# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1727 data_global #================================================================= # SUBMISSION DETAILS _publ_contact_author ; Dr. Michael Ward School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287655' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the crystal structures in the paper 'Complexes containing redox-actove fluorenone-based ligands....' by A. Behrendt, et al, submitted to Dalton Transactions for publication. ; #================================================================= data_andys _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C62.50 H73 B2 Cl13 Mo2 N16 O3' _chemical_formula_weight 1770.72 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.401(2) _cell_length_b 17.730(4) _cell_length_c 25.841(7) _cell_angle_alpha 105.48(2) _cell_angle_beta 93.23(2) _cell_angle_gamma 100.63(2) _cell_volume 4054.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method ? _exptl_crystal_F_000 1798 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.93 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27335 _diffrn_reflns_av_R_equivalents 0.1575 _diffrn_reflns_av_sigmaI/netI 0.2333 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 22.50 _reflns_number_total 10527 _reflns_number_observed 4340 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 73 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1533P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10454 _refine_ls_number_parameters 919 _refine_ls_number_restraints 134 _refine_ls_R_factor_all 0.2395 _refine_ls_R_factor_obs 0.1048 _refine_ls_wR_factor_all 0.3201 _refine_ls_wR_factor_obs 0.2433 _refine_ls_goodness_of_fit_all 1.002 _refine_ls_goodness_of_fit_obs 1.251 _refine_ls_restrained_S_all 1.020 _refine_ls_restrained_S_obs 1.259 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.88843(15) 0.12749(10) 0.40316(6) 0.0491(5) Uani 1 d . . Cl1 Cl 0.7085(6) 0.1634(4) 0.3490(2) 0.104(2) Uani 1 d . . N1 N 0.8013(27) 0.0170(12) 0.3764(8) 0.056(7) Uani 1 d . . O1 O 0.7697(24) -0.0349(13) 0.3598(9) 0.100(8) Uani 1 d . . B1 B 1.0084(16) 0.2369(12) 0.5245(7) 0.040(5) Uani 1 d . . H1 H 1.0450(16) 0.2695(12) 0.5625(7) 0.048 Uiso 1 calc R . Mo2 Mo 2.63601(15) -0.35377(9) -0.17081(6) 0.0444(5) Uani 1 d . . Cl2 Cl 2.8411(8) -0.2856(5) -0.1007(3) 0.138(3) Uani 1 d . . N2 N 2.7094(35) -0.2915(17) -0.2261(20) 0.097(13) Uani 1 d . . O2 O 2.7475(33) -0.2621(18) -0.2317(13) 0.127(12) Uani 1 d . . B2 B 2.4917(28) -0.5423(14) -0.2030(9) 0.070(7) Uani 1 d . . H2 H 2.4502(28) -0.6011(14) -0.2135(9) 0.084 Uiso 1 calc R . N111 N 0.8424(13) 0.2006(8) 0.5221(5) 0.044(4) Uani 1 d . . N112 N 0.7694(13) 0.1516(8) 0.4729(5) 0.045(4) Uani 1 d . . C113 C 0.6302(19) 0.1255(13) 0.4815(7) 0.070(6) Uani 1 d . . C114 C 0.6136(18) 0.1567(12) 0.5354(8) 0.073(6) Uani 1 d . . H11A H 0.5267(18) 0.1481(12) 0.5520(8) 0.088 Uiso 1 calc R . C115 C 0.7466(20) 0.2025(11) 0.5604(7) 0.059(5) Uani 1 d . . C116 C 0.7970(19) 0.2525(12) 0.6183(6) 0.074(6) Uani 1 d . . H11B H 0.9006(19) 0.2772(12) 0.6214(6) 0.111 Uiso 1 calc R . H11C H 0.7826(19) 0.2182(12) 0.6425(6) 0.111 Uiso 1 calc R . H11D H 0.7404(19) 0.2944(12) 0.6283(6) 0.111 Uiso 1 calc R . C117 C 0.5214(18) 0.0702(13) 0.4374(7) 0.091(8) Uani 1 d . . H11E H 0.5661(18) 0.0590(13) 0.4036(7) 0.137 Uiso 1 calc R . H11F H 0.4383(18) 0.0951(13) 0.4331(7) 0.137 Uiso 1 calc R . H11G H 0.4879(18) 0.0201(13) 0.4465(7) 0.137 Uiso 1 calc R . N121 N 1.0327(14) 0.2903(10) 0.4879(6) 0.049(4) Uani 1 d . . N122 N 0.9967(14) 0.2547(10) 0.4322(6) 0.058(4) Uani 1 d . . C123 C 1.0321(20) 0.3166(14) 0.4099(8) 0.058(5) Uani 1 d . . C124 C 1.0793(21) 0.3846(13) 0.4499(9) 0.069(6) Uani 1 d . . H12A H 1.1090(21) 0.4361(13) 0.4449(9) 0.083 Uiso 1 calc R . C125 C 1.0784(20) 0.3688(13) 0.4982(7) 0.059(5) Uani 1 d . . C126 C 1.1275(24) 0.4248(12) 0.5549(7) 0.092(7) Uani 1 d . . H12B H 1.1123(24) 0.3945(12) 0.5814(7) 0.138 Uiso 1 calc R . H12C H 1.0708(24) 0.4669(12) 0.5620(7) 0.138 Uiso 1 calc R . H12D H 1.2311(24) 0.4491(12) 0.5576(7) 0.138 Uiso 1 calc R . C127 C 1.0161(21) 0.3061(12) 0.3511(7) 0.078(6) Uani 1 d . . H12E H 0.9791(21) 0.2494(12) 0.3320(7) 0.117 Uiso 1 calc R . H12F H 1.1110(21) 0.3242(12) 0.3397(7) 0.117 Uiso 1 calc R . H12G H 0.9476(21) 0.3377(12) 0.3425(7) 0.117 Uiso 1 calc R . N131 N 1.0857(13) 0.1679(8) 0.5100(5) 0.041(3) Uani 1 d . . N132 N 1.0518(12) 0.1104(8) 0.4608(5) 0.040(3) Uani 1 d . . C133 C 1.1247(16) 0.0529(10) 0.4622(7) 0.043(4) Uani 1 d . . C134 C 1.2080(16) 0.0712(10) 0.5120(6) 0.041(4) Uani 1 d . . H13A H 1.2691(16) 0.0400(10) 0.5231(6) 0.050 Uiso 1 calc R . C135 C 1.1840(16) 0.1434(11) 0.5418(7) 0.046(4) Uani 1 d . . C136 C 1.2439(18) 0.1930(11) 0.5962(6) 0.059(5) Uani 1 d . . H13B H 1.2029(18) 0.2413(11) 0.6050(6) 0.089 Uiso 1 calc R . H13C H 1.3501(18) 0.2083(11) 0.5979(6) 0.089 Uiso 1 calc R . H13D H 1.2190(18) 0.1628(11) 0.6223(6) 0.089 Uiso 1 calc R . C137 C 1.1160(16) -0.0192(9) 0.4130(6) 0.050(5) Uani 1 d . . H13E H 1.0481(16) -0.0159(9) 0.3839(6) 0.075 Uiso 1 calc R . H13F H 1.0815(16) -0.0686(9) 0.4229(6) 0.075 Uiso 1 calc R . H13G H 1.2128(16) -0.0193(9) 0.4008(6) 0.075 Uiso 1 calc R . N211 N 2.4765(17) -0.5051(11) -0.1426(6) 0.063(4) Uani 1 d . . N212 N 2.5380(15) -0.4275(9) -0.1191(5) 0.052(4) Uani 1 d . . C213 C 2.5111(20) -0.4119(13) -0.0665(7) 0.055(5) Uani 1 d . . C214 C 2.4310(27) -0.4819(15) -0.0596(8) 0.085(7) Uani 1 d . . H21A H 2.3983(27) -0.4884(15) -0.0266(8) 0.102 Uiso 1 calc R . C215 C 2.4076(23) -0.5388(14) -0.1071(9) 0.071(6) Uani 1 d . . C216 C 2.3240(28) -0.6234(16) -0.1244(9) 0.118(9) Uani 1 d . . H21B H 2.3312(28) -0.6471(16) -0.1628(9) 0.177 Uiso 1 calc R . H21C H 2.2215(28) -0.6243(16) -0.1187(9) 0.177 Uiso 1 calc R . H21D H 2.3643(28) -0.6541(16) -0.1030(9) 0.177 Uiso 1 calc R . C217 C 2.5666(23) -0.3319(12) -0.0266(6) 0.082(7) Uani 1 d . . H21E H 2.6195(23) -0.2952(12) -0.0447(6) 0.124 Uiso 1 calc R . H21F H 2.6323(23) -0.3374(12) 0.0024(6) 0.124 Uiso 1 calc R . H21G H 2.4844(23) -0.3106(12) -0.0112(6) 0.124 Uiso 1 calc R . N221 N 2.4113(14) -0.5035(9) -0.2370(5) 0.043(3) Uani 1 d . . N222 N 2.4534(14) -0.4229(8) -0.2313(5) 0.041(3) Uani 1 d . . C223 C 2.3636(20) -0.4055(12) -0.2686(7) 0.060(6) Uani 1 d . . C224 C 2.2692(20) -0.4777(14) -0.2974(7) 0.072(6) Uani 1 d . . H22A H 2.1956(20) -0.4844(14) -0.3259(7) 0.086 Uiso 1 calc R . C225 C 2.3023(24) -0.5355(12) -0.2772(8) 0.064(6) Uani 1 d . . C226 C 2.2285(24) -0.6225(12) -0.2951(9) 0.107(8) Uani 1 d . . H22B H 2.2741(24) -0.6515(12) -0.2736(9) 0.160 Uiso 1 calc R . H22C H 2.2383(24) -0.6450(12) -0.3334(9) 0.160 Uiso 1 calc R . H22D H 2.1250(24) -0.6278(12) -0.2899(9) 0.160 Uiso 1 calc R . C227 C 2.3829(23) -0.3221(12) -0.2745(7) 0.084(7) Uani 1 d . . H22E H 2.4597(23) -0.2862(12) -0.2471(7) 0.126 Uiso 1 calc R . H22F H 2.2913(23) -0.3035(12) -0.2696(7) 0.126 Uiso 1 calc R . H22G H 2.4101(23) -0.3224(12) -0.3106(7) 0.126 Uiso 1 calc R . N231 N 2.6570(19) -0.5274(10) -0.2118(6) 0.063(5) Uani 1 d . . N232 N 2.7354(14) -0.4525(10) -0.2037(5) 0.051(4) Uani 1 d . . C233 C 2.8705(23) -0.4594(13) -0.2167(8) 0.074(6) Uani 1 d . . C234 C 2.8765(27) -0.5385(16) -0.2306(9) 0.090(8) Uani 1 d . . H23A H 2.9602(27) -0.5598(16) -0.2399(9) 0.108 Uiso 1 calc R . C235 C 2.7404(33) -0.5824(14) -0.2287(7) 0.083(8) Uani 1 d . . C236 C 2.6791(28) -0.6730(14) -0.2403(8) 0.112(9) Uani 1 d . . H23B H 2.5758(28) -0.6820(14) -0.2346(8) 0.168 Uiso 1 calc R . H23C H 2.7329(28) -0.6943(14) -0.2158(8) 0.168 Uiso 1 calc R . H23D H 2.6896(28) -0.7004(14) -0.2778(8) 0.168 Uiso 1 calc R . C237 C 2.9854(19) -0.3886(14) -0.2143(8) 0.092(8) Uani 1 d . . H23E H 2.9460(19) -0.3400(14) -0.2028(8) 0.138 Uiso 1 calc R . H23F H 3.0185(19) -0.3932(14) -0.2501(8) 0.138 Uiso 1 calc R . H23G H 3.0676(19) -0.3856(14) -0.1883(8) 0.138 Uiso 1 calc R . N311 N 1.0384(13) 0.1129(8) 0.3414(6) 0.048(4) Uani 1 d . . C312 C 1.1813(17) 0.1454(10) 0.3534(6) 0.051(5) Uani 1 d . . H31A H 1.2154(17) 0.1789(10) 0.3889(6) 0.061 Uiso 1 calc R . C313 C 1.2829(17) 0.1318(11) 0.3154(7) 0.052(5) Uani 1 d . . H31B H 1.3830(17) 0.1566(11) 0.3249(7) 0.062 Uiso 1 calc R . C314 C 1.2336(21) 0.0815(12) 0.2640(7) 0.063(6) Uani 1 d . . C315 C 1.0886(19) 0.0510(12) 0.2510(7) 0.067(6) Uani 1 d . . H31C H 1.0517(19) 0.0185(12) 0.2155(7) 0.080 Uiso 1 calc R . C316 C 0.9961(20) 0.0678(12) 0.2898(7) 0.063(6) Uani 1 d . . H31D H 0.8950(20) 0.0462(12) 0.2796(7) 0.076 Uiso 1 calc R . C317 C 1.3363(22) 0.0620(12) 0.2220(7) 0.063(6) Uani 1 d . . H31E H 1.3006(22) 0.0204(12) 0.1896(7) 0.076 Uiso 1 calc R . C318 C 1.4711(21) 0.0994(11) 0.2278(7) 0.056(5) Uani 1 d . . H31F H 1.4999(21) 0.1437(11) 0.2591(7) 0.068 Uiso 1 calc R . C411 C 1.5879(23) 0.0819(12) 0.1916(7) 0.057(6) Uani 1 d . . C412 C 1.5638(19) 0.0133(12) 0.1481(7) 0.064(6) Uani 1 d . . H41A H 1.4701(19) -0.0208(12) 0.1381(7) 0.076 Uiso 1 calc R . C413 C 1.6817(19) -0.0043(11) 0.1191(7) 0.059(5) Uani 1 d . . C414 C 1.8185(18) 0.0480(11) 0.1348(6) 0.044(4) Uani 1 d . . C415 C 1.8400(19) 0.1164(10) 0.1773(7) 0.054(5) Uani 1 d . . H41B H 1.9326(19) 0.1517(10) 0.1872(7) 0.065 Uiso 1 calc R . C416 C 1.7218(23) 0.1322(12) 0.2052(8) 0.064(6) Uani 1 d . . H41C H 1.7343(23) 0.1793(12) 0.2345(8) 0.077 Uiso 1 calc R . C421 C 1.6949(21) -0.0714(15) 0.0730(7) 0.085(8) Uani 1 d . . O422 O 1.5968(15) -0.1272(11) 0.0501(6) 0.113(6) Uani 1 d . . C511 C 2.0706(19) -0.0815(12) 0.0263(7) 0.054(5) Uani 1 d . . C512 C 1.9199(19) -0.1064(11) 0.0258(6) 0.056(5) Uani 1 d . . H51A H 1.8684(19) -0.1541(11) 0.0002(6) 0.067 Uiso 1 calc R . C513 C 1.8463(17) -0.0602(11) 0.0634(7) 0.054(5) Uani 1 d . . C514 C 1.9237(17) 0.0121(10) 0.0985(7) 0.044(4) Uani 1 d . . C515 C 2.0707(19) 0.0383(11) 0.0999(6) 0.059(5) Uani 1 d . . H51B H 2.1224(19) 0.0864(11) 0.1250(6) 0.071 Uiso 1 calc R . C516 C 2.1412(19) -0.0112(12) 0.0611(7) 0.063(5) Uani 1 d . . H51E H 2.2424(19) 0.0059(12) 0.0597(7) 0.076 Uiso 1 calc R . C517 C 2.1443(22) -0.1318(12) -0.0158(8) 0.077(6) Uani 1 d . . H51F H 2.0851(22) -0.1800(12) -0.0384(8) 0.093 Uiso 1 calc R . C518 C 2.2741(22) -0.1177(12) -0.0243(7) 0.072(6) Uani 1 d . . H51G H 2.3333(22) -0.0690(12) -0.0025(7) 0.087 Uiso 1 calc R . N611 N 2.5023(13) -0.2690(9) -0.1324(5) 0.045(4) Uani 1 d . . C612 C 2.3617(17) -0.2957(10) -0.1269(5) 0.043(4) Uani 1 d . . H61A H 2.3164(17) -0.3494(10) -0.1454(5) 0.052 Uiso 1 calc R . C613 C 2.2813(18) -0.2473(11) -0.0951(6) 0.054(5) Uani 1 d . . H61B H 2.1811(18) -0.2672(11) -0.0937(6) 0.065 Uiso 1 calc R . C614 C 2.3460(20) -0.1700(10) -0.0655(6) 0.048(5) Uani 1 d . . C615 C 2.4919(19) -0.1429(11) -0.0719(7) 0.060(5) Uani 1 d . . H61C H 2.5412(19) -0.0901(11) -0.0527(7) 0.072 Uiso 1 calc R . C616 C 2.5631(19) -0.1929(11) -0.1060(7) 0.065(6) Uani 1 d . . H61D H 2.6604(19) -0.1726(11) -0.1111(7) 0.078 Uiso 1 calc R . C10 C 0.8419(54) -0.1603(31) 0.2411(11) 0.360(43) Uani 1 d D . Cl11 Cl 0.8523(17) -0.1472(7) 0.1794(5) 0.267(7) Uani 1 d DU . Cl12 Cl 0.9735(15) -0.2020(9) 0.2589(5) 0.258(6) Uani 1 d DU . C20 C 1.4059(22) 0.6973(14) 0.5352(14) 0.155(12) Uani 1 d D . Cl21 Cl 1.3329(22) 0.6062(10) 0.5347(10) 0.432(16) Uani 1 d DU . Cl22 Cl 1.5845(9) 0.7106(7) 0.5257(4) 0.225(6) Uani 1 d DU . C30 C 1.3567(22) 0.5001(14) 0.3494(9) 0.113(9) Uani 1 d D . Cl31 Cl 1.4612(14) 0.6001(8) 0.3791(6) 0.277(7) Uani 1 d DU . Cl32 Cl 1.1897(18) 0.5128(8) 0.3590(5) 0.197(6) Uani 0.75 d PDU 1 Cl33 Cl 1.4283(31) 0.4445(24) 0.3872(13) 0.155(13) Uani 0.25 d PU 2 C40 C 1.4824(31) -0.0650(16) 0.2833(9) 0.182(17) Uani 1 d D . Cl41 Cl 1.4825(25) -0.1252(8) 0.2237(7) 0.358(12) Uani 1 d DU . Cl42 Cl 1.3597(14) -0.1051(8) 0.3146(7) 0.337(12) Uani 1 d DU . C50 C 2.0986(23) -0.5456(16) 0.0707(15) 0.182(17) Uani 1 d DU . Cl51 Cl 1.9174(9) -0.5430(6) 0.0854(4) 0.180(4) Uani 1 d DU . Cl52 Cl 2.0905(27) -0.5979(27) 0.0020(12) 0.454(32) Uani 0.50 d PDU 1 Cl53 Cl 2.1861(31) -0.4457(18) 0.0790(10) 0.266(13) Uani 0.50 d PDU 2 Cl54 Cl 1.6793(22) -0.6636(13) -0.0873(8) 0.189(8) Uani 0.50 d PDU 1 C55 C 1.7157(35) -0.7451(19) -0.0660(14) 0.067(12) Uani 0.50 d PDU 1 Cl56 Cl 1.8319(27) -0.7864(14) -0.1080(9) 0.226(11) Uani 0.50 d PDU 1 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 0.0327(9) 0.0795(14) 0.0334(9) 0.0073(8) 0.0103(7) 0.0179(9) Cl1 0.088(4) 0.146(6) 0.077(4) 0.023(4) 0.032(3) 0.030(4) N1 0.069(15) 0.090(17) 0.023(11) 0.018(11) 0.032(10) 0.043(14) O1 0.059(11) 0.181(24) 0.074(16) 0.047(16) 0.010(10) 0.040(17) B1 0.010(9) 0.064(14) 0.034(11) -0.002(10) -0.007(8) 0.007(9) Mo2 0.0346(9) 0.0575(11) 0.0372(9) -0.0018(8) 0.0103(7) 0.0202(8) Cl2 0.124(6) 0.159(7) 0.142(6) 0.020(5) 0.054(5) 0.078(5) N2 0.024(12) 0.025(11) 0.225(36) 0.014(13) 0.018(14) -0.001(9) O2 0.086(22) 0.189(34) 0.098(16) -0.006(21) 0.034(15) 0.067(21) B2 0.104(21) 0.052(16) 0.048(15) 0.003(12) 0.007(13) 0.016(15) N111 0.048(8) 0.071(10) 0.017(7) 0.009(7) 0.016(6) 0.027(8) N112 0.031(8) 0.073(10) 0.036(9) 0.016(8) 0.009(6) 0.020(7) C113 0.038(12) 0.118(18) 0.047(13) 0.012(12) 0.010(9) 0.015(11) C114 0.018(10) 0.123(18) 0.064(14) 0.006(12) 0.005(9) 0.007(11) C115 0.057(13) 0.069(14) 0.063(13) 0.015(11) 0.031(10) 0.038(11) C116 0.070(13) 0.120(18) 0.030(11) 0.013(11) 0.026(9) 0.024(12) C117 0.038(11) 0.153(21) 0.055(13) -0.014(13) 0.018(10) 0.009(13) N121 0.055(9) 0.058(11) 0.044(10) 0.028(9) 0.005(7) 0.018(8) N122 0.053(9) 0.098(13) 0.033(9) 0.020(9) 0.009(7) 0.033(9) C123 0.065(13) 0.072(16) 0.046(13) 0.027(13) 0.012(10) 0.019(11) C124 0.089(15) 0.077(17) 0.068(15) 0.048(14) 0.017(12) 0.038(13) C125 0.081(14) 0.063(15) 0.047(13) 0.023(11) 0.008(10) 0.036(12) C126 0.120(19) 0.078(16) 0.047(13) -0.011(11) -0.011(12) -0.006(14) C127 0.087(15) 0.093(17) 0.060(14) 0.020(12) 0.021(11) 0.034(13) N131 0.037(8) 0.057(9) 0.030(8) 0.002(7) 0.018(6) 0.024(7) N132 0.032(7) 0.062(10) 0.035(8) 0.017(7) 0.017(6) 0.023(7) C133 0.029(9) 0.049(12) 0.056(12) 0.022(9) 0.014(8) 0.008(9) C134 0.036(10) 0.054(12) 0.035(10) 0.006(9) 0.003(8) 0.022(9) C135 0.023(9) 0.071(14) 0.044(11) 0.020(10) 0.003(8) 0.004(9) C136 0.057(11) 0.099(15) 0.032(11) 0.028(10) -0.009(8) 0.033(11) C137 0.037(10) 0.049(11) 0.050(11) -0.007(9) 0.008(8) 0.007(8) N211 0.086(12) 0.074(13) 0.044(10) 0.030(10) 0.027(9) 0.028(10) N212 0.056(9) 0.059(11) 0.042(10) 0.004(8) 0.018(7) 0.026(8) C213 0.064(13) 0.074(15) 0.027(11) 0.003(11) 0.005(9) 0.028(11) C214 0.133(21) 0.097(19) 0.046(15) 0.033(15) 0.022(13) 0.053(17) C215 0.082(15) 0.081(17) 0.053(15) 0.016(14) 0.002(12) 0.027(13) C216 0.154(24) 0.129(24) 0.078(18) 0.061(17) 0.035(16) -0.008(20) C217 0.127(18) 0.112(19) 0.016(10) 0.016(11) 0.026(11) 0.041(15) N221 0.051(9) 0.050(11) 0.032(9) 0.015(7) 0.000(7) 0.019(8) N222 0.055(9) 0.033(9) 0.037(8) 0.000(7) 0.014(7) 0.028(7) C223 0.069(13) 0.077(16) 0.039(11) 0.003(11) 0.005(10) 0.051(13) C224 0.057(13) 0.090(18) 0.038(12) -0.021(13) -0.011(9) 0.004(13) C225 0.096(17) 0.047(14) 0.048(13) 0.004(11) 0.014(12) 0.025(13) C226 0.115(19) 0.078(18) 0.083(17) -0.042(13) 0.011(14) 0.006(15) C227 0.122(19) 0.075(16) 0.056(13) 0.003(11) -0.020(12) 0.054(14) N231 0.093(13) 0.059(12) 0.055(10) 0.019(9) 0.014(9) 0.053(11) N232 0.035(9) 0.066(12) 0.049(9) 0.006(8) 0.011(7) 0.020(8) C233 0.059(15) 0.061(15) 0.093(16) -0.011(12) 0.010(12) 0.037(12) C234 0.079(17) 0.102(21) 0.083(17) -0.006(14) 0.016(13) 0.050(16) C235 0.152(24) 0.061(17) 0.046(13) 0.004(11) -0.010(14) 0.069(18) C236 0.182(26) 0.108(21) 0.072(16) 0.023(14) 0.052(16) 0.085(19) C237 0.036(12) 0.152(23) 0.060(14) -0.027(14) -0.005(10) 0.036(14) N311 0.026(8) 0.061(10) 0.053(10) 0.005(8) 0.012(7) 0.012(7) C312 0.040(11) 0.083(14) 0.038(10) 0.022(9) 0.013(8) 0.025(10) C313 0.038(10) 0.082(14) 0.040(12) 0.022(10) 0.005(8) 0.018(10) C314 0.068(14) 0.119(17) 0.034(11) 0.045(12) 0.029(10) 0.061(13) C315 0.045(12) 0.109(17) 0.044(11) -0.003(11) 0.004(9) 0.049(12) C316 0.059(12) 0.100(16) 0.045(12) 0.020(11) 0.013(10) 0.050(12) C317 0.068(14) 0.096(16) 0.031(11) 0.011(10) -0.002(10) 0.045(13) C318 0.060(13) 0.072(14) 0.051(12) 0.017(10) 0.022(10) 0.043(12) C411 0.086(15) 0.074(15) 0.043(12) 0.029(11) 0.037(11) 0.066(13) C412 0.052(11) 0.119(17) 0.047(11) 0.033(12) 0.026(9) 0.063(12) C413 0.044(12) 0.078(14) 0.044(11) -0.005(10) 0.000(9) 0.022(11) C414 0.052(11) 0.067(13) 0.026(9) 0.017(9) 0.021(8) 0.036(10) C415 0.058(12) 0.058(13) 0.058(12) 0.023(10) 0.022(10) 0.029(10) C416 0.084(15) 0.058(14) 0.067(14) 0.034(11) 0.046(12) 0.023(12) C421 0.043(13) 0.151(22) 0.042(13) -0.022(13) -0.017(10) 0.054(14) O422 0.052(9) 0.193(17) 0.060(10) -0.036(10) 0.000(8) 0.048(10) C511 0.047(12) 0.075(15) 0.043(11) 0.009(10) 0.019(9) 0.030(11) C512 0.057(12) 0.077(14) 0.036(10) 0.006(9) -0.003(9) 0.033(11) C513 0.036(10) 0.071(14) 0.053(12) 0.005(10) 0.016(9) 0.023(10) C514 0.036(10) 0.049(12) 0.063(12) 0.023(10) 0.013(9) 0.032(9) C515 0.057(13) 0.079(14) 0.041(11) 0.006(10) 0.008(9) 0.030(11) C516 0.047(11) 0.091(16) 0.068(14) 0.028(12) 0.040(10) 0.034(12) C517 0.066(14) 0.097(17) 0.082(15) 0.022(12) 0.035(12) 0.050(13) C518 0.075(15) 0.088(16) 0.058(13) 0.008(11) 0.036(11) 0.038(12) N611 0.032(8) 0.065(11) 0.038(8) 0.004(8) 0.013(6) 0.022(8) C612 0.041(10) 0.064(12) 0.020(9) 0.002(8) -0.005(7) 0.017(9) C613 0.045(11) 0.084(15) 0.043(11) 0.016(11) 0.018(9) 0.034(11) C614 0.073(13) 0.046(12) 0.028(10) -0.004(9) 0.010(9) 0.037(10) C615 0.055(12) 0.063(13) 0.067(13) 0.015(10) 0.036(10) 0.020(10) C616 0.056(12) 0.049(13) 0.066(13) -0.022(11) 0.019(10) 0.009(10) C10 0.623(108) 0.414(75) 0.121(34) 0.017(40) -0.001(47) 0.403(82) Cl11 0.387(19) 0.219(12) 0.187(11) 0.104(10) -0.077(12) 0.003(12) Cl12 0.276(14) 0.325(17) 0.227(13) 0.117(12) 0.039(11) 0.138(13) C20 0.121(24) 0.113(24) 0.257(39) 0.071(25) 0.028(24) 0.062(20) Cl21 0.421(26) 0.220(16) 0.699(41) 0.165(21) 0.326(28) 0.046(16) Cl22 0.102(6) 0.287(13) 0.215(11) -0.042(9) -0.012(6) 0.036(7) C30 0.097(19) 0.159(28) 0.092(19) 0.039(18) 0.033(15) 0.036(19) Cl31 0.209(12) 0.248(14) 0.333(18) -0.008(12) 0.103(12) 0.057(11) Cl32 0.250(16) 0.175(12) 0.154(11) 0.048(9) 0.032(11) 0.005(11) Cl33 0.107(21) 0.270(41) 0.146(26) 0.124(28) 0.072(20) 0.074(24) C40 0.248(42) 0.118(27) 0.171(34) 0.072(25) -0.099(32) 0.004(27) Cl41 0.641(34) 0.183(13) 0.282(18) 0.107(12) 0.203(21) 0.060(17) Cl42 0.261(14) 0.191(11) 0.423(21) -0.106(12) 0.236(15) -0.066(10) C50 0.061(17) 0.106(23) 0.386(54) 0.085(29) 0.057(25) 0.002(16) Cl51 0.133(7) 0.247(11) 0.202(10) 0.114(8) 0.027(6) 0.067(7) Cl52 0.282(28) 1.087(91) 0.376(36) 0.576(53) 0.265(29) 0.482(47) Cl53 0.277(31) 0.388(43) 0.160(21) 0.101(25) 0.018(20) 0.106(31) Cl54 0.185(18) 0.249(23) 0.159(17) 0.084(16) 0.077(14) 0.052(17) C55 0.061(23) 0.098(30) 0.106(30) 0.093(25) 0.054(21) 0.062(22) Cl56 0.311(27) 0.273(24) 0.220(21) 0.165(19) 0.154(20) 0.200(22) _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 1.90(2) . ? Mo1 N112 2.163(12) . ? Mo1 N311 2.184(12) . ? Mo1 N132 2.195(12) . ? Mo1 N122 2.20(2) . ? Mo1 Cl1 2.415(6) . ? N1 O1 0.89(2) . ? B1 N121 1.51(2) . ? B1 N131 1.51(2) . ? B1 N111 1.57(2) . ? Mo2 N2 2.10(4) . ? Mo2 N232 2.135(13) . ? Mo2 N222 2.189(13) . ? Mo2 N611 2.206(11) . ? Mo2 N212 2.230(15) . ? Mo2 Cl2 2.457(8) . ? N2 O2 0.63(5) . ? B2 N221 1.50(3) . ? B2 N211 1.55(2) . ? B2 N231 1.57(3) . ? N111 C115 1.37(2) . ? N111 N112 1.39(2) . ? N112 C113 1.36(2) . ? C113 C114 1.39(2) . ? C113 C117 1.48(2) . ? C114 C115 1.38(2) . ? C115 C116 1.52(2) . ? N121 C125 1.33(2) . ? N121 N122 1.40(2) . ? N122 C123 1.37(2) . ? C123 C124 1.34(2) . ? C123 C127 1.48(2) . ? C124 C125 1.35(2) . ? C125 C126 1.52(2) . ? N131 N132 1.38(2) . ? N131 C135 1.41(2) . ? N132 C133 1.34(2) . ? C133 C134 1.39(2) . ? C133 C137 1.53(2) . ? C134 C135 1.37(2) . ? C135 C136 1.46(2) . ? N211 N212 1.35(2) . ? N211 C215 1.36(2) . ? N212 C213 1.36(2) . ? C213 C214 1.39(3) . ? C213 C217 1.50(2) . ? C214 C215 1.34(3) . ? C215 C216 1.49(3) . ? N221 C225 1.34(2) . ? N221 N222 1.38(2) . ? N222 C223 1.38(2) . ? C223 C224 1.41(2) . ? C223 C227 1.50(2) . ? C224 C225 1.34(3) . ? C225 C226 1.50(3) . ? N231 N232 1.35(2) . ? N231 C235 1.36(2) . ? N232 C233 1.35(2) . ? C233 C234 1.37(3) . ? C233 C237 1.48(3) . ? C234 C235 1.38(3) . ? C235 C236 1.55(3) . ? N311 C312 1.34(2) . ? N311 C316 1.35(2) . ? C312 C313 1.41(2) . ? C313 C314 1.39(2) . ? C314 C315 1.36(2) . ? C314 C317 1.51(2) . ? C315 C316 1.37(2) . ? C317 C318 1.30(2) . ? C318 C411 1.50(2) . ? C411 C416 1.37(2) . ? C411 C412 1.39(2) . ? C412 C413 1.41(2) . ? C413 C414 1.41(2) . ? C413 C421 1.47(2) . ? C414 C415 1.37(2) . ? C414 C514 1.51(2) . ? C415 C416 1.39(2) . ? C421 O422 1.21(2) . ? C421 C513 1.45(2) . ? C511 C516 1.35(2) . ? C511 C512 1.40(2) . ? C511 C517 1.50(2) . ? C512 C513 1.40(2) . ? C513 C514 1.40(2) . ? C514 C515 1.37(2) . ? C515 C516 1.43(2) . ? C517 C518 1.24(2) . ? C518 C614 1.49(2) . ? N611 C616 1.34(2) . ? N611 C612 1.35(2) . ? C612 C613 1.38(2) . ? C613 C614 1.38(2) . ? C614 C615 1.40(2) . ? C615 C616 1.37(2) . ? C10 Cl12 1.66(2) . ? C10 Cl11 1.67(2) . ? C20 Cl21 1.63(2) . ? C20 Cl22 1.69(2) . ? C30 Cl32 1.65(2) . ? C30 Cl33 1.75(4) . ? C30 Cl31 1.80(2) . ? C40 Cl42 1.61(2) . ? C40 Cl41 1.62(2) . ? C50 Cl52 1.76(2) . ? C50 Cl53 1.76(2) . ? C50 Cl51 1.77(2) . ? Cl54 C55 1.76(2) . ? C55 Cl56 1.71(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 N1 Mo1 N112 96.2(7) . . ? N1 Mo1 N311 89.7(7) . . ? N112 Mo1 N311 171.2(5) . . ? N1 Mo1 N132 94.6(8) . . ? N112 Mo1 N132 83.2(4) . . ? N311 Mo1 N132 89.8(5) . . ? N1 Mo1 N122 177.7(7) . . ? N112 Mo1 N122 86.0(5) . . ? N311 Mo1 N122 88.1(5) . . ? N132 Mo1 N122 84.9(5) . . ? N1 Mo1 Cl1 91.9(8) . . ? N112 Mo1 Cl1 91.7(3) . . ? N311 Mo1 Cl1 94.7(4) . . ? N132 Mo1 Cl1 172.1(4) . . ? N122 Mo1 Cl1 88.7(4) . . ? O1 N1 Mo1 171.0(32) . . ? N121 B1 N131 112.8(13) . . ? N121 B1 N111 110.7(12) . . ? N131 B1 N111 107.4(13) . . ? N2 Mo2 N232 94.5(10) . . ? N2 Mo2 N222 88.5(11) . . ? N232 Mo2 N222 83.6(5) . . ? N2 Mo2 N611 95.3(10) . . ? N232 Mo2 N611 168.9(6) . . ? N222 Mo2 N611 91.3(4) . . ? N2 Mo2 N212 173.7(11) . . ? N232 Mo2 N212 84.8(5) . . ? N222 Mo2 N212 85.2(5) . . ? N611 Mo2 N212 85.0(5) . . ? N2 Mo2 Cl2 95.1(11) . . ? N232 Mo2 Cl2 93.5(4) . . ? N222 Mo2 Cl2 175.5(4) . . ? N611 Mo2 Cl2 90.9(4) . . ? N212 Mo2 Cl2 91.2(4) . . ? O2 N2 Mo2 151.5(79) . . ? N221 B2 N211 109.4(16) . . ? N221 B2 N231 109.5(17) . . ? N211 B2 N231 109.1(16) . . ? C115 N111 N112 108.2(13) . . ? C115 N111 B1 133.4(14) . . ? N112 N111 B1 118.3(11) . . ? C113 N112 N111 107.3(12) . . ? C113 N112 Mo1 133.4(11) . . ? N111 N112 Mo1 119.2(9) . . ? N112 C113 C114 109.3(16) . . ? N112 C113 C117 121.9(15) . . ? C114 C113 C117 128.8(16) . . ? C115 C114 C113 107.1(16) . . ? N111 C115 C114 108.1(16) . . ? N111 C115 C116 119.6(16) . . ? C114 C115 C116 132.2(16) . . ? C125 N121 N122 110.5(14) . . ? C125 N121 B1 131.8(15) . . ? N122 N121 B1 117.6(15) . . ? C123 N122 N121 104.2(15) . . ? C123 N122 Mo1 136.4(13) . . ? N121 N122 Mo1 119.0(12) . . ? C124 C123 N122 108.7(17) . . ? C124 C123 C127 128.2(21) . . ? N122 C123 C127 123.1(19) . . ? C123 C124 C125 110.0(19) . . ? N121 C125 C124 106.5(17) . . ? N121 C125 C126 123.6(18) . . ? C124 C125 C126 129.8(21) . . ? N132 N131 C135 107.8(12) . . ? N132 N131 B1 121.5(12) . . ? C135 N131 B1 130.3(13) . . ? C133 N132 N131 107.6(12) . . ? C133 N132 Mo1 135.5(11) . . ? N131 N132 Mo1 116.8(9) . . ? N132 C133 C134 110.6(14) . . ? N132 C133 C137 121.2(15) . . ? C134 C133 C137 128.1(14) . . ? C135 C134 C133 106.2(14) . . ? C134 C135 N131 107.8(14) . . ? C134 C135 C136 131.1(15) . . ? N131 C135 C136 121.1(15) . . ? N212 N211 C215 111.1(16) . . ? N212 N211 B2 119.1(16) . . ? C215 N211 B2 129.8(19) . . ? N211 N212 C213 106.4(15) . . ? N211 N212 Mo2 118.5(10) . . ? C213 N212 Mo2 134.8(14) . . ? N212 C213 C214 107.5(17) . . ? N212 C213 C217 122.3(19) . . ? C214 C213 C217 130.1(18) . . ? C215 C214 C213 108.7(20) . . ? C214 C215 N211 106.2(21) . . ? C214 C215 C216 132.5(24) . . ? N211 C215 C216 121.3(19) . . ? C225 N221 N222 109.3(13) . . ? C225 N221 B2 130.5(17) . . ? N222 N221 B2 120.1(15) . . ? N221 N222 C223 106.9(13) . . ? N221 N222 Mo2 118.3(9) . . ? C223 N222 Mo2 134.9(13) . . ? N222 C223 C224 107.0(17) . . ? N222 C223 C227 121.0(17) . . ? C224 C223 C227 131.9(18) . . ? C225 C224 C223 107.6(18) . . ? N221 C225 C224 109.3(17) . . ? N221 C225 C226 124.3(20) . . ? C224 C225 C226 126.4(21) . . ? N232 N231 C235 110.7(19) . . ? N232 N231 B2 120.9(14) . . ? C235 N231 B2 128.4(21) . . ? N231 N232 C233 107.0(15) . . ? N231 N232 Mo2 118.7(10) . . ? C233 N232 Mo2 134.2(14) . . ? N232 C233 C234 108.4(20) . . ? N232 C233 C237 121.9(17) . . ? C234 C233 C237 129.7(20) . . ? C233 C234 C235 108.5(19) . . ? N231 C235 C234 105.3(20) . . ? N231 C235 C236 121.8(26) . . ? C234 C235 C236 132.8(22) . . ? C312 N311 C316 115.8(13) . . ? C312 N311 Mo1 121.4(11) . . ? C316 N311 Mo1 122.8(11) . . ? N311 C312 C313 122.7(16) . . ? C314 C313 C312 118.7(16) . . ? C315 C314 C313 118.9(15) . . ? C315 C314 C317 119.5(17) . . ? C313 C314 C317 121.6(18) . . ? C314 C315 C316 119.2(17) . . ? N311 C316 C315 124.7(17) . . ? C318 C317 C314 123.1(18) . . ? C317 C318 C411 128.6(19) . . ? C416 C411 C412 120.9(16) . . ? C416 C411 C318 118.0(18) . . ? C412 C411 C318 120.9(20) . . ? C411 C412 C413 118.3(18) . . ? C414 C413 C412 119.1(16) . . ? C414 C413 C421 108.6(15) . . ? C412 C413 C421 132.3(19) . . ? C415 C414 C413 121.9(14) . . ? C415 C414 C514 130.9(16) . . ? C413 C414 C514 107.2(15) . . ? C414 C415 C416 117.7(17) . . ? C411 C416 C415 122.0(18) . . ? O422 C421 C513 127.6(17) . . ? O422 C421 C413 125.2(18) . . ? C513 C421 C413 107.1(18) . . ? C516 C511 C512 119.6(14) . . ? C516 C511 C517 122.7(17) . . ? C512 C511 C517 117.5(17) . . ? C513 C512 C511 119.3(16) . . ? C512 C513 C514 118.9(15) . . ? C512 C513 C421 131.4(18) . . ? C514 C513 C421 109.6(15) . . ? C515 C514 C513 123.2(14) . . ? C515 C514 C414 129.2(16) . . ? C513 C514 C414 107.4(14) . . ? C514 C515 C516 115.8(17) . . ? C511 C516 C515 123.0(16) . . ? C518 C517 C511 127.5(21) . . ? C517 C518 C614 126.4(20) . . ? C616 N611 C612 117.6(13) . . ? C616 N611 Mo2 121.1(10) . . ? C612 N611 Mo2 120.3(11) . . ? N611 C612 C613 122.1(16) . . ? C614 C613 C612 120.4(16) . . ? C613 C614 C615 116.8(14) . . ? C613 C614 C518 123.9(17) . . ? C615 C614 C518 119.0(17) . . ? C616 C615 C614 119.6(17) . . ? N611 C616 C615 123.3(16) . . ? Cl12 C10 Cl11 112.4(20) . . ? Cl21 C20 Cl22 113.8(15) . . ? Cl32 C30 Cl31 101.5(13) . . ? Cl33 C30 Cl31 103.2(18) . . ? Cl42 C40 Cl41 109.5(17) . . ? Cl52 C50 Cl51 107.3(16) . . ? Cl53 C50 Cl51 106.1(17) . . ? Cl56 C55 Cl54 106.3(17) . . ? _refine_diff_density_max 0.959 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.122