Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804005148/fl6073sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804005148/fl6073Isup2.hkl |
CCDC reference: 238648
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.005 Å
- R factor = 0.051
- wR factor = 0.122
- Data-to-parameter ratio = 14.5
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT035_ALERT_1_A No _chemical_absolute_configuration info given . ? PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.22 Ratio
Alert level B PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 4 PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.36 Ratio
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.632 0.849 Tmin' and Tmax expected: 0.960 0.984 RR' = 0.763 Please check that your absorption correction is appropriate. PLAT024_ALERT_4_C Merging of Friedel Data Preferred for Z<=Si .... ! PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.76 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.16 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C33 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C31B PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C33B PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C36B PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C24 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C32 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C32B PLAT301_ALERT_3_C Main Residue Disorder ......................... 11.00 Perc. PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5 PLAT701_ALERT_1_C Bond Calc 2.069(2), Rep 2.066(2), Dev.. 1.50 Sigma N1 -MG1 1.555 1.555
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 1.160 Tmax scaled 0.984 Tmin scaled 0.733 REFLT03_ALERT_4_G ALERT: MoKa measured Friedel data cannot be used to determine absolute structure in a light-atom study EXCEPT under VERY special conditions. It is preferred that Friedel data is merged in such cases. From the CIF: _diffrn_reflns_theta_max 25.05 From the CIF: _reflns_number_total 6009 Count of symmetry unique reflns 3272 Completeness (_total/calc) 183.65% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2737 Fraction of Friedel pairs measured 0.836 Are heavy atom types Z>Si present no
2 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 9 ALERT type 2 Indicator that the structure model may be wrong or deficient 7 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: D*TREK (Molecular Structure Corporation, 2001); cell refinement: CrystalClear (Rigaku/MSC, 2003); data reduction: CrystalClear; program(s) used to solve structure: SHELXL97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Mg(C29H41N2)(C5H9)(C4H8O)] | F(000) = 640 |
Mr = 583.17 | Dx = 1.085 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.8292 (7) Å | Cell parameters from 5264 reflections |
b = 16.631 (1) Å | θ = 1.9–25.3° |
c = 11.5822 (8) Å | µ = 0.08 mm−1 |
β = 109.52 (1)° | T = 173 K |
V = 1784.5 (2) Å3 | Irregular, red |
Z = 2 | 0.50 × 0.20 × 0.20 mm |
Rigaku/ADSC CCD area-detector diffractometer | 6009 independent reflections |
Radiation source: fine-focus sealed tube | 4812 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
Detector resolution: 11.76 pixels mm-1 | θmax = 25.1°, θmin = 2.2° |
area detector scans | h = 0→11 |
Absorption correction: multi-scan (Blessing, 1995) | k = −19→18 |
Tmin = 0.632, Tmax = 0.849 | l = −13→12 |
25493 measured reflections |
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)] = 0.051 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.122 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.97 | w = 1/[σ2(Fo2) + (0.0799)2] where P = (Fo2 + 2Fc2)/3 |
6009 reflections | (Δ/σ)max = 0.001 |
414 parameters | Δρmax = 0.40 e Å−3 |
16 restraints | Δρmin = −0.29 e Å−3 |
Experimental. Data were collected in 0.50° oscillations with 35.0 s exposures. A sweep of data was done using φ oscillations from 0.0 to 190.0° at χ = -90° and a second sweep was performed using ω oscillations between -17.0 and 23.0° at χ = 90.0°. The crystal-to-detector distance was 38.44 mm. The detector swing angle was -5.60°. The absorption correction is based on a three-dimensional analysis of symmetry-equivalent data and is performed along with batch scaling in a single step. The resulting transmission factors, therefore, include contributions from absorption, crystal decay, and detectable variations in beam intensity. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was solved using an HKLF4 format data set containing only non-overlapped reflections from the major twin component. Refinements were carried out using an HKLF5 format data set with data (both overlapped and non-overlapped) from the major twin component. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 0.1135 (3) | 0.07459 (19) | 0.4818 (2) | 0.0180 (6) | |
C2 | 0.2558 (3) | 0.0815 (2) | 0.5675 (2) | 0.0215 (6) | |
C3 | 0.2941 (3) | 0.0331 (2) | 0.6701 (3) | 0.0293 (7) | |
H3 | 0.3875 | 0.0388 | 0.7296 | 0.035* | |
C4 | 0.2002 (3) | −0.0236 (2) | 0.6888 (3) | 0.0324 (8) | |
H4 | 0.2287 | −0.0562 | 0.7603 | 0.039* | |
C5 | 0.0652 (3) | −0.0321 (2) | 0.6025 (3) | 0.0281 (7) | |
H5 | 0.0016 | −0.0719 | 0.6144 | 0.034* | |
C6 | 0.0197 (3) | 0.01579 (19) | 0.4991 (3) | 0.0213 (6) | |
C7 | 0.3641 (3) | 0.1399 (2) | 0.5450 (3) | 0.0265 (7) | |
H7 | 0.3457 | 0.1403 | 0.4546 | 0.032* | |
C8 | 0.5196 (4) | 0.1125 (3) | 0.6059 (4) | 0.0532 (11) | |
H8A | 0.5463 | 0.1182 | 0.6950 | 0.080* | |
H8B | 0.5838 | 0.1456 | 0.5765 | 0.080* | |
H8C | 0.5287 | 0.0560 | 0.5854 | 0.080* | |
C9 | 0.3448 (4) | 0.2251 (2) | 0.5813 (4) | 0.0463 (10) | |
H9A | 0.2484 | 0.2444 | 0.5326 | 0.069* | |
H9B | 0.4182 | 0.2597 | 0.5664 | 0.069* | |
H9C | 0.3554 | 0.2268 | 0.6685 | 0.069* | |
C10 | −0.1286 (3) | 0.0012 (2) | 0.4048 (3) | 0.0277 (7) | |
H10 | −0.1472 | 0.0450 | 0.3423 | 0.033* | |
C11 | −0.1323 (4) | −0.0780 (2) | 0.3393 (3) | 0.0399 (9) | |
H11A | −0.0520 | −0.0801 | 0.3070 | 0.060* | |
H11B | −0.2240 | −0.0828 | 0.2715 | 0.060* | |
H11C | −0.1234 | −0.1225 | 0.3969 | 0.060* | |
C12 | −0.2484 (4) | 0.0050 (3) | 0.4629 (4) | 0.0459 (10) | |
H12A | −0.2387 | −0.0407 | 0.5185 | 0.069* | |
H12B | −0.3430 | 0.0029 | 0.3982 | 0.069* | |
H12C | −0.2399 | 0.0554 | 0.5089 | 0.069* | |
C13 | −0.0497 (3) | 0.2111 (2) | 0.4848 (3) | 0.0239 (7) | |
H13A | −0.1266 | 0.1730 | 0.4827 | 0.036* | |
H13B | −0.0874 | 0.2662 | 0.4782 | 0.036* | |
H13C | 0.0304 | 0.2051 | 0.5622 | 0.036* | |
C14 | 0.0039 (3) | 0.19429 (18) | 0.3784 (2) | 0.0165 (6) | |
C15 | −0.0218 (3) | 0.25502 (19) | 0.2894 (2) | 0.0188 (6) | |
H15 | −0.0899 | 0.2949 | 0.2921 | 0.023* | |
C16 | 0.0402 (3) | 0.26471 (19) | 0.1959 (2) | 0.0196 (6) | |
C17 | 0.0201 (4) | 0.3472 (2) | 0.1363 (3) | 0.0320 (8) | |
H17A | 0.0668 | 0.3485 | 0.0735 | 0.048* | 0.50 |
H17B | 0.0637 | 0.3882 | 0.1987 | 0.048* | 0.50 |
H17C | −0.0833 | 0.3584 | 0.0982 | 0.048* | 0.50 |
H17D | −0.0353 | 0.3815 | 0.1734 | 0.048* | 0.50 |
H17E | −0.0323 | 0.3418 | 0.0482 | 0.048* | 0.50 |
H17F | 0.1148 | 0.3716 | 0.1487 | 0.048* | 0.50 |
C18 | 0.1948 (3) | 0.2300 (2) | 0.0837 (3) | 0.0208 (6) | |
C19 | 0.3355 (3) | 0.2600 (2) | 0.1380 (3) | 0.0272 (7) | |
C20 | 0.4150 (4) | 0.2794 (2) | 0.0627 (3) | 0.0342 (8) | |
H20 | 0.5096 | 0.3007 | 0.0982 | 0.041* | |
C21 | 0.3596 (4) | 0.2683 (2) | −0.0627 (3) | 0.0390 (9) | |
H21 | 0.4154 | 0.2824 | −0.1128 | 0.047* | |
C22 | 0.2241 (4) | 0.2369 (2) | −0.1143 (3) | 0.0353 (8) | |
H22 | 0.1875 | 0.2285 | −0.2004 | 0.042* | |
C23 | 0.1376 (3) | 0.2170 (2) | −0.0436 (3) | 0.0257 (7) | |
C24 | 0.4050 (3) | 0.2704 (2) | 0.2762 (3) | 0.0318 (8) | |
H24 | 0.3356 | 0.2488 | 0.3150 | 0.038* | |
C25 | 0.5417 (4) | 0.2212 (4) | 0.3242 (4) | 0.0658 (13) | |
H25A | 0.5201 | 0.1647 | 0.3011 | 0.099* | |
H25B | 0.5807 | 0.2257 | 0.4137 | 0.099* | |
H25C | 0.6130 | 0.2413 | 0.2889 | 0.099* | |
C26 | 0.4317 (6) | 0.3591 (3) | 0.3135 (4) | 0.0667 (13) | |
H26A | 0.5020 | 0.3819 | 0.2792 | 0.100* | |
H26B | 0.4694 | 0.3633 | 0.4031 | 0.100* | |
H26C | 0.3406 | 0.3890 | 0.2820 | 0.100* | |
C27 | −0.0131 (4) | 0.1836 (2) | −0.1057 (3) | 0.0340 (8) | |
H27 | −0.0564 | 0.1710 | −0.0409 | 0.041* | |
C28 | −0.0107 (4) | 0.1067 (2) | −0.1760 (3) | 0.0490 (10) | |
H28A | −0.1082 | 0.0839 | −0.2070 | 0.073* | |
H28B | 0.0550 | 0.0678 | −0.1214 | 0.073* | |
H28C | 0.0228 | 0.1187 | −0.2450 | 0.073* | |
C29 | −0.1102 (4) | 0.2458 (3) | −0.1936 (4) | 0.0525 (10) | |
H29A | −0.1130 | 0.2953 | −0.1484 | 0.079* | |
H29B | −0.2081 | 0.2241 | −0.2289 | 0.079* | |
H29C | −0.0713 | 0.2577 | −0.2594 | 0.079* | |
C31 | 0.3244 (9) | −0.0503 (5) | 0.2850 (6) | 0.036 (3)* | 0.522 (14) |
H31A | 0.2773 | −0.0844 | 0.3308 | 0.043* | 0.522 (14) |
H31B | 0.3877 | −0.0108 | 0.3422 | 0.043* | 0.522 (14) |
C32 | 0.4130 (8) | −0.1030 (4) | 0.2237 (8) | 0.029 (2)* | 0.522 (14) |
H32A | 0.5092 | −0.1159 | 0.2834 | 0.035* | 0.522 (14) |
H32B | 0.3616 | −0.1539 | 0.1925 | 0.035* | 0.522 (14) |
C33 | 0.4278 (10) | −0.0539 (6) | 0.1210 (7) | 0.055 (3)* | 0.522 (14) |
H33A | 0.3969 | −0.0841 | 0.0427 | 0.065* | 0.522 (14) |
H33B | 0.5280 | −0.0345 | 0.1385 | 0.065* | 0.522 (14) |
C34 | 0.3234 (8) | 0.0156 (5) | 0.1196 (8) | 0.043 (2)* | 0.522 (14) |
H34A | 0.3795 | 0.0625 | 0.1631 | 0.051* | 0.522 (14) |
H34B | 0.2720 | 0.0318 | 0.0337 | 0.051* | 0.522 (14) |
C35 | −0.2523 (4) | 0.1147 (2) | 0.0974 (3) | 0.0411 (9) | |
H35A | −0.2259 | 0.1724 | 0.1081 | 0.049* | |
H35B | −0.2966 | 0.0992 | 0.1595 | 0.049* | |
C36 | −0.3541 (8) | 0.0991 (5) | −0.0289 (8) | 0.036 (3) | 0.58 (2) |
H36A | −0.4557 | 0.1063 | −0.0329 | 0.043* | 0.58 (2) |
H36B | −0.3342 | 0.1354 | −0.0893 | 0.043* | 0.58 (2) |
C37 | −0.3244 (4) | 0.0137 (3) | −0.0514 (4) | 0.0598 (12) | |
H37A | −0.3345 | 0.0055 | −0.1387 | 0.072* | |
H37B | −0.3927 | −0.0227 | −0.0306 | 0.072* | |
C38 | −0.1731 (4) | −0.0031 (2) | 0.0289 (3) | 0.0382 (8) | |
H38A | −0.1693 | −0.0526 | 0.0775 | 0.046* | |
H38B | −0.1096 | −0.0104 | −0.0212 | 0.046* | |
N1 | 0.0724 (2) | 0.12570 (16) | 0.3755 (2) | 0.0148 (5) | |
N2 | 0.1113 (3) | 0.20795 (17) | 0.1606 (2) | 0.0181 (5) | |
C30 | 0.2130 (4) | −0.0081 (2) | 0.1802 (4) | 0.0436 (9) | |
O2 | −0.1269 (2) | 0.06588 (16) | 0.10907 (19) | 0.0297 (5) | |
Mg1 | 0.08982 (10) | 0.09038 (12) | 0.20977 (8) | 0.0180 (2) | |
C31B | 0.2966 (14) | −0.0524 (7) | 0.2966 (7) | 0.064 (5)* | 0.478 (14) |
H31C | 0.2304 | −0.0852 | 0.3259 | 0.077* | 0.478 (14) |
H31D | 0.3476 | −0.0138 | 0.3619 | 0.077* | 0.478 (14) |
C32B | 0.4071 (10) | −0.1075 (6) | 0.2645 (10) | 0.047 (3)* | 0.478 (14) |
H32C | 0.5075 | −0.0942 | 0.3154 | 0.056* | 0.478 (14) |
H32D | 0.3884 | −0.1651 | 0.2758 | 0.056* | 0.478 (14) |
C33B | 0.3799 (13) | −0.0883 (7) | 0.1317 (8) | 0.072 (4)* | 0.478 (14) |
H33C | 0.3348 | −0.1358 | 0.0818 | 0.086* | 0.478 (14) |
H33D | 0.4740 | −0.0789 | 0.1199 | 0.086* | 0.478 (14) |
C34B | 0.2818 (12) | −0.0141 (7) | 0.0829 (8) | 0.059 (3)* | 0.478 (14) |
H34C | 0.3387 | 0.0346 | 0.0799 | 0.070* | 0.478 (14) |
H34D | 0.2097 | −0.0241 | 0.0009 | 0.070* | 0.478 (14) |
C36B | −0.3760 (11) | 0.0715 (9) | 0.038 (2) | 0.068 (7) | 0.42 (2) |
H36C | −0.361 (12) | 0.029 (6) | 0.100 (10) | 0.12 (4)* | 0.42 (2) |
H36D | −0.467 (7) | 0.100 (6) | 0.027 (11) | 0.12 (4)* | 0.42 (2) |
H30 | 0.142 (5) | −0.052 (3) | 0.124 (5) | 0.090 (16)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0201 (14) | 0.0182 (16) | 0.0181 (14) | 0.0031 (11) | 0.0096 (12) | −0.0008 (11) |
C2 | 0.0222 (15) | 0.0251 (16) | 0.0192 (15) | 0.0016 (13) | 0.0096 (12) | −0.0005 (13) |
C3 | 0.0174 (16) | 0.044 (2) | 0.0238 (17) | 0.0033 (14) | 0.0037 (14) | 0.0045 (14) |
C4 | 0.036 (2) | 0.0345 (19) | 0.0262 (18) | 0.0088 (15) | 0.0100 (16) | 0.0165 (14) |
C5 | 0.0284 (18) | 0.0256 (17) | 0.0349 (19) | 0.0013 (13) | 0.0166 (16) | 0.0091 (14) |
C6 | 0.0236 (16) | 0.0168 (15) | 0.0284 (17) | −0.0003 (12) | 0.0151 (14) | −0.0005 (12) |
C7 | 0.0201 (16) | 0.0379 (18) | 0.0212 (17) | −0.0070 (13) | 0.0067 (14) | 0.0006 (13) |
C8 | 0.0228 (19) | 0.080 (3) | 0.055 (2) | −0.0030 (18) | 0.0106 (18) | 0.023 (2) |
C9 | 0.046 (2) | 0.048 (2) | 0.050 (2) | −0.0213 (18) | 0.0233 (19) | −0.0174 (18) |
C10 | 0.0244 (17) | 0.0235 (16) | 0.0353 (18) | −0.0063 (13) | 0.0101 (15) | 0.0051 (13) |
C11 | 0.041 (2) | 0.036 (2) | 0.039 (2) | −0.0136 (16) | 0.0079 (17) | −0.0061 (16) |
C12 | 0.0253 (19) | 0.056 (2) | 0.060 (3) | −0.0072 (16) | 0.0191 (18) | −0.0017 (19) |
C13 | 0.0270 (17) | 0.0272 (16) | 0.0208 (16) | −0.0017 (13) | 0.0121 (13) | 0.0012 (12) |
C14 | 0.0162 (15) | 0.0156 (15) | 0.0175 (14) | −0.0050 (11) | 0.0054 (12) | −0.0047 (11) |
C15 | 0.0211 (15) | 0.0171 (15) | 0.0207 (15) | 0.0010 (11) | 0.0103 (13) | −0.0024 (11) |
C16 | 0.0211 (15) | 0.0199 (15) | 0.0184 (15) | −0.0022 (12) | 0.0073 (13) | −0.0031 (11) |
C17 | 0.051 (2) | 0.0183 (16) | 0.0347 (18) | 0.0044 (14) | 0.0256 (17) | 0.0033 (13) |
C18 | 0.0260 (17) | 0.0177 (15) | 0.0233 (16) | 0.0042 (12) | 0.0145 (13) | 0.0025 (12) |
C19 | 0.0298 (18) | 0.0243 (17) | 0.0295 (17) | −0.0011 (13) | 0.0126 (14) | 0.0062 (13) |
C20 | 0.0284 (18) | 0.039 (2) | 0.038 (2) | −0.0050 (14) | 0.0155 (16) | 0.0072 (15) |
C21 | 0.044 (2) | 0.051 (2) | 0.033 (2) | −0.0076 (17) | 0.0270 (18) | 0.0039 (16) |
C22 | 0.042 (2) | 0.045 (2) | 0.0254 (17) | −0.0006 (16) | 0.0199 (16) | 0.0025 (14) |
C23 | 0.0312 (18) | 0.0291 (17) | 0.0225 (16) | 0.0029 (13) | 0.0164 (14) | 0.0039 (13) |
C24 | 0.0226 (17) | 0.045 (2) | 0.0287 (18) | −0.0111 (14) | 0.0102 (14) | 0.0050 (15) |
C25 | 0.043 (3) | 0.116 (4) | 0.035 (2) | 0.013 (2) | 0.0082 (19) | 0.017 (2) |
C26 | 0.092 (4) | 0.058 (3) | 0.042 (2) | −0.025 (2) | 0.011 (2) | −0.009 (2) |
C27 | 0.035 (2) | 0.050 (2) | 0.0198 (17) | −0.0038 (16) | 0.0133 (16) | −0.0031 (15) |
C28 | 0.059 (3) | 0.044 (2) | 0.043 (2) | −0.0066 (18) | 0.0157 (19) | −0.0051 (17) |
C29 | 0.041 (2) | 0.060 (3) | 0.049 (2) | 0.0096 (19) | 0.0045 (19) | −0.0084 (19) |
C35 | 0.029 (2) | 0.050 (2) | 0.040 (2) | 0.0084 (15) | 0.0058 (17) | −0.0156 (16) |
C36 | 0.029 (4) | 0.041 (4) | 0.030 (4) | −0.010 (3) | −0.001 (3) | −0.003 (3) |
C37 | 0.046 (2) | 0.059 (3) | 0.057 (3) | −0.008 (2) | −0.007 (2) | −0.021 (2) |
C38 | 0.053 (2) | 0.0284 (18) | 0.0275 (18) | −0.0042 (16) | 0.0061 (17) | −0.0079 (14) |
N1 | 0.0169 (12) | 0.0143 (12) | 0.0141 (12) | −0.0029 (9) | 0.0063 (10) | −0.0001 (9) |
N2 | 0.0258 (13) | 0.0167 (12) | 0.0147 (12) | 0.0004 (10) | 0.0106 (11) | 0.0019 (9) |
C30 | 0.045 (2) | 0.035 (2) | 0.050 (2) | 0.0146 (17) | 0.0149 (19) | −0.0046 (17) |
O2 | 0.0273 (12) | 0.0285 (12) | 0.0293 (12) | −0.0032 (9) | 0.0043 (10) | −0.0116 (9) |
Mg1 | 0.0241 (5) | 0.0139 (4) | 0.0184 (5) | 0.0029 (4) | 0.0102 (4) | −0.0011 (4) |
C36B | 0.028 (6) | 0.076 (10) | 0.094 (15) | −0.005 (6) | 0.013 (6) | −0.023 (10) |
C1—C6 | 1.402 (4) | C25—H25A | 0.9800 |
C1—C2 | 1.423 (4) | C25—H25B | 0.9800 |
C1—N1 | 1.437 (3) | C25—H25C | 0.9800 |
C2—C3 | 1.379 (4) | C26—H26A | 0.9800 |
C2—C7 | 1.524 (4) | C26—H26B | 0.9800 |
C3—C4 | 1.385 (4) | C26—H26C | 0.9800 |
C3—H3 | 0.9500 | C27—C28 | 1.520 (5) |
C4—C5 | 1.375 (4) | C27—C29 | 1.537 (5) |
C4—H4 | 0.9500 | C27—H27 | 1.0000 |
C5—C6 | 1.381 (4) | C28—H28A | 0.9800 |
C5—H5 | 0.9500 | C28—H28B | 0.9800 |
C6—C10 | 1.520 (4) | C28—H28C | 0.9800 |
C7—C9 | 1.507 (5) | C29—H29A | 0.9800 |
C7—C8 | 1.522 (4) | C29—H29B | 0.9800 |
C7—H7 | 1.0000 | C29—H29C | 0.9800 |
C8—H8A | 0.9800 | C31—C30 | 1.508 (6) |
C8—H8B | 0.9800 | C31—C32 | 1.561 (8) |
C8—H8C | 0.9800 | C31—H31A | 0.9900 |
C9—H9A | 0.9800 | C31—H31B | 0.9900 |
C9—H9B | 0.9800 | C32—C33 | 1.488 (9) |
C9—H9C | 0.9800 | C32—H32A | 0.9900 |
C10—C11 | 1.513 (5) | C32—H32B | 0.9900 |
C10—C12 | 1.539 (5) | C33—C34 | 1.541 (8) |
C10—H10 | 1.0000 | C33—H33A | 0.9900 |
C11—H11A | 0.9800 | C33—H33B | 0.9900 |
C11—H11B | 0.9800 | C34—C30 | 1.526 (6) |
C11—H11C | 0.9800 | C34—H34A | 0.9900 |
C12—H12A | 0.9800 | C34—H34B | 0.9900 |
C12—H12B | 0.9800 | C35—O2 | 1.443 (4) |
C12—H12C | 0.9800 | C35—C36 | 1.492 (7) |
C13—C14 | 1.518 (4) | C35—H35A | 0.9900 |
C13—H13A | 0.9800 | C35—H35B | 0.9900 |
C13—H13B | 0.9800 | C36—C37 | 1.490 (8) |
C13—H13C | 0.9800 | C36—H36A | 0.9900 |
C14—N1 | 1.329 (3) | C36—H36B | 0.9900 |
C14—C15 | 1.404 (4) | C37—C38 | 1.492 (5) |
C15—C16 | 1.416 (4) | C37—H37A | 0.9900 |
C15—H15 | 0.9500 | C37—H37B | 0.9900 |
C16—N2 | 1.317 (3) | C38—O2 | 1.448 (4) |
C16—C17 | 1.518 (4) | C38—H38A | 0.9900 |
C17—H17A | 0.9800 | C38—H38B | 0.9900 |
C17—H17B | 0.9800 | N1—Mg1 | 2.066 (2) |
C17—H17C | 0.9800 | N2—Mg1 | 2.065 (2) |
C17—H17D | 0.9800 | C30—C34B | 1.497 (7) |
C17—H17E | 0.9800 | C30—C31B | 1.515 (6) |
C17—H17F | 0.9800 | C30—Mg1 | 2.129 (3) |
C18—C19 | 1.404 (4) | C30—H30 | 1.06 (5) |
C18—C23 | 1.406 (4) | O2—Mg1 | 2.097 (2) |
C18—N2 | 1.445 (3) | C31B—C32B | 1.556 (9) |
C19—C20 | 1.388 (4) | C31B—H31C | 0.9900 |
C19—C24 | 1.524 (4) | C31B—H31D | 0.9900 |
C20—C21 | 1.381 (5) | C32B—C33B | 1.503 (10) |
C20—H20 | 0.9500 | C32B—H32C | 0.9900 |
C21—C22 | 1.367 (5) | C32B—H32D | 0.9900 |
C21—H21 | 0.9500 | C33B—C34B | 1.551 (8) |
C22—C23 | 1.402 (4) | C33B—H33C | 0.9900 |
C22—H22 | 0.9500 | C33B—H33D | 0.9900 |
C23—C27 | 1.518 (5) | C34B—H34C | 0.9900 |
C24—C25 | 1.510 (5) | C34B—H34D | 0.9900 |
C24—C26 | 1.535 (5) | C36B—H36C | 0.9800 (12) |
C24—H24 | 1.0000 | C36B—H36D | 0.9800 (11) |
C6—C1—C2 | 119.7 (2) | H26A—C26—H26C | 109.5 |
C6—C1—N1 | 121.6 (2) | H26B—C26—H26C | 109.5 |
C2—C1—N1 | 118.5 (2) | C23—C27—C28 | 111.9 (3) |
C3—C2—C1 | 118.3 (3) | C23—C27—C29 | 111.0 (3) |
C3—C2—C7 | 120.9 (3) | C28—C27—C29 | 109.2 (3) |
C1—C2—C7 | 120.8 (2) | C23—C27—H27 | 108.2 |
C2—C3—C4 | 121.8 (3) | C28—C27—H27 | 108.2 |
C2—C3—H3 | 119.1 | C29—C27—H27 | 108.2 |
C4—C3—H3 | 119.1 | C27—C28—H28A | 109.5 |
C5—C4—C3 | 119.2 (3) | C27—C28—H28B | 109.5 |
C5—C4—H4 | 120.4 | H28A—C28—H28B | 109.5 |
C3—C4—H4 | 120.4 | C27—C28—H28C | 109.5 |
C4—C5—C6 | 121.6 (3) | H28A—C28—H28C | 109.5 |
C4—C5—H5 | 119.2 | H28B—C28—H28C | 109.5 |
C6—C5—H5 | 119.2 | C27—C29—H29A | 109.5 |
C5—C6—C1 | 119.2 (3) | C27—C29—H29B | 109.5 |
C5—C6—C10 | 119.0 (3) | H29A—C29—H29B | 109.5 |
C1—C6—C10 | 121.8 (2) | C27—C29—H29C | 109.5 |
C9—C7—C8 | 110.6 (3) | H29A—C29—H29C | 109.5 |
C9—C7—C2 | 113.0 (3) | H29B—C29—H29C | 109.5 |
C8—C7—C2 | 112.3 (3) | C30—C31—C32 | 105.1 (5) |
C9—C7—H7 | 106.8 | C30—C31—H31A | 110.7 |
C8—C7—H7 | 106.8 | C32—C31—H31A | 110.7 |
C2—C7—H7 | 106.8 | C30—C31—H31B | 110.7 |
C7—C8—H8A | 109.5 | C32—C31—H31B | 110.7 |
C7—C8—H8B | 109.5 | H31A—C31—H31B | 108.8 |
H8A—C8—H8B | 109.5 | C33—C32—C31 | 105.9 (6) |
C7—C8—H8C | 109.5 | C33—C32—H32A | 110.6 |
H8A—C8—H8C | 109.5 | C31—C32—H32A | 110.6 |
H8B—C8—H8C | 109.5 | C33—C32—H32B | 110.6 |
C7—C9—H9A | 109.5 | C31—C32—H32B | 110.6 |
C7—C9—H9B | 109.5 | H32A—C32—H32B | 108.7 |
H9A—C9—H9B | 109.5 | C32—C33—C34 | 100.2 (6) |
C7—C9—H9C | 109.5 | C32—C33—H33A | 111.7 |
H9A—C9—H9C | 109.5 | C34—C33—H33A | 111.7 |
H9B—C9—H9C | 109.5 | C32—C33—H33B | 111.7 |
C11—C10—C6 | 110.9 (3) | C34—C33—H33B | 111.7 |
C11—C10—C12 | 111.1 (3) | H33A—C33—H33B | 109.5 |
C6—C10—C12 | 111.6 (3) | C30—C34—C33 | 112.0 (6) |
C11—C10—H10 | 107.7 | C30—C34—H34A | 109.2 |
C6—C10—H10 | 107.7 | C33—C34—H34A | 109.2 |
C12—C10—H10 | 107.7 | C30—C34—H34B | 109.2 |
C10—C11—H11A | 109.5 | C33—C34—H34B | 109.2 |
C10—C11—H11B | 109.5 | H34A—C34—H34B | 107.9 |
H11A—C11—H11B | 109.5 | O2—C35—C36 | 105.4 (4) |
C10—C11—H11C | 109.5 | O2—C35—H35A | 110.7 |
H11A—C11—H11C | 109.5 | C36—C35—H35A | 110.7 |
H11B—C11—H11C | 109.5 | O2—C35—H35B | 110.7 |
C10—C12—H12A | 109.5 | C36—C35—H35B | 110.7 |
C10—C12—H12B | 109.5 | H35A—C35—H35B | 108.8 |
H12A—C12—H12B | 109.5 | C37—C36—C35 | 103.3 (5) |
C10—C12—H12C | 109.5 | C37—C36—H36A | 111.1 |
H12A—C12—H12C | 109.5 | C35—C36—H36A | 111.1 |
H12B—C12—H12C | 109.5 | C37—C36—H36B | 111.1 |
C14—C13—H13A | 109.5 | C35—C36—H36B | 111.1 |
C14—C13—H13B | 109.5 | H36A—C36—H36B | 109.1 |
H13A—C13—H13B | 109.5 | C37—C36—H36D | 108 (4) |
C14—C13—H13C | 109.5 | C35—C36—H36D | 86 (5) |
H13A—C13—H13C | 109.5 | H36B—C36—H36D | 131.7 |
H13B—C13—H13C | 109.5 | C36—C37—C38 | 106.3 (3) |
N1—C14—C15 | 124.5 (2) | C36—C37—H37A | 110.5 |
N1—C14—C13 | 119.6 (2) | C38—C37—H37A | 110.5 |
C15—C14—C13 | 115.9 (2) | C36—C37—H37B | 110.5 |
C14—C15—C16 | 128.6 (3) | C38—C37—H37B | 110.5 |
C14—C15—H15 | 115.7 | H37A—C37—H37B | 108.7 |
C16—C15—H15 | 115.7 | O2—C38—C37 | 106.6 (3) |
N2—C16—C15 | 124.3 (2) | O2—C38—H38A | 110.4 |
N2—C16—C17 | 120.5 (2) | C37—C38—H38A | 110.4 |
C15—C16—C17 | 115.2 (2) | O2—C38—H38B | 110.4 |
C16—C17—H17A | 109.5 | C37—C38—H38B | 110.4 |
C16—C17—H17B | 109.5 | H38A—C38—H38B | 108.6 |
H17A—C17—H17B | 109.5 | C14—N1—C1 | 119.0 (2) |
C16—C17—H17C | 109.5 | C14—N1—Mg1 | 117.79 (17) |
H17A—C17—H17C | 109.5 | C1—N1—Mg1 | 122.68 (16) |
H17B—C17—H17C | 109.5 | C16—N2—C18 | 118.6 (2) |
C16—C17—H17D | 109.5 | C16—N2—Mg1 | 118.58 (17) |
H17A—C17—H17D | 141.1 | C18—N2—Mg1 | 122.72 (17) |
H17B—C17—H17D | 56.3 | C34B—C30—C31 | 100.7 (6) |
H17C—C17—H17D | 56.3 | C34B—C30—C31B | 112.9 (6) |
C16—C17—H17E | 109.5 | C31—C30—C34 | 93.1 (6) |
H17A—C17—H17E | 56.3 | C31B—C30—C34 | 106.1 (7) |
H17B—C17—H17E | 141.1 | C34B—C30—Mg1 | 126.5 (4) |
H17C—C17—H17E | 56.3 | C31—C30—Mg1 | 121.8 (4) |
H17D—C17—H17E | 109.5 | C31B—C30—Mg1 | 113.5 (5) |
C16—C17—H17F | 109.5 | C34—C30—Mg1 | 113.9 (4) |
H17A—C17—H17F | 56.3 | C34B—C30—H30 | 82 (3) |
H17B—C17—H17F | 56.3 | C31—C30—H30 | 109 (3) |
H17C—C17—H17F | 141.1 | C31B—C30—H30 | 105 (3) |
H17D—C17—H17F | 109.5 | C34—C30—H30 | 108 (3) |
H17E—C17—H17F | 109.5 | Mg1—C30—H30 | 109 (3) |
C19—C18—C23 | 120.8 (3) | C35—O2—C38 | 108.1 (2) |
C19—C18—N2 | 119.3 (2) | C35—O2—Mg1 | 128.25 (17) |
C23—C18—N2 | 119.7 (3) | C38—O2—Mg1 | 123.50 (19) |
C20—C19—C18 | 118.5 (3) | N2—Mg1—N1 | 91.98 (9) |
C20—C19—C24 | 118.9 (3) | N2—Mg1—O2 | 102.05 (9) |
C18—C19—C24 | 122.6 (3) | N1—Mg1—O2 | 100.82 (9) |
C21—C20—C19 | 121.4 (3) | N2—Mg1—C30 | 124.53 (14) |
C21—C20—H20 | 119.3 | N1—Mg1—C30 | 126.50 (13) |
C19—C20—H20 | 119.3 | O2—Mg1—C30 | 106.70 (13) |
C22—C21—C20 | 119.6 (3) | C30—C31B—C32B | 106.7 (7) |
C22—C21—H21 | 120.2 | C30—C31B—H31C | 110.4 |
C20—C21—H21 | 120.2 | C32B—C31B—H31C | 110.4 |
C21—C22—C23 | 121.7 (3) | C30—C31B—H31D | 110.4 |
C21—C22—H22 | 119.1 | C32B—C31B—H31D | 110.4 |
C23—C22—H22 | 119.1 | H31C—C31B—H31D | 108.6 |
C22—C23—C18 | 117.8 (3) | C33B—C32B—C31B | 102.7 (7) |
C22—C23—C27 | 119.6 (3) | C33B—C32B—H32C | 111.2 |
C18—C23—C27 | 122.5 (3) | C31B—C32B—H32C | 111.2 |
C25—C24—C19 | 110.9 (3) | C33B—C32B—H32D | 111.2 |
C25—C24—C26 | 111.7 (4) | C31B—C32B—H32D | 111.2 |
C19—C24—C26 | 112.2 (3) | H32C—C32B—H32D | 109.1 |
C25—C24—H24 | 107.2 | C32B—C33B—C34B | 114.7 (8) |
C19—C24—H24 | 107.2 | C32B—C33B—H33C | 108.6 |
C26—C24—H24 | 107.2 | C34B—C33B—H33C | 108.6 |
C24—C25—H25A | 109.5 | C32B—C33B—H33D | 108.6 |
C24—C25—H25B | 109.5 | C34B—C33B—H33D | 108.6 |
H25A—C25—H25B | 109.5 | H33C—C33B—H33D | 107.6 |
C24—C25—H25C | 109.5 | C30—C34B—C33B | 99.2 (6) |
H25A—C25—H25C | 109.5 | C30—C34B—H34C | 111.9 |
H25B—C25—H25C | 109.5 | C33B—C34B—H34C | 111.9 |
C24—C26—H26A | 109.5 | C30—C34B—H34D | 111.9 |
C24—C26—H26B | 109.5 | C33B—C34B—H34D | 111.9 |
H26A—C26—H26B | 109.5 | H34C—C34B—H34D | 109.6 |
C24—C26—H26C | 109.5 | H36C—C36B—H36D | 110.6 (5) |
C6—C1—C2—C3 | −4.2 (4) | C15—C16—N2—C18 | −167.1 (3) |
N1—C1—C2—C3 | 179.2 (3) | C17—C16—N2—C18 | 12.8 (4) |
C6—C1—C2—C7 | 174.7 (3) | C15—C16—N2—Mg1 | 16.2 (4) |
N1—C1—C2—C7 | −2.0 (4) | C17—C16—N2—Mg1 | −164.0 (2) |
C1—C2—C3—C4 | 2.6 (4) | C19—C18—N2—C16 | 83.8 (3) |
C7—C2—C3—C4 | −176.2 (3) | C23—C18—N2—C16 | −99.8 (3) |
C2—C3—C4—C5 | 0.2 (5) | C19—C18—N2—Mg1 | −99.7 (3) |
C3—C4—C5—C6 | −1.5 (5) | C23—C18—N2—Mg1 | 76.8 (3) |
C4—C5—C6—C1 | −0.1 (4) | C32—C31—C30—C34B | −20.8 (9) |
C4—C5—C6—C10 | 177.6 (3) | C32—C31—C30—C31B | 140 (4) |
C2—C1—C6—C5 | 3.0 (4) | C32—C31—C30—C34 | −46.2 (7) |
N1—C1—C6—C5 | 179.5 (3) | C32—C31—C30—Mg1 | −166.9 (4) |
C2—C1—C6—C10 | −174.7 (3) | C33—C34—C30—C34B | −65.2 (10) |
N1—C1—C6—C10 | 1.9 (4) | C33—C34—C30—C31 | 42.8 (7) |
C3—C2—C7—C9 | −99.6 (4) | C33—C34—C30—C31B | 44.2 (9) |
C1—C2—C7—C9 | 81.6 (3) | C33—C34—C30—Mg1 | 169.8 (5) |
C3—C2—C7—C8 | 26.4 (4) | C36—C35—O2—C38 | −27.7 (6) |
C1—C2—C7—C8 | −152.4 (3) | C36—C35—O2—Mg1 | 147.3 (5) |
C5—C6—C10—C11 | −69.0 (4) | C37—C38—O2—C35 | 11.6 (4) |
C1—C6—C10—C11 | 108.7 (3) | C37—C38—O2—Mg1 | −163.8 (2) |
C5—C6—C10—C12 | 55.5 (4) | C16—N2—Mg1—N1 | −34.4 (2) |
C1—C6—C10—C12 | −126.8 (3) | C18—N2—Mg1—N1 | 149.1 (2) |
N1—C14—C15—C16 | −13.7 (5) | C16—N2—Mg1—O2 | 67.1 (2) |
C13—C14—C15—C16 | 165.3 (3) | C18—N2—Mg1—O2 | −109.4 (2) |
C14—C15—C16—N2 | 15.2 (5) | C16—N2—Mg1—C30 | −172.6 (2) |
C14—C15—C16—C17 | −164.6 (3) | C18—N2—Mg1—C30 | 10.8 (3) |
C23—C18—C19—C20 | 2.3 (4) | C14—N1—Mg1—N2 | 35.4 (2) |
N2—C18—C19—C20 | 178.8 (3) | C1—N1—Mg1—N2 | −153.2 (2) |
C23—C18—C19—C24 | −176.3 (3) | C14—N1—Mg1—O2 | −67.3 (2) |
N2—C18—C19—C24 | 0.1 (4) | C1—N1—Mg1—O2 | 104.1 (2) |
C18—C19—C20—C21 | −1.2 (5) | C14—N1—Mg1—C30 | 172.3 (2) |
C24—C19—C20—C21 | 177.5 (3) | C1—N1—Mg1—C30 | −16.2 (3) |
C19—C20—C21—C22 | −0.6 (5) | C35—O2—Mg1—N2 | −46.9 (3) |
C20—C21—C22—C23 | 1.3 (5) | C38—O2—Mg1—N2 | 127.4 (2) |
C21—C22—C23—C18 | −0.2 (5) | C35—O2—Mg1—N1 | 47.5 (3) |
C21—C22—C23—C27 | 179.0 (3) | C38—O2—Mg1—N1 | −138.2 (2) |
C19—C18—C23—C22 | −1.7 (4) | C35—O2—Mg1—C30 | −178.9 (3) |
N2—C18—C23—C22 | −178.1 (3) | C38—O2—Mg1—C30 | −4.6 (3) |
C19—C18—C23—C27 | 179.2 (3) | C34B—C30—Mg1—N2 | −26.1 (7) |
N2—C18—C23—C27 | 2.7 (4) | C31—C30—Mg1—N2 | 110.9 (5) |
C20—C19—C24—C25 | −58.0 (4) | C31B—C30—Mg1—N2 | 122.4 (7) |
C18—C19—C24—C25 | 120.7 (3) | C34—C30—Mg1—N2 | 0.8 (5) |
C20—C19—C24—C26 | 67.6 (4) | C34B—C30—Mg1—N1 | −150.2 (7) |
C18—C19—C24—C26 | −113.7 (4) | C31—C30—Mg1—N1 | −13.2 (6) |
C22—C23—C27—C28 | 58.7 (4) | C31B—C30—Mg1—N1 | −1.8 (7) |
C18—C23—C27—C28 | −122.2 (3) | C34—C30—Mg1—N1 | −123.3 (4) |
C22—C23—C27—C29 | −63.7 (4) | C34B—C30—Mg1—O2 | 92.0 (7) |
C18—C23—C27—C29 | 115.5 (3) | C31—C30—Mg1—O2 | −131.0 (5) |
C30—C31—C32—C33 | 38.1 (9) | C31B—C30—Mg1—O2 | −119.6 (7) |
C31—C32—C33—C34 | −9.6 (8) | C34—C30—Mg1—O2 | 118.9 (5) |
C32—C33—C34—C30 | −21.6 (9) | C34B—C30—C31B—C32B | −13.8 (13) |
O2—C35—C36—C37 | 32.4 (7) | C31—C30—C31B—C32B | −35 (3) |
C35—C36—C37—C38 | −25.3 (8) | C34—C30—C31B—C32B | −40.8 (11) |
C36—C37—C38—O2 | 9.1 (6) | Mg1—C30—C31B—C32B | −166.6 (6) |
C15—C14—N1—C1 | 169.6 (2) | C30—C31B—C32B—C33B | 1.4 (13) |
C13—C14—N1—C1 | −9.3 (4) | C31B—C32B—C33B—C34B | 11.0 (13) |
C15—C14—N1—Mg1 | −18.7 (3) | C31—C30—C34B—C33B | 23.6 (9) |
C13—C14—N1—Mg1 | 162.4 (2) | C31B—C30—C34B—C33B | 18.9 (11) |
C6—C1—N1—C14 | 88.3 (3) | C34—C30—C34B—C33B | 98.7 (12) |
C2—C1—N1—C14 | −95.2 (3) | Mg1—C30—C34B—C33B | 167.5 (5) |
C6—C1—N1—Mg1 | −83.1 (3) | C32B—C33B—C34B—C30 | −18.4 (12) |
C2—C1—N1—Mg1 | 93.5 (3) |