# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1455 data_global # _publ_contact_autor ; J\"org Sundermeyer Fachbereich Chemie der Universit\"at Philipps Universit\"at Marburg Hans-Meerwein-Str. 35032 Marburg Bundesrepublik Deutschland ; _publ_contact_author_phone '+49 6421 285693 ' _publ_contact_author_fax '+49 6421 288917 ' _publ_contact_author_email kipke@chemie.uni-marburg.de _publ_requested_journal 'Chem.Commun.' _publ_requested_coeditor_name ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; The first configuratively stable chiral diimido chelate complexes of molybdenum and tungsten: Transition metal diimido complexes on the way to asymmetric catalysis. ; loop_ _publ_author_name _publ_author_address 'Kretzschmar, E.' ; Fachbereich Chemie der Philipps Universit\"at Hans-Meerwein-Str. 35032 Marburg Bundesrepublik Deutschland ; 'Kipke, J.' ; Fachbereich Chemie der Philipps Universit\"at Hans-Meerwein-Str. 35032 Marburg Bundesrepublik Deutschland ; 'Sundermeyer, J.' ; Fachbereich Chemie der Philipps Universit\"at Hans-Meerwein-Str. 35032 Marburg Bundesrepublik Deutschland ; #======================================================================= data_ek01 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H46 Cl2 Mo N2 O4' _chemical_formula_weight 809.65 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' 'Cl' 'Cl' 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5718(14) _cell_length_b 14.8923(14) _cell_length_c 12.5186(11) _cell_angle_alpha 90.000(8) _cell_angle_beta 91.504(10) _cell_angle_gamma 90.000(12) _cell_volume 1970.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8413 _exptl_absorpt_correction_T_max 0.8828 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6389 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6027 _reflns_number_gt 5748 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0567P)^2^+0.1820P] 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 ? _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 6027 _refine_ls_number_parameters 465 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.28618(2) 0.198020(17) 0.222518(18) 0.02514(9) Uani 1 1 d . . . Cl1 Cl 0.29664(9) 0.35094(6) 0.28445(7) 0.0394(2) Uani 1 1 d . . . Cl2 Cl 0.20442(9) 0.06852(6) 0.12977(8) 0.0419(2) Uani 1 1 d . . . N1 N 0.4405(2) 0.1942(3) 0.17849(18) 0.0269(5) Uani 1 1 d . . . N2 N 0.3072(3) 0.14441(19) 0.3451(2) 0.0284(6) Uani 1 1 d . . . O1 O 0.7103(2) 0.14033(16) 0.35724(19) 0.0324(6) Uani 1 1 d . . . O2 O 0.5970(2) 0.02201(18) 0.4205(2) 0.0384(6) Uani 1 1 d . . . O3 O 0.2070(2) 0.26724(19) 0.06438(19) 0.0371(6) Uani 1 1 d . . . O4 O 0.0659(2) 0.22835(17) 0.23349(19) 0.0360(6) Uani 1 1 d . . . C1 C 0.5751(3) 0.1840(3) 0.2038(2) 0.0264(8) Uani 1 1 d . . . C2 C 0.5823(3) 0.1571(2) 0.3251(3) 0.0260(7) Uani 1 1 d . . . H2B H 0.5497 0.2076 0.3679 0.031 Uiso 1 1 calc R . . C3 C 0.5096(3) 0.0706(2) 0.3541(3) 0.0294(7) Uani 1 1 d . . . H3A H 0.4910 0.0357 0.2883 0.035 Uiso 1 1 calc R . . C4 C 0.3842(3) 0.0867(2) 0.4146(3) 0.0285(7) Uani 1 1 d . . . C5 C 0.7217(3) 0.0561(3) 0.4121(3) 0.0369(8) Uani 1 1 d . . . C6 C 0.7998(4) -0.0091(3) 0.3482(4) 0.0538(11) Uani 1 1 d . . . H6A H 0.7568 -0.0214 0.2804 0.081 Uiso 1 1 calc R . . H6B H 0.8106 -0.0646 0.3880 0.081 Uiso 1 1 calc R . . H6C H 0.8821 0.0171 0.3354 0.081 Uiso 1 1 calc R . . C7 C 0.7772(5) 0.0722(3) 0.5233(4) 0.0519(12) Uani 1 1 d . . . H7A H 0.7207 0.1103 0.5630 0.078 Uiso 1 1 calc R . . H7B H 0.8588 0.1014 0.5182 0.078 Uiso 1 1 calc R . . H7C H 0.7876 0.0152 0.5600 0.078 Uiso 1 1 calc R . . C8 C 0.2687(5) 0.2486(4) -0.0351(3) 0.0550(12) Uani 1 1 d . . . H8A H 0.2398 0.2912 -0.0891 0.083 Uiso 1 1 calc R . . H8B H 0.2480 0.1881 -0.0584 0.083 Uiso 1 1 calc R . . H8C H 0.3596 0.2540 -0.0245 0.083 Uiso 1 1 calc R . . C9 C 0.0721(4) 0.2693(3) 0.0517(3) 0.0456(10) Uani 1 1 d . . . H9A H 0.0404 0.2103 0.0288 0.055 Uiso 1 1 calc R . . H9B H 0.0467 0.3137 -0.0024 0.055 Uiso 1 1 calc R . . C10 C 0.0194(4) 0.2937(3) 0.1572(3) 0.0443(10) Uani 1 1 d . . . H10A H 0.0470 0.3541 0.1783 0.053 Uiso 1 1 calc R . . H10B H -0.0733 0.2927 0.1532 0.053 Uiso 1 1 calc R . . C11 C 0.0148(4) 0.2444(3) 0.3391(3) 0.0507(11) Uani 1 1 d . . . H11A H -0.0769 0.2426 0.3344 0.076 Uiso 1 1 calc R . . H11B H 0.0421 0.3029 0.3648 0.076 Uiso 1 1 calc R . . H11C H 0.0452 0.1983 0.3882 0.076 Uiso 1 1 calc R . . C20 C 0.6340(3) 0.2764(2) 0.1826(3) 0.0258(7) Uani 1 1 d . . . C21 C 0.6435(4) 0.3055(3) 0.0771(3) 0.0374(9) Uani 1 1 d . . . H21A H 0.6166 0.2673 0.0211 0.045 Uiso 1 1 calc R . . C22 C 0.6916(4) 0.3893(3) 0.0533(3) 0.0450(10) Uani 1 1 d . . . H22A H 0.6979 0.4072 -0.0184 0.054 Uiso 1 1 calc R . . C23 C 0.7305(4) 0.4468(3) 0.1343(4) 0.0444(10) Uani 1 1 d . . . H23A H 0.7629 0.5038 0.1182 0.053 Uiso 1 1 calc R . . C24 C 0.7214(4) 0.4196(3) 0.2388(3) 0.0426(9) Uani 1 1 d . . . H24A H 0.7470 0.4586 0.2943 0.051 Uiso 1 1 calc R . . C25 C 0.6745(4) 0.3346(3) 0.2635(3) 0.0356(8) Uani 1 1 d . . . H25A H 0.6701 0.3166 0.3352 0.043 Uiso 1 1 calc R . . C30 C 0.6326(3) 0.1128(3) 0.1306(3) 0.0288(8) Uani 1 1 d . . . C31 C 0.5583(4) 0.0551(3) 0.0697(3) 0.0403(9) Uani 1 1 d . . . H31A H 0.4697 0.0572 0.0743 0.048 Uiso 1 1 calc R . . C32 C 0.6143(5) -0.0063(3) 0.0011(4) 0.0515(11) Uani 1 1 d . . . H32A H 0.5631 -0.0451 -0.0406 0.062 Uiso 1 1 calc R . . C33 C 0.7431(4) -0.0105(3) -0.0056(4) 0.0521(11) Uani 1 1 d . . . H33A H 0.7802 -0.0515 -0.0525 0.062 Uiso 1 1 calc R . . C34 C 0.8183(4) 0.0453(3) 0.0560(3) 0.0446(10) Uani 1 1 d . . . H34A H 0.9068 0.0414 0.0525 0.054 Uiso 1 1 calc R . . C35 C 0.7643(4) 0.1072(3) 0.1231(3) 0.0367(8) Uani 1 1 d . . . H35A H 0.8163 0.1460 0.1641 0.044 Uiso 1 1 calc R . . C40 C 0.4077(4) 0.1334(3) 0.5239(3) 0.0346(9) Uani 1 1 d . . . C41 C 0.4560(4) 0.0821(3) 0.6100(3) 0.0471(10) Uani 1 1 d . . . H41A H 0.4742 0.0208 0.6007 0.057 Uiso 1 1 calc R . . C42 C 0.4767(5) 0.1227(4) 0.7086(3) 0.0625(14) Uani 1 1 d . . . H42A H 0.5107 0.0887 0.7658 0.075 Uiso 1 1 calc R . . C43 C 0.4485(4) 0.2108(5) 0.7243(3) 0.0645(16) Uani 1 1 d . . . H43A H 0.4625 0.2372 0.7918 0.077 Uiso 1 1 calc R . . C44 C 0.3987(4) 0.2619(3) 0.6394(4) 0.0540(12) Uani 1 1 d . . . H44A H 0.3788 0.3228 0.6496 0.065 Uiso 1 1 calc R . . C45 C 0.3789(4) 0.2221(3) 0.5400(3) 0.0414(10) Uani 1 1 d . . . H45A H 0.3454 0.2564 0.4830 0.050 Uiso 1 1 calc R . . C50 C 0.3091(3) -0.0008(2) 0.4297(3) 0.0310(8) Uani 1 1 d . . . C51 C 0.3585(4) -0.0844(3) 0.4102(3) 0.0431(10) Uani 1 1 d . . . H51A H 0.4408 -0.0895 0.3843 0.052 Uiso 1 1 calc R . . C52 C 0.2880(4) -0.1621(3) 0.4286(3) 0.0469(10) Uani 1 1 d . . . H52A H 0.3234 -0.2189 0.4159 0.056 Uiso 1 1 calc R . . C53 C 0.1669(4) -0.1555(3) 0.4652(3) 0.0453(11) Uani 1 1 d . . . H53A H 0.1188 -0.2076 0.4765 0.054 Uiso 1 1 calc R . . C54 C 0.1166(4) -0.0721(3) 0.4851(3) 0.0471(11) Uani 1 1 d . . . H54A H 0.0340 -0.0675 0.5106 0.057 Uiso 1 1 calc R . . C55 C 0.1865(4) 0.0053(3) 0.4680(3) 0.0395(9) Uani 1 1 d . . . H55A H 0.1512 0.0619 0.4821 0.047 Uiso 1 1 calc R . . C60 C -0.0467(8) 0.2632(6) -0.2236(5) 0.094(3) Uani 1 1 d . . . C61 C 0.0603(7) 0.2385(6) -0.2673(5) 0.082(2) Uani 1 1 d . . . H61A H 0.1192 0.2838 -0.2823 0.099 Uiso 1 1 calc R . . C62 C 0.0917(7) 0.1532(5) -0.2922(5) 0.0762(18) Uani 1 1 d . . . H62A H 0.1677 0.1401 -0.3263 0.091 Uiso 1 1 calc R . . C63 C 0.0055(7) 0.0842(5) -0.2650(5) 0.089(2) Uani 1 1 d . . . H63A H 0.0228 0.0232 -0.2775 0.107 Uiso 1 1 calc R . . C64 C -0.1021(9) 0.1113(7) -0.2204(5) 0.107(3) Uani 1 1 d . . . H64A H -0.1600 0.0660 -0.2033 0.128 Uiso 1 1 calc R . . C65 C -0.1372(5) 0.1972(7) -0.1970(4) 0.0790(14) Uani 1 1 d . . . H65A H -0.2148 0.2114 -0.1661 0.095 Uiso 1 1 calc R . . C66 C -0.0734(10) 0.3544(6) -0.2002(6) 0.133(4) Uani 1 1 d . . . H66A H -0.0618 0.3907 -0.2636 0.200 Uiso 1 1 calc R . . H66B H -0.0165 0.3752 -0.1434 0.200 Uiso 1 1 calc R . . H66C H -0.1602 0.3598 -0.1776 0.200 Uiso 1 1 calc R . . 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 0.02261(13) 0.02414(15) 0.02881(12) 0.00120(13) 0.00341(8) 0.00120(15) Cl1 0.0444(5) 0.0277(5) 0.0462(5) -0.0048(4) 0.0016(4) -0.0013(4) Cl2 0.0391(5) 0.0326(5) 0.0541(6) -0.0115(4) 0.0044(4) -0.0052(4) N1 0.0271(12) 0.0223(13) 0.0313(11) 0.0020(15) 0.0030(9) 0.0005(17) N2 0.0276(15) 0.0226(16) 0.0352(14) 0.0009(12) 0.0071(12) 0.0009(12) O1 0.0247(12) 0.0305(15) 0.0418(13) 0.0107(10) -0.0012(10) -0.0020(10) O2 0.0311(14) 0.0324(15) 0.0516(15) 0.0176(12) -0.0010(11) -0.0001(11) O3 0.0362(14) 0.0443(16) 0.0307(12) 0.0034(11) -0.0017(11) 0.0026(12) O4 0.0277(13) 0.0369(16) 0.0437(13) 0.0029(10) 0.0092(10) 0.0040(10) C1 0.0234(14) 0.028(2) 0.0278(14) 0.0021(14) 0.0035(11) 0.0012(15) C2 0.0246(17) 0.0252(16) 0.0282(16) 0.0014(13) 0.0019(13) -0.0023(14) C3 0.0300(18) 0.0244(19) 0.0339(17) 0.0065(13) 0.0019(14) 0.0024(15) C4 0.0283(18) 0.030(2) 0.0272(16) 0.0042(13) 0.0036(13) -0.0010(15) C5 0.033(2) 0.032(2) 0.045(2) 0.0075(16) -0.0029(16) 0.0031(17) C6 0.047(3) 0.040(3) 0.075(3) 0.005(2) 0.006(2) 0.011(2) C7 0.055(3) 0.053(3) 0.048(2) 0.012(2) -0.009(2) -0.007(2) C8 0.064(3) 0.074(3) 0.0270(18) 0.0006(19) 0.0077(18) 0.004(2) C9 0.035(2) 0.057(3) 0.044(2) 0.0098(18) -0.0070(17) 0.002(2) C10 0.030(2) 0.043(3) 0.059(2) 0.0098(19) -0.0019(18) 0.0047(18) C11 0.039(2) 0.061(3) 0.054(2) -0.004(2) 0.0208(19) 0.011(2) C20 0.0214(16) 0.0263(18) 0.0300(17) 0.0041(14) 0.0037(14) 0.0047(15) C21 0.044(2) 0.038(2) 0.0310(18) 0.0036(16) 0.0035(16) -0.0029(18) C22 0.052(3) 0.040(3) 0.043(2) 0.0170(18) 0.0052(19) -0.003(2) C23 0.046(2) 0.024(2) 0.064(3) 0.0082(18) 0.0066(19) -0.0036(18) C24 0.048(2) 0.028(2) 0.053(2) -0.0068(17) 0.0111(18) -0.0086(18) C25 0.040(2) 0.033(2) 0.0342(18) 0.0009(15) 0.0078(15) -0.0084(18) C30 0.0316(19) 0.0262(19) 0.0289(18) -0.0013(15) 0.0061(16) 0.0034(16) C31 0.036(2) 0.039(2) 0.046(2) -0.0087(17) 0.0059(16) -0.0065(18) C32 0.057(3) 0.040(3) 0.059(3) -0.016(2) 0.014(2) -0.009(2) C33 0.053(3) 0.040(3) 0.065(3) -0.014(2) 0.021(2) 0.003(2) C34 0.037(2) 0.044(2) 0.054(2) -0.0005(19) 0.0169(18) 0.0058(19) C35 0.032(2) 0.039(2) 0.0394(19) 0.0021(16) 0.0095(15) -0.0014(17) C40 0.035(2) 0.039(3) 0.0299(17) 0.0037(16) 0.0065(14) -0.0094(18) C41 0.050(2) 0.052(3) 0.039(2) 0.0066(18) 0.0019(18) -0.010(2) C42 0.062(3) 0.093(4) 0.033(2) 0.007(3) -0.003(2) -0.024(3) C43 0.066(3) 0.092(5) 0.036(2) -0.015(3) 0.0117(18) -0.035(3) C44 0.054(3) 0.053(3) 0.056(3) -0.015(2) 0.019(2) -0.015(2) C45 0.041(2) 0.045(3) 0.0382(19) -0.0006(16) 0.0090(15) -0.0134(19) C50 0.0322(19) 0.032(2) 0.0283(17) 0.0059(14) 0.0010(14) -0.0057(16) C51 0.042(2) 0.033(2) 0.055(2) 0.0035(18) 0.0111(18) -0.0051(18) C52 0.052(3) 0.032(2) 0.057(2) -0.0025(18) 0.006(2) -0.011(2) C53 0.052(3) 0.042(3) 0.042(2) 0.0064(18) -0.0034(19) -0.019(2) C54 0.035(2) 0.058(3) 0.049(2) 0.011(2) 0.0059(18) -0.010(2) C55 0.038(2) 0.034(2) 0.046(2) 0.0101(16) 0.0044(17) 0.0002(17) C60 0.122(6) 0.100(6) 0.057(3) -0.009(3) -0.033(4) 0.046(5) C61 0.069(4) 0.114(6) 0.063(3) -0.013(3) -0.017(3) 0.010(4) C62 0.070(4) 0.084(4) 0.075(4) 0.002(3) -0.006(3) -0.007(4) C63 0.099(5) 0.094(5) 0.072(4) -0.013(3) -0.020(4) 0.035(4) C64 0.139(7) 0.132(8) 0.049(3) 0.015(4) -0.013(4) 0.014(6) C65 0.076(3) 0.106(5) 0.055(3) 0.004(4) -0.001(2) 0.003(5) C66 0.189(10) 0.126(7) 0.083(5) 0.001(5) -0.038(5) 0.057(7) _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 1.737(2) . ? Mo1 N2 1.739(3) . ? Mo1 O3 2.365(2) . ? Mo1 O4 2.380(2) . ? Mo1 Cl2 2.4003(10) . ? Mo1 Cl1 2.4072(10) . ? N1 C1 1.458(4) . ? N2 C4 1.456(4) . ? O1 C2 1.424(4) . ? O1 C5 1.434(4) . ? O2 C5 1.419(4) . ? O2 C3 1.423(4) . ? O3 C9 1.431(5) . ? O3 C8 1.448(5) . ? O4 C10 1.441(5) . ? O4 C11 1.461(5) . ? C1 C20 1.536(5) . ? C1 C30 1.537(5) . ? C1 C2 1.569(4) . ? C2 C3 1.549(5) . ? C3 C4 1.563(5) . ? C4 C50 1.540(5) . ? C4 C40 1.549(5) . ? C5 C7 1.515(6) . ? C5 C6 1.517(6) . ? C9 C10 1.492(6) . ? C20 C25 1.391(5) . ? C20 C21 1.396(5) . ? C21 C22 1.383(6) . ? C22 C23 1.382(6) . ? C23 C24 1.375(6) . ? C24 C25 1.397(6) . ? C30 C31 1.380(5) . ? C30 C35 1.401(5) . ? C31 C32 1.397(6) . ? C32 C33 1.368(7) . ? C33 C34 1.373(6) . ? C34 C35 1.381(5) . ? C40 C45 1.371(6) . ? C40 C41 1.406(6) . ? C41 C42 1.388(7) . ? C42 C43 1.360(9) . ? C43 C44 1.399(8) . ? C44 C45 1.389(6) . ? C50 C51 1.375(6) . ? C50 C55 1.397(5) . ? C51 C52 1.398(6) . ? C52 C53 1.374(6) . ? C53 C54 1.376(7) . ? C54 C55 1.389(6) . ? C60 C61 1.322(10) . ? C60 C65 1.417(11) . ? C60 C66 1.420(11) . ? C61 C62 1.351(9) . ? C62 C63 1.421(10) . ? C63 C64 1.343(10) . ? C64 C65 1.366(11) . ? 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 N2 99.54(13) . . ? N1 Mo1 O3 93.63(11) . . ? N2 Mo1 O3 166.63(11) . . ? N1 Mo1 O4 162.45(11) . . ? N2 Mo1 O4 97.97(11) . . ? O3 Mo1 O4 68.93(9) . . ? N1 Mo1 Cl2 98.61(11) . . ? N2 Mo1 Cl2 95.40(10) . . ? O3 Mo1 Cl2 80.23(7) . . ? O4 Mo1 Cl2 80.79(7) . . ? N1 Mo1 Cl1 95.59(12) . . ? N2 Mo1 Cl1 98.42(10) . . ? O3 Mo1 Cl1 82.50(7) . . ? O4 Mo1 Cl1 80.71(7) . . ? Cl2 Mo1 Cl1 158.24(4) . . ? C1 N1 Mo1 148.7(2) . . ? C4 N2 Mo1 148.7(2) . . ? C2 O1 C5 110.9(3) . . ? C5 O2 C3 111.4(3) . . ? C9 O3 C8 112.3(3) . . ? C9 O3 Mo1 115.6(2) . . ? C8 O3 Mo1 118.6(2) . . ? C10 O4 C11 111.2(3) . . ? C10 O4 Mo1 114.0(2) . . ? C11 O4 Mo1 118.0(2) . . ? N1 C1 C20 105.4(3) . . ? N1 C1 C30 109.9(3) . . ? C20 C1 C30 110.3(3) . . ? N1 C1 C2 105.0(2) . . ? C20 C1 C2 112.7(3) . . ? C30 C1 C2 113.0(3) . . ? O1 C2 C3 105.1(3) . . ? O1 C2 C1 109.9(3) . . ? C3 C2 C1 115.3(3) . . ? O2 C3 C2 104.0(3) . . ? O2 C3 C4 110.0(3) . . ? C2 C3 C4 114.7(3) . . ? N2 C4 C50 106.9(3) . . ? N2 C4 C40 109.7(3) . . ? C50 C4 C40 110.1(3) . . ? N2 C4 C3 105.6(2) . . ? C50 C4 C3 112.1(3) . . ? C40 C4 C3 112.2(3) . . ? O2 C5 O1 106.4(3) . . ? O2 C5 C7 109.1(3) . . ? O1 C5 C7 109.1(3) . . ? O2 C5 C6 109.2(3) . . ? O1 C5 C6 110.3(3) . . ? C7 C5 C6 112.5(4) . . ? O3 C9 C10 107.6(3) . . ? O4 C10 C9 107.0(3) . . ? C25 C20 C21 117.8(3) . . ? C25 C20 C1 123.4(3) . . ? C21 C20 C1 118.8(3) . . ? C22 C21 C20 121.3(4) . . ? C23 C22 C21 120.4(4) . . ? C24 C23 C22 119.2(4) . . ? C23 C24 C25 120.7(4) . . ? C20 C25 C24 120.5(3) . . ? C31 C30 C35 118.6(3) . . ? C31 C30 C1 122.1(3) . . ? C35 C30 C1 119.3(3) . . ? C30 C31 C32 120.2(4) . . ? C33 C32 C31 120.4(4) . . ? C32 C33 C34 120.0(4) . . ? C33 C34 C35 120.2(4) . . ? C34 C35 C30 120.5(4) . . ? C45 C40 C41 119.2(4) . . ? C45 C40 C4 122.1(3) . . ? C41 C40 C4 118.6(4) . . ? C42 C41 C40 119.3(5) . . ? C43 C42 C41 121.3(5) . . ? C42 C43 C44 119.6(4) . . ? C45 C44 C43 119.5(5) . . ? C40 C45 C44 121.0(4) . . ? C51 C50 C55 118.6(3) . . ? C51 C50 C4 123.1(3) . . ? C55 C50 C4 118.2(3) . . ? C50 C51 C52 120.9(4) . . ? C53 C52 C51 120.1(4) . . ? C52 C53 C54 119.5(4) . . ? C53 C54 C55 120.8(4) . . ? C54 C55 C50 120.1(4) . . ? C61 C60 C65 119.6(7) . . ? C61 C60 C66 121.9(10) . . ? C65 C60 C66 118.4(9) . . ? C60 C61 C62 125.2(8) . . ? C61 C62 C63 117.5(7) . . ? C64 C63 C62 115.9(7) . . ? C63 C64 C65 127.5(9) . . ? C64 C65 C60 114.2(7) . . ? 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 N2 Mo1 N1 C1 -19.6(6) . . . . ? O3 Mo1 N1 C1 162.7(6) . . . . ? O4 Mo1 N1 C1 156.7(4) . . . . ? Cl2 Mo1 N1 C1 -116.6(6) . . . . ? Cl1 Mo1 N1 C1 79.9(6) . . . . ? N1 Mo1 N2 C4 -18.2(5) . . . . ? O3 Mo1 N2 C4 151.6(4) . . . . ? O4 Mo1 N2 C4 162.9(5) . . . . ? Cl2 Mo1 N2 C4 81.5(5) . . . . ? Cl1 Mo1 N2 C4 -115.4(5) . . . . ? N1 Mo1 O3 C9 167.8(3) . . . . ? N2 Mo1 O3 C9 -2.2(7) . . . . ? O4 Mo1 O3 C9 -14.1(3) . . . . ? Cl2 Mo1 O3 C9 69.7(3) . . . . ? Cl1 Mo1 O3 C9 -97.0(3) . . . . ? N1 Mo1 O3 C8 30.2(3) . . . . ? N2 Mo1 O3 C8 -139.8(5) . . . . ? O4 Mo1 O3 C8 -151.8(3) . . . . ? Cl2 Mo1 O3 C8 -68.0(3) . . . . ? Cl1 Mo1 O3 C8 125.3(3) . . . . ? N1 Mo1 O4 C10 -11.8(5) . . . . ? N2 Mo1 O4 C10 164.6(3) . . . . ? O3 Mo1 O4 C10 -18.2(2) . . . . ? Cl2 Mo1 O4 C10 -101.2(2) . . . . ? Cl1 Mo1 O4 C10 67.3(2) . . . . ? N1 Mo1 O4 C11 -145.0(5) . . . . ? N2 Mo1 O4 C11 31.4(3) . . . . ? O3 Mo1 O4 C11 -151.4(3) . . . . ? Cl2 Mo1 O4 C11 125.6(3) . . . . ? Cl1 Mo1 O4 C11 -65.9(3) . . . . ? Mo1 N1 C1 C20 -111.9(5) . . . . ? Mo1 N1 C1 C30 129.3(5) . . . . ? Mo1 N1 C1 C2 7.4(7) . . . . ? C5 O1 C2 C3 -5.5(4) . . . . ? C5 O1 C2 C1 -130.2(3) . . . . ? N1 C1 C2 O1 176.7(3) . . . . ? C20 C1 C2 O1 -69.0(3) . . . . ? C30 C1 C2 O1 56.9(4) . . . . ? N1 C1 C2 C3 58.2(4) . . . . ? C20 C1 C2 C3 172.5(3) . . . . ? C30 C1 C2 C3 -61.7(4) . . . . ? C5 O2 C3 C2 -15.4(4) . . . . ? C5 O2 C3 C4 -138.7(3) . . . . ? O1 C2 C3 O2 12.4(3) . . . . ? C1 C2 C3 O2 133.6(3) . . . . ? O1 C2 C3 C4 132.6(3) . . . . ? C1 C2 C3 C4 -106.3(3) . . . . ? Mo1 N2 C4 C50 -113.0(4) . . . . ? Mo1 N2 C4 C40 127.7(4) . . . . ? Mo1 N2 C4 C3 6.5(6) . . . . ? O2 C3 C4 N2 174.2(3) . . . . ? C2 C3 C4 N2 57.4(4) . . . . ? O2 C3 C4 C50 -69.8(4) . . . . ? C2 C3 C4 C50 173.4(3) . . . . ? O2 C3 C4 C40 54.7(4) . . . . ? C2 C3 C4 C40 -62.1(4) . . . . ? C3 O2 C5 O1 12.4(4) . . . . ? C3 O2 C5 C7 130.0(3) . . . . ? C3 O2 C5 C6 -106.6(4) . . . . ? C2 O1 C5 O2 -3.7(4) . . . . ? C2 O1 C5 C7 -121.2(3) . . . . ? C2 O1 C5 C6 114.7(3) . . . . ? C8 O3 C9 C10 -177.0(3) . . . . ? Mo1 O3 C9 C10 42.7(4) . . . . ? C11 O4 C10 C9 -177.6(3) . . . . ? Mo1 O4 C10 C9 46.1(4) . . . . ? O3 C9 C10 O4 -56.9(4) . . . . ? N1 C1 C20 C25 106.3(4) . . . . ? C30 C1 C20 C25 -135.1(4) . . . . ? C2 C1 C20 C25 -7.7(4) . . . . ? N1 C1 C20 C21 -71.2(4) . . . . ? C30 C1 C20 C21 47.4(4) . . . . ? C2 C1 C20 C21 174.8(3) . . . . ? C25 C20 C21 C22 0.1(6) . . . . ? C1 C20 C21 C22 177.7(4) . . . . ? C20 C21 C22 C23 -0.6(7) . . . . ? C21 C22 C23 C24 0.3(7) . . . . ? C22 C23 C24 C25 0.6(7) . . . . ? C21 C20 C25 C24 0.7(6) . . . . ? C1 C20 C25 C24 -176.8(3) . . . . ? C23 C24 C25 C20 -1.1(6) . . . . ? N1 C1 C30 C31 -13.6(5) . . . . ? C20 C1 C30 C31 -129.4(4) . . . . ? C2 C1 C30 C31 103.4(4) . . . . ? N1 C1 C30 C35 164.9(3) . . . . ? C20 C1 C30 C35 49.0(4) . . . . ? C2 C1 C30 C35 -78.2(4) . . . . ? C35 C30 C31 C32 -0.9(6) . . . . ? C1 C30 C31 C32 177.6(4) . . . . ? C30 C31 C32 C33 0.5(7) . . . . ? C31 C32 C33 C34 0.7(7) . . . . ? C32 C33 C34 C35 -1.6(7) . . . . ? C33 C34 C35 C30 1.2(6) . . . . ? C31 C30 C35 C34 0.0(6) . . . . ? C1 C30 C35 C34 -178.4(3) . . . . ? N2 C4 C40 C45 -11.4(5) . . . . ? C50 C4 C40 C45 -128.7(4) . . . . ? C3 C4 C40 C45 105.7(4) . . . . ? N2 C4 C40 C41 166.4(3) . . . . ? C50 C4 C40 C41 49.1(4) . . . . ? C3 C4 C40 C41 -76.5(4) . . . . ? C45 C40 C41 C42 -1.6(6) . . . . ? C4 C40 C41 C42 -179.5(4) . . . . ? C40 C41 C42 C43 1.4(7) . . . . ? C41 C42 C43 C44 -0.5(7) . . . . ? C42 C43 C44 C45 -0.2(7) . . . . ? C41 C40 C45 C44 1.0(6) . . . . ? C4 C40 C45 C44 178.8(4) . . . . ? C43 C44 C45 C40 -0.1(6) . . . . ? N2 C4 C50 C51 126.7(4) . . . . ? C40 C4 C50 C51 -114.2(4) . . . . ? C3 C4 C50 C51 11.4(5) . . . . ? N2 C4 C50 C55 -55.3(4) . . . . ? C40 C4 C50 C55 63.8(4) . . . . ? C3 C4 C50 C55 -170.6(3) . . . . ? C55 C50 C51 C52 -0.2(6) . . . . ? C4 C50 C51 C52 177.8(4) . . . . ? C50 C51 C52 C53 0.9(6) . . . . ? C51 C52 C53 C54 -1.0(6) . . . . ? C52 C53 C54 C55 0.4(6) . . . . ? C53 C54 C55 C50 0.3(6) . . . . ? C51 C50 C55 C54 -0.4(5) . . . . ? C4 C50 C55 C54 -178.5(3) . . . . ? C65 C60 C61 C62 1.5(10) . . . . ? C66 C60 C61 C62 -179.6(7) . . . . ? C60 C61 C62 C63 -2.9(11) . . . . ? C61 C62 C63 C64 2.5(9) . . . . ? C62 C63 C64 C65 -0.9(10) . . . . ? C63 C64 C65 C60 -0.4(9) . . . . ? C61 C60 C65 C64 0.2(8) . . . . ? C66 C60 C65 C64 -178.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.661 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.054