | C8—H8B | 0.9900 |
N1—C1 | 1.3443 (14) | O1W—H1A | 0.879 (9) |
N2—C3 | 1.3368 (15) | O1W—H1B | 0.883 (9) |
N2—C2 | 1.3428 (14) | O2W—H2A | 0.896 (9) |
C1—C2 | 1.3962 (15) | O2W—H2B | 0.879 (9) |
C1—C5 | 1.5195 (15) | O3W—H3C | 0.904 (9) |
C2—C6 | 1.5201 (15) | O3W—H3D | 0.889 (9) |
C3—C4 | 1.3907 (15) | ||
O1i—Co1—O1 | 180.0 | N1—C4—C3 | 120.50 (10) |
O1i—Co1—N1i | 79.54 (3) | N1—C4—H4 | 119.7 |
O1—Co1—N1i | 100.46 (3) | C3—C4—H4 | 119.7 |
O1i—Co1—N1 | 100.46 (3) | O2—C5—O1 | 126.29 (10) |
O1—Co1—N1 | 79.54 (3) | O2—C5—C1 | 118.52 (10) |
N1i—Co1—N1 | 180.0 | O1—C5—C1 | 115.20 (9) |
O1i—Co1—O4ii | 94.15 (3) | O4—C6—O3 | 125.37 (10) |
O1—Co1—O4ii | 85.85 (3) | O4—C6—C2 | 119.23 (9) |
N1i—Co1—O4ii | 93.45 (3) | O3—C6—C2 | 115.28 (10) |
N1—Co1—O4ii | 86.55 (3) | C7—N3—C8 | 111.71 (9) |
O1i—Co1—O4iii | 85.85 (3) | C7—N3—H3A | 109.5 (10) |
O1—Co1—O4iii | 94.15 (3) | C8—N3—H3A | 108.6 (10) |
N1i—Co1—O4iii | 86.55 (3) | C7—N3—H3B | 110.9 (11) |
N1—Co1—O4iii | 93.45 (3) | C8—N3—H3B | 108.3 (11) |
O4ii—Co1—O4iii | 180.00 (6) | H3A—N3—H3B | 107.7 (15) |
C5—O1—Co1 | 116.34 (7) | N3—C7—C8v | 109.84 (10) |
C6—O4—Co1iv | 142.62 (7) | N3—C7—H7A | 109.7 |
C4—N1—C1 | 118.67 (10) | C8v—C7—H7A | 109.7 |
C4—N1—Co1 | 129.15 (8) | N3—C7—H7B | 109.7 |
C1—N1—Co1 | 112.14 (7) | C8v—C7—H7B | 109.7 |
C3—N2—C2 | 117.58 (10) | H7A—C7—H7B | 108.2 |
N1—C1—C2 | 120.28 (10) | N3—C8—C7v | 110.15 (9) |
N1—C1—C5 | 116.12 (9) | N3—C8—H8A | 109.6 |
C2—C1—C5 | 123.60 (9) | C7v—C8—H8A | 109.6 |
N2—C2—C1 | 121.22 (10) | N3—C8—H8B | 109.6 |
N2—C2—C6 | 114.24 (9) | C7v—C8—H8B | 109.6 |
C1—C2—C6 | 124.52 (10) | H8A—C8—H8B | 108.1 |
N2—C3—C4 | 121.68 (10) | H1A—O1W—H1B | 106.1 (16) |
N2—C3—H3 | 119.2 | H2A—O2W—H2B | 109.2 (18) |
C4—C3—H3 | 119.2 | H3C—O3W—H3D | 101.4 (16) |
C4—N1—C1—C2 | −0.35 (15) | Co1—O1—C5—O2 | 171.09 (9) |
Co1—N1—C1—C2 | −178.34 (8) | Co1—O1—C5—C1 | −9.00 (11) |
C4—N1—C1—C5 | 179.04 (9) | N1—C1—C5—O2 | −174.87 (10) |
Co1—N1—C1—C5 | 1.05 (11) | C2—C1—C5—O2 | 4.50 (16) |
C3—N2—C2—C1 | −2.56 (16) | N1—C1—C5—O1 | 5.22 (14) |
C3—N2—C2—C6 | 179.09 (10) | C2—C1—C5—O1 | −175.42 (10) |
N1—C1—C2—N2 | 2.44 (16) | Co1iv—O4—C6—O3 | −175.61 (8) |
C5—C1—C2—N2 | −176.90 (10) | Co1iv—O4—C6—C2 | 0.11 (18) |
N1—C1—C2—C6 | −179.39 (10) | N2—C2—C6—O4 | −93.41 (12) |
C5—C1—C2—C6 | 1.27 (16) | C1—C2—C6—O4 | 88.31 (14) |
C2—N2—C3—C4 | 0.75 (17) | N2—C2—C6—O3 | 82.74 (12) |
C1—N1—C4—C3 | −1.45 (16) | C1—C2—C6—O3 | −95.55 (13) |
Co1—N1—C4—C3 | 176.16 (8) | C8—N3—C7—C8v | 57.47 (13) |
N2—C3—C4—N1 | 1.29 (18) | C7—N3—C8—C7v | −57.65 (13) |
Symmetry codes: (i) −x, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y, −z; (iv) x+1, y, z; (v) −x, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N3—H3A···O3ii | 0.924 (17) | 1.851 (17) | 2.7549 (13) | 165.3 (15) |
N3—H3B···O2W | 0.884 (18) | 1.868 (18) | 2.7405 (14) | 168.7 (16) |
O1W—H1A···O3W | 0.88 (1) | 1.85 (1) | 2.7174 (15) | 171 (2) |
O1W—H1B···O1vi | 0.88 (1) | 1.97 (1) | 2.8305 (12) | 166 (2) |
O2W—H2A···O1Wvii | 0.90 (1) | 1.74 (1) | 2.6310 (14) | 170 (2) |
O2W—H2B···N2viii | 0.88 (1) | 1.97 (1) | 2.8099 (13) | 158 (2) |
O3W—H3C···O2W | 0.90 (1) | 1.87 (1) | 2.7321 (15) | 158 (2) |
O3W—H3D···O3 | 0.89 (1) | 1.89 (1) | 2.7758 (13) | 172 (2) |
Symmetry codes: (ii) x−1, y, z; (vi) −x+1/2, y+1/2, −z+1/2; (vii) x+1/2, −y+1/2, z+1/2; (viii) x−1/2, −y+1/2, z+1/2. |