The structure of 1,2-bis(4-pyridyl)ethylenium tris(malonato-κ2O,O′)chromate(III) octahydrate, (Hbpe)3[Cr(mal)3]·8H2O, where mal is the malonate dianion (C3HO42−) and bpe is 1,2-bis(4-pyridyl)ethylene (C12H12N2), is presented. The crystal structure is made up of [Cr(mal)3]3− anions, Hbpe+ cations and water molecules of crystallization. The anions are connected through hydrogen bonding involving malonate O atoms and uncoordinated water molecules in distinct layers, with the cations stacked in separate layers. One of the Hbpe cations is located on a center of inversion, another one on a twofold rotation axis.
Supporting information
CCDC reference: 242038
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.004 Å
- Disorder in solvent or counterion
- R factor = 0.067
- wR factor = 0.179
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT213_ALERT_2_B Atom C7D has ADP max/min Ratio ............. 4.20 prolat
PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.52 Ratio
PLAT250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.37
PLAT417_ALERT_2_B Short Inter D-H..H-D H2S2 .. H3S1 .. 2.07 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H5S2 .. H7S2 .. 1.92 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H6S2 .. H7S1 .. 2.06 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H6S2 .. H7S2 .. 1.69 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H7S1 .. H8S1 .. 1.76 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H7S1 .. H8S5 .. 1.79 Ang.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.43
PLAT213_ALERT_2_C Atom C4D has ADP max/min Ratio ............. 3.70 prolat
PLAT213_ALERT_2_C Atom C8D has ADP max/min Ratio ............. 3.20 prolat
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.11 Ratio
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C4D
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C7D
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C6D
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.40
PLAT301_ALERT_3_C Main Residue Disorder ......................... 2.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 10.00 Perc.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C3D - C4D ... 1.39 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C7D - C8D ... 1.39 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C7D - C8D_b ... 1.39 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 22
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 10
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 11
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 13
H2 O
0 ALERT level A = In general: serious problem
9 ALERT level B = Potentially serious problem
18 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
19 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
5 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
1,2-bis(4-pyridyl)ethylenium tris(malonato-
κ2O,
O')
chromate(III)-water (1/8)
top
Crystal data top
(C12H12N2)3[Cr(C3HO4)3]·8H2O | F(000) = 4408 |
Mr = 1051.95 | Dx = 1.451 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 9927 reflections |
a = 21.319 (4) Å | θ = 2.2–26.0° |
b = 11.997 (2) Å | µ = 0.32 mm−1 |
c = 38.300 (6) Å | T = 100 K |
β = 100.632 (3)° | Prism, purple |
V = 9628 (3) Å3 | 0.50 × 0.19 × 0.12 mm |
Z = 8 | |
Data collection top
Bruker APEX diffractometer | 9450 independent reflections |
Radiation source: fine-focus sealed tube | 8293 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
ω scans | θmax = 26.0°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | h = −26→26 |
Tmin = 0.855, Tmax = 0.962 | k = −9→14 |
26496 measured reflections | l = −47→47 |
Refinement top
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)] = 0.067 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.179 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.084P)2 + 4P] where P = (Fo2 + 2Fc2)/3 |
9450 reflections | (Δ/σ)max = 0.002 |
681 parameters | Δρmax = 1.33 e Å−3 |
1 restraint | Δρmin = −0.55 e Å−3 |
Special details top
Experimental. The first 50 frames were repeated at the end of data collection and yielded a
total of 313 peaks showing a variation of -0.21% during the data collection. |
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. The positions of H atoms bonded to carbons and N atoms were determined by
geometry and refined by a riding model. H atoms bound to water O atoms were
located on a difference map and kept fixed during refinement. The isotropic
displacement parameters of the H atoms were set to 1.2 times the isotropic
equivalent displacement parameter of the bonded atom. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cr1 | 0.12790 (2) | 0.33273 (4) | 0.123825 (12) | 0.01668 (14) | |
O1 | 0.14709 (10) | 0.33240 (17) | 0.17627 (5) | 0.0210 (4) | |
C2 | 0.16217 (13) | 0.2471 (3) | 0.19575 (8) | 0.0204 (6) | |
C3 | 0.17202 (15) | 0.1343 (3) | 0.17926 (8) | 0.0234 (6) | |
H31 | 0.1996 | 0.0890 | 0.1975 | 0.028* | |
H32 | 0.1300 | 0.0966 | 0.1739 | 0.028* | |
C4 | 0.20083 (14) | 0.1312 (2) | 0.14571 (8) | 0.0209 (6) | |
O5 | 0.19192 (9) | 0.21501 (17) | 0.12421 (6) | 0.0212 (4) | |
O6 | 0.16839 (10) | 0.25136 (18) | 0.22876 (6) | 0.0244 (5) | |
O7 | 0.23071 (11) | 0.04741 (19) | 0.13980 (6) | 0.0293 (5) | |
O8 | 0.06180 (9) | 0.22004 (17) | 0.12552 (5) | 0.0194 (4) | |
C9 | 0.05332 (13) | 0.1316 (3) | 0.10637 (8) | 0.0203 (6) | |
C10 | 0.08060 (15) | 0.1280 (3) | 0.07231 (8) | 0.0262 (7) | |
H101 | 0.0525 | 0.0797 | 0.0552 | 0.031* | |
H102 | 0.1228 | 0.0911 | 0.0778 | 0.031* | |
C11 | 0.08914 (15) | 0.2378 (3) | 0.05359 (8) | 0.0261 (7) | |
O12 | 0.10756 (10) | 0.32463 (18) | 0.07182 (5) | 0.0239 (5) | |
O13 | 0.02469 (10) | 0.04890 (18) | 0.11467 (6) | 0.0256 (5) | |
O14 | 0.07961 (12) | 0.2376 (2) | 0.02069 (6) | 0.0380 (6) | |
O15 | 0.06468 (9) | 0.45287 (17) | 0.12312 (6) | 0.0208 (4) | |
C16 | 0.07565 (14) | 0.5535 (3) | 0.13407 (8) | 0.0218 (6) | |
C17 | 0.14374 (15) | 0.5827 (3) | 0.15199 (9) | 0.0253 (7) | |
H171 | 0.1468 | 0.6644 | 0.1554 | 0.030* | |
H172 | 0.1526 | 0.5475 | 0.1758 | 0.030* | |
C18 | 0.19483 (14) | 0.5461 (3) | 0.13145 (8) | 0.0215 (6) | |
O19 | 0.19342 (10) | 0.44486 (17) | 0.12061 (6) | 0.0219 (4) | |
O20 | 0.03365 (11) | 0.62526 (19) | 0.13226 (6) | 0.0293 (5) | |
O21 | 0.23663 (10) | 0.61338 (19) | 0.12724 (6) | 0.0287 (5) | |
N1A | 0.37829 (12) | 0.4560 (2) | 0.17383 (6) | 0.0186 (5) | |
H1A | 0.3784 | 0.5290 | 0.1715 | 0.022* | |
C2A | 0.42445 (14) | 0.3934 (2) | 0.16422 (7) | 0.0181 (6) | |
H2A | 0.4577 | 0.4298 | 0.1552 | 0.022* | |
C3A | 0.42604 (13) | 0.2786 (2) | 0.16679 (7) | 0.0166 (6) | |
H3A | 0.4598 | 0.2375 | 0.1598 | 0.020* | |
C4A | 0.37726 (13) | 0.2237 (2) | 0.17984 (7) | 0.0156 (6) | |
C5A | 0.33056 (14) | 0.2901 (2) | 0.19078 (8) | 0.0190 (6) | |
H5A | 0.2976 | 0.2564 | 0.2008 | 0.023* | |
C6A | 0.33217 (14) | 0.4046 (2) | 0.18704 (8) | 0.0205 (6) | |
H6A | 0.2994 | 0.4482 | 0.1941 | 0.025* | |
C7A | 0.37281 (13) | 0.1018 (2) | 0.18161 (7) | 0.0165 (6) | |
H7A | 0.3424 | 0.0715 | 0.1942 | 0.020* | |
C8A | 0.40806 (13) | 0.0305 (2) | 0.16692 (7) | 0.0157 (5) | |
H8A | 0.4401 | 0.0599 | 0.1552 | 0.019* | |
C9A | 0.40047 (13) | −0.0908 (2) | 0.16767 (7) | 0.0142 (5) | |
C10A | 0.44587 (13) | −0.1603 (2) | 0.15684 (7) | 0.0158 (6) | |
H10A | 0.4818 | −0.1289 | 0.1490 | 0.019* | |
C11A | 0.43865 (13) | −0.2745 (2) | 0.15748 (7) | 0.0160 (6) | |
H11A | 0.4696 | −0.3216 | 0.1502 | 0.019* | |
N12A | 0.38797 (11) | −0.31924 (19) | 0.16843 (6) | 0.0168 (5) | |
C13A | 0.34290 (14) | −0.2553 (2) | 0.17868 (8) | 0.0191 (6) | |
H13A | 0.3073 | −0.2893 | 0.1861 | 0.023* | |
C14A | 0.34781 (14) | −0.1410 (2) | 0.17855 (7) | 0.0175 (6) | |
H14A | 0.3157 | −0.0963 | 0.1858 | 0.021* | |
N1B | 0.36790 (13) | 0.1602 (2) | 0.07891 (7) | 0.0212 (5) | |
H1B | 0.3712 | 0.0872 | 0.0779 | 0.025* | |
C2B | 0.31709 (14) | 0.2051 (2) | 0.08971 (7) | 0.0184 (6) | |
H2B | 0.2858 | 0.1579 | 0.0967 | 0.022* | |
C3B | 0.30994 (14) | 0.3186 (2) | 0.09066 (7) | 0.0173 (6) | |
H3B | 0.2738 | 0.3499 | 0.0983 | 0.021* | |
C4B | 0.35593 (14) | 0.3882 (2) | 0.08040 (7) | 0.0182 (6) | |
C5B | 0.40913 (15) | 0.3384 (3) | 0.07023 (9) | 0.0242 (7) | |
H5B | 0.4419 | 0.3834 | 0.0638 | 0.029* | |
C6B | 0.41386 (16) | 0.2242 (3) | 0.06953 (9) | 0.0266 (7) | |
H6B | 0.4497 | 0.1903 | 0.0624 | 0.032* | |
C7B | 0.34761 (14) | 0.5092 (2) | 0.08130 (7) | 0.0179 (6) | |
H7B | 0.3157 | 0.5378 | 0.0932 | 0.021* | |
C8B | 0.38227 (13) | 0.5819 (2) | 0.06638 (7) | 0.0181 (6) | |
H8B | 0.4132 | 0.5524 | 0.0539 | 0.022* | |
C9B | 0.37625 (14) | 0.7033 (2) | 0.06773 (7) | 0.0182 (6) | |
C10B | 0.32872 (14) | 0.7574 (2) | 0.08221 (7) | 0.0171 (6) | |
H10B | 0.2968 | 0.7157 | 0.0907 | 0.020* | |
C11B | 0.32907 (14) | 0.8727 (2) | 0.08390 (7) | 0.0187 (6) | |
H11B | 0.2967 | 0.9088 | 0.0938 | 0.022* | |
N12B | 0.37304 (12) | 0.9363 (2) | 0.07224 (7) | 0.0222 (5) | |
C13B | 0.41734 (16) | 0.8850 (3) | 0.05773 (9) | 0.0275 (7) | |
H13B | 0.4482 | 0.9292 | 0.0491 | 0.033* | |
C14B | 0.42049 (15) | 0.7704 (3) | 0.05456 (8) | 0.0240 (7) | |
H14B | 0.4524 | 0.7374 | 0.0435 | 0.029* | |
N1C | 0.24826 (13) | 0.6392 (2) | 0.00148 (7) | 0.0224 (5) | |
H1C | 0.2502 | 0.7124 | 0.0006 | 0.027* | 0.50 |
C2C | 0.20590 (16) | 0.5896 (3) | 0.01824 (9) | 0.0277 (7) | |
H2C | 0.1787 | 0.6347 | 0.0294 | 0.033* | |
C3C | 0.20047 (17) | 0.4754 (3) | 0.01984 (9) | 0.0307 (7) | |
H3C | 0.1702 | 0.4426 | 0.0321 | 0.037* | |
C4C | 0.23931 (17) | 0.4093 (3) | 0.00360 (8) | 0.0280 (7) | |
C5C | 0.28420 (18) | 0.4617 (3) | −0.01346 (9) | 0.0320 (8) | |
H5C | 0.3121 | 0.4182 | −0.0246 | 0.038* | |
C6C | 0.28775 (16) | 0.5770 (3) | −0.01395 (8) | 0.0265 (7) | |
H6C | 0.3184 | 0.6123 | −0.0253 | 0.032* | |
C7C | 0.23088 (17) | 0.2872 (3) | 0.00536 (9) | 0.0292 (7) | |
H7C | 0.1956 | 0.2603 | 0.0148 | 0.035* | |
N1D | 0.5000 | 0.3919 (3) | 0.2500 | 0.0192 (7) | |
H1D | 0.5000 | 0.3186 | 0.2500 | 0.023* | |
C2D | 0.54913 (16) | 0.4459 (3) | 0.24098 (8) | 0.0274 (7) | |
H2D | 0.5835 | 0.4051 | 0.2345 | 0.033* | |
C3D | 0.5504 (2) | 0.5605 (3) | 0.24095 (9) | 0.0441 (11) | |
H3D | 0.5858 | 0.5987 | 0.2347 | 0.053* | |
C4D | 0.5000 | 0.6203 (4) | 0.2500 | 0.0500 (18) | |
C5D | 0.5203 (3) | 0.7415 (6) | 0.24589 (15) | 0.0186 (12) | 0.50 |
H5D | 0.5582 | 0.7612 | 0.2377 | 0.022* | 0.50 |
C6D | 0.4805 (3) | 0.8160 (5) | 0.25476 (14) | 0.0158 (11) | 0.50 |
H6D | 0.4429 | 0.7963 | 0.2633 | 0.019* | 0.50 |
C7D | 0.5000 | 0.9375 (4) | 0.2500 | 0.056 (2) | |
C8D | 0.4584 (2) | 0.9971 (3) | 0.26682 (10) | 0.0492 (12) | |
H8D | 0.4292 | 0.9592 | 0.2786 | 0.059* | |
C9D | 0.46006 (16) | 1.1119 (3) | 0.26621 (8) | 0.0279 (7) | |
H9D | 0.4315 | 1.1520 | 0.2779 | 0.034* | |
N10D | 0.5000 | 1.1690 (3) | 0.2500 | 0.0222 (8) | |
O1S | 0.22933 (11) | 0.4412 (2) | 0.26154 (6) | 0.0316 (5) | |
H1S1 | 0.2067 | 0.3911 | 0.2469 | 0.038* | |
H1S2 | 0.2228 | 0.5019 | 0.2481 | 0.038* | |
O2S | 0.25834 (12) | 0.1339 (2) | 0.27427 (6) | 0.0314 (5) | |
H2S1 | 0.2288 | 0.1706 | 0.2582 | 0.038* | |
H2S2 | 0.2863 | 0.1915 | 0.2799 | 0.038* | |
O3S | 0.33754 (13) | 0.3191 (2) | 0.28892 (7) | 0.0389 (6) | |
H3S1 | 0.3044 | 0.3610 | 0.2835 | 0.047* | |
H3S2 | 0.3587 | 0.3355 | 0.3096 | 0.047* | |
O4S | 0.06961 (13) | −0.1514 (2) | 0.15227 (8) | 0.0434 (7) | |
H4S1 | 0.0914 | −0.1482 | 0.1333 | 0.052* | |
H4S2 | 0.0549 | −0.2212 | 0.1442 | 0.052* | |
O5S | 0.19487 (14) | −0.1653 (2) | 0.11021 (9) | 0.0527 (8) | |
H5S1 | 0.2104 | −0.2294 | 0.1206 | 0.063* | |
H5S2 | 0.1693 | −0.1897 | 0.0901 | 0.063* | |
O6S | −0.00988 (15) | 0.0990 (3) | −0.01621 (8) | 0.0577 (8) | |
H6S1 | 0.0180 | 0.1481 | −0.0050 | 0.069* | |
H6S2 | −0.0375 | 0.1424 | −0.0303 | 0.069* | |
O7S | 0.10686 (17) | −0.2240 (3) | 0.05337 (10) | 0.0717 (10) | |
H7S1 | 0.0834 | −0.2883 | 0.0480 | 0.086* | |
H7S2 | 0.0811 | −0.1958 | 0.0678 | 0.086* | |
O8S | −0.0391 (7) | 0.4319 (6) | −0.0497 (2) | 0.028 (3) | 0.325 (17) |
H8S1 | −0.0819 | 0.4330 | −0.0554 | 0.033* | 0.325 (17) |
H8S2 | −0.0354 | 0.4599 | −0.0280 | 0.033* | 0.325 (17) |
O8S' | 0.0371 (3) | 0.4294 (5) | −0.00765 (14) | 0.0165 (13) | 0.338 (3) |
H8S3 | 0.0407 | 0.4719 | 0.0115 | 0.020* | 0.338 (3) |
H8S4 | 0.0398 | 0.3624 | 0.0014 | 0.020* | 0.338 (3) |
O8S" | −0.0791 (6) | 0.4325 (5) | −0.04916 (16) | 0.021 (3) | 0.337 (17) |
H8S5 | −0.0391 | 0.4146 | −0.0371 | 0.025* | 0.337 (17) |
H8S6 | −0.0698 | 0.4960 | −0.0584 | 0.025* | 0.337 (17) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cr1 | 0.0141 (2) | 0.0118 (2) | 0.0257 (3) | −0.00024 (17) | 0.00763 (18) | 0.00190 (18) |
O1 | 0.0234 (11) | 0.0146 (10) | 0.0258 (10) | 0.0003 (8) | 0.0065 (8) | 0.0019 (8) |
C2 | 0.0145 (13) | 0.0186 (15) | 0.0289 (15) | −0.0020 (11) | 0.0061 (11) | −0.0009 (12) |
C3 | 0.0240 (15) | 0.0157 (15) | 0.0306 (16) | −0.0017 (12) | 0.0053 (12) | 0.0014 (12) |
C4 | 0.0171 (14) | 0.0149 (15) | 0.0300 (15) | −0.0013 (12) | 0.0026 (12) | −0.0014 (12) |
O5 | 0.0169 (10) | 0.0172 (11) | 0.0311 (11) | 0.0008 (8) | 0.0087 (8) | 0.0015 (9) |
O6 | 0.0259 (11) | 0.0229 (11) | 0.0251 (11) | −0.0001 (9) | 0.0063 (9) | 0.0005 (9) |
O7 | 0.0295 (12) | 0.0191 (12) | 0.0398 (13) | 0.0059 (10) | 0.0076 (10) | 0.0001 (10) |
O8 | 0.0162 (10) | 0.0151 (10) | 0.0289 (11) | −0.0011 (8) | 0.0093 (8) | −0.0006 (8) |
C9 | 0.0141 (13) | 0.0195 (15) | 0.0280 (15) | 0.0002 (12) | 0.0054 (11) | 0.0007 (12) |
C10 | 0.0241 (16) | 0.0268 (17) | 0.0289 (16) | −0.0014 (13) | 0.0077 (13) | −0.0044 (13) |
C11 | 0.0197 (15) | 0.0327 (19) | 0.0276 (16) | −0.0018 (13) | 0.0091 (12) | −0.0004 (14) |
O12 | 0.0249 (11) | 0.0243 (12) | 0.0241 (10) | −0.0018 (9) | 0.0089 (9) | 0.0035 (9) |
O13 | 0.0259 (11) | 0.0168 (11) | 0.0353 (12) | −0.0031 (9) | 0.0088 (9) | −0.0014 (9) |
O14 | 0.0405 (14) | 0.0504 (17) | 0.0242 (12) | −0.0128 (12) | 0.0090 (10) | −0.0002 (11) |
O15 | 0.0172 (10) | 0.0130 (10) | 0.0331 (11) | 0.0000 (8) | 0.0074 (8) | 0.0008 (8) |
C16 | 0.0195 (14) | 0.0168 (15) | 0.0324 (16) | 0.0006 (12) | 0.0136 (12) | 0.0047 (12) |
C17 | 0.0244 (16) | 0.0195 (16) | 0.0342 (17) | −0.0043 (13) | 0.0115 (13) | −0.0036 (13) |
C18 | 0.0167 (14) | 0.0197 (16) | 0.0290 (15) | −0.0010 (12) | 0.0067 (12) | 0.0029 (12) |
O19 | 0.0170 (10) | 0.0147 (10) | 0.0360 (12) | −0.0007 (8) | 0.0101 (9) | 0.0014 (9) |
O20 | 0.0244 (12) | 0.0183 (11) | 0.0487 (14) | 0.0043 (9) | 0.0160 (10) | 0.0012 (10) |
O21 | 0.0236 (11) | 0.0200 (12) | 0.0466 (14) | −0.0066 (9) | 0.0170 (10) | −0.0046 (10) |
N1A | 0.0234 (13) | 0.0071 (11) | 0.0254 (12) | 0.0007 (10) | 0.0045 (10) | −0.0012 (9) |
C2A | 0.0202 (14) | 0.0125 (14) | 0.0207 (14) | −0.0037 (11) | 0.0018 (11) | 0.0001 (11) |
C3A | 0.0167 (13) | 0.0120 (14) | 0.0208 (13) | 0.0019 (11) | 0.0024 (11) | −0.0008 (11) |
C4A | 0.0180 (14) | 0.0114 (14) | 0.0159 (12) | 0.0007 (11) | −0.0004 (10) | 0.0009 (10) |
C5A | 0.0219 (15) | 0.0117 (14) | 0.0243 (14) | −0.0004 (11) | 0.0065 (11) | 0.0004 (11) |
C6A | 0.0225 (15) | 0.0133 (14) | 0.0269 (15) | 0.0034 (12) | 0.0074 (12) | −0.0015 (11) |
C7A | 0.0176 (13) | 0.0104 (13) | 0.0208 (13) | −0.0016 (11) | 0.0016 (11) | 0.0018 (11) |
C8A | 0.0155 (13) | 0.0107 (13) | 0.0203 (13) | −0.0025 (11) | 0.0020 (10) | 0.0018 (10) |
C9A | 0.0148 (13) | 0.0120 (13) | 0.0156 (12) | 0.0004 (10) | 0.0023 (10) | 0.0010 (10) |
C10A | 0.0153 (13) | 0.0141 (14) | 0.0180 (13) | −0.0024 (11) | 0.0033 (10) | 0.0012 (10) |
C11A | 0.0179 (13) | 0.0128 (14) | 0.0179 (13) | 0.0018 (11) | 0.0046 (10) | −0.0012 (10) |
N12A | 0.0196 (12) | 0.0109 (11) | 0.0204 (11) | −0.0005 (9) | 0.0049 (9) | 0.0005 (9) |
C13A | 0.0190 (14) | 0.0156 (14) | 0.0256 (14) | −0.0014 (11) | 0.0112 (11) | −0.0006 (11) |
C14A | 0.0188 (14) | 0.0120 (14) | 0.0233 (14) | 0.0001 (11) | 0.0077 (11) | −0.0004 (11) |
N1B | 0.0294 (14) | 0.0095 (12) | 0.0263 (13) | −0.0010 (10) | 0.0094 (11) | −0.0011 (10) |
C2B | 0.0212 (14) | 0.0163 (14) | 0.0178 (13) | −0.0036 (12) | 0.0038 (11) | −0.0013 (11) |
C3B | 0.0191 (14) | 0.0165 (14) | 0.0160 (13) | −0.0004 (11) | 0.0025 (10) | −0.0013 (11) |
C4B | 0.0215 (14) | 0.0171 (15) | 0.0159 (13) | −0.0018 (12) | 0.0029 (11) | −0.0022 (11) |
C5B | 0.0270 (16) | 0.0134 (15) | 0.0356 (17) | −0.0033 (12) | 0.0143 (13) | −0.0013 (12) |
C6B | 0.0291 (17) | 0.0163 (15) | 0.0395 (18) | 0.0010 (13) | 0.0195 (14) | −0.0032 (13) |
C7B | 0.0184 (14) | 0.0143 (14) | 0.0212 (13) | 0.0020 (11) | 0.0046 (11) | −0.0010 (11) |
C8B | 0.0165 (13) | 0.0141 (14) | 0.0239 (14) | 0.0025 (11) | 0.0044 (11) | −0.0016 (11) |
C9B | 0.0226 (15) | 0.0115 (14) | 0.0198 (13) | −0.0018 (11) | 0.0019 (11) | −0.0013 (11) |
C10B | 0.0216 (14) | 0.0117 (13) | 0.0168 (13) | −0.0013 (11) | 0.0009 (11) | −0.0001 (10) |
C11B | 0.0216 (14) | 0.0138 (14) | 0.0205 (14) | 0.0038 (12) | 0.0031 (11) | −0.0020 (11) |
N12B | 0.0261 (13) | 0.0117 (12) | 0.0290 (13) | −0.0022 (10) | 0.0054 (11) | −0.0004 (10) |
C13B | 0.0305 (17) | 0.0161 (16) | 0.0394 (18) | −0.0024 (13) | 0.0157 (14) | 0.0014 (13) |
C14B | 0.0255 (16) | 0.0147 (15) | 0.0340 (16) | 0.0001 (12) | 0.0114 (13) | −0.0017 (12) |
N1C | 0.0322 (14) | 0.0080 (11) | 0.0242 (12) | −0.0008 (10) | −0.0024 (10) | 0.0014 (10) |
C2C | 0.0281 (17) | 0.0173 (16) | 0.0362 (17) | −0.0011 (13) | 0.0019 (13) | 0.0032 (13) |
C3C | 0.0359 (18) | 0.0188 (16) | 0.0359 (18) | −0.0071 (14) | 0.0025 (14) | 0.0052 (13) |
C4C | 0.0403 (19) | 0.0150 (16) | 0.0241 (15) | −0.0044 (14) | −0.0060 (13) | 0.0039 (12) |
C5C | 0.050 (2) | 0.0192 (17) | 0.0255 (16) | 0.0113 (15) | 0.0036 (15) | −0.0046 (13) |
C6C | 0.0384 (18) | 0.0155 (15) | 0.0258 (15) | −0.0006 (14) | 0.0064 (13) | 0.0024 (12) |
C7C | 0.0319 (17) | 0.0254 (18) | 0.0297 (16) | −0.0034 (14) | 0.0038 (13) | 0.0025 (13) |
N1D | 0.0284 (19) | 0.0052 (15) | 0.0226 (17) | 0.000 | 0.0008 (14) | 0.000 |
C2D | 0.0281 (17) | 0.0285 (18) | 0.0255 (15) | −0.0056 (14) | 0.0049 (13) | −0.0006 (13) |
C3D | 0.065 (3) | 0.031 (2) | 0.0303 (18) | −0.032 (2) | −0.0060 (17) | 0.0091 (15) |
C4D | 0.102 (5) | 0.009 (2) | 0.025 (2) | 0.000 | −0.025 (3) | 0.000 |
C5D | 0.018 (3) | 0.013 (3) | 0.025 (3) | 0.002 (2) | 0.005 (2) | 0.003 (2) |
C6D | 0.022 (3) | 0.007 (3) | 0.019 (3) | −0.003 (2) | 0.005 (2) | −0.001 (2) |
C7D | 0.106 (5) | 0.008 (2) | 0.036 (3) | 0.000 | −0.037 (3) | 0.000 |
C8D | 0.074 (3) | 0.027 (2) | 0.0342 (19) | −0.031 (2) | −0.0228 (19) | 0.0147 (16) |
C9D | 0.0296 (17) | 0.0225 (17) | 0.0284 (16) | −0.0033 (14) | −0.0034 (13) | 0.0039 (13) |
N10D | 0.030 (2) | 0.0080 (17) | 0.0262 (18) | 0.000 | −0.0018 (15) | 0.000 |
O1S | 0.0392 (13) | 0.0251 (12) | 0.0301 (12) | −0.0085 (10) | 0.0058 (10) | 0.0030 (10) |
O2S | 0.0358 (13) | 0.0243 (12) | 0.0329 (12) | 0.0063 (10) | 0.0028 (10) | −0.0013 (10) |
O3S | 0.0387 (14) | 0.0327 (14) | 0.0452 (15) | 0.0008 (11) | 0.0080 (11) | 0.0039 (11) |
O4S | 0.0355 (14) | 0.0308 (14) | 0.0641 (18) | 0.0004 (11) | 0.0097 (13) | 0.0010 (13) |
O5S | 0.0463 (17) | 0.0338 (16) | 0.078 (2) | 0.0045 (13) | 0.0124 (15) | 0.0050 (14) |
O6S | 0.0590 (19) | 0.059 (2) | 0.0483 (17) | −0.0164 (16) | −0.0087 (14) | 0.0011 (15) |
O7S | 0.064 (2) | 0.067 (2) | 0.088 (3) | −0.0015 (19) | 0.0240 (19) | 0.008 (2) |
O8S | 0.028 (8) | 0.017 (4) | 0.034 (4) | −0.005 (3) | −0.001 (3) | 0.010 (3) |
O8S' | 0.027 (3) | 0.010 (3) | 0.011 (3) | 0.006 (2) | 0.002 (2) | 0.004 (2) |
O8S" | 0.026 (8) | 0.012 (3) | 0.024 (3) | −0.005 (3) | 0.001 (3) | 0.006 (2) |
Geometric parameters (Å, º) top
Cr1—O19 | 1.959 (2) | C7B—C8B | 1.338 (4) |
Cr1—O12 | 1.961 (2) | C7B—H7B | 0.9500 |
Cr1—O5 | 1.962 (2) | C8B—C9B | 1.464 (4) |
Cr1—O8 | 1.963 (2) | C8B—H8B | 0.9500 |
Cr1—O15 | 1.970 (2) | C9B—C10B | 1.402 (4) |
Cr1—O1 | 1.974 (2) | C9B—C14B | 1.403 (4) |
O1—C2 | 1.273 (4) | C10B—C11B | 1.385 (4) |
C2—O6 | 1.247 (4) | C10B—H10B | 0.9500 |
C2—C3 | 1.524 (4) | C11B—N12B | 1.347 (4) |
C3—C4 | 1.524 (4) | C11B—H11B | 0.9500 |
C3—H31 | 0.9900 | N12B—C13B | 1.332 (4) |
C3—H32 | 0.9900 | C13B—C14B | 1.383 (4) |
C4—O7 | 1.233 (4) | C13B—H13B | 0.9500 |
C4—O5 | 1.291 (4) | C14B—H14B | 0.9500 |
O8—C9 | 1.283 (4) | N1C—C2C | 1.340 (4) |
C9—O13 | 1.237 (4) | N1C—C6C | 1.341 (4) |
C9—C10 | 1.524 (4) | N1C—H1C | 0.8800 |
C10—C11 | 1.526 (5) | C2C—C3C | 1.377 (5) |
C10—H101 | 0.9900 | C2C—H2C | 0.9500 |
C10—H102 | 0.9900 | C3C—C4C | 1.376 (5) |
C11—O14 | 1.239 (4) | C3C—H3C | 0.9500 |
C11—O12 | 1.275 (4) | C4C—C5C | 1.403 (5) |
O15—C16 | 1.285 (4) | C4C—C7C | 1.479 (5) |
C16—O20 | 1.235 (4) | C5C—C6C | 1.386 (5) |
C16—C17 | 1.527 (4) | C5C—H5C | 0.9500 |
C17—C18 | 1.521 (4) | C6C—H6C | 0.9500 |
C17—H171 | 0.9900 | C7C—C7Ci | 1.324 (7) |
C17—H172 | 0.9900 | C7C—H7C | 0.9500 |
C18—O21 | 1.235 (4) | N1D—C2D | 1.330 (4) |
C18—O19 | 1.282 (4) | N1D—C2Dii | 1.330 (4) |
N1A—C6A | 1.337 (4) | N1D—H1D | 0.8800 |
N1A—C2A | 1.343 (4) | C2D—C3D | 1.375 (5) |
N1A—H1A | 0.8800 | C2D—H2D | 0.9500 |
C2A—C3A | 1.380 (4) | C3D—C4D | 1.388 (5) |
C2A—H2A | 0.9500 | C3D—H3D | 0.9500 |
C3A—C4A | 1.399 (4) | C4D—C3Dii | 1.388 (5) |
C3A—H3A | 0.9500 | C4D—C5D | 1.533 (8) |
C4A—C5A | 1.398 (4) | C5D—C6D | 1.319 (8) |
C4A—C7A | 1.468 (4) | C5D—H5D | 0.9500 |
C5A—C6A | 1.383 (4) | C6D—C7D | 1.535 (7) |
C5A—H5A | 0.9500 | C6D—H6D | 0.9500 |
C6A—H6A | 0.9500 | C7D—C8Dii | 1.387 (6) |
C7A—C8A | 1.330 (4) | C7D—C8D | 1.387 (6) |
C7A—H7A | 0.9500 | C8D—C9D | 1.378 (5) |
C8A—C9A | 1.464 (4) | C8D—H8D | 0.9500 |
C8A—H8A | 0.9500 | C9D—N10D | 1.333 (4) |
C9A—C10A | 1.398 (4) | C9D—H9D | 0.9500 |
C9A—C14A | 1.404 (4) | N10D—C9Dii | 1.333 (4) |
C10A—C11A | 1.379 (4) | O1S—H1S1 | 0.8983 |
C10A—H10A | 0.9500 | O1S—H1S2 | 0.8874 |
C11A—N12A | 1.341 (4) | O2S—H2S1 | 0.9094 |
C11A—H11A | 0.9500 | O2S—H2S2 | 0.9118 |
N12A—C13A | 1.343 (4) | O3S—H3S1 | 0.8601 |
C13A—C14A | 1.375 (4) | O3S—H3S2 | 0.8598 |
C13A—H13A | 0.9500 | O4S—H4S1 | 0.9323 |
C14A—H14A | 0.9500 | O4S—H4S2 | 0.9267 |
N1B—C2B | 1.342 (4) | O5S—H5S1 | 0.9009 |
N1B—C6B | 1.345 (4) | O5S—H5S2 | 0.9050 |
N1B—H1B | 0.8800 | O6S—H6S1 | 0.8891 |
C2B—C3B | 1.372 (4) | O6S—H6S2 | 0.8917 |
C2B—H2B | 0.9500 | O7S—H7S1 | 0.9216 |
C3B—C4B | 1.398 (4) | O7S—H7S2 | 0.9137 |
C3B—H3B | 0.9500 | O8S—H8S1 | 0.8987 |
C4B—C5B | 1.400 (4) | O8S—H8S2 | 0.8885 |
C4B—C7B | 1.463 (4) | O8S'—H8S3 | 0.8844 |
C5B—C6B | 1.375 (4) | O8S'—H8S4 | 0.8730 |
C5B—H5B | 0.9500 | O8S"—H8S5 | 0.9164 |
C6B—H6B | 0.9500 | O8S"—H8S6 | 0.8784 |
| | | |
O19—Cr1—O12 | 89.82 (9) | C2B—N1B—H1B | 119.2 |
O19—Cr1—O5 | 89.52 (9) | C6B—N1B—H1B | 119.2 |
O12—Cr1—O5 | 89.72 (9) | N1B—C2B—C3B | 120.5 (3) |
O19—Cr1—O8 | 178.32 (9) | N1B—C2B—H2B | 119.8 |
O12—Cr1—O8 | 88.50 (9) | C3B—C2B—H2B | 119.8 |
O5—Cr1—O8 | 90.38 (9) | C2B—C3B—C4B | 119.9 (3) |
O19—Cr1—O15 | 89.47 (9) | C2B—C3B—H3B | 120.1 |
O12—Cr1—O15 | 89.99 (9) | C4B—C3B—H3B | 120.1 |
O5—Cr1—O15 | 178.95 (9) | C3B—C4B—C5B | 118.0 (3) |
O8—Cr1—O15 | 90.62 (8) | C3B—C4B—C7B | 119.4 (3) |
O19—Cr1—O1 | 92.81 (9) | C5B—C4B—C7B | 122.6 (3) |
O12—Cr1—O1 | 176.93 (9) | C6B—C5B—C4B | 119.8 (3) |
O5—Cr1—O1 | 88.72 (9) | C6B—C5B—H5B | 120.1 |
O8—Cr1—O1 | 88.87 (9) | C4B—C5B—H5B | 120.1 |
O15—Cr1—O1 | 91.61 (9) | N1B—C6B—C5B | 120.3 (3) |
C2—O1—Cr1 | 125.50 (19) | N1B—C6B—H6B | 119.9 |
O6—C2—O1 | 121.9 (3) | C5B—C6B—H6B | 119.9 |
O6—C2—C3 | 117.4 (3) | C8B—C7B—C4B | 123.9 (3) |
O1—C2—C3 | 120.7 (3) | C8B—C7B—H7B | 118.0 |
C4—C3—C2 | 118.7 (3) | C4B—C7B—H7B | 118.1 |
C4—C3—H31 | 107.7 | C7B—C8B—C9B | 125.1 (3) |
C2—C3—H31 | 107.7 | C7B—C8B—H8B | 117.5 |
C4—C3—H32 | 107.7 | C9B—C8B—H8B | 117.5 |
C2—C3—H32 | 107.7 | C10B—C9B—C14B | 117.3 (3) |
H31—C3—H32 | 107.1 | C10B—C9B—C8B | 123.4 (3) |
O7—C4—O5 | 122.5 (3) | C14B—C9B—C8B | 119.3 (3) |
O7—C4—C3 | 118.5 (3) | C11B—C10B—C9B | 118.9 (3) |
O5—C4—C3 | 118.9 (3) | C11B—C10B—H10B | 120.5 |
C4—O5—Cr1 | 125.84 (19) | C9B—C10B—H10B | 120.5 |
C9—O8—Cr1 | 125.22 (18) | N12B—C11B—C10B | 123.2 (3) |
O13—C9—O8 | 122.7 (3) | N12B—C11B—H11B | 118.4 |
O13—C9—C10 | 118.8 (3) | C10B—C11B—H11B | 118.4 |
O8—C9—C10 | 118.5 (3) | C13B—N12B—C11B | 117.9 (3) |
C9—C10—C11 | 118.4 (3) | N12B—C13B—C14B | 123.0 (3) |
C9—C10—H101 | 107.7 | N12B—C13B—H13B | 118.5 |
C11—C10—H101 | 107.7 | C14B—C13B—H13B | 118.5 |
C9—C10—H102 | 107.7 | C13B—C14B—C9B | 119.5 (3) |
C11—C10—H102 | 107.7 | C13B—C14B—H14B | 120.3 |
H101—C10—H102 | 107.1 | C9B—C14B—H14B | 120.3 |
O14—C11—O12 | 122.3 (3) | C2C—N1C—C6C | 119.9 (3) |
O14—C11—C10 | 117.7 (3) | C2C—N1C—H1C | 120.1 |
O12—C11—C10 | 119.9 (3) | C6C—N1C—H1C | 120.1 |
C11—O12—Cr1 | 125.8 (2) | N1C—C2C—C3C | 122.2 (3) |
C16—O15—Cr1 | 126.86 (19) | N1C—C2C—H2C | 118.9 |
O20—C16—O15 | 123.4 (3) | C3C—C2C—H2C | 118.9 |
O20—C16—C17 | 119.0 (3) | C4C—C3C—C2C | 119.4 (3) |
O15—C16—C17 | 117.5 (3) | C4C—C3C—H3C | 120.3 |
C18—C17—C16 | 114.4 (3) | C2C—C3C—H3C | 120.3 |
C18—C17—H171 | 108.7 | C3C—C4C—C5C | 118.1 (3) |
C16—C17—H171 | 108.7 | C3C—C4C—C7C | 117.5 (3) |
C18—C17—H172 | 108.7 | C5C—C4C—C7C | 124.3 (3) |
C16—C17—H172 | 108.7 | C6C—C5C—C4C | 119.8 (3) |
H171—C17—H172 | 107.6 | C6C—C5C—H5C | 120.1 |
O21—C18—O19 | 123.5 (3) | C4C—C5C—H5C | 120.1 |
O21—C18—C17 | 118.8 (3) | N1C—C6C—C5C | 120.6 (3) |
O19—C18—C17 | 117.7 (3) | N1C—C6C—H6C | 119.7 |
C18—O19—Cr1 | 127.19 (19) | C5C—C6C—H6C | 119.7 |
C6A—N1A—C2A | 118.2 (2) | C7Ci—C7C—C4C | 124.5 (4) |
C6A—N1A—H1A | 120.9 | C7Ci—C7C—H7C | 117.7 |
C2A—N1A—H1A | 120.9 | C4C—C7C—H7C | 117.7 |
N1A—C2A—C3A | 123.3 (3) | C2D—N1D—C2Dii | 121.8 (4) |
N1A—C2A—H2A | 118.4 | C2D—N1D—H1D | 119.1 |
C3A—C2A—H2A | 118.4 | C2Dii—N1D—H1D | 119.1 |
C2A—C3A—C4A | 119.0 (3) | N1D—C2D—C3D | 120.2 (3) |
C2A—C3A—H3A | 120.5 | N1D—C2D—H2D | 119.9 |
C4A—C3A—H3A | 120.5 | C3D—C2D—H2D | 119.9 |
C5A—C4A—C3A | 117.2 (3) | C2D—C3D—C4D | 120.0 (4) |
C5A—C4A—C7A | 119.9 (3) | C2D—C3D—H3D | 120.0 |
C3A—C4A—C7A | 123.0 (3) | C4D—C3D—H3D | 120.0 |
C6A—C5A—C4A | 120.2 (3) | C3D—C4D—C3Dii | 117.7 (4) |
C6A—C5A—H5A | 119.9 | C3D—C4D—C5D | 102.7 (3) |
C4A—C5A—H5A | 119.9 | C3Dii—C4D—C5D | 139.6 (3) |
N1A—C6A—C5A | 122.1 (3) | C6D—C5D—C4D | 114.2 (5) |
N1A—C6A—H6A | 118.9 | C6D—C5D—H5D | 122.9 |
C5A—C6A—H6A | 118.9 | C4D—C5D—H5D | 122.9 |
C8A—C7A—C4A | 125.1 (3) | C5D—C6D—C7D | 114.3 (5) |
C8A—C7A—H7A | 117.4 | C5D—C6D—H6D | 122.9 |
C4A—C7A—H7A | 117.4 | C7D—C6D—H6D | 122.9 |
C7A—C8A—C9A | 123.9 (3) | C8Dii—C7D—C8D | 117.9 (5) |
C7A—C8A—H8A | 118.0 | C8Dii—C7D—C6D | 139.1 (3) |
C9A—C8A—H8A | 118.0 | C8D—C7D—C6D | 102.9 (3) |
C10A—C9A—C14A | 117.8 (3) | C9D—C8D—C7D | 119.2 (4) |
C10A—C9A—C8A | 120.1 (2) | C9D—C8D—H8D | 120.4 |
C14A—C9A—C8A | 122.0 (3) | C7D—C8D—H8D | 120.4 |
C11A—C10A—C9A | 120.1 (3) | N10D—C9D—C8D | 122.8 (4) |
C11A—C10A—H10A | 119.9 | N10D—C9D—H9D | 118.6 |
C9A—C10A—H10A | 119.9 | C8D—C9D—H9D | 118.6 |
N12A—C11A—C10A | 120.1 (3) | C9D—N10D—C9Dii | 118.1 (4) |
N12A—C11A—H11A | 119.9 | H1S1—O1S—H1S2 | 100.3 |
C10A—C11A—H11A | 119.9 | H2S1—O2S—H2S2 | 97.7 |
C11A—N12A—C13A | 121.6 (2) | H3S1—O3S—H3S2 | 110.9 |
N12A—C13A—C14A | 120.6 (3) | H4S1—O4S—H4S2 | 87.9 |
N12A—C13A—H13A | 119.7 | H5S1—O5S—H5S2 | 102.4 |
C14A—C13A—H13A | 119.7 | H6S1—O6S—H6S2 | 102.4 |
C13A—C14A—C9A | 119.7 (3) | H7S1—O7S—H7S2 | 94.8 |
C13A—C14A—H14A | 120.2 | H8S1—O8S—H8S2 | 97.6 |
C9A—C14A—H14A | 120.2 | H8S3—O8S'—H8S4 | 102.2 |
C2B—N1B—C6B | 121.5 (3) | H8S5—O8S"—H8S6 | 98.5 |
| | | |
O19—Cr1—O1—C2 | −124.0 (2) | C3A—C4A—C7A—C8A | −9.8 (4) |
O8—Cr1—O1—C2 | 55.9 (2) | C4A—C7A—C8A—C9A | −177.0 (3) |
O15—Cr1—O1—C2 | 146.4 (2) | C7A—C8A—C9A—C10A | −169.5 (3) |
Cr1—O1—C2—O6 | −173.8 (2) | C7A—C8A—C9A—C14A | 11.5 (4) |
Cr1—O1—C2—C3 | 4.9 (4) | C14A—C9A—C10A—C11A | −0.8 (4) |
O6—C2—C3—C4 | −146.7 (3) | C8A—C9A—C10A—C11A | −179.9 (3) |
O1—C2—C3—C4 | 34.5 (4) | C9A—C10A—C11A—N12A | 0.1 (4) |
C2—C3—C4—O7 | 152.9 (3) | C10A—C11A—N12A—C13A | 0.6 (4) |
C2—C3—C4—O5 | −28.6 (4) | C11A—N12A—C13A—C14A | −0.6 (4) |
O7—C4—O5—Cr1 | 162.7 (2) | N12A—C13A—C14A—C9A | −0.1 (4) |
C3—C4—O5—Cr1 | −15.7 (4) | C10A—C9A—C14A—C13A | 0.8 (4) |
O19—Cr1—O5—C4 | 133.4 (2) | C8A—C9A—C14A—C13A | 179.9 (3) |
O12—Cr1—O5—C4 | −136.8 (2) | C6B—N1B—C2B—C3B | 1.6 (4) |
O8—Cr1—O5—C4 | −48.3 (2) | N1B—C2B—C3B—C4B | −0.1 (4) |
O1—Cr1—O5—C4 | 40.6 (2) | C2B—C3B—C4B—C5B | −1.6 (4) |
O12—Cr1—O8—C9 | 44.0 (2) | C2B—C3B—C4B—C7B | 179.6 (3) |
O5—Cr1—O8—C9 | −45.7 (2) | C3B—C4B—C5B—C6B | 2.0 (5) |
O15—Cr1—O8—C9 | 133.9 (2) | C7B—C4B—C5B—C6B | −179.3 (3) |
O1—Cr1—O8—C9 | −134.5 (2) | C2B—N1B—C6B—C5B | −1.1 (5) |
Cr1—O8—C9—O13 | 158.8 (2) | C4B—C5B—C6B—N1B | −0.7 (5) |
Cr1—O8—C9—C10 | −20.2 (4) | C3B—C4B—C7B—C8B | −167.9 (3) |
O13—C9—C10—C11 | 153.7 (3) | C5B—C4B—C7B—C8B | 13.4 (5) |
O8—C9—C10—C11 | −27.2 (4) | C4B—C7B—C8B—C9B | −178.2 (3) |
C9—C10—C11—O14 | −144.4 (3) | C7B—C8B—C9B—C10B | −6.2 (5) |
C9—C10—C11—O12 | 37.9 (4) | C7B—C8B—C9B—C14B | 172.6 (3) |
O14—C11—O12—Cr1 | −177.0 (2) | C14B—C9B—C10B—C11B | −2.2 (4) |
C10—C11—O12—Cr1 | 0.6 (4) | C8B—C9B—C10B—C11B | 176.7 (3) |
O19—Cr1—O12—C11 | 146.9 (2) | C9B—C10B—C11B—N12B | 0.0 (4) |
O5—Cr1—O12—C11 | 57.4 (2) | C10B—C11B—N12B—C13B | 1.5 (4) |
O8—Cr1—O12—C11 | −33.0 (2) | C11B—N12B—C13B—C14B | −0.8 (5) |
O15—Cr1—O12—C11 | −123.7 (2) | N12B—C13B—C14B—C9B | −1.4 (5) |
O19—Cr1—O15—C16 | −27.8 (2) | C10B—C9B—C14B—C13B | 2.8 (4) |
O12—Cr1—O15—C16 | −117.6 (2) | C8B—C9B—C14B—C13B | −176.1 (3) |
O8—Cr1—O15—C16 | 153.9 (2) | C6C—N1C—C2C—C3C | −1.0 (5) |
O1—Cr1—O15—C16 | 65.0 (2) | N1C—C2C—C3C—C4C | −0.4 (5) |
Cr1—O15—C16—O20 | 178.7 (2) | C2C—C3C—C4C—C5C | 1.3 (5) |
Cr1—O15—C16—C17 | −4.7 (4) | C2C—C3C—C4C—C7C | −178.7 (3) |
O20—C16—C17—C18 | −134.0 (3) | C3C—C4C—C5C—C6C | −0.8 (5) |
O15—C16—C17—C18 | 49.3 (4) | C7C—C4C—C5C—C6C | 179.2 (3) |
C16—C17—C18—O21 | 132.7 (3) | C2C—N1C—C6C—C5C | 1.5 (5) |
C16—C17—C18—O19 | −50.0 (4) | C4C—C5C—C6C—N1C | −0.6 (5) |
O21—C18—O19—Cr1 | −177.1 (2) | C3C—C4C—C7C—C7Ci | −172.0 (4) |
C17—C18—O19—Cr1 | 5.7 (4) | C5C—C4C—C7C—C7Ci | 8.0 (6) |
O12—Cr1—O19—C18 | 117.3 (2) | C2Dii—N1D—C2D—C3D | 0.3 (2) |
O5—Cr1—O19—C18 | −153.0 (3) | N1D—C2D—C3D—C4D | −0.7 (5) |
O15—Cr1—O19—C18 | 27.3 (2) | C2D—C3D—C4D—C3Dii | 0.3 (2) |
O1—Cr1—O19—C18 | −64.3 (3) | C2D—C3D—C4D—C5D | −179.1 (4) |
C6A—N1A—C2A—C3A | 1.1 (4) | C3D—C4D—C5D—C6D | −177.1 (4) |
N1A—C2A—C3A—C4A | 0.3 (4) | C3Dii—C4D—C5D—C6D | 3.7 (7) |
C2A—C3A—C4A—C5A | −2.2 (4) | C4D—C5D—C6D—C7D | −178.9 (3) |
C2A—C3A—C4A—C7A | 176.3 (3) | C5D—C6D—C7D—C8Dii | 15.1 (7) |
C3A—C4A—C5A—C6A | 2.8 (4) | C5D—C6D—C7D—C8D | −169.5 (4) |
C7A—C4A—C5A—C6A | −175.8 (3) | C8Dii—C7D—C8D—C9D | −0.1 (2) |
C2A—N1A—C6A—C5A | −0.5 (4) | C6D—C7D—C8D—C9D | −176.7 (3) |
C4A—C5A—C6A—N1A | −1.5 (5) | C7D—C8D—C9D—N10D | 0.1 (5) |
C5A—C4A—C7A—C8A | 168.7 (3) | C8D—C9D—N10D—C9Dii | −0.1 (2) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z; (ii) −x+1, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1A—H1A···N12Aiii | 0.88 | 1.84 | 2.715 (3) | 174 |
N1B—H1B···N12Biv | 0.88 | 1.82 | 2.702 (4) | 175 |
N1C—H1C···N1Cv | 0.88 | 1.78 | 2.664 (5) | 179 |
N1D—H1D···N10Div | 0.88 | 1.79 | 2.674 (5) | 180 |
O1S—H1S1···O6 | 0.90 | 1.94 | 2.802 (3) | 161 |
O2S—H2S1···O6 | 0.91 | 1.83 | 2.733 (3) | 176 |
O2S—H2S2···O3S | 0.91 | 1.88 | 2.784 (4) | 174 |
O3S—H3S1···O1S | 0.86 | 1.92 | 2.770 (4) | 168 |
O4S—H4S1···O5S | 0.93 | 2.53 | 3.368 (4) | 149 |
O4S—H4S2···O20iv | 0.93 | 1.93 | 2.853 (4) | 172 |
O5S—H5S1···O21iv | 0.90 | 1.97 | 2.838 (4) | 161 |
O5S—H5S2···O7S | 0.90 | 1.80 | 2.692 (5) | 169 |
O6S—H6S1···O14 | 0.89 | 1.84 | 2.722 (4) | 174 |
O8S′—H8S3···O8Svi | 0.88 | 1.87 | 2.751 (10) | 174 |
O8S′—H8S4···O14 | 0.87 | 1.81 | 2.632 (6) | 156 |
Symmetry codes: (iii) x, y+1, z; (iv) x, y−1, z; (v) −x+1/2, −y+3/2, −z; (vi) −x, −y+1, −z. |