# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Manish Bhattacharjee' _publ_contact_author_address ; Chemistry Indian Institute of Technology Department of Chemistry Indian Institute of Technology Kharagpur 721 302 INDIA ; _publ_contact_author_email MXB@IITKGP.AC.IN _publ_section_title ; Spontaneous Resolution of a Bimetallic Racemate Owing to Helical Assembly: Solvent and pH Dependent Assembly/Dis-assembly, Mutual Interconversion and Chirality Control Using Chiral Impurities ; loop_ _publ_author_name 'Manish Bhattacharjee' 'Takunori Harada' 'snehadrinarayan khatua' 'Reiko Kuroda' # Attachment 'Compound_3.cif' data_mbsnk71 _database_code_depnum_ccdc_archive 'CCDC 640669' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H148 Co2 Mo4 N4 O44' _chemical_formula_weight 2395.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1258(15) _cell_length_b 13.0812(17) _cell_length_c 22.454(10) _cell_angle_alpha 73.80(3) _cell_angle_beta 77.93(3) _cell_angle_gamma 81.742(11) _cell_volume 2781.5(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 12 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1242 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method /w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10383 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 24.97 _reflns_number_total 9771 _reflns_number_gt 6925 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SIR-92 (J.Appl.Cryst.1993,26,343-350)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.One DANG restraint [dC32-C33 = 2.54(2)Angstrom] is applied for C32-C33 distance. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+3.1326P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9771 _refine_ls_number_parameters 631 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1807 _refine_ls_wR_factor_gt 0.1624 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0901(6) -0.0307(5) 0.7630(3) 0.0407(14) Uani 1 1 d . . . C2 C 0.1912(6) -0.1159(4) 0.7715(3) 0.0387(13) Uani 1 1 d . . . C3 C 0.1587(7) -0.2106(5) 0.8152(3) 0.0486(16) Uani 1 1 d . . . H3 H 0.2258 -0.2672 0.8210 0.058 Uiso 1 1 calc R . . C4 C 0.0291(7) -0.2245(5) 0.8508(3) 0.0555(17) Uani 1 1 d . . . C5 C -0.0693(7) -0.1386(6) 0.8390(3) 0.0574(18) Uani 1 1 d . . . H5 H -0.1570 -0.1467 0.8614 0.069 Uiso 1 1 calc R . . C6 C -0.0433(6) -0.0409(5) 0.7952(3) 0.0484(16) Uani 1 1 d . . . C7 C 0.3356(6) -0.1058(4) 0.7369(3) 0.0392(13) Uani 1 1 d . . . H7A H 0.3791 -0.0631 0.7549 0.047 Uiso 1 1 calc R . . H7B H 0.3845 -0.1763 0.7431 0.047 Uiso 1 1 calc R . . C8 C 0.4888(6) -0.0456(5) 0.6364(3) 0.0436(15) Uani 1 1 d . . . H8A H 0.5290 -0.1129 0.6276 0.052 Uiso 1 1 calc R . . H8B H 0.5390 -0.0290 0.6644 0.052 Uiso 1 1 calc R . . C9 C 0.4971(6) 0.0420(5) 0.5757(3) 0.0434(14) Uani 1 1 d . . . C10 C 0.2784(6) -0.1143(4) 0.6359(3) 0.0377(13) Uani 1 1 d . . . H10A H 0.2347 -0.1723 0.6675 0.045 Uiso 1 1 calc R . . H10B H 0.3470 -0.1454 0.6072 0.045 Uiso 1 1 calc R . . C11 C 0.1745(6) -0.0445(5) 0.5997(3) 0.0389(14) Uani 1 1 d . . . C12 C -0.0004(9) -0.3291(6) 0.9004(4) 0.076(2) Uani 1 1 d . . . C13 C 0.0578(13) -0.4256(7) 0.8738(5) 0.109(4) Uani 1 1 d . . . H13A H 0.0058 -0.4301 0.8436 0.164 Uiso 1 1 calc R . . H13B H 0.0534 -0.4898 0.9075 0.164 Uiso 1 1 calc R . . H13C H 0.1505 -0.4173 0.8537 0.164 Uiso 1 1 calc R . . C14 C 0.0744(14) -0.3343(9) 0.9544(5) 0.129(5) Uani 1 1 d . . . H14A H 0.1690 -0.3272 0.9379 0.194 Uiso 1 1 calc R . . H14B H 0.0638 -0.4016 0.9852 0.194 Uiso 1 1 calc R . . H14C H 0.0370 -0.2772 0.9739 0.194 Uiso 1 1 calc R . . C15 C -0.1482(11) -0.3380(9) 0.9278(6) 0.139(6) Uani 1 1 d . . . H15A H -0.1821 -0.2815 0.9481 0.208 Uiso 1 1 calc R . . H15B H -0.1593 -0.4058 0.9581 0.208 Uiso 1 1 calc R . . H15C H -0.1976 -0.3323 0.8947 0.208 Uiso 1 1 calc R . . C16 C -0.1585(7) 0.0505(6) 0.7824(3) 0.0602(19) Uani 1 1 d . . . C17 C -0.1276(11) 0.1504(9) 0.7969(6) 0.118(4) Uani 1 1 d . . . H17A H -0.0417 0.1719 0.7725 0.177 Uiso 1 1 calc R . . H17B H -0.1243 0.1355 0.8410 0.177 Uiso 1 1 calc R . . H17C H -0.1973 0.2068 0.7865 0.177 Uiso 1 1 calc R . . C18 C -0.1705(9) 0.0771(7) 0.7131(4) 0.085(3) Uani 1 1 d . . . H18A H -0.1918 0.0148 0.7036 0.128 Uiso 1 1 calc R . . H18B H -0.0861 0.0995 0.6874 0.128 Uiso 1 1 calc R . . H18C H -0.2412 0.1336 0.7047 0.128 Uiso 1 1 calc R . . C19 C -0.2956(9) 0.0163(9) 0.8213(5) 0.121(5) Uani 1 1 d . . . H19A H -0.3637 0.0752 0.8138 0.181 Uiso 1 1 calc R . . H19B H -0.2897 -0.0051 0.8652 0.181 Uiso 1 1 calc R . . H19C H -0.3192 -0.0425 0.8092 0.181 Uiso 1 1 calc R . . C20 C 0.3926(7) 0.3864(5) 0.8163(3) 0.0458(15) Uani 1 1 d . . . C21 C 0.3092(7) 0.3344(5) 0.7932(3) 0.0467(15) Uani 1 1 d . . . C22 C 0.2720(7) 0.2337(5) 0.8285(3) 0.0500(16) Uani 1 1 d . . . H22 H 0.2180 0.1990 0.8130 0.060 Uiso 1 1 calc R . . C23 C 0.3114(8) 0.1836(6) 0.8850(3) 0.0548(17) Uani 1 1 d . . . C24 C 0.3960(8) 0.2364(6) 0.9064(3) 0.0570(18) Uani 1 1 d . . . H24 H 0.4244 0.2031 0.9445 0.068 Uiso 1 1 calc R . . C25 C 0.4402(7) 0.3374(5) 0.8728(3) 0.0523(17) Uani 1 1 d . . . C26 C 0.2548(6) 0.3843(5) 0.7340(3) 0.0463(15) Uani 1 1 d . . . H26A H 0.1811 0.4376 0.7420 0.056 Uiso 1 1 calc R . . H26B H 0.2175 0.3297 0.7224 0.056 Uiso 1 1 calc R . . C27 C 0.2917(8) 0.4834(6) 0.6241(3) 0.0570(18) Uani 1 1 d . . . H27A H 0.1991 0.5103 0.6377 0.068 Uiso 1 1 calc R . . H27B H 0.2891 0.4290 0.6027 0.068 Uiso 1 1 calc R . . C28 C 0.3693(7) 0.5745(5) 0.5789(3) 0.0537(17) Uani 1 1 d . . . C29 C 0.4759(6) 0.3608(5) 0.6661(3) 0.0489(16) Uani 1 1 d . . . H29A H 0.4718 0.3418 0.6278 0.059 Uiso 1 1 calc R . . H29B H 0.4704 0.2960 0.7002 0.059 Uiso 1 1 calc R . . C30 C 0.6113(6) 0.4037(5) 0.6586(3) 0.0436(14) Uani 1 1 d . . . C31 C 0.2663(8) 0.0731(6) 0.9231(4) 0.064(2) Uani 1 1 d . . . C32 C 0.356(2) -0.0103(10) 0.8985(10) 0.291(16) Uani 1 1 d D . . H32A H 0.4159 -0.0458 0.9274 0.437 Uiso 1 1 calc R . . H32B H 0.4083 0.0218 0.8583 0.437 Uiso 1 1 calc R . . H32C H 0.3023 -0.0613 0.8936 0.437 Uiso 1 1 calc R . . C33 C 0.1219(15) 0.0648(13) 0.9198(9) 0.239(12) Uani 1 1 d D . . H33A H 0.0659 0.0637 0.9601 0.358 Uiso 1 1 calc R . . H33B H 0.1160 0.0001 0.9086 0.358 Uiso 1 1 calc R . . H33C H 0.0915 0.1251 0.8885 0.358 Uiso 1 1 calc R . . C34 C 0.268(2) 0.0501(13) 0.9909(6) 0.232(12) Uani 1 1 d . . . H34A H 0.2236 -0.0133 1.0128 0.348 Uiso 1 1 calc R . . H34B H 0.2219 0.1092 1.0067 0.348 Uiso 1 1 calc R . . H34C H 0.3604 0.0394 0.9975 0.348 Uiso 1 1 calc R . . C35 C 0.5347(8) 0.3908(6) 0.8978(4) 0.063(2) Uani 1 1 d . . . C36 C 0.5702(12) 0.3228(9) 0.9607(5) 0.102(3) Uani 1 1 d . . . H36A H 0.6211 0.2574 0.9548 0.153 Uiso 1 1 calc R . . H36B H 0.4882 0.3067 0.9906 0.153 Uiso 1 1 calc R . . H36C H 0.6234 0.3614 0.9761 0.153 Uiso 1 1 calc R . . C37 C 0.6632(9) 0.4134(9) 0.8496(5) 0.091(3) Uani 1 1 d . . . H37A H 0.7099 0.3472 0.8428 0.136 Uiso 1 1 calc R . . H37B H 0.7207 0.4489 0.8648 0.136 Uiso 1 1 calc R . . H37C H 0.6404 0.4582 0.8106 0.136 Uiso 1 1 calc R . . C38 C 0.4626(11) 0.4971(8) 0.9099(5) 0.096(3) Uani 1 1 d . . . H38A H 0.5151 0.5248 0.9319 0.144 Uiso 1 1 calc R . . H38B H 0.3744 0.4850 0.9350 0.144 Uiso 1 1 calc R . . H38C H 0.4536 0.5476 0.8704 0.144 Uiso 1 1 calc R . . C39 C -0.1009(12) 0.5767(9) 0.7092(6) 0.118(4) Uani 1 1 d . . . H39A H -0.0535 0.5646 0.7437 0.177 Uiso 1 1 calc R . . H39B H -0.0477 0.5431 0.6779 0.177 Uiso 1 1 calc R . . H39C H -0.1867 0.5469 0.7242 0.177 Uiso 1 1 calc R . . C40 C -0.123(2) 0.6890(10) 0.6820(6) 0.155(7) Uani 1 1 d . . . H40A H -0.0279 0.6969 0.6614 0.186 Uiso 1 1 calc R . . C41 C -0.131(2) 0.7646(11) 0.7087(7) 0.233(12) Uani 1 1 d . . . H41A H -0.0858 0.8235 0.6798 0.350 Uiso 1 1 calc R . . H41B H -0.0885 0.7396 0.7453 0.350 Uiso 1 1 calc R . . H41C H -0.2245 0.7876 0.7212 0.350 Uiso 1 1 calc R . . N1 N 0.3452(4) -0.0554(3) 0.6673(2) 0.0340(10) Uani 1 1 d . . . N2 N 0.3577(5) 0.4362(4) 0.6794(2) 0.0407(11) Uani 1 1 d . . . O1 O 0.1805(5) 0.2472(3) 0.6250(2) 0.0601(13) Uani 1 1 d . . . O2 O 0.3722(5) 0.1391(3) 0.6946(2) 0.0572(12) Uani 1 1 d . . . O1W O -0.1705(5) -0.0680(4) 0.5554(3) 0.0664(14) Uani 1 1 d . . . O3 O 0.1226(4) 0.0651(3) 0.7235(2) 0.0487(11) Uani 1 1 d . . . O2W O -0.0475(5) 0.1386(4) 0.5352(2) 0.0539(12) Uani 1 1 d . . . O4 O 0.3969(4) 0.1183(3) 0.5754(2) 0.0517(11) Uani 1 1 d . . . O3W O -0.0299(5) 0.4078(4) 0.5931(2) 0.0571(12) Uani 1 1 d . . . O5 O 0.5893(4) 0.0434(4) 0.5313(2) 0.0531(11) Uani 1 1 d . . . O4W O 0.0132(6) 0.6345(4) 0.5331(3) 0.0678(14) Uani 1 1 d . . . O6 O 0.1481(4) 0.0524(3) 0.6044(2) 0.0481(11) Uani 1 1 d . . . O5W O 0.2099(4) 0.4638(4) 0.4910(2) 0.0561(12) Uani 1 1 d . . . O7 O 0.1191(4) -0.0837(3) 0.5678(2) 0.0464(10) Uani 1 1 d . . . O6W O -0.3434(5) 0.7228(4) 0.5348(3) 0.0694(14) Uani 1 1 d . . . O8 O 0.2580(5) 0.6317(4) 0.7144(3) 0.0696(15) Uani 1 1 d . . . O7W O 0.3003(5) 0.7946(4) 0.4247(3) 0.0699(15) Uani 1 1 d . . . O9 O 0.5152(6) 0.6828(4) 0.7005(3) 0.0752(16) Uani 1 1 d . . . O10 O 0.4295(5) 0.4844(4) 0.7829(2) 0.0589(13) Uani 1 1 d . . . O11 O 0.4276(5) 0.6249(3) 0.6067(2) 0.0537(12) Uani 1 1 d . . . O12 O 0.3686(6) 0.5985(4) 0.5228(3) 0.0692(15) Uani 1 1 d . . . O13 O 0.6082(4) 0.4931(3) 0.6718(3) 0.0570(13) Uani 1 1 d . . . O14 O 0.7144(5) 0.3510(4) 0.6412(3) 0.0592(13) Uani 1 1 d . . . O40 O -0.1728(7) 0.7132(6) 0.6250(3) 0.093(2) Uani 1 1 d . . . H40 H -0.1092 0.7196 0.5953 0.140 Uiso 1 1 calc R . . Co1 Co 0.0000 0.0000 0.5000 0.0429(3) Uani 1 2 d S . . Co2 Co 0.0000 0.5000 0.5000 0.0436(3) Uani 1 2 d S . . Mo1 Mo 0.25564(5) 0.12258(4) 0.65434(3) 0.03930(17) Uani 1 1 d . . . Mo2 Mo 0.42330(6) 0.58175(4) 0.70305(3) 0.04756(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.049(4) 0.035(3) 0.036(3) -0.007(3) -0.005(3) -0.003(3) C2 0.047(3) 0.033(3) 0.037(3) -0.010(2) -0.009(3) -0.002(3) C3 0.056(4) 0.038(3) 0.046(4) -0.006(3) -0.007(3) 0.002(3) C4 0.062(4) 0.048(4) 0.049(4) 0.000(3) -0.009(3) -0.007(3) C5 0.052(4) 0.067(5) 0.041(4) 0.002(3) 0.000(3) -0.009(3) C6 0.043(4) 0.052(4) 0.041(4) -0.006(3) -0.003(3) 0.003(3) C7 0.043(3) 0.031(3) 0.043(3) -0.006(2) -0.015(3) 0.002(2) C8 0.028(3) 0.038(3) 0.059(4) -0.008(3) -0.007(3) 0.003(2) C9 0.034(3) 0.039(3) 0.054(4) -0.006(3) -0.007(3) -0.006(3) C10 0.041(3) 0.026(3) 0.046(3) -0.011(2) -0.010(3) 0.001(2) C11 0.029(3) 0.040(3) 0.041(3) -0.006(3) -0.001(3) 0.000(2) C12 0.087(6) 0.057(5) 0.061(5) 0.013(4) 0.000(4) -0.008(4) C13 0.151(10) 0.051(5) 0.105(8) 0.000(5) 0.007(7) -0.025(6) C14 0.196(14) 0.100(8) 0.068(7) 0.021(6) -0.025(8) -0.021(9) C15 0.105(9) 0.092(8) 0.150(11) 0.053(7) 0.025(8) -0.022(7) C16 0.047(4) 0.064(5) 0.055(4) -0.006(4) 0.003(3) 0.010(3) C17 0.104(8) 0.101(8) 0.156(11) -0.069(8) -0.027(8) 0.048(7) C18 0.064(5) 0.085(6) 0.088(7) -0.002(5) -0.020(5) 0.023(5) C19 0.053(5) 0.126(9) 0.125(9) 0.027(7) 0.009(6) 0.026(6) C20 0.056(4) 0.038(3) 0.045(4) -0.016(3) -0.002(3) -0.011(3) C21 0.054(4) 0.040(3) 0.047(4) -0.011(3) -0.008(3) -0.008(3) C22 0.056(4) 0.052(4) 0.041(4) -0.007(3) -0.005(3) -0.015(3) C23 0.065(4) 0.052(4) 0.043(4) -0.005(3) -0.003(3) -0.016(3) C24 0.071(5) 0.056(4) 0.042(4) -0.006(3) -0.011(3) -0.010(4) C25 0.063(4) 0.053(4) 0.045(4) -0.016(3) -0.010(3) -0.011(3) C26 0.044(4) 0.044(3) 0.047(4) -0.006(3) -0.004(3) -0.010(3) C27 0.065(5) 0.055(4) 0.048(4) 0.004(3) -0.016(3) -0.019(3) C28 0.056(4) 0.046(4) 0.050(4) 0.005(3) -0.014(3) -0.004(3) C29 0.054(4) 0.031(3) 0.064(4) -0.019(3) -0.002(3) -0.012(3) C30 0.043(4) 0.033(3) 0.055(4) -0.012(3) -0.011(3) -0.003(3) C31 0.066(5) 0.064(5) 0.052(4) 0.005(4) -0.002(4) -0.024(4) C32 0.36(3) 0.058(8) 0.33(3) -0.046(11) 0.22(2) -0.059(12) C33 0.162(15) 0.196(17) 0.28(2) 0.152(16) -0.083(15) -0.122(14) C34 0.47(3) 0.164(14) 0.084(9) 0.062(9) -0.111(15) -0.200(18) C35 0.071(5) 0.061(5) 0.067(5) -0.022(4) -0.023(4) -0.012(4) C36 0.126(9) 0.103(8) 0.092(7) -0.012(6) -0.056(7) -0.027(7) C37 0.071(6) 0.120(8) 0.099(7) -0.046(6) -0.016(5) -0.026(6) C38 0.123(8) 0.084(7) 0.105(8) -0.055(6) -0.038(7) -0.003(6) C39 0.112(9) 0.106(9) 0.140(11) -0.032(8) -0.022(8) -0.018(7) C40 0.30(2) 0.085(8) 0.099(9) -0.029(7) -0.103(12) 0.024(10) C41 0.52(4) 0.097(10) 0.137(13) -0.031(9) -0.165(19) -0.045(16) N1 0.029(2) 0.027(2) 0.044(3) -0.007(2) -0.009(2) -0.0013(19) N2 0.045(3) 0.036(3) 0.041(3) -0.007(2) -0.009(2) -0.006(2) O1 0.060(3) 0.024(2) 0.085(4) -0.001(2) -0.014(3) 0.007(2) O2 0.061(3) 0.039(2) 0.081(3) -0.018(2) -0.025(3) -0.007(2) O1W 0.045(3) 0.064(3) 0.073(3) 0.001(3) -0.002(2) 0.002(2) O3 0.047(2) 0.027(2) 0.059(3) -0.0042(19) 0.006(2) 0.0038(18) O2W 0.050(3) 0.053(3) 0.061(3) -0.022(2) -0.017(2) 0.010(2) O4 0.040(2) 0.035(2) 0.065(3) 0.003(2) -0.001(2) 0.0026(18) O3W 0.048(3) 0.053(3) 0.059(3) 0.004(2) -0.013(2) 0.001(2) O5 0.041(3) 0.052(3) 0.060(3) -0.010(2) -0.001(2) -0.005(2) O4W 0.091(4) 0.046(3) 0.069(3) -0.014(2) -0.015(3) -0.015(3) O6 0.043(2) 0.039(2) 0.064(3) -0.013(2) -0.022(2) 0.0086(19) O5W 0.044(3) 0.050(3) 0.071(3) -0.009(2) -0.017(2) 0.002(2) O7 0.046(2) 0.046(2) 0.053(3) -0.016(2) -0.020(2) 0.004(2) O6W 0.056(3) 0.067(3) 0.076(4) -0.003(3) -0.015(3) -0.001(3) O8 0.071(3) 0.048(3) 0.083(4) -0.022(3) -0.005(3) 0.012(2) O7W 0.057(3) 0.078(4) 0.088(4) -0.046(3) -0.023(3) 0.016(3) O9 0.085(4) 0.032(2) 0.116(5) -0.029(3) -0.014(3) -0.014(2) O10 0.084(4) 0.046(3) 0.054(3) -0.013(2) -0.019(3) -0.018(2) O11 0.070(3) 0.036(2) 0.055(3) -0.003(2) -0.014(2) -0.016(2) O12 0.085(4) 0.059(3) 0.060(3) 0.005(3) -0.021(3) -0.025(3) O13 0.042(2) 0.041(2) 0.098(4) -0.033(3) -0.015(3) -0.003(2) O14 0.048(3) 0.042(3) 0.089(4) -0.025(3) -0.008(3) 0.000(2) O40 0.088(4) 0.108(5) 0.097(5) -0.036(4) -0.037(4) 0.000(4) Co1 0.0325(6) 0.0495(7) 0.0477(7) -0.0167(6) -0.0106(5) 0.0066(5) Co2 0.0422(7) 0.0336(6) 0.0519(7) -0.0043(5) -0.0121(6) -0.0010(5) Mo1 0.0395(3) 0.0211(2) 0.0542(4) -0.0060(2) -0.0078(2) -0.00056(19) Mo2 0.0587(4) 0.0262(3) 0.0572(4) -0.0128(2) -0.0060(3) -0.0046(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O3 1.357(7) . ? C1 C6 1.399(9) . ? C1 C2 1.401(8) . ? C2 C3 1.382(8) . ? C2 C7 1.511(8) . ? C3 C4 1.394(9) . ? C3 H3 0.9300 . ? C4 C5 1.396(10) . ? C4 C12 1.526(9) . ? C5 C6 1.398(9) . ? C5 H5 0.9300 . ? C6 C16 1.556(9) . ? C7 N1 1.505(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N1 1.481(7) . ? C8 C9 1.513(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O5 1.213(7) . ? C9 O4 1.316(7) . ? C10 N1 1.484(7) . ? C10 C11 1.506(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O7 1.244(7) . ? C11 O6 1.286(7) . ? C12 C15 1.502(13) . ? C12 C13 1.536(13) . ? C12 C14 1.541(14) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.520(13) . ? C16 C18 1.524(11) . ? C16 C19 1.530(11) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O10 1.352(7) . ? C20 C25 1.401(9) . ? C20 C21 1.410(9) . ? C21 C22 1.394(9) . ? C21 C26 1.489(9) . ? C22 C23 1.368(9) . ? C22 H22 0.9300 . ? C23 C24 1.402(10) . ? C23 C31 1.538(9) . ? C24 C25 1.410(10) . ? C24 H24 0.9300 . ? C25 C35 1.535(10) . ? C26 N2 1.502(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 N2 1.472(8) . ? C27 C28 1.526(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O12 1.212(8) . ? C28 O11 1.292(8) . ? C29 N2 1.473(8) . ? C29 C30 1.514(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O14 1.221(7) . ? C30 O13 1.280(7) . ? C31 C32 1.470(15) . ? C31 C34 1.471(13) . ? C31 C33 1.500(15) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C37 1.514(12) . ? C35 C36 1.528(12) . ? C35 C38 1.541(11) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.429(15) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.277(15) . ? C40 O40 1.412(12) . ? C40 H40A 0.9800 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? N1 Mo1 2.335(4) . ? N2 Mo2 2.330(5) . ? O1 Mo1 1.710(4) . ? O2 Mo1 1.698(4) . ? O1W Co1 2.059(5) . ? O3 Mo1 1.886(4) . ? O2W Co1 2.129(4) . ? O4 Mo1 2.040(5) . ? O3W Co2 2.087(5) . ? O4W Co2 2.123(5) . ? O6 Mo1 2.158(4) . ? O5W Co2 2.090(4) . ? O7 Co1 2.105(4) . ? O8 Mo2 1.701(5) . ? O9 Mo2 1.705(5) . ? O10 Mo2 1.894(5) . ? O11 Mo2 2.071(5) . ? O13 Mo2 2.150(4) . ? O40 H40 0.8200 . ? Co1 O1W 2.059(5) 2_556 ? Co1 O7 2.105(4) 2_556 ? Co1 O2W 2.129(4) 2_556 ? Co2 O3W 2.087(5) 2_566 ? Co2 O5W 2.090(4) 2_566 ? Co2 O4W 2.123(5) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C1 C6 118.9(5) . . ? O3 C1 C2 119.4(5) . . ? C6 C1 C2 121.7(6) . . ? C3 C2 C1 118.7(6) . . ? C3 C2 C7 119.1(5) . . ? C1 C2 C7 122.1(5) . . ? C2 C3 C4 122.4(6) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C5 116.8(6) . . ? C3 C4 C12 120.5(6) . . ? C5 C4 C12 122.8(7) . . ? C4 C5 C6 123.7(6) . . ? C4 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C5 C6 C1 116.7(6) . . ? C5 C6 C16 121.2(6) . . ? C1 C6 C16 122.0(6) . . ? N1 C7 C2 113.0(5) . . ? N1 C7 H7A 109.0 . . ? C2 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C2 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C9 109.8(5) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O5 C9 O4 122.6(6) . . ? O5 C9 C8 123.2(6) . . ? O4 C9 C8 114.3(5) . . ? N1 C10 C11 113.0(4) . . ? N1 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N1 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? O7 C11 O6 124.2(5) . . ? O7 C11 C10 118.5(5) . . ? O6 C11 C10 117.3(5) . . ? C15 C12 C4 114.0(7) . . ? C15 C12 C13 109.6(9) . . ? C4 C12 C13 110.9(7) . . ? C15 C12 C14 107.9(9) . . ? C4 C12 C14 107.0(8) . . ? C13 C12 C14 107.1(9) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 108.7(8) . . ? C17 C16 C19 109.4(8) . . ? C18 C16 C19 107.5(8) . . ? C17 C16 C6 110.9(7) . . ? C18 C16 C6 108.9(6) . . ? C19 C16 C6 111.4(6) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O10 C20 C25 119.4(6) . . ? O10 C20 C21 119.6(6) . . ? C25 C20 C21 121.1(6) . . ? C22 C21 C20 118.7(6) . . ? C22 C21 C26 118.5(6) . . ? C20 C21 C26 122.8(6) . . ? C23 C22 C21 122.8(6) . . ? C23 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C22 C23 C24 117.4(6) . . ? C22 C23 C31 121.2(6) . . ? C24 C23 C31 121.4(6) . . ? C23 C24 C25 123.2(6) . . ? C23 C24 H24 118.4 . . ? C25 C24 H24 118.4 . . ? C20 C25 C24 116.9(6) . . ? C20 C25 C35 122.1(6) . . ? C24 C25 C35 121.0(6) . . ? C21 C26 N2 114.3(5) . . ? C21 C26 H26A 108.7 . . ? N2 C26 H26A 108.7 . . ? C21 C26 H26B 108.7 . . ? N2 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? N2 C27 C28 110.2(6) . . ? N2 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? N2 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? O12 C28 O11 124.7(6) . . ? O12 C28 C27 121.6(7) . . ? O11 C28 C27 113.6(6) . . ? N2 C29 C30 114.2(5) . . ? N2 C29 H29A 108.7 . . ? C30 C29 H29A 108.7 . . ? N2 C29 H29B 108.7 . . ? C30 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? O14 C30 O13 124.9(6) . . ? O14 C30 C29 118.5(5) . . ? O13 C30 C29 116.6(5) . . ? C32 C31 C34 108.0(13) . . ? C32 C31 C33 110.1(12) . . ? C34 C31 C33 104.5(12) . . ? C32 C31 C23 109.4(8) . . ? C34 C31 C23 113.8(8) . . ? C33 C31 C23 110.9(8) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.4 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 C36 109.9(8) . . ? C37 C35 C25 109.7(6) . . ? C36 C35 C25 112.3(7) . . ? C37 C35 C38 109.1(8) . . ? C36 C35 C38 106.4(8) . . ? C25 C35 C38 109.3(7) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 O40 117.4(12) . . ? C41 C40 C39 127.7(12) . . ? O40 C40 C39 112.9(10) . . ? C41 C40 H40A 94.6 . . ? O40 C40 H40A 94.7 . . ? C39 C40 H40A 94.7 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C8 N1 C10 110.2(5) . . ? C8 N1 C7 110.4(4) . . ? C10 N1 C7 112.9(4) . . ? C8 N1 Mo1 102.8(3) . . ? C10 N1 Mo1 112.4(3) . . ? C7 N1 Mo1 107.8(3) . . ? C27 N2 C29 112.2(5) . . ? C27 N2 C26 109.2(5) . . ? C29 N2 C26 111.8(5) . . ? C27 N2 Mo2 104.6(4) . . ? C29 N2 Mo2 110.8(4) . . ? C26 N2 Mo2 107.9(4) . . ? C1 O3 Mo1 139.8(4) . . ? C9 O4 Mo1 121.5(4) . . ? C11 O6 Mo1 123.6(4) . . ? C11 O7 Co1 126.7(4) . . ? C20 O10 Mo2 140.4(4) . . ? C28 O11 Mo2 123.1(4) . . ? C30 O13 Mo2 123.2(4) . . ? C40 O40 H40 109.5 . . ? O1W Co1 O1W 180.0(3) . 2_556 ? O1W Co1 O7 91.21(19) . . ? O1W Co1 O7 88.79(19) 2_556 . ? O1W Co1 O7 88.79(19) . 2_556 ? O1W Co1 O7 91.21(19) 2_556 2_556 ? O7 Co1 O7 180.00(18) . 2_556 ? O1W Co1 O2W 92.2(2) . . ? O1W Co1 O2W 87.8(2) 2_556 . ? O7 Co1 O2W 95.12(16) . . ? O7 Co1 O2W 84.88(16) 2_556 . ? O1W Co1 O2W 87.8(2) . 2_556 ? O1W Co1 O2W 92.2(2) 2_556 2_556 ? O7 Co1 O2W 84.88(16) . 2_556 ? O7 Co1 O2W 95.12(16) 2_556 2_556 ? O2W Co1 O2W 180.0(2) . 2_556 ? O3W Co2 O3W 180.000(1) . 2_566 ? O3W Co2 O5W 91.43(18) . . ? O3W Co2 O5W 88.57(18) 2_566 . ? O3W Co2 O5W 88.57(18) . 2_566 ? O3W Co2 O5W 91.43(18) 2_566 2_566 ? O5W Co2 O5W 180.000(1) . 2_566 ? O3W Co2 O4W 89.0(2) . . ? O3W Co2 O4W 91.0(2) 2_566 . ? O5W Co2 O4W 90.6(2) . . ? O5W Co2 O4W 89.4(2) 2_566 . ? O3W Co2 O4W 91.0(2) . 2_566 ? O3W Co2 O4W 89.0(2) 2_566 2_566 ? O5W Co2 O4W 89.4(2) . 2_566 ? O5W Co2 O4W 90.6(2) 2_566 2_566 ? O4W Co2 O4W 180.000(1) . 2_566 ? O2 Mo1 O1 106.5(2) . . ? O2 Mo1 O3 98.7(2) . . ? O1 Mo1 O3 102.1(2) . . ? O2 Mo1 O4 92.9(2) . . ? O1 Mo1 O4 96.3(2) . . ? O3 Mo1 O4 154.42(18) . . ? O2 Mo1 O6 161.13(18) . . ? O1 Mo1 O6 91.5(2) . . ? O3 Mo1 O6 82.80(19) . . ? O4 Mo1 O6 79.02(18) . . ? O2 Mo1 N1 88.02(18) . . ? O1 Mo1 N1 163.1(2) . . ? O3 Mo1 N1 83.79(16) . . ? O4 Mo1 N1 73.88(16) . . ? O6 Mo1 N1 73.40(15) . . ? O8 Mo2 O9 105.7(3) . . ? O8 Mo2 O10 100.0(3) . . ? O9 Mo2 O10 105.4(2) . . ? O8 Mo2 O11 89.7(2) . . ? O9 Mo2 O11 93.8(2) . . ? O10 Mo2 O11 155.10(18) . . ? O8 Mo2 O13 162.1(2) . . ? O9 Mo2 O13 89.2(2) . . ? O10 Mo2 O13 85.1(2) . . ? O11 Mo2 O13 79.3(2) . . ? O8 Mo2 N2 89.3(2) . . ? O9 Mo2 N2 160.7(2) . . ? O10 Mo2 N2 83.28(18) . . ? O11 Mo2 N2 73.86(17) . . ? O13 Mo2 N2 74.14(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 C1 C2 C3 175.5(6) . . . . ? C6 C1 C2 C3 -3.1(9) . . . . ? O3 C1 C2 C7 -1.5(9) . . . . ? C6 C1 C2 C7 180.0(6) . . . . ? C1 C2 C3 C4 0.3(10) . . . . ? C7 C2 C3 C4 177.3(6) . . . . ? C2 C3 C4 C5 2.0(10) . . . . ? C2 C3 C4 C12 -177.5(7) . . . . ? C3 C4 C5 C6 -1.6(11) . . . . ? C12 C4 C5 C6 177.9(7) . . . . ? C4 C5 C6 C1 -1.0(11) . . . . ? C4 C5 C6 C16 177.7(7) . . . . ? O3 C1 C6 C5 -175.2(6) . . . . ? C2 C1 C6 C5 3.4(10) . . . . ? O3 C1 C6 C16 6.1(10) . . . . ? C2 C1 C6 C16 -175.3(6) . . . . ? C3 C2 C7 N1 135.2(6) . . . . ? C1 C2 C7 N1 -47.9(7) . . . . ? N1 C8 C9 O5 -153.1(6) . . . . ? N1 C8 C9 O4 28.3(7) . . . . ? N1 C10 C11 O7 174.9(5) . . . . ? N1 C10 C11 O6 -5.6(8) . . . . ? C3 C4 C12 C15 -171.3(9) . . . . ? C5 C4 C12 C15 9.2(13) . . . . ? C3 C4 C12 C13 -47.0(11) . . . . ? C5 C4 C12 C13 133.5(9) . . . . ? C3 C4 C12 C14 69.5(10) . . . . ? C5 C4 C12 C14 -110.0(9) . . . . ? C5 C6 C16 C17 120.3(9) . . . . ? C1 C6 C16 C17 -61.0(10) . . . . ? C5 C6 C16 C18 -120.1(8) . . . . ? C1 C6 C16 C18 58.6(9) . . . . ? C5 C6 C16 C19 -1.8(11) . . . . ? C1 C6 C16 C19 176.9(8) . . . . ? O10 C20 C21 C22 -179.8(6) . . . . ? C25 C20 C21 C22 1.5(10) . . . . ? O10 C20 C21 C26 -2.2(10) . . . . ? C25 C20 C21 C26 179.0(6) . . . . ? C20 C21 C22 C23 0.9(10) . . . . ? C26 C21 C22 C23 -176.8(7) . . . . ? C21 C22 C23 C24 -1.9(11) . . . . ? C21 C22 C23 C31 179.0(7) . . . . ? C22 C23 C24 C25 0.6(11) . . . . ? C31 C23 C24 C25 179.7(7) . . . . ? O10 C20 C25 C24 178.6(6) . . . . ? C21 C20 C25 C24 -2.6(10) . . . . ? O10 C20 C25 C35 -0.8(10) . . . . ? C21 C20 C25 C35 178.0(6) . . . . ? C23 C24 C25 C20 1.6(11) . . . . ? C23 C24 C25 C35 -179.0(7) . . . . ? C22 C21 C26 N2 -136.3(6) . . . . ? C20 C21 C26 N2 46.1(9) . . . . ? N2 C27 C28 O12 152.1(7) . . . . ? N2 C27 C28 O11 -31.3(9) . . . . ? N2 C29 C30 O14 -172.6(6) . . . . ? N2 C29 C30 O13 8.1(9) . . . . ? C22 C23 C31 C32 82.6(14) . . . . ? C24 C23 C31 C32 -96.4(14) . . . . ? C22 C23 C31 C34 -156.5(12) . . . . ? C24 C23 C31 C34 24.5(15) . . . . ? C22 C23 C31 C33 -39.0(14) . . . . ? C24 C23 C31 C33 141.9(12) . . . . ? C20 C25 C35 C37 -58.6(10) . . . . ? C24 C25 C35 C37 122.0(8) . . . . ? C20 C25 C35 C36 178.8(8) . . . . ? C24 C25 C35 C36 -0.5(11) . . . . ? C20 C25 C35 C38 61.0(10) . . . . ? C24 C25 C35 C38 -118.3(8) . . . . ? C9 C8 N1 C10 77.9(6) . . . . ? C9 C8 N1 C7 -156.7(5) . . . . ? C9 C8 N1 Mo1 -42.0(5) . . . . ? C11 C10 N1 C8 -110.6(5) . . . . ? C11 C10 N1 C7 125.5(5) . . . . ? C11 C10 N1 Mo1 3.4(6) . . . . ? C2 C7 N1 C8 178.8(5) . . . . ? C2 C7 N1 C10 -57.4(6) . . . . ? C2 C7 N1 Mo1 67.2(5) . . . . ? C28 C27 N2 C29 -80.2(7) . . . . ? C28 C27 N2 C26 155.3(6) . . . . ? C28 C27 N2 Mo2 39.9(7) . . . . ? C30 C29 N2 C27 105.5(6) . . . . ? C30 C29 N2 C26 -131.5(6) . . . . ? C30 C29 N2 Mo2 -11.0(7) . . . . ? C21 C26 N2 C27 -179.3(6) . . . . ? C21 C26 N2 C29 56.0(7) . . . . ? C21 C26 N2 Mo2 -66.2(6) . . . . ? C6 C1 O3 Mo1 -158.9(5) . . . . ? C2 C1 O3 Mo1 22.5(10) . . . . ? O5 C9 O4 Mo1 -172.7(5) . . . . ? C8 C9 O4 Mo1 5.9(7) . . . . ? O7 C11 O6 Mo1 -175.2(4) . . . . ? C10 C11 O6 Mo1 5.3(7) . . . . ? O6 C11 O7 Co1 12.9(9) . . . . ? C10 C11 O7 Co1 -167.6(4) . . . . ? C25 C20 O10 Mo2 169.2(5) . . . . ? C21 C20 O10 Mo2 -9.6(11) . . . . ? O12 C28 O11 Mo2 179.1(6) . . . . ? C27 C28 O11 Mo2 2.6(8) . . . . ? O14 C30 O13 Mo2 -179.4(5) . . . . ? C29 C30 O13 Mo2 -0.2(8) . . . . ? C11 O7 Co1 O1W -113.3(5) . . . . ? C11 O7 Co1 O1W 66.7(5) . . . 2_556 ? C11 O7 Co1 O7 147(54) . . . 2_556 ? C11 O7 Co1 O2W -21.0(5) . . . . ? C11 O7 Co1 O2W 159.0(5) . . . 2_556 ? C1 O3 Mo1 O2 -86.9(7) . . . . ? C1 O3 Mo1 O1 164.1(6) . . . . ? C1 O3 Mo1 O4 29.2(9) . . . . ? C1 O3 Mo1 O6 74.1(6) . . . . ? C1 O3 Mo1 N1 0.1(6) . . . . ? C9 O4 Mo1 O2 63.5(5) . . . . ? C9 O4 Mo1 O1 170.4(5) . . . . ? C9 O4 Mo1 O3 -53.8(7) . . . . ? C9 O4 Mo1 O6 -99.3(5) . . . . ? C9 O4 Mo1 N1 -23.6(4) . . . . ? C11 O6 Mo1 O2 7.8(9) . . . . ? C11 O6 Mo1 O1 169.9(5) . . . . ? C11 O6 Mo1 O3 -88.1(5) . . . . ? C11 O6 Mo1 O4 73.8(5) . . . . ? C11 O6 Mo1 N1 -2.5(4) . . . . ? C8 N1 Mo1 O2 -59.1(4) . . . . ? C10 N1 Mo1 O2 -177.5(4) . . . . ? C7 N1 Mo1 O2 57.5(4) . . . . ? C8 N1 Mo1 O1 90.5(8) . . . . ? C10 N1 Mo1 O1 -28.0(9) . . . . ? C7 N1 Mo1 O1 -152.9(7) . . . . ? C8 N1 Mo1 O3 -158.1(4) . . . . ? C10 N1 Mo1 O3 83.5(4) . . . . ? C7 N1 Mo1 O3 -41.5(3) . . . . ? C8 N1 Mo1 O4 34.5(4) . . . . ? C10 N1 Mo1 O4 -83.9(4) . . . . ? C7 N1 Mo1 O4 151.1(4) . . . . ? C8 N1 Mo1 O6 117.6(4) . . . . ? C10 N1 Mo1 O6 -0.8(4) . . . . ? C7 N1 Mo1 O6 -125.8(4) . . . . ? C20 O10 Mo2 O8 77.1(7) . . . . ? C20 O10 Mo2 O9 -173.4(7) . . . . ? C20 O10 Mo2 O11 -34.2(10) . . . . ? C20 O10 Mo2 O13 -85.5(7) . . . . ? C20 O10 Mo2 N2 -11.0(7) . . . . ? C28 O11 Mo2 O8 -73.5(5) . . . . ? C28 O11 Mo2 O9 -179.2(5) . . . . ? C28 O11 Mo2 O10 40.0(8) . . . . ? C28 O11 Mo2 O13 92.3(5) . . . . ? C28 O11 Mo2 N2 15.9(5) . . . . ? C30 O13 Mo2 O8 -27.7(10) . . . . ? C30 O13 Mo2 O9 -174.7(6) . . . . ? C30 O13 Mo2 O10 79.8(5) . . . . ? C30 O13 Mo2 O11 -80.7(5) . . . . ? C30 O13 Mo2 N2 -4.6(5) . . . . ? C27 N2 Mo2 O8 60.2(4) . . . . ? C29 N2 Mo2 O8 -178.7(4) . . . . ? C26 N2 Mo2 O8 -56.0(4) . . . . ? C27 N2 Mo2 O9 -81.6(8) . . . . ? C29 N2 Mo2 O9 39.5(9) . . . . ? C26 N2 Mo2 O9 162.2(7) . . . . ? C27 N2 Mo2 O10 160.3(4) . . . . ? C29 N2 Mo2 O10 -78.6(4) . . . . ? C26 N2 Mo2 O10 44.1(4) . . . . ? C27 N2 Mo2 O11 -29.7(4) . . . . ? C29 N2 Mo2 O11 91.4(4) . . . . ? C26 N2 Mo2 O11 -145.9(4) . . . . ? C27 N2 Mo2 O13 -112.9(4) . . . . ? C29 N2 Mo2 O13 8.2(4) . . . . ? C26 N2 Mo2 O13 130.9(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.853 _refine_diff_density_min -1.325 _refine_diff_density_rms 0.106 # Attachment 'Compound_2b.cif' data_mbsnk83 _database_code_depnum_ccdc_archive 'CCDC 640670' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H72 Co Mo2 N2 O22' _chemical_formula_weight 1183.81 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.792(2) _cell_length_b 11.692(2) _cell_length_c 16.692(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.428(8) _cell_angle_gamma 90.00 _cell_volume 2674.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 13 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1226 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-MACH3 _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5161 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4944 _reflns_number_gt 3284 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SIR-92 (J.Appl.Cryst.1993,26,343-350)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(0.18(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0619P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 4944 _refine_ls_number_parameters 616 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3256(8) 0.5259(8) 0.6501(6) 0.034(3) Uani 1 1 d . . . C2 C 0.2436(8) 0.5673(8) 0.6851(6) 0.035(3) Uani 1 1 d . . . C3 C 0.2297(8) 0.6847(9) 0.6879(6) 0.038(3) Uani 1 1 d . . . H3 H 0.1775 0.7125 0.7128 0.046 Uiso 1 1 calc R . . C4 C 0.2900(9) 0.7621(8) 0.6555(6) 0.041(3) Uani 1 1 d . . . C5 C 0.3686(8) 0.7152(9) 0.6207(6) 0.039(3) Uani 1 1 d . . . H5 H 0.4121 0.7650 0.6001 0.047 Uiso 1 1 calc R . . C6 C 0.3856(8) 0.5974(10) 0.6152(6) 0.040(3) Uani 1 1 d . . . C7 C 0.1748(8) 0.4856(9) 0.7153(6) 0.036(3) Uani 1 1 d . . . H7A H 0.1484 0.4366 0.6713 0.044 Uiso 1 1 calc R . . H7B H 0.1210 0.5276 0.7339 0.044 Uiso 1 1 calc R . . C8 C 0.1527(7) 0.3297(9) 0.8136(7) 0.046(3) Uani 1 1 d . . . H8A H 0.1112 0.2965 0.7689 0.055 Uiso 1 1 calc R . . H8B H 0.1117 0.3682 0.8488 0.055 Uiso 1 1 calc R . . C9 C 0.2133(10) 0.2362(11) 0.8601(8) 0.058(4) Uani 1 1 d . . . C10 C 0.2688(8) 0.4811(10) 0.8496(6) 0.044(3) Uani 1 1 d . . . H10A H 0.2465 0.4553 0.8996 0.053 Uiso 1 1 calc R . . H10B H 0.2487 0.5601 0.8414 0.053 Uiso 1 1 calc R . . C11 C 0.3798(9) 0.4752(12) 0.8574(7) 0.054(3) Uani 1 1 d . . . C12 C 0.2766(10) 0.8886(10) 0.6620(7) 0.047(3) Uani 1 1 d . . . C13 C 0.3383(17) 0.9610(12) 0.6203(14) 0.163(12) Uani 1 1 d . . . H13A H 0.3227 1.0396 0.6294 0.244 Uiso 1 1 calc R . . H13B H 0.3281 0.9449 0.5636 0.244 Uiso 1 1 calc R . . H13C H 0.4053 0.9470 0.6401 0.244 Uiso 1 1 calc R . . C14 C 0.1712(15) 0.9196(13) 0.6325(15) 0.152(10) Uani 1 1 d . . . H14A H 0.1285 0.8859 0.6675 0.229 Uiso 1 1 calc R . . H14B H 0.1550 0.8913 0.5787 0.229 Uiso 1 1 calc R . . H14C H 0.1638 1.0013 0.6327 0.229 Uiso 1 1 calc R . . C15 C 0.290(2) 0.9241(14) 0.7467(11) 0.169(12) Uani 1 1 d . . . H15A H 0.3576 0.9406 0.7624 0.254 Uiso 1 1 calc R . . H15B H 0.2692 0.8637 0.7798 0.254 Uiso 1 1 calc R . . H15C H 0.2518 0.9914 0.7534 0.254 Uiso 1 1 calc R . . C16 C 0.4706(8) 0.5513(10) 0.5727(7) 0.045(3) Uani 1 1 d . . . C17 C 0.4319(10) 0.4694(11) 0.5057(8) 0.067(4) Uani 1 1 d . . . H17A H 0.4140 0.3984 0.5288 0.100 Uiso 1 1 calc R . . H17B H 0.4815 0.4558 0.4708 0.100 Uiso 1 1 calc R . . H17C H 0.3757 0.5025 0.4751 0.100 Uiso 1 1 calc R . . C18 C 0.5238(10) 0.6503(11) 0.5322(9) 0.073(4) Uani 1 1 d . . . H18A H 0.5773 0.6195 0.5070 0.109 Uiso 1 1 calc R . . H18B H 0.5480 0.7049 0.5725 0.109 Uiso 1 1 calc R . . H18C H 0.4788 0.6872 0.4924 0.109 Uiso 1 1 calc R . . C19 C 0.5460(9) 0.4889(12) 0.6321(8) 0.072(4) Uani 1 1 d . . . H19A H 0.5150 0.4264 0.6565 0.107 Uiso 1 1 calc R . . H19B H 0.5725 0.5412 0.6732 0.107 Uiso 1 1 calc R . . H19C H 0.5976 0.4600 0.6037 0.107 Uiso 1 1 calc R . . C20 C 0.5379(17) 0.726(2) 0.8154(12) 0.145(9) Uani 1 1 d . . . H20A H 0.5248 0.6631 0.7788 0.218 Uiso 1 1 calc R . . H20B H 0.5754 0.7828 0.7911 0.218 Uiso 1 1 calc R . . H20C H 0.4774 0.7588 0.8274 0.218 Uiso 1 1 calc R . . C21 C 0.9415(8) 0.8593(10) 0.7383(6) 0.043(3) Uani 1 1 d . . . C22 C 0.9651(7) 0.9599(10) 0.7777(6) 0.040(3) Uani 1 1 d . . . C23 C 0.9374(8) 1.0624(11) 0.7416(6) 0.049(3) Uani 1 1 d . . . H23 H 0.9520 1.1304 0.7693 0.059 Uiso 1 1 calc R . . C24 C 0.8885(10) 1.0656(11) 0.6654(7) 0.056(3) Uani 1 1 d . . . C25 C 0.8639(9) 0.9631(12) 0.6281(7) 0.059(4) Uani 1 1 d . . . H25 H 0.8283 0.9649 0.5774 0.071 Uiso 1 1 calc R . . C26 C 0.8887(9) 0.8581(12) 0.6613(7) 0.056(3) Uani 1 1 d . . . C27 C 1.0279(8) 0.9619(10) 0.8582(6) 0.038(3) Uani 1 1 d . . . H27A H 1.0950 0.9457 0.8497 0.046 Uiso 1 1 calc R . . H27B H 1.0260 1.0379 0.8813 0.046 Uiso 1 1 calc R . . C28 C 1.0613(9) 0.8778(11) 0.9942(7) 0.049(3) Uani 1 1 d . . . H28A H 1.1277 0.8920 0.9828 0.058 Uiso 1 1 calc R . . H28B H 1.0423 0.9395 1.0279 0.058 Uiso 1 1 calc R . . C29 C 1.0577(9) 0.7682(11) 1.0382(7) 0.054(4) Uani 1 1 d . . . C30 C 0.8932(9) 0.9012(11) 0.9327(7) 0.052(3) Uani 1 1 d . . . H30A H 0.8698 0.9684 0.9024 0.063 Uiso 1 1 calc R . . H30B H 0.8925 0.9180 0.9895 0.063 Uiso 1 1 calc R . . C31 C 0.8252(11) 0.8014(18) 0.9097(10) 0.087(5) Uani 1 1 d . . . C32 C 0.8603(14) 1.1829(15) 0.6268(9) 0.092(5) Uani 1 1 d . . . C33 C 0.834(2) 1.171(2) 0.5346(11) 0.231(18) Uani 1 1 d . . . H33A H 0.8120 1.2431 0.5123 0.347 Uiso 1 1 calc R . . H33B H 0.7825 1.1152 0.5241 0.347 Uiso 1 1 calc R . . H33C H 0.8900 1.1459 0.5104 0.347 Uiso 1 1 calc R . . C34 C 0.930(2) 1.2723(18) 0.6458(17) 0.224(17) Uani 1 1 d . . . H34A H 0.9933 1.2470 0.6342 0.336 Uiso 1 1 calc R . . H34B H 0.9326 1.2912 0.7020 0.336 Uiso 1 1 calc R . . H34C H 0.9113 1.3387 0.6139 0.336 Uiso 1 1 calc R . . C35 C 0.761(2) 1.219(3) 0.656(2) 0.255(18) Uani 1 1 d . . . H35A H 0.7723 1.2521 0.7085 0.383 Uiso 1 1 calc R . . H35B H 0.7197 1.1532 0.6572 0.383 Uiso 1 1 calc R . . H35C H 0.7296 1.2745 0.6189 0.383 Uiso 1 1 calc R . . C36 C 0.8596(11) 0.7469(12) 0.6172(9) 0.066(4) Uani 1 1 d . . . C37 C 0.8043(13) 0.7695(16) 0.5309(9) 0.106(6) Uani 1 1 d . . . H37A H 0.7933 0.6982 0.5029 0.160 Uiso 1 1 calc R . . H37B H 0.8430 0.8187 0.5012 0.160 Uiso 1 1 calc R . . H37C H 0.7427 0.8055 0.5362 0.160 Uiso 1 1 calc R . . C38 C 0.7926(13) 0.6801(18) 0.6619(10) 0.122(7) Uani 1 1 d . . . H38A H 0.8282 0.6475 0.7091 0.184 Uiso 1 1 calc R . . H38B H 0.7637 0.6200 0.6281 0.184 Uiso 1 1 calc R . . H38C H 0.7423 0.7294 0.6775 0.184 Uiso 1 1 calc R . . C39 C 0.9512(13) 0.6756(17) 0.6030(10) 0.117(7) Uani 1 1 d . . . H39A H 0.9900 0.6625 0.6536 0.175 Uiso 1 1 calc R . . H39B H 0.9891 0.7168 0.5676 0.175 Uiso 1 1 calc R . . H39C H 0.9312 0.6036 0.5789 0.175 Uiso 1 1 calc R . . N1 N 0.2218(6) 0.4122(7) 0.7833(5) 0.036(2) Uani 1 1 d . . . N2 N 0.9949(6) 0.8765(8) 0.9166(5) 0.041(2) Uani 1 1 d . . . O1 O 0.4331(6) 0.2102(8) 0.7234(5) 0.065(2) Uani 1 1 d . . . O2 O 0.2396(6) 0.2164(6) 0.6782(5) 0.055(2) Uani 1 1 d . . . O1W O 0.5581(9) 0.3860(15) 1.0103(9) 0.149(6) Uani 1 1 d . . . O3 O 0.3408(6) 0.4099(6) 0.6527(4) 0.044(2) Uani 1 1 d . . . O2W O 0.6070(7) 0.4373(14) 0.8509(7) 0.125(5) Uani 1 1 d . . . O4 O 0.3001(6) 0.2217(6) 0.8369(5) 0.050(2) Uani 1 1 d . . . O3W O 0.7280(6) 0.5418(8) 0.9807(5) 0.075(3) Uani 1 1 d . . . O5 O 0.1822(6) 0.1823(9) 0.9127(6) 0.081(3) Uani 1 1 d . . . O4W O 0.5464(8) 0.6284(15) 1.0496(7) 0.140(6) Uani 1 1 d . . . O6 O 0.4167(5) 0.4082(7) 0.8100(5) 0.048(2) Uani 1 1 d . . . O7 O 0.4245(6) 0.5361(9) 0.9094(6) 0.079(3) Uani 1 1 d . . . O8 O 0.9979(7) 0.5493(8) 0.8547(5) 0.078(3) Uani 1 1 d . . . O9 O 1.1368(6) 0.7151(7) 0.8750(5) 0.060(2) Uani 1 1 d . . . O10 O 0.9742(7) 0.7575(6) 0.7706(5) 0.062(3) Uani 1 1 d . . . O11 O 1.0237(6) 0.6806(8) 0.9929(5) 0.055(2) Uani 1 1 d . . . O12 O 1.0826(8) 0.7608(9) 1.1085(5) 0.086(3) Uani 1 1 d . . . O13 O 0.8590(7) 0.7111(9) 0.8879(7) 0.080(3) Uani 1 1 d . . . O14 O 0.7376(7) 0.8237(9) 0.9167(9) 0.127(5) Uani 1 1 d . . . O20 O 0.5893(8) 0.6877(15) 0.8850(8) 0.133(5) Uani 1 1 d . . . Co1 Co 0.57486(13) 0.53687(17) 0.94658(12) 0.0713(6) Uani 1 1 d . . . Mo1 Mo 0.33172(7) 0.29028(7) 0.72813(6) 0.0406(3) Uani 1 1 d . . . Mo2 Mo 1.01384(8) 0.69220(9) 0.87132(6) 0.0505(3) Uani 1 1 d . . . O6W O 0.7962(7) 0.4474(12) 0.8370(7) 0.109(4) Uani 1 1 d . . . O5W O 0.6881(15) 0.2319(17) 1.0152(16) 0.288(15) Uani 1 1 d . . . O40A O 0.632(3) 0.040(4) 0.8942(17) 0.158(17) Uiso 0.51 1 d PD . . O40B O 0.608(6) 0.016(6) 0.875(2) 0.33(5) Uiso 0.49 1 d PD . . C40 C 0.640(3) 0.081(5) 0.814(3) 0.41(4) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.045(7) 0.026(5) 0.032(6) 0.003(4) 0.005(5) 0.003(5) C2 0.046(7) 0.026(5) 0.034(6) 0.001(5) 0.005(5) -0.008(5) C3 0.055(7) 0.029(5) 0.033(5) 0.001(5) 0.013(5) 0.004(6) C4 0.062(8) 0.023(6) 0.041(6) -0.001(4) 0.016(6) 0.004(5) C5 0.053(7) 0.030(7) 0.037(6) 0.002(5) 0.017(6) -0.001(5) C6 0.039(7) 0.043(7) 0.037(6) -0.007(5) 0.006(5) -0.015(6) C7 0.033(6) 0.039(6) 0.035(6) 0.002(5) -0.003(5) -0.004(5) C8 0.027(6) 0.053(7) 0.059(7) 0.027(6) 0.007(5) -0.008(5) C9 0.055(9) 0.057(7) 0.057(8) 0.014(7) -0.014(7) -0.017(7) C10 0.038(7) 0.045(6) 0.049(7) -0.007(6) 0.005(6) -0.008(6) C11 0.042(8) 0.067(8) 0.050(7) -0.010(7) -0.012(6) 0.004(7) C12 0.061(9) 0.032(6) 0.049(7) -0.004(6) 0.014(6) -0.005(6) C13 0.25(3) 0.027(8) 0.26(3) 0.024(12) 0.20(2) 0.016(12) C14 0.137(19) 0.034(9) 0.28(3) -0.015(13) -0.01(2) 0.013(10) C15 0.36(4) 0.038(9) 0.117(16) -0.008(10) 0.06(2) -0.001(15) C16 0.041(7) 0.039(6) 0.060(7) 0.001(6) 0.026(6) -0.001(6) C17 0.079(10) 0.050(8) 0.076(9) -0.013(7) 0.030(8) -0.002(8) C18 0.060(9) 0.056(8) 0.113(12) 0.005(8) 0.055(9) 0.001(7) C19 0.044(8) 0.061(9) 0.109(11) 0.000(8) 0.005(8) 0.009(7) C20 0.15(2) 0.15(2) 0.128(17) 0.005(16) -0.001(16) 0.002(17) C21 0.046(7) 0.053(8) 0.031(6) 0.004(5) 0.012(5) 0.004(6) C22 0.028(6) 0.053(7) 0.039(6) 0.003(5) 0.009(5) -0.002(6) C23 0.044(7) 0.059(8) 0.043(7) -0.004(6) 0.000(6) -0.001(6) C24 0.074(9) 0.060(8) 0.031(6) 0.005(6) -0.004(6) 0.001(7) C25 0.058(9) 0.077(10) 0.039(7) -0.001(7) -0.006(6) -0.009(8) C26 0.049(8) 0.074(9) 0.042(7) -0.005(7) -0.012(6) 0.001(7) C27 0.030(6) 0.044(6) 0.041(6) 0.004(5) 0.003(5) 0.002(6) C28 0.048(8) 0.052(7) 0.045(7) -0.015(6) 0.001(6) 0.000(6) C29 0.054(8) 0.069(10) 0.038(7) 0.025(7) -0.004(6) 0.009(7) C30 0.052(8) 0.060(8) 0.047(7) 0.009(6) 0.013(6) 0.008(7) C31 0.060(11) 0.095(14) 0.098(12) 0.048(12) -0.026(9) -0.007(11) C32 0.112(14) 0.073(10) 0.079(10) 0.018(9) -0.038(10) 0.005(11) C33 0.41(4) 0.14(2) 0.101(14) 0.074(15) -0.13(2) -0.09(3) C34 0.25(3) 0.086(16) 0.29(3) 0.112(19) -0.18(3) -0.07(2) C35 0.23(3) 0.17(3) 0.37(5) 0.15(3) 0.04(3) 0.08(3) C36 0.059(9) 0.066(8) 0.068(9) -0.024(7) -0.008(8) -0.001(7) C37 0.129(14) 0.101(14) 0.077(10) -0.031(10) -0.041(10) 0.003(12) C38 0.118(15) 0.136(16) 0.106(13) -0.043(13) -0.019(12) -0.068(15) C39 0.109(14) 0.116(15) 0.111(13) -0.061(12) -0.053(11) 0.048(13) N1 0.028(5) 0.040(5) 0.038(5) 0.005(4) 0.000(4) -0.008(4) N2 0.027(5) 0.046(5) 0.048(6) 0.012(5) 0.003(4) -0.005(4) O1 0.062(6) 0.051(5) 0.083(6) -0.001(5) 0.009(5) 0.022(5) O2 0.077(6) 0.030(4) 0.055(5) -0.001(4) -0.009(4) -0.012(4) O1W 0.101(10) 0.176(14) 0.162(13) 0.042(12) -0.013(9) -0.033(10) O3 0.046(5) 0.031(4) 0.056(5) -0.004(3) 0.014(4) 0.002(4) O2W 0.050(6) 0.215(15) 0.105(8) -0.090(9) -0.009(6) 0.007(8) O4 0.044(5) 0.044(5) 0.060(5) 0.011(4) 0.003(4) 0.007(4) O3W 0.050(5) 0.083(7) 0.086(6) -0.032(6) -0.017(5) 0.009(5) O5 0.052(6) 0.093(7) 0.097(7) 0.065(7) 0.009(5) 0.006(6) O4W 0.064(7) 0.230(16) 0.122(10) -0.113(11) -0.006(7) 0.018(9) O6 0.034(4) 0.051(5) 0.057(5) -0.018(4) 0.001(4) -0.002(4) O7 0.034(5) 0.101(7) 0.098(7) -0.062(6) -0.009(5) 0.000(5) O8 0.105(8) 0.051(6) 0.075(6) 0.006(5) -0.002(6) -0.015(6) O9 0.048(5) 0.064(6) 0.068(5) 0.007(5) 0.006(4) 0.013(5) O10 0.089(7) 0.040(5) 0.053(5) -0.013(4) -0.010(5) 0.001(4) O11 0.065(6) 0.049(5) 0.050(5) 0.008(4) 0.005(4) -0.009(5) O12 0.111(8) 0.095(8) 0.050(5) 0.021(5) 0.001(6) -0.008(6) O13 0.052(6) 0.070(7) 0.115(8) 0.018(7) -0.004(6) -0.020(6) O14 0.031(6) 0.084(9) 0.267(16) 0.044(9) 0.017(8) 0.002(6) O20 0.067(8) 0.156(12) 0.163(12) 0.044(11) -0.047(8) -0.015(9) Co1 0.0445(11) 0.0864(14) 0.0778(13) -0.0359(11) -0.0155(10) 0.0045(10) Mo1 0.0452(6) 0.0273(4) 0.0477(6) -0.0008(5) -0.0015(5) -0.0014(5) Mo2 0.0564(8) 0.0419(6) 0.0523(7) 0.0004(6) 0.0019(6) -0.0029(6) O6W 0.061(7) 0.141(11) 0.124(9) 0.011(8) 0.001(6) -0.013(7) O5W 0.196(19) 0.20(2) 0.43(3) 0.16(2) -0.13(2) -0.079(16) C40 0.31(5) 0.37(7) 0.58(9) 0.33(7) 0.20(5) 0.07(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.354(14) . ? C1 O3 1.372(12) . ? C1 C2 1.415(14) . ? C2 C3 1.388(15) . ? C2 C7 1.473(14) . ? C3 C4 1.379(15) . ? C3 H3 0.9300 . ? C4 C5 1.398(15) . ? C4 C12 1.496(16) . ? C5 C6 1.402(16) . ? C5 H5 0.9300 . ? C6 C16 1.535(15) . ? C7 N1 1.511(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N1 1.482(12) . ? C8 C9 1.533(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O5 1.198(14) . ? C9 O4 1.311(15) . ? C10 N1 1.460(12) . ? C10 C11 1.524(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O7 1.234(13) . ? C11 O6 1.260(13) . ? C12 C13 1.435(19) . ? C12 C15 1.47(2) . ? C12 C14 1.52(2) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.522(16) . ? C16 C19 1.539(16) . ? C16 C18 1.564(16) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O20 1.37(2) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O10 1.362(13) . ? C21 C22 1.369(15) . ? C21 C26 1.404(15) . ? C22 C23 1.376(16) . ? C22 C27 1.516(14) . ? C23 C24 1.373(15) . ? C23 H23 0.9300 . ? C24 C25 1.375(17) . ? C24 C32 1.55(2) . ? C25 C26 1.374(18) . ? C25 H25 0.9300 . ? C26 C36 1.526(17) . ? C27 N2 1.502(13) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.480(17) . ? C28 N2 1.500(14) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O12 1.188(12) . ? C29 O11 1.327(15) . ? C30 N2 1.486(14) . ? C30 C31 1.52(2) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 O13 1.23(2) . ? C31 O14 1.255(18) . ? C32 C34 1.43(2) . ? C32 C33 1.55(2) . ? C32 C35 1.56(3) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C38 1.47(2) . ? C36 C39 1.55(2) . ? C36 C37 1.575(18) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? N1 Mo1 2.344(9) . ? N2 Mo2 2.308(10) . ? O1 Mo1 1.691(8) . ? O2 Mo1 1.679(7) . ? O1W Co1 2.086(15) . ? O3 Mo1 1.896(7) . ? O2W Co1 2.064(11) . ? O4 Mo1 2.075(8) . ? O3W Co1 2.126(8) . ? O4W Co1 2.099(10) . ? O6 Mo1 2.187(7) . ? O7 Co1 2.097(8) . ? O8 Mo2 1.704(9) . ? O9 Mo2 1.711(8) . ? O10 Mo2 1.871(8) . ? O11 Mo2 2.023(8) . ? O13 Mo2 2.195(11) . ? O20 Co1 2.062(15) . ? O40A O40B 0.52(2) . ? O40A C40 1.43(2) . ? O40B C40 1.37(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 O3 121.7(10) . . ? C6 C1 C2 121.5(10) . . ? O3 C1 C2 116.9(9) . . ? C3 C2 C1 118.1(10) . . ? C3 C2 C7 122.2(10) . . ? C1 C2 C7 119.6(9) . . ? C4 C3 C2 123.0(11) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C3 C4 C5 115.8(9) . . ? C3 C4 C12 122.4(11) . . ? C5 C4 C12 121.7(10) . . ? C4 C5 C6 123.7(10) . . ? C4 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C1 C6 C5 117.6(11) . . ? C1 C6 C16 121.2(10) . . ? C5 C6 C16 121.2(10) . . ? C2 C7 N1 112.8(8) . . ? C2 C7 H7A 109.0 . . ? N1 C7 H7A 109.0 . . ? C2 C7 H7B 109.0 . . ? N1 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C9 107.6(9) . . ? N1 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? N1 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O5 C9 O4 124.3(12) . . ? O5 C9 C8 121.8(13) . . ? O4 C9 C8 114.0(11) . . ? N1 C10 C11 113.3(9) . . ? N1 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? N1 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? O7 C11 O6 126.6(11) . . ? O7 C11 C10 116.8(11) . . ? O6 C11 C10 116.6(10) . . ? C13 C12 C15 106.4(15) . . ? C13 C12 C4 117.6(12) . . ? C15 C12 C4 110.3(11) . . ? C13 C12 C14 107.4(15) . . ? C15 C12 C14 104.9(16) . . ? C4 C12 C14 109.5(11) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C6 109.7(9) . . ? C17 C16 C19 109.4(10) . . ? C6 C16 C19 111.4(10) . . ? C17 C16 C18 107.0(10) . . ? C6 C16 C18 111.1(9) . . ? C19 C16 C18 108.3(10) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O20 C20 H20A 109.5 . . ? O20 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O20 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O10 C21 C22 120.7(9) . . ? O10 C21 C26 118.0(10) . . ? C22 C21 C26 121.2(11) . . ? C21 C22 C23 119.9(10) . . ? C21 C22 C27 121.4(10) . . ? C23 C22 C27 118.5(10) . . ? C24 C23 C22 120.9(12) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 117.8(12) . . ? C23 C24 C32 119.0(12) . . ? C25 C24 C32 123.2(11) . . ? C24 C25 C26 123.9(11) . . ? C24 C25 H25 118.0 . . ? C26 C25 H25 118.0 . . ? C25 C26 C21 116.1(12) . . ? C25 C26 C36 121.8(10) . . ? C21 C26 C36 122.1(12) . . ? N2 C27 C22 112.3(9) . . ? N2 C27 H27A 109.1 . . ? C22 C27 H27A 109.1 . . ? N2 C27 H27B 109.1 . . ? C22 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C29 C28 N2 111.7(10) . . ? C29 C28 H28A 109.3 . . ? N2 C28 H28A 109.3 . . ? C29 C28 H28B 109.3 . . ? N2 C28 H28B 109.3 . . ? H28A C28 H28B 107.9 . . ? O12 C29 O11 123.5(12) . . ? O12 C29 C28 122.1(12) . . ? O11 C29 C28 114.5(9) . . ? N2 C30 C31 111.9(12) . . ? N2 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? N2 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? O13 C31 O14 127.5(17) . . ? O13 C31 C30 119.5(14) . . ? O14 C31 C30 113.0(18) . . ? C34 C32 C24 115.1(13) . . ? C34 C32 C33 111.5(19) . . ? C24 C32 C33 110.6(16) . . ? C34 C32 C35 109(2) . . ? C24 C32 C35 107.5(16) . . ? C33 C32 C35 102(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 C26 110.7(13) . . ? C38 C36 C39 111.1(15) . . ? C26 C36 C39 110.9(12) . . ? C38 C36 C37 106.5(13) . . ? C26 C36 C37 111.8(12) . . ? C39 C36 C37 105.6(12) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C10 N1 C8 110.4(8) . . ? C10 N1 C7 111.8(8) . . ? C8 N1 C7 112.8(8) . . ? C10 N1 Mo1 112.4(6) . . ? C8 N1 Mo1 101.9(6) . . ? C7 N1 Mo1 107.0(6) . . ? C30 N2 C28 109.8(9) . . ? C30 N2 C27 110.4(8) . . ? C28 N2 C27 110.7(9) . . ? C30 N2 Mo2 112.6(7) . . ? C28 N2 Mo2 102.2(6) . . ? C27 N2 Mo2 110.8(6) . . ? C1 O3 Mo1 136.8(7) . . ? C9 O4 Mo1 119.8(7) . . ? C11 O6 Mo1 123.9(7) . . ? C11 O7 Co1 127.6(8) . . ? C21 O10 Mo2 139.7(7) . . ? C29 O11 Mo2 120.0(7) . . ? C31 O13 Mo2 122.1(10) . . ? C20 O20 Co1 129.3(13) . . ? O20 Co1 O2W 93.2(6) . . ? O20 Co1 O1W 178.8(7) . . ? O2W Co1 O1W 87.9(7) . . ? O20 Co1 O7 90.2(4) . . ? O2W Co1 O7 93.4(4) . . ? O1W Co1 O7 89.1(5) . . ? O20 Co1 O4W 90.6(7) . . ? O2W Co1 O4W 175.8(7) . . ? O1W Co1 O4W 88.4(7) . . ? O7 Co1 O4W 88.5(4) . . ? O20 Co1 O3W 87.8(4) . . ? O2W Co1 O3W 86.0(4) . . ? O1W Co1 O3W 92.8(5) . . ? O7 Co1 O3W 177.9(5) . . ? O4W Co1 O3W 92.2(4) . . ? O2 Mo1 O1 106.0(4) . . ? O2 Mo1 O3 98.7(3) . . ? O1 Mo1 O3 105.1(4) . . ? O2 Mo1 O4 90.8(3) . . ? O1 Mo1 O4 94.7(4) . . ? O3 Mo1 O4 154.5(3) . . ? O2 Mo1 O6 163.3(4) . . ? O1 Mo1 O6 89.4(4) . . ? O3 Mo1 O6 83.1(3) . . ? O4 Mo1 O6 81.2(3) . . ? O2 Mo1 N1 91.2(4) . . ? O1 Mo1 N1 158.3(3) . . ? O3 Mo1 N1 84.6(3) . . ? O4 Mo1 N1 71.5(3) . . ? O6 Mo1 N1 72.3(3) . . ? O8 Mo2 O9 105.6(5) . . ? O8 Mo2 O10 103.6(4) . . ? O9 Mo2 O10 99.0(4) . . ? O8 Mo2 O11 95.2(4) . . ? O9 Mo2 O11 91.1(4) . . ? O10 Mo2 O11 155.3(3) . . ? O8 Mo2 O13 90.6(5) . . ? O9 Mo2 O13 162.6(4) . . ? O10 Mo2 O13 83.2(4) . . ? O11 Mo2 O13 80.7(4) . . ? O8 Mo2 N2 162.1(4) . . ? O9 Mo2 N2 89.4(4) . . ? O10 Mo2 N2 83.2(3) . . ? O11 Mo2 N2 74.4(3) . . ? O13 Mo2 N2 73.6(4) . . ? O40B O40A C40 73(3) . . ? O40A O40B C40 86(3) . . ? O40B C40 O40A 21.1(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -4.5(15) . . . . ? O3 C1 C2 C3 176.1(9) . . . . ? C6 C1 C2 C7 174.0(10) . . . . ? O3 C1 C2 C7 -5.4(14) . . . . ? C1 C2 C3 C4 2.6(16) . . . . ? C7 C2 C3 C4 -175.9(10) . . . . ? C2 C3 C4 C5 -1.5(16) . . . . ? C2 C3 C4 C12 -177.4(11) . . . . ? C3 C4 C5 C6 2.3(17) . . . . ? C12 C4 C5 C6 178.3(12) . . . . ? O3 C1 C6 C5 -175.4(10) . . . . ? C2 C1 C6 C5 5.2(16) . . . . ? O3 C1 C6 C16 3.3(16) . . . . ? C2 C1 C6 C16 -176.1(10) . . . . ? C4 C5 C6 C1 -4.2(17) . . . . ? C4 C5 C6 C16 177.1(10) . . . . ? C3 C2 C7 N1 -119.1(11) . . . . ? C1 C2 C7 N1 62.5(12) . . . . ? N1 C8 C9 O5 154.1(12) . . . . ? N1 C8 C9 O4 -26.1(14) . . . . ? N1 C10 C11 O7 176.3(11) . . . . ? N1 C10 C11 O6 -3.9(15) . . . . ? C3 C4 C12 C13 -174.9(16) . . . . ? C5 C4 C12 C13 9(2) . . . . ? C3 C4 C12 C15 62.8(19) . . . . ? C5 C4 C12 C15 -112.9(16) . . . . ? C3 C4 C12 C14 -52.1(17) . . . . ? C5 C4 C12 C14 132.2(15) . . . . ? C1 C6 C16 C17 57.9(14) . . . . ? C5 C6 C16 C17 -123.4(12) . . . . ? C1 C6 C16 C19 -63.3(14) . . . . ? C5 C6 C16 C19 115.3(12) . . . . ? C1 C6 C16 C18 175.9(11) . . . . ? C5 C6 C16 C18 -5.4(16) . . . . ? O10 C21 C22 C23 175.3(11) . . . . ? C26 C21 C22 C23 -0.4(17) . . . . ? O10 C21 C22 C27 0.0(17) . . . . ? C26 C21 C22 C27 -175.8(10) . . . . ? C21 C22 C23 C24 -1.8(17) . . . . ? C27 C22 C23 C24 173.7(11) . . . . ? C22 C23 C24 C25 3.3(19) . . . . ? C22 C23 C24 C32 -179.0(13) . . . . ? C23 C24 C25 C26 -3(2) . . . . ? C32 C24 C25 C26 179.7(16) . . . . ? C24 C25 C26 C21 1(2) . . . . ? C24 C25 C26 C36 -179.9(14) . . . . ? O10 C21 C26 C25 -174.8(12) . . . . ? C22 C21 C26 C25 1.0(18) . . . . ? O10 C21 C26 C36 5.6(19) . . . . ? C22 C21 C26 C36 -178.5(13) . . . . ? C21 C22 C27 N2 -47.8(14) . . . . ? C23 C22 C27 N2 136.8(11) . . . . ? N2 C28 C29 O12 -159.3(12) . . . . ? N2 C28 C29 O11 20.0(15) . . . . ? N2 C30 C31 O13 6.0(18) . . . . ? N2 C30 C31 O14 -174.6(12) . . . . ? C23 C24 C32 C34 36(3) . . . . ? C25 C24 C32 C34 -146(2) . . . . ? C23 C24 C32 C33 163.7(17) . . . . ? C25 C24 C32 C33 -19(2) . . . . ? C23 C24 C32 C35 -85(2) . . . . ? C25 C24 C32 C35 92(2) . . . . ? C25 C26 C36 C38 -116.1(17) . . . . ? C21 C26 C36 C38 63.5(18) . . . . ? C25 C26 C36 C39 120.2(16) . . . . ? C21 C26 C36 C39 -60.3(19) . . . . ? C25 C26 C36 C37 3(2) . . . . ? C21 C26 C36 C37 -177.9(13) . . . . ? C11 C10 N1 C8 124.0(10) . . . . ? C11 C10 N1 C7 -109.5(10) . . . . ? C11 C10 N1 Mo1 10.9(11) . . . . ? C9 C8 N1 C10 -72.7(11) . . . . ? C9 C8 N1 C7 161.3(9) . . . . ? C9 C8 N1 Mo1 46.9(10) . . . . ? C2 C7 N1 C10 55.0(11) . . . . ? C2 C7 N1 C8 -179.8(9) . . . . ? C2 C7 N1 Mo1 -68.5(9) . . . . ? C31 C30 N2 C28 -117.2(11) . . . . ? C31 C30 N2 C27 120.4(10) . . . . ? C31 C30 N2 Mo2 -4.0(11) . . . . ? C29 C28 N2 C30 81.4(12) . . . . ? C29 C28 N2 C27 -156.4(10) . . . . ? C29 C28 N2 Mo2 -38.4(11) . . . . ? C22 C27 N2 C30 -60.5(12) . . . . ? C22 C27 N2 C28 177.6(9) . . . . ? C22 C27 N2 Mo2 65.0(9) . . . . ? C6 C1 O3 Mo1 140.3(9) . . . . ? C2 C1 O3 Mo1 -40.3(15) . . . . ? O5 C9 O4 Mo1 164.7(10) . . . . ? C8 C9 O4 Mo1 -15.2(13) . . . . ? O7 C11 O6 Mo1 173.4(11) . . . . ? C10 C11 O6 Mo1 -6.4(15) . . . . ? O6 C11 O7 Co1 -7(2) . . . . ? C10 C11 O7 Co1 172.3(8) . . . . ? C22 C21 O10 Mo2 26.2(19) . . . . ? C26 C21 O10 Mo2 -158.0(10) . . . . ? O12 C29 O11 Mo2 -165.4(10) . . . . ? C28 C29 O11 Mo2 15.3(14) . . . . ? O14 C31 O13 Mo2 175.6(13) . . . . ? C30 C31 O13 Mo2 -5.1(19) . . . . ? C20 O20 Co1 O2W 61.2(18) . . . . ? C20 O20 Co1 O1W -89(25) . . . . ? C20 O20 Co1 O7 -32.3(18) . . . . ? C20 O20 Co1 O4W -120.8(18) . . . . ? C20 O20 Co1 O3W 147.0(18) . . . . ? C11 O7 Co1 O20 105.3(13) . . . . ? C11 O7 Co1 O2W 12.1(13) . . . . ? C11 O7 Co1 O1W -75.8(13) . . . . ? C11 O7 Co1 O4W -164.2(13) . . . . ? C11 O7 Co1 O3W 86(10) . . . . ? C1 O3 Mo1 O2 114.2(10) . . . . ? C1 O3 Mo1 O1 -136.5(10) . . . . ? C1 O3 Mo1 O4 3.4(15) . . . . ? C1 O3 Mo1 O6 -49.0(10) . . . . ? C1 O3 Mo1 N1 23.8(10) . . . . ? C9 O4 Mo1 O2 -58.1(9) . . . . ? C9 O4 Mo1 O1 -164.2(9) . . . . ? C9 O4 Mo1 O3 54.4(12) . . . . ? C9 O4 Mo1 O6 107.1(8) . . . . ? C9 O4 Mo1 N1 32.9(8) . . . . ? C11 O6 Mo1 O2 -1.4(17) . . . . ? C11 O6 Mo1 O1 -158.7(9) . . . . ? C11 O6 Mo1 O3 96.0(9) . . . . ? C11 O6 Mo1 O4 -63.8(9) . . . . ? C11 O6 Mo1 N1 9.5(9) . . . . ? C10 N1 Mo1 O2 166.7(7) . . . . ? C8 N1 Mo1 O2 48.4(6) . . . . ? C7 N1 Mo1 O2 -70.2(6) . . . . ? C10 N1 Mo1 O1 23.6(14) . . . . ? C8 N1 Mo1 O1 -94.6(11) . . . . ? C7 N1 Mo1 O1 146.7(10) . . . . ? C10 N1 Mo1 O3 -94.7(7) . . . . ? C8 N1 Mo1 O3 147.1(6) . . . . ? C7 N1 Mo1 O3 28.5(6) . . . . ? C10 N1 Mo1 O4 76.2(7) . . . . ? C8 N1 Mo1 O4 -42.0(6) . . . . ? C7 N1 Mo1 O4 -160.7(6) . . . . ? C10 N1 Mo1 O6 -10.2(6) . . . . ? C8 N1 Mo1 O6 -128.4(6) . . . . ? C7 N1 Mo1 O6 112.9(6) . . . . ? C21 O10 Mo2 O8 157.8(13) . . . . ? C21 O10 Mo2 O9 -93.7(13) . . . . ? C21 O10 Mo2 O11 19.4(18) . . . . ? C21 O10 Mo2 O13 68.9(13) . . . . ? C21 O10 Mo2 N2 -5.4(13) . . . . ? C29 O11 Mo2 O8 165.5(9) . . . . ? C29 O11 Mo2 O9 59.8(9) . . . . ? C29 O11 Mo2 O10 -54.9(13) . . . . ? C29 O11 Mo2 O13 -104.8(9) . . . . ? C29 O11 Mo2 N2 -29.3(8) . . . . ? C31 O13 Mo2 O8 173.5(12) . . . . ? C31 O13 Mo2 O9 16(2) . . . . ? C31 O13 Mo2 O10 -82.9(12) . . . . ? C31 O13 Mo2 O11 78.4(12) . . . . ? C31 O13 Mo2 N2 2.0(11) . . . . ? C30 N2 Mo2 O8 -27.1(16) . . . . ? C28 N2 Mo2 O8 90.8(14) . . . . ? C27 N2 Mo2 O8 -151.3(12) . . . . ? C30 N2 Mo2 O9 -174.4(7) . . . . ? C28 N2 Mo2 O9 -56.6(7) . . . . ? C27 N2 Mo2 O9 61.4(7) . . . . ? C30 N2 Mo2 O10 86.4(7) . . . . ? C28 N2 Mo2 O10 -155.8(7) . . . . ? C27 N2 Mo2 O10 -37.8(7) . . . . ? C30 N2 Mo2 O11 -83.2(7) . . . . ? C28 N2 Mo2 O11 34.6(7) . . . . ? C27 N2 Mo2 O11 152.6(7) . . . . ? C30 N2 Mo2 O13 1.5(7) . . . . ? C28 N2 Mo2 O13 119.3(7) . . . . ? C27 N2 Mo2 O13 -122.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.509 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.093 # Attachment 'Compound_2a.cif' data_mbsnk46 _database_code_depnum_ccdc_archive 'CCDC 640671' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H72 Co Mo2 N2 O22' _chemical_formula_weight 1183.81 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.735(3) _cell_length_b 11.7385(11) _cell_length_c 16.8051(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.542(9) _cell_angle_gamma 90.00 _cell_volume 2691.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 13 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1226 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-MACH3 _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5203 _diffrn_reflns_av_R_equivalents 0.0097 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4980 _reflns_number_gt 4488 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SIR-92 (J.Appl.Cryst.1993,26,343-350)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+1.3575P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 4980 _refine_ls_number_parameters 614 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6749(5) 0.5801(6) 0.3491(4) 0.0341(14) Uani 1 1 d . . . C2 C 0.7562(5) 0.5393(6) 0.3146(4) 0.0358(14) Uani 1 1 d . . . C3 C 0.7711(5) 0.4216(6) 0.3110(4) 0.0364(14) Uani 1 1 d . . . H3 H 0.8233 0.3939 0.2860 0.044 Uiso 1 1 calc R . . C4 C 0.7091(5) 0.3447(5) 0.3441(4) 0.0377(16) Uani 1 1 d . . . C5 C 0.6327(6) 0.3905(6) 0.3813(4) 0.0399(16) Uani 1 1 d . . . H5 H 0.5923 0.3407 0.4053 0.048 Uiso 1 1 calc R . . C6 C 0.6130(5) 0.5078(6) 0.3847(4) 0.0363(15) Uani 1 1 d . . . C7 C 0.8267(5) 0.6199(6) 0.2813(4) 0.0352(14) Uani 1 1 d . . . H7A H 0.8573 0.6675 0.3243 0.042 Uiso 1 1 calc R . . H7B H 0.8779 0.5762 0.2602 0.042 Uiso 1 1 calc R . . C8 C 0.8476(5) 0.7775(6) 0.1863(4) 0.0417(16) Uani 1 1 d . . . H8A H 0.8900 0.8095 0.2309 0.050 Uiso 1 1 calc R . . H8B H 0.8881 0.7397 0.1508 0.050 Uiso 1 1 calc R . . C9 C 0.7885(5) 0.8697(7) 0.1425(5) 0.0494(19) Uani 1 1 d . . . C10 C 0.7297(5) 0.6269(7) 0.1480(4) 0.0418(16) Uani 1 1 d . . . H10A H 0.7489 0.5477 0.1552 0.050 Uiso 1 1 calc R . . H10B H 0.7528 0.6537 0.0989 0.050 Uiso 1 1 calc R . . C11 C 0.6209(5) 0.6350(7) 0.1404(5) 0.0448(17) Uani 1 1 d . . . C12 C 0.7256(6) 0.2159(7) 0.3387(5) 0.0493(19) Uani 1 1 d . . . C13 C 0.8346(11) 0.1862(10) 0.3679(12) 0.126(6) Uani 1 1 d . . . H13A H 0.8490 0.2066 0.4233 0.189 Uiso 1 1 calc R . . H13B H 0.8769 0.2277 0.3366 0.189 Uiso 1 1 calc R . . H13C H 0.8449 0.1059 0.3618 0.189 Uiso 1 1 calc R . . C14 C 0.6626(13) 0.1454(9) 0.3802(11) 0.144(8) Uani 1 1 d . . . H14A H 0.6617 0.1733 0.4339 0.216 Uiso 1 1 calc R . . H14B H 0.6865 0.0685 0.3820 0.216 Uiso 1 1 calc R . . H14C H 0.5974 0.1473 0.3527 0.216 Uiso 1 1 calc R . . C15 C 0.714(2) 0.1799(11) 0.2500(10) 0.194(12) Uani 1 1 d . . . H15A H 0.7635 0.1257 0.2411 0.290 Uiso 1 1 calc R . . H15B H 0.7193 0.2456 0.2169 0.290 Uiso 1 1 calc R . . H15C H 0.6502 0.1458 0.2368 0.290 Uiso 1 1 calc R . . C16 C 0.5296(5) 0.5537(6) 0.4298(5) 0.0450(17) Uani 1 1 d . . . C17 C 0.4775(7) 0.4562(9) 0.4712(6) 0.068(3) Uani 1 1 d . . . H17A H 0.5252 0.4135 0.5053 0.102 Uiso 1 1 calc R . . H17B H 0.4449 0.4067 0.4312 0.102 Uiso 1 1 calc R . . H17C H 0.4303 0.4883 0.5028 0.102 Uiso 1 1 calc R . . C18 C 0.4532(6) 0.6172(9) 0.3737(6) 0.064(2) Uani 1 1 d . . . H18A H 0.4009 0.6417 0.4029 0.096 Uiso 1 1 calc R . . H18B H 0.4277 0.5675 0.3310 0.096 Uiso 1 1 calc R . . H18C H 0.4830 0.6824 0.3518 0.096 Uiso 1 1 calc R . . C19 C 0.5692(7) 0.6353(8) 0.4963(5) 0.062(2) Uani 1 1 d . . . H19A H 0.6166 0.5966 0.5331 0.093 Uiso 1 1 calc R . . H19B H 0.5162 0.6615 0.5243 0.093 Uiso 1 1 calc R . . H19C H 0.5996 0.6993 0.4735 0.093 Uiso 1 1 calc R . . C20 C 0.4633(13) 0.3858(16) 0.1857(9) 0.134(6) Uani 1 1 d . . . H20A H 0.5130 0.4414 0.2016 0.200 Uiso 1 1 calc R . . H20B H 0.4929 0.3121 0.1832 0.200 Uiso 1 1 calc R . . H20C H 0.4166 0.3844 0.2242 0.200 Uiso 1 1 calc R . . C21 C 0.0594(6) 0.2493(7) 0.2623(4) 0.0444(17) Uani 1 1 d . . . C22 C 0.0348(5) 0.1488(7) 0.2218(4) 0.0429(16) Uani 1 1 d . . . C23 C 0.0633(6) 0.0440(7) 0.2580(5) 0.0506(19) Uani 1 1 d . . . H23 H 0.0500 -0.0235 0.2299 0.061 Uiso 1 1 calc R . . C24 C 0.1102(7) 0.0407(8) 0.3341(5) 0.057(2) Uani 1 1 d . . . C25 C 0.1355(6) 0.1422(8) 0.3719(5) 0.055(2) Uani 1 1 d . . . H25 H 0.1701 0.1393 0.4228 0.067 Uiso 1 1 calc R . . C26 C 0.1122(6) 0.2498(7) 0.3385(5) 0.0487(19) Uani 1 1 d . . . C27 C -0.0276(5) 0.1468(7) 0.1409(4) 0.0395(15) Uani 1 1 d . . . H27A H -0.0261 0.0707 0.1187 0.047 Uiso 1 1 calc R . . H27B H -0.0950 0.1637 0.1488 0.047 Uiso 1 1 calc R . . C28 C -0.0615(6) 0.2292(7) 0.0057(4) 0.0450(17) Uani 1 1 d . . . H28A H -0.1281 0.2163 0.0176 0.054 Uiso 1 1 calc R . . H28B H -0.0437 0.1674 -0.0281 0.054 Uiso 1 1 calc R . . C29 C -0.0563(6) 0.3407(7) -0.0381(5) 0.0488(19) Uani 1 1 d . . . C30 C 0.1076(5) 0.2042(7) 0.0654(5) 0.0466(18) Uani 1 1 d . . . H30A H 0.1076 0.1850 0.0092 0.056 Uiso 1 1 calc R . . H30B H 0.1304 0.1380 0.0966 0.056 Uiso 1 1 calc R . . C31 C 0.1777(6) 0.3006(10) 0.0855(6) 0.064(2) Uani 1 1 d . . . C32 C 0.1382(10) -0.0770(11) 0.3739(6) 0.085(4) Uani 1 1 d . . . C33 C 0.1549(18) -0.0591(15) 0.4647(9) 0.196(12) Uani 1 1 d . . . H33A H 0.1018 -0.0155 0.4815 0.295 Uiso 1 1 calc R . . H33B H 0.2154 -0.0190 0.4783 0.295 Uiso 1 1 calc R . . H33C H 0.1580 -0.1318 0.4911 0.295 Uiso 1 1 calc R . . C34 C 0.0670(17) -0.1628(16) 0.3532(14) 0.233(16) Uani 1 1 d . . . H34A H 0.0517 -0.1653 0.2960 0.349 Uiso 1 1 calc R . . H34B H 0.0087 -0.1459 0.3775 0.349 Uiso 1 1 calc R . . H34C H 0.0925 -0.2353 0.3720 0.349 Uiso 1 1 calc R . . C35 C 0.2336(19) -0.1158(17) 0.3464(18) 0.214(13) Uani 1 1 d . . . H35A H 0.2411 -0.1964 0.3549 0.321 Uiso 1 1 calc R . . H35B H 0.2871 -0.0765 0.3764 0.321 Uiso 1 1 calc R . . H35C H 0.2335 -0.0993 0.2905 0.321 Uiso 1 1 calc R . . C36 C 0.1399(8) 0.3614(9) 0.3823(6) 0.067(3) Uani 1 1 d . . . C37 C 0.1948(10) 0.3405(11) 0.4668(7) 0.101(5) Uani 1 1 d . . . H37A H 0.1960 0.4096 0.4974 0.151 Uiso 1 1 calc R . . H37B H 0.2608 0.3167 0.4619 0.151 Uiso 1 1 calc R . . H37C H 0.1618 0.2822 0.4934 0.151 Uiso 1 1 calc R . . C38 C 0.0537(9) 0.4373(11) 0.3916(8) 0.100(4) Uani 1 1 d . . . H38A H 0.0281 0.4669 0.3402 0.150 Uiso 1 1 calc R . . H38B H 0.0741 0.4992 0.4269 0.150 Uiso 1 1 calc R . . H38C H 0.0037 0.3942 0.4136 0.150 Uiso 1 1 calc R . . C39 C 0.2151(12) 0.4240(15) 0.3356(10) 0.129(6) Uani 1 1 d . . . H39A H 0.1830 0.4501 0.2852 0.194 Uiso 1 1 calc R . . H39B H 0.2670 0.3726 0.3264 0.194 Uiso 1 1 calc R . . H39C H 0.2417 0.4879 0.3663 0.194 Uiso 1 1 calc R . . C40 C 0.646(2) 0.537(3) 0.813(2) 0.29(2) Uani 1 1 d . . . H40A H 0.6481 0.5978 0.7755 0.442 Uiso 1 1 calc R . . H40B H 0.5995 0.4807 0.7920 0.442 Uiso 1 1 calc R . . H40C H 0.7101 0.5022 0.8226 0.442 Uiso 1 1 calc R . . N1 N 0.7774(4) 0.6944(5) 0.2163(3) 0.0321(11) Uani 1 1 d . . . N2 N 0.0056(4) 0.2306(5) 0.0810(3) 0.0383(13) Uani 1 1 d . . . O1 O 0.5671(4) 0.8952(5) 0.2784(4) 0.0602(15) Uani 1 1 d . . . O2 O 0.7605(4) 0.8890(4) 0.3222(3) 0.0534(14) Uani 1 1 d . . . O1W O 0.4357(8) 0.7306(11) -0.0088(7) 0.138(4) Uani 1 1 d D . . O3 O 0.6589(4) 0.6953(4) 0.3475(3) 0.0422(11) Uani 1 1 d . . . O2W O 0.4499(6) 0.4935(11) -0.0537(5) 0.117(4) Uani 1 1 d . . . O4 O 0.7003(4) 0.8860(4) 0.1639(3) 0.0487(13) Uani 1 1 d . . . O3W O 0.2706(4) 0.5627(6) 0.0200(4) 0.0731(19) Uani 1 1 d . . . O5 O 0.8199(4) 0.9265(7) 0.0908(4) 0.077(2) Uani 1 1 d . . . O4W O 0.3898(5) 0.6624(11) 0.1515(6) 0.127(4) Uani 1 1 d . . . O6 O 0.5826(3) 0.7003(5) 0.1897(3) 0.0474(12) Uani 1 1 d . . . O7 O 0.5750(4) 0.5777(6) 0.0874(4) 0.072(2) Uani 1 1 d . . . O6W O 0.2021(6) 0.6646(12) 0.1690(7) 0.137(4) Uani 1 1 d . . . O8 O 0.0076(6) 0.5584(6) 0.1452(4) 0.0760(19) Uani 1 1 d . . . O9 O -0.1345(4) 0.3957(6) 0.1250(3) 0.0590(16) Uani 1 1 d . . . O10 O 0.0284(5) 0.3509(5) 0.2283(3) 0.0542(14) Uani 1 1 d . . . O11 O -0.0236(4) 0.4261(5) 0.0052(3) 0.0538(14) Uani 1 1 d . . . O12 O -0.0832(5) 0.3469(6) -0.1095(3) 0.076(2) Uani 1 1 d . . . O13 O 0.1444(4) 0.3940(6) 0.1088(4) 0.0649(17) Uani 1 1 d . . . O14 O 0.2629(4) 0.2816(7) 0.0758(6) 0.102(3) Uani 1 1 d . . . O20 O 0.4149(6) 0.4149(10) 0.1093(6) 0.113(3) Uani 1 1 d . . . O40 O 0.6193(13) 0.580(2) 0.8861(13) 0.223(10) Uani 1 1 d . . . H40 H 0.6636 0.6195 0.9077 0.335 Uiso 1 1 calc R . . Co1 Co 0.42360(9) 0.57258(12) 0.05249(8) 0.0656(4) Uani 1 1 d . . . Mo1 Mo 0.66780(4) 0.81559(4) 0.27258(3) 0.03722(16) Uani 1 1 d . . . Mo2 Mo -0.01172(5) 0.41622(5) 0.12720(4) 0.04497(18) Uani 1 1 d . . . O5W O 0.299(2) 0.897(3) -0.006(2) 0.47(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(3) 0.025(3) 0.039(3) -0.001(3) 0.007(3) 0.000(3) C2 0.041(4) 0.026(3) 0.042(3) -0.002(3) 0.010(3) -0.007(3) C3 0.044(4) 0.022(3) 0.044(3) -0.001(3) 0.010(3) 0.006(3) C4 0.051(4) 0.021(4) 0.043(4) 0.000(2) 0.015(3) -0.001(3) C5 0.048(4) 0.031(4) 0.042(4) 0.001(3) 0.012(3) -0.009(3) C6 0.044(4) 0.028(3) 0.038(3) -0.007(3) 0.013(3) -0.004(3) C7 0.031(3) 0.028(3) 0.046(4) 0.010(3) 0.001(3) -0.001(3) C8 0.037(4) 0.035(4) 0.052(4) 0.013(3) -0.002(3) -0.012(3) C9 0.037(4) 0.050(4) 0.058(4) 0.014(4) -0.008(3) -0.013(3) C10 0.040(4) 0.043(4) 0.043(4) -0.011(3) 0.006(3) -0.002(3) C11 0.036(4) 0.042(4) 0.055(4) 0.000(4) -0.001(3) -0.002(3) C12 0.064(5) 0.030(4) 0.059(5) -0.006(3) 0.025(4) -0.005(4) C13 0.108(10) 0.039(6) 0.232(19) -0.003(9) 0.021(11) 0.006(6) C14 0.216(17) 0.034(5) 0.215(17) 0.015(8) 0.168(15) 0.019(8) C15 0.44(4) 0.038(6) 0.126(13) -0.020(7) 0.118(18) -0.003(13) C16 0.046(4) 0.032(4) 0.060(4) -0.008(3) 0.022(3) -0.002(3) C17 0.060(5) 0.063(6) 0.090(7) 0.002(5) 0.043(5) -0.003(4) C18 0.045(5) 0.057(5) 0.092(6) 0.003(5) 0.014(4) 0.004(4) C19 0.076(6) 0.053(5) 0.063(5) -0.016(4) 0.031(4) 0.000(5) C20 0.143(13) 0.127(14) 0.119(11) 0.026(10) -0.038(10) -0.005(11) C21 0.044(4) 0.053(5) 0.036(4) 0.002(3) 0.005(3) 0.000(3) C22 0.042(4) 0.051(4) 0.036(3) 0.001(3) 0.008(3) -0.002(3) C23 0.059(5) 0.045(4) 0.046(4) 0.000(3) 0.000(4) 0.005(4) C24 0.065(5) 0.056(5) 0.048(4) 0.010(4) -0.003(4) -0.008(4) C25 0.058(5) 0.069(6) 0.036(4) -0.001(4) -0.007(3) 0.003(4) C26 0.042(4) 0.056(5) 0.045(4) -0.006(4) -0.004(3) -0.010(4) C27 0.037(4) 0.040(4) 0.042(4) 0.006(3) 0.006(3) -0.009(3) C28 0.053(4) 0.047(4) 0.035(3) -0.001(3) 0.004(3) -0.004(4) C29 0.046(4) 0.053(5) 0.048(4) 0.008(4) 0.008(3) 0.000(4) C30 0.043(4) 0.052(5) 0.047(4) -0.002(3) 0.017(3) -0.002(4) C31 0.039(4) 0.076(7) 0.077(6) 0.010(5) 0.004(4) 0.001(5) C32 0.113(9) 0.069(7) 0.065(6) 0.026(6) -0.028(6) -0.019(7) C33 0.37(3) 0.100(12) 0.089(10) 0.043(9) -0.085(15) -0.061(17) C34 0.25(2) 0.123(15) 0.27(3) 0.136(17) -0.19(2) -0.111(16) C35 0.23(2) 0.107(16) 0.32(3) 0.094(19) 0.11(2) 0.079(17) C36 0.070(6) 0.067(6) 0.059(5) -0.024(5) -0.016(5) 0.002(5) C37 0.136(11) 0.080(9) 0.073(7) -0.025(6) -0.049(7) 0.003(8) C38 0.088(8) 0.092(9) 0.108(9) -0.051(8) -0.038(7) 0.021(7) C39 0.138(13) 0.126(13) 0.123(11) -0.034(10) 0.006(9) -0.086(11) C40 0.26(3) 0.25(3) 0.42(5) -0.22(4) 0.22(3) -0.13(3) N1 0.026(3) 0.031(3) 0.039(3) 0.002(2) 0.003(2) -0.006(2) N2 0.041(3) 0.037(3) 0.038(3) 0.004(2) 0.007(2) -0.003(3) O1 0.067(4) 0.039(3) 0.075(4) -0.004(3) 0.008(3) 0.015(3) O2 0.069(4) 0.031(3) 0.057(3) -0.004(2) -0.010(3) -0.011(2) O1W 0.107(7) 0.133(9) 0.166(10) 0.033(8) -0.022(7) -0.038(7) O3 0.051(3) 0.022(2) 0.054(3) -0.005(2) 0.012(2) 0.001(2) O2W 0.074(5) 0.189(11) 0.087(5) -0.077(7) 0.003(4) -0.022(6) O4 0.053(3) 0.038(3) 0.053(3) 0.014(2) -0.005(2) 0.001(2) O3W 0.047(3) 0.084(5) 0.082(4) -0.028(4) -0.020(3) 0.009(3) O5 0.055(3) 0.083(5) 0.093(4) 0.058(4) 0.001(3) -0.002(4) O4W 0.047(4) 0.210(12) 0.120(7) -0.103(8) -0.004(4) -0.003(5) O6 0.030(2) 0.049(3) 0.062(3) -0.016(3) 0.001(2) -0.004(2) O7 0.048(3) 0.087(5) 0.077(4) -0.051(4) -0.013(3) -0.005(3) O6W 0.064(5) 0.169(12) 0.181(10) 0.035(9) 0.021(6) -0.011(6) O8 0.108(5) 0.043(4) 0.076(4) 0.002(3) 0.009(4) -0.003(4) O9 0.040(3) 0.079(4) 0.059(3) -0.007(3) 0.010(2) 0.007(3) O10 0.074(4) 0.045(3) 0.041(3) -0.003(2) 0.000(3) 0.004(3) O11 0.064(4) 0.050(3) 0.048(3) 0.010(3) 0.009(3) 0.002(3) O12 0.098(5) 0.082(5) 0.045(3) 0.017(3) -0.006(3) -0.007(4) O13 0.045(3) 0.064(4) 0.085(4) 0.004(3) 0.003(3) -0.017(3) O14 0.034(3) 0.084(6) 0.185(9) 0.017(6) 0.008(4) -0.001(3) O20 0.077(5) 0.123(7) 0.127(7) 0.032(7) -0.037(5) -0.014(6) O40 0.195(15) 0.24(2) 0.261(19) -0.092(16) 0.135(15) -0.107(15) Co1 0.0428(6) 0.0786(9) 0.0710(8) -0.0301(7) -0.0125(5) 0.0006(6) Mo1 0.0420(3) 0.0227(2) 0.0454(3) -0.0020(2) -0.0017(2) 0.0005(3) Mo2 0.0506(4) 0.0376(3) 0.0468(3) -0.0012(3) 0.0059(3) 0.0000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O3 1.369(8) . ? C1 C6 1.386(10) . ? C1 C2 1.400(10) . ? C2 C3 1.399(10) . ? C2 C7 1.506(9) . ? C3 C4 1.399(10) . ? C3 H3 0.9300 . ? C4 C5 1.391(10) . ? C4 C12 1.533(10) . ? C5 C6 1.405(10) . ? C5 H5 0.9300 . ? C6 C16 1.540(9) . ? C7 N1 1.500(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.495(10) . ? C8 N1 1.499(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O5 1.212(10) . ? C9 O4 1.316(10) . ? C10 N1 1.483(8) . ? C10 C11 1.489(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O7 1.230(9) . ? C11 O6 1.285(9) . ? C12 C14 1.435(14) . ? C12 C15 1.539(17) . ? C12 C13 1.561(17) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C18 1.523(12) . ? C16 C19 1.524(11) . ? C16 C17 1.556(11) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O20 1.419(16) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O10 1.369(10) . ? C21 C22 1.384(11) . ? C21 C26 1.399(11) . ? C22 C23 1.408(11) . ? C22 C27 1.524(9) . ? C23 C24 1.366(11) . ? C23 H23 0.9300 . ? C24 C25 1.376(13) . ? C24 C32 1.564(14) . ? C25 C26 1.405(13) . ? C25 H25 0.9300 . ? C26 C36 1.529(12) . ? C27 N2 1.514(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N2 1.478(9) . ? C28 C29 1.507(11) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O12 1.218(9) . ? C29 O11 1.288(10) . ? C30 N2 1.488(9) . ? C30 C31 1.499(13) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 O14 1.221(11) . ? C31 O13 1.266(13) . ? C32 C34 1.419(18) . ? C32 C35 1.51(2) . ? C32 C33 1.531(18) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C38 1.505(15) . ? C36 C37 1.549(13) . ? C36 C39 1.551(18) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O40 1.41(2) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? N1 Mo1 2.347(5) . ? N2 Mo2 2.334(6) . ? O1 Mo1 1.681(6) . ? O2 Mo1 1.679(5) . ? O1W Co1 2.137(12) . ? O3 Mo1 1.905(5) . ? O2W Co1 2.079(8) . ? O4 Mo1 2.098(5) . ? O3W Co1 2.113(6) . ? O4W Co1 2.067(8) . ? O6 Mo1 2.184(5) . ? O7 Co1 2.096(6) . ? O8 Mo2 1.711(7) . ? O9 Mo2 1.700(5) . ? O10 Mo2 1.888(5) . ? O11 Mo2 2.041(5) . ? O13 Mo2 2.217(6) . ? O20 Co1 2.093(11) . ? O40 H40 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C1 C6 120.5(6) . . ? O3 C1 C2 117.7(6) . . ? C6 C1 C2 121.8(6) . . ? C3 C2 C1 118.9(6) . . ? C3 C2 C7 120.1(6) . . ? C1 C2 C7 121.0(6) . . ? C4 C3 C2 121.5(6) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 116.9(6) . . ? C5 C4 C12 122.2(6) . . ? C3 C4 C12 120.9(6) . . ? C4 C5 C6 123.9(6) . . ? C4 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C1 C6 C5 116.9(6) . . ? C1 C6 C16 121.7(6) . . ? C5 C6 C16 121.4(6) . . ? N1 C7 C2 112.4(5) . . ? N1 C7 H7A 109.1 . . ? C2 C7 H7A 109.1 . . ? N1 C7 H7B 109.1 . . ? C2 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C9 C8 N1 107.6(5) . . ? C9 C8 H8A 110.2 . . ? N1 C8 H8A 110.2 . . ? C9 C8 H8B 110.2 . . ? N1 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O5 C9 O4 122.0(7) . . ? O5 C9 C8 122.2(7) . . ? O4 C9 C8 115.7(6) . . ? N1 C10 C11 112.5(6) . . ? N1 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N1 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? O7 C11 O6 125.4(7) . . ? O7 C11 C10 117.0(7) . . ? O6 C11 C10 117.6(6) . . ? C14 C12 C4 116.0(7) . . ? C14 C12 C15 108.0(12) . . ? C4 C12 C15 109.1(8) . . ? C14 C12 C13 109.1(11) . . ? C4 C12 C13 110.2(8) . . ? C15 C12 C13 103.7(13) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C19 108.0(7) . . ? C18 C16 C6 111.4(6) . . ? C19 C16 C6 111.0(6) . . ? C18 C16 C17 108.5(7) . . ? C19 C16 C17 106.1(7) . . ? C6 C16 C17 111.6(6) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O20 C20 H20A 109.5 . . ? O20 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O20 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O10 C21 C22 119.4(6) . . ? O10 C21 C26 118.8(7) . . ? C22 C21 C26 121.8(7) . . ? C21 C22 C23 119.5(6) . . ? C21 C22 C27 122.2(7) . . ? C23 C22 C27 118.2(7) . . ? C24 C23 C22 120.5(8) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 118.4(8) . . ? C23 C24 C32 119.5(8) . . ? C25 C24 C32 122.1(7) . . ? C24 C25 C26 124.1(7) . . ? C24 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? C21 C26 C25 115.6(7) . . ? C21 C26 C36 121.3(8) . . ? C25 C26 C36 123.1(7) . . ? N2 C27 C22 113.7(6) . . ? N2 C27 H27A 108.8 . . ? C22 C27 H27A 108.8 . . ? N2 C27 H27B 108.8 . . ? C22 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? N2 C28 C29 110.4(6) . . ? N2 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? N2 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? O12 C29 O11 123.9(8) . . ? O12 C29 C28 120.5(8) . . ? O11 C29 C28 115.6(6) . . ? N2 C30 C31 113.3(7) . . ? N2 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? N2 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? O14 C31 O13 125.8(10) . . ? O14 C31 C30 115.6(10) . . ? O13 C31 C30 118.6(7) . . ? C34 C32 C35 108.0(19) . . ? C34 C32 C33 111.3(15) . . ? C35 C32 C33 108.0(17) . . ? C34 C32 C24 113.2(10) . . ? C35 C32 C24 108.4(11) . . ? C33 C32 C24 107.9(12) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 C26 113.6(8) . . ? C38 C36 C37 107.8(9) . . ? C26 C36 C37 112.0(9) . . ? C38 C36 C39 110.4(12) . . ? C26 C36 C39 107.8(9) . . ? C37 C36 C39 104.9(10) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O40 C40 H40A 109.5 . . ? O40 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O40 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C10 N1 C8 109.4(5) . . ? C10 N1 C7 112.0(5) . . ? C8 N1 C7 111.7(5) . . ? C10 N1 Mo1 112.9(4) . . ? C8 N1 Mo1 102.0(4) . . ? C7 N1 Mo1 108.5(4) . . ? C28 N2 C30 110.8(6) . . ? C28 N2 C27 110.9(6) . . ? C30 N2 C27 110.0(6) . . ? C28 N2 Mo2 102.6(5) . . ? C30 N2 Mo2 112.8(5) . . ? C27 N2 Mo2 109.6(4) . . ? C1 O3 Mo1 136.3(5) . . ? C9 O4 Mo1 118.4(4) . . ? C11 O6 Mo1 123.5(4) . . ? C11 O7 Co1 128.9(6) . . ? C21 O10 Mo2 140.7(5) . . ? C29 O11 Mo2 120.4(5) . . ? C31 O13 Mo2 122.3(5) . . ? C20 O20 Co1 125.5(10) . . ? C40 O40 H40 109.5 . . ? O4W Co1 O2W 174.6(5) . . ? O4W Co1 O20 93.1(5) . . ? O2W Co1 O20 91.2(5) . . ? O4W Co1 O7 93.8(3) . . ? O2W Co1 O7 89.4(3) . . ? O20 Co1 O7 90.3(3) . . ? O4W Co1 O3W 85.9(3) . . ? O2W Co1 O3W 91.0(3) . . ? O20 Co1 O3W 87.8(3) . . ? O7 Co1 O3W 178.1(3) . . ? O4W Co1 O1W 89.0(5) . . ? O2W Co1 O1W 86.8(5) . . ? O20 Co1 O1W 177.8(5) . . ? O7 Co1 O1W 88.9(4) . . ? O3W Co1 O1W 93.0(4) . . ? O2 Mo1 O1 105.6(3) . . ? O2 Mo1 O3 98.9(2) . . ? O1 Mo1 O3 105.0(3) . . ? O2 Mo1 O4 90.3(2) . . ? O1 Mo1 O4 95.2(3) . . ? O3 Mo1 O4 154.6(2) . . ? O2 Mo1 O6 163.0(2) . . ? O1 Mo1 O6 89.8(2) . . ? O3 Mo1 O6 83.8(2) . . ? O4 Mo1 O6 80.8(2) . . ? O2 Mo1 N1 91.5(2) . . ? O1 Mo1 N1 158.4(2) . . ? O3 Mo1 N1 84.80(19) . . ? O4 Mo1 N1 71.22(19) . . ? O6 Mo1 N1 71.89(18) . . ? O9 Mo2 O8 106.0(4) . . ? O9 Mo2 O10 98.6(3) . . ? O8 Mo2 O10 102.3(3) . . ? O9 Mo2 O11 91.2(2) . . ? O8 Mo2 O11 96.6(3) . . ? O10 Mo2 O11 155.3(2) . . ? O9 Mo2 O13 162.5(3) . . ? O8 Mo2 O13 90.4(3) . . ? O10 Mo2 O13 83.6(3) . . ? O11 Mo2 O13 80.5(2) . . ? O9 Mo2 N2 90.0(3) . . ? O8 Mo2 N2 161.7(3) . . ? O10 Mo2 N2 83.7(2) . . ? O11 Mo2 N2 73.6(2) . . ? O13 Mo2 N2 73.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 C1 C2 C3 -176.1(6) . . . . ? C6 C1 C2 C3 4.7(10) . . . . ? O3 C1 C2 C7 3.5(10) . . . . ? C6 C1 C2 C7 -175.7(6) . . . . ? C1 C2 C3 C4 -2.8(11) . . . . ? C7 C2 C3 C4 177.5(6) . . . . ? C2 C3 C4 C5 -0.5(11) . . . . ? C2 C3 C4 C12 179.2(7) . . . . ? C3 C4 C5 C6 2.3(11) . . . . ? C12 C4 C5 C6 -177.4(8) . . . . ? O3 C1 C6 C5 177.8(7) . . . . ? C2 C1 C6 C5 -3.0(11) . . . . ? O3 C1 C6 C16 -5.3(11) . . . . ? C2 C1 C6 C16 173.9(7) . . . . ? C4 C5 C6 C1 -0.6(12) . . . . ? C4 C5 C6 C16 -177.5(7) . . . . ? C3 C2 C7 N1 120.7(7) . . . . ? C1 C2 C7 N1 -58.9(8) . . . . ? N1 C8 C9 O5 -155.3(8) . . . . ? N1 C8 C9 O4 25.3(9) . . . . ? N1 C10 C11 O7 -177.0(7) . . . . ? N1 C10 C11 O6 2.6(10) . . . . ? C5 C4 C12 C14 -5.1(15) . . . . ? C3 C4 C12 C14 175.1(12) . . . . ? C5 C4 C12 C15 117.1(13) . . . . ? C3 C4 C12 C15 -62.7(14) . . . . ? C5 C4 C12 C13 -129.7(10) . . . . ? C3 C4 C12 C13 50.5(12) . . . . ? C1 C6 C16 C18 64.2(9) . . . . ? C5 C6 C16 C18 -119.1(8) . . . . ? C1 C6 C16 C19 -56.2(10) . . . . ? C5 C6 C16 C19 120.5(8) . . . . ? C1 C6 C16 C17 -174.4(7) . . . . ? C5 C6 C16 C17 2.4(11) . . . . ? O10 C21 C22 C23 -177.5(7) . . . . ? C26 C21 C22 C23 0.0(11) . . . . ? O10 C21 C22 C27 -1.1(11) . . . . ? C26 C21 C22 C27 176.4(7) . . . . ? C21 C22 C23 C24 3.5(12) . . . . ? C27 C22 C23 C24 -173.0(7) . . . . ? C22 C23 C24 C25 -4.9(14) . . . . ? C22 C23 C24 C32 178.1(9) . . . . ? C23 C24 C25 C26 2.9(14) . . . . ? C32 C24 C25 C26 179.9(10) . . . . ? O10 C21 C26 C25 175.6(7) . . . . ? C22 C21 C26 C25 -2.0(12) . . . . ? O10 C21 C26 C36 -3.0(12) . . . . ? C22 C21 C26 C36 179.4(8) . . . . ? C24 C25 C26 C21 0.5(13) . . . . ? C24 C25 C26 C36 179.1(10) . . . . ? C21 C22 C27 N2 48.1(9) . . . . ? C23 C22 C27 N2 -135.4(7) . . . . ? N2 C28 C29 O12 159.5(8) . . . . ? N2 C28 C29 O11 -21.6(10) . . . . ? N2 C30 C31 O14 178.0(8) . . . . ? N2 C30 C31 O13 -3.6(12) . . . . ? C23 C24 C32 C34 -37(2) . . . . ? C25 C24 C32 C34 146.5(17) . . . . ? C23 C24 C32 C35 83.1(17) . . . . ? C25 C24 C32 C35 -93.8(17) . . . . ? C23 C24 C32 C33 -160.2(13) . . . . ? C25 C24 C32 C33 22.9(17) . . . . ? C21 C26 C36 C38 55.5(13) . . . . ? C25 C26 C36 C38 -123.1(11) . . . . ? C21 C26 C36 C37 178.0(9) . . . . ? C25 C26 C36 C37 -0.6(14) . . . . ? C21 C26 C36 C39 -67.2(12) . . . . ? C25 C26 C36 C39 114.2(12) . . . . ? C11 C10 N1 C8 -123.5(6) . . . . ? C11 C10 N1 C7 112.1(7) . . . . ? C11 C10 N1 Mo1 -10.7(7) . . . . ? C9 C8 N1 C10 73.1(7) . . . . ? C9 C8 N1 C7 -162.4(6) . . . . ? C9 C8 N1 Mo1 -46.7(6) . . . . ? C2 C7 N1 C10 -59.4(7) . . . . ? C2 C7 N1 C8 177.5(6) . . . . ? C2 C7 N1 Mo1 65.9(6) . . . . ? C29 C28 N2 C30 -81.7(8) . . . . ? C29 C28 N2 C27 155.8(6) . . . . ? C29 C28 N2 Mo2 38.9(7) . . . . ? C31 C30 N2 C28 116.5(7) . . . . ? C31 C30 N2 C27 -120.6(7) . . . . ? C31 C30 N2 Mo2 2.1(8) . . . . ? C22 C27 N2 C28 -176.6(6) . . . . ? C22 C27 N2 C30 60.5(8) . . . . ? C22 C27 N2 Mo2 -64.0(7) . . . . ? C6 C1 O3 Mo1 -140.8(6) . . . . ? C2 C1 O3 Mo1 40.0(10) . . . . ? O5 C9 O4 Mo1 -163.8(7) . . . . ? C8 C9 O4 Mo1 15.7(9) . . . . ? O7 C11 O6 Mo1 -172.1(7) . . . . ? C10 C11 O6 Mo1 8.3(10) . . . . ? O6 C11 O7 Co1 4.5(14) . . . . ? C10 C11 O7 Co1 -175.9(6) . . . . ? C22 C21 O10 Mo2 -23.6(12) . . . . ? C26 C21 O10 Mo2 158.8(7) . . . . ? O12 C29 O11 Mo2 165.2(7) . . . . ? C28 C29 O11 Mo2 -13.7(9) . . . . ? O14 C31 O13 Mo2 -178.3(8) . . . . ? C30 C31 O13 Mo2 3.5(12) . . . . ? C20 O20 Co1 O4W -50.9(13) . . . . ? C20 O20 Co1 O2W 132.3(13) . . . . ? C20 O20 Co1 O7 42.9(13) . . . . ? C20 O20 Co1 O3W -136.7(13) . . . . ? C20 O20 Co1 O1W 110(10) . . . . ? C11 O7 Co1 O4W -11.8(9) . . . . ? C11 O7 Co1 O2W 163.8(9) . . . . ? C11 O7 Co1 O20 -105.0(9) . . . . ? C11 O7 Co1 O3W -93(8) . . . . ? C11 O7 Co1 O1W 77.1(9) . . . . ? C1 O3 Mo1 O2 -113.6(7) . . . . ? C1 O3 Mo1 O1 137.5(7) . . . . ? C1 O3 Mo1 O4 -3.6(10) . . . . ? C1 O3 Mo1 O6 49.4(7) . . . . ? C1 O3 Mo1 N1 -22.9(7) . . . . ? C9 O4 Mo1 O2 58.4(6) . . . . ? C9 O4 Mo1 O1 164.0(6) . . . . ? C9 O4 Mo1 O3 -53.4(8) . . . . ? C9 O4 Mo1 O6 -107.0(6) . . . . ? C9 O4 Mo1 N1 -33.1(5) . . . . ? C11 O6 Mo1 O2 2.8(12) . . . . ? C11 O6 Mo1 O1 157.6(6) . . . . ? C11 O6 Mo1 O3 -97.3(6) . . . . ? C11 O6 Mo1 O4 62.4(6) . . . . ? C11 O6 Mo1 N1 -10.7(6) . . . . ? C10 N1 Mo1 O2 -165.3(5) . . . . ? C8 N1 Mo1 O2 -48.1(4) . . . . ? C7 N1 Mo1 O2 69.9(4) . . . . ? C10 N1 Mo1 O1 -22.5(9) . . . . ? C8 N1 Mo1 O1 94.8(8) . . . . ? C7 N1 Mo1 O1 -147.2(7) . . . . ? C10 N1 Mo1 O3 95.9(5) . . . . ? C8 N1 Mo1 O3 -146.8(4) . . . . ? C7 N1 Mo1 O3 -28.9(4) . . . . ? C10 N1 Mo1 O4 -75.5(4) . . . . ? C8 N1 Mo1 O4 41.8(4) . . . . ? C7 N1 Mo1 O4 159.7(4) . . . . ? C10 N1 Mo1 O6 10.7(4) . . . . ? C8 N1 Mo1 O6 128.0(4) . . . . ? C7 N1 Mo1 O6 -114.0(4) . . . . ? C21 O10 Mo2 O9 92.8(9) . . . . ? C21 O10 Mo2 O8 -158.7(9) . . . . ? C21 O10 Mo2 O11 -19.4(12) . . . . ? C21 O10 Mo2 O13 -69.7(8) . . . . ? C21 O10 Mo2 N2 3.8(8) . . . . ? C29 O11 Mo2 O9 -61.4(6) . . . . ? C29 O11 Mo2 O8 -167.6(6) . . . . ? C29 O11 Mo2 O10 52.4(9) . . . . ? C29 O11 Mo2 O13 103.1(6) . . . . ? C29 O11 Mo2 N2 28.2(6) . . . . ? C31 O13 Mo2 O9 -14.7(13) . . . . ? C31 O13 Mo2 O8 -174.0(7) . . . . ? C31 O13 Mo2 O10 83.7(7) . . . . ? C31 O13 Mo2 O11 -77.3(7) . . . . ? C31 O13 Mo2 N2 -1.7(7) . . . . ? C28 N2 Mo2 O9 56.4(4) . . . . ? C30 N2 Mo2 O9 175.6(5) . . . . ? C27 N2 Mo2 O9 -61.4(4) . . . . ? C28 N2 Mo2 O8 -94.5(10) . . . . ? C30 N2 Mo2 O8 24.7(11) . . . . ? C27 N2 Mo2 O8 147.6(9) . . . . ? C28 N2 Mo2 O10 155.1(5) . . . . ? C30 N2 Mo2 O10 -85.7(5) . . . . ? C27 N2 Mo2 O10 37.2(4) . . . . ? C28 N2 Mo2 O11 -34.8(4) . . . . ? C30 N2 Mo2 O11 84.4(5) . . . . ? C27 N2 Mo2 O11 -152.7(5) . . . . ? C28 N2 Mo2 O13 -119.7(5) . . . . ? C30 N2 Mo2 O13 -0.5(4) . . . . ? C27 N2 Mo2 O13 122.5(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.112 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.084 data_mbsnk33 _database_code_depnum_ccdc_archive 'CCDC 640672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H70 Co Mo2 N2 O23' _chemical_formula_weight 1173.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a' _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 12.156(9) _cell_length_b 9.139(7) _cell_length_c 23.765(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.00(9) _cell_angle_gamma 90.00 _cell_volume 2630(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 12 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1214 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6737 _exptl_absorpt_correction_T_max 0.9191 _exptl_absorpt_process_details XABS2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-MACH3 _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5192 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0974 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4767 _reflns_number_gt 2759 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4767 _refine_ls_number_parameters 334 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1855 _refine_ls_R_factor_gt 0.1036 _refine_ls_wR_factor_ref 0.3244 _refine_ls_wR_factor_gt 0.2681 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9797(8) 0.4863(11) 0.7927(6) 0.043(3) Uani 1 1 d . . . C2 C 1.0149(9) 0.6303(11) 0.7813(6) 0.041(3) Uani 1 1 d . . . C3 C 1.0892(8) 0.6974(10) 0.8201(5) 0.036(3) Uani 1 1 d . . . H3 H 1.1135 0.7916 0.8129 0.043 Uiso 1 1 calc R . . C4 C 1.1292(9) 0.6268(12) 0.8700(6) 0.050(3) Uani 1 1 d . . . C5 C 1.0956(10) 0.4851(11) 0.8808(5) 0.040(3) Uani 1 1 d . . . H5 H 1.1236 0.4372 0.9135 0.048 Uiso 1 1 calc R . . C6 C 1.0180(8) 0.4130(11) 0.8415(6) 0.043(3) Uani 1 1 d . . . C7 C 0.9722(10) 0.7206(12) 0.7314(6) 0.047(3) Uani 1 1 d . . . H7A H 1.0312 0.7850 0.7218 0.057 Uiso 1 1 calc R . . H7B H 0.9132 0.7822 0.7431 0.057 Uiso 1 1 calc R . . C8 C 0.8814(10) 0.7477(14) 0.6356(6) 0.058(4) Uani 1 1 d . . . H8A H 0.8764 0.8433 0.6529 0.069 Uiso 1 1 calc R . . H8B H 0.9297 0.7558 0.6054 0.069 Uiso 1 1 calc R . . C9 C 0.7690(10) 0.7007(13) 0.6117(7) 0.053(3) Uani 1 1 d . . . C10 C 1.0177(9) 0.5535(14) 0.6563(6) 0.055(4) Uani 1 1 d . . . H10A H 1.0704 0.5238 0.6871 0.066 Uiso 1 1 calc R . . H10B H 1.0564 0.6132 0.6306 0.066 Uiso 1 1 calc R . . C11 C 0.9715(10) 0.4191(14) 0.6255(7) 0.056(4) Uani 1 1 d . . . C12 C 1.2121(10) 0.7020(12) 0.9123(6) 0.054(4) Uani 1 1 d D . . C13A C 1.320(2) 0.729(4) 0.8839(18) 0.093(12) Uani 0.50 1 d PD . . C13B C 1.323(3) 0.617(4) 0.924(3) 0.17(3) Uani 0.50 1 d P . . C14A C 1.164(3) 0.851(3) 0.9254(15) 0.076(10) Uani 0.50 1 d PD . . C14B C 1.243(3) 0.852(3) 0.8970(14) 0.082(12) Uani 0.50 1 d PD . . C15A C 1.252(5) 0.609(5) 0.964(2) 0.15(3) Uani 0.50 1 d PD . . C15B C 1.153(3) 0.726(6) 0.968(2) 0.121(18) Uani 0.50 1 d P . . C16 C 0.9779(9) 0.2575(12) 0.8548(6) 0.049(3) Uani 1 1 d . . . C17 C 1.0094(12) 0.1519(14) 0.8075(8) 0.076(5) Uani 1 1 d . . . H17A H 1.0880 0.1389 0.8103 0.115 Uiso 1 1 calc R . . H17B H 0.9854 0.1927 0.7713 0.115 Uiso 1 1 calc R . . H17C H 0.9741 0.0590 0.8117 0.115 Uiso 1 1 calc R . . C18 C 0.8524(11) 0.2598(16) 0.8565(8) 0.075(5) Uani 1 1 d . . . H18A H 0.8256 0.1615 0.8593 0.113 Uiso 1 1 calc R . . H18B H 0.8190 0.3042 0.8226 0.113 Uiso 1 1 calc R . . H18C H 0.8337 0.3152 0.8886 0.113 Uiso 1 1 calc R . . C19 C 1.0262(12) 0.2027(15) 0.9095(9) 0.097(7) Uani 1 1 d . . . H19A H 0.9918 0.1117 0.9179 0.145 Uiso 1 1 calc R . . H19B H 1.0143 0.2728 0.9384 0.145 Uiso 1 1 calc R . . H19C H 1.1040 0.1878 0.9079 0.145 Uiso 1 1 calc R . . Co1 Co 0.5000 0.5000 0.5000 0.0410(6) Uani 1 2 d S . . Mo1 Mo 0.79010(7) 0.48146(10) 0.70342(5) 0.0436(4) Uani 1 1 d . . . N1 N 0.9294(7) 0.6410(9) 0.6788(5) 0.047(3) Uani 1 1 d . . . O1 O 0.9090(6) 0.4141(8) 0.7515(4) 0.052(2) Uani 1 1 d . . . O2 O 0.6985(7) 0.3393(10) 0.6977(5) 0.073(3) Uani 1 1 d . . . O1W O 0.4727(6) 0.2715(8) 0.4864(4) 0.057(3) Uani 1 1 d . . . O3 O 0.7382(7) 0.6066(10) 0.7449(5) 0.069(3) Uani 1 1 d . . . O2W O 0.3317(6) 0.5217(8) 0.5052(4) 0.052(2) Uani 1 1 d . . . O4 O 0.7216(6) 0.5904(9) 0.6333(5) 0.065(3) Uani 1 1 d . . . O3W O 0.4718(7) 0.5402(9) 0.4126(4) 0.055(2) Uani 1 1 d . . . O5 O 0.7247(7) 0.7706(10) 0.5700(5) 0.068(3) Uani 1 1 d . . . O4W O 0.2444(9) 0.3207(19) 0.5700(8) 0.165(9) Uani 1 1 d . . . O6 O 0.8778(6) 0.3771(9) 0.6367(4) 0.059(3) Uani 1 1 d . . . O5W O 0.762(3) 0.007(3) 0.726(2) 0.164(17) Uani 0.50 1 d P . . O7 O 1.0275(7) 0.3571(10) 0.5921(5) 0.070(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(5) 0.031(6) 0.080(9) -0.005(6) 0.002(5) 0.001(4) C2 0.033(6) 0.025(5) 0.067(9) 0.000(5) 0.009(6) -0.001(4) C3 0.033(6) 0.016(5) 0.058(8) 0.000(4) 0.003(5) -0.001(4) C4 0.025(6) 0.030(6) 0.096(11) -0.017(6) 0.007(6) -0.005(5) C5 0.048(7) 0.036(6) 0.037(6) 0.016(5) 0.001(5) 0.014(5) C6 0.025(5) 0.022(5) 0.083(10) 0.006(5) 0.004(6) 0.003(4) C7 0.037(6) 0.030(6) 0.074(10) 0.007(5) 0.003(6) -0.010(5) C8 0.047(7) 0.045(7) 0.079(11) 0.019(7) -0.007(7) -0.017(6) C9 0.037(6) 0.039(6) 0.085(11) 0.005(6) 0.012(7) -0.009(5) C10 0.030(6) 0.055(7) 0.085(11) -0.004(7) 0.029(6) -0.015(6) C11 0.033(6) 0.046(7) 0.091(11) -0.014(7) 0.010(7) -0.010(6) C12 0.042(7) 0.037(6) 0.083(11) -0.006(6) 0.003(7) 0.003(5) C13A 0.07(2) 0.09(3) 0.13(4) -0.02(2) 0.05(2) 0.000(19) C13B 0.06(2) 0.024(17) 0.42(10) -0.03(3) -0.08(4) 0.015(16) C14A 0.10(3) 0.054(18) 0.07(2) -0.015(16) -0.03(2) -0.012(19) C14B 0.11(3) 0.039(15) 0.09(3) 0.028(16) -0.05(2) -0.046(18) C15A 0.12(4) 0.10(3) 0.19(6) 0.07(4) -0.12(4) -0.07(3) C15B 0.09(3) 0.17(4) 0.11(4) -0.06(3) 0.05(3) -0.08(3) C16 0.032(6) 0.026(5) 0.086(10) 0.018(6) 0.000(6) -0.005(5) C17 0.049(8) 0.040(7) 0.140(17) 0.001(8) 0.007(9) 0.005(6) C18 0.046(8) 0.067(9) 0.116(15) 0.035(9) 0.025(8) 0.000(7) C19 0.049(9) 0.040(8) 0.21(2) 0.043(10) 0.031(11) 0.004(7) Co1 0.0220(10) 0.0282(11) 0.0739(16) 0.0003(10) 0.0109(10) -0.0006(8) Mo1 0.0217(5) 0.0344(6) 0.0764(8) 0.0009(5) 0.0133(4) -0.0078(4) N1 0.021(4) 0.025(4) 0.094(9) 0.012(5) 0.003(5) 0.000(4) O1 0.036(4) 0.023(4) 0.096(8) 0.018(4) 0.003(4) -0.005(3) O2 0.040(5) 0.058(5) 0.125(10) 0.001(6) 0.024(5) -0.035(4) O1W 0.032(4) 0.032(4) 0.107(8) -0.004(4) 0.016(4) -0.004(4) O3 0.042(5) 0.061(6) 0.109(9) -0.005(5) 0.029(5) 0.019(4) O2W 0.027(4) 0.036(4) 0.095(7) 0.003(4) 0.012(4) 0.004(3) O4 0.029(4) 0.048(5) 0.119(9) 0.008(5) 0.010(5) -0.018(4) O3W 0.034(4) 0.049(5) 0.083(7) 0.004(5) 0.013(4) -0.001(4) O5 0.048(5) 0.047(5) 0.106(9) 0.014(5) -0.009(5) -0.015(4) O4W 0.057(7) 0.190(15) 0.26(2) 0.154(15) 0.072(10) 0.046(9) O6 0.030(4) 0.049(5) 0.102(8) -0.024(5) 0.023(5) -0.017(4) O5W 0.11(2) 0.10(2) 0.27(5) -0.05(2) -0.06(3) -0.022(17) O7 0.038(5) 0.066(6) 0.107(9) -0.030(6) 0.019(5) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.383(18) . ? C1 O1 1.410(14) . ? C1 C2 1.418(14) . ? C2 C3 1.377(16) . ? C2 C7 1.499(17) . ? C3 C4 1.400(18) . ? C3 H3 0.9300 . ? C4 C5 1.388(15) . ? C4 C12 1.524(17) . ? C5 C6 1.430(16) . ? C5 H5 0.9300 . ? C6 C16 1.545(14) . ? C7 N1 1.500(17) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.496(16) . ? C8 N1 1.496(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O5 1.259(17) . ? C9 O4 1.290(14) . ? C10 N1 1.475(14) . ? C10 C11 1.513(17) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O7 1.227(15) . ? C11 O6 1.253(14) . ? C12 C14B 1.48(3) . ? C12 C14A 1.525(18) . ? C12 C15A 1.546(19) . ? C12 C13A 1.547(18) . ? C12 C13B 1.56(3) . ? C12 C15B 1.57(4) . ? C13A C13B 1.40(7) . ? C13A C14B 1.515(19) . ? C13B C15A 1.34(8) . ? C14A C14B 1.22(4) . ? C14A C15B 1.54(6) . ? C15A C15B 1.62(7) . ? C16 C19 1.47(2) . ? C16 C18 1.530(16) . ? C16 C17 1.55(2) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? Co1 O2W 2.070(8) 3_666 ? Co1 O2W 2.070(8) . ? Co1 O3W 2.108(10) 3_666 ? Co1 O3W 2.108(10) . ? Co1 O1W 2.135(8) . ? Co1 O1W 2.135(8) 3_666 ? Mo1 O3 1.669(9) . ? Mo1 O2 1.708(8) . ? Mo1 O1 1.867(8) . ? Mo1 O4 2.054(10) . ? Mo1 O6 2.203(9) . ? Mo1 N1 2.347(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 O1 119.7(9) . . ? C6 C1 C2 121.7(11) . . ? O1 C1 C2 118.5(11) . . ? C3 C2 C1 118.5(11) . . ? C3 C2 C7 116.5(9) . . ? C1 C2 C7 125.0(11) . . ? C2 C3 C4 121.4(10) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 120.1(11) . . ? C5 C4 C12 119.1(12) . . ? C3 C4 C12 120.8(10) . . ? C4 C5 C6 119.8(11) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 118.6(9) . . ? C1 C6 C16 121.9(11) . . ? C5 C6 C16 119.5(11) . . ? C2 C7 N1 117.6(9) . . ? C2 C7 H7A 107.9 . . ? N1 C7 H7A 107.9 . . ? C2 C7 H7B 107.9 . . ? N1 C7 H7B 107.9 . . ? H7A C7 H7B 107.2 . . ? C9 C8 N1 111.3(10) . . ? C9 C8 H8A 109.4 . . ? N1 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? N1 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? O5 C9 O4 122.3(12) . . ? O5 C9 C8 117.9(11) . . ? O4 C9 C8 119.8(13) . . ? N1 C10 C11 111.4(9) . . ? N1 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N1 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? O7 C11 O6 124.2(12) . . ? O7 C11 C10 118.9(10) . . ? O6 C11 C10 116.8(12) . . ? C14B C12 C4 115.2(16) . . ? C14B C12 C14A 47.8(18) . . ? C4 C12 C14A 107.2(14) . . ? C14B C12 C15A 130(2) . . ? C4 C12 C15A 115.1(17) . . ? C14A C12 C15A 115(3) . . ? C14B C12 C13A 60.0(11) . . ? C4 C12 C13A 108.8(19) . . ? C14A C12 C13A 107.4(19) . . ? C15A C12 C13A 102(3) . . ? C14B C12 C13B 106(2) . . ? C4 C12 C13B 114(2) . . ? C14A C12 C13B 138(2) . . ? C15A C12 C13B 51(3) . . ? C13A C12 C13B 54(3) . . ? C14B C12 C15B 103(2) . . ? C4 C12 C15B 107.1(16) . . ? C14A C12 C15B 60(2) . . ? C15A C12 C15B 63(3) . . ? C13A C12 C15B 144(2) . . ? C13B C12 C15B 112(4) . . ? C13B C13A C14B 112(3) . . ? C13B C13A C12 64(2) . . ? C14B C13A C12 57.8(13) . . ? C15A C13B C13A 123(3) . . ? C15A C13B C12 64(2) . . ? C13A C13B C12 62.9(18) . . ? C14B C14A C12 64.1(17) . . ? C14B C14A C15B 119(3) . . ? C12 C14A C15B 61.7(19) . . ? C14A C14B C12 68.0(17) . . ? C14A C14B C13A 129(2) . . ? C12 C14B C13A 62.2(11) . . ? C13B C15A C12 65(2) . . ? C13B C15A C15B 122(3) . . ? C12 C15A C15B 59(2) . . ? C14A C15B C12 58.7(18) . . ? C14A C15B C15A 110(3) . . ? C12 C15B C15A 57.9(19) . . ? C19 C16 C18 107.7(12) . . ? C19 C16 C6 112.8(11) . . ? C18 C16 C6 109.0(10) . . ? C19 C16 C17 108.9(11) . . ? C18 C16 C17 109.7(12) . . ? C6 C16 C17 108.7(11) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2W Co1 O2W 180.000(1) 3_666 . ? O2W Co1 O3W 88.0(4) 3_666 3_666 ? O2W Co1 O3W 92.0(4) . 3_666 ? O2W Co1 O3W 92.0(4) 3_666 . ? O2W Co1 O3W 88.0(4) . . ? O3W Co1 O3W 180.00(13) 3_666 . ? O2W Co1 O1W 92.2(3) 3_666 . ? O2W Co1 O1W 87.8(3) . . ? O3W Co1 O1W 89.3(4) 3_666 . ? O3W Co1 O1W 90.7(4) . . ? O2W Co1 O1W 87.8(3) 3_666 3_666 ? O2W Co1 O1W 92.2(3) . 3_666 ? O3W Co1 O1W 90.7(4) 3_666 3_666 ? O3W Co1 O1W 89.3(4) . 3_666 ? O1W Co1 O1W 180.0(6) . 3_666 ? O3 Mo1 O2 106.9(5) . . ? O3 Mo1 O1 100.2(5) . . ? O2 Mo1 O1 105.2(4) . . ? O3 Mo1 O4 90.0(5) . . ? O2 Mo1 O4 95.1(4) . . ? O1 Mo1 O4 153.3(3) . . ? O3 Mo1 O6 162.4(4) . . ? O2 Mo1 O6 88.1(4) . . ? O1 Mo1 O6 84.3(4) . . ? O4 Mo1 O6 79.3(4) . . ? O3 Mo1 N1 92.3(4) . . ? O2 Mo1 N1 158.7(5) . . ? O1 Mo1 N1 79.7(3) . . ? O4 Mo1 N1 75.3(3) . . ? O6 Mo1 N1 71.6(3) . . ? C10 N1 C8 110.9(12) . . ? C10 N1 C7 110.8(9) . . ? C8 N1 C7 110.0(9) . . ? C10 N1 Mo1 108.5(6) . . ? C8 N1 Mo1 109.2(6) . . ? C7 N1 Mo1 107.4(7) . . ? C1 O1 Mo1 131.6(6) . . ? C9 O4 Mo1 122.6(9) . . ? C11 O6 Mo1 121.8(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.1(17) . . . . ? O1 C1 C2 C3 -176.1(10) . . . . ? C6 C1 C2 C7 -176.0(11) . . . . ? O1 C1 C2 C7 7.9(17) . . . . ? C1 C2 C3 C4 -0.5(17) . . . . ? C7 C2 C3 C4 175.9(11) . . . . ? C2 C3 C4 C5 1.3(18) . . . . ? C2 C3 C4 C12 179.5(10) . . . . ? C3 C4 C5 C6 -1.6(17) . . . . ? C12 C4 C5 C6 -179.9(11) . . . . ? O1 C1 C6 C5 175.7(10) . . . . ? C2 C1 C6 C5 -0.4(17) . . . . ? O1 C1 C6 C16 -5.3(17) . . . . ? C2 C1 C6 C16 178.6(11) . . . . ? C4 C5 C6 C1 1.2(17) . . . . ? C4 C5 C6 C16 -177.8(11) . . . . ? C3 C2 C7 N1 156.4(10) . . . . ? C1 C2 C7 N1 -27.5(17) . . . . ? N1 C8 C9 O5 -171.4(13) . . . . ? N1 C8 C9 O4 7.7(19) . . . . ? N1 C10 C11 O7 160.8(14) . . . . ? N1 C10 C11 O6 -20.2(19) . . . . ? C5 C4 C12 C14B 179.8(18) . . . . ? C3 C4 C12 C14B 2(2) . . . . ? C5 C4 C12 C14A -129(2) . . . . ? C3 C4 C12 C14A 52(2) . . . . ? C5 C4 C12 C15A 1(4) . . . . ? C3 C4 C12 C15A -178(3) . . . . ? C5 C4 C12 C13A 114.8(19) . . . . ? C3 C4 C12 C13A -63(2) . . . . ? C5 C4 C12 C13B 57(3) . . . . ? C3 C4 C12 C13B -121(3) . . . . ? C5 C4 C12 C15B -67(3) . . . . ? C3 C4 C12 C15B 115(3) . . . . ? C14B C12 C13A C13B 145(3) . . . . ? C4 C12 C13A C13B -106(3) . . . . ? C14A C12 C13A C13B 138(3) . . . . ? C15A C12 C13A C13B 16(4) . . . . ? C15B C12 C13A C13B 76(5) . . . . ? C4 C12 C13A C14B 108.8(19) . . . . ? C14A C12 C13A C14B -7(2) . . . . ? C15A C12 C13A C14B -129(3) . . . . ? C13B C12 C13A C14B -145(3) . . . . ? C15B C12 C13A C14B -69(5) . . . . ? C14B C13A C13B C15A 10(6) . . . . ? C12 C13A C13B C15A -22(4) . . . . ? C14B C13A C13B C12 32(3) . . . . ? C14B C12 C13B C15A 129(3) . . . . ? C4 C12 C13B C15A -104(3) . . . . ? C14A C12 C13B C15A 85(5) . . . . ? C13A C12 C13B C15A 160(4) . . . . ? C15B C12 C13B C15A 18(3) . . . . ? C14B C12 C13B C13A -31(3) . . . . ? C4 C12 C13B C13A 96(2) . . . . ? C14A C12 C13B C13A -74(6) . . . . ? C15A C12 C13B C13A -160(4) . . . . ? C15B C12 C13B C13A -142(3) . . . . ? C4 C12 C14A C14B -109(2) . . . . ? C15A C12 C14A C14B 122(3) . . . . ? C13A C12 C14A C14B 8(3) . . . . ? C13B C12 C14A C14B 62(5) . . . . ? C15B C12 C14A C14B 151(3) . . . . ? C14B C12 C14A C15B -151(3) . . . . ? C4 C12 C14A C15B 100(2) . . . . ? C15A C12 C14A C15B -30(3) . . . . ? C13A C12 C14A C15B -143(3) . . . . ? C13B C12 C14A C15B -89(5) . . . . ? C15B C14A C14B C12 29(3) . . . . ? C12 C14A C14B C13A -10(4) . . . . ? C15B C14A C14B C13A 19(6) . . . . ? C4 C12 C14B C14A 91(2) . . . . ? C15A C12 C14B C14A -90(4) . . . . ? C13A C12 C14B C14A -171(3) . . . . ? C13B C12 C14B C14A -142(4) . . . . ? C15B C12 C14B C14A -25(3) . . . . ? C4 C12 C14B C13A -98(2) . . . . ? C14A C12 C14B C13A 171(3) . . . . ? C15A C12 C14B C13A 81(5) . . . . ? C13B C12 C14B C13A 29(4) . . . . ? C15B C12 C14B C13A 146(3) . . . . ? C13B C13A C14B C14A -23(6) . . . . ? C12 C13A C14B C14A 11(4) . . . . ? C13B C13A C14B C12 -34(3) . . . . ? C13A C13B C15A C12 22(4) . . . . ? C13A C13B C15A C15B 3(7) . . . . ? C12 C13B C15A C15B -19(3) . . . . ? C14B C12 C15A C13B -78(5) . . . . ? C4 C12 C15A C13B 101(2) . . . . ? C14A C12 C15A C13B -133(3) . . . . ? C13A C12 C15A C13B -17(3) . . . . ? C15B C12 C15A C13B -162(3) . . . . ? C14B C12 C15A C15B 84(3) . . . . ? C4 C12 C15A C15B -97(2) . . . . ? C14A C12 C15A C15B 29(3) . . . . ? C13A C12 C15A C15B 145(2) . . . . ? C13B C12 C15A C15B 162(3) . . . . ? C14B C14A C15B C12 -30(3) . . . . ? C14B C14A C15B C15A -3(5) . . . . ? C12 C14A C15B C15A 27(2) . . . . ? C14B C12 C15B C14A 21(2) . . . . ? C4 C12 C15B C14A -100.3(18) . . . . ? C15A C12 C15B C14A 150(3) . . . . ? C13A C12 C15B C14A 77(5) . . . . ? C13B C12 C15B C14A 134(2) . . . . ? C14B C12 C15B C15A -128(2) . . . . ? C4 C12 C15B C15A 110(2) . . . . ? C14A C12 C15B C15A -150(3) . . . . ? C13A C12 C15B C15A -73(5) . . . . ? C13B C12 C15B C15A -15(2) . . . . ? C13B C15A C15B C14A -8(5) . . . . ? C12 C15A C15B C14A -27(2) . . . . ? C13B C15A C15B C12 20(4) . . . . ? C1 C6 C16 C19 -178.0(12) . . . . ? C5 C6 C16 C19 1.0(17) . . . . ? C1 C6 C16 C18 -58.4(17) . . . . ? C5 C6 C16 C18 120.6(13) . . . . ? C1 C6 C16 C17 61.1(14) . . . . ? C5 C6 C16 C17 -119.9(13) . . . . ? C11 C10 N1 C8 -87.4(13) . . . . ? C11 C10 N1 C7 150.1(11) . . . . ? C11 C10 N1 Mo1 32.5(14) . . . . ? C9 C8 N1 C10 106.4(12) . . . . ? C9 C8 N1 C7 -130.7(11) . . . . ? C9 C8 N1 Mo1 -13.1(14) . . . . ? C2 C7 N1 C10 -62.0(13) . . . . ? C2 C7 N1 C8 175.0(10) . . . . ? C2 C7 N1 Mo1 56.3(11) . . . . ? O3 Mo1 N1 C10 161.2(9) . . . . ? O2 Mo1 N1 C10 -44.1(15) . . . . ? O1 Mo1 N1 C10 61.2(9) . . . . ? O4 Mo1 N1 C10 -109.4(9) . . . . ? O6 Mo1 N1 C10 -26.1(8) . . . . ? O3 Mo1 N1 C8 -77.8(10) . . . . ? O2 Mo1 N1 C8 76.9(14) . . . . ? O1 Mo1 N1 C8 -177.7(10) . . . . ? O4 Mo1 N1 C8 11.6(9) . . . . ? O6 Mo1 N1 C8 94.9(9) . . . . ? O3 Mo1 N1 C7 41.4(7) . . . . ? O2 Mo1 N1 C7 -163.9(11) . . . . ? O1 Mo1 N1 C7 -58.5(7) . . . . ? O4 Mo1 N1 C7 130.8(7) . . . . ? O6 Mo1 N1 C7 -145.9(7) . . . . ? C6 C1 O1 Mo1 144.6(9) . . . . ? C2 C1 O1 Mo1 -39.2(15) . . . . ? O3 Mo1 O1 C1 -34.1(11) . . . . ? O2 Mo1 O1 C1 -144.9(10) . . . . ? O4 Mo1 O1 C1 76.8(14) . . . . ? O6 Mo1 O1 C1 128.7(10) . . . . ? N1 Mo1 O1 C1 56.4(10) . . . . ? O5 C9 O4 Mo1 -177.2(11) . . . . ? C8 C9 O4 Mo1 3.8(18) . . . . ? O3 Mo1 O4 C9 83.6(11) . . . . ? O2 Mo1 O4 C9 -169.5(11) . . . . ? O1 Mo1 O4 C9 -29.6(16) . . . . ? O6 Mo1 O4 C9 -82.4(10) . . . . ? N1 Mo1 O4 C9 -8.8(10) . . . . ? O7 C11 O6 Mo1 173.7(12) . . . . ? C10 C11 O6 Mo1 -5.2(19) . . . . ? O3 Mo1 O6 C11 43(2) . . . . ? O2 Mo1 O6 C11 -168.3(12) . . . . ? O1 Mo1 O6 C11 -62.9(11) . . . . ? O4 Mo1 O6 C11 96.1(11) . . . . ? N1 Mo1 O6 C11 18.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.238 _refine_diff_density_min -1.878 _refine_diff_density_rms 0.201