data_002245m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(1-AdNC)2Mo(N[iPr]Ar)3' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H90 Mo N5' _chemical_formula_weight 977.31 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' '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 10.6383(11) _cell_length_b 10.9340(11) _cell_length_c 24.980(3) _cell_angle_alpha 91.598(2) _cell_angle_beta 101.624(2) _cell_angle_gamma 101.257(2) _cell_volume 2784.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 22.50 _exptl_crystal_description 'block' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1054 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2828 _exptl_absorpt_correction_T_max 0.3918 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10591 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 22.50 _reflns_number_total 7199 _reflns_number_gt 6210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0712P)^2^+24.6213P] 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 7199 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1238 _refine_ls_R_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.2566 _refine_ls_wR_factor_gt 0.2495 _refine_ls_goodness_of_fit_ref 1.219 _refine_ls_restrained_S_all 1.219 _refine_ls_shift/su_max 0.108 _refine_ls_shift/su_mean 0.023 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 0.65252(8) -0.40053(8) 0.72173(3) 0.0258(3) Uani 1 1 d . . . N1 N 0.7309(8) -0.4256(8) 0.6519(3) 0.035(2) Uani 1 1 d . . . N2 N 0.5448(7) -0.2706(7) 0.7163(3) 0.0322(19) Uani 1 1 d . . . N3 N 0.6478(8) -0.4904(7) 0.7897(3) 0.039(2) Uani 1 1 d . . . N4 N 0.4063(8) -0.6085(8) 0.6500(4) 0.045(2) Uani 1 1 d . . . N5 N 0.9243(9) -0.2171(9) 0.7821(4) 0.049(2) Uani 1 1 d . . . C11 C 0.7400(9) -0.5481(10) 0.6392(4) 0.038(2) Uani 1 1 d . . . C12 C 0.7815(9) -0.6200(10) 0.6818(4) 0.040(3) Uani 1 1 d . . . H12A H 0.8051 -0.5830 0.7173 0.048 Uiso 1 1 calc R . . C13 C 0.7895(10) -0.7449(10) 0.6738(5) 0.045(3) Uani 1 1 d . . . C14 C 0.7501(11) -0.7983(11) 0.6202(5) 0.055(3) Uani 1 1 d . . . H14A H 0.7504 -0.8825 0.6139 0.065 Uiso 1 1 calc R . . C15 C 0.7105(10) -0.7311(11) 0.5758(5) 0.048(3) Uani 1 1 d . . . C16 C 0.7070(9) -0.6077(10) 0.5857(4) 0.040(3) Uani 1 1 d . . . H16A H 0.6819 -0.5616 0.5561 0.048 Uiso 1 1 calc R . . C17 C 0.7354(10) -0.3393(10) 0.6088(4) 0.042(3) Uani 1 1 d . . . H17A H 0.7825 -0.3696 0.5829 0.051 Uiso 1 1 calc R . . C18 C 0.8113(13) -0.2097(10) 0.6328(5) 0.060(3) Uani 1 1 d . . . H18A H 0.8971 -0.2156 0.6524 0.090 Uiso 1 1 calc R . . H18B H 0.7653 -0.1770 0.6574 0.090 Uiso 1 1 calc R . . H18C H 0.8192 -0.1550 0.6037 0.090 Uiso 1 1 calc R . . C19 C 0.5989(12) -0.3326(13) 0.5773(5) 0.063(4) Uani 1 1 d . . . H19A H 0.5531 -0.4146 0.5620 0.095 Uiso 1 1 calc R . . H19B H 0.6061 -0.2775 0.5483 0.095 Uiso 1 1 calc R . . H19C H 0.5514 -0.3015 0.6016 0.095 Uiso 1 1 calc R . . C21 C 0.4037(9) -0.3115(9) 0.7064(4) 0.035(2) Uani 1 1 d . . . C22 C 0.3446(10) -0.3695(9) 0.7458(5) 0.042(3) Uani 1 1 d . . . H22A H 0.3958 -0.3767 0.7799 0.051 Uiso 1 1 calc R . . C23 C 0.2095(11) -0.4178(10) 0.7359(5) 0.049(3) Uani 1 1 d . . . C24 C 0.1333(11) -0.4058(11) 0.6843(5) 0.052(3) Uani 1 1 d . . . H24A H 0.0435 -0.4382 0.6772 0.062 Uiso 1 1 calc R . . C25 C 0.1884(10) -0.3470(10) 0.6439(5) 0.045(3) Uani 1 1 d . . . C26 C 0.3248(10) -0.2996(10) 0.6552(5) 0.047(3) Uani 1 1 d . . . H26A H 0.3633 -0.2599 0.6283 0.056 Uiso 1 1 calc R . . C27 C 0.5910(10) -0.1372(9) 0.7357(5) 0.042(3) Uani 1 1 d . . . H27A H 0.6842 -0.1152 0.7345 0.050 Uiso 1 1 calc R . . C28 C 0.5808(12) -0.1104(11) 0.7940(5) 0.060(3) Uani 1 1 d . . . H28A H 0.6255 -0.1636 0.8174 0.090 Uiso 1 1 calc R . . H28B H 0.4902 -0.1260 0.7963 0.090 Uiso 1 1 calc R . . H28C H 0.6203 -0.0245 0.8054 0.090 Uiso 1 1 calc R . . C29 C 0.5216(12) -0.0507(10) 0.6984(6) 0.068(4) Uani 1 1 d . . . H29A H 0.5285 -0.0676 0.6613 0.102 Uiso 1 1 calc R . . H29B H 0.5620 0.0348 0.7101 0.102 Uiso 1 1 calc R . . H29C H 0.4308 -0.0653 0.7005 0.102 Uiso 1 1 calc R . . C31 C 0.7490(10) -0.4578(9) 0.8398(4) 0.039(3) Uani 1 1 d . . . C32 C 0.7413(12) -0.3646(10) 0.8773(4) 0.049(3) Uani 1 1 d . . . H32A H 0.6722 -0.3229 0.8700 0.059 Uiso 1 1 calc R . . C33 C 0.8360(12) -0.3328(10) 0.9257(4) 0.049(3) Uani 1 1 d . . . C34 C 0.9372(12) -0.3980(11) 0.9354(5) 0.052(3) Uani 1 1 d . . . H34A H 1.0000 -0.3780 0.9678 0.063 Uiso 1 1 calc R . . C35 C 0.9492(10) -0.4903(10) 0.8997(4) 0.041(3) Uani 1 1 d . . . C36 C 0.8532(10) -0.5198(10) 0.8506(4) 0.039(2) Uani 1 1 d . . . H36A H 0.8595 -0.5810 0.8252 0.046 Uiso 1 1 calc R . . C37 C 0.5390(10) -0.5979(9) 0.7953(4) 0.041(3) Uani 1 1 d . . . H37A H 0.4622 -0.5942 0.7666 0.049 Uiso 1 1 calc R . . C38 C 0.4989(11) -0.5931(11) 0.8498(5) 0.053(3) Uani 1 1 d . . . H38A H 0.4724 -0.5155 0.8553 0.079 Uiso 1 1 calc R . . H38B H 0.5717 -0.5994 0.8786 0.079 Uiso 1 1 calc R . . H38C H 0.4271 -0.6614 0.8502 0.079 Uiso 1 1 calc R . . C39 C 0.5791(12) -0.7244(10) 0.7858(6) 0.059(3) Uani 1 1 d . . . H39A H 0.6052 -0.7271 0.7513 0.088 Uiso 1 1 calc R . . H39B H 0.5059 -0.7917 0.7856 0.088 Uiso 1 1 calc R . . H39C H 0.6509 -0.7327 0.8147 0.088 Uiso 1 1 calc R . . C41 C 0.4895(10) -0.5344(10) 0.6764(4) 0.036(2) Uani 1 1 d . . . C42 C 0.3099(10) -0.7097(9) 0.6206(4) 0.037(2) Uani 1 1 d . . . C43 C 0.3697(13) -0.8246(12) 0.6175(6) 0.073(4) Uani 1 1 d . . . H43A H 0.4024 -0.8474 0.6542 0.087 Uiso 1 1 calc R . . H43B H 0.4426 -0.8066 0.5991 0.087 Uiso 1 1 calc R . . C44 C 0.1966(14) -0.7337(14) 0.6499(7) 0.084(5) Uani 1 1 d . . . H44A H 0.1593 -0.6598 0.6512 0.101 Uiso 1 1 calc R . . H44B H 0.2263 -0.7551 0.6871 0.101 Uiso 1 1 calc R . . C45 C 0.2622(16) -0.6718(15) 0.5639(6) 0.085(4) Uani 1 1 d . . . H45A H 0.3346 -0.6518 0.5453 0.101 Uiso 1 1 calc R . . H45B H 0.2241 -0.5986 0.5658 0.101 Uiso 1 1 calc R . . C46 C 0.2568(14) -0.9411(14) 0.5836(6) 0.077(4) Uani 1 1 d . . . H46A H 0.2914 -1.0173 0.5810 0.092 Uiso 1 1 calc R . . C47 C 0.2221(15) -0.8925(13) 0.5300(6) 0.073(4) Uani 1 1 d . . . H47A H 0.1675 -0.9599 0.5047 0.087 Uiso 1 1 calc R . . H47B H 0.3016 -0.8639 0.5167 0.087 Uiso 1 1 calc R . . C48 C 0.1521(16) -0.7888(15) 0.5304(6) 0.084(5) Uani 1 1 d . . . H48A H 0.1184 -0.7684 0.4930 0.101 Uiso 1 1 calc R . . C49 C 0.0501(16) -0.8013(17) 0.5624(8) 0.100(6) Uani 1 1 d . . . H49A H -0.0284 -0.8567 0.5418 0.120 Uiso 1 1 calc R . . H49B H 0.0290 -0.7201 0.5679 0.120 Uiso 1 1 calc R . . C51 C 0.8258(10) -0.2792(10) 0.7601(4) 0.039(3) Uani 1 1 d . . . C52 C 1.0303(9) -0.1186(9) 0.8112(4) 0.037(2) Uani 1 1 d . . . C53 C 0.9735(12) -0.0386(12) 0.8469(6) 0.072(4) Uani 1 1 d . . . H53A H 0.9297 -0.0901 0.8715 0.086 Uiso 1 1 calc R . . H53B H 0.9098 0.0010 0.8242 0.086 Uiso 1 1 calc R . . C54 C 1.0918(15) -0.0344(13) 0.7705(5) 0.076(4) Uani 1 1 d . . . H54A H 1.1290 -0.0835 0.7473 0.091 Uiso 1 1 calc R . . H54B H 1.0249 0.0007 0.7474 0.091 Uiso 1 1 calc R . . C55 C 1.1336(13) -0.1739(12) 0.8465(6) 0.078(4) Uani 1 1 d . . . H55A H 1.1682 -0.2270 0.8239 0.093 Uiso 1 1 calc R . . H55B H 1.0953 -0.2249 0.8726 0.093 Uiso 1 1 calc R . . C56 C 1.0895(14) 0.0639(13) 0.8810(6) 0.073(4) Uani 1 1 d . . . H56A H 1.0551 0.1125 0.9061 0.088 Uiso 1 1 calc R . . C57 C 1.1910(15) 0.0046(15) 0.9131(6) 0.085(5) Uani 1 1 d . . . H57A H 1.2615 0.0687 0.9339 0.102 Uiso 1 1 calc R . . H57B H 1.1534 -0.0483 0.9388 0.102 Uiso 1 1 calc R . . C58 C 1.2435(15) -0.0705(13) 0.8769(7) 0.085(5) Uani 1 1 d . . . H58A H 1.3125 -0.1071 0.8987 0.101 Uiso 1 1 calc R . . C59 C 1.3004(12) 0.0133(14) 0.8364(7) 0.078(4) Uani 1 1 d . . . H59A H 1.3705 0.0792 0.8562 0.093 Uiso 1 1 calc R . . H59B H 1.3372 -0.0352 0.8128 0.093 Uiso 1 1 calc R . . C61 C 0.560(2) 0.355(3) 1.0462(10) 0.171(12) Uani 1 1 d . . . H61A H 0.4742 0.3539 1.0533 0.257 Uiso 1 1 calc R . . H61B H 0.5956 0.4372 1.0364 0.257 Uiso 1 1 calc R . . H61C H 0.6160 0.3352 1.0784 0.257 Uiso 1 1 calc R . . C62 C 0.550(2) 0.263(2) 1.0008(8) 0.118(7) Uani 1 1 d . . . H62A H 0.5095 0.1821 1.0108 0.142 Uiso 1 1 calc R . . H62B H 0.4909 0.2842 0.9691 0.142 Uiso 1 1 calc R . . C63 C 0.6704(14) 0.2517(17) 0.9848(6) 0.083(4) Uani 1 1 d . . . H63A H 0.7350 0.2467 1.0177 0.100 Uiso 1 1 calc R . . H63B H 0.7020 0.3277 0.9682 0.100 Uiso 1 1 calc R . . C64 C 0.6645(16) 0.1454(17) 0.9467(7) 0.094(5) Uani 1 1 d . . . H64A H 0.6339 0.0696 0.9636 0.113 Uiso 1 1 calc R . . H64B H 0.5985 0.1497 0.9142 0.113 Uiso 1 1 calc R . . C65 C 0.7840(17) 0.1329(17) 0.9293(7) 0.100(5) Uani 1 1 d . . . H65A H 0.7663 0.0603 0.9043 0.150 Uiso 1 1 calc R . . H65B H 0.8497 0.1243 0.9607 0.150 Uiso 1 1 calc R . . H65C H 0.8148 0.2059 0.9113 0.150 Uiso 1 1 calc R . . C131 C 0.8413(12) -0.8149(12) 0.7211(5) 0.063(3) Uani 1 1 d . . . H13A H 0.8409 -0.8986 0.7084 0.094 Uiso 1 1 calc R . . H13B H 0.7868 -0.8174 0.7476 0.094 Uiso 1 1 calc R . . H13C H 0.9293 -0.7736 0.7378 0.094 Uiso 1 1 calc R . . C151 C 0.6718(12) -0.7899(12) 0.5196(5) 0.064(4) Uani 1 1 d . . . H15A H 0.6474 -0.7295 0.4945 0.095 Uiso 1 1 calc R . . H15B H 0.5986 -0.8584 0.5172 0.095 Uiso 1 1 calc R . . H15C H 0.7441 -0.8203 0.5104 0.095 Uiso 1 1 calc R . . C231 C 0.1500(13) -0.4887(12) 0.7780(5) 0.063(3) Uani 1 1 d . . . H23A H 0.2162 -0.4872 0.8106 0.095 Uiso 1 1 calc R . . H23B H 0.1140 -0.5737 0.7640 0.095 Uiso 1 1 calc R . . H23C H 0.0817 -0.4508 0.7865 0.095 Uiso 1 1 calc R . . C251 C 0.1052(11) -0.3382(14) 0.5888(6) 0.072(4) Uani 1 1 d . . . H25A H 0.0157 -0.3760 0.5885 0.108 Uiso 1 1 calc R . . H25B H 0.1353 -0.3811 0.5614 0.108 Uiso 1 1 calc R . . H25C H 0.1112 -0.2519 0.5812 0.108 Uiso 1 1 calc R . . C331 C 0.8243(14) -0.2349(13) 0.9661(5) 0.075(4) Uani 1 1 d . . . H33A H 0.8970 -0.2244 0.9968 0.112 Uiso 1 1 calc R . . H33B H 0.7438 -0.2598 0.9784 0.112 Uiso 1 1 calc R . . H33C H 0.8245 -0.1573 0.9490 0.112 Uiso 1 1 calc R . . C351 C 1.0625(12) -0.5574(13) 0.9106(5) 0.067(4) Uani 1 1 d . . . H35A H 1.1187 -0.5261 0.9453 0.101 Uiso 1 1 calc R . . H35B H 1.1112 -0.5432 0.8822 0.101 Uiso 1 1 calc R . . H35C H 1.0293 -0.6454 0.9113 0.101 Uiso 1 1 calc R . . C410 C 0.0878(16) -0.8496(16) 0.6151(7) 0.090(5) Uani 1 1 d . . . H41A H 0.0120 -0.8687 0.6324 0.107 Uiso 1 1 calc R . . C411 C 0.1527(16) -0.9571(15) 0.6166(7) 0.088(5) Uani 1 1 d . . . H41B H 0.0875 -1.0322 0.6026 0.106 Uiso 1 1 calc R . . H41C H 0.1917 -0.9679 0.6543 0.106 Uiso 1 1 calc R . . C510 C 1.1978(13) 0.0697(13) 0.8025(6) 0.074(4) Uani 1 1 d . . . H51A H 1.2362 0.1251 0.7773 0.089 Uiso 1 1 calc R . . C511 C 1.1368(17) 0.1453(13) 0.8410(6) 0.086(5) Uani 1 1 d . . . H51B H 1.2024 0.2160 0.8597 0.103 Uiso 1 1 calc R . . H51C H 1.0648 0.1768 0.8195 0.103 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 0.0201(4) 0.0215(4) 0.0308(5) 0.0022(3) 0.0014(3) -0.0038(3) N1 0.032(5) 0.042(5) 0.028(4) 0.007(4) 0.006(4) -0.003(4) N2 0.024(4) 0.027(4) 0.039(5) 0.008(4) 0.004(4) -0.007(3) N3 0.030(5) 0.034(5) 0.045(5) 0.004(4) 0.014(4) -0.016(4) N4 0.031(5) 0.044(5) 0.049(6) -0.008(5) -0.001(4) -0.007(5) N5 0.039(6) 0.053(6) 0.048(6) -0.006(5) 0.009(5) -0.010(5) C11 0.030(6) 0.046(7) 0.035(6) 0.000(5) 0.007(5) 0.004(5) C12 0.027(5) 0.048(7) 0.042(6) 0.009(5) 0.004(5) 0.006(5) C13 0.037(6) 0.042(7) 0.057(8) 0.013(6) 0.008(5) 0.011(5) C14 0.039(7) 0.047(7) 0.076(9) 0.001(7) 0.011(6) 0.006(6) C15 0.029(6) 0.052(7) 0.059(8) -0.009(6) 0.003(5) 0.004(5) C16 0.023(5) 0.051(7) 0.045(7) 0.007(5) 0.001(5) 0.012(5) C17 0.046(6) 0.045(6) 0.036(6) 0.011(5) 0.010(5) 0.005(5) C18 0.083(9) 0.044(7) 0.060(8) 0.018(6) 0.042(7) -0.003(6) C19 0.056(8) 0.089(10) 0.054(8) 0.031(7) 0.015(6) 0.029(7) C21 0.026(5) 0.033(6) 0.044(6) -0.003(5) 0.005(5) 0.005(4) C22 0.039(6) 0.035(6) 0.053(7) 0.006(5) 0.008(5) 0.006(5) C23 0.039(7) 0.043(7) 0.064(8) -0.001(6) 0.021(6) -0.003(5) C24 0.027(6) 0.053(7) 0.073(9) 0.005(6) 0.010(6) 0.002(5) C25 0.028(6) 0.044(6) 0.061(7) 0.005(6) 0.003(5) 0.007(5) C26 0.044(7) 0.037(6) 0.059(8) 0.017(5) 0.013(6) 0.002(5) C27 0.035(6) 0.020(5) 0.066(8) 0.001(5) 0.009(5) -0.001(4) C28 0.061(8) 0.036(7) 0.072(9) -0.022(6) 0.006(7) -0.006(6) C29 0.052(8) 0.033(7) 0.103(11) 0.004(7) -0.013(7) 0.002(6) C31 0.043(6) 0.037(6) 0.030(6) 0.007(5) 0.003(5) -0.005(5) C32 0.055(7) 0.040(6) 0.045(7) 0.002(5) 0.007(6) -0.004(5) C33 0.058(8) 0.043(7) 0.035(6) 0.005(5) 0.000(6) -0.004(6) C34 0.050(7) 0.060(8) 0.037(7) 0.010(6) 0.000(6) -0.003(6) C35 0.041(6) 0.041(6) 0.034(6) 0.015(5) -0.003(5) 0.001(5) C36 0.035(6) 0.039(6) 0.041(6) 0.006(5) 0.011(5) 0.002(5) C37 0.032(6) 0.040(6) 0.042(6) 0.011(5) 0.007(5) -0.013(5) C38 0.053(7) 0.048(7) 0.051(7) 0.006(6) 0.015(6) -0.008(6) C39 0.055(8) 0.026(6) 0.087(10) 0.006(6) 0.011(7) -0.008(5) C41 0.025(6) 0.037(6) 0.044(6) 0.003(5) 0.006(5) 0.005(5) C42 0.040(6) 0.035(6) 0.033(6) -0.005(5) 0.004(5) 0.007(5) C43 0.056(8) 0.056(8) 0.098(11) 0.012(8) 0.010(8) -0.002(7) C44 0.064(9) 0.067(9) 0.109(12) -0.014(9) 0.028(9) -0.025(7) C45 0.092(11) 0.083(11) 0.070(10) 0.005(8) 0.006(8) 0.006(9) C46 0.075(10) 0.075(10) 0.084(11) -0.012(8) 0.019(8) 0.023(8) C47 0.082(10) 0.075(10) 0.059(9) -0.007(7) 0.017(8) 0.009(8) C48 0.080(11) 0.097(12) 0.067(10) 0.013(9) -0.010(8) 0.027(9) C49 0.060(10) 0.094(13) 0.135(17) -0.026(12) -0.009(11) 0.025(9) C51 0.032(6) 0.042(6) 0.042(6) 0.004(5) 0.009(5) 0.000(5) C52 0.023(5) 0.032(6) 0.047(6) 0.000(5) -0.001(5) -0.010(4) C53 0.048(8) 0.058(8) 0.093(11) -0.016(7) 0.005(7) -0.013(6) C54 0.087(10) 0.071(9) 0.054(8) 0.016(7) 0.012(7) -0.020(8) C55 0.061(9) 0.055(8) 0.090(11) 0.012(7) -0.025(8) -0.011(7) C56 0.063(9) 0.064(9) 0.078(10) -0.023(8) 0.008(8) -0.009(7) C57 0.073(10) 0.079(11) 0.070(10) 0.011(8) -0.019(8) -0.030(8) C58 0.071(10) 0.061(9) 0.091(11) -0.009(9) -0.046(9) 0.010(8) C59 0.032(7) 0.078(10) 0.108(12) -0.014(9) 0.014(8) -0.020(7) C61 0.089(15) 0.26(3) 0.15(2) -0.09(2) 0.031(14) 0.032(17) C62 0.108(16) 0.161(19) 0.082(13) 0.016(13) 0.015(11) 0.023(14) C63 0.055(9) 0.115(13) 0.073(10) 0.010(10) 0.000(8) 0.014(9) C64 0.072(11) 0.106(13) 0.091(12) 0.010(11) 0.000(9) 0.000(10) C65 0.097(13) 0.117(14) 0.091(12) 0.011(10) 0.033(10) 0.020(11) C131 0.052(8) 0.053(8) 0.082(9) 0.009(7) 0.006(7) 0.017(6) C151 0.056(8) 0.068(9) 0.066(9) -0.012(7) 0.001(7) 0.025(7) C231 0.059(8) 0.065(8) 0.066(9) 0.008(7) 0.020(7) 0.001(7) C251 0.031(7) 0.092(10) 0.083(10) 0.021(8) -0.009(6) 0.009(7) C331 0.078(10) 0.082(10) 0.058(8) -0.019(7) 0.006(7) 0.013(8) C351 0.054(8) 0.084(10) 0.061(8) 0.018(7) 0.003(7) 0.016(7) C410 0.069(10) 0.101(13) 0.103(13) 0.004(10) 0.045(10) 0.000(9) C411 0.090(12) 0.071(10) 0.104(13) 0.005(9) 0.039(10) -0.001(9) C510 0.058(9) 0.080(10) 0.065(9) 0.027(8) 0.012(7) -0.035(8) C511 0.120(13) 0.042(8) 0.088(11) 0.012(8) 0.004(10) 0.019(9) _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 N2 1.983(8) . ? Mo1 N3 1.990(8) . ? Mo1 C51 2.083(11) . ? Mo1 N1 2.112(8) . ? Mo1 C41 2.135(11) . ? N1 C11 1.395(13) . ? N1 C17 1.454(13) . ? N2 C21 1.448(12) . ? N2 C27 1.480(12) . ? N3 C31 1.462(13) . ? N3 C37 1.511(12) . ? N4 C41 1.153(12) . ? N4 C42 1.422(13) . ? N5 C51 1.153(13) . ? N5 C52 1.454(13) . ? C11 C12 1.391(14) . ? C11 C16 1.418(14) . ? C12 C13 1.396(15) . ? C13 C14 1.395(16) . ? C13 C131 1.497(16) . ? C14 C15 1.386(17) . ? C15 C16 1.374(15) . ? C15 C151 1.473(16) . ? C17 C18 1.527(15) . ? C17 C19 1.522(15) . ? C21 C22 1.376(14) . ? C21 C26 1.406(15) . ? C22 C23 1.400(15) . ? C23 C24 1.401(17) . ? C23 C231 1.494(16) . ? C24 C25 1.380(16) . ? C25 C26 1.410(15) . ? C25 C251 1.495(16) . ? C27 C28 1.507(16) . ? C27 C29 1.533(15) . ? C31 C36 1.394(14) . ? C31 C32 1.389(15) . ? C32 C33 1.396(15) . ? C33 C34 1.389(16) . ? C33 C331 1.490(17) . ? C34 C35 1.370(16) . ? C35 C36 1.414(14) . ? C35 C351 1.513(16) . ? C37 C38 1.509(15) . ? C37 C39 1.550(15) . ? C42 C45 1.504(17) . ? C42 C43 1.522(16) . ? C42 C44 1.516(17) . ? C43 C46 1.648(19) . ? C44 C410 1.63(2) . ? C45 C48 1.63(2) . ? C46 C47 1.46(2) . ? C46 C411 1.50(2) . ? C47 C48 1.47(2) . ? C48 C49 1.46(2) . ? C49 C410 1.44(2) . ? C52 C55 1.500(16) . ? C52 C53 1.519(17) . ? C52 C54 1.547(16) . ? C53 C56 1.577(17) . ? C54 C510 1.514(18) . ? C55 C58 1.517(17) . ? C56 C57 1.48(2) . ? C56 C511 1.46(2) . ? C57 C58 1.46(2) . ? C58 C59 1.52(2) . ? C59 C510 1.49(2) . ? C61 C62 1.47(3) . ? C62 C63 1.45(2) . ? C63 C64 1.46(2) . ? C64 C65 1.45(2) . ? C410 C411 1.47(2) . ? C510 C511 1.56(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 N2 Mo1 N3 111.6(3) . . ? N2 Mo1 C51 94.7(4) . . ? N3 Mo1 C51 90.8(4) . . ? N2 Mo1 N1 114.1(3) . . ? N3 Mo1 N1 133.9(3) . . ? C51 Mo1 N1 90.7(4) . . ? N2 Mo1 C41 90.7(3) . . ? N3 Mo1 C41 91.6(4) . . ? C51 Mo1 C41 172.8(4) . . ? N1 Mo1 C41 82.7(3) . . ? C11 N1 C17 117.3(8) . . ? C11 N1 Mo1 115.0(6) . . ? C17 N1 Mo1 124.6(7) . . ? C21 N2 C27 113.5(8) . . ? C21 N2 Mo1 117.9(6) . . ? C27 N2 Mo1 126.5(6) . . ? C31 N3 C37 113.0(8) . . ? C31 N3 Mo1 123.2(6) . . ? C37 N3 Mo1 123.8(6) . . ? C41 N4 C42 173.9(11) . . ? C51 N5 C52 167.1(11) . . ? N1 C11 C12 118.6(9) . . ? N1 C11 C16 124.9(9) . . ? C12 C11 C16 116.5(10) . . ? C11 C12 C13 123.2(10) . . ? C14 C13 C12 116.8(10) . . ? C14 C13 C131 122.7(11) . . ? C12 C13 C131 120.4(11) . . ? C13 C14 C15 122.7(11) . . ? C16 C15 C14 118.2(11) . . ? C16 C15 C151 120.5(11) . . ? C14 C15 C151 121.3(11) . . ? C15 C16 C11 122.4(10) . . ? N1 C17 C18 110.1(9) . . ? N1 C17 C19 112.1(9) . . ? C18 C17 C19 110.6(10) . . ? C22 C21 C26 118.5(9) . . ? C22 C21 N2 120.7(9) . . ? C26 C21 N2 120.7(9) . . ? C21 C22 C23 121.8(10) . . ? C22 C23 C24 118.5(10) . . ? C22 C23 C231 120.4(11) . . ? C24 C23 C231 120.9(10) . . ? C25 C24 C23 121.5(10) . . ? C24 C25 C26 118.5(10) . . ? C24 C25 C251 120.3(10) . . ? C26 C25 C251 121.1(11) . . ? C21 C26 C25 121.1(10) . . ? N2 C27 C28 113.4(9) . . ? N2 C27 C29 112.7(9) . . ? C28 C27 C29 109.5(10) . . ? C36 C31 C32 119.6(10) . . ? C36 C31 N3 120.6(9) . . ? C32 C31 N3 119.9(10) . . ? C31 C32 C33 120.9(11) . . ? C34 C33 C32 117.9(11) . . ? C34 C33 C331 122.0(11) . . ? C32 C33 C331 120.1(12) . . ? C35 C34 C33 123.4(11) . . ? C34 C35 C36 117.8(10) . . ? C34 C35 C351 122.2(10) . . ? C36 C35 C351 120.0(10) . . ? C31 C36 C35 120.5(10) . . ? N3 C37 C38 113.5(8) . . ? N3 C37 C39 110.3(8) . . ? C38 C37 C39 109.5(9) . . ? N4 C41 Mo1 175.9(9) . . ? N4 C42 C45 108.4(10) . . ? N4 C42 C43 109.7(9) . . ? C45 C42 C43 110.1(10) . . ? N4 C42 C44 108.0(9) . . ? C45 C42 C44 109.2(11) . . ? C43 C42 C44 111.4(11) . . ? C42 C43 C46 109.1(10) . . ? C42 C44 C410 106.8(11) . . ? C42 C45 C48 107.9(11) . . ? C47 C46 C411 115.6(14) . . ? C47 C46 C43 102.3(12) . . ? C411 C46 C43 103.4(12) . . ? C46 C47 C48 113.7(12) . . ? C49 C48 C47 117.0(15) . . ? C49 C48 C45 102.3(13) . . ? C47 C48 C45 104.7(12) . . ? C48 C49 C410 113.2(13) . . ? N5 C51 Mo1 176.7(10) . . ? N5 C52 C55 110.3(9) . . ? N5 C52 C53 108.1(8) . . ? C55 C52 C53 109.6(11) . . ? N5 C52 C54 110.7(9) . . ? C55 C52 C54 109.8(11) . . ? C53 C52 C54 108.3(10) . . ? C52 C53 C56 108.2(10) . . ? C510 C54 C52 109.0(10) . . ? C52 C55 C58 109.9(11) . . ? C57 C56 C511 113.6(13) . . ? C57 C56 C53 110.5(12) . . ? C511 C56 C53 105.5(12) . . ? C58 C57 C56 110.6(13) . . ? C57 C58 C59 108.9(12) . . ? C57 C58 C55 109.0(14) . . ? C59 C58 C55 110.1(12) . . ? C510 C59 C58 110.8(11) . . ? C63 C62 C61 117.0(18) . . ? C62 C63 C64 117.0(16) . . ? C65 C64 C63 118.0(15) . . ? C49 C410 C411 117.1(15) . . ? C49 C410 C44 103.4(14) . . ? C411 C410 C44 106.1(14) . . ? C410 C411 C46 112.3(13) . . ? C59 C510 C54 108.6(12) . . ? C59 C510 C511 109.1(12) . . ? C54 C510 C511 109.1(12) . . ? C56 C511 C510 109.2(11) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.827 _refine_diff_density_min -1.450 _refine_diff_density_rms 0.116 #===END data_003154m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common '(tBuNC)Mo(N[tBu]Ar)3' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H63 Mo N4' _chemical_formula_weight 707.89 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' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.1350(14) _cell_length_b 13.5623(12) _cell_length_c 19.6178(18) _cell_angle_alpha 90.00 _cell_angle_beta 91.1720(10) _cell_angle_gamma 90.00 _cell_volume 4026.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 102 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 22.50 _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2228 _exptl_absorpt_correction_T_max 0.2677 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14846 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5247 _reflns_number_gt 4498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0534P)^2^+19.0564P] 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 5247 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.087 _refine_ls_shift/su_mean 0.017 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 0.25689(3) 0.29529(4) 0.02314(2) 0.0263(2) Uani 1 1 d . . . N1 N 0.2404(3) 0.4120(4) -0.0357(2) 0.0306(12) Uani 1 1 d . . . N2 N 0.3758(3) 0.2348(4) 0.0198(2) 0.0344(13) Uani 1 1 d . . . N3 N 0.1490(3) 0.2149(4) 0.0277(3) 0.0368(13) Uani 1 1 d . . . N4 N 0.2709(5) 0.4052(5) 0.1624(3) 0.0577(17) Uani 1 1 d . . . C11 C 0.1935(4) 0.3833(5) -0.0971(3) 0.0395(16) Uani 1 1 d . . . C12 C 0.1012(5) 0.3948(5) -0.1030(4) 0.0458(18) Uani 1 1 d . . . H12A H 0.0707 0.4232 -0.0673 0.055 Uiso 1 1 calc R . . C13 C 0.0550(5) 0.3647(6) -0.1609(4) 0.0481(18) Uani 1 1 d . . . C14 C 0.1013(5) 0.3217(5) -0.2132(4) 0.0467(18) Uani 1 1 d . . . H14A H 0.0704 0.2997 -0.2517 0.056 Uiso 1 1 calc R . . C15 C 0.1930(5) 0.3102(5) -0.2100(3) 0.0442(17) Uani 1 1 d . . . C16 C 0.2388(5) 0.3411(5) -0.1513(3) 0.0342(15) Uani 1 1 d . . . H16A H 0.2999 0.3336 -0.1482 0.041 Uiso 1 1 calc R . . C17 C 0.2542(5) 0.5215(5) -0.0252(3) 0.0388(16) Uani 1 1 d . . . C18 C 0.2557(7) 0.5755(6) -0.0928(4) 0.077(3) Uani 1 1 d . . . H18A H 0.2006 0.5654 -0.1169 0.116 Uiso 1 1 calc R . . H18B H 0.3032 0.5506 -0.1196 0.116 Uiso 1 1 calc R . . H18C H 0.2642 0.6447 -0.0848 0.116 Uiso 1 1 calc R . . C19 C 0.3415(5) 0.5374(6) 0.0124(4) 0.055(2) Uani 1 1 d . . . H19A H 0.3410 0.5028 0.0551 0.082 Uiso 1 1 calc R . . H19B H 0.3499 0.6065 0.0207 0.082 Uiso 1 1 calc R . . H19C H 0.3888 0.5129 -0.0147 0.082 Uiso 1 1 calc R . . C21 C 0.4056(4) 0.2302(5) -0.0509(3) 0.0358(16) Uani 1 1 d . . . C22 C 0.3848(4) 0.1466(5) -0.0901(3) 0.0388(16) Uani 1 1 d . . . H22A H 0.3516 0.0956 -0.0720 0.047 Uiso 1 1 calc R . . C23 C 0.4149(5) 0.1412(5) -0.1571(4) 0.0467(18) Uani 1 1 d . . . C24 C 0.4646(5) 0.2167(6) -0.1832(4) 0.0518(19) Uani 1 1 d . . . H24A H 0.4849 0.2118 -0.2275 0.062 Uiso 1 1 calc R . . C25 C 0.4855(5) 0.3009(6) -0.1448(4) 0.0476(18) Uani 1 1 d . . . C26 C 0.4558(4) 0.3057(5) -0.0783(3) 0.0389(16) Uani 1 1 d . . . H26A H 0.4698 0.3605 -0.0516 0.047 Uiso 1 1 calc R . . C27 C 0.4437(4) 0.2088(6) 0.0713(3) 0.0477(18) Uani 1 1 d . . . C28 C 0.5109(8) 0.1368(12) 0.0438(5) 0.145(7) Uani 1 1 d . . . H28A H 0.5416 0.1670 0.0069 0.218 Uiso 1 1 calc R . . H28B H 0.4812 0.0785 0.0277 0.218 Uiso 1 1 calc R . . H28C H 0.5525 0.1195 0.0795 0.218 Uiso 1 1 calc R . . C29 C 0.4893(7) 0.3010(8) 0.0991(5) 0.095(4) Uani 1 1 d . . . H29A H 0.5181 0.3347 0.0627 0.143 Uiso 1 1 calc R . . H29B H 0.5323 0.2826 0.1334 0.143 Uiso 1 1 calc R . . H29C H 0.4462 0.3439 0.1187 0.143 Uiso 1 1 calc R . . C31 C 0.1637(4) 0.1243(5) -0.0104(3) 0.0379(16) Uani 1 1 d . . . C32 C 0.2006(4) 0.0419(5) 0.0223(3) 0.0398(16) Uani 1 1 d . . . H32A H 0.2145 0.0450 0.0686 0.048 Uiso 1 1 calc R . . C33 C 0.2169(5) -0.0451(5) -0.0136(4) 0.0458(18) Uani 1 1 d . . . C34 C 0.1946(5) -0.0477(5) -0.0821(4) 0.053(2) Uani 1 1 d . . . H34A H 0.2044 -0.1052 -0.1066 0.063 Uiso 1 1 calc R . . C35 C 0.1575(5) 0.0340(6) -0.1159(4) 0.053(2) Uani 1 1 d . . . C36 C 0.1424(5) 0.1211(5) -0.0801(3) 0.0444(17) Uani 1 1 d . . . H36A H 0.1186 0.1760 -0.1022 0.053 Uiso 1 1 calc R . . C37 C 0.0626(4) 0.2199(5) 0.0646(3) 0.0404(17) Uani 1 1 d . . . C38 C 0.0525(5) 0.3243(5) 0.0928(4) 0.0522(19) Uani 1 1 d . . . H38A H 0.0991 0.3372 0.1255 0.078 Uiso 1 1 calc R . . H38B H -0.0036 0.3302 0.1145 0.078 Uiso 1 1 calc R . . H38C H 0.0556 0.3710 0.0562 0.078 Uiso 1 1 calc R . . C39 C 0.0581(5) 0.1455(6) 0.1218(4) 0.060(2) Uani 1 1 d . . . H39A H 0.1054 0.1574 0.1541 0.090 Uiso 1 1 calc R . . H39B H 0.0635 0.0802 0.1035 0.090 Uiso 1 1 calc R . . H39C H 0.0025 0.1517 0.1441 0.090 Uiso 1 1 calc R . . C41 C 0.2659(4) 0.3588(4) 0.1114(3) 0.0279(14) Uani 1 1 d . . . C42 C 0.2690(6) 0.3867(6) 0.2375(3) 0.053(2) Uani 1 1 d . . . C43 C 0.2311(6) 0.2871(7) 0.2529(4) 0.071(3) Uani 1 1 d . . . H43A H 0.1708 0.2843 0.2367 0.106 Uiso 1 1 calc R . . H43B H 0.2332 0.2761 0.3013 0.106 Uiso 1 1 calc R . . H43C H 0.2649 0.2371 0.2306 0.106 Uiso 1 1 calc R . . C44 C 0.3643(7) 0.3940(8) 0.2657(4) 0.086(3) Uani 1 1 d . . . H44A H 0.3873 0.4586 0.2567 0.128 Uiso 1 1 calc R . . H44B H 0.4003 0.3454 0.2441 0.128 Uiso 1 1 calc R . . H44C H 0.3648 0.3826 0.3140 0.128 Uiso 1 1 calc R . . C45 C 0.2167(10) 0.4674(9) 0.2672(5) 0.128(6) Uani 1 1 d . . . H45A H 0.1569 0.4637 0.2501 0.192 Uiso 1 1 calc R . . H45B H 0.2419 0.5297 0.2547 0.192 Uiso 1 1 calc R . . H45C H 0.2173 0.4612 0.3159 0.192 Uiso 1 1 calc R . . C110 C 0.1816(6) 0.5629(6) 0.0189(5) 0.068(2) Uani 1 1 d . . . H11A H 0.1253 0.5537 -0.0037 0.102 Uiso 1 1 calc R . . H11B H 0.1916 0.6320 0.0264 0.102 Uiso 1 1 calc R . . H11C H 0.1819 0.5292 0.0619 0.102 Uiso 1 1 calc R . . C131 C -0.0436(5) 0.3782(7) -0.1660(4) 0.066(2) Uani 1 1 d . . . H13A H -0.0640 0.4093 -0.1253 0.099 Uiso 1 1 calc R . . H13B H -0.0716 0.3150 -0.1712 0.099 Uiso 1 1 calc R . . H13C H -0.0582 0.4187 -0.2047 0.099 Uiso 1 1 calc R . . C151 C 0.2417(5) 0.2637(6) -0.2680(3) 0.052(2) Uani 1 1 d . . . H15A H 0.2007 0.2485 -0.3044 0.078 Uiso 1 1 calc R . . H15B H 0.2699 0.2042 -0.2524 0.078 Uiso 1 1 calc R . . H15C H 0.2855 0.3088 -0.2840 0.078 Uiso 1 1 calc R . . C210 C 0.3979(5) 0.1566(6) 0.1305(4) 0.054(2) Uani 1 1 d . . . H21A H 0.3692 0.0980 0.1139 0.081 Uiso 1 1 calc R . . H21B H 0.3547 0.2000 0.1496 0.081 Uiso 1 1 calc R . . H21C H 0.4411 0.1393 0.1650 0.081 Uiso 1 1 calc R . . C231 C 0.3948(6) 0.0502(6) -0.1994(4) 0.062(2) Uani 1 1 d . . . H23A H 0.4193 0.0578 -0.2439 0.093 Uiso 1 1 calc R . . H23B H 0.3319 0.0418 -0.2038 0.093 Uiso 1 1 calc R . . H23C H 0.4203 -0.0066 -0.1775 0.093 Uiso 1 1 calc R . . C251 C 0.5375(5) 0.3835(6) -0.1740(4) 0.059(2) Uani 1 1 d . . . H25A H 0.5516 0.3684 -0.2204 0.088 Uiso 1 1 calc R . . H25B H 0.5911 0.3922 -0.1477 0.088 Uiso 1 1 calc R . . H25C H 0.5033 0.4430 -0.1729 0.088 Uiso 1 1 calc R . . C310 C -0.0135(5) 0.2012(7) 0.0126(4) 0.065(2) Uani 1 1 d . . . H31A H -0.0082 0.1359 -0.0058 0.097 Uiso 1 1 calc R . . H31B H -0.0105 0.2486 -0.0236 0.097 Uiso 1 1 calc R . . H31C H -0.0691 0.2074 0.0349 0.097 Uiso 1 1 calc R . . C331 C 0.2547(6) -0.1344(5) 0.0225(4) 0.062(2) Uani 1 1 d . . . H33A H 0.2621 -0.1868 -0.0097 0.093 Uiso 1 1 calc R . . H33B H 0.2151 -0.1552 0.0573 0.093 Uiso 1 1 calc R . . H33C H 0.3110 -0.1179 0.0430 0.093 Uiso 1 1 calc R . . C351 C 0.1312(6) 0.0307(6) -0.1927(4) 0.066(2) Uani 1 1 d . . . H35A H 0.1446 -0.0332 -0.2108 0.099 Uiso 1 1 calc R . . H35B H 0.1637 0.0801 -0.2167 0.099 Uiso 1 1 calc R . . H35C H 0.0690 0.0433 -0.1981 0.099 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 0.0344(3) 0.0227(3) 0.0218(3) -0.0004(2) -0.0013(2) -0.0026(3) N1 0.046(3) 0.022(3) 0.023(3) -0.005(2) -0.003(2) -0.005(2) N2 0.039(3) 0.035(3) 0.029(3) 0.002(2) 0.002(2) 0.002(2) N3 0.040(3) 0.034(3) 0.036(3) -0.005(3) 0.002(2) -0.006(3) N4 0.091(5) 0.041(4) 0.041(4) 0.002(3) -0.003(3) 0.005(3) C11 0.042(4) 0.036(4) 0.040(4) 0.006(3) -0.003(3) -0.004(3) C12 0.048(4) 0.049(5) 0.040(4) 0.007(3) -0.002(3) 0.009(4) C13 0.047(4) 0.053(5) 0.044(4) 0.002(4) -0.007(3) 0.003(4) C14 0.058(5) 0.046(4) 0.036(4) 0.009(3) -0.015(3) -0.005(4) C15 0.061(5) 0.035(4) 0.037(4) 0.006(3) 0.003(3) -0.001(4) C16 0.048(4) 0.028(3) 0.026(3) 0.002(3) -0.001(3) -0.001(3) C17 0.060(5) 0.021(3) 0.035(4) 0.005(3) -0.003(3) -0.009(3) C18 0.144(9) 0.038(5) 0.048(5) 0.018(4) -0.019(5) -0.023(5) C19 0.070(5) 0.042(4) 0.053(5) 0.003(4) -0.008(4) -0.019(4) C21 0.030(4) 0.041(4) 0.036(4) 0.001(3) 0.001(3) 0.002(3) C22 0.045(4) 0.037(4) 0.034(4) -0.005(3) -0.002(3) 0.003(3) C23 0.052(4) 0.044(4) 0.045(4) -0.010(4) 0.004(3) 0.003(4) C24 0.049(4) 0.065(5) 0.043(4) -0.002(4) 0.010(3) 0.000(4) C25 0.045(4) 0.055(5) 0.043(4) -0.005(4) 0.008(3) -0.009(4) C26 0.037(4) 0.042(4) 0.037(4) -0.008(3) 0.000(3) -0.003(3) C27 0.033(4) 0.070(5) 0.040(4) 0.010(4) -0.001(3) 0.011(4) C28 0.119(10) 0.253(18) 0.063(7) 0.008(9) -0.001(6) 0.136(11) C29 0.094(7) 0.128(9) 0.062(6) 0.031(6) -0.037(5) -0.058(7) C31 0.039(4) 0.032(4) 0.042(4) 0.000(3) 0.001(3) -0.010(3) C32 0.051(4) 0.029(4) 0.039(4) -0.001(3) -0.004(3) -0.003(3) C33 0.053(5) 0.034(4) 0.051(5) 0.000(4) 0.006(4) -0.010(3) C34 0.064(5) 0.032(4) 0.062(5) -0.007(4) 0.016(4) -0.012(4) C35 0.052(5) 0.060(5) 0.046(4) -0.006(4) 0.004(4) -0.025(4) C36 0.056(4) 0.034(4) 0.043(4) -0.006(3) -0.002(3) -0.016(3) C37 0.034(4) 0.047(4) 0.040(4) -0.002(3) 0.003(3) -0.007(3) C38 0.043(4) 0.050(5) 0.064(5) 0.000(4) 0.008(4) 0.005(4) C39 0.059(5) 0.063(6) 0.059(5) 0.013(4) 0.021(4) 0.001(4) C41 0.043(4) 0.026(3) 0.014(3) 0.001(3) -0.004(3) 0.000(3) C42 0.083(6) 0.046(5) 0.030(4) 0.006(3) -0.001(4) 0.005(4) C43 0.099(7) 0.075(6) 0.039(4) 0.004(4) 0.011(4) -0.020(5) C44 0.102(8) 0.100(8) 0.054(5) 0.006(5) -0.015(5) -0.037(6) C45 0.236(16) 0.101(9) 0.046(6) -0.012(6) 0.001(7) 0.086(10) C110 0.077(6) 0.047(5) 0.080(6) -0.005(5) 0.010(5) 0.003(4) C131 0.061(5) 0.090(7) 0.047(5) -0.011(5) -0.017(4) 0.005(5) C151 0.071(5) 0.056(5) 0.029(4) -0.005(3) 0.004(4) -0.006(4) C210 0.061(5) 0.057(5) 0.043(4) 0.020(4) -0.007(4) -0.002(4) C231 0.084(6) 0.055(5) 0.046(5) -0.020(4) 0.006(4) 0.002(5) C251 0.071(5) 0.066(5) 0.040(4) 0.005(4) 0.009(4) -0.020(5) C310 0.036(4) 0.081(6) 0.078(6) -0.006(5) -0.002(4) -0.008(4) C331 0.076(6) 0.032(4) 0.077(6) -0.005(4) 0.000(4) 0.000(4) C351 0.092(7) 0.061(5) 0.045(5) -0.017(4) 0.006(4) -0.024(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C41 1.936(6) . ? Mo1 N1 1.972(5) . ? Mo1 N3 1.967(5) . ? Mo1 N2 1.981(5) . ? N1 C11 1.439(8) . ? N1 C17 1.514(8) . ? N2 C27 1.469(8) . ? N2 C21 1.468(8) . ? N3 C31 1.457(8) . ? N3 C37 1.510(8) . ? N4 C41 1.184(8) . ? N4 C42 1.495(9) . ? C11 C12 1.409(9) . ? C11 C16 1.400(9) . ? C12 C13 1.383(10) . ? C13 C14 1.384(10) . ? C13 C131 1.506(10) . ? C14 C15 1.396(10) . ? C15 C16 1.398(9) . ? C15 C151 1.505(10) . ? C17 C110 1.521(10) . ? C17 C18 1.515(9) . ? C17 C19 1.515(10) . ? C21 C26 1.389(9) . ? C21 C22 1.402(9) . ? C22 C23 1.401(9) . ? C23 C24 1.377(10) . ? C23 C231 1.514(10) . ? C24 C25 1.400(10) . ? C25 C26 1.391(9) . ? C25 C251 1.490(10) . ? C27 C28 1.517(12) . ? C27 C29 1.525(12) . ? C27 C210 1.537(10) . ? C31 C32 1.399(9) . ? C31 C36 1.400(9) . ? C32 C33 1.399(10) . ? C33 C34 1.379(10) . ? C33 C331 1.510(10) . ? C34 C35 1.403(11) . ? C35 C36 1.395(10) . ? C35 C351 1.551(10) . ? C37 C39 1.511(10) . ? C37 C38 1.529(10) . ? C37 C310 1.544(10) . ? C42 C45 1.476(12) . ? C42 C43 1.502(11) . ? C42 C44 1.537(12) . ? 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 C41 Mo1 N1 99.9(2) . . ? C41 Mo1 N3 104.4(2) . . ? N1 Mo1 N3 112.1(2) . . ? C41 Mo1 N2 99.6(2) . . ? N1 Mo1 N2 114.7(2) . . ? N3 Mo1 N2 121.9(2) . . ? C11 N1 C17 116.4(5) . . ? C11 N1 Mo1 109.1(4) . . ? C17 N1 Mo1 133.8(4) . . ? C27 N2 C21 114.6(5) . . ? C27 N2 Mo1 134.4(4) . . ? C21 N2 Mo1 110.2(4) . . ? C31 N3 C37 115.2(5) . . ? C31 N3 Mo1 108.0(4) . . ? C37 N3 Mo1 136.5(4) . . ? C41 N4 C42 137.8(7) . . ? C12 C11 C16 118.9(6) . . ? C12 C11 N1 120.7(6) . . ? C16 C11 N1 120.3(6) . . ? C11 C12 C13 121.2(7) . . ? C12 C13 C14 118.6(7) . . ? C12 C13 C131 120.1(7) . . ? C14 C13 C131 121.2(6) . . ? C15 C14 C13 122.2(7) . . ? C14 C15 C16 118.6(6) . . ? C14 C15 C151 121.0(6) . . ? C16 C15 C151 120.4(7) . . ? C11 C16 C15 120.4(6) . . ? N1 C17 C110 109.9(6) . . ? N1 C17 C18 111.1(5) . . ? C110 C17 C18 110.1(7) . . ? N1 C17 C19 108.8(5) . . ? C110 C17 C19 107.7(6) . . ? C18 C17 C19 109.3(6) . . ? C26 C21 C22 120.2(6) . . ? C26 C21 N2 121.0(6) . . ? C22 C21 N2 118.9(6) . . ? C21 C22 C23 118.9(6) . . ? C24 C23 C22 120.0(7) . . ? C24 C23 C231 120.5(7) . . ? C22 C23 C231 119.4(7) . . ? C23 C24 C25 121.7(7) . . ? C24 C25 C26 118.0(7) . . ? C24 C25 C251 121.4(6) . . ? C26 C25 C251 120.6(7) . . ? C21 C26 C25 121.2(6) . . ? N2 C27 C28 112.0(6) . . ? N2 C27 C29 110.7(6) . . ? C28 C27 C29 110.7(9) . . ? N2 C27 C210 108.1(5) . . ? C28 C27 C210 106.8(8) . . ? C29 C27 C210 108.4(6) . . ? C32 C31 C36 120.3(6) . . ? C32 C31 N3 120.2(6) . . ? C36 C31 N3 119.5(6) . . ? C31 C32 C33 121.1(6) . . ? C34 C33 C32 118.0(7) . . ? C34 C33 C331 121.3(7) . . ? C32 C33 C331 120.6(7) . . ? C33 C34 C35 121.9(7) . . ? C34 C35 C36 119.9(7) . . ? C34 C35 C351 121.9(7) . . ? C36 C35 C351 118.2(7) . . ? C31 C36 C35 118.8(7) . . ? N3 C37 C39 112.3(6) . . ? N3 C37 C38 108.0(5) . . ? C39 C37 C38 110.1(6) . . ? N3 C37 C310 108.5(5) . . ? C39 C37 C310 109.7(6) . . ? C38 C37 C310 108.2(6) . . ? N4 C41 Mo1 174.2(5) . . ? C45 C42 N4 106.5(6) . . ? C45 C42 C43 112.2(8) . . ? N4 C42 C43 111.4(6) . . ? C45 C42 C44 108.5(9) . . ? N4 C42 C44 107.9(7) . . ? C43 C42 C44 110.2(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.578 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.086 #===END