Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email cotton@tamu.edu _publ_contact_author_name 'Dr F Albert Cotton' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry Texas A&M University, PO Box 30012 College Station, TX 77842-3012, USA ; _publ_contact_author_fax '(979) 845 9351' _publ_contact_author_phone '(979) 845 4432' # TITLE AND AUTHOR LIST _publ_section_title ; A molecular loop with interstitial cannels in a chiral environment: Exploration of the chemistry of Mo2(4+) species with chiral and non-chiral dicarboxylate anions ; loop_ _publ_author_name _publ_author_address 'John F. Berry' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, PO Box 30012 College Station, TX 77842-3012, USA ; 'F. Albert Cotton' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, PO Box 30012 College Station, TX 77842-3012, USA ; 'Sergey A. Ibragimov' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, PO Box 30012 College Station, TX 77842-3012, USA ; 'Carlos A. Murillo' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, PO Box 30012 College Station, TX 77842-3012, USA ; 'Xiaoping Wang' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, PO Box 30012 College Station, TX 77842-3012, USA ; #======================================================== #Compound 1.4CH2Cl2 #======================================================== data_cmpd1 _database_code_CSD 217277 _chemical_name_common (Mo2(DaniF)2(p-O2CCH(CH3)OC6H4OCH(CH3)CO2)2,4CH2Cl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C88 H92 Cl8 Mo4 N8 O20' _chemical_formula_sum 'C88 H92 Cl8 Mo4 N8 O20' _chemical_formula_weight 2249.06 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M I222 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' _cell_length_a 13.970(3) _cell_length_b 20.450(5) _cell_length_c 37.216(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10632(4) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 78 _cell_measurement_theta_min 18.2 _cell_measurement_theta_max 41.6 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4560 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7599 _exptl_absorpt_correction_T_max 0.8684 _exptl_absorpt_process_details SORTAV _exptl_special_details ; The disordered anisyl groups on the DAniF ligands were refined with distance restrains. ; _diffrn_ambient_temperature 213(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 'Nonius FAST' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12987 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 22.55 _reflns_number_total 6212 _reflns_number_gt 5010 _reflns_threshold_expression >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction PROCOR _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0152P)^2^+376.0578P] 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 mixed _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 0.03(14) _refine_ls_number_reflns 6212 _refine_ls_number_parameters 526 _refine_ls_number_restraints 359 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.1102 _refine_ls_wR_factor_ref 0.2404 _refine_ls_wR_factor_gt 0.2226 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.001 _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 Mo1 Mo 0.04162(14) 0.23570(7) 0.65704(5) 0.0602(5) Uani 1 1 d . . . Mo2 Mo 0.15487(14) 0.25654(8) 0.62255(4) 0.0597(5) Uani 1 1 d . . . N1 N 0.1279(16) 0.1840(7) 0.6909(4) 0.065(5) Uani 1 1 d . . . N2 N 0.2540(14) 0.2033(7) 0.6534(4) 0.068(5) Uani 1 1 d . . . N3 N 0.0023(13) 0.1514(7) 0.6285(5) 0.067(5) Uani 1 1 d . . . N4 N 0.1244(16) 0.1761(8) 0.5893(4) 0.073(6) Uani 1 1 d . . . C2 C 0.0582(19) 0.1382(9) 0.5990(5) 0.066(7) Uani 1 1 d . A . H2A H 0.0467 0.0998 0.5857 0.079 Uiso 1 1 calc R . . C1 C 0.222(2) 0.1768(10) 0.6836(6) 0.076(8) Uani 1 1 d . A . H1A H 0.2634 0.1541 0.6993 0.091 Uiso 1 1 calc R . . C11 C 0.1009(14) 0.1559(7) 0.7238(4) 0.063(6) Uani 1 1 d D . . C12 C 0.0407(15) 0.1913(7) 0.7463(4) 0.072(6) Uani 1 1 d D . . H12A H 0.0272 0.2349 0.7400 0.086 Uiso 1 1 calc R . . C13 C -0.0009(15) 0.1669(7) 0.7775(5) 0.078(7) Uani 1 1 d D . . H13A H -0.0435 0.1928 0.7909 0.093 Uiso 1 1 calc R . . C14 C 0.0211(14) 0.1043(7) 0.7884(5) 0.062(6) Uani 1 1 d D . . C15 C 0.0811(14) 0.0670(7) 0.7668(5) 0.079(8) Uani 1 1 d D . . H15A H 0.0959 0.0240 0.7736 0.095 Uiso 1 1 calc R . . C16 C 0.1198(16) 0.0922(7) 0.7350(4) 0.084(8) Uani 1 1 d D . . H16A H 0.1597 0.0655 0.7209 0.101 Uiso 1 1 calc R . . O1 O -0.0079(11) 0.0752(7) 0.8194(4) 0.071(4) Uani 1 1 d D . . C17 C -0.0519(18) 0.1145(9) 0.8466(5) 0.084(7) Uani 1 1 d D . . H17A H -0.0688 0.0872 0.8670 0.126 Uiso 1 1 calc R . . H17B H -0.1093 0.1347 0.8370 0.126 Uiso 1 1 calc R . . H17C H -0.0076 0.1482 0.8543 0.126 Uiso 1 1 calc R . . C21 C 0.354(3) 0.206(4) 0.6434(16) 0.060(6) Uiso 0.35(3) 1 d PD A 1 C22 C 0.399(3) 0.234(3) 0.6135(13) 0.073(9) Uiso 0.35(3) 1 d PD A 1 H22 H 0.3599 0.2535 0.5961 0.087 Uiso 0.35(3) 1 calc PR A 1 C23 C 0.497(3) 0.234(3) 0.6077(12) 0.064(8) Uiso 0.35(3) 1 d PD A 1 H23 H 0.5231 0.2533 0.5868 0.076 Uiso 0.35(3) 1 calc PR A 1 C24 C 0.556(2) 0.206(2) 0.6330(13) 0.082(8) Uiso 0.35(3) 1 d PD A 1 C25 C 0.516(4) 0.186(4) 0.6653(14) 0.077(9) Uiso 0.35(3) 1 d PD A 1 H25 H 0.5560 0.1712 0.6839 0.093 Uiso 0.35(3) 1 calc PR A 1 C26 C 0.417(4) 0.187(6) 0.6706(15) 0.081(9) Uiso 0.35(3) 1 d PD A 1 H26 H 0.3916 0.1738 0.6929 0.098 Uiso 0.35(3) 1 calc PR A 1 O11 O 0.652(3) 0.199(3) 0.6266(13) 0.097(7) Uiso 0.35(3) 1 d PD A 1 C27 C 0.667(7) 0.225(5) 0.5916(16) 0.141(16) Uiso 0.35(3) 1 d PD A 1 H27A H 0.7328 0.2187 0.5845 0.211 Uiso 0.35(3) 1 calc PR A 1 H27B H 0.6516 0.2713 0.5914 0.211 Uiso 0.35(3) 1 calc PR A 1 H27C H 0.6251 0.2024 0.5748 0.211 Uiso 0.35(3) 1 calc PR A 1 C21B C 0.3533(16) 0.200(2) 0.6478(8) 0.060(6) Uiso 0.65(3) 1 d PD A 2 C22B C 0.3831(16) 0.2080(17) 0.6124(7) 0.073(9) Uiso 0.65(3) 1 d PD A 2 H22B H 0.3355 0.2127 0.5947 0.087 Uiso 0.65(3) 1 calc PR A 2 C23B C 0.4781(18) 0.2101(15) 0.6013(6) 0.064(8) Uiso 0.65(3) 1 d PD A 2 H23B H 0.4937 0.2099 0.5767 0.076 Uiso 0.65(3) 1 calc PR A 2 C24B C 0.5489(14) 0.2124(11) 0.6270(8) 0.082(8) Uiso 0.65(3) 1 d PD A 2 C25B C 0.5232(19) 0.201(2) 0.6626(7) 0.077(9) Uiso 0.65(3) 1 d PD A 2 H25B H 0.5712 0.1982 0.6802 0.093 Uiso 0.65(3) 1 calc PR A 2 C26B C 0.427(2) 0.192(3) 0.6726(7) 0.081(9) Uiso 0.65(3) 1 d PD A 2 H26B H 0.4126 0.1818 0.6965 0.098 Uiso 0.65(3) 1 calc PR A 2 O11B O 0.6415(15) 0.2273(13) 0.6184(7) 0.097(7) Uiso 0.65(3) 1 d PD A 2 C27B C 0.711(3) 0.233(3) 0.6459(10) 0.141(16) Uiso 0.65(3) 1 d PD A 2 H27D H 0.7718 0.2459 0.6354 0.211 Uiso 0.65(3) 1 calc PR A 2 H27E H 0.7184 0.1911 0.6579 0.211 Uiso 0.65(3) 1 calc PR A 2 H27F H 0.6907 0.2655 0.6632 0.211 Uiso 0.65(3) 1 calc PR A 2 C31 C 0.186(3) 0.1504(19) 0.5651(10) 0.069(7) Uiso 0.55(3) 1 d PD A 1 C32 C 0.196(3) 0.1908(15) 0.5352(9) 0.072(9) Uiso 0.55(3) 1 d PD A 1 H32A H 0.1622 0.2304 0.5351 0.086 Uiso 0.55(3) 1 calc PR A 1 C33 C 0.253(3) 0.1769(18) 0.5054(8) 0.099(12) Uiso 0.55(3) 1 d PD A 1 H33A H 0.2617 0.2079 0.4871 0.119 Uiso 0.55(3) 1 calc PR A 1 C34 C 0.296(2) 0.1163(18) 0.5035(8) 0.113(12) Uiso 0.55(3) 1 d PD A 1 C35 C 0.304(3) 0.0808(18) 0.5354(11) 0.125(15) Uiso 0.55(3) 1 d PD A 1 H35A H 0.3493 0.0473 0.5373 0.150 Uiso 0.55(3) 1 calc PR A 1 C36 C 0.243(3) 0.0945(16) 0.5645(9) 0.076(10) Uiso 0.55(3) 1 d PD A 1 H36A H 0.2413 0.0654 0.5841 0.091 Uiso 0.55(3) 1 calc PR A 1 C31B C 0.182(4) 0.1591(19) 0.5592(14) 0.069(7) Uiso 0.45(3) 1 d PD A 2 C32B C 0.235(4) 0.1999(14) 0.5370(12) 0.072(9) Uiso 0.45(3) 1 d PD A 2 H32B H 0.2254 0.2452 0.5390 0.086 Uiso 0.45(3) 1 calc PR A 2 C33B C 0.303(4) 0.179(2) 0.5120(13) 0.099(12) Uiso 0.45(3) 1 d PD A 2 H33B H 0.3352 0.2090 0.4974 0.119 Uiso 0.45(3) 1 calc PR A 2 C34B C 0.321(3) 0.113(2) 0.5090(9) 0.113(12) Uiso 0.45(3) 1 d PD A 2 C35B C 0.262(4) 0.0699(16) 0.5281(15) 0.125(15) Uiso 0.45(3) 1 d PD A 2 H35B H 0.2641 0.0250 0.5227 0.150 Uiso 0.45(3) 1 calc PR A 2 C36B C 0.201(3) 0.0927(17) 0.5550(13) 0.076(10) Uiso 0.45(3) 1 d PD A 2 H36B H 0.1717 0.0625 0.5706 0.091 Uiso 0.45(3) 1 calc PR A 2 O3 O 0.330(3) 0.0867(19) 0.4730(10) 0.151(13) Uiso 0.55(3) 1 d PD A 1 C37 C 0.412(4) 0.125(3) 0.4640(16) 0.162(17) Uiso 0.55(3) 1 d PD A 1 H37A H 0.4515 0.1003 0.4473 0.243 Uiso 0.55(3) 1 calc PR A 1 H37B H 0.4478 0.1341 0.4856 0.243 Uiso 0.55(3) 1 calc PR A 1 H37C H 0.3914 0.1652 0.4528 0.243 Uiso 0.55(3) 1 calc PR A 1 O3B O 0.392(4) 0.086(3) 0.4880(12) 0.151(13) Uiso 0.45(3) 1 d PD A 2 C37B C 0.397(5) 0.132(2) 0.4591(14) 0.162(17) Uiso 0.45(3) 1 d PD A 2 H37D H 0.4350 0.1132 0.4397 0.243 Uiso 0.45(3) 1 calc PR A 2 H37E H 0.4267 0.1720 0.4673 0.243 Uiso 0.45(3) 1 calc PR A 2 H37F H 0.3330 0.1410 0.4504 0.243 Uiso 0.45(3) 1 calc PR A 2 C41 C -0.0835(19) 0.1126(17) 0.6329(9) 0.065(8) Uiso 0.528(12) 1 d PD B 1 C42 C -0.112(3) 0.097(2) 0.6678(7) 0.108(13) Uiso 0.528(12) 1 d PD B 1 H42A H -0.0768 0.1150 0.6869 0.130 Uiso 0.528(12) 1 calc PR B 1 C43 C -0.189(3) 0.057(2) 0.6762(7) 0.094(11) Uiso 0.528(12) 1 d PD B 1 H43A H -0.2003 0.0436 0.7000 0.112 Uiso 0.528(12) 1 calc PR B 1 C44 C -0.250(2) 0.0377(18) 0.6489(9) 0.077(9) Uiso 0.528(12) 1 d PD B 1 C45 C -0.233(2) 0.062(2) 0.6146(8) 0.095(11) Uiso 0.528(12) 1 d PD B 1 H45A H -0.2779 0.0533 0.5963 0.113 Uiso 0.528(12) 1 calc PR B 1 C46 C -0.152(2) 0.0989(16) 0.6066(6) 0.065(8) Uiso 0.528(12) 1 d PD B 1 H46A H -0.1426 0.1147 0.5832 0.078 Uiso 0.528(12) 1 calc PR B 1 O2 O -0.325(3) 0.0015(19) 0.6626(11) 0.134(11) Uiso 0.528(12) 1 d PD B 1 C47 C -0.398(4) -0.016(3) 0.6381(17) 0.16(2) Uiso 0.528(12) 1 d PD B 1 H47A H -0.4484 -0.0386 0.6507 0.246 Uiso 0.528(12) 1 calc PR B 1 H47B H -0.3716 -0.0438 0.6195 0.246 Uiso 0.528(12) 1 calc PR B 1 H47C H -0.4236 0.0236 0.6271 0.246 Uiso 0.528(12) 1 calc PR B 1 C41B C -0.063(2) 0.1088(14) 0.6402(12) 0.065(8) Uiso 0.472(12) 1 d PD B 2 C42B C -0.156(3) 0.1313(12) 0.6468(14) 0.108(13) Uiso 0.472(12) 1 d PD B 2 H42B H -0.1689 0.1755 0.6420 0.130 Uiso 0.472(12) 1 calc PR B 2 C43B C -0.230(2) 0.0930(16) 0.6600(13) 0.094(11) Uiso 0.472(12) 1 d PD B 2 H43B H -0.2880 0.1122 0.6676 0.112 Uiso 0.472(12) 1 calc PR B 2 C44B C -0.218(2) 0.0262(15) 0.6616(13) 0.077(9) Uiso 0.472(12) 1 d PD B 2 C45B C -0.126(3) 0.0017(12) 0.6565(13) 0.095(11) Uiso 0.472(12) 1 d PD B 2 H45B H -0.1133 -0.0425 0.6617 0.113 Uiso 0.472(12) 1 calc PR B 2 C46B C -0.052(2) 0.0416(15) 0.6439(10) 0.065(8) Uiso 0.472(12) 1 d PD B 2 H46B H 0.0074 0.0225 0.6378 0.078 Uiso 0.472(12) 1 calc PR B 2 O2B O -0.2733(12) -0.0256(15) 0.6719(12) 0.134(11) Uiso 0.472(12) 1 d PD B 2 C47B C -0.3714(11) -0.0084(6) 0.6700(3) 0.16(2) Uiso 0.472(12) 1 d PD B 2 H47D H -0.4103 -0.0452 0.6775 0.246 Uiso 0.472(12) 1 calc PR B 2 H47E H -0.3875 0.0035 0.6455 0.246 Uiso 0.472(12) 1 calc PR B 2 H47F H -0.3837 0.0285 0.6857 0.246 Uiso 0.472(12) 1 calc PR B 2 C51 C 0.1917(11) 0.5829(6) 0.6137(3) 0.063(6) Uani 1 1 d R . . C52 C 0.1075(11) 0.5508(6) 0.6228(3) 0.064(6) Uani 1 1 d RD . . H52A H 0.0465 0.5597 0.6133 0.077 Uiso 1 1 calc R . . C53 C 0.1282(11) 0.5033(8) 0.6486(4) 0.063(6) Uani 1 1 d D . . H53A H 0.0777 0.4764 0.6563 0.075 Uiso 1 1 calc R . . C54 C 0.2180(13) 0.4927(8) 0.6636(4) 0.067(7) Uani 1 1 d D . . C55 C 0.2947(11) 0.5290(10) 0.6515(5) 0.081(8) Uani 1 1 d D . . H55A H 0.3566 0.5220 0.6607 0.097 Uiso 1 1 calc R . . C56 C 0.2779(12) 0.5763(9) 0.6254(5) 0.067(6) Uani 1 1 d D . . H56A H 0.3278 0.6026 0.6166 0.080 Uiso 1 1 calc R . . C57 C 0.094(2) 0.6499(10) 0.5725(5) 0.074(7) Uani 1 1 d . . . H57A H 0.0622 0.6090 0.5645 0.089 Uiso 1 1 calc R . . C58 C 0.110(2) 0.6904(12) 0.5396(6) 0.102(9) Uani 1 1 d . . . H58A H 0.1543 0.6679 0.5237 0.153 Uiso 1 1 calc R . . H58B H 0.1370 0.7323 0.5464 0.153 Uiso 1 1 calc R . . H58C H 0.0498 0.6973 0.5272 0.153 Uiso 1 1 calc R . . C59 C 0.0262(16) 0.6825(8) 0.5981(5) 0.048(5) Uani 1 1 d . . . C60 C 0.171(2) 0.4074(10) 0.7061(6) 0.079(7) Uani 1 1 d . . . H60A H 0.1153 0.4348 0.7122 0.095 Uiso 1 1 calc R . . C61 C 0.209(2) 0.3785(16) 0.7404(6) 0.135(13) Uani 1 1 d . . . H61A H 0.2281 0.4134 0.7565 0.203 Uiso 1 1 calc R . . H61B H 0.2643 0.3513 0.7351 0.203 Uiso 1 1 calc R . . H61C H 0.1598 0.3522 0.7516 0.203 Uiso 1 1 calc R . . C62 C 0.1387(19) 0.3551(9) 0.6808(6) 0.061(6) Uani 1 1 d . A . O5 O 0.0642(13) 0.3203(7) 0.6881(4) 0.078(5) Uani 1 1 d . . . O6 O 0.1894(10) 0.3428(5) 0.6529(3) 0.057(4) Uani 1 1 d . . . O7 O 0.0575(9) 0.7094(5) 0.6251(4) 0.054(3) Uani 1 1 d . . . O8 O -0.0646(12) 0.6849(6) 0.5898(4) 0.065(4) Uani 1 1 d . . . O9 O 0.2447(11) 0.4495(6) 0.6922(4) 0.069(4) Uani 1 1 d . . . O10 O 0.1793(12) 0.6326(7) 0.5868(4) 0.072(4) Uani 1 1 d . . . C1S C 0.162(2) 0.3621(7) 0.2925(6) 0.101(9) Uani 1 1 d D . . H1SA H 0.2259 0.3787 0.2980 0.121 Uiso 1 1 calc R . . H1SB H 0.1237 0.3639 0.3147 0.121 Uiso 1 1 calc R . . Cl1 Cl 0.1699(7) 0.2817(3) 0.2782(2) 0.128(3) Uani 1 1 d D . . Cl2 Cl 0.1084(7) 0.4123(4) 0.2599(2) 0.123(3) Uani 1 1 d D . . C2S C 0.7731(19) 0.4271(11) 0.4275(7) 0.118(11) Uani 1 1 d DU . . H2SA H 0.8146 0.4192 0.4067 0.141 Uiso 1 1 calc R . . H2SB H 0.7292 0.4626 0.4210 0.141 Uiso 1 1 calc R . . Cl3 Cl 0.7072(9) 0.3582(5) 0.4351(3) 0.177(5) Uani 1 1 d D . . Cl4 Cl 0.8419(13) 0.4525(5) 0.4620(3) 0.222(7) 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 Mo1 0.0827(13) 0.0375(8) 0.0606(10) 0.0069(8) 0.0100(9) 0.0090(9) Mo2 0.0799(13) 0.0438(9) 0.0554(9) 0.0032(8) 0.0082(9) 0.0110(9) N1 0.107(18) 0.038(9) 0.050(11) 0.001(7) 0.012(10) 0.012(10) N2 0.114(17) 0.046(9) 0.045(10) 0.006(8) -0.003(10) 0.008(10) N3 0.089(15) 0.042(9) 0.069(12) 0.014(8) 0.009(10) -0.002(9) N4 0.12(2) 0.040(9) 0.055(11) 0.010(8) 0.028(11) 0.023(11) C2 0.11(2) 0.036(11) 0.049(13) -0.013(9) -0.012(13) 0.012(13) C1 0.11(2) 0.055(13) 0.061(15) -0.009(11) -0.025(14) 0.037(15) C11 0.067(16) 0.049(12) 0.074(15) -0.009(11) 0.006(11) 0.020(11) C12 0.103(19) 0.044(11) 0.069(14) 0.024(10) 0.010(14) 0.041(13) C13 0.09(2) 0.061(13) 0.081(16) 0.004(12) 0.035(13) 0.024(12) C14 0.047(15) 0.049(12) 0.091(16) 0.001(11) 0.013(11) 0.004(11) C15 0.066(18) 0.035(11) 0.14(2) 0.039(13) -0.006(14) -0.003(11) C16 0.14(3) 0.037(11) 0.076(16) -0.002(11) -0.003(15) -0.003(13) O1 0.088(13) 0.064(9) 0.061(9) 0.013(7) -0.014(8) -0.003(8) C17 0.10(2) 0.075(14) 0.074(16) 0.021(13) 0.024(16) -0.003(15) C51 0.070(18) 0.046(11) 0.074(15) -0.009(10) 0.000(12) -0.003(12) C52 0.076(17) 0.064(12) 0.053(12) -0.012(11) -0.010(12) 0.021(12) C53 0.068(17) 0.073(13) 0.048(13) -0.006(10) 0.006(11) 0.012(11) C54 0.10(2) 0.041(11) 0.062(14) -0.029(10) -0.001(13) -0.005(12) C55 0.063(18) 0.082(16) 0.096(19) -0.042(15) -0.042(15) 0.018(14) C56 0.063(17) 0.071(14) 0.066(14) -0.018(12) -0.018(12) -0.017(12) C57 0.12(2) 0.055(13) 0.052(14) 0.022(11) -0.004(13) -0.008(13) C58 0.13(3) 0.13(2) 0.046(14) 0.009(14) -0.017(14) -0.003(18) C59 0.067(17) 0.039(10) 0.039(11) -0.013(8) 0.004(10) 0.023(11) C60 0.12(2) 0.049(12) 0.072(15) -0.021(11) -0.016(14) -0.014(14) C61 0.19(4) 0.17(3) 0.045(15) 0.019(17) -0.045(18) 0.00(3) C62 0.09(2) 0.033(10) 0.057(14) -0.013(9) 0.003(13) 0.019(12) O5 0.107(15) 0.047(8) 0.079(11) 0.003(7) 0.012(10) 0.008(9) O6 0.082(11) 0.033(6) 0.057(8) 0.003(6) -0.004(8) -0.001(6) O7 0.043(9) 0.044(6) 0.076(9) -0.007(7) -0.021(7) 0.009(6) O8 0.087(14) 0.045(8) 0.063(9) -0.009(6) -0.024(8) 0.004(8) O9 0.098(13) 0.046(8) 0.063(9) -0.006(7) -0.003(8) 0.001(8) O10 0.097(14) 0.063(9) 0.056(9) 0.003(7) -0.004(8) -0.002(9) C1S 0.17(3) 0.061(14) 0.071(16) -0.030(12) 0.011(18) -0.023(18) Cl1 0.160(8) 0.092(5) 0.131(6) -0.044(4) 0.009(6) -0.004(5) Cl2 0.159(8) 0.104(5) 0.106(6) -0.028(5) 0.033(5) -0.027(5) C2S 0.19(3) 0.069(16) 0.09(2) 0.000(14) 0.03(2) -0.014(19) Cl3 0.209(12) 0.124(7) 0.197(10) 0.036(7) 0.061(9) -0.022(7) Cl4 0.39(2) 0.155(9) 0.116(7) -0.041(6) -0.043(11) -0.004(12) _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 Mo1 N1 2.038(18) . ? Mo1 Mo2 2.081(2) . ? Mo1 N3 2.097(16) . ? Mo1 O5 2.104(15) . ? Mo1 O7 2.144(13) 2_565 ? Mo2 N2 2.103(17) . ? Mo2 N4 2.103(18) . ? Mo2 O8 2.124(15) 2_565 ? Mo2 O6 2.149(12) . ? N1 C1 1.35(3) . ? N1 C11 1.40(2) . ? N2 C1 1.32(3) . ? N2 C21B 1.40(3) . ? N2 C21 1.45(4) . ? N3 C41B 1.34(3) . ? N3 C2 1.38(3) . ? N3 C41 1.45(3) . ? N4 C2 1.26(3) . ? N4 C31 1.36(3) . ? N4 C31B 1.42(4) . ? C11 C12 1.392(7) . ? C11 C16 1.392(7) . ? C12 C13 1.389(7) . ? C13 C14 1.379(7) . ? C14 O1 1.360(18) . ? C14 C15 1.390(7) . ? C15 C16 1.399(7) . ? O1 C17 1.431(14) . ? C21 C26 1.393(8) . ? C21 C22 1.393(8) . ? C22 C23 1.391(8) . ? C23 C24 1.379(8) . ? C24 O11 1.367(10) . ? C24 C25 1.390(8) . ? C25 C26 1.400(9) . ? O11 C27 1.418(9) . ? C21B C26B 1.392(8) . ? C21B C22B 1.393(8) . ? C22B C23B 1.391(8) . ? C23B C24B 1.379(8) . ? C24B O11B 1.367(10) . ? C24B C25B 1.390(8) . ? C25B C26B 1.400(8) . ? O11B C27B 1.415(9) . ? C31 C32 1.393(8) . ? C31 C36 1.393(8) . ? C32 C33 1.391(8) . ? C33 C34 1.380(8) . ? C34 O3 1.371(10) . ? C34 C35 1.393(8) . ? C35 C36 1.402(8) . ? C31B C36B 1.393(8) . ? C31B C32B 1.393(8) . ? C32B C33B 1.390(8) . ? C33B C34B 1.379(8) . ? C34B O3B 1.376(10) . ? C34B C35B 1.391(8) . ? C35B C36B 1.401(8) . ? O3 C37 1.422(16) . ? O3B C37B 1.421(10) . ? C41 C46 1.393(8) . ? C41 C42 1.394(8) . ? C42 C43 1.391(8) . ? C43 C44 1.379(8) . ? C44 O2 1.375(10) . ? C44 C45 1.390(8) . ? C45 C46 1.400(8) . ? O2 C47 1.416(9) . ? C41B C46B 1.392(8) . ? C41B C42B 1.393(8) . ? C42B C43B 1.391(8) . ? C43B C44B 1.379(8) . ? C44B O2B 1.368(10) . ? C44B C45B 1.390(8) . ? C45B C46B 1.400(9) . ? O2B C47B 1.417(9) . ? C51 C56 1.288(16) . ? C51 C52 1.3898 . ? C51 O10 1.436(18) . ? C52 C53 1.394(8) . ? C53 C54 1.390(8) . ? C54 C55 1.379(8) . ? C54 O9 1.434(18) . ? C55 C56 1.390(8) . ? C57 O10 1.36(3) . ? C57 C58 1.50(3) . ? C57 C59 1.50(3) . ? C59 O7 1.23(2) . ? C59 O8 1.31(2) . ? C60 O9 1.43(3) . ? C60 C62 1.50(3) . ? C60 C61 1.50(3) . ? C62 O6 1.28(2) . ? C62 O5 1.29(3) . ? O7 Mo1 2.144(13) 2_565 ? O8 Mo2 2.124(15) 2_565 ? C1S Cl1 1.734(14) . ? C1S Cl2 1.757(16) . ? C2S Cl4 1.686(18) . ? C2S Cl3 1.707(17) . ? 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 N1 Mo1 Mo2 92.2(6) . . ? N1 Mo1 N3 92.4(6) . . ? Mo2 Mo1 N3 93.2(5) . . ? N1 Mo1 O5 89.9(6) . . ? Mo2 Mo1 O5 93.2(5) . . ? N3 Mo1 O5 173.1(7) . . ? N1 Mo1 O7 175.2(6) . 2_565 ? Mo2 Mo1 O7 92.4(3) . 2_565 ? N3 Mo1 O7 88.9(6) . 2_565 ? O5 Mo1 O7 88.3(5) . 2_565 ? Mo1 Mo2 N2 93.3(5) . . ? Mo1 Mo2 N4 92.8(6) . . ? N2 Mo2 N4 92.9(7) . . ? Mo1 Mo2 O8 91.0(4) . 2_565 ? N2 Mo2 O8 175.2(7) . 2_565 ? N4 Mo2 O8 89.0(6) . 2_565 ? Mo1 Mo2 O6 90.9(4) . . ? N2 Mo2 O6 89.4(6) . . ? N4 Mo2 O6 175.5(6) . . ? O8 Mo2 O6 88.4(5) 2_565 . ? C1 N1 C11 113.0(19) . . ? C1 N1 Mo1 120.6(15) . . ? C11 N1 Mo1 126.3(16) . . ? C1 N2 C21B 116(2) . . ? C1 N2 C21 124(3) . . ? C1 N2 Mo2 117.1(16) . . ? C21B N2 Mo2 126.7(18) . . ? C21 N2 Mo2 118(3) . . ? C41B N3 C2 121(2) . . ? C2 N3 C41 117(2) . . ? C41B N3 Mo1 123(2) . . ? C2 N3 Mo1 114.7(14) . . ? C41 N3 Mo1 127.6(19) . . ? C2 N4 C31 115(3) . . ? C2 N4 C31B 119(3) . . ? C2 N4 Mo2 117.4(14) . . ? C31 N4 Mo2 124(3) . . ? C31B N4 Mo2 123(3) . . ? N4 C2 N3 121.7(18) . . ? N2 C1 N1 117(2) . . ? C12 C11 C16 114.9(10) . . ? C12 C11 N1 118.3(12) . . ? C16 C11 N1 126.4(13) . . ? C13 C12 C11 124.6(10) . . ? C14 C13 C12 119.2(10) . . ? O1 C14 C13 126.2(13) . . ? O1 C14 C15 115.5(12) . . ? C13 C14 C15 118.2(10) . . ? C14 C15 C16 121.4(11) . . ? C11 C16 C15 121.6(11) . . ? C14 O1 C17 118.8(14) . . ? C26 C21 C22 114.6(12) . . ? C26 C21 N2 114(4) . . ? C22 C21 N2 131(4) . . ? C23 C22 C21 124.7(11) . . ? C24 C23 C22 118.8(11) . . ? O11 C24 C23 120(4) . . ? O11 C24 C25 121(4) . . ? C23 C24 C25 118.1(11) . . ? C24 C25 C26 121.4(11) . . ? C21 C26 C25 121.3(12) . . ? C24 O11 C27 105(6) . . ? C26B C21B C22B 114.7(11) . . ? C26B C21B N2 130(2) . . ? C22B C21B N2 115(2) . . ? C23B C22B C21B 124.8(10) . . ? C24B C23B C22B 118.6(11) . . ? O11B C24B C23B 122(2) . . ? O11B C24B C25B 120(2) . . ? C23B C24B C25B 118.0(11) . . ? C24B C25B C26B 121.4(11) . . ? C21B C26B C25B 121.4(11) . . ? C24B O11B C27B 120(3) . . ? N4 C31 C32 111(2) . . ? N4 C31 C36 134(3) . . ? C32 C31 C36 114.8(10) . . ? C33 C32 C31 124.8(11) . . ? C34 C33 C32 118.3(11) . . ? O3 C34 C33 126(3) . . ? O3 C34 C35 117(3) . . ? C33 C34 C35 117.2(11) . . ? C34 C35 C36 120.7(12) . . ? C31 C36 C35 121.1(12) . . ? C36B C31B C32B 114.7(11) . . ? C36B C31B N4 116(3) . . ? C32B C31B N4 129(3) . . ? C33B C32B C31B 124.9(11) . . ? C34B C33B C32B 118.9(11) . . ? O3B C34B C33B 124(4) . . ? O3B C34B C35B 118(4) . . ? C33B C34B C35B 117.8(11) . . ? C34B C35B C36B 121.2(12) . . ? C31B C36B C35B 121.2(12) . . ? C34 O3 C37 103(3) . . ? C34B O3B C37B 102(3) . . ? C46 C41 C42 114.3(11) . . ? C46 C41 N3 127(2) . . ? C42 C41 N3 118(2) . . ? C43 C42 C41 124.4(11) . . ? C44 C43 C42 118.7(11) . . ? O2 C44 C43 110(3) . . ? O2 C44 C45 131(3) . . ? C43 C44 C45 118.0(11) . . ? C44 C45 C46 121.6(11) . . ? C41 C46 C45 121.2(12) . . ? C44 O2 C47 116(4) . . ? N3 C41B C46B 126(3) . . ? N3 C41B C42B 119(2) . . ? C46B C41B C42B 114.7(11) . . ? C43B C42B C41B 124.7(11) . . ? C44B C43B C42B 118.6(11) . . ? O2B C44B C43B 135(3) . . ? O2B C44B C45B 107(2) . . ? C43B C44B C45B 117.9(11) . . ? C44B C45B C46B 121.3(12) . . ? C41B C46B C45B 121.4(12) . . ? C44B O2B C47B 110(2) . . ? C56 C51 C52 131.2(10) . . ? C56 C51 O10 115.1(15) . . ? C52 C51 O10 113.7(9) . . ? C51 C52 C53 108.7(8) . . ? C54 C53 C52 124.9(11) . . ? C55 C54 C53 119.1(10) . . ? C55 C54 O9 111.8(14) . . ? C53 C54 O9 129.1(14) . . ? C54 C55 C56 118.0(11) . . ? C51 C56 C55 117.9(11) . . ? O10 C57 C58 109(2) . . ? O10 C57 C59 114.9(18) . . ? C58 C57 C59 111.8(19) . . ? O7 C59 O8 121.6(16) . . ? O7 C59 C57 120(2) . . ? O8 C59 C57 118.5(18) . . ? O9 C60 C62 114.8(19) . . ? O9 C60 C61 107(2) . . ? C62 C60 C61 111(2) . . ? O6 C62 O5 120.6(17) . . ? O6 C62 C60 119(2) . . ? O5 C62 C60 120(2) . . ? C62 O5 Mo1 117.3(13) . . ? C62 O6 Mo2 117.5(13) . . ? C59 O7 Mo1 117.3(12) . 2_565 ? C59 O8 Mo2 117.5(11) . 2_565 ? C54 O9 C60 116.9(16) . . ? C57 O10 C51 124.4(15) . . ? Cl1 C1S Cl2 111.6(12) . . ? Cl4 C2S Cl3 115.8(16) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 22.55 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.718 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.135 #========================================================================= # compound 4*C6H6 #========================================================================= data_cmpd4 _database_code_CSD 217278 _chemical_name_common (Mo2(Danif)2(m-O2CC(CH3)2OC6H4OC(CH3)2CO2),C6H6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C44 H46 Mo2 N4 O10,C6H6' _chemical_formula_sum 'C50 H52 Mo2 N4 O10' _chemical_formula_weight 1060.84 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' 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 P21/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.837(5) _cell_length_b 16.094(5) _cell_length_c 19.036(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.727(5) _cell_angle_gamma 90.00 _cell_volume 4647(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 512 _cell_measurement_theta_min 4.970 _cell_measurement_theta_max 55.040 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7419 _exptl_absorpt_correction_T_max 0.9567 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Nonius APEX' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45863 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.58 _reflns_number_total 10508 _reflns_number_gt 8644 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0290P)^2^+2.7224P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10508 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.004 _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 Mo1 Mo 1.288080(13) 1.102349(11) -0.155826(11) 0.01578(6) Uani 1 1 d . . . Mo2 Mo 1.174688(13) 1.095048(11) -0.138108(11) 0.01564(6) Uani 1 1 d . . . O3 O 1.17604(10) 0.96178(9) -0.13976(8) 0.0184(3) Uani 1 1 d . . . O1 O 1.37274(10) 1.08680(9) -0.03598(9) 0.0191(3) Uani 1 1 d . . . O2 O 1.25285(10) 1.08304(9) -0.01423(9) 0.0179(3) Uani 1 1 d . . . N3 N 1.09047(12) 1.09837(10) -0.25907(11) 0.0167(4) Uani 1 1 d . . . O4 O 1.29747(10) 0.96939(9) -0.15897(9) 0.0191(3) Uani 1 1 d . . . N4 N 1.21576(13) 1.10901(10) -0.27734(10) 0.0168(4) Uani 1 1 d . . . N1 N 1.29732(12) 1.23285(11) -0.13997(10) 0.0174(4) Uani 1 1 d . . . N2 N 1.17027(12) 1.22507(11) -0.12440(10) 0.0171(4) Uani 1 1 d . . . C3 C 1.12864(16) 1.10534(12) -0.30710(13) 0.0183(5) Uani 1 1 d . . . H3A H 1.0946 1.1076 -0.3608 0.022 Uiso 1 1 calc R . . O7A O 1.39438(12) 1.16527(11) -0.46028(10) 0.0337(4) Uani 1 1 d . . . C2 C 1.23599(15) 1.27018(14) -0.12536(12) 0.0189(5) Uani 1 1 d . . . H2A H 1.2388 1.3271 -0.1159 0.023 Uiso 1 1 calc R . . C4 C 1.24187(15) 0.92886(14) -0.14428(12) 0.0190(5) Uani 1 1 d . . . C1 C 1.33519(15) 1.07621(13) 0.00847(13) 0.0186(5) Uani 1 1 d . . . C8 C 1.36274(16) 1.36277(13) -0.16136(13) 0.0210(5) Uani 1 1 d . . . H8A H 1.3108 1.3917 -0.1727 0.025 Uiso 1 1 calc R . . C8A C 1.43323(17) 1.40288(14) -0.16547(14) 0.0246(5) Uani 1 1 d . . . H8AA H 1.4285 1.4588 -0.1792 0.029 Uiso 1 1 calc R . . C8C C 1.51119(15) 1.36040(14) -0.14929(13) 0.0224(5) Uani 1 1 d . . . C8D C 1.51940(16) 1.27807(14) -0.12667(13) 0.0243(5) Uani 1 1 d . . . H8DA H 1.5717 1.2494 -0.1147 0.029 Uiso 1 1 calc R . . C8E C 1.44822(16) 1.23878(14) -0.12217(13) 0.0224(5) Uani 1 1 d . . . H8EA H 1.4540 1.1835 -0.1064 0.027 Uiso 1 1 calc R . . C8B C 1.36902(15) 1.27915(13) -0.14035(12) 0.0177(4) Uani 1 1 d . . . C7 C 1.25835(15) 1.12028(13) -0.32710(13) 0.0178(5) Uani 1 1 d . . . C7A C 1.34049(17) 1.08476(14) -0.30567(14) 0.0250(5) Uani 1 1 d . . . H7AA H 1.3639 1.0509 -0.2617 0.030 Uiso 1 1 calc R . . C7C C 1.38897(17) 1.09822(14) -0.34790(14) 0.0247(5) Uani 1 1 d . . . H7CA H 1.4444 1.0744 -0.3320 0.030 Uiso 1 1 calc R . . C7B C 1.35389(16) 1.14712(15) -0.41344(14) 0.0240(5) Uani 1 1 d . . . C7E C 1.27148(17) 1.18286(16) -0.43553(14) 0.0287(6) Uani 1 1 d . . . H7EA H 1.2481 1.2164 -0.4797 0.034 Uiso 1 1 calc R . . C7D C 1.22375(16) 1.16966(15) -0.39344(13) 0.0248(5) Uani 1 1 d . . . H7DA H 1.1684 1.1938 -0.4094 0.030 Uiso 1 1 calc R . . O8A O 1.57523(12) 1.40517(10) -0.15929(11) 0.0311(4) Uani 1 1 d . . . C7F C 1.48038(17) 1.13356(17) -0.43819(16) 0.0315(6) Uani 1 1 d . . . H7FA H 1.5015 1.1510 -0.4753 0.047 Uiso 1 1 calc R . . H7FB H 1.4789 1.0740 -0.4369 0.047 Uiso 1 1 calc R . . H7FC H 1.5190 1.1542 -0.3874 0.047 Uiso 1 1 calc R . . O9 O 1.21997(11) 0.80274(9) -0.08182(9) 0.0221(3) Uani 1 1 d . . . O10 O 1.34901(11) 1.00726(10) 0.12790(9) 0.0236(4) Uani 1 1 d . . . C11 C 1.35062(17) 0.80865(15) -0.10522(16) 0.0293(6) Uani 1 1 d . . . H11A H 1.3858 0.8350 -0.0562 0.044 Uiso 1 1 calc R . . H11B H 1.3713 0.8251 -0.1429 0.044 Uiso 1 1 calc R . . H11C H 1.3553 0.7494 -0.0988 0.044 Uiso 1 1 calc R . . C10 C 1.19683(18) 0.79410(15) -0.21132(14) 0.0288(6) Uani 1 1 d . . . H10A H 1.2035 0.7348 -0.2065 0.043 Uiso 1 1 calc R . . H10B H 1.2141 0.8134 -0.2504 0.043 Uiso 1 1 calc R . . H10C H 1.1363 0.8085 -0.2261 0.043 Uiso 1 1 calc R . . C9 C 1.25494(16) 0.83460(13) -0.13335(13) 0.0212(5) Uani 1 1 d . . . C18 C 1.39483(15) 1.05527(14) 0.09315(13) 0.0213(5) Uani 1 1 d . . . C20 C 1.47871(16) 1.01120(16) 0.10286(14) 0.0294(6) Uani 1 1 d . . . H20A H 1.4639 0.9601 0.0740 0.044 Uiso 1 1 calc R . . H20B H 1.5142 0.9996 0.1571 0.044 Uiso 1 1 calc R . . H20C H 1.5111 1.0461 0.0836 0.044 Uiso 1 1 calc R . . C19 C 1.41626(18) 1.13696(16) 0.13824(14) 0.0308(6) Uani 1 1 d . . . H19A H 1.3625 1.1639 0.1314 0.046 Uiso 1 1 calc R . . H19B H 1.4484 1.1724 0.1191 0.046 Uiso 1 1 calc R . . H19C H 1.4514 1.1260 0.1926 0.046 Uiso 1 1 calc R . . C8F C 1.64947(18) 1.36049(18) -0.15576(19) 0.0419(7) Uani 1 1 d . . . H8FA H 1.6892 1.3980 -0.1636 0.063 Uiso 1 1 calc R . . H8FB H 1.6304 1.3187 -0.1957 0.063 Uiso 1 1 calc R . . H8FC H 1.6790 1.3345 -0.1056 0.063 Uiso 1 1 calc R . . C5 C 0.93928(16) 1.11831(13) -0.36495(13) 0.0213(5) Uani 1 1 d . . . H5A H 0.9612 1.1481 -0.3946 0.026 Uiso 1 1 calc R . . C5E C 0.99660(15) 1.08972(12) -0.29202(13) 0.0176(4) Uani 1 1 d . . . C5A C 0.96122(16) 1.04891(14) -0.24747(14) 0.0240(5) Uani 1 1 d . . . H5AA H 0.9986 1.0304 -0.1977 0.029 Uiso 1 1 calc R . . C5B C 0.87158(17) 1.03545(15) -0.27605(14) 0.0271(5) Uani 1 1 d . . . H5BA H 0.8490 1.0091 -0.2451 0.033 Uiso 1 1 calc R . . C5C C 0.81538(16) 1.06095(14) -0.35033(14) 0.0238(5) Uani 1 1 d . . . C5D C 0.84937(16) 1.10322(14) -0.39466(14) 0.0234(5) Uani 1 1 d . . . H5DA H 0.8118 1.1215 -0.4445 0.028 Uiso 1 1 calc R . . O5A O 0.72764(12) 1.04252(11) -0.37490(10) 0.0333(4) Uani 1 1 d . . . C5F C 0.67243(17) 1.05151(19) -0.45550(16) 0.0380(7) Uani 1 1 d . . . H5FA H 0.6131 1.0367 -0.4659 0.057 Uiso 1 1 calc R . . H5FB H 0.6928 1.0157 -0.4846 0.057 Uiso 1 1 calc R . . H5FC H 0.6739 1.1082 -0.4707 0.057 Uiso 1 1 calc R . . C12 C 1.24138(16) 0.83527(13) -0.00897(13) 0.0215(5) Uani 1 1 d . . . C13 C 1.29693(15) 0.90280(13) 0.02356(13) 0.0204(5) Uani 1 1 d . . . H13A H 1.3282 0.9261 -0.0016 0.025 Uiso 1 1 calc R . . C14 C 1.30512(15) 0.93507(14) 0.09415(13) 0.0222(5) Uani 1 1 d . . . C15 C 1.26396(16) 0.89641(15) 0.13478(14) 0.0268(5) Uani 1 1 d . . . H15A H 1.2712 0.9169 0.1829 0.032 Uiso 1 1 calc R . . C16 C 1.21233(17) 0.82737(15) 0.10297(15) 0.0290(6) Uani 1 1 d . . . H16A H 1.1854 0.8009 0.1304 0.035 Uiso 1 1 calc R . . C17 C 1.19985(16) 0.79668(14) 0.03107(14) 0.0242(5) Uani 1 1 d . . . H17A H 1.1640 0.7507 0.0098 0.029 Uiso 1 1 calc R . . C1S C 0.8450(2) 0.89525(16) -0.12883(16) 0.0340(6) Uani 1 1 d G . . H1SA H 0.7932 0.9097 -0.1257 0.041 Uiso 1 1 calc R . . C2S C 0.84530(18) 0.83099(15) -0.17692(14) 0.0287(6) Uani 1 1 d G . . H2SA H 0.7937 0.8019 -0.2062 0.034 Uiso 1 1 calc R . . C3S C 0.92290(18) 0.81028(14) -0.18121(14) 0.0270(5) Uani 1 1 d G . . H3SA H 0.9231 0.7676 -0.2141 0.032 Uiso 1 1 calc R . . C4S C 0.99965(18) 0.85233(16) -0.13731(15) 0.0298(6) Uani 1 1 d G . . H4SA H 1.0516 0.8376 -0.1401 0.036 Uiso 1 1 calc R . . C5S C 0.99958(19) 0.91570(16) -0.08963(15) 0.0329(6) Uani 1 1 d G . . H5SA H 1.0516 0.9440 -0.0599 0.040 Uiso 1 1 calc R . . C6S C 0.9222(2) 0.93791(16) -0.08539(15) 0.0371(7) Uani 1 1 d G . . H6SA H 0.9223 0.9815 -0.0533 0.044 Uiso 1 1 calc R . . C6 C 1.10431(15) 1.26507(13) -0.10871(12) 0.0184(5) Uani 1 1 d . . . C6A C 1.07043(15) 1.22191(13) -0.06372(13) 0.0191(5) Uani 1 1 d . . . H6AA H 1.0908 1.1686 -0.0461 0.023 Uiso 1 1 calc R . . C6B C 1.00745(15) 1.25735(14) -0.04524(13) 0.0208(5) Uani 1 1 d . . . H6BA H 0.9857 1.2279 -0.0153 0.025 Uiso 1 1 calc R . . C6D C 0.97639(15) 1.33660(14) -0.07097(13) 0.0205(5) Uani 1 1 d . . . C6E C 1.00838(16) 1.38019(14) -0.11658(13) 0.0219(5) Uani 1 1 d . . . H6EA H 0.9875 1.4333 -0.1344 0.026 Uiso 1 1 calc R . . C6C C 1.07182(16) 1.34379(14) -0.13532(13) 0.0215(5) Uani 1 1 d . . . H6CA H 1.0927 1.3728 -0.1662 0.026 Uiso 1 1 calc R . . C6F C 0.88064(17) 1.44779(14) -0.07447(16) 0.0301(6) Uani 1 1 d . . . H6FA H 0.8379 1.4615 -0.0555 0.045 Uiso 1 1 calc R . . H6FB H 0.8533 1.4497 -0.1304 0.045 Uiso 1 1 calc R . . H6FC H 0.9282 1.4871 -0.0546 0.045 Uiso 1 1 calc R . . O6A O 0.91396(11) 1.36654(10) -0.04919(10) 0.0274(4) Uiso 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 Mo1 0.01684(11) 0.01678(10) 0.01563(10) 0.00207(7) 0.00884(8) -0.00009(7) Mo2 0.01653(11) 0.01655(10) 0.01549(10) 0.00242(7) 0.00849(8) 0.00034(7) O3 0.0183(9) 0.0188(8) 0.0196(8) 0.0025(6) 0.0096(7) 0.0008(6) O1 0.0184(8) 0.0231(8) 0.0173(8) 0.0016(6) 0.0091(7) -0.0017(6) O2 0.0173(8) 0.0200(7) 0.0166(8) 0.0027(6) 0.0075(7) 0.0003(6) N3 0.0167(10) 0.0151(9) 0.0180(9) 0.0016(7) 0.0073(8) 0.0004(7) O4 0.0200(9) 0.0195(8) 0.0199(8) 0.0018(6) 0.0107(7) -0.0002(6) N4 0.0201(10) 0.0158(9) 0.0166(9) 0.0011(7) 0.0100(8) 0.0007(7) N1 0.0202(10) 0.0176(9) 0.0167(9) 0.0004(7) 0.0102(8) -0.0016(8) N2 0.0195(10) 0.0200(9) 0.0145(9) 0.0019(7) 0.0098(8) 0.0011(8) C3 0.0233(12) 0.0164(10) 0.0159(11) 0.0002(8) 0.0091(9) -0.0002(9) O7A 0.0331(11) 0.0473(11) 0.0306(10) 0.0123(8) 0.0231(9) 0.0113(9) C2 0.0227(12) 0.0184(10) 0.0171(11) 0.0011(8) 0.0101(10) -0.0003(9) C4 0.0202(12) 0.0205(11) 0.0155(11) 0.0002(8) 0.0071(10) -0.0012(9) C1 0.0216(12) 0.0164(10) 0.0193(11) -0.0006(8) 0.0101(10) -0.0015(9) C8 0.0215(12) 0.0197(11) 0.0232(12) 0.0001(9) 0.0111(10) 0.0013(9) C8A 0.0274(14) 0.0194(11) 0.0265(13) 0.0008(9) 0.0113(11) -0.0030(10) C8C 0.0199(13) 0.0258(12) 0.0206(12) -0.0005(9) 0.0080(10) -0.0080(10) C8D 0.0204(13) 0.0265(12) 0.0256(13) 0.0024(9) 0.0095(10) 0.0009(10) C8E 0.0248(13) 0.0189(11) 0.0238(12) 0.0028(9) 0.0107(10) -0.0013(10) C8B 0.0197(12) 0.0200(11) 0.0143(10) -0.0018(8) 0.0081(9) -0.0025(9) C7 0.0208(12) 0.0183(10) 0.0168(11) -0.0012(8) 0.0104(9) -0.0001(9) C7A 0.0283(14) 0.0260(12) 0.0224(12) 0.0079(9) 0.0126(11) 0.0056(10) C7C 0.0219(13) 0.0269(12) 0.0285(13) 0.0041(10) 0.0138(11) 0.0063(10) C7B 0.0268(13) 0.0289(12) 0.0225(12) 0.0016(9) 0.0163(11) 0.0034(10) C7E 0.0303(15) 0.0398(14) 0.0194(12) 0.0109(10) 0.0139(11) 0.0103(11) C7D 0.0212(13) 0.0350(13) 0.0202(12) 0.0047(10) 0.0108(10) 0.0086(10) O8A 0.0217(10) 0.0292(9) 0.0440(11) 0.0074(8) 0.0157(9) -0.0052(7) C7F 0.0268(14) 0.0411(15) 0.0332(14) 0.0030(11) 0.0192(12) 0.0024(12) O9 0.0264(9) 0.0191(8) 0.0237(8) 0.0020(6) 0.0137(7) -0.0033(7) O10 0.0252(9) 0.0288(9) 0.0174(8) 0.0021(6) 0.0099(7) -0.0044(7) C11 0.0313(15) 0.0228(12) 0.0411(15) 0.0068(10) 0.0224(13) 0.0055(11) C10 0.0397(16) 0.0235(12) 0.0283(13) -0.0033(10) 0.0195(12) -0.0052(11) C9 0.0245(13) 0.0192(11) 0.0235(12) 0.0036(9) 0.0138(10) 0.0003(9) C18 0.0205(12) 0.0270(12) 0.0166(11) 0.0019(9) 0.0082(10) -0.0045(10) C20 0.0217(13) 0.0415(15) 0.0220(12) 0.0075(11) 0.0066(11) 0.0005(11) C19 0.0360(16) 0.0340(14) 0.0214(13) -0.0051(10) 0.0117(12) -0.0110(12) C8F 0.0267(15) 0.0417(16) 0.064(2) 0.0107(14) 0.0255(15) -0.0015(13) C5 0.0237(13) 0.0200(11) 0.0216(12) 0.0022(9) 0.0113(10) -0.0004(9) C5E 0.0177(12) 0.0149(10) 0.0195(11) -0.0017(8) 0.0076(9) 0.0005(9) C5A 0.0247(13) 0.0265(12) 0.0221(12) 0.0041(9) 0.0113(11) 0.0003(10) C5B 0.0277(14) 0.0277(13) 0.0290(13) 0.0041(10) 0.0152(11) -0.0035(10) C5C 0.0204(13) 0.0216(11) 0.0292(13) -0.0032(9) 0.0106(11) -0.0023(10) C5D 0.0212(13) 0.0218(11) 0.0231(12) 0.0020(9) 0.0059(10) 0.0012(10) O5A 0.0203(10) 0.0432(11) 0.0341(10) 0.0012(8) 0.0098(8) -0.0076(8) C5F 0.0209(14) 0.0514(17) 0.0356(15) -0.0080(13) 0.0066(12) -0.0038(13) C12 0.0217(13) 0.0209(11) 0.0223(12) 0.0065(9) 0.0100(10) 0.0053(9) C13 0.0197(12) 0.0216(11) 0.0217(12) 0.0089(9) 0.0106(10) 0.0021(9) C14 0.0191(12) 0.0250(12) 0.0218(12) 0.0049(9) 0.0082(10) 0.0007(10) C15 0.0279(14) 0.0340(14) 0.0214(12) 0.0073(10) 0.0134(11) 0.0017(11) C16 0.0296(15) 0.0314(13) 0.0308(14) 0.0100(10) 0.0177(12) -0.0001(11) C17 0.0241(13) 0.0223(11) 0.0276(13) 0.0052(9) 0.0125(11) -0.0015(10) C1S 0.0382(16) 0.0409(15) 0.0316(14) 0.0116(12) 0.0232(13) 0.0121(13) C2S 0.0275(14) 0.0296(13) 0.0237(13) 0.0060(10) 0.0063(11) -0.0050(11) C3S 0.0387(16) 0.0211(11) 0.0218(12) 0.0021(9) 0.0137(11) 0.0025(11) C4S 0.0285(14) 0.0341(14) 0.0288(14) 0.0117(11) 0.0144(12) 0.0034(11) C5S 0.0366(16) 0.0317(14) 0.0226(13) 0.0014(10) 0.0055(12) -0.0092(12) C6S 0.061(2) 0.0292(14) 0.0219(13) -0.0039(10) 0.0189(14) 0.0026(13) C6 0.0199(12) 0.0225(11) 0.0141(11) -0.0019(8) 0.0086(9) -0.0020(9) C6A 0.0216(12) 0.0164(10) 0.0208(11) 0.0029(8) 0.0106(10) 0.0005(9) C6B 0.0231(12) 0.0218(11) 0.0206(11) 0.0030(9) 0.0125(10) -0.0036(9) C6D 0.0206(12) 0.0231(11) 0.0199(11) 0.0003(9) 0.0108(10) 0.0017(9) C6E 0.0252(13) 0.0174(11) 0.0250(12) 0.0042(9) 0.0127(11) 0.0018(9) C6C 0.0257(13) 0.0225(11) 0.0200(12) 0.0025(9) 0.0135(10) -0.0018(10) C6F 0.0311(15) 0.0242(12) 0.0422(15) 0.0056(11) 0.0225(13) 0.0080(11) _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 Mo1 Mo2 2.0812(7) . ? Mo1 N4 2.0975(19) . ? Mo1 O1 2.1156(16) . ? Mo1 N1 2.1179(19) . ? Mo1 O4 2.1483(16) . ? Mo2 N2 2.1141(19) . ? Mo2 N3 2.1167(19) . ? Mo2 O3 2.1452(16) . ? Mo2 O2 2.1531(16) . ? O3 C4 1.265(3) . ? O1 C1 1.269(3) . ? O2 C1 1.265(3) . ? N3 C3 1.331(3) . ? N3 C5E 1.432(3) . ? O4 C4 1.268(3) . ? N4 C3 1.325(3) . ? N4 C7 1.426(3) . ? N1 C2 1.324(3) . ? N1 C8B 1.421(3) . ? N2 C2 1.330(3) . ? N2 C6 1.423(3) . ? O7A C7B 1.368(3) . ? O7A C7F 1.416(3) . ? C4 C9 1.534(3) . ? C1 C18 1.521(3) . ? C8 C8A 1.383(3) . ? C8 C8B 1.395(3) . ? C8A C8C 1.391(3) . ? C8C O8A 1.377(3) . ? C8C C8D 1.381(3) . ? C8D C8E 1.390(3) . ? C8E C8B 1.385(3) . ? C7 C7A 1.384(3) . ? C7 C7D 1.388(3) . ? C7A C7C 1.389(3) . ? C7C C7B 1.373(3) . ? C7B C7E 1.388(3) . ? C7E C7D 1.375(3) . ? O8A C8F 1.418(3) . ? O9 C12 1.376(3) . ? O9 C9 1.440(3) . ? O10 C14 1.377(3) . ? O10 C18 1.440(3) . ? C11 C9 1.519(3) . ? C10 C9 1.525(3) . ? C18 C20 1.518(3) . ? C18 C19 1.525(3) . ? C5 C5E 1.381(3) . ? C5 C5D 1.388(3) . ? C5E C5A 1.394(3) . ? C5A C5B 1.381(3) . ? C5B C5C 1.379(3) . ? C5C O5A 1.374(3) . ? C5C C5D 1.386(3) . ? O5A C5F 1.414(3) . ? C12 C17 1.385(3) . ? C12 C13 1.392(3) . ? C13 C14 1.391(3) . ? C14 C15 1.389(3) . ? C15 C16 1.378(3) . ? C16 C17 1.382(3) . ? C1S C2S 1.383(4) . ? C1S C6S 1.383(4) . ? C2S C3S 1.385(4) . ? C3S C4S 1.374(4) . ? C4S C5S 1.366(4) . ? C5S C6S 1.386(4) . ? C6 C6C 1.386(3) . ? C6 C6A 1.402(3) . ? C6A C6B 1.377(3) . ? C6B C6D 1.385(3) . ? C6D O6A 1.374(3) . ? C6D C6E 1.394(3) . ? C6E C6C 1.394(3) . ? C6F O6A 1.422(3) . ? 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 Mo2 Mo1 N4 92.72(6) . . ? Mo2 Mo1 O1 93.13(5) . . ? N4 Mo1 O1 172.80(6) . . ? Mo2 Mo1 N1 92.79(5) . . ? N4 Mo1 N1 94.48(7) . . ? O1 Mo1 N1 89.44(6) . . ? Mo2 Mo1 O4 91.84(4) . . ? N4 Mo1 O4 91.98(6) . . ? O1 Mo1 O4 83.63(6) . . ? N1 Mo1 O4 171.86(7) . . ? Mo1 Mo2 N2 92.75(5) . . ? Mo1 Mo2 N3 92.91(6) . . ? N2 Mo2 N3 93.81(7) . . ? Mo1 Mo2 O3 92.17(4) . . ? N2 Mo2 O3 173.01(6) . . ? N3 Mo2 O3 90.90(6) . . ? Mo1 Mo2 O2 90.86(5) . . ? N2 Mo2 O2 89.50(6) . . ? N3 Mo2 O2 174.86(6) . . ? O3 Mo2 O2 85.47(6) . . ? C4 O3 Mo2 115.78(14) . . ? C1 O1 Mo1 115.95(15) . . ? C1 O2 Mo2 116.11(14) . . ? C3 N3 C5E 118.52(19) . . ? C3 N3 Mo2 117.01(16) . . ? C5E N3 Mo2 124.40(14) . . ? C4 O4 Mo1 115.84(14) . . ? C3 N4 C7 120.28(19) . . ? C3 N4 Mo1 118.32(15) . . ? C7 N4 Mo1 121.36(15) . . ? C2 N1 C8B 120.30(19) . . ? C2 N1 Mo1 117.65(15) . . ? C8B N1 Mo1 121.95(14) . . ? C2 N2 C6 119.06(19) . . ? C2 N2 Mo2 117.68(15) . . ? C6 N2 Mo2 123.10(14) . . ? N4 C3 N3 119.0(2) . . ? C7B O7A C7F 117.6(2) . . ? N1 C2 N2 119.0(2) . . ? O3 C4 O4 123.5(2) . . ? O3 C4 C9 118.9(2) . . ? O4 C4 C9 117.55(19) . . ? O2 C1 O1 123.4(2) . . ? O2 C1 C18 120.2(2) . . ? O1 C1 C18 116.5(2) . . ? C8A C8 C8B 120.4(2) . . ? C8 C8A C8C 120.6(2) . . ? O8A C8C C8D 124.5(2) . . ? O8A C8C C8A 115.6(2) . . ? C8D C8C C8A 119.8(2) . . ? C8C C8D C8E 118.9(2) . . ? C8B C8E C8D 122.2(2) . . ? C8E C8B C8 118.0(2) . . ? C8E C8B N1 118.71(19) . . ? C8 C8B N1 123.3(2) . . ? C7A C7 C7D 118.4(2) . . ? C7A C7 N4 118.5(2) . . ? C7D C7 N4 122.9(2) . . ? C7 C7A C7C 121.9(2) . . ? C7B C7C C7A 119.1(2) . . ? O7A C7B C7C 125.1(2) . . ? O7A C7B C7E 115.4(2) . . ? C7C C7B C7E 119.5(2) . . ? C7D C7E C7B 121.3(2) . . ? C7E C7D C7 119.9(2) . . ? C8C O8A C8F 117.1(2) . . ? C12 O9 C9 123.05(17) . . ? C14 O10 C18 121.63(17) . . ? O9 C9 C11 110.29(19) . . ? O9 C9 C10 103.39(18) . . ? C11 C9 C10 111.1(2) . . ? O9 C9 C4 111.57(18) . . ? C11 C9 C4 112.79(19) . . ? C10 C9 C4 107.28(19) . . ? O10 C18 C20 110.42(19) . . ? O10 C18 C1 111.52(18) . . ? C20 C18 C1 112.56(19) . . ? O10 C18 C19 104.31(18) . . ? C20 C18 C19 110.7(2) . . ? C1 C18 C19 106.94(19) . . ? C5E C5 C5D 120.9(2) . . ? C5 C5E C5A 118.2(2) . . ? C5 C5E N3 124.4(2) . . ? C5A C5E N3 117.5(2) . . ? C5B C5A C5E 121.1(2) . . ? C5C C5B C5A 120.2(2) . . ? O5A C5C C5B 116.3(2) . . ? O5A C5C C5D 124.4(2) . . ? C5B C5C C5D 119.3(2) . . ? C5C C5D C5 120.2(2) . . ? C5C O5A C5F 116.8(2) . . ? O9 C12 C17 114.2(2) . . ? O9 C12 C13 125.2(2) . . ? C17 C12 C13 120.5(2) . . ? C14 C13 C12 119.2(2) . . ? O10 C14 C15 114.5(2) . . ? O10 C14 C13 125.0(2) . . ? C15 C14 C13 120.4(2) . . ? C16 C15 C14 119.2(2) . . ? C15 C16 C17 121.3(2) . . ? C16 C17 C12 119.2(2) . . ? C2S C1S C6S 119.7(3) . . ? C3S C2S C1S 119.6(2) . . ? C2S C3S C4S 120.5(2) . . ? C5S C4S C3S 120.0(3) . . ? C4S C5S C6S 120.2(3) . . ? C5S C6S C1S 120.0(2) . . ? C6C C6 C6A 118.4(2) . . ? C6C C6 N2 123.8(2) . . ? C6A C6 N2 117.76(19) . . ? C6B C6A C6 120.9(2) . . ? C6A C6B C6D 120.4(2) . . ? O6A C6D C6B 115.9(2) . . ? O6A C6D C6E 124.4(2) . . ? C6B C6D C6E 119.7(2) . . ? C6C C6E C6D 119.6(2) . . ? C6 C6C C6E 121.0(2) . . ? C6D O6A C6F 117.49(18) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.969 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.076