Cucurbit[6]uril crystallizes with bis(μ-oxo-κ
2O:
O)bis[aquaoxodichloromolybdenum(VI)] as the 10.5-hydrate, with the formula [Mo
2O
4Cl
4(H
2O)
2]·(C
36H
36N
24O
12)·10.5H
2O. The molybdenum-bearing component interacts indirectly with two cryptands through the two coordinated water molecules, each outer-sphere-coordination cryptand forming only one hydrogen bond with each water molecule. The asymmetric unit has two cryptands, both of which lie on special positions of
site symmetry. One of them encapsulates a water molecule that is disordered over two general positions, whereas the other encapsulates one that lies on a centre of inversion. The solvent water molecules interact with the dinuclear complex and with both cucurbituril molecules to form a three-dimensional network structure.
Supporting information
CCDC reference: 271819
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.005 Å
- H-atom completeness 99%
- Disorder in solvent or counterion
- R factor = 0.046
- wR factor = 0.139
- Data-to-parameter ratio = 14.4
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT430_ALERT_2_A Short Inter D...A Contact O13' .. O13W .. 1.98 Ang.
| Author Response: The two atoms are disordered with respect to each other.
|
PLAT430_ALERT_2_A Short Inter D...A Contact O13W .. O13W .. 2.47 Ang.
| Author Response: The two atoms are disordered with respect to each other.
|
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.96
PLAT417_ALERT_2_B Short Inter D-H..H-D H22 .. H62 .. 2.05 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H61 .. H72 .. 2.05 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H81 .. H102 .. 2.05 Ang.
PLAT420_ALERT_2_B D-H Without Acceptor O6W - H62 ... ?
PLAT430_ALERT_2_B Short Inter D...A Contact O13' .. O13' .. 2.69 Ang.
| Author Response: The two atoms are disordered with respect to each other.
|
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 18.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O12'
PLAT417_ALERT_2_C Short Inter D-H..H-D H41 .. H52 .. 2.12 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D H102 .. H112 .. 2.12 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact O9 .. C5 .. 2.93 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact O12W .. C7 .. 2.99 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact O13 .. C22 .. 2.96 Ang.
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 9
H2 O
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. # 12
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 13
H2 O0.70
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 15
O
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C36 H61 Cl4 Mo2 N24 O28.5
Atom count from _chemical_formula_moiety:C36 H97 Cl80 N24 O122.5
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C36 H61 Cl4 Mo2 N24 O28.5
Atom count from the _atom_site data: C36 H60 Cl4 Mo2 N24 O28.5
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 2
From the CIF: _chemical_formula_sum C36 H61 Cl4 Mo2 N24 O28.50
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 72.00 72.00 0.00
H 122.00 120.00 2.00
Cl 8.00 8.00 0.00
Mo 4.00 4.00 0.00
N 48.00 48.00 0.00
O 57.00 57.00 0.00
2 ALERT level A = In general: serious problem
6 ALERT level B = Potentially serious problem
17 ALERT level C = Check and explain
4 ALERT level G = General alerts; check
7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
14 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
7 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Bis[µ-oxoaquadichloromolybdenum(VI)]–cucurbit[6]uril 10.5-hydrate
top
Crystal data top
[Mo2O4Cl4(H2O)2]·(C36H36N24O12)·10.5H2O | Z = 2 |
Mr = 1619.77 | F(000) = 1650 |
Triclinic, P1 | Dx = 1.866 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.4125 (5) Å | Cell parameters from 8301 reflections |
b = 15.4864 (6) Å | θ = 2.8–28.3° |
c = 17.5542 (7) Å | µ = 0.73 mm−1 |
α = 106.082 (1)° | T = 173 K |
β = 105.386 (1)° | Rod, brown |
γ = 106.520 (1)° | 0.41 × 0.40 × 0.10 mm |
V = 2883.5 (2) Å3 | |
Data collection top
Bruker APEX CCD area-detector diffractometer | 12659 independent reflections |
Radiation source: fine-focus sealed tube | 11649 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.016 |
φ and ω scans | θmax = 27.5°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −16→16 |
Tmin = 0.701, Tmax = 0.930 | k = −20→20 |
24428 measured reflections | l = −22→22 |
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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.139 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0814P)2 + 8.1614P] where P = (Fo2 + 2Fc2)/3 |
12659 reflections | (Δ/σ)max = 0.001 |
879 parameters | Δρmax = 1.75 e Å−3 |
75 restraints | Δρmin = −1.70 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo1 | 0.60746 (2) | 0.334298 (19) | 0.844003 (17) | 0.01660 (8) | |
Mo2 | 0.45234 (2) | 0.179157 (19) | 0.716433 (17) | 0.01717 (8) | |
Cl1 | 0.59089 (15) | 0.47195 (10) | 0.93595 (9) | 0.0593 (3) | |
Cl2 | 0.83062 (8) | 0.42171 (6) | 0.89688 (6) | 0.02733 (18) | |
Cl3 | 0.22912 (8) | 0.10991 (6) | 0.63950 (6) | 0.02900 (19) | |
Cl4 | 0.47979 (10) | 0.06971 (7) | 0.59802 (7) | 0.0390 (2) | |
O1 | 0.9720 (2) | 0.5054 (2) | 0.74476 (18) | 0.0336 (6) | |
O2 | 0.5981 (3) | 0.4594 (2) | 0.41654 (17) | 0.0332 (6) | |
O3 | 1.1486 (2) | 0.7330 (2) | 0.76140 (18) | 0.0308 (6) | |
O4 | 0.7872 (3) | 0.6859 (2) | 0.43772 (18) | 0.0410 (7) | |
O5 | 1.3632 (2) | 0.76091 (19) | 0.69062 (15) | 0.0249 (5) | |
O6 | 0.9999 (2) | 0.7096 (2) | 0.35269 (17) | 0.0302 (6) | |
O7 | 0.6779 (2) | 0.77056 (19) | 0.75935 (17) | 0.0275 (5) | |
O8 | 0.6833 (3) | 1.06307 (19) | 1.08288 (16) | 0.0289 (6) | |
O9 | 0.7813 (2) | 0.64015 (18) | 0.86873 (16) | 0.0246 (5) | |
O10 | 0.8346 (2) | 0.95723 (18) | 1.18661 (17) | 0.0283 (6) | |
O11 | 1.0998 (2) | 0.7571 (2) | 0.95076 (17) | 0.0337 (6) | |
O12 | 1.1398 (2) | 1.03028 (19) | 1.29138 (17) | 0.0297 (6) | |
O13 | 0.6217 (2) | 0.28867 (18) | 0.92072 (16) | 0.0273 (5) | |
O14 | 0.4414 (2) | 0.10072 (18) | 0.76637 (16) | 0.0248 (5) | |
O15 | 0.6244 (2) | 0.24796 (16) | 0.74973 (15) | 0.0196 (5) | |
O16 | 0.4351 (2) | 0.29330 (17) | 0.78371 (15) | 0.0207 (5) | |
O1W | 0.6288 (2) | 0.44041 (17) | 0.77717 (15) | 0.0228 (5) | |
H11 | 0.6861 | 0.4942 | 0.8074 | 0.050* | |
H12 | 0.5664 | 0.4520 | 0.7608 | 0.050* | |
O2W | 0.4299 (2) | 0.25623 (19) | 0.61839 (16) | 0.0256 (5) | |
H21 | 0.3967 | 0.2960 | 0.6243 | 0.050* | |
H22 | 0.4060 | 0.2226 | 0.5666 | 0.050* | |
O3W | 0.4309 (3) | 0.4608 (3) | 0.7047 (2) | 0.0421 (7) | |
H31 | 0.4125 | 0.4832 | 0.6672 | 0.050* | |
H32 | 0.3731 | 0.4477 | 0.7212 | 0.050* | |
O4W | 0.2475 (3) | 0.3547 (2) | 0.7529 (2) | 0.0371 (6) | |
H41 | 0.2892 | 0.3208 | 0.7480 | 0.050* | |
H42 | 0.1798 | 0.3234 | 0.7132 | 0.050* | |
O5W | 0.4050 (6) | 0.5109 (4) | 0.8859 (4) | 0.036 (2) | 0.537 (14) |
H51 | 0.3707 | 0.5267 | 0.9201 | 0.050* | |
H52 | 0.3515 | 0.4605 | 0.8446 | 0.050* | |
O5' | 0.3453 (10) | 0.5272 (6) | 0.9108 (5) | 0.055 (3) | 0.463 (14) |
O6W | 0.3312 (4) | 0.1247 (3) | 0.4535 (2) | 0.0704 (13) | |
H61 | 0.3173 | 0.0810 | 0.4076 | 0.050* | |
H62 | 0.2657 | 0.1116 | 0.4627 | 0.050* | |
O7W | 0.3257 (11) | −0.0436 (9) | 0.4110 (8) | 0.206 (5) | |
H71 | 0.3220 | −0.0928 | 0.3696 | 0.050* | |
H72 | 0.2498 | −0.0580 | 0.4036 | 0.050* | |
O8W | 1.1187 (4) | 0.4680 (3) | 0.6336 (3) | 0.0751 (13) | |
H81 | 1.1411 | 0.4450 | 0.5934 | 0.050* | |
H82 | 1.0633 | 0.4204 | 0.6323 | 0.050* | |
O9W | 1.1348 (3) | 0.5295 (3) | 0.9029 (2) | 0.0572 (10) | |
H91 | 1.1299 | 0.5490 | 0.9512 | 0.050* | |
H92 | 1.0698 | 0.5240 | 0.8672 | 0.050* | |
O10W | 1.3020 (3) | 0.6148 (2) | 0.7409 (2) | 0.0399 (7) | |
H101 | 1.3199 | 0.6500 | 0.7140 | 0.050* | |
H102 | 1.2502 | 0.5607 | 0.7061 | 0.050* | |
O11W | 1.2667 (3) | 0.6789 (3) | 0.8744 (2) | 0.0451 (8) | |
H111 | 1.2159 | 0.7008 | 0.8546 | 0.050* | |
H112 | 1.2747 | 0.6432 | 0.8321 | 0.050* | |
O12W | 0.9333 (5) | 1.0992 (4) | 1.1297 (4) | 0.0593 (18) | 0.705 (11) |
H121 | 0.9544 | 1.0704 | 1.0917 | 0.050* | |
H122 | 0.8805 | 1.1165 | 1.1064 | 0.050* | |
O12' | 1.0770 (15) | 1.1282 (14) | 1.0802 (12) | 0.085 (6) | 0.295 (11) |
O13W | 0.946 (3) | 0.538 (2) | 0.5397 (15) | 0.121 (7) | 0.25 |
O13' | 1.076 (3) | 0.594 (2) | 0.5325 (15) | 0.121 (7) | 0.25 |
N1 | 0.7798 (3) | 0.4069 (2) | 0.64596 (18) | 0.0220 (6) | |
N2 | 0.6295 (3) | 0.3891 (2) | 0.51503 (18) | 0.0215 (6) | |
N3 | 0.8304 (3) | 0.5663 (2) | 0.69580 (19) | 0.0232 (6) | |
N4 | 0.6856 (3) | 0.5492 (2) | 0.56199 (19) | 0.0230 (6) | |
N5 | 0.9530 (3) | 0.7228 (2) | 0.7040 (2) | 0.0254 (6) | |
N6 | 0.8045 (3) | 0.7119 (2) | 0.5768 (2) | 0.0268 (6) | |
N7 | 1.0997 (3) | 0.8239 (2) | 0.68472 (19) | 0.0228 (6) | |
N8 | 0.9516 (3) | 0.8060 (2) | 0.55287 (19) | 0.0239 (6) | |
N9 | 1.2607 (3) | 0.8423 (2) | 0.62929 (18) | 0.0225 (6) | |
N10 | 1.1079 (3) | 0.8140 (2) | 0.49380 (19) | 0.0229 (6) | |
N11 | 1.3405 (3) | 0.7564 (2) | 0.55489 (18) | 0.0220 (6) | |
N12 | 1.2015 (3) | 0.7446 (2) | 0.42053 (18) | 0.0245 (6) | |
N13 | 0.6291 (3) | 0.9026 (2) | 0.81093 (18) | 0.0198 (5) | |
N14 | 0.6244 (3) | 1.0164 (2) | 0.93701 (18) | 0.0204 (6) | |
N15 | 0.5905 (3) | 0.7851 (2) | 0.86106 (18) | 0.0201 (6) | |
N16 | 0.5960 (3) | 0.9021 (2) | 0.98990 (18) | 0.0230 (6) | |
N17 | 0.6719 (3) | 0.6988 (2) | 0.94186 (18) | 0.0202 (6) | |
N18 | 0.6895 (3) | 0.8220 (2) | 1.07105 (19) | 0.0215 (6) | |
N19 | 0.8389 (3) | 0.6877 (2) | 1.01472 (18) | 0.0216 (6) | |
N20 | 0.8566 (3) | 0.8101 (2) | 1.14469 (18) | 0.0219 (6) | |
N21 | 1.0575 (2) | 0.7584 (2) | 1.07165 (18) | 0.0202 (6) | |
N22 | 1.0753 (3) | 0.8675 (2) | 1.20886 (19) | 0.0220 (6) | |
N23 | 1.2367 (2) | 0.8589 (2) | 1.08683 (18) | 0.0197 (5) | |
N24 | 1.2505 (3) | 0.9695 (2) | 1.22090 (18) | 0.0210 (6) | |
C1 | 0.8712 (3) | 0.4947 (3) | 0.7002 (2) | 0.0231 (7) | |
C2 | 0.6687 (3) | 0.4177 (2) | 0.6065 (2) | 0.0189 (6) | |
H2 | 0.6050 | 0.3866 | 0.6229 | 0.023* | |
C3 | 0.7051 (3) | 0.5295 (2) | 0.6396 (2) | 0.0207 (6) | |
H3 | 0.6563 | 0.5493 | 0.6694 | 0.025* | |
C4 | 0.6352 (3) | 0.4653 (3) | 0.4898 (2) | 0.0220 (7) | |
C5 | 0.9011 (3) | 0.6678 (3) | 0.7489 (2) | 0.0248 (7) | |
H5A | 0.9652 | 0.6728 | 0.7969 | 0.030* | |
H5B | 0.8505 | 0.6960 | 0.7706 | 0.030* | |
C6 | 0.6869 (3) | 0.6420 (3) | 0.5598 (3) | 0.0269 (7) | |
H6A | 0.6328 | 0.6312 | 0.5044 | 0.032* | |
H6B | 0.6562 | 0.6696 | 0.6011 | 0.032* | |
C7 | 1.0746 (3) | 0.7569 (3) | 0.7203 (2) | 0.0229 (7) | |
C8 | 0.8927 (3) | 0.7736 (2) | 0.6619 (2) | 0.0222 (7) | |
H8 | 0.8596 | 0.8093 | 0.6966 | 0.027* | |
C9 | 0.9954 (3) | 0.8420 (2) | 0.6452 (2) | 0.0210 (6) | |
H9 | 1.0071 | 0.9091 | 0.6699 | 0.025* | |
C10 | 0.8424 (3) | 0.7294 (3) | 0.5143 (2) | 0.0269 (7) | |
C11 | 1.0142 (3) | 0.8488 (3) | 0.5060 (2) | 0.0233 (7) | |
H11A | 1.0504 | 0.9182 | 0.5359 | 0.028* | |
H11B | 0.9564 | 0.8348 | 0.4510 | 0.028* | |
C12 | 1.2230 (3) | 0.8812 (3) | 0.6985 (2) | 0.0229 (7) | |
H12A | 1.2767 | 0.8843 | 0.7508 | 0.027* | |
H12B | 1.2302 | 0.9465 | 0.7051 | 0.027* | |
C13 | 1.3231 (3) | 0.7829 (2) | 0.6304 (2) | 0.0205 (6) | |
C14 | 1.2344 (3) | 0.8610 (2) | 0.5519 (2) | 0.0210 (6) | |
H14 | 1.2662 | 0.9295 | 0.5637 | 0.025* | |
C15 | 1.2974 (3) | 0.8070 (2) | 0.5023 (2) | 0.0212 (7) | |
H15 | 1.3631 | 0.8517 | 0.4963 | 0.025* | |
C16 | 1.0932 (3) | 0.7513 (3) | 0.4164 (2) | 0.0226 (7) | |
C17 | 1.2180 (3) | 0.6841 (3) | 0.3490 (2) | 0.0237 (7) | |
H17A | 1.1534 | 0.6704 | 0.2973 | 0.028* | |
H17B | 1.2927 | 0.7198 | 0.3458 | 0.028* | |
C18 | 1.4256 (3) | 0.7116 (2) | 0.5448 (2) | 0.0221 (7) | |
H18A | 1.4714 | 0.7145 | 0.5996 | 0.027* | |
H18B | 1.4812 | 0.7488 | 0.5258 | 0.027* | |
C19 | 0.6368 (3) | 0.8142 (2) | 0.8055 (2) | 0.0199 (6) | |
C20 | 0.6434 (3) | 0.9417 (2) | 0.7467 (2) | 0.0218 (7) | |
H20A | 0.6485 | 0.8936 | 0.7011 | 0.026* | |
H20B | 0.5729 | 0.9542 | 0.7233 | 0.026* | |
C21 | 0.5595 (3) | 0.9278 (2) | 0.8615 (2) | 0.0181 (6) | |
H21A | 0.4850 | 0.9276 | 0.8270 | 0.022* | |
C22 | 0.6582 (3) | 1.1120 (2) | 0.9351 (2) | 0.0199 (6) | |
H22A | 0.6740 | 1.1581 | 0.9903 | 0.024* | |
H22B | 0.5911 | 1.1145 | 0.8945 | 0.024* | |
C23 | 0.5359 (3) | 0.8473 (2) | 0.8985 (2) | 0.0184 (6) | |
H23 | 0.4508 | 0.8124 | 0.8827 | 0.022* | |
C24 | 0.6402 (3) | 1.0003 (2) | 1.0108 (2) | 0.0210 (6) | |
C25 | 0.5967 (3) | 0.8602 (3) | 1.0539 (2) | 0.0205 (6) | |
H25A | 0.6077 | 0.9092 | 1.1060 | 0.025* | |
H25B | 0.5192 | 0.8087 | 1.0354 | 0.025* | |
C26 | 0.5773 (3) | 0.6923 (2) | 0.8686 (2) | 0.0199 (6) | |
H26A | 0.5774 | 0.6488 | 0.8176 | 0.024* | |
H26B | 0.5003 | 0.6649 | 0.8727 | 0.024* | |
C27 | 0.6705 (3) | 0.7217 (2) | 1.0272 (2) | 0.0176 (6) | |
H27 | 0.5993 | 0.6772 | 1.0280 | 0.021* | |
C28 | 0.7877 (3) | 0.7134 (2) | 1.0786 (2) | 0.0195 (6) | |
H28 | 0.7700 | 0.6646 | 1.1023 | 0.023* | |
C29 | 0.7975 (3) | 0.8719 (2) | 1.1391 (2) | 0.0206 (6) | |
C30 | 0.7665 (3) | 0.6733 (2) | 0.9353 (2) | 0.0194 (6) | |
C31 | 0.9493 (3) | 0.6698 (2) | 1.0304 (2) | 0.0222 (7) | |
H31A | 0.9494 | 0.6319 | 0.9769 | 0.027* | |
H31B | 0.9508 | 0.6323 | 1.0656 | 0.027* | |
C32 | 1.1283 (3) | 0.7879 (2) | 1.0286 (2) | 0.0215 (7) | |
C33 | 1.1221 (3) | 0.8038 (2) | 1.1632 (2) | 0.0196 (6) | |
H33 | 1.1309 | 0.7565 | 1.1875 | 0.024* | |
C34 | 0.9614 (3) | 0.8343 (3) | 1.2191 (2) | 0.0221 (7) | |
H34A | 0.9621 | 0.8841 | 1.2664 | 0.027* | |
H34B | 0.9536 | 0.7777 | 1.2332 | 0.027* | |
C35 | 1.1535 (3) | 0.9632 (2) | 1.2445 (2) | 0.0211 (6) | |
C36 | 1.2463 (3) | 0.8747 (2) | 1.1734 (2) | 0.0188 (6) | |
H36 | 1.3120 | 0.8611 | 1.2037 | 0.023* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo1 | 0.01957 (14) | 0.01388 (14) | 0.01605 (14) | 0.00537 (10) | 0.00654 (10) | 0.00651 (10) |
Mo2 | 0.01846 (14) | 0.01453 (14) | 0.01714 (14) | 0.00418 (10) | 0.00697 (10) | 0.00602 (11) |
Cl1 | 0.0757 (9) | 0.0469 (7) | 0.0522 (7) | 0.0164 (6) | 0.0287 (7) | 0.0173 (6) |
Cl2 | 0.0204 (4) | 0.0222 (4) | 0.0324 (4) | 0.0062 (3) | 0.0050 (3) | 0.0072 (3) |
Cl3 | 0.0195 (4) | 0.0260 (4) | 0.0355 (5) | 0.0040 (3) | 0.0060 (3) | 0.0122 (4) |
Cl4 | 0.0402 (5) | 0.0308 (5) | 0.0329 (5) | 0.0043 (4) | 0.0160 (4) | 0.0006 (4) |
O1 | 0.0217 (13) | 0.0370 (15) | 0.0320 (14) | 0.0056 (11) | 0.0011 (11) | 0.0135 (12) |
O2 | 0.0346 (15) | 0.0339 (15) | 0.0204 (13) | 0.0044 (12) | 0.0019 (11) | 0.0122 (11) |
O3 | 0.0260 (13) | 0.0334 (14) | 0.0333 (14) | 0.0102 (11) | 0.0103 (11) | 0.0152 (12) |
O4 | 0.0425 (17) | 0.0320 (15) | 0.0244 (14) | −0.0078 (13) | 0.0044 (12) | 0.0066 (12) |
O5 | 0.0214 (12) | 0.0289 (13) | 0.0191 (12) | 0.0071 (10) | 0.0063 (9) | 0.0055 (10) |
O6 | 0.0266 (13) | 0.0361 (15) | 0.0231 (13) | 0.0132 (11) | 0.0045 (10) | 0.0079 (11) |
O7 | 0.0331 (14) | 0.0284 (13) | 0.0278 (13) | 0.0161 (11) | 0.0183 (11) | 0.0095 (11) |
O8 | 0.0384 (15) | 0.0220 (12) | 0.0185 (12) | 0.0098 (11) | 0.0083 (11) | 0.0008 (10) |
O9 | 0.0268 (12) | 0.0263 (13) | 0.0249 (12) | 0.0114 (10) | 0.0153 (10) | 0.0093 (10) |
O10 | 0.0311 (14) | 0.0186 (12) | 0.0253 (13) | 0.0076 (10) | 0.0075 (11) | −0.0008 (10) |
O11 | 0.0257 (13) | 0.0396 (16) | 0.0181 (12) | 0.0033 (12) | 0.0053 (10) | −0.0016 (11) |
O12 | 0.0283 (13) | 0.0218 (12) | 0.0294 (14) | 0.0055 (10) | 0.0133 (11) | −0.0020 (10) |
O13 | 0.0333 (14) | 0.0223 (12) | 0.0229 (12) | 0.0062 (11) | 0.0067 (10) | 0.0119 (10) |
O14 | 0.0258 (12) | 0.0187 (12) | 0.0282 (13) | 0.0044 (10) | 0.0092 (10) | 0.0119 (10) |
O15 | 0.0198 (11) | 0.0167 (11) | 0.0224 (11) | 0.0062 (9) | 0.0090 (9) | 0.0073 (9) |
O16 | 0.0201 (11) | 0.0187 (11) | 0.0231 (12) | 0.0076 (9) | 0.0086 (9) | 0.0071 (9) |
O1W | 0.0251 (12) | 0.0184 (11) | 0.0224 (12) | 0.0045 (9) | 0.0070 (10) | 0.0099 (10) |
O2W | 0.0253 (12) | 0.0289 (13) | 0.0209 (12) | 0.0079 (10) | 0.0071 (10) | 0.0110 (10) |
O3W | 0.0329 (15) | 0.0544 (19) | 0.0450 (17) | 0.0136 (14) | 0.0109 (13) | 0.0343 (16) |
O4W | 0.0366 (15) | 0.0437 (17) | 0.0385 (16) | 0.0233 (13) | 0.0154 (13) | 0.0170 (13) |
O5W | 0.034 (3) | 0.032 (3) | 0.034 (3) | 0.005 (2) | 0.010 (2) | 0.013 (2) |
O5' | 0.082 (6) | 0.052 (4) | 0.031 (4) | 0.028 (4) | 0.019 (4) | 0.017 (3) |
O6W | 0.068 (3) | 0.071 (3) | 0.0259 (17) | −0.015 (2) | 0.0071 (16) | 0.0050 (17) |
O7W | 0.203 (8) | 0.214 (8) | 0.212 (8) | 0.126 (7) | 0.086 (6) | 0.040 (6) |
O8W | 0.074 (3) | 0.047 (2) | 0.080 (3) | 0.001 (2) | 0.022 (2) | 0.020 (2) |
O9W | 0.0447 (19) | 0.069 (2) | 0.0372 (18) | 0.0007 (17) | 0.0044 (15) | 0.0235 (17) |
O10W | 0.0354 (15) | 0.0442 (17) | 0.0408 (17) | 0.0137 (13) | 0.0131 (13) | 0.0201 (14) |
O11W | 0.0421 (17) | 0.061 (2) | 0.0366 (16) | 0.0224 (16) | 0.0153 (14) | 0.0228 (15) |
O12W | 0.049 (3) | 0.038 (3) | 0.067 (4) | 0.008 (2) | 0.005 (2) | 0.011 (2) |
O12' | 0.068 (8) | 0.088 (9) | 0.096 (9) | 0.012 (6) | 0.049 (7) | 0.032 (7) |
O13W | 0.152 (18) | 0.144 (17) | 0.071 (10) | 0.065 (15) | 0.014 (12) | 0.066 (11) |
O13' | 0.152 (18) | 0.144 (17) | 0.071 (10) | 0.065 (15) | 0.014 (12) | 0.066 (11) |
N1 | 0.0217 (14) | 0.0218 (14) | 0.0198 (14) | 0.0066 (11) | 0.0066 (11) | 0.0071 (11) |
N2 | 0.0229 (14) | 0.0223 (14) | 0.0154 (13) | 0.0064 (11) | 0.0073 (11) | 0.0036 (11) |
N3 | 0.0203 (14) | 0.0202 (14) | 0.0215 (14) | 0.0026 (11) | 0.0050 (11) | 0.0051 (11) |
N4 | 0.0215 (14) | 0.0220 (14) | 0.0202 (14) | 0.0032 (11) | 0.0060 (11) | 0.0078 (11) |
N5 | 0.0199 (14) | 0.0278 (15) | 0.0274 (15) | 0.0048 (12) | 0.0099 (12) | 0.0123 (13) |
N6 | 0.0226 (15) | 0.0224 (15) | 0.0268 (15) | −0.0004 (12) | 0.0063 (12) | 0.0092 (12) |
N7 | 0.0178 (13) | 0.0218 (14) | 0.0260 (15) | 0.0051 (11) | 0.0100 (11) | 0.0062 (12) |
N8 | 0.0221 (14) | 0.0232 (14) | 0.0232 (15) | 0.0041 (12) | 0.0104 (12) | 0.0071 (12) |
N9 | 0.0217 (14) | 0.0245 (14) | 0.0199 (14) | 0.0079 (12) | 0.0106 (11) | 0.0050 (11) |
N10 | 0.0201 (14) | 0.0239 (14) | 0.0228 (14) | 0.0073 (12) | 0.0089 (11) | 0.0062 (12) |
N11 | 0.0212 (14) | 0.0260 (15) | 0.0181 (13) | 0.0090 (12) | 0.0095 (11) | 0.0054 (11) |
N12 | 0.0253 (15) | 0.0293 (16) | 0.0170 (13) | 0.0109 (12) | 0.0085 (11) | 0.0051 (12) |
N13 | 0.0232 (14) | 0.0162 (13) | 0.0185 (13) | 0.0056 (11) | 0.0094 (11) | 0.0050 (11) |
N14 | 0.0240 (14) | 0.0136 (13) | 0.0179 (13) | 0.0043 (11) | 0.0065 (11) | 0.0022 (10) |
N15 | 0.0251 (14) | 0.0163 (13) | 0.0198 (13) | 0.0083 (11) | 0.0109 (11) | 0.0054 (11) |
N16 | 0.0314 (15) | 0.0185 (14) | 0.0167 (13) | 0.0085 (12) | 0.0091 (12) | 0.0046 (11) |
N17 | 0.0218 (14) | 0.0208 (14) | 0.0185 (13) | 0.0097 (11) | 0.0085 (11) | 0.0057 (11) |
N18 | 0.0205 (14) | 0.0175 (13) | 0.0229 (14) | 0.0077 (11) | 0.0067 (11) | 0.0035 (11) |
N19 | 0.0189 (13) | 0.0219 (14) | 0.0215 (14) | 0.0082 (11) | 0.0076 (11) | 0.0043 (11) |
N20 | 0.0201 (13) | 0.0186 (14) | 0.0201 (14) | 0.0050 (11) | 0.0038 (11) | 0.0037 (11) |
N21 | 0.0175 (13) | 0.0148 (13) | 0.0203 (14) | 0.0029 (10) | 0.0044 (11) | 0.0012 (11) |
N22 | 0.0195 (13) | 0.0168 (13) | 0.0232 (14) | 0.0039 (11) | 0.0083 (11) | 0.0010 (11) |
N23 | 0.0182 (13) | 0.0174 (13) | 0.0192 (13) | 0.0056 (11) | 0.0071 (11) | 0.0022 (11) |
N24 | 0.0219 (14) | 0.0152 (13) | 0.0197 (13) | 0.0021 (11) | 0.0092 (11) | 0.0017 (11) |
C1 | 0.0219 (16) | 0.0267 (17) | 0.0179 (15) | 0.0054 (14) | 0.0085 (13) | 0.0075 (13) |
C2 | 0.0184 (15) | 0.0201 (15) | 0.0163 (15) | 0.0050 (12) | 0.0087 (12) | 0.0047 (12) |
C3 | 0.0182 (15) | 0.0203 (16) | 0.0206 (16) | 0.0032 (12) | 0.0091 (12) | 0.0063 (13) |
C4 | 0.0153 (14) | 0.0249 (17) | 0.0224 (16) | 0.0032 (13) | 0.0078 (12) | 0.0081 (13) |
C5 | 0.0254 (17) | 0.0235 (17) | 0.0170 (15) | 0.0009 (14) | 0.0076 (13) | 0.0048 (13) |
C6 | 0.0160 (15) | 0.0250 (17) | 0.036 (2) | 0.0033 (13) | 0.0063 (14) | 0.0134 (15) |
C7 | 0.0210 (16) | 0.0210 (16) | 0.0201 (16) | 0.0041 (13) | 0.0080 (13) | 0.0023 (13) |
C8 | 0.0180 (15) | 0.0207 (16) | 0.0254 (17) | 0.0039 (13) | 0.0111 (13) | 0.0059 (13) |
C9 | 0.0191 (15) | 0.0167 (15) | 0.0245 (17) | 0.0041 (12) | 0.0114 (13) | 0.0039 (13) |
C10 | 0.0281 (18) | 0.0195 (16) | 0.0280 (18) | 0.0042 (14) | 0.0099 (15) | 0.0072 (14) |
C11 | 0.0255 (17) | 0.0222 (16) | 0.0291 (18) | 0.0111 (14) | 0.0152 (14) | 0.0129 (14) |
C12 | 0.0191 (15) | 0.0205 (16) | 0.0208 (16) | 0.0016 (13) | 0.0091 (13) | 0.0007 (13) |
C13 | 0.0135 (14) | 0.0208 (15) | 0.0172 (15) | 0.0001 (12) | 0.0047 (12) | 0.0006 (12) |
C14 | 0.0197 (15) | 0.0177 (15) | 0.0228 (16) | 0.0041 (12) | 0.0103 (13) | 0.0048 (13) |
C15 | 0.0197 (15) | 0.0217 (16) | 0.0198 (16) | 0.0043 (13) | 0.0103 (13) | 0.0056 (13) |
C16 | 0.0273 (17) | 0.0222 (16) | 0.0217 (16) | 0.0094 (14) | 0.0115 (13) | 0.0114 (13) |
C17 | 0.0314 (18) | 0.0261 (17) | 0.0176 (15) | 0.0125 (14) | 0.0124 (14) | 0.0095 (13) |
C18 | 0.0166 (15) | 0.0228 (16) | 0.0202 (16) | 0.0051 (13) | 0.0062 (12) | 0.0018 (13) |
C19 | 0.0180 (15) | 0.0181 (15) | 0.0180 (15) | 0.0044 (12) | 0.0039 (12) | 0.0042 (12) |
C20 | 0.0238 (16) | 0.0178 (15) | 0.0146 (15) | 0.0015 (13) | 0.0037 (12) | 0.0031 (12) |
C21 | 0.0173 (14) | 0.0154 (14) | 0.0174 (15) | 0.0048 (12) | 0.0044 (12) | 0.0038 (12) |
C22 | 0.0201 (15) | 0.0162 (15) | 0.0234 (16) | 0.0073 (12) | 0.0106 (13) | 0.0049 (12) |
C23 | 0.0179 (14) | 0.0156 (14) | 0.0189 (15) | 0.0051 (12) | 0.0066 (12) | 0.0044 (12) |
C24 | 0.0197 (15) | 0.0199 (16) | 0.0218 (16) | 0.0081 (13) | 0.0082 (13) | 0.0051 (13) |
C25 | 0.0229 (16) | 0.0236 (16) | 0.0196 (15) | 0.0112 (13) | 0.0124 (13) | 0.0084 (13) |
C26 | 0.0209 (15) | 0.0131 (14) | 0.0192 (15) | 0.0035 (12) | 0.0046 (12) | 0.0028 (12) |
C27 | 0.0178 (14) | 0.0133 (14) | 0.0198 (15) | 0.0030 (11) | 0.0081 (12) | 0.0058 (12) |
C28 | 0.0191 (15) | 0.0155 (15) | 0.0211 (15) | 0.0034 (12) | 0.0082 (12) | 0.0059 (12) |
C29 | 0.0203 (15) | 0.0211 (16) | 0.0198 (15) | 0.0064 (13) | 0.0102 (13) | 0.0060 (13) |
C30 | 0.0182 (15) | 0.0118 (14) | 0.0250 (16) | 0.0020 (11) | 0.0077 (12) | 0.0067 (12) |
C31 | 0.0164 (15) | 0.0129 (14) | 0.0309 (18) | 0.0043 (12) | 0.0062 (13) | 0.0032 (13) |
C32 | 0.0187 (15) | 0.0185 (15) | 0.0243 (17) | 0.0079 (13) | 0.0069 (13) | 0.0043 (13) |
C33 | 0.0194 (15) | 0.0168 (15) | 0.0223 (16) | 0.0075 (12) | 0.0061 (12) | 0.0080 (12) |
C34 | 0.0194 (15) | 0.0245 (17) | 0.0189 (15) | 0.0051 (13) | 0.0067 (12) | 0.0070 (13) |
C35 | 0.0208 (15) | 0.0198 (16) | 0.0168 (15) | 0.0053 (13) | 0.0040 (12) | 0.0041 (12) |
C36 | 0.0177 (15) | 0.0167 (15) | 0.0212 (16) | 0.0080 (12) | 0.0047 (12) | 0.0071 (12) |
Geometric parameters (Å, º) top
Mo1—O13 | 1.678 (2) | N12—C17 | 1.445 (4) |
Mo1—O15 | 1.921 (2) | N13—C19 | 1.378 (4) |
Mo1—O16 | 1.937 (2) | N13—C21 | 1.447 (4) |
Mo1—O1W | 2.266 (2) | N13—C20 | 1.447 (4) |
Mo1—Cl1 | 2.390 (2) | N14—C24 | 1.361 (4) |
Mo1—Cl2 | 2.485 (1) | N14—C22 | 1.432 (4) |
Mo1—Mo2 | 2.5680 (4) | N14—C21 | 1.444 (4) |
Mo2—O14 | 1.680 (2) | N15—C19 | 1.370 (4) |
Mo2—O15 | 1.933 (2) | N15—C23 | 1.441 (4) |
Mo2—O16 | 1.938 (2) | N15—C26 | 1.446 (4) |
Mo2—O2W | 2.353 (2) | N16—C24 | 1.363 (4) |
Mo2—Cl3 | 2.485 (1) | N16—C25 | 1.443 (4) |
Mo2—Cl4 | 2.462 (1) | N16—C23 | 1.450 (4) |
O1—C1 | 1.223 (4) | N17—C30 | 1.365 (4) |
O2—C4 | 1.213 (4) | N17—C27 | 1.447 (4) |
O3—C7 | 1.220 (5) | N17—C26 | 1.450 (4) |
O4—C10 | 1.216 (5) | N18—C29 | 1.368 (4) |
O5—C13 | 1.224 (4) | N18—C25 | 1.439 (4) |
O6—C16 | 1.223 (4) | N18—C27 | 1.446 (4) |
O7—C19 | 1.219 (4) | N19—C30 | 1.361 (4) |
O8—C24 | 1.222 (4) | N19—C31 | 1.444 (4) |
O9—C30 | 1.223 (4) | N19—C28 | 1.448 (4) |
O10—C29 | 1.222 (4) | N20—C29 | 1.370 (4) |
O11—C32 | 1.226 (4) | N20—C34 | 1.445 (4) |
O12—C35 | 1.220 (4) | N20—C28 | 1.450 (4) |
O1W—H11 | 0.84 | N21—C32 | 1.367 (5) |
O1W—H12 | 0.84 | N21—C33 | 1.446 (4) |
O2W—H21 | 0.83 | N21—C31 | 1.448 (4) |
O2W—H22 | 0.83 | N22—C35 | 1.369 (4) |
O3W—H31 | 0.84 | N22—C34 | 1.438 (4) |
O3W—H32 | 0.84 | N22—C33 | 1.446 (4) |
O4W—H41 | 0.84 | N23—C32 | 1.368 (4) |
O4W—H42 | 0.84 | N23—C36 | 1.438 (4) |
O5W—H51 | 0.85 | N23—C22ii | 1.443 (4) |
O5W—H52 | 0.84 | N24—C35 | 1.360 (4) |
O6W—H61 | 0.84 | N24—C20ii | 1.445 (4) |
O6W—H62 | 0.85 | N24—C36 | 1.452 (4) |
O7W—H71 | 0.88 | C2—C3 | 1.548 (5) |
O7W—H72 | 0.87 | C2—H2 | 0.9600 |
O8W—H81 | 0.85 | C3—H3 | 0.9600 |
O8W—H82 | 0.84 | C5—H5A | 0.9600 |
O9W—H91 | 0.84 | C5—H5B | 0.9600 |
O9W—H92 | 0.84 | C6—H6A | 0.9600 |
O10W—H101 | 0.84 | C6—H6B | 0.9600 |
O10W—H102 | 0.83 | C8—C9 | 1.561 (5) |
O11W—H111 | 0.84 | C8—H8 | 0.9600 |
O11W—H112 | 0.84 | C9—H9 | 0.9600 |
O12W—H121 | 0.84 | C11—H11A | 0.9600 |
O12W—H122 | 0.83 | C11—H11B | 0.9600 |
N1—C1 | 1.370 (4) | C12—H12A | 0.9600 |
N1—C17i | 1.444 (4) | C12—H12B | 0.9600 |
N1—C2 | 1.449 (4) | C14—C15 | 1.549 (5) |
N2—C4 | 1.361 (5) | C14—H14 | 0.9600 |
N2—C2 | 1.442 (4) | C15—H15 | 0.9600 |
N2—C18i | 1.452 (4) | C17—N1i | 1.444 (4) |
N3—C1 | 1.355 (5) | C17—H17A | 0.9600 |
N3—C5 | 1.443 (4) | C17—H17B | 0.9600 |
N3—C3 | 1.444 (4) | C18—N2i | 1.452 (4) |
N4—C4 | 1.375 (4) | C18—H18A | 0.9600 |
N4—C6 | 1.445 (5) | C18—H18B | 0.9600 |
N4—C3 | 1.450 (4) | C20—N24ii | 1.445 (4) |
N5—C7 | 1.368 (4) | C20—H20A | 0.9600 |
N5—C8 | 1.444 (5) | C20—H20B | 0.9600 |
N5—C5 | 1.447 (4) | C21—C23 | 1.551 (4) |
N6—C10 | 1.365 (5) | C21—H21A | 0.9600 |
N6—C6 | 1.443 (4) | C22—N23ii | 1.443 (4) |
N6—C8 | 1.446 (5) | C22—H22A | 0.9600 |
N7—C7 | 1.358 (5) | C22—H22B | 0.9600 |
N7—C9 | 1.440 (4) | C23—H23 | 0.9600 |
N7—C12 | 1.449 (4) | C25—H25A | 0.9600 |
N8—C10 | 1.363 (5) | C25—H25B | 0.9600 |
N8—C11 | 1.438 (4) | C26—H26A | 0.9600 |
N8—C9 | 1.446 (4) | C26—H26B | 0.9600 |
N9—C13 | 1.361 (5) | C27—C28 | 1.555 (5) |
N9—C14 | 1.439 (5) | C27—H27 | 0.9600 |
N9—C12 | 1.455 (4) | C28—H28 | 0.9600 |
N10—C16 | 1.364 (4) | C31—H31A | 0.9600 |
N10—C11 | 1.453 (4) | C31—H31B | 0.9600 |
N10—C14 | 1.457 (4) | C33—C36 | 1.548 (5) |
N11—C13 | 1.369 (4) | C33—H33 | 0.9600 |
N11—C18 | 1.442 (4) | C34—H34A | 0.9600 |
N11—C15 | 1.459 (5) | C34—H34B | 0.9600 |
N12—C16 | 1.362 (5) | C36—H36 | 0.9600 |
N12—C15 | 1.443 (4) | | |
| | | |
O13—Mo1—O15 | 107.3 (1) | N6—C6—N4 | 114.7 (3) |
O13—Mo1—O16 | 106.3 (1) | N6—C6—H6A | 108.6 |
O13—Mo1—O1W | 161.5 (1) | N4—C6—H6A | 108.6 |
O13—Mo1—Cl1 | 90.0 (1) | N6—C6—H6B | 108.6 |
O13—Mo1—Cl2 | 91.2 (1) | N4—C6—H6B | 108.6 |
O15—Mo1—O16 | 92.9 (1) | H6A—C6—H6B | 107.6 |
O15—Mo1—O1W | 86.0 (1) | O3—C7—N7 | 125.6 (3) |
O15—Mo1—Cl1 | 162.4 (1) | O3—C7—N5 | 126.1 (3) |
O15—Mo1—Cl2 | 85.9 (1) | N7—C7—N5 | 108.3 (3) |
O16—Mo1—O1W | 85.3 (1) | N5—C8—N6 | 113.5 (3) |
O16—Mo1—Cl1 | 85.0 (1) | N5—C8—C9 | 103.0 (3) |
O16—Mo1—Cl2 | 162.0 (1) | N6—C8—C9 | 103.1 (3) |
O1W—Mo1—Cl1 | 76.42 (7) | N5—C8—H8 | 112.2 |
O1W—Mo1—Cl2 | 76.78 (7) | N6—C8—H8 | 112.2 |
Cl1—Mo1—Cl2 | 90.72 (4) | C9—C8—H8 | 112.2 |
O13—Mo1—Mo2 | 99.00 (9) | N7—C9—N8 | 114.8 (3) |
O15—Mo1—Mo2 | 48.42 (7) | N7—C9—C8 | 102.9 (3) |
O16—Mo1—Mo2 | 48.52 (7) | N8—C9—C8 | 102.7 (3) |
O1W—Mo1—Mo2 | 99.44 (6) | N7—C9—H9 | 111.9 |
Cl1—Mo1—Mo2 | 133.37 (4) | N8—C9—H9 | 111.9 |
Cl2—Mo1—Mo2 | 134.26 (2) | C8—C9—H9 | 111.9 |
O14—Mo2—O15 | 104.8 (1) | O4—C10—N8 | 126.0 (4) |
O14—Mo2—O16 | 108.4 (1) | O4—C10—N6 | 126.1 (3) |
O14—Mo2—O2W | 166.1 (1) | N8—C10—N6 | 107.9 (3) |
O14—Mo2—Cl3 | 91.4 (1) | N8—C11—N10 | 113.6 (3) |
O14—Mo2—Cl4 | 92.8 (1) | N8—C11—H11A | 108.9 |
O15—Mo2—O16 | 92.5 (1) | N10—C11—H11A | 108.9 |
O15—Mo2—O2W | 85.4 (1) | N8—C11—H11B | 108.9 |
O15—Mo2—Cl3 | 163.0 (1) | N10—C11—H11B | 108.9 |
O15—Mo2—Cl4 | 82.2 (1) | H11A—C11—H11B | 107.7 |
O16—Mo2—O2W | 80.0 (1) | N7—C12—N9 | 113.3 (3) |
O16—Mo2—Cl3 | 87.2 (1) | N7—C12—H12A | 108.9 |
O16—Mo2—Cl4 | 158.8 (1) | N9—C12—H12A | 108.9 |
O2W—Mo2—Cl3 | 77.8 (1) | N7—C12—H12B | 108.9 |
O2W—Mo2—Cl4 | 79.1 (1) | N9—C12—H12B | 108.9 |
Cl3—Mo2—Cl4 | 91.95 (4) | H12A—C12—H12B | 107.7 |
O14—Mo2—Mo1 | 98.75 (9) | O5—C13—N9 | 125.9 (3) |
O15—Mo2—Mo1 | 48.01 (7) | O5—C13—N11 | 125.2 (3) |
O16—Mo2—Mo1 | 48.48 (7) | N9—C13—N11 | 108.8 (3) |
O2W—Mo2—Mo1 | 95.09 (6) | N9—C14—N10 | 115.5 (3) |
Cl4—Mo2—Mo1 | 130.21 (3) | N9—C14—C15 | 103.1 (3) |
Cl3—Mo2—Mo1 | 135.56 (3) | N10—C14—C15 | 102.9 (3) |
Mo1—O15—Mo2 | 83.57 (9) | N9—C14—H14 | 111.5 |
Mo1—O16—Mo2 | 83.00 (9) | N10—C14—H14 | 111.5 |
Mo1—O1W—H11 | 113.4 | C15—C14—H14 | 111.5 |
Mo1—O1W—H12 | 113.0 | N12—C15—N11 | 115.0 (3) |
H11—O1W—H12 | 106.8 | N12—C15—C14 | 103.4 (3) |
Mo2—O2W—H21 | 118.6 | N11—C15—C14 | 103.5 (3) |
Mo2—O2W—H22 | 118.5 | N12—C15—H15 | 111.5 |
H21—O2W—H22 | 108.8 | N11—C15—H15 | 111.5 |
H31—O3W—H32 | 107.7 | C14—C15—H15 | 111.5 |
H41—O4W—H42 | 107.6 | O6—C16—N12 | 125.0 (3) |
H51—O5W—H52 | 105.3 | O6—C16—N10 | 126.4 (3) |
H61—O6W—H62 | 106.4 | N12—C16—N10 | 108.6 (3) |
H71—O7W—H72 | 101.8 | N1i—C17—N12 | 113.7 (3) |
H81—O8W—H82 | 106.0 | N1i—C17—H17A | 108.8 |
H91—O9W—H92 | 106.0 | N12—C17—H17A | 108.8 |
H101—O10W—H102 | 108.5 | N1i—C17—H17B | 108.8 |
H111—O11W—H112 | 106.4 | N12—C17—H17B | 108.8 |
H121—O12W—H122 | 107.5 | H17A—C17—H17B | 107.7 |
C1—N1—C17i | 122.1 (3) | N11—C18—N2i | 114.4 (3) |
C1—N1—C2 | 112.0 (3) | N11—C18—H18A | 108.7 |
C17i—N1—C2 | 122.6 (3) | N2i—C18—H18A | 108.7 |
C4—N2—C2 | 113.1 (3) | N11—C18—H18B | 108.7 |
C4—N2—C18i | 122.8 (3) | N2i—C18—H18B | 108.7 |
C2—N2—C18i | 123.6 (3) | H18A—C18—H18B | 107.6 |
C1—N3—C5 | 123.0 (3) | O7—C19—N15 | 126.6 (3) |
C1—N3—C3 | 113.1 (3) | O7—C19—N13 | 125.6 (3) |
C5—N3—C3 | 123.5 (3) | N15—C19—N13 | 107.8 (3) |
C4—N4—C6 | 122.9 (3) | N24ii—C20—N13 | 113.4 (3) |
C4—N4—C3 | 112.2 (3) | N24ii—C20—H20A | 108.9 |
C6—N4—C3 | 122.8 (3) | N13—C20—H20A | 108.9 |
C7—N5—C8 | 112.4 (3) | N24ii—C20—H20B | 108.9 |
C7—N5—C5 | 122.0 (3) | N13—C20—H20B | 108.9 |
C8—N5—C5 | 122.5 (3) | H20A—C20—H20B | 107.7 |
C10—N6—C6 | 123.6 (3) | N14—C21—N13 | 115.4 (3) |
C10—N6—C8 | 112.9 (3) | N14—C21—C23 | 103.2 (3) |
C6—N6—C8 | 123.5 (3) | N13—C21—C23 | 103.5 (2) |
C7—N7—C9 | 113.2 (3) | N14—C21—H21A | 111.4 |
C7—N7—C12 | 121.7 (3) | N13—C21—H21A | 111.4 |
C9—N7—C12 | 124.4 (3) | C23—C21—H21A | 111.4 |
C10—N8—C11 | 123.0 (3) | N14—C22—N23ii | 114.0 (3) |
C10—N8—C9 | 113.3 (3) | N14—C22—H22A | 108.8 |
C11—N8—C9 | 123.7 (3) | N23ii—C22—H22A | 108.8 |
C13—N9—C14 | 112.9 (3) | N14—C22—H22B | 108.8 |
C13—N9—C12 | 123.4 (3) | N23ii—C22—H22B | 108.8 |
C14—N9—C12 | 123.7 (3) | H22A—C22—H22B | 107.7 |
C16—N10—C11 | 121.8 (3) | N15—C23—N16 | 115.5 (3) |
C16—N10—C14 | 112.0 (3) | N15—C23—C21 | 103.3 (3) |
C11—N10—C14 | 124.0 (3) | N16—C23—C21 | 102.8 (3) |
C13—N11—C18 | 121.1 (3) | N15—C23—H23 | 111.5 |
C13—N11—C15 | 111.3 (3) | N16—C23—H23 | 111.5 |
C18—N11—C15 | 124.5 (3) | C21—C23—H23 | 111.5 |
C16—N12—C15 | 112.6 (3) | O8—C24—N14 | 125.8 (3) |
C16—N12—C17 | 123.0 (3) | O8—C24—N16 | 126.3 (3) |
C15—N12—C17 | 124.3 (3) | N14—C24—N16 | 107.9 (3) |
C19—N13—C21 | 112.0 (3) | N18—C25—N16 | 113.9 (3) |
C19—N13—C20 | 121.1 (3) | N18—C25—H25A | 108.8 |
C21—N13—C20 | 122.3 (3) | N16—C25—H25A | 108.8 |
C24—N14—C22 | 122.9 (3) | N18—C25—H25B | 108.8 |
C24—N14—C21 | 113.0 (3) | N16—C25—H25B | 108.8 |
C22—N14—C21 | 123.8 (3) | H25A—C25—H25B | 107.7 |
C19—N15—C23 | 112.7 (3) | N15—C26—N17 | 113.6 (3) |
C19—N15—C26 | 123.1 (3) | N15—C26—H26A | 108.8 |
C23—N15—C26 | 123.1 (3) | N17—C26—H26A | 108.8 |
C24—N16—C25 | 122.0 (3) | N15—C26—H26B | 108.8 |
C24—N16—C23 | 112.8 (3) | N17—C26—H26B | 108.8 |
C25—N16—C23 | 124.7 (3) | H26A—C26—H26B | 107.7 |
C30—N17—C27 | 112.2 (3) | N18—C27—N17 | 114.6 (3) |
C30—N17—C26 | 122.7 (3) | N18—C27—C28 | 103.1 (3) |
C27—N17—C26 | 124.8 (3) | N17—C27—C28 | 103.5 (3) |
C29—N18—C25 | 123.2 (3) | N18—C27—H27 | 111.7 |
C29—N18—C27 | 112.7 (3) | N17—C27—H27 | 111.7 |
C25—N18—C27 | 123.3 (3) | C28—C27—H27 | 111.7 |
C30—N19—C31 | 122.4 (3) | N19—C28—N20 | 114.6 (3) |
C30—N19—C28 | 112.9 (3) | N19—C28—C27 | 102.6 (3) |
C31—N19—C28 | 124.5 (3) | N20—C28—C27 | 103.5 (3) |
C29—N20—C34 | 122.0 (3) | N19—C28—H28 | 111.8 |
C29—N20—C28 | 112.2 (3) | N20—C28—H28 | 111.8 |
C34—N20—C28 | 124.4 (3) | C27—C28—H28 | 111.8 |
C32—N21—C33 | 112.0 (3) | O10—C29—N18 | 125.5 (3) |
C32—N21—C31 | 121.6 (3) | O10—C29—N20 | 126.0 (3) |
C33—N21—C31 | 123.2 (3) | N18—C29—N20 | 108.5 (3) |
C35—N22—C34 | 123.4 (3) | O9—C30—N19 | 126.0 (3) |
C35—N22—C33 | 112.6 (3) | O9—C30—N17 | 125.6 (3) |
C34—N22—C33 | 124.0 (3) | N19—C30—N17 | 108.4 (3) |
C32—N23—C36 | 112.3 (3) | N19—C31—N21 | 113.2 (3) |
C32—N23—C22ii | 122.1 (3) | N19—C31—H31A | 108.9 |
C36—N23—C22ii | 122.2 (3) | N21—C31—H31A | 108.9 |
C35—N24—C20ii | 123.4 (3) | N19—C31—H31B | 108.9 |
C35—N24—C36 | 112.5 (3) | N21—C31—H31B | 108.9 |
C20ii—N24—C36 | 123.1 (3) | H31A—C31—H31B | 107.8 |
O1—C1—N3 | 126.6 (3) | O11—C32—N21 | 126.2 (3) |
O1—C1—N1 | 125.1 (3) | O11—C32—N23 | 125.3 (3) |
N3—C1—N1 | 108.3 (3) | N21—C32—N23 | 108.5 (3) |
N2—C2—N1 | 114.6 (3) | N22—C33—N21 | 115.1 (3) |
N2—C2—C3 | 103.3 (3) | N22—C33—C36 | 103.2 (3) |
N1—C2—C3 | 103.5 (3) | N21—C33—C36 | 103.4 (3) |
N2—C2—H2 | 111.6 | N22—C33—H33 | 111.5 |
N1—C2—H2 | 111.6 | N21—C33—H33 | 111.5 |
C3—C2—H2 | 111.6 | C36—C33—H33 | 111.5 |
N3—C3—N4 | 115.0 (3) | N22—C34—N20 | 114.4 (3) |
N3—C3—C2 | 102.9 (3) | N22—C34—H34A | 108.7 |
N4—C3—C2 | 103.2 (3) | N20—C34—H34A | 108.7 |
N3—C3—H3 | 111.7 | N22—C34—H34B | 108.7 |
N4—C3—H3 | 111.7 | N20—C34—H34B | 108.7 |
C2—C3—H3 | 111.7 | H34A—C34—H34B | 107.6 |
O2—C4—N2 | 125.7 (3) | O12—C35—N24 | 126.2 (3) |
O2—C4—N4 | 126.3 (3) | O12—C35—N22 | 125.5 (3) |
N2—C4—N4 | 107.9 (3) | N24—C35—N22 | 108.2 (3) |
N3—C5—N5 | 113.0 (3) | N23—C36—N24 | 114.2 (3) |
N3—C5—H5A | 109.0 | N23—C36—C33 | 103.6 (3) |
N5—C5—H5A | 109.0 | N24—C36—C33 | 103.2 (3) |
N3—C5—H5B | 109.0 | N23—C36—H36 | 111.7 |
N5—C5—H5B | 109.0 | N24—C36—H36 | 111.7 |
H5A—C5—H5B | 107.8 | C33—C36—H36 | 111.7 |
| | | |
O13—Mo1—Mo2—O14 | −3.10 (13) | C11—N10—C14—N9 | 77.9 (4) |
O15—Mo1—Mo2—O14 | 102.11 (13) | C16—N10—C14—C15 | −7.3 (4) |
O16—Mo1—Mo2—O14 | −106.88 (13) | C11—N10—C14—C15 | −170.5 (3) |
O1W—Mo1—Mo2—O14 | 178.12 (11) | C16—N12—C15—N11 | 109.7 (3) |
Cl1—Mo1—Mo2—O14 | −101.69 (10) | C17—N12—C15—N11 | −72.7 (4) |
Cl2—Mo1—Mo2—O14 | 97.43 (10) | C16—N12—C15—C14 | −2.3 (4) |
O13—Mo1—Mo2—O15 | −105.22 (13) | C17—N12—C15—C14 | 175.3 (3) |
O16—Mo1—Mo2—O15 | 151.01 (14) | C13—N11—C15—N12 | −118.9 (3) |
O1W—Mo1—Mo2—O15 | 76.01 (11) | C18—N11—C15—N12 | 80.9 (4) |
Cl1—Mo1—Mo2—O15 | 156.20 (11) | C13—N11—C15—C14 | −6.9 (3) |
Cl2—Mo1—Mo2—O15 | −4.68 (10) | C18—N11—C15—C14 | −167.1 (3) |
O13—Mo1—Mo2—O16 | 103.78 (14) | N9—C14—C15—N12 | 126.0 (3) |
O15—Mo1—Mo2—O16 | −151.01 (14) | N10—C14—C15—N12 | 5.5 (3) |
O1W—Mo1—Mo2—O16 | −75.00 (12) | N9—C14—C15—N11 | 5.7 (3) |
Cl1—Mo1—Mo2—O16 | 5.19 (10) | N10—C14—C15—N11 | −114.8 (3) |
Cl2—Mo1—Mo2—O16 | −155.69 (10) | C15—N12—C16—O6 | 176.0 (3) |
O13—Mo1—Mo2—O2W | 175.63 (12) | C17—N12—C16—O6 | −1.6 (6) |
O15—Mo1—Mo2—O2W | −79.15 (11) | C15—N12—C16—N10 | −2.2 (4) |
O16—Mo1—Mo2—O2W | 71.86 (11) | C17—N12—C16—N10 | −179.8 (3) |
O1W—Mo1—Mo2—O2W | −3.14 (9) | C11—N10—C16—O6 | −8.3 (5) |
Cl1—Mo1—Mo2—O2W | 77.05 (8) | C14—N10—C16—O6 | −172.0 (3) |
Cl2—Mo1—Mo2—O2W | −83.83 (7) | C11—N10—C16—N12 | 169.9 (3) |
O13—Mo1—Mo2—Cl4 | −104.29 (10) | C14—N10—C16—N12 | 6.2 (4) |
O15—Mo1—Mo2—Cl4 | 0.93 (10) | C16—N12—C17—N1i | −101.4 (4) |
O16—Mo1—Mo2—Cl4 | 151.93 (10) | C15—N12—C17—N1i | 81.3 (4) |
O1W—Mo1—Mo2—Cl4 | 76.93 (8) | C13—N11—C18—N2i | 113.0 (3) |
Cl1—Mo1—Mo2—Cl4 | 157.12 (6) | C15—N11—C18—N2i | −88.7 (4) |
Cl2—Mo1—Mo2—Cl4 | −3.76 (5) | C23—N15—C19—O7 | −172.9 (3) |
O13—Mo1—Mo2—Cl3 | 97.96 (10) | C26—N15—C19—O7 | −4.0 (5) |
O15—Mo1—Mo2—Cl3 | −156.82 (10) | C23—N15—C19—N13 | 7.3 (4) |
O16—Mo1—Mo2—Cl3 | −5.81 (10) | C26—N15—C19—N13 | 176.1 (3) |
O1W—Mo1—Mo2—Cl3 | −80.81 (7) | C21—N13—C19—O7 | 171.2 (3) |
Cl1—Mo1—Mo2—Cl3 | −0.62 (6) | C20—N13—C19—O7 | 14.9 (5) |
Cl2—Mo1—Mo2—Cl3 | −161.50 (5) | C21—N13—C19—N15 | −9.0 (4) |
O13—Mo1—O15—Mo2 | 86.69 (12) | C20—N13—C19—N15 | −165.2 (3) |
O16—Mo1—O15—Mo2 | −21.32 (10) | C19—N13—C20—N24ii | −114.8 (3) |
O1W—Mo1—O15—Mo2 | −106.36 (9) | C21—N13—C20—N24ii | 91.4 (4) |
Cl1—Mo1—O15—Mo2 | −103.8 (3) | C24—N14—C21—N13 | −113.1 (3) |
Cl2—Mo1—O15—Mo2 | 176.64 (7) | C22—N14—C21—N13 | 72.9 (4) |
O14—Mo2—O15—Mo1 | −88.48 (11) | C24—N14—C21—C23 | −1.0 (4) |
O16—Mo2—O15—Mo1 | 21.30 (10) | C22—N14—C21—C23 | −175.0 (3) |
O2W—Mo2—O15—Mo1 | 101.07 (9) | C19—N13—C21—N14 | 118.9 (3) |
Cl4—Mo2—O15—Mo1 | −179.29 (8) | C20—N13—C21—N14 | −85.2 (4) |
Cl3—Mo2—O15—Mo1 | 110.0 (2) | C19—N13—C21—C23 | 6.9 (3) |
O13—Mo1—O16—Mo2 | −87.69 (12) | C20—N13—C21—C23 | 162.8 (3) |
O15—Mo1—O16—Mo2 | 21.29 (10) | C24—N14—C22—N23ii | 108.3 (4) |
O1W—Mo1—O16—Mo2 | 107.04 (9) | C21—N14—C22—N23ii | −78.3 (4) |
Cl1—Mo1—O16—Mo2 | −176.21 (8) | C19—N15—C23—N16 | −114.3 (3) |
Cl2—Mo1—O16—Mo2 | 107.1 (2) | C26—N15—C23—N16 | 76.9 (4) |
O14—Mo2—O16—Mo1 | 85.38 (11) | C19—N15—C23—C21 | −2.9 (3) |
O15—Mo2—O16—Mo1 | −21.14 (10) | C26—N15—C23—C21 | −171.7 (3) |
O2W—Mo2—O16—Mo1 | −106.03 (9) | C24—N16—C23—N15 | 117.1 (3) |
Cl4—Mo2—O16—Mo1 | −95.8 (2) | C25—N16—C23—N15 | −70.6 (4) |
Cl3—Mo2—O16—Mo1 | 175.93 (7) | C24—N16—C23—C21 | 5.3 (4) |
C5—N3—C1—O1 | −3.9 (6) | C25—N16—C23—C21 | 177.7 (3) |
C3—N3—C1—O1 | −177.7 (3) | N14—C21—C23—N15 | −123.0 (3) |
C5—N3—C1—N1 | 176.0 (3) | N13—C21—C23—N15 | −2.4 (3) |
C3—N3—C1—N1 | 2.3 (4) | N14—C21—C23—N16 | −2.5 (3) |
C17i—N1—C1—O1 | 16.0 (5) | N13—C21—C23—N16 | 118.2 (3) |
C2—N1—C1—O1 | 176.1 (3) | C22—N14—C24—O8 | 0.3 (5) |
C17i—N1—C1—N3 | −164.0 (3) | C21—N14—C24—O8 | −173.7 (3) |
C2—N1—C1—N3 | −3.9 (4) | C22—N14—C24—N16 | 178.4 (3) |
C4—N2—C2—N1 | −112.9 (3) | C21—N14—C24—N16 | 4.4 (4) |
C18i—N2—C2—N1 | 74.9 (4) | C25—N16—C24—O8 | −0.7 (6) |
C4—N2—C2—C3 | −1.1 (4) | C23—N16—C24—O8 | 171.9 (3) |
C18i—N2—C2—C3 | −173.3 (3) | C25—N16—C24—N14 | −178.8 (3) |
C1—N1—C2—N2 | 115.5 (3) | C23—N16—C24—N14 | −6.2 (4) |
C17i—N1—C2—N2 | −84.5 (4) | C29—N18—C25—N16 | 98.8 (4) |
C1—N1—C2—C3 | 3.8 (3) | C27—N18—C25—N16 | −91.9 (4) |
C17i—N1—C2—C3 | 163.7 (3) | C24—N16—C25—N18 | −103.9 (4) |
C1—N3—C3—N4 | −111.4 (3) | C23—N16—C25—N18 | 84.5 (4) |
C5—N3—C3—N4 | 75.0 (4) | C19—N15—C26—N17 | 101.1 (4) |
C1—N3—C3—C2 | 0.1 (4) | C23—N15—C26—N17 | −91.2 (4) |
C5—N3—C3—C2 | −173.6 (3) | C30—N17—C26—N15 | −102.0 (4) |
C4—N4—C3—N3 | 116.0 (3) | C27—N17—C26—N15 | 85.4 (4) |
C6—N4—C3—N3 | −80.2 (4) | C29—N18—C27—N17 | −112.1 (3) |
C4—N4—C3—C2 | 4.7 (4) | C25—N18—C27—N17 | 77.6 (4) |
C6—N4—C3—C2 | 168.5 (3) | C29—N18—C27—C28 | −0.4 (4) |
N2—C2—C3—N3 | −122.0 (3) | C25—N18—C27—C28 | −170.7 (3) |
N1—C2—C3—N3 | −2.2 (3) | C30—N17—C27—N18 | 115.2 (3) |
N2—C2—C3—N4 | −2.0 (3) | C26—N17—C27—N18 | −71.5 (4) |
N1—C2—C3—N4 | 117.8 (3) | C30—N17—C27—C28 | 3.7 (3) |
C2—N2—C4—O2 | −173.6 (3) | C26—N17—C27—C28 | 177.0 (3) |
C18i—N2—C4—O2 | −1.3 (5) | C30—N19—C28—N20 | −115.8 (3) |
C2—N2—C4—N4 | 4.1 (4) | C31—N19—C28—N20 | 69.6 (4) |
C18i—N2—C4—N4 | 176.3 (3) | C30—N19—C28—C27 | −4.4 (3) |
C6—N4—C4—O2 | 8.3 (6) | C31—N19—C28—C27 | −179.0 (3) |
C3—N4—C4—O2 | 172.1 (3) | C29—N20—C28—N19 | 111.0 (3) |
C6—N4—C4—N2 | −169.3 (3) | C34—N20—C28—N19 | −82.2 (4) |
C3—N4—C4—N2 | −5.5 (4) | C29—N20—C28—C27 | 0.0 (4) |
C1—N3—C5—N5 | 103.3 (4) | C34—N20—C28—C27 | 166.8 (3) |
C3—N3—C5—N5 | −83.7 (4) | N18—C27—C28—N19 | −119.3 (3) |
C7—N5—C5—N3 | −109.1 (4) | N17—C27—C28—N19 | 0.4 (3) |
C8—N5—C5—N3 | 92.4 (4) | N18—C27—C28—N20 | 0.2 (3) |
C10—N6—C6—N4 | 99.2 (4) | N17—C27—C28—N20 | 120.0 (3) |
C8—N6—C6—N4 | −83.4 (4) | C25—N18—C29—O10 | −9.4 (6) |
C4—N4—C6—N6 | −108.8 (4) | C27—N18—C29—O10 | −179.7 (3) |
C3—N4—C6—N6 | 89.1 (4) | C25—N18—C29—N20 | 170.7 (3) |
C9—N7—C7—O3 | −175.9 (3) | C27—N18—C29—N20 | 0.4 (4) |
C12—N7—C7—O3 | −5.3 (5) | C34—N20—C29—O10 | 12.6 (5) |
C9—N7—C7—N5 | 2.7 (4) | C28—N20—C29—O10 | 179.8 (3) |
C12—N7—C7—N5 | 173.3 (3) | C34—N20—C29—N18 | −167.5 (3) |
C8—N5—C7—O3 | 173.4 (3) | C28—N20—C29—N18 | −0.3 (4) |
C5—N5—C7—O3 | 12.9 (6) | C31—N19—C30—O9 | 3.8 (5) |
C8—N5—C7—N7 | −5.1 (4) | C28—N19—C30—O9 | −170.9 (3) |
C5—N5—C7—N7 | −165.6 (3) | C31—N19—C30—N17 | −178.4 (3) |
C7—N5—C8—N6 | 115.9 (3) | C28—N19—C30—N17 | 6.9 (4) |
C5—N5—C8—N6 | −83.7 (4) | C27—N17—C30—O9 | 171.3 (3) |
C7—N5—C8—C9 | 5.2 (4) | C26—N17—C30—O9 | −2.2 (5) |
C5—N5—C8—C9 | 165.6 (3) | C27—N17—C30—N19 | −6.5 (4) |
C10—N6—C8—N5 | −107.0 (3) | C26—N17—C30—N19 | 180.0 (3) |
C6—N6—C8—N5 | 75.4 (4) | C30—N19—C31—N21 | 106.2 (4) |
C10—N6—C8—C9 | 3.7 (4) | C28—N19—C31—N21 | −79.7 (4) |
C6—N6—C8—C9 | −173.9 (3) | C32—N21—C31—N19 | −107.8 (4) |
C7—N7—C9—N8 | −110.2 (3) | C33—N21—C31—N19 | 94.0 (4) |
C12—N7—C9—N8 | 79.5 (4) | C33—N21—C32—O11 | 175.3 (3) |
C7—N7—C9—C8 | 0.5 (4) | C31—N21—C32—O11 | 14.9 (5) |
C12—N7—C9—C8 | −169.8 (3) | C33—N21—C32—N23 | −5.3 (4) |
C10—N8—C9—N7 | 110.8 (3) | C31—N21—C32—N23 | −165.8 (3) |
C11—N8—C9—N7 | −71.5 (4) | C36—N23—C32—O11 | −176.1 (3) |
C10—N8—C9—C8 | 0.0 (4) | C22ii—N23—C32—O11 | −16.6 (5) |
C11—N8—C9—C8 | 177.7 (3) | C36—N23—C32—N21 | 4.6 (4) |
N5—C8—C9—N7 | −3.3 (3) | C22ii—N23—C32—N21 | 164.1 (3) |
N6—C8—C9—N7 | −121.6 (3) | C35—N22—C33—N21 | −112.8 (3) |
N5—C8—C9—N8 | 116.2 (3) | C34—N22—C33—N21 | 69.7 (4) |
N6—C8—C9—N8 | −2.1 (3) | C35—N22—C33—C36 | −0.9 (4) |
C11—N8—C10—O4 | 2.9 (6) | C34—N22—C33—C36 | −178.4 (3) |
C9—N8—C10—O4 | −179.3 (4) | C32—N21—C33—N22 | 115.7 (3) |
C11—N8—C10—N6 | −175.4 (3) | C31—N21—C33—N22 | −84.2 (4) |
C9—N8—C10—N6 | 2.3 (4) | C32—N21—C33—C36 | 3.9 (3) |
C6—N6—C10—O4 | −4.6 (6) | C31—N21—C33—C36 | 164.0 (3) |
C8—N6—C10—O4 | 177.8 (4) | C35—N22—C34—N20 | 104.6 (4) |
C6—N6—C10—N8 | 173.7 (3) | C33—N22—C34—N20 | −78.2 (4) |
C8—N6—C10—N8 | −3.9 (4) | C29—N20—C34—N22 | −101.7 (4) |
C10—N8—C11—N10 | −98.1 (4) | C28—N20—C34—N22 | 92.7 (4) |
C9—N8—C11—N10 | 84.4 (4) | C20ii—N24—C35—O12 | 3.9 (6) |
C16—N10—C11—N8 | 106.7 (4) | C36—N24—C35—O12 | 172.6 (3) |
C14—N10—C11—N8 | −91.7 (4) | C20ii—N24—C35—N22 | −174.0 (3) |
C7—N7—C12—N9 | 97.8 (4) | C36—N24—C35—N22 | −5.2 (4) |
C9—N7—C12—N9 | −92.7 (4) | C34—N22—C35—O12 | 3.4 (6) |
C13—N9—C12—N7 | −95.6 (4) | C33—N22—C35—O12 | −174.1 (3) |
C14—N9—C12—N7 | 83.3 (4) | C34—N22—C35—N24 | −178.8 (3) |
C14—N9—C13—O5 | 175.1 (3) | C33—N22—C35—N24 | 3.7 (4) |
C12—N9—C13—O5 | −5.9 (5) | C32—N23—C36—N24 | −113.5 (3) |
C14—N9—C13—N11 | −1.3 (4) | C22ii—N23—C36—N24 | 87.0 (4) |
C12—N9—C13—N11 | 177.8 (3) | C32—N23—C36—C33 | −2.0 (3) |
C18—N11—C13—O5 | −10.0 (5) | C22ii—N23—C36—C33 | −161.5 (3) |
C15—N11—C13—O5 | −171.0 (3) | C35—N24—C36—N23 | 116.2 (3) |
C18—N11—C13—N9 | 166.3 (3) | C20ii—N24—C36—N23 | −75.0 (4) |
C15—N11—C13—N9 | 5.4 (4) | C35—N24—C36—C33 | 4.5 (4) |
C13—N9—C14—N10 | 108.5 (3) | C20ii—N24—C36—C33 | 173.3 (3) |
C12—N9—C14—N10 | −70.5 (4) | N22—C33—C36—N23 | −121.4 (3) |
C13—N9—C14—C15 | −3.0 (4) | N21—C33—C36—N23 | −1.1 (3) |
C12—N9—C14—C15 | 178.0 (3) | N22—C33—C36—N24 | −2.0 (3) |
C16—N10—C14—N9 | −118.9 (3) | N21—C33—C36—N24 | 118.3 (3) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+2, −y+2, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H11···O9 | 0.84 | 2.03 | 2.835 (3) | 161 |
O1W—H12···O3W | 0.84 | 1.77 | 2.599 (4) | 168 |
O2W—H21···O4iii | 0.83 | 2.39 | 3.080 (4) | 142 |
O2W—H21···O3W | 0.83 | 2.40 | 3.105 (4) | 143 |
O2W—H22···O6W | 0.83 | 1.91 | 2.731 (4) | 168 |
O3W—H31···O2iii | 0.84 | 1.91 | 2.738 (4) | 169 |
O3W—H32···O4W | 0.84 | 2.11 | 2.874 (4) | 152 |
O4W—H42···O6iii | 0.84 | 2.06 | 2.842 (4) | 157 |
O4W—H41···O16 | 0.84 | 1.96 | 2.738 (4) | 154 |
O5W—H51···Cl1iv | 0.85 | 2.44 | 3.050 (7) | 130 |
O5W—H52···O4W | 0.84 | 1.78 | 2.624 (6) | 175 |
O6W—H61···O12v | 0.84 | 2.32 | 2.831 (4) | 120 |
O7W—H71···Cl4vi | 0.88 | 2.27 | 2.60 (1) | 102 |
O8W—H82···O6i | 0.84 | 2.06 | 2.835 (5) | 153 |
O8W—H81···O13Wi | 0.85 | 2.42 | 2.90 (2) | 116 |
O9W—H91···Cl2vii | 0.84 | 2.46 | 3.264 (4) | 159 |
O9W—H92···O1 | 0.84 | 2.06 | 2.819 (4) | 149 |
O10W—H101···O5 | 0.84 | 1.84 | 2.638 (4) | 159 |
O10W—H102···O8W | 0.83 | 1.70 | 2.511 (5) | 164 |
O11W—H112···O10W | 0.84 | 1.69 | 2.485 (5) | 156 |
O11W—H111···O3 | 0.84 | 1.89 | 2.619 (4) | 144 |
O12W—H122···O11ii | 0.83 | 2.42 | 3.012 (7) | 129 |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+2, −y+2, −z+2; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y+1, −z+2; (v) x−1, y−1, z−1; (vi) −x+1, −y, −z+1; (vii) −x+2, −y+1, −z+2. |