data_global _audit_creation_method 'APEX2 v2014.1-1' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_I _chemical_name_systematic ? _chemical_name_common wb27may2 _chemical_formula_moiety ? _chemical_formula_sum 'C33 H39 Mo N P2' _chemical_formula_iupac ? _chemical_formula_weight 607.53 _chemical_absolute_configuration ? _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.3171(7) _cell_length_b 15.3059(11) _cell_length_c 18.2283(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2878.5(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5776 _cell_measurement_theta_min 2.2684 _cell_measurement_theta_max 17.4370 _cell_measurement_temperature 183.(2) _exptl_crystal_description chunk _exptl_crystal_colour 'clear light gold-yellow' _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.94 _exptl_special_details ; ; _diffrn_ambient_temperature 183.(2) _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 11497 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_unetI/netI 0.0300 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 17.44 _diffrn_reflns_theta_full 17.44 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _refine_special_details ; ; _reflns_number_total 1811 _reflns_number_gt 1708 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.0541 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 0.999 _refine_ls_number_reflns 1811 _refine_ls_number_parameters 358 _refine_ls_number_restraints 8 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+1.1041P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.343 _refine_diff_density_min -0.154 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 690 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.03(3) # start Validation Reply Form _vrf_DIFF003_I ; PROBLEM: _diffrn_measurement_device_type is missing RESPONSE: _diffrn_measurement_device_type Bruker D8 Quest ; _vrf_REFNR01_I ; PROBLEM: Ratio of reflections to parameters is < 6 for a RESPONSE: Mo radiation used - max. two theta data for crystal collected ; _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Mo radiation used - max. two theta data for crystal collected ; _vrf_PLAT090_I ; PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........ 2.99 Note RESPONSE: Mo radiation used - max. two theta data for crystal collected ; # end Validation Reply Form 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' P P 0.1023 0.0942 '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' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.0945(12) 0.5130(6) 0.8533(6) 0.020(3) Uani d . . . 1 . . C C2 -0.0251(13) 0.5151(7) 0.8202(6) 0.029(3) Uani d . . . 1 . . H H2 -0.0513 0.4658 0.7922 0.034 Uiso calc U . R 1 . . C C3 -0.1088(10) 0.5844(9) 0.8254(5) 0.031(3) Uani d . . . 1 . . H H3 -0.1908 0.5831 0.8017 0.037 Uiso calc U . R 1 . . C C4 -0.0706(13) 0.6563(7) 0.8659(7) 0.033(3) Uani d . . . 1 . . H H4 -0.1266 0.7053 0.8701 0.039 Uiso calc U . R 1 . . C C5 0.0467(14) 0.6571(6) 0.8998(6) 0.031(3) Uani d . . . 1 . . H H5 0.0713 0.7062 0.9285 0.037 Uiso calc U . R 1 . . C C6 0.1308(9) 0.5868(8) 0.8930(4) 0.027(2) Uani d . . . 1 . . H H6 0.2137 0.589 0.9155 0.032 Uiso calc U . R 1 . . C C7 0.0806(10) 0.3328(7) 0.8543(8) 0.028(3) Uani d . . . 1 . . C C8 0.0405(11) 0.2798(8) 0.7983(7) 0.035(3) Uani d . . . 1 . . H H8 0.078 0.286 0.751 0.042 Uiso calc U . R 1 . . C C9 -0.0548(13) 0.2166(7) 0.8100(8) 0.040(3) Uani d . . . 1 . . H H9 -0.0805 0.1793 0.771 0.048 Uiso calc U . R 1 . . C C10 -0.1106(10) 0.2084(7) 0.8765(10) 0.043(3) Uani d . . . 1 . . H H10 -0.1765 0.1659 0.8837 0.051 Uiso calc U . R 1 . . C C11 -0.0735(12) 0.2607(9) 0.9342(7) 0.047(3) Uani d . . . 1 . . H H11 -0.112 0.2546 0.9813 0.056 Uiso calc U . R 1 . . C C12 0.0222(13) 0.3229(7) 0.9214(7) 0.040(3) Uani d . . . 1 . . H H12 0.048 0.3599 0.9606 0.048 Uiso calc U . R 1 . . C C13 0.3037(9) 0.4082(7) 0.9190(4) 0.032(3) Uani d . . . 1 . . H H13A 0.2911 0.46 0.9508 0.039 Uiso calc U . R 1 . . H H13B 0.2754 0.3561 0.9469 0.039 Uiso calc U . R 1 . . C C14 0.4482(10) 0.3992(8) 0.9011(6) 0.040(3) Uani d . . . 1 . . H H14A 0.4899 0.457 0.9072 0.048 Uiso calc U . R 1 . . H H14B 0.4881 0.3589 0.937 0.048 Uiso calc U . R 1 . . C C15 0.6159(10) 0.3558(7) 0.8152(6) 0.042(3) Uani d . . . 1 . . H H15A 0.6512 0.3165 0.8534 0.051 Uiso calc U . R 1 . . H H15B 0.6594 0.4131 0.8202 0.051 Uiso calc U . R 1 . . C C16 0.6465(9) 0.3177(6) 0.7394(5) 0.035(3) Uani d . . . 1 . . H H16A 0.6353 0.2535 0.7409 0.042 Uiso calc U . R 1 . . H H16B 0.7382 0.33 0.7271 0.042 Uiso calc U . R 1 . . C C17 0.5371(13) 0.2730(6) 0.6023(6) 0.025(3) Uani d . . . 1 . . C C18 0.4311(11) 0.2171(8) 0.6022(6) 0.029(3) Uani d . . . 1 . . H H18 0.3625 0.227 0.6359 0.035 Uiso calc U . R 1 . . C C19 0.4229(12) 0.1472(7) 0.5539(7) 0.039(3) Uani d . . . 1 . . H H19 0.3498 0.1094 0.5549 0.047 Uiso calc U . R 1 . . C C20 0.5215(16) 0.1332(7) 0.5049(6) 0.043(3) Uani d . . . 1 . . H H20 0.5162 0.0857 0.4715 0.052 Uiso calc U . R 1 . . C C21 0.6278(13) 0.1871(9) 0.5036(6) 0.040(3) Uani d . . . 1 . . H H21 0.6958 0.1769 0.4695 0.048 Uiso calc U . R 1 . . C C22 0.6356(12) 0.2563(7) 0.5520(7) 0.036(3) Uani d . . . 1 . . H H22 0.7096 0.2932 0.551 0.043 Uiso calc U . R 1 . . C C23 0.6460(11) 0.4411(5) 0.6202(6) 0.022(2) Uani d . . . 1 . . C C24 0.6131(10) 0.4682(7) 0.5509(7) 0.032(3) Uani d . . . 1 . . H H24 0.5405 0.4424 0.5272 0.039 Uiso calc U . R 1 . . C C25 0.6827(13) 0.5318(8) 0.5149(6) 0.037(3) Uani d . . . 1 . . H H25 0.6591 0.5484 0.4664 0.045 Uiso calc U . R 1 . . C C26 0.7869(13) 0.5716(7) 0.5490(8) 0.047(3) Uani d . . . 1 . . H H26 0.8338 0.6166 0.5248 0.057 Uiso calc U . R 1 . . C C27 0.8210(11) 0.5457(8) 0.6170(9) 0.051(3) Uani d . . . 1 . . H H27 0.8925 0.5724 0.641 0.061 Uiso calc U . R 1 . . C C28 0.7526(13) 0.4807(8) 0.6517(6) 0.043(3) Uani d . . . 1 . . H H28 0.7796 0.4624 0.6991 0.051 Uiso calc U . R 1 . . C C29 0.3739(11) 0.5530(6) 0.7801(6) 0.035(3) Uani d . . D 1 . . H H29A 0.312(6) 0.589(4) 0.755(4) 0.053 Uiso d U . D 1 . . H H29B 0.375(10) 0.559(6) 0.8317(19) 0.053 Uiso d U . D 1 . . C C30 0.4831(11) 0.5354(6) 0.7387(6) 0.036(3) Uani d . . D 1 . . H H30A 0.560(6) 0.527(6) 0.767(5) 0.054 Uiso d U . D 1 . . H H30B 0.490(9) 0.554(5) 0.688(2) 0.054 Uiso d U . D 1 . . C C31 0.1861(12) 0.4745(7) 0.6716(6) 0.032(3) Uani d . . D 1 . . H H31A 0.122(7) 0.428(4) 0.670(5) 0.049 Uiso d U . D 1 . . H H31B 0.161(9) 0.525(4) 0.698(4) 0.049 Uiso d U . D 1 . . C C32 0.2928(11) 0.4703(7) 0.6263(6) 0.034(3) Uani d . . D 1 . . H H32A 0.348(8) 0.519(4) 0.618(5) 0.051 Uiso d U . D 1 . . H H32B 0.297(8) 0.428(5) 0.588(4) 0.051 Uiso d U . D 1 . . C C33 0.3958(10) 0.2949(7) 0.8012(5) 0.040(3) Uani d . . . 1 . . H H33A 0.341 0.2738 0.8414 0.061 Uiso calc U . R 1 . . H H33B 0.4515 0.2473 0.7839 0.061 Uiso calc U . R 1 . . H H33C 0.3409 0.3152 0.7608 0.061 Uiso calc U . R 1 . . Mo Mo1 0.35312(7) 0.41345(5) 0.73627(4) 0.0212(3) Uani d . . . 1 . . N N1 0.4763(8) 0.3671(5) 0.8273(5) 0.026(2) Uani d . . . 1 . . P P1 0.2007(2) 0.41959(18) 0.83633(12) 0.0245(7) Uani d . . . 1 . . P P2 0.5418(3) 0.36322(17) 0.66769(14) 0.0256(8) Uani d . . . 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.016(9) 0.023(8) 0.020(7) 0.003(6) -0.002(6) 0.002(6) C2 0.036(10) 0.023(8) 0.027(7) 0.009(7) 0.005(8) -0.009(5) C3 0.025(7) 0.036(7) 0.032(7) 0.000(9) -0.007(5) -0.014(7) C4 0.021(9) 0.040(10) 0.038(8) 0.014(6) 0.008(7) 0.010(8) C5 0.040(9) 0.018(8) 0.035(8) 0.007(8) 0.011(8) -0.015(5) C6 0.016(6) 0.040(7) 0.025(6) 0.000(9) -0.002(5) -0.014(6) C7 0.031(7) 0.021(7) 0.033(9) 0.007(6) 0.002(8) -0.004(7) C8 0.022(8) 0.023(7) 0.059(10) 0.001(7) 0.008(7) 0.014(8) C9 0.032(8) 0.025(8) 0.063(11) 0.000(7) 0.011(8) -0.001(6) C10 0.019(8) 0.017(7) 0.092(10) 0.000(6) 0.019(9) 0.000(9) C11 0.046(9) 0.030(8) 0.066(11) 0.002(7) 0.029(8) 0.018(9) C12 0.060(9) 0.026(8) 0.035(10) 0.008(8) 0.005(8) -0.001(6) C13 0.039(8) 0.037(6) 0.021(6) 0.011(6) 0.006(5) 0.001(6) C14 0.036(9) 0.049(8) 0.036(8) 0.011(7) -0.008(6) -0.004(7) C15 0.029(10) 0.054(7) 0.044(8) 0.012(7) -0.017(6) 0.009(6) C16 0.021(6) 0.042(6) 0.041(7) 0.009(5) -0.001(7) -0.008(6) C17 0.016(7) 0.020(7) 0.041(8) 0.006(8) -0.001(7) 0.000(6) C18 0.026(9) 0.031(7) 0.030(8) 0.015(7) -0.005(6) -0.007(7) C19 0.046(9) 0.032(9) 0.039(8) -0.002(6) -0.013(8) -0.002(7) C20 0.080(10) 0.022(7) 0.028(8) 0.023(9) -0.008(9) -0.006(6) C21 0.049(10) 0.025(8) 0.046(9) 0.014(8) 0.002(7) 0.007(8) C22 0.037(9) 0.018(8) 0.052(8) 0.011(7) -0.009(9) -0.003(7) C23 0.021(8) 0.031(6) 0.015(7) 0.003(7) 0.005(6) -0.002(6) C24 0.024(7) 0.026(7) 0.046(10) -0.006(6) 0.009(7) -0.002(6) C25 0.047(9) 0.039(7) 0.025(7) 0.014(7) 0.001(8) -0.001(7) C26 0.054(10) 0.049(8) 0.039(9) -0.009(8) 0.017(7) 0.003(8) C27 0.035(9) 0.057(9) 0.060(11) -0.034(8) 0.013(9) -0.014(7) C28 0.030(9) 0.057(9) 0.041(8) -0.013(7) 0.001(8) -0.010(8) C29 0.029(8) 0.030(7) 0.047(8) -0.004(6) -0.004(8) -0.008(6) C30 0.043(8) 0.026(6) 0.039(8) -0.009(6) -0.001(8) 0.000(6) C31 0.040(10) 0.030(8) 0.027(8) 0.002(6) -0.009(7) 0.004(6) C32 0.023(8) 0.042(8) 0.037(8) 0.001(6) -0.008(7) -0.004(7) C33 0.042(8) 0.048(8) 0.032(7) 0.015(7) -0.012(6) 0.013(6) Mo1 0.0189(5) 0.0177(5) 0.0271(5) 0.0016(5) -0.0055(5) -0.0023(4) N1 0.013(6) 0.029(5) 0.036(7) 0.002(5) -0.009(5) -0.003(5) P1 0.0247(16) 0.0210(16) 0.0277(16) -0.0003(16) -0.0024(12) -0.0005(16) P2 0.0187(17) 0.0279(16) 0.0302(19) 0.0036(16) -0.0037(15) -0.0021(14) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 . 1.374(13) ? C1 C6 . 1.392(12) ? C1 P1 . 1.828(10) ? C2 C3 . 1.371(12) ? C2 H2 . 0.95 ? C3 C4 . 1.383(13) ? C3 H3 . 0.95 ? C4 C5 . 1.359(13) ? C4 H4 . 0.95 ? C5 C6 . 1.388(12) ? C5 H5 . 0.95 ? C6 H6 . 0.95 ? C7 C12 . 1.371(13) ? C7 C8 . 1.368(12) ? C7 P1 . 1.846(11) ? C8 C9 . 1.396(13) ? C8 H8 . 0.95 ? C9 C10 . 1.347(14) ? C9 H9 . 0.95 ? C10 C11 . 1.376(14) ? C10 H10 . 0.95 ? C11 C12 . 1.391(13) ? C11 H11 . 0.95 ? C12 H12 . 0.95 ? C13 C14 . 1.533(12) ? C13 P1 . 1.852(8) ? C13 H13A . 0.99 ? C13 H13B . 0.99 ? C14 N1 . 1.460(12) ? C14 H14A . 0.99 ? C14 H14B . 0.99 ? C15 N1 . 1.466(11) ? C15 C16 . 1.533(12) ? C15 H15A . 0.99 ? C15 H15B . 0.99 ? C16 P2 . 1.834(9) ? C16 H16A . 0.99 ? C16 H16B . 0.99 ? C17 C22 . 1.392(13) ? C17 C18 . 1.389(13) ? C17 P2 . 1.825(10) ? C18 C19 . 1.389(13) ? C18 H18 . 0.95 ? C19 C20 . 1.370(13) ? C19 H19 . 0.95 ? C20 C21 . 1.373(13) ? C20 H20 . 0.95 ? C21 C22 . 1.380(12) ? C21 H21 . 0.95 ? C22 H22 . 0.95 ? C23 C24 . 1.373(11) ? C23 C28 . 1.381(13) ? C23 P2 . 1.823(10) ? C24 C25 . 1.376(13) ? C24 H24 . 0.95 ? C25 C26 . 1.384(13) ? C25 H25 . 0.95 ? C26 C27 . 1.349(13) ? C26 H26 . 0.95 ? C27 C28 . 1.373(13) ? C27 H27 . 0.95 ? C28 H28 . 0.95 ? C29 C30 . 1.382(15) ? C29 Mo1 . 2.291(9) ? C29 H29A . 0.96(3) ? C29 H29B . 0.95(3) ? C30 Mo1 . 2.299(9) ? C30 H30A . 0.96(3) ? C30 H30B . 0.97(3) ? C31 C32 . 1.377(15) ? C31 Mo1 . 2.288(10) ? C31 H31A . 0.97(3) ? C31 H31B . 0.94(3) ? C32 Mo1 . 2.272(11) ? C32 H32A . 0.95(3) ? C32 H32B . 0.95(3) ? C33 N1 . 1.463(11) ? C33 Mo1 . 2.211(9) ? C33 H33A . 0.98 ? C33 H33B . 0.98 ? C33 H33C . 0.98 ? Mo1 N1 . 2.207(8) ? Mo1 P1 . 2.410(2) ? Mo1 P2 . 2.438(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 C1 C6 . . 116.8(9) ? C2 C1 P1 . . 118.9(9) ? C6 C1 P1 . . 124.1(10) ? C3 C2 C1 . . 123.7(9) ? C3 C2 H2 . . 118.2 ? C1 C2 H2 . . 118.2 ? C2 C3 C4 . . 118.2(9) ? C2 C3 H3 . . 120.9 ? C4 C3 H3 . . 120.9 ? C5 C4 C3 . . 120.3(10) ? C5 C4 H4 . . 119.9 ? C3 C4 H4 . . 119.9 ? C4 C5 C6 . . 120.6(9) ? C4 C5 H5 . . 119.7 ? C6 C5 H5 . . 119.7 ? C5 C6 C1 . . 120.5(8) ? C5 C6 H6 . . 119.8 ? C1 C6 H6 . . 119.8 ? C12 C7 C8 . . 117.8(10) ? C12 C7 P1 . . 122.2(11) ? C8 C7 P1 . . 119.8(10) ? C7 C8 C9 . . 120.6(10) ? C7 C8 H8 . . 119.7 ? C9 C8 H8 . . 119.7 ? C10 C9 C8 . . 120.2(11) ? C10 C9 H9 . . 119.9 ? C8 C9 H9 . . 119.9 ? C9 C10 C11 . . 121.0(10) ? C9 C10 H10 . . 119.5 ? C11 C10 H10 . . 119.5 ? C10 C11 C12 . . 117.8(10) ? C10 C11 H11 . . 121.1 ? C12 C11 H11 . . 121.1 ? C7 C12 C11 . . 122.5(10) ? C7 C12 H12 . . 118.7 ? C11 C12 H12 . . 118.7 ? C14 C13 P1 . . 113.1(6) ? C14 C13 H13A . . 109.0 ? P1 C13 H13A . . 109.0 ? C14 C13 H13B . . 109.0 ? P1 C13 H13B . . 109.0 ? H13A C13 H13B . . 107.8 ? N1 C14 C13 . . 114.8(8) ? N1 C14 H14A . . 108.6 ? C13 C14 H14A . . 108.6 ? N1 C14 H14B . . 108.6 ? C13 C14 H14B . . 108.6 ? H14A C14 H14B . . 107.5 ? N1 C15 C16 . . 112.5(9) ? N1 C15 H15A . . 109.1 ? C16 C15 H15A . . 109.1 ? N1 C15 H15B . . 109.1 ? C16 C15 H15B . . 109.1 ? H15A C15 H15B . . 107.8 ? C15 C16 P2 . . 112.1(6) ? C15 C16 H16A . . 109.2 ? P2 C16 H16A . . 109.2 ? C15 C16 H16B . . 109.2 ? P2 C16 H16B . . 109.2 ? H16A C16 H16B . . 107.9 ? C22 C17 C18 . . 117.4(9) ? C22 C17 P2 . . 123.4(10) ? C18 C17 P2 . . 119.2(10) ? C19 C18 C17 . . 121.6(10) ? C19 C18 H18 . . 119.2 ? C17 C18 H18 . . 119.2 ? C20 C19 C18 . . 119.2(10) ? C20 C19 H19 . . 120.4 ? C18 C19 H19 . . 120.4 ? C19 C20 C21 . . 120.7(10) ? C19 C20 H20 . . 119.7 ? C21 C20 H20 . . 119.7 ? C20 C21 C22 . . 119.8(10) ? C20 C21 H21 . . 120.1 ? C22 C21 H21 . . 120.1 ? C21 C22 C17 . . 121.3(10) ? C21 C22 H22 . . 119.3 ? C17 C22 H22 . . 119.3 ? C24 C23 C28 . . 116.6(9) ? C24 C23 P2 . . 119.2(10) ? C28 C23 P2 . . 124.0(10) ? C25 C24 C23 . . 121.6(9) ? C25 C24 H24 . . 119.2 ? C23 C24 H24 . . 119.2 ? C24 C25 C26 . . 120.1(10) ? C24 C25 H25 . . 119.9 ? C26 C25 H25 . . 119.9 ? C27 C26 C25 . . 119.1(10) ? C27 C26 H26 . . 120.4 ? C25 C26 H26 . . 120.4 ? C26 C27 C28 . . 120.2(11) ? C26 C27 H27 . . 119.9 ? C28 C27 H27 . . 119.9 ? C27 C28 C23 . . 122.4(10) ? C27 C28 H28 . . 118.8 ? C23 C28 H28 . . 118.8 ? C30 C29 Mo1 . . 72.8(6) ? C30 C29 H29A . . 114.(5) ? Mo1 C29 H29A . . 108.(5) ? C30 C29 H29B . . 124.(7) ? Mo1 C29 H29B . . 116.(5) ? H29A C29 H29B . . 115.(9) ? C29 C30 Mo1 . . 72.2(6) ? C29 C30 H30A . . 114.(6) ? Mo1 C30 H30A . . 113.(6) ? C29 C30 H30B . . 121.(6) ? Mo1 C30 H30B . . 105.(5) ? H30A C30 H30B . . 119.(9) ? C32 C31 Mo1 . . 71.8(6) ? C32 C31 H31A . . 119.(6) ? Mo1 C31 H31A . . 103.(5) ? C32 C31 H31B . . 125.(6) ? Mo1 C31 H31B . . 106.(6) ? H31A C31 H31B . . 115.(8) ? C31 C32 Mo1 . . 73.0(6) ? C31 C32 H32A . . 123.(6) ? Mo1 C32 H32A . . 106.(6) ? C31 C32 H32B . . 121.(6) ? Mo1 C32 H32B . . 112.(6) ? H32A C32 H32B . . 112.(9) ? N1 C33 Mo1 . . 70.5(5) ? N1 C33 H33A . . 109.5 ? Mo1 C33 H33A . . 123.8 ? N1 C33 H33B . . 109.5 ? Mo1 C33 H33B . . 123.7 ? H33A C33 H33B . . 109.5 ? N1 C33 H33C . . 109.5 ? Mo1 C33 H33C . . 38.9 ? H33A C33 H33C . . 109.5 ? H33B C33 H33C . . 109.5 ? N1 Mo1 C33 . . 38.7(3) ? N1 Mo1 C32 . . 160.7(4) ? C33 Mo1 C32 . . 147.2(4) ? N1 Mo1 C29 . . 89.0(4) ? C33 Mo1 C29 . . 124.1(4) ? C32 Mo1 C29 . . 88.6(4) ? N1 Mo1 C31 . . 162.3(4) ? C33 Mo1 C31 . . 139.6(4) ? C32 Mo1 C31 . . 35.2(4) ? C29 Mo1 C31 . . 82.5(4) ? N1 Mo1 C30 . . 84.8(3) ? C33 Mo1 C30 . . 122.7(4) ? C32 Mo1 C30 . . 82.3(4) ? C29 Mo1 C30 . . 35.0(4) ? C31 Mo1 C30 . . 96.8(4) ? N1 Mo1 P1 . . 79.6(2) ? C33 Mo1 P1 . . 75.9(3) ? C32 Mo1 P1 . . 118.3(3) ? C29 Mo1 P1 . . 76.2(3) ? C31 Mo1 P1 . . 83.3(3) ? C30 Mo1 P1 . . 109.5(3) ? N1 Mo1 P2 . . 79.9(2) ? C33 Mo1 P2 . . 81.8(3) ? C32 Mo1 P2 . . 83.5(3) ? C29 Mo1 P2 . . 113.5(3) ? C31 Mo1 P2 . . 117.8(3) ? C30 Mo1 P2 . . 78.5(3) ? P1 Mo1 P2 . . 157.13(9) ? C14 N1 C33 . . 116.2(8) ? C14 N1 C15 . . 111.9(8) ? C33 N1 C15 . . 114.8(8) ? C14 N1 Mo1 . . 118.0(6) ? C33 N1 Mo1 . . 70.8(5) ? C15 N1 Mo1 . . 119.4(6) ? C1 P1 C7 . . 97.5(5) ? C1 P1 C13 . . 106.3(6) ? C7 P1 C13 . . 100.0(5) ? C1 P1 Mo1 . . 123.3(3) ? C7 P1 Mo1 . . 123.0(5) ? C13 P1 Mo1 . . 103.8(3) ? C23 P2 C17 . . 101.5(5) ? C23 P2 C16 . . 103.9(6) ? C17 P2 C16 . . 101.2(4) ? C23 P2 Mo1 . . 120.5(3) ? C17 P2 Mo1 . . 123.5(5) ? C16 P2 Mo1 . . 103.0(3) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . -0.9(14) ? P1 C1 C2 C3 . . . . -175.7(7) ? C1 C2 C3 C4 . . . . 0.1(15) ? C2 C3 C4 C5 . . . . -0.3(14) ? C3 C4 C5 C6 . . . . 1.4(15) ? C4 C5 C6 C1 . . . . -2.2(15) ? C2 C1 C6 C5 . . . . 1.9(13) ? P1 C1 C6 C5 . . . . 176.4(6) ? C12 C7 C8 C9 . . . . -1.3(14) ? P1 C7 C8 C9 . . . . -176.8(7) ? C7 C8 C9 C10 . . . . 1.4(15) ? C8 C9 C10 C11 . . . . -1.1(15) ? C9 C10 C11 C12 . . . . 0.8(15) ? C8 C7 C12 C11 . . . . 1.0(14) ? P1 C7 C12 C11 . . . . 176.4(7) ? C10 C11 C12 C7 . . . . -0.7(14) ? P1 C13 C14 N1 . . . . -23.0(13) ? N1 C15 C16 P2 . . . . 39.5(10) ? C22 C17 C18 C19 . . . . 0.0(13) ? P2 C17 C18 C19 . . . . -179.6(7) ? C17 C18 C19 C20 . . . . -0.4(13) ? C18 C19 C20 C21 . . . . 0.5(14) ? C19 C20 C21 C22 . . . . -0.1(14) ? C20 C21 C22 C17 . . . . -0.3(13) ? C18 C17 C22 C21 . . . . 0.4(13) ? P2 C17 C22 C21 . . . . 179.9(7) ? C28 C23 C24 C25 . . . . -0.2(13) ? P2 C23 C24 C25 . . . . 174.9(7) ? C23 C24 C25 C26 . . . . -1.5(14) ? C24 C25 C26 C27 . . . . 1.6(14) ? C25 C26 C27 C28 . . . . -0.1(15) ? C26 C27 C28 C23 . . . . -1.6(16) ? C24 C23 C28 C27 . . . . 1.7(14) ? P2 C23 C28 C27 . . . . -173.1(8) ? C13 C14 N1 C33 . . . . -42.5(13) ? C13 C14 N1 C15 . . . . -177.0(9) ? C13 C14 N1 Mo1 . . . . 38.6(12) ? Mo1 C33 N1 C14 . . . . 112.5(7) ? Mo1 C33 N1 C15 . . . . -114.3(8) ? C16 C15 N1 C14 . . . . 177.0(8) ? C16 C15 N1 C33 . . . . 41.9(11) ? C16 C15 N1 Mo1 . . . . -39.2(10) ? C2 C1 P1 C7 . . . . -48.8(9) ? C6 C1 P1 C7 . . . . 136.8(9) ? C2 C1 P1 C13 . . . . -151.6(8) ? C6 C1 P1 C13 . . . . 34.1(9) ? C2 C1 P1 Mo1 . . . . 89.2(8) ? C6 C1 P1 Mo1 . . . . -85.1(9) ? C12 C7 P1 C1 . . . . -61.7(9) ? C8 C7 P1 C1 . . . . 113.6(9) ? C12 C7 P1 C13 . . . . 46.3(9) ? C8 C7 P1 C13 . . . . -138.4(8) ? C12 C7 P1 Mo1 . . . . 160.0(6) ? C8 C7 P1 Mo1 . . . . -24.7(9) ? C14 C13 P1 C1 . . . . -131.0(9) ? C14 C13 P1 C7 . . . . 128.1(9) ? C14 C13 P1 Mo1 . . . . 0.3(10) ? C24 C23 P2 C17 . . . . 56.0(8) ? C28 C23 P2 C17 . . . . -129.2(8) ? C24 C23 P2 C16 . . . . 160.8(7) ? C28 C23 P2 C16 . . . . -24.5(9) ? C24 C23 P2 Mo1 . . . . -84.8(7) ? C28 C23 P2 Mo1 . . . . 90.0(8) ? C22 C17 P2 C23 . . . . 26.5(9) ? C18 C17 P2 C23 . . . . -154.0(7) ? C22 C17 P2 C16 . . . . -80.3(8) ? C18 C17 P2 C16 . . . . 99.2(8) ? C22 C17 P2 Mo1 . . . . 165.7(6) ? C18 C17 P2 Mo1 . . . . -14.8(8) ? C15 C16 P2 C23 . . . . 103.5(7) ? C15 C16 P2 C17 . . . . -151.5(8) ? C15 C16 P2 Mo1 . . . . -22.9(7) ? _shelx_res_file ; TITL wb27may2_0m in P2(1)2(1)2(1) CELL 0.71073 10.3171 15.3059 18.2283 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0011 0.0013 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N P Mo UNIT 132 156 4 8 4 L.S. 10 BOND $H CONF ACTA FMAP 2 PLAN 20 SIZE 0.100 0.100 0.120 TEMP -89.860 DFIX 0.95 C29 H29A C29 H29B DFIX 0.95 C30 H30A C30 H30B DFIX 0.95 C31 H31A C31 H31B DFIX 0.95 C32 H32A C32 H32B WGHT 0.035300 1.104100 FVAR 0.39374 C1 1 0.094491 0.513019 0.853262 11.00000 0.01605 0.02303 = 0.02033 0.00152 -0.00190 0.00272 C2 1 -0.025130 0.515141 0.820219 11.00000 0.03650 0.02306 = 0.02650 -0.00941 0.00457 0.00894 AFIX 43 H2 2 -0.051318 0.465837 0.792245 11.00000 -1.20000 AFIX 0 C3 1 -0.108810 0.584422 0.825357 11.00000 0.02493 0.03643 = 0.03200 -0.01446 -0.00750 0.00036 AFIX 43 H3 2 -0.190820 0.583107 0.801684 11.00000 -1.20000 AFIX 0 C4 1 -0.070627 0.656277 0.865929 11.00000 0.02092 0.03975 = 0.03774 0.00990 0.00796 0.01390 AFIX 43 H4 2 -0.126642 0.705285 0.870127 11.00000 -1.20000 AFIX 0 C5 1 0.046659 0.657100 0.899820 11.00000 0.03977 0.01793 = 0.03472 -0.01473 0.01080 0.00657 AFIX 43 H5 2 0.071310 0.706216 0.928466 11.00000 -1.20000 AFIX 0 C6 1 0.130772 0.586798 0.892951 11.00000 0.01574 0.03967 = 0.02523 -0.01413 -0.00182 -0.00003 AFIX 43 H6 2 0.213721 0.589038 0.915499 11.00000 -1.20000 AFIX 0 C7 1 0.080617 0.332780 0.854313 11.00000 0.03115 0.02102 = 0.03304 -0.00429 0.00161 0.00737 C8 1 0.040546 0.279756 0.798293 11.00000 0.02210 0.02347 = 0.05912 0.01363 0.00766 0.00097 AFIX 43 H8 2 0.077983 0.285984 0.750966 11.00000 -1.20000 AFIX 0 C9 1 -0.054812 0.216608 0.810036 11.00000 0.03164 0.02507 = 0.06293 -0.00144 0.01055 0.00008 AFIX 43 H9 2 -0.080492 0.179269 0.771023 11.00000 -1.20000 AFIX 0 C10 1 -0.110562 0.208432 0.876520 11.00000 0.01908 0.01748 = 0.09174 -0.00004 0.01861 0.00024 AFIX 43 H10 2 -0.176462 0.165926 0.883667 11.00000 -1.20000 AFIX 0 C11 1 -0.073492 0.260708 0.934207 11.00000 0.04613 0.02951 = 0.06553 0.01782 0.02870 0.00222 AFIX 43 H11 2 -0.111979 0.254556 0.981270 11.00000 -1.20000 AFIX 0 C12 1 0.022176 0.322859 0.921366 11.00000 0.05960 0.02603 = 0.03536 -0.00083 0.00516 0.00761 AFIX 43 H12 2 0.048041 0.359871 0.960557 11.00000 -1.20000 AFIX 0 C13 1 0.303700 0.408199 0.919017 11.00000 0.03870 0.03660 = 0.02130 0.00078 0.00568 0.01107 AFIX 23 H13A 2 0.291058 0.459976 0.950771 11.00000 -1.20000 H13B 2 0.275374 0.356115 0.946946 11.00000 -1.20000 AFIX 0 C14 1 0.448243 0.399219 0.901052 11.00000 0.03567 0.04916 = 0.03561 -0.00393 -0.00798 0.01106 AFIX 23 H14A 2 0.489924 0.457018 0.907195 11.00000 -1.20000 H14B 2 0.488094 0.358918 0.937050 11.00000 -1.20000 AFIX 0 C15 1 0.615857 0.355822 0.815202 11.00000 0.02891 0.05395 = 0.04401 0.00902 -0.01731 0.01224 AFIX 23 H15A 2 0.651158 0.316517 0.853429 11.00000 -1.20000 H15B 2 0.659433 0.413137 0.820226 11.00000 -1.20000 AFIX 0 C16 1 0.646532 0.317689 0.739414 11.00000 0.02076 0.04213 = 0.04120 -0.00832 -0.00093 0.00906 AFIX 23 H16A 2 0.635347 0.253475 0.740939 11.00000 -1.20000 H16B 2 0.738183 0.330037 0.727113 11.00000 -1.20000 AFIX 0 C17 1 0.537125 0.273015 0.602271 11.00000 0.01581 0.02018 = 0.04051 -0.00019 -0.00101 0.00596 C18 1 0.431075 0.217149 0.602170 11.00000 0.02610 0.03064 = 0.02995 -0.00664 -0.00549 0.01468 AFIX 43 H18 2 0.362465 0.227049 0.635920 11.00000 -1.20000 AFIX 0 C19 1 0.422910 0.147161 0.553921 11.00000 0.04611 0.03189 = 0.03879 -0.00196 -0.01279 -0.00193 AFIX 43 H19 2 0.349842 0.109408 0.554867 11.00000 -1.20000 AFIX 0 C20 1 0.521495 0.133190 0.504923 11.00000 0.08002 0.02160 = 0.02778 -0.00582 -0.00759 0.02251 AFIX 43 H20 2 0.516221 0.085694 0.471506 11.00000 -1.20000 AFIX 0 C21 1 0.627837 0.187138 0.503626 11.00000 0.04927 0.02526 = 0.04636 0.00705 0.00234 0.01422 AFIX 43 H21 2 0.695809 0.176891 0.469537 11.00000 -1.20000 AFIX 0 C22 1 0.635612 0.256262 0.551998 11.00000 0.03714 0.01831 = 0.05211 -0.00253 -0.00937 0.01135 AFIX 43 H22 2 0.709636 0.293158 0.550980 11.00000 -1.20000 AFIX 0 C23 1 0.646009 0.441104 0.620228 11.00000 0.02085 0.03119 = 0.01481 -0.00216 0.00466 0.00342 C24 1 0.613087 0.468190 0.550894 11.00000 0.02418 0.02610 = 0.04602 -0.00166 0.00877 -0.00554 AFIX 43 H24 2 0.540525 0.442409 0.527213 11.00000 -1.20000 AFIX 0 C25 1 0.682654 0.531793 0.514855 11.00000 0.04689 0.03949 = 0.02493 -0.00121 0.00086 0.01434 AFIX 43 H25 2 0.659067 0.548406 0.466447 11.00000 -1.20000 AFIX 0 C26 1 0.786894 0.571585 0.549003 11.00000 0.05436 0.04896 = 0.03869 0.00253 0.01660 -0.00931 AFIX 43 H26 2 0.833835 0.616568 0.524844 11.00000 -1.20000 AFIX 0 C27 1 0.820959 0.545660 0.617035 11.00000 0.03544 0.05682 = 0.06039 -0.01444 0.01322 -0.03400 AFIX 43 H27 2 0.892452 0.572389 0.641016 11.00000 -1.20000 AFIX 0 C28 1 0.752576 0.480733 0.651726 11.00000 0.02997 0.05709 = 0.04145 -0.01035 0.00087 -0.01307 AFIX 43 H28 2 0.779564 0.462412 0.699120 11.00000 -1.20000 AFIX 0 C29 1 0.373932 0.553033 0.780082 11.00000 0.02888 0.03041 = 0.04684 -0.00805 -0.00388 -0.00369 H29A 2 0.311665 0.589231 0.755389 11.00000 -1.50000 H29B 2 0.374712 0.558619 0.831725 11.00000 -1.50000 C30 1 0.483091 0.535403 0.738733 11.00000 0.04349 0.02587 = 0.03859 -0.00026 -0.00140 -0.00855 H30A 2 0.560331 0.527002 0.767024 11.00000 -1.50000 H30B 2 0.490098 0.554108 0.688277 11.00000 -1.50000 C31 1 0.186078 0.474472 0.671583 11.00000 0.04047 0.02999 = 0.02697 0.00394 -0.00868 0.00216 H31A 2 0.122118 0.428190 0.669936 11.00000 -1.50000 H31B 2 0.160661 0.524552 0.698064 11.00000 -1.50000 C32 1 0.292794 0.470258 0.626307 11.00000 0.02293 0.04229 = 0.03746 -0.00354 -0.00775 0.00071 H32A 2 0.348213 0.519143 0.617919 11.00000 -1.50000 H32B 2 0.297485 0.428381 0.587706 11.00000 -1.50000 C33 1 0.395781 0.294876 0.801195 11.00000 0.04160 0.04783 = 0.03200 0.01270 -0.01234 0.01484 AFIX 33 H33A 2 0.340995 0.273798 0.841390 11.00000 -1.50000 H33B 2 0.451499 0.247261 0.783949 11.00000 -1.50000 H33C 2 0.340891 0.315163 0.760759 11.00000 -1.50000 AFIX 0 MO1 5 0.353123 0.413449 0.736274 11.00000 0.01888 0.01772 = 0.02707 -0.00232 -0.00549 0.00165 N1 3 0.476346 0.367149 0.827304 11.00000 0.01266 0.02868 = 0.03574 -0.00281 -0.00899 0.00249 P1 4 0.200692 0.419586 0.836329 11.00000 0.02475 0.02101 = 0.02772 -0.00051 -0.00240 -0.00033 P2 4 0.541825 0.363218 0.667692 11.00000 0.01871 0.02787 = 0.03022 -0.00207 -0.00371 0.00359 HKLF 4 REM wb27may2_0m in P2(1)2(1)2(1) REM R1 = 0.0212 for 1708 Fo > 4sig(Fo) and 0.0244 for all 1811 data REM 358 parameters refined using 8 restraints END WGHT 0.0334 0.8664 REM Highest difference peak 0.343, deepest hole -0.154, 1-sigma level 0.037 Q1 1 0.2802 0.2535 0.7367 11.00000 0.05 0.34 Q2 1 0.2565 0.3383 0.6960 11.00000 0.05 0.26 Q3 1 0.4619 0.2564 0.8624 11.00000 0.05 0.18 Q4 1 0.2477 0.3718 0.7819 11.00000 0.05 0.14 Q5 1 0.0425 0.3557 0.7011 11.00000 0.05 0.13 Q6 1 0.2699 0.5848 0.7582 11.00000 0.05 0.13 Q7 1 0.4277 0.5847 0.6415 11.00000 0.05 0.13 Q8 1 0.4701 0.2286 0.6770 11.00000 0.05 0.12 Q9 1 0.7582 0.2767 0.7182 11.00000 0.05 0.12 Q10 1 0.4019 0.3340 0.6887 11.00000 0.05 0.12 Q11 1 0.1247 0.2566 0.7177 11.00000 0.05 0.12 Q12 1 0.4761 0.3732 0.7185 11.00000 0.05 0.12 Q13 1 0.4389 0.2490 0.7474 11.00000 0.05 0.12 Q14 1 0.6872 0.3380 0.6735 11.00000 0.05 0.12 Q15 1 -0.0253 0.2772 0.7200 11.00000 0.05 0.12 Q16 1 0.4405 0.3551 0.6994 11.00000 0.05 0.12 Q17 1 0.6367 0.4613 0.8395 11.00000 0.05 0.11 Q18 1 0.2819 0.4803 0.7020 11.00000 0.05 0.11 Q19 1 0.4924 0.5618 0.8603 11.00000 0.05 0.11 Q20 1 0.2841 0.4598 0.8018 11.00000 0.05 0.11 ; _shelx_res_checksum 36337 _shelx_hkl_file ; 2 0 0 1401.76 43.00 -2 0 0 1347.37 42.20 3 0 0 1.10 11.50 -3 0 0 2.70 11.10 -3 0 0 0.60 10.10 -4 0 0 2817.22 82.79 4 0 0 2705.13 82.39 4 0 0 2680.83 82.69 -4 0 0 2753.72 82.59 5 0 0 8.70 13.80 5 0 0 -1.60 11.50 -5 0 0 0.50 12.10 -5 0 0 -0.70 12.30 -6 0 0 897.21 53.89 6 0 0 714.13 42.50 6 0 0 745.13 43.60 -6 0 0 679.43 42.10 7 0 0 6.90 18.50 -7 0 0 -6.70 17.00 7 0 0 10.90 16.10 -7 0 0 -8.90 15.70 -8 0 0 13.70 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