# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address C.J.Weiss ;Pacific Northwest National Laboratories P.O. Box 999 Richland, WA 99352 ; A.N.Groves ;Pacific Northwest National Laboratories P.O. Box 999 Richland, WA 99352 ; M.T.Mock ;Pacific Northwest National Laboratories P.O. Box 999 Richland, WA 99352 ; M.L.Helm ;Department of Chemistry Fort Lewis College Durango, CO 81301 ; W.G.Dougherty ;Department of Chemistry Villanova University Villanova, PA 19085 ; ; W.S.Kassel ; ;Department of Chemistry Villanova University Villanova, PA 19085 ; D.L.DuBois ;Pacific Northwest National Laboratories P.O. Box 999 Richland, WA 99352 ; R.M.Bullock ;Pacific Northwest National Laboratories P.O. Box 999 Richland, WA 99352 ; _publ_contact_author_address ;Pacific Northwest National Laboratories P.O. Box 999 Richland, WA 99352 ; _publ_contact_author_email morris.bullock@pnnl.gov _publ_contact_author_phone 5093726589 _publ_contact_author_name 'R. Morris Bullock' #===END data_cis-WCl2(PEtNMePEt)2 _database_code_depnum_ccdc_archive 'CCDC 854188' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common W((PEt2)2NMe1)2(Cl)2 _chemical_melting_point ? _chemical_formula_moiety 'C22 H54 Cl2 N2 P4 W' _chemical_formula_sum 'C11 H27 Cl N P2 W0.5' _chemical_formula_weight 362.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.2599(4) _cell_length_b 15.0108(4) _cell_length_c 17.8358(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.1260(10) _cell_angle_gamma 90.00 _cell_volume 3153.19(17) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9888 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 4.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3763 _exptl_absorpt_correction_T_max 0.3763 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19912 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0142 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.16 _reflns_number_total 3487 _reflns_number_gt 3431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0132P)^2^+4.6140P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3487 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0136 _refine_ls_R_factor_gt 0.0133 _refine_ls_wR_factor_ref 0.0330 _refine_ls_wR_factor_gt 0.0328 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.0000 0.181337(6) 0.2500 0.00911(3) Uani 1 2 d S . . Cl1 Cl 0.13569(4) 0.31016(3) 0.26014(3) 0.01944(9) Uani 1 1 d . . . P1 P 0.02366(4) 0.20135(3) 0.39189(3) 0.01254(9) Uani 1 1 d . . . P2 P 0.18172(4) 0.11094(3) 0.25684(3) 0.01412(9) Uani 1 1 d . . . N1 N -0.18116(13) 0.13575(10) 0.39897(9) 0.0169(3) Uani 1 1 d . . . C1 C -0.10910(15) 0.21517(12) 0.41978(11) 0.0167(3) Uani 1 1 d . . . H1A H -0.0911 0.2255 0.4767 0.020 Uiso 1 1 calc R . . H1B H -0.1507 0.2679 0.3929 0.020 Uiso 1 1 calc R . . C2 C 0.25327(15) 0.14092(13) 0.18152(11) 0.0182(4) Uani 1 1 d . . . H2A H 0.2828 0.2024 0.1916 0.022 Uiso 1 1 calc R . . H2B H 0.3191 0.1008 0.1870 0.022 Uiso 1 1 calc R . . C3 C -0.25299(18) 0.12629(15) 0.45164(12) 0.0276(4) Uani 1 1 d . . . H3A H -0.3041 0.1776 0.4456 0.041 Uiso 1 1 calc R . . H3B H -0.2051 0.1234 0.5057 0.041 Uiso 1 1 calc R . . H3C H -0.2979 0.0715 0.4390 0.041 Uiso 1 1 calc R . . C4 C 0.10568(17) 0.29669(12) 0.44303(12) 0.0219(4) Uani 1 1 d . . . H4A H 0.1208 0.2869 0.4999 0.026 Uiso 1 1 calc R . . H4B H 0.1799 0.2977 0.4312 0.026 Uiso 1 1 calc R . . C5 C 0.0501(2) 0.38800(13) 0.42323(13) 0.0300(5) Uani 1 1 d . . . H5A H 0.0326 0.3982 0.3669 0.045 Uiso 1 1 calc R . . H5B H 0.1023 0.4343 0.4509 0.045 Uiso 1 1 calc R . . H5C H -0.0201 0.3901 0.4392 0.045 Uiso 1 1 calc R . . C6 C 0.08908(17) 0.10828(12) 0.45581(11) 0.0201(4) Uani 1 1 d . . . H6A H 0.0533 0.0526 0.4309 0.024 Uiso 1 1 calc R . . H6B H 0.1701 0.1058 0.4566 0.024 Uiso 1 1 calc R . . C7 C 0.08424(19) 0.10716(14) 0.54021(11) 0.0257(4) Uani 1 1 d . . . H7A H 0.1194 0.1615 0.5666 0.039 Uiso 1 1 calc R . . H7B H 0.1253 0.0550 0.5669 0.039 Uiso 1 1 calc R . . H7C H 0.0049 0.1043 0.5414 0.039 Uiso 1 1 calc R . . C8 C 0.18433(18) -0.01065(13) 0.24813(12) 0.0251(4) Uani 1 1 d . . . H8A H 0.1276 -0.0280 0.1991 0.030 Uiso 1 1 calc R . . H8B H 0.2599 -0.0283 0.2434 0.030 Uiso 1 1 calc R . . C9 C 0.1606(2) -0.06374(14) 0.31499(14) 0.0356(5) Uani 1 1 d . . . H9A H 0.2171 -0.0484 0.3640 0.053 Uiso 1 1 calc R . . H9B H 0.1651 -0.1276 0.3048 0.053 Uiso 1 1 calc R . . H9C H 0.0845 -0.0493 0.3190 0.053 Uiso 1 1 calc R . . C10 C 0.30009(16) 0.13310(16) 0.34432(12) 0.0268(4) Uani 1 1 d . . . H10A H 0.3008 0.1978 0.3551 0.032 Uiso 1 1 calc R . . H10B H 0.2830 0.1024 0.3889 0.032 Uiso 1 1 calc R . . C11 C 0.41980(19) 0.1063(2) 0.34350(14) 0.0474(7) Uani 1 1 d . . . H11A H 0.4198 0.0439 0.3273 0.071 Uiso 1 1 calc R . . H11B H 0.4717 0.1135 0.3959 0.071 Uiso 1 1 calc R . . H11C H 0.4448 0.1443 0.3068 0.071 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 W1 0.01000(5) 0.00826(5) 0.00910(5) 0.000 0.00269(3) 0.000 Cl1 0.0228(2) 0.01543(19) 0.0226(2) -0.00361(16) 0.01038(18) -0.00827(15) P1 0.0142(2) 0.01272(19) 0.0109(2) -0.00129(15) 0.00381(16) -0.00111(15) P2 0.0135(2) 0.0178(2) 0.0113(2) 0.00148(16) 0.00389(17) 0.00456(16) N1 0.0174(7) 0.0207(7) 0.0146(7) -0.0019(6) 0.0077(6) -0.0038(6) C1 0.0175(8) 0.0182(8) 0.0160(9) -0.0033(7) 0.0070(7) -0.0002(7) C2 0.0141(8) 0.0257(9) 0.0164(9) 0.0023(7) 0.0067(7) 0.0027(7) C3 0.0278(10) 0.0399(12) 0.0198(10) -0.0018(8) 0.0144(8) -0.0083(9) C4 0.0260(10) 0.0211(9) 0.0179(9) -0.0063(7) 0.0048(8) -0.0086(7) C5 0.0442(13) 0.0171(9) 0.0302(11) -0.0077(8) 0.0127(10) -0.0070(8) C6 0.0234(9) 0.0226(9) 0.0148(9) 0.0037(7) 0.0061(7) 0.0046(7) C7 0.0329(11) 0.0291(10) 0.0159(9) 0.0046(8) 0.0080(8) -0.0002(8) C8 0.0356(11) 0.0187(9) 0.0259(11) 0.0054(8) 0.0169(9) 0.0131(8) C9 0.0554(15) 0.0218(10) 0.0385(13) 0.0132(9) 0.0279(12) 0.0169(10) C10 0.0151(9) 0.0471(13) 0.0166(10) 0.0001(9) 0.0017(7) 0.0054(8) C11 0.0168(10) 0.098(2) 0.0254(12) 0.0057(13) 0.0027(9) 0.0163(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 P2 2.4380(4) . ? W1 P2 2.4381(4) 2 ? W1 P1 2.4842(4) . ? W1 P1 2.4842(4) 2 ? W1 Cl1 2.5244(4) . ? W1 Cl1 2.5244(4) 2 ? P1 C4 1.8389(19) . ? P1 C6 1.8404(19) . ? P1 C1 1.8411(18) . ? P2 C8 1.8328(19) . ? P2 C10 1.842(2) . ? P2 C2 1.8523(18) . ? N1 C3 1.462(2) . ? N1 C2 1.464(2) 2 ? N1 C1 1.469(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N1 1.464(2) 2 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.528(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.523(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.528(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.526(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? 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 P2 W1 P2 128.63(2) . 2 ? P2 W1 P1 98.914(15) . . ? P2 W1 P1 87.129(14) 2 . ? P2 W1 P1 87.127(14) . 2 ? P2 W1 P1 98.914(15) 2 2 ? P1 W1 P1 166.11(2) . 2 ? P2 W1 Cl1 75.735(15) . . ? P2 W1 Cl1 155.570(15) 2 . ? P1 W1 Cl1 86.917(14) . . ? P1 W1 Cl1 82.443(15) 2 . ? P2 W1 Cl1 155.570(15) . 2 ? P2 W1 Cl1 75.735(15) 2 2 ? P1 W1 Cl1 82.443(15) . 2 ? P1 W1 Cl1 86.918(14) 2 2 ? Cl1 W1 Cl1 80.00(2) . 2 ? C4 P1 C6 101.50(9) . . ? C4 P1 C1 100.43(9) . . ? C6 P1 C1 100.60(9) . . ? C4 P1 W1 119.50(7) . . ? C6 P1 W1 116.54(6) . . ? C1 P1 W1 115.28(6) . . ? C8 P2 C10 102.91(10) . . ? C8 P2 C2 99.07(9) . . ? C10 P2 C2 98.63(9) . . ? C8 P2 W1 117.69(7) . . ? C10 P2 W1 117.26(7) . . ? C2 P2 W1 117.95(6) . . ? C3 N1 C2 109.13(15) . 2 ? C3 N1 C1 110.11(15) . . ? C2 N1 C1 111.21(14) 2 . ? N1 C1 P1 110.80(12) . . ? N1 C1 H1A 109.5 . . ? P1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N1 C2 P2 114.81(12) 2 . ? N1 C2 H2A 108.6 2 . ? P2 C2 H2A 108.6 . . ? N1 C2 H2B 108.6 2 . ? P2 C2 H2B 108.6 . . ? H2A C2 H2B 107.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 P1 115.87(14) . . ? C5 C4 H4A 108.3 . . ? P1 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? P1 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 P1 119.39(14) . . ? C7 C6 H6A 107.5 . . ? P1 C6 H6A 107.5 . . ? C7 C6 H6B 107.5 . . ? P1 C6 H6B 107.5 . . ? H6A C6 H6B 107.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 P2 116.22(14) . . ? C9 C8 H8A 108.2 . . ? P2 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? P2 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P2 118.55(16) . . ? C11 C10 H10A 107.7 . . ? P2 C10 H10A 107.7 . . ? C11 C10 H10B 107.7 . . ? P2 C10 H10B 107.7 . . ? H10A C10 H10B 107.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.16 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.803 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.066 #===END data_trans-W(N2)2(dppp)2_(14) _database_code_depnum_ccdc_archive 'CCDC 854189' _audit_creation_date 2011-03-11 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C27 H26 N2 P2 W0.5), 2(C4 H6.487 O)' _chemical_formula_sum 'C62 H64.97 N4 O2 P4 W' _chemical_formula_weight 1205.88 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 9.9919(5) _cell_length_b 15.5200(8) _cell_length_c 17.6634(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.533(3) _cell_angle_gamma 90.00 _cell_volume 2715.5(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9900 _cell_measurement_temperature 373.1(10) _cell_measurement_theta_max 29.57 _cell_measurement_theta_min 2.58 _exptl_absorpt_coefficient_mu 2.293 _exptl_absorpt_correction_T_max 0.8031 _exptl_absorpt_correction_T_min 0.7248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1230 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_special_details 'SADABS; (Sheldrick, 2006)' _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 61951 _diffrn_reflns_theta_full 29.65 _diffrn_reflns_theta_max 29.65 _diffrn_reflns_theta_min 1.75 _diffrn_ambient_temperature 373.1(10) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 5685 _reflns_number_total 7635 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 2.053 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.108 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 350 _refine_ls_number_reflns 7635 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0269 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+2.9615P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.0661 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 W1 W 0.0000 0.5000 0.0000 0.00990(4) Uani 1 2 d S . . P1 P -0.03428(7) 0.61248(4) 0.09444(4) 0.01303(13) Uani 1 1 d . . . P2 P -0.01269(6) 0.39707(4) 0.10616(4) 0.01227(13) Uani 1 1 d . . . N1 N 0.1923(2) 0.50963(12) 0.04689(12) 0.0140(4) Uani 1 1 d . . . N2 N 0.2979(2) 0.51534(14) 0.07768(14) 0.0216(5) Uani 1 1 d . . . C1 C 0.0342(3) 0.72163(16) 0.08268(15) 0.0192(6) Uani 1 1 d . . . C2 C 0.1644(3) 0.72867(17) 0.06378(16) 0.0223(6) Uani 1 1 d . . . H2 H 0.2115 0.6793 0.0534 0.027 Uiso 1 1 calc R . . C3 C 0.2249(3) 0.8088(2) 0.06026(19) 0.0326(7) Uani 1 1 d . . . H3 H 0.3129 0.8128 0.0486 0.039 Uiso 1 1 calc R . . C4 C 0.1548(4) 0.8827(2) 0.0740(2) 0.0408(9) Uani 1 1 d . . . H4 H 0.1950 0.9364 0.0709 0.049 Uiso 1 1 calc R . . C5 C 0.0259(4) 0.87681(19) 0.09211(19) 0.0373(8) Uani 1 1 d . . . H5 H -0.0212 0.9267 0.1010 0.045 Uiso 1 1 calc R . . C6 C -0.0352(4) 0.79658(18) 0.09735(17) 0.0276(7) Uani 1 1 d . . . H6 H -0.1221 0.7930 0.1106 0.033 Uiso 1 1 calc R . . C7 C -0.3105(3) 0.63782(17) 0.05736(16) 0.0202(5) Uani 1 1 d . . . H7 H -0.2928 0.6267 0.0079 0.024 Uiso 1 1 calc R . . C8 C -0.4414(3) 0.6551(2) 0.07000(17) 0.0271(6) Uani 1 1 d . . . H8 H -0.5104 0.6554 0.0292 0.033 Uiso 1 1 calc R . . C9 C -0.4699(3) 0.6719(2) 0.14258(18) 0.0333(8) Uani 1 1 d . . . H9 H -0.5580 0.6832 0.1512 0.040 Uiso 1 1 calc R . . C10 C -0.3667(3) 0.6718(2) 0.20221(19) 0.0374(8) Uani 1 1 d . . . H10 H -0.3855 0.6835 0.2514 0.045 Uiso 1 1 calc R . . C11 C -0.2347(3) 0.6544(2) 0.19017(17) 0.0274(6) Uani 1 1 d . . . H11 H -0.1662 0.6545 0.2312 0.033 Uiso 1 1 calc R . . C12 C -0.2043(3) 0.63666(16) 0.11710(16) 0.0166(5) Uani 1 1 d . . . C13 C 0.0610(3) 0.59557(16) 0.19030(15) 0.0161(5) Uani 1 1 d . . . H13A H 0.1565 0.5954 0.1854 0.019 Uiso 1 1 calc R . . H13B H 0.0444 0.6444 0.2221 0.019 Uiso 1 1 calc R . . C14 C 0.0287(3) 0.51318(15) 0.23182(14) 0.0166(5) Uani 1 1 d . . . H14A H 0.0668 0.5178 0.2851 0.020 Uiso 1 1 calc R . . H14B H -0.0685 0.5083 0.2299 0.020 Uiso 1 1 calc R . . C15 C 0.0822(3) 0.43152(16) 0.19864(15) 0.0156(5) Uani 1 1 d . . . H15A H 0.0799 0.3852 0.2353 0.019 Uiso 1 1 calc R . . H15B H 0.1758 0.4407 0.1916 0.019 Uiso 1 1 calc R . . C16 C -0.1737(3) 0.37071(16) 0.14061(15) 0.0161(5) Uani 1 1 d . . . C17 C -0.1794(3) 0.31429(18) 0.20160(16) 0.0216(6) Uani 1 1 d . . . H17 H -0.1009 0.2874 0.2241 0.026 Uiso 1 1 calc R . . C18 C -0.2997(3) 0.2980(2) 0.22897(17) 0.0281(7) Uani 1 1 d . . . H18 H -0.3021 0.2596 0.2692 0.034 Uiso 1 1 calc R . . C19 C -0.4168(3) 0.3383(2) 0.19688(18) 0.0283(7) Uani 1 1 d . . . H19 H -0.4981 0.3268 0.2152 0.034 Uiso 1 1 calc R . . C20 C -0.4125(3) 0.3956(2) 0.13736(17) 0.0255(6) Uani 1 1 d . . . H20 H -0.4908 0.4236 0.1161 0.031 Uiso 1 1 calc R . . C21 C -0.2917(3) 0.41151(18) 0.10932(16) 0.0199(5) Uani 1 1 d . . . H21 H -0.2897 0.4499 0.0691 0.024 Uiso 1 1 calc R . . C22 C 0.0687(3) 0.29031(16) 0.10400(14) 0.0157(5) Uani 1 1 d . . . C23 C -0.0005(3) 0.21231(17) 0.09765(16) 0.0197(6) Uani 1 1 d . . . H23 H -0.0939 0.2117 0.0961 0.024 Uiso 1 1 calc R . . C24 C 0.0691(3) 0.13524(18) 0.09367(17) 0.0267(7) Uani 1 1 d . . . H24 H 0.0218 0.0834 0.0904 0.032 Uiso 1 1 calc R . . C25 C 0.2066(3) 0.13466(19) 0.09445(18) 0.0294(7) Uani 1 1 d . . . H25 H 0.2520 0.0828 0.0908 0.035 Uiso 1 1 calc R . . C26 C 0.2774(3) 0.21122(18) 0.10059(17) 0.0252(6) Uani 1 1 d . . . H26 H 0.3706 0.2112 0.1011 0.030 Uiso 1 1 calc R . . C27 C 0.2090(3) 0.28836(17) 0.10603(15) 0.0181(5) Uani 1 1 d . . . H27 H 0.2574 0.3397 0.1111 0.022 Uiso 1 1 calc R . . O1S O 0.2897(4) 0.5091(2) 0.4207(3) 0.0956(15) Uani 1 1 d . . . C1S C 0.3416(11) 0.4319(7) 0.3997(7) 0.044(3) Uani 0.513(14) 1 d P A 1 H1S H 0.3036 0.3773 0.4011 0.053 Uiso 0.513(14) 1 calc PR A 1 C2S C 0.4733(10) 0.4561(6) 0.3740(5) 0.042(3) Uani 0.513(14) 1 d P A 1 H2SA H 0.5401 0.4729 0.4163 0.051 Uiso 0.513(14) 1 calc PR A 1 H2SB H 0.5092 0.4103 0.3451 0.051 Uiso 0.513(14) 1 calc PR A 1 C1S' C 0.3862(15) 0.4310(8) 0.4322(8) 0.056(3) Uani 0.487(14) 1 d P A 2 H1SA H 0.4700 0.4442 0.4644 0.067 Uiso 0.487(14) 1 calc PR A 2 H1SB H 0.3441 0.3807 0.4516 0.067 Uiso 0.487(14) 1 calc PR A 2 C2S' C 0.4038(12) 0.4225(7) 0.3498(5) 0.049(3) Uani 0.487(14) 1 d P A 2 H2SC H 0.3241 0.3984 0.3200 0.059 Uiso 0.487(14) 1 calc PR A 2 H2SD H 0.4818 0.3876 0.3430 0.059 Uiso 0.487(14) 1 calc PR A 2 C3S C 0.4271(5) 0.5277(4) 0.3269(3) 0.0695(15) Uani 1 1 d . . . H3SA H 0.3730 0.5094 0.2800 0.083 Uiso 0.513(14) 1 calc PR A 1 H3SB H 0.5014 0.5631 0.3147 0.083 Uiso 0.513(14) 1 calc PR A 1 H3SC H 0.5214 0.5440 0.3372 0.083 Uiso 0.487(14) 1 calc PR A 2 H3SD H 0.3943 0.5391 0.2737 0.083 Uiso 0.487(14) 1 calc PR A 2 C4S C 0.3445(5) 0.5729(3) 0.3786(3) 0.0720(15) Uani 1 1 d . A . H4S H 0.3319 0.6321 0.3821 0.086 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 W1 0.01278(6) 0.00562(6) 0.01118(6) 0.00016(6) 0.00115(4) -0.00001(6) P1 0.0171(3) 0.0083(3) 0.0137(3) -0.0014(2) 0.0021(2) -0.0006(2) P2 0.0157(3) 0.0080(3) 0.0132(3) 0.0017(2) 0.0020(2) 0.0004(2) N1 0.0204(10) 0.0078(10) 0.0144(9) 0.0014(8) 0.0046(8) 0.0012(8) N2 0.0203(11) 0.0204(13) 0.0234(12) 0.0018(9) 0.0002(9) 0.0002(9) C1 0.0322(15) 0.0092(11) 0.0150(13) -0.0016(10) -0.0010(11) -0.0043(10) C2 0.0302(15) 0.0145(13) 0.0198(14) 0.0022(10) -0.0048(12) -0.0049(11) C3 0.0401(18) 0.0233(15) 0.0320(18) 0.0044(13) -0.0046(14) -0.0151(13) C4 0.073(3) 0.0142(15) 0.0330(19) -0.0004(13) -0.0024(18) -0.0202(16) C5 0.072(3) 0.0073(13) 0.0317(18) -0.0035(12) 0.0046(17) -0.0031(14) C6 0.0491(19) 0.0125(13) 0.0217(15) -0.0027(11) 0.0067(13) 0.0016(13) C7 0.0238(13) 0.0185(13) 0.0181(13) -0.0039(10) 0.0023(11) 0.0039(11) C8 0.0246(14) 0.0349(17) 0.0212(15) -0.0066(13) 0.0003(11) 0.0066(12) C9 0.0239(15) 0.049(2) 0.0273(17) -0.0097(15) 0.0063(13) 0.0102(14) C10 0.0379(18) 0.056(2) 0.0191(15) -0.0111(15) 0.0071(14) 0.0161(16) C11 0.0309(15) 0.0345(17) 0.0161(14) -0.0064(12) -0.0001(12) 0.0093(13) C12 0.0211(13) 0.0112(12) 0.0179(13) -0.0031(10) 0.0043(10) 0.0035(10) C13 0.0205(12) 0.0118(12) 0.0152(12) -0.0017(10) 0.0000(10) -0.0013(10) C14 0.0228(12) 0.0144(14) 0.0120(11) -0.0006(9) 0.0003(9) 0.0011(9) C15 0.0202(13) 0.0103(12) 0.0158(13) 0.0023(10) 0.0006(10) 0.0000(10) C16 0.0189(12) 0.0128(12) 0.0169(13) -0.0013(10) 0.0036(10) -0.0022(10) C17 0.0266(14) 0.0177(13) 0.0205(14) 0.0050(11) 0.0033(11) -0.0002(11) C18 0.0375(17) 0.0273(16) 0.0210(15) 0.0060(12) 0.0097(13) -0.0054(13) C19 0.0267(15) 0.0337(17) 0.0266(16) -0.0026(13) 0.0110(13) -0.0096(13) C20 0.0198(13) 0.0312(16) 0.0258(15) 0.0008(13) 0.0046(11) 0.0009(12) C21 0.0228(13) 0.0186(13) 0.0185(13) 0.0027(10) 0.0033(11) -0.0019(10) C22 0.0269(14) 0.0094(11) 0.0105(12) 0.0018(9) 0.0017(10) 0.0023(10) C23 0.0289(14) 0.0128(12) 0.0176(13) 0.0011(10) 0.0035(11) -0.0011(11) C24 0.0499(19) 0.0089(12) 0.0212(15) -0.0001(11) 0.0037(13) -0.0012(12) C25 0.0465(19) 0.0156(14) 0.0260(16) 0.0009(12) 0.0038(14) 0.0131(13) C26 0.0310(15) 0.0217(14) 0.0228(15) 0.0005(12) 0.0030(12) 0.0096(12) C27 0.0243(13) 0.0124(12) 0.0172(13) 0.0012(10) 0.0017(10) 0.0017(10) O1S 0.105(3) 0.067(3) 0.133(4) -0.013(2) 0.084(3) 0.001(2) C1S 0.048(6) 0.035(4) 0.051(7) 0.016(5) 0.011(5) -0.006(4) C2S 0.042(5) 0.042(5) 0.044(5) -0.010(4) 0.010(4) 0.010(4) C1S' 0.076(9) 0.052(6) 0.039(7) -0.005(5) 0.004(5) 0.002(6) C2S' 0.054(6) 0.061(6) 0.030(5) 0.000(4) 0.000(4) 0.006(5) C3S 0.050(3) 0.107(4) 0.051(3) 0.030(3) 0.004(2) -0.009(3) C4S 0.078(3) 0.042(3) 0.100(4) -0.010(3) 0.025(3) -0.011(2) _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 W1 P1 2.4692(7) . ? W1 P1 2.4691(7) 3_565 ? W1 P2 2.4792(6) . ? W1 P2 2.4793(6) 3_565 ? W1 N1 1.996(2) 3_565 ? W1 N1 1.996(2) . ? P1 C1 1.849(3) . ? P1 C12 1.835(3) . ? P1 C13 1.849(3) . ? P2 C15 1.857(3) . ? P2 C16 1.839(3) . ? P2 C22 1.848(3) . ? N1 N2 1.125(3) . ? C1 C2 1.389(4) . ? C1 C6 1.396(4) . ? C2 C3 1.388(4) . ? C3 C4 1.381(5) . ? C4 C5 1.370(5) . ? C5 C6 1.395(4) . ? C7 C8 1.381(4) . ? C7 C12 1.395(4) . ? C8 C9 1.374(4) . ? C9 C10 1.374(4) . ? C10 C11 1.390(4) . ? C11 C12 1.392(4) . ? C13 C14 1.529(3) . ? C14 C15 1.523(3) . ? C16 C17 1.395(4) . ? C16 C21 1.388(4) . ? C17 C18 1.376(4) . ? C18 C19 1.381(4) . ? C19 C20 1.383(4) . ? C20 C21 1.385(4) . ? C22 C23 1.391(4) . ? C22 C27 1.397(4) . ? C23 C24 1.390(4) . ? C24 C25 1.373(5) . ? C25 C26 1.380(4) . ? C26 C27 1.388(4) . ? O1S C1S 1.377(12) . ? O1S C1S' 1.547(15) . ? O1S C4S 1.393(6) . ? C1S C2S 1.495(14) . ? C2S C3S 1.428(9) . ? C1S' C2S' 1.495(16) . ? C2S' C3S 1.705(12) . ? C3S C4S 1.485(7) . ? 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 P1 W1 P1 180.00(3) 3_565 . ? P1 W1 P2 85.37(2) . . ? P1 W1 P2 94.63(2) 3_565 . ? P1 W1 P2 94.64(2) . 3_565 ? P1 W1 P2 85.37(2) 3_565 3_565 ? P2 W1 P2 180.0 . 3_565 ? N1 W1 P1 97.01(6) 3_565 . ? N1 W1 P1 97.01(6) . 3_565 ? N1 W1 P1 82.99(6) 3_565 3_565 ? N1 W1 P1 82.99(6) . . ? N1 W1 P2 97.11(6) 3_565 . ? N1 W1 P2 97.11(6) . 3_565 ? N1 W1 P2 82.89(6) 3_565 3_565 ? N1 W1 P2 82.89(6) . . ? N1 W1 N1 180.0 3_565 . ? C1 P1 W1 119.06(9) . . ? C1 P1 C13 94.54(12) . . ? C12 P1 W1 120.43(9) . . ? C12 P1 C1 101.78(12) . . ? C12 P1 C13 102.08(12) . . ? C13 P1 W1 114.71(9) . . ? C15 P2 W1 114.14(8) . . ? C16 P2 W1 121.82(9) . . ? C16 P2 C15 98.11(12) . . ? C16 P2 C22 102.35(12) . . ? C22 P2 W1 119.71(9) . . ? C22 P2 C15 95.79(11) . . ? N2 N1 W1 175.6(2) . . ? C2 C1 P1 118.1(2) . . ? C2 C1 C6 118.9(3) . . ? C6 C1 P1 122.9(2) . . ? C3 C2 C1 120.6(3) . . ? C4 C3 C2 120.1(3) . . ? C5 C4 C3 120.0(3) . . ? C4 C5 C6 120.5(3) . . ? C5 C6 C1 119.9(3) . . ? C8 C7 C12 121.5(3) . . ? C9 C8 C7 120.3(3) . . ? C10 C9 C8 119.2(3) . . ? C9 C10 C11 121.0(3) . . ? C10 C11 C12 120.5(3) . . ? C7 C12 P1 118.2(2) . . ? C11 C12 P1 124.3(2) . . ? C11 C12 C7 117.5(3) . . ? C14 C13 P1 116.24(18) . . ? C15 C14 C13 113.9(2) . . ? C14 C15 P2 114.44(17) . . ? C17 C16 P2 121.4(2) . . ? C21 C16 P2 120.1(2) . . ? C21 C16 C17 118.4(2) . . ? C18 C17 C16 120.8(3) . . ? C17 C18 C19 120.3(3) . . ? C18 C19 C20 119.7(3) . . ? C19 C20 C21 120.1(3) . . ? C20 C21 C16 120.7(3) . . ? C23 C22 P2 124.5(2) . . ? C23 C22 C27 118.0(2) . . ? C27 C22 P2 117.48(19) . . ? C24 C23 C22 120.4(3) . . ? C25 C24 C23 120.8(3) . . ? C24 C25 C26 119.8(3) . . ? C25 C26 C27 119.7(3) . . ? C26 C27 C22 121.2(3) . . ? C1S O1S C1S' 26.1(5) . . ? C1S O1S C4S 106.6(5) . . ? C4S O1S C1S' 110.2(6) . . ? O1S C1S C2S 103.9(8) . . ? C3S C2S C1S 98.1(7) . . ? C2S' C1S' O1S 95.3(9) . . ? C1S' C2S' C3S 100.6(8) . . ? C2S C3S C2S' 32.9(4) . . ? C2S C3S C4S 100.0(5) . . ? C4S C3S C2S' 101.7(5) . . ? O1S C4S C3S 106.4(4) . . ? #===END data_trans-W(N2)2(dppe)(PEtNMePEt)_(9) _database_code_depnum_ccdc_archive 'CCDC 854190' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H102 N10 P8 W2' _chemical_formula_weight 1747.12 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' W W -0.8490 6.8722 '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 10.3311(5) _cell_length_b 19.3128(9) _cell_length_c 20.2295(10) _cell_angle_alpha 109.1660(10) _cell_angle_beta 94.039(2) _cell_angle_gamma 100.228(2) _cell_volume 3715.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 33.20 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 3.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5868 _exptl_absorpt_correction_T_max 0.7774 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 79213 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 33.35 _reflns_number_total 28417 _reflns_number_gt 21888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0225P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28417 _refine_ls_number_parameters 857 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.637317(8) 0.046154(4) 0.810235(4) 0.01105(2) Uani 1 1 d . . . W2 W 0.672982(7) 0.555590(4) 0.313503(4) 0.01000(2) Uani 1 1 d . . . N1 N 0.26521(17) -0.01601(10) 0.84807(9) 0.0163(4) Uani 1 1 d . . . N2 N 0.58505(17) 0.09707(10) 0.74287(9) 0.0158(3) Uani 1 1 d . . . N3 N 0.5526(2) 0.12328(12) 0.70393(11) 0.0258(4) Uani 1 1 d . . . N4 N 0.66836(17) -0.00887(10) 0.87674(9) 0.0148(3) Uani 1 1 d . . . N5 N 0.67863(19) -0.04099(11) 0.91375(10) 0.0218(4) Uani 1 1 d . . . N6 N 0.31916(16) 0.49417(10) 0.36515(9) 0.0153(3) Uani 1 1 d . . . N7 N 0.60681(16) 0.61680(10) 0.26018(9) 0.0144(3) Uani 1 1 d . . . N8 N 0.56179(19) 0.64976(11) 0.23178(10) 0.0223(4) Uani 1 1 d . . . N9 N 0.70232(16) 0.49200(10) 0.37164(9) 0.0144(3) Uani 1 1 d . . . N10 N 0.70584(19) 0.45558(11) 0.40493(10) 0.0212(4) Uani 1 1 d . . . P1 P 0.78761(5) -0.00358(3) 0.72858(3) 0.01236(10) Uani 1 1 d . . . P2 P 0.83281(5) 0.14820(3) 0.85618(3) 0.01279(10) Uani 1 1 d . . . P3 P 0.48289(5) 0.10332(3) 0.88697(3) 0.01396(10) Uani 1 1 d . . . P4 P 0.44444(5) -0.05540(3) 0.75278(3) 0.01237(10) Uani 1 1 d . . . P5 P 0.82014(5) 0.50698(3) 0.22839(3) 0.01196(10) Uani 1 1 d . . . P6 P 0.87561(5) 0.65326(3) 0.36103(3) 0.01105(9) Uani 1 1 d . . . P7 P 0.54059(5) 0.61086(3) 0.40425(3) 0.01192(10) Uani 1 1 d . . . P8 P 0.47341(5) 0.45848(3) 0.25782(3) 0.01210(10) Uani 1 1 d . . . C1 C 0.6446(2) -0.05050(12) 0.59288(11) 0.0181(4) Uani 1 1 d . . . H1A H 0.5943 -0.0883 0.6068 0.022 Uiso 1 1 calc R . . C2 C 0.6094(2) -0.04650(13) 0.52739(11) 0.0210(5) Uani 1 1 d . . . H2A H 0.5366 -0.0822 0.4962 0.025 Uiso 1 1 calc R . . C3 C 0.6796(2) 0.00939(14) 0.50675(11) 0.0224(5) Uani 1 1 d . . . H3A H 0.6531 0.0131 0.4623 0.027 Uiso 1 1 calc R . . C4 C 0.7875(2) 0.05924(13) 0.55102(12) 0.0223(5) Uani 1 1 d . . . H4A H 0.8367 0.0971 0.5368 0.027 Uiso 1 1 calc R . . C5 C 0.8254(2) 0.05478(12) 0.61646(11) 0.0194(4) Uani 1 1 d . . . H5A H 0.9012 0.0892 0.6461 0.023 Uiso 1 1 calc R . . C6 C 0.7541(2) 0.00065(12) 0.63952(10) 0.0150(4) Uani 1 1 d . . . C7 C 0.8144(2) -0.13151(12) 0.75881(12) 0.0190(4) Uani 1 1 d . . . H7A H 0.7887 -0.1057 0.8029 0.023 Uiso 1 1 calc R . . C8 C 0.8425(2) -0.20228(13) 0.74664(12) 0.0226(5) Uani 1 1 d . . . H8A H 0.8356 -0.2245 0.7821 0.027 Uiso 1 1 calc R . . C9 C 0.8807(2) -0.24004(12) 0.68253(12) 0.0205(5) Uani 1 1 d . . . H9A H 0.8994 -0.2884 0.6738 0.025 Uiso 1 1 calc R . . C10 C 0.8915(2) -0.20736(12) 0.63140(12) 0.0205(4) Uani 1 1 d . . . H10A H 0.9186 -0.2331 0.5877 0.025 Uiso 1 1 calc R . . C11 C 0.8628(2) -0.13692(12) 0.64333(11) 0.0172(4) Uani 1 1 d . . . H11A H 0.8702 -0.1151 0.6076 0.021 Uiso 1 1 calc R . . C12 C 0.82342(19) -0.09792(11) 0.70723(11) 0.0142(4) Uani 1 1 d . . . C13 C 0.9585(2) 0.05424(11) 0.75880(11) 0.0155(4) Uani 1 1 d . . . H13A H 1.0038 0.0388 0.7947 0.019 Uiso 1 1 calc R . . H13B H 1.0098 0.0466 0.7184 0.019 Uiso 1 1 calc R . . C14 C 0.9525(2) 0.13727(12) 0.79060(11) 0.0173(4) Uani 1 1 d . . . H14A H 0.9237 0.1554 0.7527 0.021 Uiso 1 1 calc R . . H14B H 1.0417 0.1675 0.8140 0.021 Uiso 1 1 calc R . . C15 C 0.7848(2) 0.26568(12) 0.80974(12) 0.0188(4) Uani 1 1 d . . . H15A H 0.7961 0.2344 0.7642 0.023 Uiso 1 1 calc R . . C16 C 0.7462(2) 0.33317(13) 0.81770(12) 0.0214(5) Uani 1 1 d . . . H16A H 0.7310 0.3474 0.7776 0.026 Uiso 1 1 calc R . . C17 C 0.7298(2) 0.37943(13) 0.88351(13) 0.0228(5) Uani 1 1 d . . . H17A H 0.7029 0.4253 0.8887 0.027 Uiso 1 1 calc R . . C18 C 0.7528(2) 0.35863(12) 0.94198(12) 0.0213(5) Uani 1 1 d . . . H18A H 0.7422 0.3904 0.9874 0.026 Uiso 1 1 calc R . . C19 C 0.7914(2) 0.29144(12) 0.93417(11) 0.0182(4) Uani 1 1 d . . . H19A H 0.8074 0.2779 0.9746 0.022 Uiso 1 1 calc R . . C20 C 0.8071(2) 0.24327(11) 0.86774(11) 0.0153(4) Uani 1 1 d . . . C21 C 0.9546(2) 0.11464(12) 0.96842(11) 0.0179(4) Uani 1 1 d . . . H21A H 0.8822 0.0727 0.9561 0.021 Uiso 1 1 calc R . . C22 C 1.0578(2) 0.12329(14) 1.02059(12) 0.0218(5) Uani 1 1 d . . . H22A H 1.0557 0.0871 1.0432 0.026 Uiso 1 1 calc R . . C23 C 1.1635(2) 0.18447(14) 1.03959(12) 0.0226(5) Uani 1 1 d . . . H23A H 1.2339 0.1905 1.0752 0.027 Uiso 1 1 calc R . . C24 C 1.1658(2) 0.23670(13) 1.00617(11) 0.0219(5) Uani 1 1 d . . . H24A H 1.2381 0.2787 1.0190 0.026 Uiso 1 1 calc R . . C25 C 1.0634(2) 0.22825(12) 0.95402(11) 0.0182(4) Uani 1 1 d . . . H25A H 1.0660 0.2646 0.9317 0.022 Uiso 1 1 calc R . . C26 C 0.95601(19) 0.16647(11) 0.93408(10) 0.0145(4) Uani 1 1 d . . . C27 C 0.3665(2) 0.15000(12) 0.85298(12) 0.0208(4) Uani 1 1 d . . . H27A H 0.3319 0.1191 0.8031 0.025 Uiso 1 1 calc R . . H27B H 0.2902 0.1513 0.8800 0.025 Uiso 1 1 calc R . . C28 C 0.4241(3) 0.22924(13) 0.85664(14) 0.0286(5) Uani 1 1 d . . . H28A H 0.3564 0.2484 0.8357 0.043 Uiso 1 1 calc R . . H28B H 0.5005 0.2290 0.8305 0.043 Uiso 1 1 calc R . . H28C H 0.4529 0.2615 0.9061 0.043 Uiso 1 1 calc R . . C29 C 0.5352(2) 0.17177(12) 0.97713(11) 0.0180(4) Uani 1 1 d . . . H29A H 0.5918 0.2176 0.9745 0.022 Uiso 1 1 calc R . . H29B H 0.4554 0.1859 0.9977 0.022 Uiso 1 1 calc R . . C30 C 0.6112(2) 0.14293(14) 1.02599(12) 0.0256(5) Uani 1 1 d . . . H30A H 0.6430 0.1834 1.0715 0.038 Uiso 1 1 calc R . . H30B H 0.6871 0.1256 1.0046 0.038 Uiso 1 1 calc R . . H30C H 0.5524 0.1011 1.0334 0.038 Uiso 1 1 calc R . . C31 C 0.3587(2) 0.03643(12) 0.90980(11) 0.0172(4) Uani 1 1 d . . . H31A H 0.4054 0.0074 0.9319 0.021 Uiso 1 1 calc R . . H31B H 0.3080 0.0649 0.9450 0.021 Uiso 1 1 calc R . . C32 C 0.1449(2) -0.04543(13) 0.87275(12) 0.0235(5) Uani 1 1 d . . . H32A H 0.0827 -0.0814 0.8322 0.035 Uiso 1 1 calc R . . H32B H 0.1033 -0.0040 0.8971 0.035 Uiso 1 1 calc R . . H32C H 0.1680 -0.0706 0.9054 0.035 Uiso 1 1 calc R . . C33 C 0.3237(2) -0.07887(11) 0.80934(11) 0.0164(4) Uani 1 1 d . . . H33A H 0.2514 -0.1208 0.7794 0.020 Uiso 1 1 calc R . . H33B H 0.3686 -0.0964 0.8438 0.020 Uiso 1 1 calc R . . C34 C 0.3390(2) -0.03873(12) 0.68438(11) 0.0182(4) Uani 1 1 d . . . H34A H 0.3353 0.0150 0.7015 0.022 Uiso 1 1 calc R . . H34B H 0.3841 -0.0480 0.6417 0.022 Uiso 1 1 calc R . . C35 C 0.1967(2) -0.08446(13) 0.66213(12) 0.0227(5) Uani 1 1 d . . . H35A H 0.1563 -0.0754 0.6213 0.034 Uiso 1 1 calc R . . H35B H 0.1453 -0.0694 0.7014 0.034 Uiso 1 1 calc R . . H35C H 0.1971 -0.1379 0.6494 0.034 Uiso 1 1 calc R . . C36 C 0.4611(2) -0.15273(11) 0.70488(11) 0.0174(4) Uani 1 1 d . . . H36A H 0.3793 -0.1791 0.6710 0.021 Uiso 1 1 calc R . . H36B H 0.5358 -0.1504 0.6771 0.021 Uiso 1 1 calc R . . C37 C 0.4844(2) -0.19947(13) 0.75081(12) 0.0235(5) Uani 1 1 d . . . H37A H 0.5134 -0.2445 0.7226 0.035 Uiso 1 1 calc R . . H37B H 0.4017 -0.2143 0.7684 0.035 Uiso 1 1 calc R . . H37C H 0.5532 -0.1697 0.7909 0.035 Uiso 1 1 calc R . . C38 C 0.6818(2) 0.53073(12) 0.11632(11) 0.0186(4) Uani 1 1 d . . . H38A H 0.6063 0.5189 0.1380 0.022 Uiso 1 1 calc R . . C39 C 0.6651(2) 0.55184(13) 0.05774(12) 0.0238(5) Uani 1 1 d . . . H39A H 0.5794 0.5550 0.0402 0.029 Uiso 1 1 calc R . . C40 C 0.7733(2) 0.56843(13) 0.02471(12) 0.0245(5) Uani 1 1 d . . . H40A H 0.7626 0.5829 -0.0156 0.029 Uiso 1 1 calc R . . C41 C 0.8976(2) 0.56362(13) 0.05127(12) 0.0239(5) Uani 1 1 d . . . H41A H 0.9723 0.5746 0.0288 0.029 Uiso 1 1 calc R . . C42 C 0.9140(2) 0.54299(12) 0.11015(11) 0.0196(4) Uani 1 1 d . . . H42A H 1.0000 0.5401 0.1276 0.024 Uiso 1 1 calc R . . C43 C 0.8057(2) 0.52625(11) 0.14466(10) 0.0150(4) Uani 1 1 d . . . C44 C 0.8442(2) 0.37620(13) 0.25285(12) 0.0201(4) Uani 1 1 d . . . H44A H 0.8248 0.4024 0.2984 0.024 Uiso 1 1 calc R . . C45 C 0.8704(2) 0.30504(13) 0.23857(12) 0.0218(5) Uani 1 1 d . . . H45A H 0.8687 0.2829 0.2742 0.026 Uiso 1 1 calc R . . C46 C 0.8988(2) 0.26647(13) 0.17244(12) 0.0220(5) Uani 1 1 d . . . H46A H 0.9167 0.2177 0.1624 0.026 Uiso 1 1 calc R . . C47 C 0.9012(2) 0.29905(12) 0.12095(12) 0.0209(5) Uani 1 1 d . . . H47A H 0.9212 0.2726 0.0756 0.025 Uiso 1 1 calc R . . C48 C 0.8744(2) 0.37028(12) 0.13479(11) 0.0165(4) Uani 1 1 d . . . H48A H 0.8755 0.3919 0.0988 0.020 Uiso 1 1 calc R . . C49 C 0.84596(19) 0.41002(11) 0.20155(11) 0.0145(4) Uani 1 1 d . . . C50 C 0.99485(19) 0.55570(11) 0.26649(11) 0.0154(4) Uani 1 1 d . . . H50A H 1.0261 0.5372 0.3037 0.018 Uiso 1 1 calc R . . H50B H 1.0532 0.5456 0.2292 0.018 Uiso 1 1 calc R . . C51 C 0.9997(2) 0.63946(12) 0.29779(11) 0.0158(4) Uani 1 1 d . . . H51A H 0.9780 0.6591 0.2599 0.019 Uiso 1 1 calc R . . H51B H 1.0897 0.6665 0.3226 0.019 Uiso 1 1 calc R . . C52 C 0.8311(2) 0.76785(12) 0.31239(11) 0.0163(4) Uani 1 1 d . . . H52A H 0.8240 0.7311 0.2668 0.020 Uiso 1 1 calc R . . C53 C 0.8090(2) 0.83844(13) 0.31871(12) 0.0199(4) Uani 1 1 d . . . H53A H 0.7852 0.8493 0.2776 0.024 Uiso 1 1 calc R . . C54 C 0.8216(2) 0.89303(13) 0.38484(12) 0.0224(5) Uani 1 1 d . . . H54A H 0.8075 0.9415 0.3891 0.027 Uiso 1 1 calc R . . C55 C 0.8549(2) 0.87670(13) 0.44463(12) 0.0206(4) Uani 1 1 d . . . H55A H 0.8642 0.9142 0.4900 0.025 Uiso 1 1 calc R . . C56 C 0.8748(2) 0.80578(12) 0.43865(11) 0.0157(4) Uani 1 1 d . . . H56A H 0.8962 0.7949 0.4801 0.019 Uiso 1 1 calc R . . C57 C 0.86380(19) 0.75003(11) 0.37223(10) 0.0138(4) Uani 1 1 d . . . C58 C 0.9658(2) 0.61750(12) 0.47858(11) 0.0157(4) Uani 1 1 d . . . H58A H 0.8874 0.5791 0.4649 0.019 Uiso 1 1 calc R . . C59 C 1.0568(2) 0.62363(13) 0.53543(11) 0.0203(4) Uani 1 1 d . . . H59A H 1.0409 0.5892 0.5599 0.024 Uiso 1 1 calc R . . C60 C 1.1708(2) 0.68005(13) 0.55634(11) 0.0198(4) Uani 1 1 d . . . H60A H 1.2331 0.6842 0.5950 0.024 Uiso 1 1 calc R . . C61 C 1.1935(2) 0.73031(12) 0.52073(11) 0.0180(4) Uani 1 1 d . . . H61A H 1.2706 0.7696 0.5357 0.022 Uiso 1 1 calc R . . C62 C 1.10435(19) 0.72340(12) 0.46345(11) 0.0153(4) Uani 1 1 d . . . H62A H 1.1220 0.7574 0.4386 0.018 Uiso 1 1 calc R . . C63 C 0.98821(19) 0.66697(11) 0.44148(10) 0.0136(4) Uani 1 1 d . . . C64 C 0.4326(2) 0.67133(12) 0.38793(11) 0.0174(4) Uani 1 1 d . . . H64A H 0.3842 0.6469 0.3394 0.021 Uiso 1 1 calc R . . H64B H 0.3657 0.6750 0.4210 0.021 Uiso 1 1 calc R . . C65 C 0.5044(2) 0.75067(13) 0.39614(13) 0.0255(5) Uani 1 1 d . . . H65A H 0.4405 0.7777 0.3835 0.038 Uiso 1 1 calc R . . H65B H 0.5731 0.7479 0.3649 0.038 Uiso 1 1 calc R . . H65C H 0.5457 0.7772 0.4453 0.038 Uiso 1 1 calc R . . C66 C 0.6293(2) 0.66548(12) 0.49378(10) 0.0169(4) Uani 1 1 d . . . H66A H 0.6812 0.6333 0.5085 0.020 Uiso 1 1 calc R . . H66B H 0.6938 0.7083 0.4905 0.020 Uiso 1 1 calc R . . C67 C 0.5483(2) 0.69672(14) 0.55307(11) 0.0232(5) Uani 1 1 d . . . H67A H 0.6087 0.7279 0.5963 0.035 Uiso 1 1 calc R . . H67B H 0.4916 0.6551 0.5617 0.035 Uiso 1 1 calc R . . H67C H 0.4928 0.7272 0.5391 0.035 Uiso 1 1 calc R . . C68 C 0.4174(2) 0.54291(12) 0.42613(11) 0.0164(4) Uani 1 1 d . . . H68A H 0.4644 0.5113 0.4447 0.020 Uiso 1 1 calc R . . H68B H 0.3706 0.5706 0.4639 0.020 Uiso 1 1 calc R . . C69 C 0.1975(2) 0.46593(13) 0.38969(12) 0.0210(5) Uani 1 1 d . . . H69A H 0.1634 0.5083 0.4191 0.032 Uiso 1 1 calc R . . H69B H 0.2170 0.4350 0.4175 0.032 Uiso 1 1 calc R . . H69C H 0.1307 0.4355 0.3489 0.032 Uiso 1 1 calc R . . C70 C 0.3698(2) 0.43152(12) 0.31983(11) 0.0162(4) Uani 1 1 d . . . H70A H 0.2940 0.3904 0.2926 0.019 Uiso 1 1 calc R . . H70B H 0.4231 0.4124 0.3498 0.019 Uiso 1 1 calc R . . C71 C 0.3497(2) 0.48174(12) 0.20302(11) 0.0168(4) Uani 1 1 d . . . H71A H 0.3306 0.5304 0.2314 0.020 Uiso 1 1 calc R . . H71B H 0.3909 0.4891 0.1624 0.020 Uiso 1 1 calc R . . C72 C 0.2171(2) 0.42519(13) 0.17401(12) 0.0209(5) Uani 1 1 d . . . H72A H 0.1642 0.4413 0.1419 0.031 Uiso 1 1 calc R . . H72B H 0.1684 0.4225 0.2133 0.031 Uiso 1 1 calc R . . H72C H 0.2337 0.3756 0.1483 0.031 Uiso 1 1 calc R . . C73 C 0.4843(2) 0.36278(12) 0.20268(11) 0.0190(4) Uani 1 1 d . . . H73A H 0.5548 0.3472 0.2267 0.023 Uiso 1 1 calc R . . H73B H 0.3992 0.3282 0.1997 0.023 Uiso 1 1 calc R . . C74 C 0.5136(2) 0.35364(13) 0.12756(12) 0.0247(5) Uani 1 1 d . . . H74A H 0.5208 0.3018 0.1030 0.037 Uiso 1 1 calc R . . H74B H 0.5973 0.3878 0.1295 0.037 Uiso 1 1 calc R . . H74C H 0.4414 0.3655 0.1020 0.037 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 W1 0.01295(4) 0.00959(4) 0.01034(4) 0.00355(3) 0.00055(3) 0.00196(3) W2 0.01003(4) 0.00999(4) 0.00986(4) 0.00316(3) 0.00127(3) 0.00246(3) N1 0.0150(8) 0.0137(8) 0.0178(9) 0.0024(7) 0.0041(7) 0.0023(7) N2 0.0172(9) 0.0136(8) 0.0167(8) 0.0062(7) 0.0016(7) 0.0020(7) N3 0.0275(11) 0.0262(11) 0.0265(11) 0.0150(9) -0.0014(8) 0.0033(9) N4 0.0144(8) 0.0126(8) 0.0152(8) 0.0025(7) 0.0013(6) 0.0024(6) N5 0.0255(10) 0.0212(10) 0.0207(9) 0.0097(8) 0.0024(8) 0.0058(8) N6 0.0135(8) 0.0165(9) 0.0147(8) 0.0051(7) 0.0029(6) 0.0006(7) N7 0.0133(8) 0.0131(8) 0.0150(8) 0.0033(7) 0.0026(6) 0.0013(6) N8 0.0209(10) 0.0233(10) 0.0259(10) 0.0134(8) 0.0011(8) 0.0042(8) N9 0.0116(8) 0.0146(8) 0.0160(8) 0.0030(7) 0.0028(6) 0.0039(6) N10 0.0224(10) 0.0219(10) 0.0228(10) 0.0110(8) 0.0036(7) 0.0071(8) P1 0.0139(2) 0.0110(2) 0.0116(2) 0.00348(19) 0.00109(18) 0.00222(19) P2 0.0147(2) 0.0106(2) 0.0117(2) 0.00331(19) 0.00048(18) 0.00114(19) P3 0.0164(2) 0.0110(2) 0.0135(2) 0.00290(19) 0.00130(19) 0.00343(19) P4 0.0137(2) 0.0111(2) 0.0116(2) 0.00360(19) 0.00081(18) 0.00181(19) P5 0.0118(2) 0.0116(2) 0.0113(2) 0.00228(19) 0.00144(18) 0.00300(19) P6 0.0108(2) 0.0111(2) 0.0104(2) 0.00294(18) 0.00129(17) 0.00188(18) P7 0.0116(2) 0.0125(2) 0.0110(2) 0.00297(19) 0.00232(18) 0.00272(18) P8 0.0119(2) 0.0110(2) 0.0125(2) 0.00334(19) 0.00080(18) 0.00192(18) C1 0.0168(10) 0.0206(11) 0.0178(10) 0.0067(8) 0.0033(8) 0.0062(8) C2 0.0166(10) 0.0277(12) 0.0182(10) 0.0059(9) 0.0002(8) 0.0087(9) C3 0.0271(12) 0.0323(13) 0.0145(10) 0.0107(9) 0.0048(8) 0.0171(10) C4 0.0295(12) 0.0230(11) 0.0201(11) 0.0119(9) 0.0072(9) 0.0101(9) C5 0.0240(11) 0.0158(10) 0.0181(10) 0.0055(8) 0.0019(8) 0.0051(8) C6 0.0167(10) 0.0174(10) 0.0127(9) 0.0054(8) 0.0030(7) 0.0071(8) C7 0.0209(11) 0.0180(10) 0.0194(10) 0.0070(8) 0.0046(8) 0.0061(8) C8 0.0238(11) 0.0212(11) 0.0280(12) 0.0139(10) 0.0059(9) 0.0065(9) C9 0.0176(10) 0.0120(10) 0.0302(12) 0.0049(9) -0.0014(9) 0.0052(8) C10 0.0199(11) 0.0180(11) 0.0214(11) 0.0030(9) 0.0016(8) 0.0067(8) C11 0.0172(10) 0.0160(10) 0.0173(10) 0.0041(8) 0.0014(8) 0.0044(8) C12 0.0110(9) 0.0136(9) 0.0164(9) 0.0042(8) -0.0001(7) 0.0013(7) C13 0.0156(10) 0.0145(9) 0.0150(9) 0.0045(8) 0.0017(7) 0.0013(8) C14 0.0187(10) 0.0167(10) 0.0136(9) 0.0030(8) 0.0029(8) 0.0003(8) C15 0.0184(10) 0.0192(11) 0.0199(10) 0.0092(9) 0.0016(8) 0.0025(8) C16 0.0208(11) 0.0227(11) 0.0258(12) 0.0164(10) 0.0003(9) 0.0030(9) C17 0.0210(11) 0.0152(10) 0.0331(13) 0.0111(9) -0.0013(9) 0.0029(8) C18 0.0206(11) 0.0159(10) 0.0238(11) 0.0027(9) -0.0004(9) 0.0043(8) C19 0.0190(10) 0.0157(10) 0.0185(10) 0.0057(8) -0.0027(8) 0.0026(8) C20 0.0141(9) 0.0120(9) 0.0186(10) 0.0057(8) 0.0000(7) 0.0000(7) C21 0.0172(10) 0.0193(10) 0.0173(10) 0.0072(8) 0.0012(8) 0.0030(8) C22 0.0205(11) 0.0281(12) 0.0205(11) 0.0122(9) 0.0041(8) 0.0074(9) C23 0.0149(10) 0.0323(13) 0.0174(10) 0.0034(9) -0.0014(8) 0.0086(9) C24 0.0173(10) 0.0230(11) 0.0192(11) 0.0014(9) -0.0013(8) 0.0019(9) C25 0.0187(10) 0.0159(10) 0.0170(10) 0.0037(8) -0.0010(8) 0.0011(8) C26 0.0137(9) 0.0143(9) 0.0129(9) 0.0015(7) -0.0001(7) 0.0036(7) C27 0.0230(11) 0.0189(11) 0.0226(11) 0.0088(9) 0.0022(9) 0.0070(9) C28 0.0321(13) 0.0220(12) 0.0353(14) 0.0143(11) 0.0015(11) 0.0075(10) C29 0.0204(10) 0.0149(10) 0.0153(10) 0.0014(8) 0.0029(8) 0.0029(8) C30 0.0294(13) 0.0245(12) 0.0184(11) 0.0045(9) -0.0032(9) 0.0029(10) C31 0.0188(10) 0.0168(10) 0.0141(9) 0.0028(8) 0.0056(8) 0.0024(8) C32 0.0156(10) 0.0229(12) 0.0290(12) 0.0048(10) 0.0073(9) 0.0028(9) C33 0.0188(10) 0.0130(9) 0.0160(10) 0.0035(8) 0.0036(8) 0.0023(8) C34 0.0172(10) 0.0180(10) 0.0191(10) 0.0075(8) -0.0023(8) 0.0032(8) C35 0.0178(11) 0.0198(11) 0.0263(12) 0.0047(9) -0.0049(9) 0.0025(9) C36 0.0197(10) 0.0127(9) 0.0184(10) 0.0041(8) 0.0023(8) 0.0026(8) C37 0.0283(12) 0.0165(11) 0.0287(12) 0.0093(9) 0.0078(10) 0.0078(9) C38 0.0188(10) 0.0224(11) 0.0146(10) 0.0057(8) 0.0022(8) 0.0057(8) C39 0.0264(12) 0.0270(12) 0.0179(11) 0.0070(9) 0.0002(9) 0.0085(10) C40 0.0389(14) 0.0180(11) 0.0173(11) 0.0087(9) 0.0021(9) 0.0037(10) C41 0.0276(12) 0.0210(11) 0.0242(12) 0.0112(9) 0.0082(9) -0.0001(9) C42 0.0179(10) 0.0211(11) 0.0190(10) 0.0070(9) 0.0037(8) 0.0014(8) C43 0.0189(10) 0.0123(9) 0.0125(9) 0.0033(7) 0.0021(7) 0.0024(8) C44 0.0224(11) 0.0200(11) 0.0212(11) 0.0077(9) 0.0055(8) 0.0106(9) C45 0.0251(12) 0.0201(11) 0.0248(11) 0.0105(9) 0.0039(9) 0.0113(9) C46 0.0208(11) 0.0146(10) 0.0282(12) 0.0044(9) -0.0008(9) 0.0051(8) C47 0.0240(11) 0.0167(10) 0.0180(10) -0.0006(8) 0.0007(8) 0.0081(9) C48 0.0162(10) 0.0169(10) 0.0156(10) 0.0035(8) 0.0017(8) 0.0059(8) C49 0.0112(9) 0.0132(9) 0.0171(10) 0.0027(8) 0.0005(7) 0.0034(7) C50 0.0119(9) 0.0155(10) 0.0155(9) 0.0015(8) 0.0009(7) 0.0024(7) C51 0.0151(10) 0.0148(10) 0.0156(9) 0.0036(8) 0.0033(7) 0.0014(8) C52 0.0163(10) 0.0168(10) 0.0160(10) 0.0071(8) 0.0021(8) 0.0015(8) C53 0.0212(11) 0.0213(11) 0.0217(11) 0.0135(9) 0.0026(8) 0.0045(9) C54 0.0254(12) 0.0170(10) 0.0290(12) 0.0111(9) 0.0080(9) 0.0076(9) C55 0.0238(11) 0.0168(10) 0.0212(11) 0.0050(9) 0.0066(9) 0.0062(9) C56 0.0162(10) 0.0157(10) 0.0169(10) 0.0067(8) 0.0032(8) 0.0049(8) C57 0.0123(9) 0.0139(9) 0.0159(9) 0.0060(8) 0.0024(7) 0.0025(7) C58 0.0143(9) 0.0165(10) 0.0162(10) 0.0052(8) 0.0019(7) 0.0045(8) C59 0.0194(11) 0.0237(11) 0.0203(11) 0.0104(9) 0.0025(8) 0.0059(9) C60 0.0156(10) 0.0263(12) 0.0158(10) 0.0048(9) -0.0012(8) 0.0063(9) C61 0.0132(9) 0.0189(10) 0.0179(10) 0.0017(8) 0.0001(8) 0.0035(8) C62 0.0150(10) 0.0146(10) 0.0149(9) 0.0030(8) 0.0026(7) 0.0033(8) C63 0.0119(9) 0.0148(9) 0.0127(9) 0.0021(7) 0.0023(7) 0.0042(7) C64 0.0180(10) 0.0178(10) 0.0167(10) 0.0040(8) 0.0026(8) 0.0083(8) C65 0.0295(13) 0.0177(11) 0.0310(13) 0.0086(10) 0.0042(10) 0.0091(9) C66 0.0133(9) 0.0220(11) 0.0130(9) 0.0034(8) -0.0005(7) 0.0039(8) C67 0.0192(11) 0.0321(13) 0.0137(10) 0.0013(9) 0.0010(8) 0.0070(9) C68 0.0165(10) 0.0189(10) 0.0140(9) 0.0062(8) 0.0033(7) 0.0029(8) C69 0.0157(10) 0.0221(11) 0.0249(11) 0.0084(9) 0.0061(8) 0.0015(8) C70 0.0157(10) 0.0146(10) 0.0188(10) 0.0079(8) 0.0023(8) 0.0006(8) C71 0.0159(10) 0.0171(10) 0.0168(10) 0.0056(8) -0.0012(8) 0.0042(8) C72 0.0139(10) 0.0238(11) 0.0200(11) 0.0026(9) -0.0024(8) 0.0031(9) C73 0.0176(10) 0.0126(9) 0.0235(11) 0.0022(8) 0.0026(8) 0.0026(8) C74 0.0208(11) 0.0207(11) 0.0238(11) -0.0038(9) 0.0014(9) 0.0050(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 W1 N4 2.0102(19) . ? W1 N2 2.0200(18) . ? W1 P1 2.4313(5) . ? W1 P2 2.4385(5) . ? W1 P4 2.4407(5) . ? W1 P3 2.4542(5) . ? W2 N9 2.0034(19) . ? W2 N7 2.0122(19) . ? W2 P8 2.4392(5) . ? W2 P7 2.4424(5) . ? W2 P5 2.4437(5) . ? W2 P6 2.4470(5) . ? N1 C32 1.463(3) . ? N1 C33 1.468(3) . ? N1 C31 1.473(3) . ? N2 N3 1.128(2) . ? N4 N5 1.129(2) . ? N6 C70 1.464(3) . ? N6 C69 1.465(3) . ? N6 C68 1.470(3) . ? N7 N8 1.122(2) . ? N9 N10 1.125(2) . ? P1 C12 1.841(2) . ? P1 C6 1.842(2) . ? P1 C13 1.854(2) . ? P2 C20 1.843(2) . ? P2 C26 1.850(2) . ? P2 C14 1.864(2) . ? P3 C29 1.841(2) . ? P3 C27 1.846(2) . ? P3 C31 1.848(2) . ? P4 C34 1.846(2) . ? P4 C33 1.847(2) . ? P4 C36 1.856(2) . ? P5 C49 1.845(2) . ? P5 C43 1.851(2) . ? P5 C50 1.861(2) . ? P6 C57 1.835(2) . ? P6 C63 1.847(2) . ? P6 C51 1.865(2) . ? P7 C64 1.839(2) . ? P7 C66 1.844(2) . ? P7 C68 1.845(2) . ? P8 C71 1.842(2) . ? P8 C73 1.847(2) . ? P8 C70 1.847(2) . ? C1 C2 1.380(3) . ? C1 C6 1.409(3) . ? C1 H1A 0.9500 . ? C2 C3 1.388(3) . ? C2 H2A 0.9500 . ? C3 C4 1.373(3) . ? C3 H3A 0.9500 . ? C4 C5 1.388(3) . ? C4 H4A 0.9500 . ? C5 C6 1.396(3) . ? C5 H5A 0.9500 . ? C7 C8 1.394(3) . ? C7 C12 1.398(3) . ? C7 H7A 0.9500 . ? C8 C9 1.387(3) . ? C8 H8A 0.9500 . ? C9 C10 1.379(3) . ? C9 H9A 0.9500 . ? C10 C11 1.391(3) . ? C10 H10A 0.9500 . ? C11 C12 1.396(3) . ? C11 H11A 0.9500 . ? C13 C14 1.534(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.393(3) . ? C15 C20 1.396(3) . ? C15 H15A 0.9500 . ? C16 C17 1.380(3) . ? C16 H16A 0.9500 . ? C17 C18 1.387(3) . ? C17 H17A 0.9500 . ? C18 C19 1.387(3) . ? C18 H18A 0.9500 . ? C19 C20 1.400(3) . ? C19 H19A 0.9500 . ? C21 C26 1.392(3) . ? C21 C22 1.393(3) . ? C21 H21A 0.9500 . ? C22 C23 1.386(3) . ? C22 H22A 0.9500 . ? C23 C24 1.384(3) . ? C23 H23A 0.9500 . ? C24 C25 1.388(3) . ? C24 H24A 0.9500 . ? C25 C26 1.403(3) . ? C25 H25A 0.9500 . ? C27 C28 1.516(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.520(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.526(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.527(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.383(3) . ? C38 C43 1.394(3) . ? C38 H38A 0.9500 . ? C39 C40 1.385(3) . ? C39 H39A 0.9500 . ? C40 C41 1.387(3) . ? C40 H40A 0.9500 . ? C41 C42 1.383(3) . ? C41 H41A 0.9500 . ? C42 C43 1.405(3) . ? C42 H42A 0.9500 . ? C44 C45 1.388(3) . ? C44 C49 1.396(3) . ? C44 H44A 0.9500 . ? C45 C46 1.382(3) . ? C45 H45A 0.9500 . ? C46 C47 1.382(3) . ? C46 H46A 0.9500 . ? C47 C48 1.393(3) . ? C47 H47A 0.9500 . ? C48 C49 1.398(3) . ? C48 H48A 0.9500 . ? C50 C51 1.521(3) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.388(3) . ? C52 C57 1.398(3) . ? C52 H52A 0.9500 . ? C53 C54 1.385(3) . ? C53 H53A 0.9500 . ? C54 C55 1.383(3) . ? C54 H54A 0.9500 . ? C55 C56 1.388(3) . ? C55 H55A 0.9500 . ? C56 C57 1.401(3) . ? C56 H56A 0.9500 . ? C58 C59 1.393(3) . ? C58 C63 1.395(3) . ? C58 H58A 0.9500 . ? C59 C60 1.387(3) . ? C59 H59A 0.9500 . ? C60 C61 1.385(3) . ? C60 H60A 0.9500 . ? C61 C62 1.383(3) . ? C61 H61A 0.9500 . ? C62 C63 1.403(3) . ? C62 H62A 0.9500 . ? C64 C65 1.529(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.532(3) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.533(3) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.530(3) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? 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 N4 W1 N2 173.83(7) . . ? N4 W1 P1 97.26(5) . . ? N2 W1 P1 86.56(5) . . ? N4 W1 P2 98.05(5) . . ? N2 W1 P2 87.35(5) . . ? P1 W1 P2 80.250(18) . . ? N4 W1 P4 86.58(5) . . ? N2 W1 P4 88.22(5) . . ? P1 W1 P4 96.037(18) . . ? P2 W1 P4 174.375(17) . . ? N4 W1 P3 87.56(5) . . ? N2 W1 P3 88.67(5) . . ? P1 W1 P3 175.149(19) . . ? P2 W1 P3 98.638(18) . . ? P4 W1 P3 84.708(18) . . ? N9 W2 N7 168.63(6) . . ? N9 W2 P8 84.49(5) . . ? N7 W2 P8 87.96(5) . . ? N9 W2 P7 84.37(5) . . ? N7 W2 P7 86.69(5) . . ? P8 W2 P7 86.451(17) . . ? N9 W2 P5 95.28(5) . . ? N7 W2 P5 94.16(5) . . ? P8 W2 P5 97.795(17) . . ? P7 W2 P5 175.692(17) . . ? N9 W2 P6 98.57(5) . . ? N7 W2 P6 89.41(5) . . ? P8 W2 P6 175.935(17) . . ? P7 W2 P6 96.488(17) . . ? P5 W2 P6 79.307(17) . . ? C32 N1 C33 108.93(17) . . ? C32 N1 C31 108.66(16) . . ? C33 N1 C31 110.77(16) . . ? N3 N2 W1 177.58(17) . . ? N5 N4 W1 176.31(17) . . ? C70 N6 C69 110.15(16) . . ? C70 N6 C68 112.25(16) . . ? C69 N6 C68 109.74(16) . . ? N8 N7 W2 175.34(16) . . ? N10 N9 W2 173.17(17) . . ? C12 P1 C6 100.99(9) . . ? C12 P1 C13 99.88(9) . . ? C6 P1 C13 101.75(9) . . ? C12 P1 W1 125.04(7) . . ? C6 P1 W1 115.26(7) . . ? C13 P1 W1 110.64(7) . . ? C20 P2 C26 101.66(9) . . ? C20 P2 C14 101.24(10) . . ? C26 P2 C14 96.27(9) . . ? C20 P2 W1 116.51(7) . . ? C26 P2 W1 127.15(7) . . ? C14 P2 W1 109.57(7) . . ? C29 P3 C27 99.77(10) . . ? C29 P3 C31 96.97(9) . . ? C27 P3 C31 97.76(10) . . ? C29 P3 W1 123.73(7) . . ? C27 P3 W1 118.79(8) . . ? C31 P3 W1 114.86(7) . . ? C34 P4 C33 102.66(10) . . ? C34 P4 C36 100.65(10) . . ? C33 P4 C36 96.88(9) . . ? C34 P4 W1 113.96(7) . . ? C33 P4 W1 117.37(7) . . ? C36 P4 W1 122.03(7) . . ? C49 P5 C43 104.12(9) . . ? C49 P5 C50 97.49(9) . . ? C43 P5 C50 101.15(9) . . ? C49 P5 W2 123.88(7) . . ? C43 P5 W2 117.18(7) . . ? C50 P5 W2 109.08(6) . . ? C57 P6 C63 101.60(9) . . ? C57 P6 C51 100.13(9) . . ? C63 P6 C51 97.59(9) . . ? C57 P6 W2 117.58(7) . . ? C63 P6 W2 125.13(7) . . ? C51 P6 W2 110.50(6) . . ? C64 P7 C66 103.39(10) . . ? C64 P7 C68 99.52(10) . . ? C66 P7 C68 99.05(9) . . ? C64 P7 W2 119.13(7) . . ? C66 P7 W2 117.30(7) . . ? C68 P7 W2 115.18(7) . . ? C71 P8 C73 103.00(10) . . ? C71 P8 C70 100.76(10) . . ? C73 P8 C70 97.10(10) . . ? C71 P8 W2 116.44(7) . . ? C73 P8 W2 121.13(7) . . ? C70 P8 W2 114.95(7) . . ? C2 C1 C6 121.0(2) . . ? C2 C1 H1A 119.5 . . ? C6 C1 H1A 119.5 . . ? C1 C2 C3 120.4(2) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C4 C3 C2 119.5(2) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 120.5(2) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.7 . . ? C4 C5 C6 121.2(2) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C5 C6 C1 117.31(19) . . ? C5 C6 P1 123.99(16) . . ? C1 C6 P1 118.56(16) . . ? C8 C7 C12 121.1(2) . . ? C8 C7 H7A 119.5 . . ? C12 C7 H7A 119.5 . . ? C9 C8 C7 119.7(2) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? C10 C9 C8 120.0(2) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 120.4(2) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C10 C11 C12 120.7(2) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C7 118.1(2) . . ? C11 C12 P1 123.78(17) . . ? C7 C12 P1 118.07(16) . . ? C14 C13 P1 109.50(14) . . ? C14 C13 H13A 109.8 . . ? P1 C13 H13A 109.8 . . ? C14 C13 H13B 109.8 . . ? P1 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? C13 C14 P2 109.24(14) . . ? C13 C14 H14A 109.8 . . ? P2 C14 H14A 109.8 . . ? C13 C14 H14B 109.8 . . ? P2 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C16 C15 C20 121.0(2) . . ? C16 C15 H15A 119.5 . . ? C20 C15 H15A 119.5 . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 119.6(2) . . ? C16 C17 H17A 120.2 . . ? C18 C17 H17A 120.2 . . ? C17 C18 C19 120.1(2) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C20 121.2(2) . . ? C18 C19 H19A 119.4 . . ? C20 C19 H19A 119.4 . . ? C15 C20 C19 117.8(2) . . ? C15 C20 P2 121.20(16) . . ? C19 C20 P2 120.47(17) . . ? C26 C21 C22 121.0(2) . . ? C26 C21 H21A 119.5 . . ? C22 C21 H21A 119.5 . . ? C23 C22 C21 120.2(2) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 119.4(2) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C23 C24 C25 120.6(2) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C24 C25 C26 120.6(2) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C21 C26 C25 118.2(2) . . ? C21 C26 P2 121.03(15) . . ? C25 C26 P2 120.22(17) . . ? C28 C27 P3 115.44(16) . . ? C28 C27 H27A 108.4 . . ? P3 C27 H27A 108.4 . . ? C28 C27 H27B 108.4 . . ? P3 C27 H27B 108.4 . . ? H27A C27 H27B 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P3 113.71(16) . . ? C30 C29 H29A 108.8 . . ? P3 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? P3 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 P3 112.95(14) . . ? N1 C31 H31A 109.0 . . ? P3 C31 H31A 109.0 . . ? N1 C31 H31B 109.0 . . ? P3 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? N1 C32 H32A 109.5 . . ? N1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N1 C33 P4 113.89(14) . . ? N1 C33 H33A 108.8 . . ? P4 C33 H33A 108.8 . . ? N1 C33 H33B 108.8 . . ? P4 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C35 C34 P4 117.97(16) . . ? C35 C34 H34A 107.8 . . ? P4 C34 H34A 107.8 . . ? C35 C34 H34B 107.8 . . ? P4 C34 H34B 107.8 . . ? H34A C34 H34B 107.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 P4 115.88(15) . . ? C37 C36 H36A 108.3 . . ? P4 C36 H36A 108.3 . . ? C37 C36 H36B 108.3 . . ? P4 C36 H36B 108.3 . . ? H36A C36 H36B 107.4 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C43 122.2(2) . . ? C39 C38 H38A 118.9 . . ? C43 C38 H38A 118.9 . . ? C40 C39 C38 120.0(2) . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C39 C40 C41 119.1(2) . . ? C39 C40 H40A 120.5 . . ? C41 C40 H40A 120.5 . . ? C42 C41 C40 120.7(2) . . ? C42 C41 H41A 119.6 . . ? C40 C41 H41A 119.6 . . ? C41 C42 C43 121.1(2) . . ? C41 C42 H42A 119.4 . . ? C43 C42 H42A 119.4 . . ? C38 C43 C42 116.9(2) . . ? C38 C43 P5 118.72(15) . . ? C42 C43 P5 124.19(17) . . ? C45 C44 C49 121.3(2) . . ? C45 C44 H44A 119.4 . . ? C49 C44 H44A 119.4 . . ? C46 C45 C44 119.8(2) . . ? C46 C45 H45A 120.1 . . ? C44 C45 H45A 120.1 . . ? C47 C46 C45 119.7(2) . . ? C47 C46 H46A 120.1 . . ? C45 C46 H46A 120.1 . . ? C46 C47 C48 120.7(2) . . ? C46 C47 H47A 119.6 . . ? C48 C47 H47A 119.6 . . ? C47 C48 C49 120.1(2) . . ? C47 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? C44 C49 C48 118.3(2) . . ? C44 C49 P5 117.32(15) . . ? C48 C49 P5 124.28(17) . . ? C51 C50 P5 108.23(14) . . ? C51 C50 H50A 110.1 . . ? P5 C50 H50A 110.1 . . ? C51 C50 H50B 110.1 . . ? P5 C50 H50B 110.1 . . ? H50A C50 H50B 108.4 . . ? C50 C51 P6 107.65(14) . . ? C50 C51 H51A 110.2 . . ? P6 C51 H51A 110.2 . . ? C50 C51 H51B 110.2 . . ? P6 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? C53 C52 C57 120.9(2) . . ? C53 C52 H52A 119.5 . . ? C57 C52 H52A 119.5 . . ? C54 C53 C52 120.2(2) . . ? C54 C53 H53A 119.9 . . ? C52 C53 H53A 119.9 . . ? C55 C54 C53 119.7(2) . . ? C55 C54 H54A 120.1 . . ? C53 C54 H54A 120.1 . . ? C54 C55 C56 120.3(2) . . ? C54 C55 H55A 119.9 . . ? C56 C55 H55A 119.9 . . ? C55 C56 C57 120.8(2) . . ? C55 C56 H56A 119.6 . . ? C57 C56 H56A 119.6 . . ? C52 C57 C56 118.0(2) . . ? C52 C57 P6 118.95(15) . . ? C56 C57 P6 122.83(16) . . ? C59 C58 C63 120.9(2) . . ? C59 C58 H58A 119.5 . . ? C63 C58 H58A 119.5 . . ? C60 C59 C58 119.9(2) . . ? C60 C59 H59A 120.0 . . ? C58 C59 H59A 120.0 . . ? C61 C60 C59 119.9(2) . . ? C61 C60 H60A 120.1 . . ? C59 C60 H60A 120.1 . . ? C62 C61 C60 120.2(2) . . ? C62 C61 H61A 119.9 . . ? C60 C61 H61A 119.9 . . ? C61 C62 C63 121.0(2) . . ? C61 C62 H62A 119.5 . . ? C63 C62 H62A 119.5 . . ? C58 C63 C62 118.11(19) . . ? C58 C63 P6 120.75(15) . . ? C62 C63 P6 120.92(16) . . ? C65 C64 P7 114.99(15) . . ? C65 C64 H64A 108.5 . . ? P7 C64 H64A 108.5 . . ? C65 C64 H64B 108.5 . . ? P7 C64 H64B 108.5 . . ? H64A C64 H64B 107.5 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 P7 118.69(14) . . ? C67 C66 H66A 107.6 . . ? P7 C66 H66A 107.6 . . ? C67 C66 H66B 107.6 . . ? P7 C66 H66B 107.6 . . ? H66A C66 H66B 107.1 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N6 C68 P7 112.96(14) . . ? N6 C68 H68A 109.0 . . ? P7 C68 H68A 109.0 . . ? N6 C68 H68B 109.0 . . ? P7 C68 H68B 109.0 . . ? H68A C68 H68B 107.8 . . ? N6 C69 H69A 109.5 . . ? N6 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N6 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N6 C70 P8 112.52(14) . . ? N6 C70 H70A 109.1 . . ? P8 C70 H70A 109.1 . . ? N6 C70 H70B 109.1 . . ? P8 C70 H70B 109.1 . . ? H70A C70 H70B 107.8 . . ? C72 C71 P8 117.46(16) . . ? C72 C71 H71A 107.9 . . ? P8 C71 H71A 107.9 . . ? C72 C71 H71B 107.9 . . ? P8 C71 H71B 107.9 . . ? H71A C71 H71B 107.2 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 P8 115.31(16) . . ? C74 C73 H73A 108.4 . . ? P8 C73 H73A 108.4 . . ? C74 C73 H73B 108.4 . . ? P8 C73 H73B 108.4 . . ? H73A C73 H73B 107.5 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.341 _refine_diff_density_min -1.464 _refine_diff_density_rms 0.129 #===END data_trans-Mo(N2)2(PEtNBnPEt)2_(trans-5) _database_code_depnum_ccdc_archive 'CCDC 854191' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H31 Mo0.50 N3 P2' _chemical_formula_weight 387.36 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' _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 8.6590(8) _cell_length_b 11.0792(11) _cell_length_c 11.0863(11) _cell_angle_alpha 100.910(3) _cell_angle_beta 108.761(3) _cell_angle_gamma 93.405(3) _cell_volume 980.54(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9878 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 33.34 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 410 _exptl_absorpt_coefficient_mu 0.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9201 _exptl_absorpt_correction_T_max 0.9690 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23514 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 33.37 _reflns_number_total 7522 _reflns_number_gt 6633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0245P)^2^+0.3097P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7522 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0624 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.5000 1.0000 0.5000 0.00955(3) Uani 1 2 d S . . N1 N 0.22329(11) 0.75714(9) 0.60746(9) 0.01428(17) Uani 1 1 d . . . N2 N 0.66572(12) 0.89037(9) 0.46548(9) 0.01475(17) Uani 1 1 d . . . N3 N 0.75566(13) 0.82773(11) 0.44614(11) 0.0237(2) Uani 1 1 d . . . P1 P 0.28194(3) 0.82464(3) 0.39484(3) 0.01231(6) Uani 1 1 d . . . P2 P 0.51821(3) 0.92171(3) 0.69671(3) 0.01149(5) Uani 1 1 d . . . C1 C 0.34999(15) 0.67011(11) 0.36532(12) 0.0194(2) Uani 1 1 d . . . H1A H 0.3895 0.6633 0.2902 0.023 Uiso 1 1 calc R . . H1B H 0.4456 0.6666 0.4425 0.023 Uiso 1 1 calc R . . C2 C 0.22536(18) 0.55627(12) 0.33817(14) 0.0259(3) Uani 1 1 d . . . H2A H 0.2774 0.4811 0.3247 0.039 Uiso 1 1 calc R . . H2B H 0.1315 0.5556 0.2596 0.039 Uiso 1 1 calc R . . H2C H 0.1872 0.5591 0.4127 0.039 Uiso 1 1 calc R . . C3 C 0.11686(14) 0.81442(11) 0.23625(11) 0.0181(2) Uani 1 1 d . . . H3A H 0.1664 0.8087 0.1667 0.022 Uiso 1 1 calc R . . H3B H 0.0401 0.7376 0.2160 0.022 Uiso 1 1 calc R . . C4 C 0.02026(16) 0.92529(14) 0.23561(13) 0.0265(3) Uani 1 1 d . . . H4A H -0.0537 0.9215 0.1466 0.040 Uiso 1 1 calc R . . H4B H 0.0969 1.0022 0.2663 0.040 Uiso 1 1 calc R . . H4C H -0.0444 0.9233 0.2935 0.040 Uiso 1 1 calc R . . C5 C 0.14399(13) 0.80071(11) 0.48813(11) 0.0158(2) Uani 1 1 d . . . H5A H 0.1023 0.8799 0.5119 0.019 Uiso 1 1 calc R . . H5B H 0.0483 0.7395 0.4312 0.019 Uiso 1 1 calc R . . C6 C 0.09574(14) 0.69960(12) 0.64851(12) 0.0191(2) Uani 1 1 d . . . H6A H 0.0114 0.6458 0.5708 0.023 Uiso 1 1 calc R . . H6B H 0.0412 0.7656 0.6857 0.023 Uiso 1 1 calc R . . C7 C 0.13660(17) 0.64509(12) 0.86679(12) 0.0229(2) Uani 1 1 d . . . H7A H 0.0804 0.7125 0.8884 0.027 Uiso 1 1 calc R . . C8 C 0.19120(19) 0.56868(14) 0.95437(13) 0.0300(3) Uani 1 1 d . . . H8A H 0.1717 0.5839 1.0351 0.036 Uiso 1 1 calc R . . C9 C 0.2735(2) 0.47108(15) 0.92384(16) 0.0350(3) Uani 1 1 d . . . H9A H 0.3108 0.4192 0.9836 0.042 Uiso 1 1 calc R . . C10 C 0.3017(2) 0.44873(15) 0.80584(17) 0.0356(3) Uani 1 1 d . . . H10A H 0.3582 0.3814 0.7846 0.043 Uiso 1 1 calc R . . C11 C 0.24736(18) 0.52465(13) 0.71902(14) 0.0272(3) Uani 1 1 d . . . H11A H 0.2674 0.5091 0.6385 0.033 Uiso 1 1 calc R . . C12 C 0.16382(14) 0.62333(11) 0.74833(12) 0.0175(2) Uani 1 1 d . . . C13 C 0.32485(14) 0.85830(11) 0.71404(11) 0.0152(2) Uani 1 1 d . . . H13A H 0.3535 0.8285 0.7963 0.018 Uiso 1 1 calc R . . H13B H 0.2580 0.9268 0.7225 0.018 Uiso 1 1 calc R . . C14 C 0.63941(15) 0.79086(12) 0.72221(12) 0.0192(2) Uani 1 1 d . . . H14A H 0.5768 0.7168 0.6547 0.023 Uiso 1 1 calc R . . H14B H 0.7426 0.8104 0.7053 0.023 Uiso 1 1 calc R . . C15 C 0.6854(2) 0.75506(16) 0.85300(14) 0.0372(4) Uani 1 1 d . . . H15A H 0.7451 0.6827 0.8504 0.056 Uiso 1 1 calc R . . H15B H 0.5854 0.7347 0.8723 0.056 Uiso 1 1 calc R . . H15C H 0.7555 0.8245 0.9211 0.056 Uiso 1 1 calc R . . C16 C 0.59490(14) 1.02523(11) 0.86178(11) 0.0163(2) Uani 1 1 d . . . H16A H 0.5754 0.9795 0.9252 0.020 Uiso 1 1 calc R . . H16B H 0.7151 1.0483 0.8873 0.020 Uiso 1 1 calc R . . C17 C 0.51226(15) 1.14346(11) 0.86921(12) 0.0200(2) Uani 1 1 d . . . H17A H 0.5638 1.1977 0.9561 0.030 Uiso 1 1 calc R . . H17B H 0.3950 1.1218 0.8535 0.030 Uiso 1 1 calc R . . H17C H 0.5251 1.1866 0.8029 0.030 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 0.00894(6) 0.01018(6) 0.00990(5) 0.00205(4) 0.00384(4) 0.00094(4) N1 0.0122(4) 0.0163(4) 0.0154(4) 0.0056(3) 0.0054(3) -0.0010(3) N2 0.0139(4) 0.0160(4) 0.0138(4) 0.0033(3) 0.0044(3) 0.0001(3) N3 0.0182(5) 0.0272(6) 0.0256(5) 0.0031(4) 0.0085(4) 0.0064(4) P1 0.01097(12) 0.01250(12) 0.01281(12) 0.00220(10) 0.00379(9) -0.00035(9) P2 0.01142(12) 0.01265(12) 0.01125(11) 0.00331(9) 0.00460(9) 0.00154(9) C1 0.0189(5) 0.0132(5) 0.0240(5) 0.0014(4) 0.0062(4) 0.0011(4) C2 0.0324(7) 0.0138(5) 0.0293(6) -0.0004(5) 0.0116(5) -0.0035(5) C3 0.0150(5) 0.0214(6) 0.0150(5) 0.0033(4) 0.0027(4) -0.0018(4) C4 0.0202(6) 0.0357(7) 0.0215(6) 0.0086(5) 0.0021(5) 0.0092(5) C5 0.0118(4) 0.0194(5) 0.0170(5) 0.0072(4) 0.0046(4) 0.0004(4) C6 0.0140(5) 0.0227(6) 0.0229(5) 0.0101(5) 0.0071(4) -0.0002(4) C7 0.0264(6) 0.0212(6) 0.0189(5) 0.0015(5) 0.0079(5) -0.0050(5) C8 0.0370(8) 0.0324(7) 0.0166(5) 0.0064(5) 0.0057(5) -0.0095(6) C9 0.0395(8) 0.0325(8) 0.0326(7) 0.0209(6) 0.0051(6) -0.0013(6) C10 0.0421(9) 0.0299(8) 0.0434(9) 0.0204(7) 0.0174(7) 0.0135(6) C11 0.0326(7) 0.0278(7) 0.0284(6) 0.0123(5) 0.0159(6) 0.0079(5) C12 0.0154(5) 0.0182(5) 0.0192(5) 0.0066(4) 0.0058(4) -0.0035(4) C13 0.0144(5) 0.0167(5) 0.0156(5) 0.0029(4) 0.0074(4) -0.0002(4) C14 0.0224(6) 0.0221(6) 0.0180(5) 0.0090(4) 0.0097(4) 0.0103(4) C15 0.0573(10) 0.0433(9) 0.0233(6) 0.0192(6) 0.0186(7) 0.0341(8) C16 0.0185(5) 0.0181(5) 0.0122(4) 0.0028(4) 0.0056(4) 0.0006(4) C17 0.0227(6) 0.0189(5) 0.0174(5) -0.0006(4) 0.0083(4) 0.0012(4) _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 2.0163(10) . ? Mo1 N2 2.0163(10) 2_676 ? Mo1 P1 2.4474(3) 2_676 ? Mo1 P1 2.4474(3) . ? Mo1 P2 2.4585(3) . ? Mo1 P2 2.4585(3) 2_676 ? N1 C13 1.4625(14) . ? N1 C5 1.4668(14) . ? N1 C6 1.4773(15) . ? N2 N3 1.1178(14) . ? P1 C1 1.8486(12) . ? P1 C5 1.8513(12) . ? P1 C3 1.8536(11) . ? P2 C14 1.8515(12) . ? P2 C16 1.8544(11) . ? P2 C13 1.8579(12) . ? C1 C2 1.5270(18) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.5265(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C12 1.5099(17) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.3872(17) . ? C7 C8 1.395(2) . ? C7 H7A 0.9500 . ? C8 C9 1.378(2) . ? C8 H8A 0.9500 . ? C9 C10 1.386(2) . ? C9 H9A 0.9500 . ? C10 C11 1.385(2) . ? C10 H10A 0.9500 . ? C11 C12 1.3910(18) . ? C11 H11A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.5110(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.5307(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 N2 180.0 . 2_676 ? N2 Mo1 P1 90.26(3) . 2_676 ? N2 Mo1 P1 89.74(3) 2_676 2_676 ? N2 Mo1 P1 89.74(3) . . ? N2 Mo1 P1 90.26(3) 2_676 . ? P1 Mo1 P1 180.0 2_676 . ? N2 Mo1 P2 90.21(3) . . ? N2 Mo1 P2 89.79(3) 2_676 . ? P1 Mo1 P2 97.255(11) 2_676 . ? P1 Mo1 P2 82.744(11) . . ? N2 Mo1 P2 89.79(3) . 2_676 ? N2 Mo1 P2 90.21(3) 2_676 2_676 ? P1 Mo1 P2 82.744(11) 2_676 2_676 ? P1 Mo1 P2 97.257(11) . 2_676 ? P2 Mo1 P2 180.0 . 2_676 ? C13 N1 C5 111.83(9) . . ? C13 N1 C6 109.02(9) . . ? C5 N1 C6 109.31(9) . . ? N3 N2 Mo1 178.71(10) . . ? C1 P1 C5 101.86(6) . . ? C1 P1 C3 100.23(6) . . ? C5 P1 C3 96.32(5) . . ? C1 P1 Mo1 116.17(4) . . ? C5 P1 Mo1 114.78(4) . . ? C3 P1 Mo1 123.68(4) . . ? C14 P2 C16 101.76(5) . . ? C14 P2 C13 100.17(6) . . ? C16 P2 C13 94.63(5) . . ? C14 P2 Mo1 116.09(4) . . ? C16 P2 Mo1 121.66(4) . . ? C13 P2 Mo1 118.37(4) . . ? C2 C1 P1 117.98(9) . . ? C2 C1 H1A 107.8 . . ? P1 C1 H1A 107.8 . . ? C2 C1 H1B 107.8 . . ? P1 C1 H1B 107.8 . . ? H1A C1 H1B 107.1 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 112.88(8) . . ? C4 C3 H3A 109.0 . . ? P1 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? P1 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 P1 113.75(7) . . ? N1 C5 H5A 108.8 . . ? P1 C5 H5A 108.8 . . ? N1 C5 H5B 108.8 . . ? P1 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N1 C6 C12 112.99(9) . . ? N1 C6 H6A 109.0 . . ? C12 C6 H6A 109.0 . . ? N1 C6 H6B 109.0 . . ? C12 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C12 C7 C8 120.45(13) . . ? C12 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C9 C8 C7 120.07(13) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 119.93(14) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 119.93(15) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.80(13) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C7 C12 C11 118.82(12) . . ? C7 C12 C6 121.19(12) . . ? C11 C12 C6 119.88(11) . . ? N1 C13 P2 115.89(8) . . ? N1 C13 H13A 108.3 . . ? P2 C13 H13A 108.3 . . ? N1 C13 H13B 108.3 . . ? P2 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C15 C14 P2 118.98(9) . . ? C15 C14 H14A 107.6 . . ? P2 C14 H14A 107.6 . . ? C15 C14 H14B 107.6 . . ? P2 C14 H14B 107.6 . . ? H14A C14 H14B 107.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 P2 112.95(8) . . ? C17 C16 H16A 109.0 . . ? P2 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? P2 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.518 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.070 #===END data_trans-W(N2)2(PEtNMePEt)2/trans-WCl2(PEtNMePEt)2_(trans-12) _database_code_depnum_ccdc_archive 'CCDC 854192' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H42 Cl0.72 N1.54 P3 W0.50' _chemical_formula_weight 622.81 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4043(8) _cell_length_b 11.0166(11) _cell_length_c 16.7489(16) _cell_angle_alpha 88.878(3) _cell_angle_beta 83.125(3) _cell_angle_gamma 72.038(3) _cell_volume 1464.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9674 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 33.36 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 2.242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6627 _exptl_absorpt_correction_T_max 0.6627 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38753 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 33.46 _reflns_number_total 11204 _reflns_number_gt 11121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0226P)^2^+0.2654P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11204 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0173 _refine_ls_R_factor_gt 0.0170 _refine_ls_wR_factor_ref 0.0411 _refine_ls_wR_factor_gt 0.0410 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.5000 0.0000 0.5000 0.01163(2) Uani 1 2 d S . . Cl1 Cl 0.75786(8) -0.00530(6) 0.41435(4) 0.0176(3) Uani 0.725(5) 1 d P A 1 N2 N 0.7108(11) -0.0122(7) 0.4303(5) 0.0230(12) Uani 0.275(5) 1 d P A 2 N3 N 0.8358(11) -0.0248(5) 0.3883(4) 0.0284(10) Uani 0.275(5) 1 d P A 2 N1 N 0.34147(12) 0.32362(9) 0.37558(6) 0.01619(16) Uani 1 1 d . A . P1 P 0.34604(3) 0.07162(2) 0.381896(16) 0.01345(5) Uani 1 1 d . A . P2 P 0.55762(3) -0.23071(2) 0.477308(16) 0.01381(5) Uani 1 1 d . . . P3 P 0.76010(4) 0.20667(3) 0.065677(19) 0.01965(5) Uani 1 1 d . . . C1 C 0.36921(14) -0.03145(11) 0.29340(7) 0.01844(19) Uani 1 1 d . . . H1A H 0.3215 -0.1012 0.3095 0.022 Uiso 1 1 calc R A . H1B H 0.3023 0.0193 0.2526 0.022 Uiso 1 1 calc R . . C2 C 0.55066(15) -0.09012(12) 0.25494(7) 0.0233(2) Uani 1 1 d . A . H2A H 0.5539 -0.1508 0.2123 0.035 Uiso 1 1 calc R . . H2B H 0.6204 -0.1347 0.2959 0.035 Uiso 1 1 calc R . . H2C H 0.5942 -0.0225 0.2319 0.035 Uiso 1 1 calc R . . C3 C 0.11507(13) 0.13536(11) 0.40330(7) 0.01874(19) Uani 1 1 d . . . H3A H 0.0733 0.0658 0.4262 0.022 Uiso 1 1 calc R A . H3B H 0.0883 0.2026 0.4456 0.022 Uiso 1 1 calc R . . C4 C 0.01611(15) 0.19105(13) 0.33397(8) 0.0252(2) Uani 1 1 d . A . H4A H -0.1042 0.2232 0.3537 0.038 Uiso 1 1 calc R . . H4B H 0.0347 0.1246 0.2927 0.038 Uiso 1 1 calc R . . H4C H 0.0539 0.2612 0.3107 0.038 Uiso 1 1 calc R . . C5 C 0.39619(14) 0.20556(10) 0.32720(6) 0.01694(18) Uani 1 1 d . . . H5A H 0.5193 0.1818 0.3114 0.020 Uiso 1 1 calc R A . H5B H 0.3406 0.2205 0.2775 0.020 Uiso 1 1 calc R . . C6 C 0.31613(16) 0.43437(11) 0.32318(7) 0.0224(2) Uani 1 1 d . . . H6A H 0.2769 0.5129 0.3561 0.034 Uiso 1 1 calc R A . H6B H 0.2317 0.4341 0.2876 0.034 Uiso 1 1 calc R . . H6C H 0.4228 0.4303 0.2907 0.034 Uiso 1 1 calc R . . C7 C 0.46177(14) 0.32468(10) 0.43124(7) 0.01747(18) Uani 1 1 d . . . H7A H 0.4453 0.4141 0.4475 0.021 Uiso 1 1 calc R A . H7B H 0.5773 0.2901 0.4031 0.021 Uiso 1 1 calc R . . C8 C 0.42725(14) -0.29387(10) 0.41866(7) 0.01759(19) Uani 1 1 d . . . H8A H 0.4462 -0.2713 0.3616 0.021 Uiso 1 1 calc R A . H8B H 0.4646 -0.3881 0.4216 0.021 Uiso 1 1 calc R . . C9 C 0.23877(14) -0.24350(11) 0.44756(8) 0.0208(2) Uani 1 1 d . A . H9A H 0.1761 -0.2731 0.4105 0.031 Uiso 1 1 calc R . . H9B H 0.2025 -0.1500 0.4491 0.031 Uiso 1 1 calc R . . H9C H 0.2168 -0.2751 0.5015 0.031 Uiso 1 1 calc R . . C10 C 0.77020(14) -0.32025(11) 0.42819(7) 0.01906(19) Uani 1 1 d . . . H10A H 0.7744 -0.3017 0.3700 0.023 Uiso 1 1 calc R A . H10B H 0.8531 -0.2865 0.4499 0.023 Uiso 1 1 calc R . . C11 C 0.82726(15) -0.46501(11) 0.43719(8) 0.0227(2) Uani 1 1 d . A . H11A H 0.9364 -0.5021 0.4048 0.034 Uiso 1 1 calc R . . H11B H 0.7438 -0.5001 0.4187 0.034 Uiso 1 1 calc R . . H11C H 0.8382 -0.4858 0.4938 0.034 Uiso 1 1 calc R . . C12 C 0.75375(17) 0.37745(14) 0.18484(8) 0.0277(2) Uani 1 1 d . . . H12A H 0.7354 0.3125 0.2195 0.033 Uiso 1 1 calc R . . C13 C 0.77016(19) 0.48680(15) 0.21721(9) 0.0329(3) Uani 1 1 d . . . H13A H 0.7611 0.4972 0.2739 0.039 Uiso 1 1 calc R . . C14 C 0.79987(17) 0.58163(14) 0.16723(9) 0.0302(3) Uani 1 1 d . . . H14A H 0.8128 0.6561 0.1896 0.036 Uiso 1 1 calc R . . C15 C 0.81052(16) 0.56715(12) 0.08468(9) 0.0270(2) Uani 1 1 d . . . H15A H 0.8301 0.6320 0.0503 0.032 Uiso 1 1 calc R . . C16 C 0.79258(15) 0.45778(12) 0.05198(8) 0.0227(2) Uani 1 1 d . . . H16A H 0.7999 0.4485 -0.0047 0.027 Uiso 1 1 calc R . . C17 C 0.76396(14) 0.36162(11) 0.10155(7) 0.0205(2) Uani 1 1 d . . . C18 C 0.94573(16) 0.15155(13) -0.08419(9) 0.0286(3) Uani 1 1 d . . . H18A H 1.0312 0.1011 -0.0544 0.034 Uiso 1 1 calc R . . C19 C 0.97765(19) 0.15615(16) -0.16743(10) 0.0380(3) Uani 1 1 d . . . H19A H 1.0842 0.1084 -0.1942 0.046 Uiso 1 1 calc R . . C20 C 0.8549(2) 0.22995(17) -0.21111(9) 0.0365(3) Uani 1 1 d . . . H20A H 0.8774 0.2343 -0.2679 0.044 Uiso 1 1 calc R . . C21 C 0.6983(2) 0.29790(15) -0.17189(8) 0.0317(3) Uani 1 1 d . . . H21A H 0.6134 0.3483 -0.2020 0.038 Uiso 1 1 calc R . . C22 C 0.66536(16) 0.29253(13) -0.08887(8) 0.0246(2) Uani 1 1 d . . . H22A H 0.5575 0.3385 -0.0626 0.030 Uiso 1 1 calc R . . C23 C 0.78928(14) 0.22034(11) -0.04393(7) 0.0195(2) Uani 1 1 d . . . C24 C 0.50062(16) 0.10256(13) 0.08083(8) 0.0255(2) Uani 1 1 d . . . H24A H 0.5900 0.0257 0.0681 0.031 Uiso 1 1 calc R . . C25 C 0.33572(18) 0.09866(16) 0.09453(8) 0.0310(3) Uani 1 1 d . . . H25A H 0.3128 0.0200 0.0903 0.037 Uiso 1 1 calc R . . C26 C 0.20546(17) 0.20984(17) 0.11432(8) 0.0327(3) Uani 1 1 d . . . H26A H 0.0927 0.2076 0.1241 0.039 Uiso 1 1 calc R . . C27 C 0.23939(16) 0.32435(15) 0.11995(8) 0.0303(3) Uani 1 1 d . . . H27A H 0.1496 0.4005 0.1339 0.036 Uiso 1 1 calc R . . C28 C 0.40472(15) 0.32891(13) 0.10531(8) 0.0247(2) Uani 1 1 d . . . H28A H 0.4268 0.4081 0.1089 0.030 Uiso 1 1 calc R . . C29 C 0.53705(14) 0.21759(12) 0.08550(7) 0.0206(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01326(3) 0.01054(3) 0.01215(3) -0.00049(2) -0.00166(2) -0.00510(2) Cl1 0.0164(5) 0.0184(2) 0.0189(4) -0.00024(18) 0.0000(3) -0.0073(2) N2 0.025(3) 0.021(2) 0.024(3) 0.004(2) -0.008(2) -0.008(2) N3 0.023(3) 0.032(2) 0.029(2) -0.0040(19) 0.003(3) -0.0092(19) N1 0.0211(4) 0.0133(4) 0.0150(4) 0.0013(3) -0.0032(3) -0.0062(3) P1 0.01457(10) 0.01286(11) 0.01359(11) -0.00041(9) -0.00194(9) -0.00506(9) P2 0.01594(11) 0.01189(11) 0.01480(11) -0.00057(9) -0.00206(9) -0.00592(9) P3 0.01651(12) 0.01798(13) 0.02225(14) 0.00240(10) -0.00443(10) -0.00146(10) C1 0.0221(5) 0.0167(4) 0.0164(5) -0.0016(4) -0.0044(4) -0.0050(4) C2 0.0252(5) 0.0213(5) 0.0199(5) -0.0039(4) -0.0020(4) -0.0021(4) C3 0.0159(4) 0.0217(5) 0.0184(5) 0.0010(4) -0.0025(4) -0.0053(4) C4 0.0181(5) 0.0316(6) 0.0236(6) 0.0054(5) -0.0057(4) -0.0032(4) C5 0.0216(5) 0.0153(4) 0.0145(4) 0.0001(3) -0.0009(4) -0.0072(4) C6 0.0299(6) 0.0168(5) 0.0210(5) 0.0039(4) -0.0050(4) -0.0072(4) C7 0.0215(5) 0.0154(4) 0.0183(5) 0.0018(4) -0.0038(4) -0.0094(4) C8 0.0207(4) 0.0142(4) 0.0200(5) -0.0010(4) -0.0051(4) -0.0073(4) C9 0.0193(5) 0.0204(5) 0.0248(5) 0.0003(4) -0.0050(4) -0.0084(4) C10 0.0188(4) 0.0171(5) 0.0207(5) -0.0025(4) -0.0014(4) -0.0048(4) C11 0.0240(5) 0.0170(5) 0.0240(5) -0.0023(4) -0.0046(4) -0.0011(4) C12 0.0296(6) 0.0319(6) 0.0198(5) -0.0002(5) -0.0034(5) -0.0067(5) C13 0.0338(7) 0.0390(8) 0.0225(6) -0.0085(5) -0.0042(5) -0.0055(6) C14 0.0260(6) 0.0272(6) 0.0342(7) -0.0107(5) -0.0057(5) -0.0022(5) C15 0.0269(6) 0.0220(5) 0.0312(6) -0.0019(5) -0.0059(5) -0.0052(4) C16 0.0243(5) 0.0216(5) 0.0211(5) 0.0004(4) -0.0060(4) -0.0043(4) C17 0.0175(4) 0.0221(5) 0.0200(5) -0.0006(4) -0.0039(4) -0.0024(4) C18 0.0204(5) 0.0280(6) 0.0345(7) -0.0059(5) 0.0027(5) -0.0049(4) C19 0.0314(7) 0.0448(9) 0.0359(8) -0.0136(7) 0.0125(6) -0.0146(6) C20 0.0462(8) 0.0494(9) 0.0218(6) -0.0083(6) 0.0040(6) -0.0289(7) C21 0.0377(7) 0.0394(7) 0.0224(6) 0.0016(5) -0.0078(5) -0.0165(6) C22 0.0236(5) 0.0268(6) 0.0217(5) -0.0013(4) -0.0036(4) -0.0048(4) C23 0.0181(4) 0.0171(5) 0.0225(5) -0.0026(4) -0.0013(4) -0.0043(4) C24 0.0265(5) 0.0299(6) 0.0208(5) 0.0005(5) -0.0007(4) -0.0106(5) C25 0.0336(6) 0.0446(8) 0.0213(6) 0.0014(5) -0.0033(5) -0.0217(6) C26 0.0220(5) 0.0579(9) 0.0206(6) 0.0061(6) -0.0047(5) -0.0156(6) C27 0.0194(5) 0.0437(8) 0.0215(6) 0.0046(5) -0.0032(4) -0.0003(5) C28 0.0199(5) 0.0285(6) 0.0214(5) 0.0039(4) -0.0038(4) -0.0012(4) C29 0.0185(4) 0.0254(5) 0.0167(5) 0.0030(4) -0.0029(4) -0.0047(4) _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 W1 N2 1.971(9) . ? W1 N2 1.971(9) 2_656 ? W1 Cl1 2.4369(7) . ? W1 Cl1 2.4370(7) 2_656 ? W1 P2 2.4645(4) . ? W1 P2 2.4645(4) 2_656 ? W1 P1 2.4762(3) 2_656 ? W1 P1 2.4762(3) . ? N2 N3 1.163(15) . ? N1 C7 1.4578(14) . ? N1 C5 1.4638(14) . ? N1 C6 1.4652(15) . ? P1 C1 1.8397(11) . ? P1 C3 1.8418(11) . ? P1 C5 1.8526(11) . ? P2 C8 1.8451(11) . ? P2 C7 1.8511(11) 2_656 ? P2 C10 1.8533(11) . ? P3 C29 1.8309(12) . ? P3 C17 1.8316(13) . ? P3 C23 1.8323(13) . ? C1 C2 1.5269(16) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.5182(17) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 P2 1.8511(11) 2_656 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.5285(16) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.5271(16) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.382(2) . ? C12 C17 1.3985(17) . ? C12 H12A 0.9500 . ? C13 C14 1.390(2) . ? C13 H13A 0.9500 . ? C14 C15 1.384(2) . ? C14 H14A 0.9500 . ? C15 C16 1.3901(18) . ? C15 H15A 0.9500 . ? C16 C17 1.3944(17) . ? C16 H16A 0.9500 . ? C18 C19 1.391(2) . ? C18 C23 1.3967(16) . ? C18 H18A 0.9500 . ? C19 C20 1.379(3) . ? C19 H19A 0.9500 . ? C20 C21 1.389(2) . ? C20 H20A 0.9500 . ? C21 C22 1.3885(19) . ? C21 H21A 0.9500 . ? C22 C23 1.3918(17) . ? C22 H22A 0.9500 . ? C24 C25 1.3912(18) . ? C24 C29 1.3981(18) . ? C24 H24A 0.9500 . ? C25 C26 1.382(2) . ? C25 H25A 0.9500 . ? C26 C27 1.384(2) . ? C26 H26A 0.9500 . ? C27 C28 1.3979(18) . ? C27 H27A 0.9500 . ? C28 C29 1.3918(17) . ? C28 H28A 0.9500 . ? 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 W1 N2 180.0(5) . 2_656 ? N2 W1 Cl1 2.4(2) . . ? N2 W1 Cl1 177.6(2) 2_656 . ? N2 W1 Cl1 177.6(2) . 2_656 ? N2 W1 Cl1 2.4(2) 2_656 2_656 ? Cl1 W1 Cl1 180.00(3) . 2_656 ? N2 W1 P2 88.3(2) . . ? N2 W1 P2 91.7(2) 2_656 . ? Cl1 W1 P2 90.707(17) . . ? Cl1 W1 P2 89.294(17) 2_656 . ? N2 W1 P2 91.7(2) . 2_656 ? N2 W1 P2 88.3(2) 2_656 2_656 ? Cl1 W1 P2 89.293(17) . 2_656 ? Cl1 W1 P2 90.706(17) 2_656 2_656 ? P2 W1 P2 180.0 . 2_656 ? N2 W1 P1 91.7(2) . 2_656 ? N2 W1 P1 88.3(2) 2_656 2_656 ? Cl1 W1 P1 92.160(19) . 2_656 ? Cl1 W1 P1 87.841(19) 2_656 2_656 ? P2 W1 P1 83.304(10) . 2_656 ? P2 W1 P1 96.696(10) 2_656 2_656 ? N2 W1 P1 88.3(2) . . ? N2 W1 P1 91.7(2) 2_656 . ? Cl1 W1 P1 87.841(19) . . ? Cl1 W1 P1 92.159(19) 2_656 . ? P2 W1 P1 96.695(10) . . ? P2 W1 P1 83.305(10) 2_656 . ? P1 W1 P1 180.0 2_656 . ? N3 N2 W1 177.1(6) . . ? C7 N1 C5 111.45(9) . . ? C7 N1 C6 110.48(9) . . ? C5 N1 C6 110.18(9) . . ? C1 P1 C3 101.24(5) . . ? C1 P1 C5 96.96(5) . . ? C3 P1 C5 101.39(5) . . ? C1 P1 W1 123.12(4) . . ? C3 P1 W1 115.82(4) . . ? C5 P1 W1 114.68(4) . . ? C8 P2 C7 96.79(5) . 2_656 ? C8 P2 C10 99.85(5) . . ? C7 P2 C10 102.12(5) 2_656 . ? C8 P2 W1 122.05(4) . . ? C7 P2 W1 115.60(4) 2_656 . ? C10 P2 W1 116.76(4) . . ? C29 P3 C17 103.15(5) . . ? C29 P3 C23 102.23(5) . . ? C17 P3 C23 103.03(5) . . ? C2 C1 P1 114.40(8) . . ? C2 C1 H1A 108.7 . . ? P1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? P1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 117.79(8) . . ? C4 C3 H3A 107.9 . . ? P1 C3 H3A 107.9 . . ? C4 C3 H3B 107.9 . . ? P1 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 P1 112.42(7) . . ? N1 C5 H5A 109.1 . . ? P1 C5 H5A 109.1 . . ? N1 C5 H5B 109.1 . . ? P1 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 P2 113.51(7) . 2_656 ? N1 C7 H7A 108.9 . . ? P2 C7 H7A 108.9 2_656 . ? N1 C7 H7B 108.9 . . ? P2 C7 H7B 108.9 2_656 . ? H7A C7 H7B 107.7 . . ? C9 C8 P2 113.66(8) . . ? C9 C8 H8A 108.8 . . ? P2 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? P2 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P2 117.09(8) . . ? C11 C10 H10A 108.0 . . ? P2 C10 H10A 108.0 . . ? C11 C10 H10B 108.0 . . ? P2 C10 H10B 108.0 . . ? H10A C10 H10B 107.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 120.55(13) . . ? C13 C12 H12A 119.7 . . ? C17 C12 H12A 119.7 . . ? C12 C13 C14 120.34(13) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C15 C14 C13 119.73(13) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 120.06(13) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C17 120.69(12) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C16 C17 C12 118.63(12) . . ? C16 C17 P3 124.68(9) . . ? C12 C17 P3 116.37(10) . . ? C19 C18 C23 120.67(14) . . ? C19 C18 H18A 119.7 . . ? C23 C18 H18A 119.7 . . ? C20 C19 C18 120.09(13) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 119.79(14) . . ? C19 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? C20 C21 C22 120.29(14) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C21 C22 C23 120.46(12) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C18 118.67(12) . . ? C22 C23 P3 124.21(9) . . ? C18 C23 P3 117.11(10) . . ? C25 C24 C29 121.13(13) . . ? C25 C24 H24A 119.4 . . ? C29 C24 H24A 119.4 . . ? C26 C25 C24 119.67(14) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C25 C26 C27 119.97(12) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C26 C27 C28 120.53(13) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C29 C28 C27 120.06(13) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C24 118.64(11) . . ? C28 C29 P3 125.57(10) . . ? C24 C29 P3 115.79(9) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.819 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.067 #===END data_trans-W(N2)2(dppe)(PPhNMePPh)_(10) _database_code_depnum_ccdc_archive 'CCDC 854193' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H51 N5 P4 W' _chemical_formula_weight 1065.72 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' W W -0.8490 6.8722 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.6481(7) _cell_length_b 11.6215(3) _cell_length_c 17.3542(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.1780(10) _cell_angle_gamma 90.00 _cell_volume 4643.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9501 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 34.42 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 2.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6748 _exptl_absorpt_correction_T_max 0.8563 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 63240 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 34.81 _reflns_number_total 18422 _reflns_number_gt 15560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0206P)^2^+1.1759P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18422 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.0468 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.257163(2) 0.929122(5) 0.279177(3) 0.00975(2) Uani 1 1 d . . . N1 N 0.26820(6) 1.03606(12) 0.06207(7) 0.0167(3) Uani 1 1 d . . . N2 N 0.28455(5) 0.79164(11) 0.22853(7) 0.0138(2) Uani 1 1 d . . . N3 N 0.29999(6) 0.71884(12) 0.19532(8) 0.0189(3) Uani 1 1 d . . . N4 N 0.23114(6) 1.07952(11) 0.31990(7) 0.0150(2) Uani 1 1 d . . . N5 N 0.21782(6) 1.16359(13) 0.34183(9) 0.0234(3) Uani 1 1 d . . . P1 P 0.326560(16) 1.03578(3) 0.22305(2) 0.01177(7) Uani 1 1 d . . . P2 P 0.189816(16) 0.96317(4) 0.15263(2) 0.01252(7) Uani 1 1 d . . . P3 P 0.189200(16) 0.82705(3) 0.34299(2) 0.01242(7) Uani 1 1 d . . . P4 P 0.315754(16) 0.91442(3) 0.41518(2) 0.01195(7) Uani 1 1 d . . . C1 C 0.42356(7) 0.89475(14) 0.27594(9) 0.0169(3) Uani 1 1 d . . . H1A H 0.3954 0.8373 0.2783 0.020 Uiso 1 1 calc R . . C2 C 0.48212(7) 0.86655(15) 0.29631(10) 0.0212(3) Uani 1 1 d . . . H2A H 0.4936 0.7904 0.3127 0.025 Uiso 1 1 calc R . . C3 C 0.52402(8) 0.94861(17) 0.29300(12) 0.0296(4) Uani 1 1 d . . . H3A H 0.5641 0.9292 0.3070 0.035 Uiso 1 1 calc R . . C4 C 0.50670(8) 1.05903(18) 0.26911(14) 0.0352(5) Uani 1 1 d . . . H4A H 0.5351 1.1160 0.2669 0.042 Uiso 1 1 calc R . . C5 C 0.44777(8) 1.08776(16) 0.24821(12) 0.0279(4) Uani 1 1 d . . . H5A H 0.4365 1.1638 0.2312 0.033 Uiso 1 1 calc R . . C6 C 0.40534(6) 1.00591(14) 0.25205(9) 0.0152(3) Uani 1 1 d . . . C7 C 0.29917(7) 1.26497(15) 0.16989(10) 0.0215(3) Uani 1 1 d . . . H7A H 0.2823 1.2337 0.1193 0.026 Uiso 1 1 calc R . . C8 C 0.29782(8) 1.38354(15) 0.18194(11) 0.0270(4) Uani 1 1 d . . . H8A H 0.2802 1.4324 0.1394 0.032 Uiso 1 1 calc R . . C9 C 0.32179(8) 1.43039(15) 0.25492(11) 0.0232(3) Uani 1 1 d . . . H9A H 0.3215 1.5113 0.2625 0.028 Uiso 1 1 calc R . . C10 C 0.34616(9) 1.35884(15) 0.31688(11) 0.0261(4) Uani 1 1 d . . . H10A H 0.3620 1.3904 0.3677 0.031 Uiso 1 1 calc R . . C11 C 0.34769(8) 1.24119(15) 0.30542(10) 0.0238(4) Uani 1 1 d . . . H11A H 0.3644 1.1928 0.3487 0.029 Uiso 1 1 calc R . . C12 C 0.32506(6) 1.19249(13) 0.23135(9) 0.0136(3) Uani 1 1 d . . . C13 C 0.32292(7) 1.00892(14) 0.11709(9) 0.0159(3) Uani 1 1 d . . . H13A H 0.3540 1.0542 0.1016 0.019 Uiso 1 1 calc R . . H13B H 0.3316 0.9266 0.1107 0.019 Uiso 1 1 calc R . . C14 C 0.27702(8) 1.03860(19) -0.01908(10) 0.0273(4) Uani 1 1 d . . . H14A H 0.3069 1.0957 -0.0225 0.041 Uiso 1 1 calc R . . H14B H 0.2405 1.0593 -0.0559 0.041 Uiso 1 1 calc R . . H14C H 0.2896 0.9625 -0.0329 0.041 Uiso 1 1 calc R . . C15 C 0.22233(7) 0.95337(14) 0.06543(9) 0.0175(3) Uani 1 1 d . . . H15A H 0.2383 0.8749 0.0638 0.021 Uiso 1 1 calc R . . H15B H 0.1909 0.9630 0.0172 0.021 Uiso 1 1 calc R . . C16 C 0.15685(7) 1.18019(16) 0.07898(10) 0.0244(4) Uani 1 1 d . . . H16A H 0.1819 1.1638 0.0447 0.029 Uiso 1 1 calc R . . C17 C 0.12580(8) 1.28320(17) 0.07111(12) 0.0304(4) Uani 1 1 d . . . H17A H 0.1307 1.3375 0.0322 0.036 Uiso 1 1 calc R . . C18 C 0.08806(8) 1.30731(16) 0.11898(12) 0.0293(4) Uani 1 1 d . . . H18A H 0.0669 1.3774 0.1128 0.035 Uiso 1 1 calc R . . C19 C 0.08135(8) 1.22862(16) 0.17600(11) 0.0259(4) Uani 1 1 d . . . H19A H 0.0549 1.2439 0.2086 0.031 Uiso 1 1 calc R . . C20 C 0.11321(7) 1.12734(15) 0.18557(10) 0.0202(3) Uani 1 1 d . . . H20A H 0.1092 1.0748 0.2259 0.024 Uiso 1 1 calc R . . C21 C 0.15101(7) 1.10122(14) 0.13722(9) 0.0165(3) Uani 1 1 d . . . C22 C 0.14301(7) 0.74440(14) 0.11874(9) 0.0184(3) Uani 1 1 d . . . H22A H 0.1798 0.7202 0.1488 0.022 Uiso 1 1 calc R . . C23 C 0.10262(8) 0.66239(15) 0.08345(10) 0.0231(3) Uani 1 1 d . . . H23A H 0.1120 0.5829 0.0892 0.028 Uiso 1 1 calc R . . C24 C 0.04865(8) 0.69649(17) 0.03981(10) 0.0258(4) Uani 1 1 d . . . H24A H 0.0210 0.6406 0.0153 0.031 Uiso 1 1 calc R . . C25 C 0.03527(7) 0.81231(17) 0.03209(11) 0.0264(4) Uani 1 1 d . . . H25A H -0.0019 0.8358 0.0026 0.032 Uiso 1 1 calc R . . C26 C 0.07568(7) 0.89462(16) 0.06703(10) 0.0213(3) Uani 1 1 d . . . H26A H 0.0660 0.9740 0.0611 0.026 Uiso 1 1 calc R . . C27 C 0.13046(6) 0.86163(14) 0.11089(9) 0.0155(3) Uani 1 1 d . . . C28 C 0.12360(7) 0.63558(15) 0.36997(9) 0.0174(3) Uani 1 1 d . . . H28A H 0.1045 0.6883 0.3974 0.021 Uiso 1 1 calc R . . C29 C 0.10962(7) 0.51907(15) 0.36865(10) 0.0212(3) Uani 1 1 d . . . H29A H 0.0814 0.4925 0.3956 0.025 Uiso 1 1 calc R . . C30 C 0.13674(7) 0.44177(14) 0.32813(10) 0.0215(3) Uani 1 1 d . . . H30A H 0.1269 0.3625 0.3269 0.026 Uiso 1 1 calc R . . C31 C 0.17816(7) 0.48004(15) 0.28943(10) 0.0212(3) Uani 1 1 d . . . H31A H 0.1965 0.4271 0.2612 0.025 Uiso 1 1 calc R . . C32 C 0.19317(7) 0.59637(14) 0.29172(9) 0.0178(3) Uani 1 1 d . . . H32A H 0.2224 0.6218 0.2662 0.021 Uiso 1 1 calc R . . C33 C 0.16565(6) 0.67551(14) 0.33108(8) 0.0146(3) Uani 1 1 d . . . C34 C 0.11245(7) 0.99162(16) 0.38199(10) 0.0213(3) Uani 1 1 d . . . H34A H 0.1440 1.0141 0.4237 0.026 Uiso 1 1 calc R . . C35 C 0.06031(8) 1.05240(17) 0.36902(11) 0.0282(4) Uani 1 1 d . . . H35A H 0.0566 1.1162 0.4017 0.034 Uiso 1 1 calc R . . C36 C 0.01386(8) 1.02012(18) 0.30866(11) 0.0284(4) Uani 1 1 d . . . H36A H -0.0216 1.0617 0.2997 0.034 Uiso 1 1 calc R . . C37 C 0.01959(7) 0.92710(16) 0.26162(11) 0.0249(4) Uani 1 1 d . . . H37A H -0.0122 0.9045 0.2204 0.030 Uiso 1 1 calc R . . C38 C 0.07143(7) 0.86616(15) 0.27395(9) 0.0186(3) Uani 1 1 d . . . H38A H 0.0747 0.8023 0.2411 0.022 Uiso 1 1 calc R . . C39 C 0.11884(7) 0.89823(14) 0.33439(9) 0.0160(3) Uani 1 1 d . . . C40 C 0.21880(7) 0.82102(14) 0.45181(8) 0.0161(3) Uani 1 1 d . . . H40A H 0.1865 0.8298 0.4790 0.019 Uiso 1 1 calc R . . H40B H 0.2368 0.7447 0.4660 0.019 Uiso 1 1 calc R . . C41 C 0.26377(7) 0.91406(14) 0.48067(9) 0.0152(3) Uani 1 1 d . . . H41A H 0.2845 0.8983 0.5360 0.018 Uiso 1 1 calc R . . H41B H 0.2446 0.9900 0.4790 0.018 Uiso 1 1 calc R . . C42 C 0.42133(7) 1.03263(15) 0.44747(9) 0.0176(3) Uani 1 1 d . . . H42A H 0.4348 0.9690 0.4223 0.021 Uiso 1 1 calc R . . C43 C 0.45830(7) 1.12471(15) 0.47257(10) 0.0224(3) Uani 1 1 d . . . H43A H 0.4962 1.1249 0.4629 0.027 Uiso 1 1 calc R . . C44 C 0.43995(8) 1.21624(16) 0.51173(10) 0.0248(4) Uani 1 1 d . . . H44A H 0.4652 1.2793 0.5291 0.030 Uiso 1 1 calc R . . C45 C 0.38491(8) 1.21514(15) 0.52533(11) 0.0260(4) Uani 1 1 d . . . H45A H 0.3727 1.2766 0.5537 0.031 Uiso 1 1 calc R . . C46 C 0.34679(7) 1.12462(15) 0.49779(10) 0.0213(3) Uani 1 1 d . . . H46A H 0.3084 1.1264 0.5059 0.026 Uiso 1 1 calc R . . C47 C 0.36471(7) 1.03187(14) 0.45853(9) 0.0145(3) Uani 1 1 d . . . C48 C 0.38921(7) 0.78524(15) 0.53614(9) 0.0179(3) Uani 1 1 d . . . H48A H 0.3827 0.8445 0.5708 0.021 Uiso 1 1 calc R . . C49 C 0.42550(7) 0.69360(15) 0.56591(10) 0.0216(3) Uani 1 1 d . . . H49A H 0.4432 0.6899 0.6208 0.026 Uiso 1 1 calc R . . C50 C 0.43590(7) 0.60761(16) 0.51538(11) 0.0239(4) Uani 1 1 d . . . H50A H 0.4610 0.5454 0.5356 0.029 Uiso 1 1 calc R . . C51 C 0.40978(7) 0.61250(15) 0.43560(11) 0.0226(3) Uani 1 1 d . . . H51A H 0.4174 0.5543 0.4009 0.027 Uiso 1 1 calc R . . C52 C 0.37221(7) 0.70294(14) 0.40616(10) 0.0180(3) Uani 1 1 d . . . H52A H 0.3533 0.7043 0.3516 0.022 Uiso 1 1 calc R . . C53 C 0.36209(6) 0.79094(13) 0.45551(9) 0.0141(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.00940(2) 0.00985(3) 0.00980(3) 0.00004(2) 0.00180(2) -0.00037(2) N1 0.0162(6) 0.0219(7) 0.0121(6) 0.0006(5) 0.0032(5) -0.0030(5) N2 0.0125(5) 0.0144(6) 0.0143(6) 0.0025(5) 0.0024(4) -0.0019(5) N3 0.0205(6) 0.0169(7) 0.0197(6) 0.0000(5) 0.0053(5) -0.0005(5) N4 0.0141(6) 0.0165(6) 0.0141(6) 0.0001(5) 0.0024(4) -0.0004(5) N5 0.0243(7) 0.0193(7) 0.0262(7) -0.0051(6) 0.0046(6) 0.0020(6) P1 0.01161(16) 0.01073(16) 0.01303(16) 0.00052(13) 0.00295(12) -0.00074(13) P2 0.01181(16) 0.01353(17) 0.01155(16) 0.00048(13) 0.00129(12) -0.00108(14) P3 0.01091(16) 0.01433(18) 0.01196(16) 0.00044(14) 0.00248(12) -0.00096(14) P4 0.01105(16) 0.01259(18) 0.01165(16) -0.00019(13) 0.00140(12) -0.00084(13) C1 0.0157(7) 0.0154(7) 0.0193(7) -0.0019(6) 0.0034(5) -0.0001(6) C2 0.0184(7) 0.0216(8) 0.0231(8) -0.0015(6) 0.0037(6) 0.0066(6) C3 0.0136(7) 0.0358(11) 0.0381(10) 0.0051(8) 0.0033(7) 0.0034(7) C4 0.0154(8) 0.0343(11) 0.0549(13) 0.0157(10) 0.0061(8) -0.0023(8) C5 0.0160(7) 0.0251(9) 0.0413(11) 0.0115(8) 0.0039(7) -0.0009(7) C6 0.0140(6) 0.0169(7) 0.0150(7) 0.0007(6) 0.0038(5) -0.0011(6) C7 0.0236(8) 0.0173(8) 0.0214(8) 0.0007(6) 0.0003(6) 0.0034(6) C8 0.0336(10) 0.0153(8) 0.0292(9) 0.0046(7) 0.0011(7) 0.0076(7) C9 0.0289(9) 0.0117(7) 0.0318(9) -0.0012(7) 0.0127(7) 0.0002(7) C10 0.0397(10) 0.0160(8) 0.0225(8) -0.0035(7) 0.0068(7) -0.0068(7) C11 0.0367(10) 0.0150(8) 0.0171(7) 0.0007(6) 0.0011(7) -0.0045(7) C12 0.0131(6) 0.0121(7) 0.0159(6) 0.0007(5) 0.0040(5) -0.0013(5) C13 0.0166(7) 0.0155(7) 0.0165(7) -0.0005(6) 0.0059(5) -0.0008(6) C14 0.0236(8) 0.0442(11) 0.0147(7) 0.0006(7) 0.0056(6) -0.0102(8) C15 0.0196(7) 0.0199(8) 0.0133(7) -0.0028(6) 0.0046(5) -0.0042(6) C16 0.0196(8) 0.0246(9) 0.0276(9) 0.0094(7) 0.0025(6) 0.0008(7) C17 0.0272(9) 0.0221(9) 0.0375(10) 0.0148(8) -0.0017(7) 0.0001(7) C18 0.0233(9) 0.0180(8) 0.0400(11) -0.0014(8) -0.0068(7) 0.0044(7) C19 0.0247(8) 0.0231(9) 0.0270(9) -0.0047(7) -0.0003(7) 0.0065(7) C20 0.0219(8) 0.0183(8) 0.0186(7) -0.0008(6) 0.0009(6) 0.0030(6) C21 0.0130(6) 0.0168(7) 0.0173(7) 0.0007(6) -0.0017(5) -0.0011(5) C22 0.0176(7) 0.0186(8) 0.0181(7) 0.0007(6) 0.0018(5) -0.0043(6) C23 0.0252(8) 0.0185(8) 0.0257(8) -0.0023(7) 0.0061(6) -0.0073(7) C24 0.0208(8) 0.0301(10) 0.0256(8) -0.0055(7) 0.0038(6) -0.0119(7) C25 0.0158(7) 0.0317(10) 0.0283(9) -0.0025(8) -0.0018(6) -0.0048(7) C26 0.0162(7) 0.0236(8) 0.0219(8) 0.0003(7) -0.0003(6) -0.0013(6) C27 0.0137(6) 0.0198(8) 0.0125(6) -0.0010(6) 0.0023(5) -0.0028(6) C28 0.0155(7) 0.0201(8) 0.0165(7) 0.0000(6) 0.0034(5) -0.0048(6) C29 0.0190(7) 0.0246(9) 0.0192(7) 0.0012(6) 0.0028(6) -0.0101(7) C30 0.0220(8) 0.0163(8) 0.0235(8) -0.0003(6) -0.0001(6) -0.0070(6) C31 0.0235(8) 0.0177(8) 0.0214(8) -0.0022(6) 0.0032(6) -0.0022(6) C32 0.0172(7) 0.0189(8) 0.0172(7) 0.0016(6) 0.0036(5) -0.0016(6) C33 0.0127(6) 0.0166(7) 0.0133(6) 0.0013(5) 0.0003(5) -0.0029(5) C34 0.0170(7) 0.0264(9) 0.0214(8) -0.0012(7) 0.0059(6) 0.0026(6) C35 0.0253(9) 0.0320(11) 0.0297(9) -0.0022(8) 0.0110(7) 0.0069(8) C36 0.0167(8) 0.0358(11) 0.0337(10) 0.0053(8) 0.0083(7) 0.0069(7) C37 0.0137(7) 0.0327(10) 0.0274(9) 0.0070(8) 0.0028(6) -0.0002(7) C38 0.0132(7) 0.0227(8) 0.0198(7) 0.0032(6) 0.0035(5) -0.0010(6) C39 0.0127(6) 0.0190(7) 0.0171(7) 0.0031(6) 0.0052(5) 0.0002(6) C40 0.0157(7) 0.0206(8) 0.0120(6) 0.0027(6) 0.0033(5) -0.0011(6) C41 0.0149(6) 0.0189(8) 0.0116(6) -0.0007(5) 0.0029(5) -0.0011(6) C42 0.0158(7) 0.0180(7) 0.0177(7) 0.0002(6) 0.0008(5) -0.0019(6) C43 0.0171(7) 0.0243(9) 0.0227(8) 0.0022(7) -0.0017(6) -0.0057(6) C44 0.0262(8) 0.0193(8) 0.0243(8) 0.0003(7) -0.0042(6) -0.0085(7) C45 0.0293(9) 0.0162(8) 0.0297(9) -0.0062(7) 0.0010(7) -0.0012(7) C46 0.0206(8) 0.0189(8) 0.0235(8) -0.0042(6) 0.0030(6) -0.0008(6) C47 0.0156(7) 0.0135(7) 0.0124(6) 0.0009(5) -0.0009(5) -0.0011(5) C48 0.0167(7) 0.0200(8) 0.0156(7) 0.0026(6) 0.0011(5) -0.0011(6) C49 0.0163(7) 0.0262(9) 0.0204(7) 0.0092(7) 0.0002(6) 0.0001(6) C50 0.0172(7) 0.0194(8) 0.0332(9) 0.0100(7) 0.0021(6) 0.0020(6) C51 0.0217(8) 0.0155(8) 0.0304(9) 0.0001(7) 0.0054(7) 0.0016(6) C52 0.0171(7) 0.0155(7) 0.0198(7) 0.0003(6) 0.0008(5) -0.0011(6) C53 0.0117(6) 0.0148(7) 0.0151(6) 0.0021(5) 0.0016(5) -0.0015(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 W1 N2 2.0011(13) . ? W1 N4 2.0326(13) . ? W1 P1 2.4305(4) . ? W1 P2 2.4333(4) . ? W1 P4 2.4553(4) . ? W1 P3 2.4552(4) . ? N1 C13 1.457(2) . ? N1 C15 1.460(2) . ? N1 C14 1.470(2) . ? N2 N3 1.1301(18) . ? N4 N5 1.1195(19) . ? P1 C12 1.8279(15) . ? P1 C6 1.8485(15) . ? P1 C13 1.8478(15) . ? P2 C21 1.8372(17) . ? P2 C27 1.8504(16) . ? P2 C15 1.8506(16) . ? P3 C39 1.8336(16) . ? P3 C33 1.8445(16) . ? P3 C40 1.8599(15) . ? P4 C47 1.8365(16) . ? P4 C53 1.8439(16) . ? P4 C41 1.8549(15) . ? C1 C2 1.388(2) . ? C1 C6 1.395(2) . ? C1 H1A 0.9500 . ? C2 C3 1.386(3) . ? C2 H2A 0.9500 . ? C3 C4 1.382(3) . ? C3 H3A 0.9500 . ? C4 C5 1.398(3) . ? C4 H4A 0.9500 . ? C5 C6 1.395(2) . ? C5 H5A 0.9500 . ? C7 C12 1.387(2) . ? C7 C8 1.395(2) . ? C7 H7A 0.9500 . ? C8 C9 1.376(3) . ? C8 H8A 0.9500 . ? C9 C10 1.377(3) . ? C9 H9A 0.9500 . ? C10 C11 1.383(2) . ? C10 H10A 0.9500 . ? C11 C12 1.395(2) . ? C11 H11A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.395(3) . ? C16 C21 1.395(2) . ? C16 H16A 0.9500 . ? C17 C18 1.380(3) . ? C17 H17A 0.9500 . ? C18 C19 1.383(3) . ? C18 H18A 0.9500 . ? C19 C20 1.387(2) . ? C19 H19A 0.9500 . ? C20 C21 1.392(2) . ? C20 H20A 0.9500 . ? C22 C23 1.389(2) . ? C22 C27 1.394(2) . ? C22 H22A 0.9500 . ? C23 C24 1.385(2) . ? C23 H23A 0.9500 . ? C24 C25 1.382(3) . ? C24 H24A 0.9500 . ? C25 C26 1.390(2) . ? C25 H25A 0.9500 . ? C26 C27 1.398(2) . ? C26 H26A 0.9500 . ? C28 C29 1.393(2) . ? C28 C33 1.402(2) . ? C28 H28A 0.9500 . ? C29 C30 1.385(3) . ? C29 H29A 0.9500 . ? C30 C31 1.381(2) . ? C30 H30A 0.9500 . ? C31 C32 1.396(2) . ? C31 H31A 0.9500 . ? C32 C33 1.392(2) . ? C32 H32A 0.9500 . ? C34 C35 1.394(2) . ? C34 C39 1.393(2) . ? C34 H34A 0.9500 . ? C35 C36 1.386(3) . ? C35 H35A 0.9500 . ? C36 C37 1.380(3) . ? C36 H36A 0.9500 . ? C37 C38 1.389(2) . ? C37 H37A 0.9500 . ? C38 C39 1.400(2) . ? C38 H38A 0.9500 . ? C40 C41 1.519(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.388(2) . ? C42 C47 1.395(2) . ? C42 H42A 0.9500 . ? C43 C44 1.384(3) . ? C43 H43A 0.9500 . ? C44 C45 1.375(3) . ? C44 H44A 0.9500 . ? C45 C46 1.397(2) . ? C45 H45A 0.9500 . ? C46 C47 1.392(2) . ? C46 H46A 0.9500 . ? C48 C49 1.391(2) . ? C48 C53 1.402(2) . ? C48 H48A 0.9500 . ? C49 C50 1.388(3) . ? C49 H49A 0.9500 . ? C50 C51 1.383(3) . ? C50 H50A 0.9500 . ? C51 C52 1.396(2) . ? C51 H51A 0.9500 . ? C52 C53 1.389(2) . ? C52 H52A 0.9500 . ? 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 W1 N4 173.35(5) . . ? N2 W1 P1 85.15(4) . . ? N4 W1 P1 89.22(4) . . ? N2 W1 P2 86.80(4) . . ? N4 W1 P2 89.21(4) . . ? P1 W1 P2 85.307(13) . . ? N2 W1 P4 101.45(4) . . ? N4 W1 P4 82.81(4) . . ? P1 W1 P4 97.821(13) . . ? P2 W1 P4 171.367(13) . . ? N2 W1 P3 97.07(4) . . ? N4 W1 P3 88.71(4) . . ? P1 W1 P3 176.757(13) . . ? P2 W1 P3 97.156(13) . . ? P4 W1 P3 79.444(13) . . ? C13 N1 C15 112.85(13) . . ? C13 N1 C14 109.47(13) . . ? C15 N1 C14 108.69(13) . . ? N3 N2 W1 175.05(12) . . ? N5 N4 W1 178.42(14) . . ? C12 P1 C6 101.66(7) . . ? C12 P1 C13 104.44(7) . . ? C6 P1 C13 93.13(7) . . ? C12 P1 W1 116.72(5) . . ? C6 P1 W1 121.72(5) . . ? C13 P1 W1 115.48(5) . . ? C21 P2 C27 101.00(7) . . ? C21 P2 C15 102.80(8) . . ? C27 P2 C15 93.45(7) . . ? C21 P2 W1 118.41(5) . . ? C27 P2 W1 122.11(5) . . ? C15 P2 W1 114.80(5) . . ? C39 P3 C33 100.16(7) . . ? C39 P3 C40 102.95(7) . . ? C33 P3 C40 96.42(7) . . ? C39 P3 W1 114.87(5) . . ? C33 P3 W1 128.52(5) . . ? C40 P3 W1 110.04(5) . . ? C47 P4 C53 99.11(7) . . ? C47 P4 C41 101.22(7) . . ? C53 P4 C41 100.67(7) . . ? C47 P4 W1 120.47(5) . . ? C53 P4 W1 125.12(5) . . ? C41 P4 W1 106.36(5) . . ? C2 C1 C6 121.13(15) . . ? C2 C1 H1A 119.4 . . ? C6 C1 H1A 119.4 . . ? C3 C2 C1 120.54(16) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C4 C3 C2 119.07(17) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C3 C4 C5 120.62(18) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C6 C5 C4 120.67(17) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C1 C6 C5 117.96(15) . . ? C1 C6 P1 118.61(11) . . ? C5 C6 P1 123.38(13) . . ? C12 C7 C8 120.36(16) . . ? C12 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C9 C8 C7 120.67(16) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C10 C9 C8 119.38(16) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C9 C10 C11 120.30(16) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C12 121.09(16) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C7 C12 C11 118.14(15) . . ? C7 C12 P1 123.88(12) . . ? C11 C12 P1 117.82(12) . . ? N1 C13 P1 116.65(11) . . ? N1 C13 H13A 108.1 . . ? P1 C13 H13A 108.1 . . ? N1 C13 H13B 108.1 . . ? P1 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 P2 116.30(11) . . ? N1 C15 H15A 108.2 . . ? P2 C15 H15A 108.2 . . ? N1 C15 H15B 108.2 . . ? P2 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? C17 C16 C21 119.92(17) . . ? C17 C16 H16A 120.0 . . ? C21 C16 H16A 120.0 . . ? C18 C17 C16 120.92(18) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C17 C18 C19 119.48(17) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? C18 C19 C20 119.94(18) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C21 121.26(17) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C20 C21 C16 118.45(16) . . ? C20 C21 P2 118.08(12) . . ? C16 C21 P2 123.46(13) . . ? C23 C22 C27 121.17(15) . . ? C23 C22 H22A 119.4 . . ? C27 C22 H22A 119.4 . . ? C24 C23 C22 120.01(17) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 119.59(16) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C24 C25 C26 120.56(16) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C25 C26 C27 120.55(17) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C22 C27 C26 118.12(15) . . ? C22 C27 P2 117.34(11) . . ? C26 C27 P2 124.35(13) . . ? C29 C28 C33 120.37(15) . . ? C29 C28 H28A 119.8 . . ? C33 C28 H28A 119.8 . . ? C30 C29 C28 120.22(15) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C31 C30 C29 119.98(16) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.12(16) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C33 C32 C31 120.62(15) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C28 118.66(15) . . ? C32 C33 P3 121.51(12) . . ? C28 C33 P3 119.43(12) . . ? C35 C34 C39 120.70(16) . . ? C35 C34 H34A 119.7 . . ? C39 C34 H34A 119.7 . . ? C36 C35 C34 120.29(18) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C37 C36 C35 119.44(17) . . ? C37 C36 H36A 120.3 . . ? C35 C36 H36A 120.3 . . ? C36 C37 C38 120.70(16) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.6 . . ? C37 C38 C39 120.49(16) . . ? C37 C38 H38A 119.8 . . ? C39 C38 H38A 119.8 . . ? C34 C39 C38 118.38(15) . . ? C34 C39 P3 121.49(12) . . ? C38 C39 P3 119.85(13) . . ? C41 C40 P3 112.40(10) . . ? C41 C40 H40A 109.1 . . ? P3 C40 H40A 109.1 . . ? C41 C40 H40B 109.1 . . ? P3 C40 H40B 109.1 . . ? H40A C40 H40B 107.9 . . ? C40 C41 P4 108.15(10) . . ? C40 C41 H41A 110.1 . . ? P4 C41 H41A 110.1 . . ? C40 C41 H41B 110.1 . . ? P4 C41 H41B 110.1 . . ? H41A C41 H41B 108.4 . . ? C43 C42 C47 121.15(16) . . ? C43 C42 H42A 119.4 . . ? C47 C42 H42A 119.4 . . ? C44 C43 C42 120.07(16) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C45 C44 C43 119.49(16) . . ? C45 C44 H44A 120.3 . . ? C43 C44 H44A 120.3 . . ? C44 C45 C46 120.71(17) . . ? C44 C45 H45A 119.6 . . ? C46 C45 H45A 119.6 . . ? C45 C46 C47 120.38(16) . . ? C45 C46 H46A 119.8 . . ? C47 C46 H46A 119.8 . . ? C46 C47 C42 118.12(15) . . ? C46 C47 P4 122.83(12) . . ? C42 C47 P4 118.91(12) . . ? C49 C48 C53 120.67(16) . . ? C49 C48 H48A 119.7 . . ? C53 C48 H48A 119.7 . . ? C50 C49 C48 119.98(15) . . ? C50 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C51 C50 C49 119.99(16) . . ? C51 C50 H50A 120.0 . . ? C49 C50 H50A 120.0 . . ? C50 C51 C52 119.96(17) . . ? C50 C51 H51A 120.0 . . ? C52 C51 H51A 120.0 . . ? C53 C52 C51 120.89(15) . . ? C53 C52 H52A 119.6 . . ? C51 C52 H52A 119.6 . . ? C52 C53 C48 118.46(14) . . ? C52 C53 P4 120.66(11) . . ? C48 C53 P4 120.85(12) . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.299 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.098 #===END data_trans-W(N2)2(PMePh2)4 _database_code_depnum_ccdc_archive 'CCDC 854194' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H64 N4 O1.50 P4 W' _chemical_formula_weight 1148.86 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' W W -0.8490 6.8722 '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' _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 11.5609(4) _cell_length_b 14.1387(5) _cell_length_c 17.2056(6) _cell_angle_alpha 77.0490(10) _cell_angle_beta 72.3200(10) _cell_angle_gamma 83.3430(10) _cell_volume 2607.89(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9781 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 33.22 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 2.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6222 _exptl_absorpt_correction_T_max 0.7017 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56743 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 33.38 _reflns_number_total 19916 _reflns_number_gt 18079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.500 484 118 ' ' _platon_squeeze_details ; SQUEEZE results are consistent with 1.5 molecules of THF per asymmetric unit. These molecules were located from the difference map but one was disordered over the special position and would not stabilize during refinement. PLATON Reference : Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13. Spek, A.L. (2009). Acta Cryst. D65, 148-155. ; _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^)+(0.0245P)^2^+0.6341P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19916 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0522 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.758200(5) 0.760597(4) 0.743477(3) 0.00954(2) Uani 1 1 d . . . N1 N 0.62104(11) 0.67201(9) 0.78913(8) 0.0137(2) Uani 1 1 d . . . N2 N 0.54261(12) 0.62187(10) 0.81468(9) 0.0193(3) Uani 1 1 d . . . N3 N 0.89473(11) 0.85092(9) 0.69740(8) 0.0138(2) Uani 1 1 d . . . N4 N 0.97127(12) 0.90269(10) 0.67138(9) 0.0208(3) Uani 1 1 d . . . P1 P 0.85227(3) 0.63859(3) 0.65652(2) 0.01153(6) Uani 1 1 d . . . P2 P 0.87011(3) 0.68371(3) 0.84506(2) 0.01123(6) Uani 1 1 d . . . P3 P 0.63009(3) 0.85950(3) 0.84245(2) 0.01144(6) Uani 1 1 d . . . P4 P 0.68040(3) 0.85902(3) 0.62976(2) 0.01139(6) Uani 1 1 d . . . C1 C 1.02691(14) 0.48380(11) 0.68770(10) 0.0167(3) Uani 1 1 d . . . H1A H 1.0875 0.5223 0.6465 0.020 Uiso 1 1 calc R . . C2 C 1.05963(15) 0.39244(12) 0.72895(11) 0.0205(3) Uani 1 1 d . . . H2A H 1.1425 0.3697 0.7165 0.025 Uiso 1 1 calc R . . C3 C 0.97191(16) 0.33515(11) 0.78776(10) 0.0200(3) Uani 1 1 d . . . H3A H 0.9945 0.2730 0.8155 0.024 Uiso 1 1 calc R . . C4 C 0.85080(15) 0.36840(11) 0.80635(10) 0.0183(3) Uani 1 1 d . . . H4A H 0.7901 0.3285 0.8459 0.022 Uiso 1 1 calc R . . C5 C 0.81860(14) 0.46019(11) 0.76693(9) 0.0154(3) Uani 1 1 d . . . H5A H 0.7360 0.4835 0.7812 0.018 Uiso 1 1 calc R . . C6 C 0.90562(13) 0.51873(10) 0.70677(9) 0.0136(3) Uani 1 1 d . . . C7 C 1.07464(14) 0.71877(11) 0.56688(10) 0.0178(3) Uani 1 1 d . . . H7A H 1.0689 0.7386 0.6172 0.021 Uiso 1 1 calc R . . C8 C 1.17508(15) 0.74242(13) 0.49853(10) 0.0220(3) Uani 1 1 d . . . H8A H 1.2376 0.7778 0.5022 0.026 Uiso 1 1 calc R . . C9 C 1.18357(15) 0.71395(13) 0.42439(10) 0.0224(3) Uani 1 1 d . . . H9A H 1.2514 0.7306 0.3771 0.027 Uiso 1 1 calc R . . C10 C 1.09300(15) 0.66148(12) 0.41995(10) 0.0205(3) Uani 1 1 d . . . H10A H 1.0992 0.6417 0.3695 0.025 Uiso 1 1 calc R . . C11 C 0.99282(15) 0.63737(11) 0.48858(9) 0.0177(3) Uani 1 1 d . . . H11A H 0.9314 0.6010 0.4848 0.021 Uiso 1 1 calc R . . C12 C 0.98182(14) 0.66629(10) 0.56310(9) 0.0141(3) Uani 1 1 d . . . C13 C 0.74454(14) 0.59181(11) 0.61643(10) 0.0168(3) Uani 1 1 d . . . H13A H 0.7829 0.5358 0.5916 0.025 Uiso 1 1 calc R . . H13B H 0.7216 0.6428 0.5741 0.025 Uiso 1 1 calc R . . H13C H 0.6718 0.5718 0.6622 0.025 Uiso 1 1 calc R . . C14 C 0.91551(14) 0.49237(11) 0.93186(9) 0.0154(3) Uani 1 1 d . . . H14A H 0.9997 0.5028 0.9078 0.018 Uiso 1 1 calc R . . C15 C 0.87876(15) 0.40497(11) 0.98613(10) 0.0198(3) Uani 1 1 d . . . H15A H 0.9381 0.3561 0.9982 0.024 Uiso 1 1 calc R . . C16 C 0.75668(16) 0.38877(12) 1.02259(10) 0.0228(3) Uani 1 1 d . . . H16A H 0.7320 0.3295 1.0602 0.027 Uiso 1 1 calc R . . C17 C 0.67024(15) 0.46004(12) 1.00365(10) 0.0215(3) Uani 1 1 d . . . H17A H 0.5861 0.4495 1.0282 0.026 Uiso 1 1 calc R . . C18 C 0.70702(14) 0.54647(11) 0.94892(9) 0.0165(3) Uani 1 1 d . . . H18A H 0.6473 0.5944 0.9359 0.020 Uiso 1 1 calc R . . C19 C 0.83014(13) 0.56462(10) 0.91256(9) 0.0129(2) Uani 1 1 d . . . C20 C 0.82923(13) 0.71930(11) 1.00910(9) 0.0152(3) Uani 1 1 d . . . H20A H 0.7828 0.6631 1.0286 0.018 Uiso 1 1 calc R . . C21 C 0.84401(15) 0.76940(12) 1.06598(10) 0.0195(3) Uani 1 1 d . . . H21A H 0.8062 0.7482 1.1238 0.023 Uiso 1 1 calc R . . C22 C 0.91361(15) 0.85003(12) 1.03860(11) 0.0210(3) Uani 1 1 d . . . H22A H 0.9255 0.8833 1.0776 0.025 Uiso 1 1 calc R . . C23 C 0.96623(15) 0.88225(12) 0.95353(11) 0.0204(3) Uani 1 1 d . . . H23A H 1.0140 0.9377 0.9345 0.025 Uiso 1 1 calc R . . C24 C 0.94912(14) 0.83379(11) 0.89662(10) 0.0169(3) Uani 1 1 d . . . H24A H 0.9835 0.8574 0.8387 0.020 Uiso 1 1 calc R . . C25 C 0.88170(13) 0.75043(10) 0.92345(9) 0.0131(2) Uani 1 1 d . . . C26 C 1.03491(13) 0.66645(11) 0.79820(9) 0.0154(3) Uani 1 1 d . . . H26A H 1.0749 0.6453 0.8424 0.023 Uiso 1 1 calc R . . H26B H 1.0672 0.7279 0.7633 0.023 Uiso 1 1 calc R . . H26C H 1.0504 0.6169 0.7640 0.023 Uiso 1 1 calc R . . C27 C 0.39672(13) 0.86196(11) 0.82735(9) 0.0159(3) Uani 1 1 d . . . H27A H 0.4117 0.7935 0.8356 0.019 Uiso 1 1 calc R . . C28 C 0.28499(14) 0.90198(13) 0.81825(10) 0.0199(3) Uani 1 1 d . . . H28A H 0.2234 0.8609 0.8217 0.024 Uiso 1 1 calc R . . C29 C 0.26330(15) 1.00226(13) 0.80402(10) 0.0222(3) Uani 1 1 d . . . H29A H 0.1873 1.0299 0.7970 0.027 Uiso 1 1 calc R . . C30 C 0.35271(15) 1.06178(12) 0.80017(10) 0.0218(3) Uani 1 1 d . . . H30A H 0.3380 1.1303 0.7902 0.026 Uiso 1 1 calc R . . C31 C 0.46408(14) 1.02168(11) 0.81079(10) 0.0174(3) Uani 1 1 d . . . H31A H 0.5245 1.0631 0.8086 0.021 Uiso 1 1 calc R . . C32 C 0.48768(13) 0.92113(10) 0.82459(9) 0.0135(3) Uani 1 1 d . . . C33 C 0.67105(14) 0.96929(11) 0.95077(9) 0.0166(3) Uani 1 1 d . . . H33A H 0.6214 0.9256 0.9954 0.020 Uiso 1 1 calc R . . C34 C 0.72113(14) 1.04465(11) 0.96754(10) 0.0184(3) Uani 1 1 d . . . H34A H 0.7068 1.0510 1.0235 0.022 Uiso 1 1 calc R . . C35 C 0.79147(15) 1.11026(11) 0.90365(10) 0.0188(3) Uani 1 1 d . . . H35A H 0.8247 1.1620 0.9155 0.023 Uiso 1 1 calc R . . C36 C 0.81348(15) 1.10004(11) 0.82143(10) 0.0197(3) Uani 1 1 d . . . H36A H 0.8612 1.1452 0.7771 0.024 Uiso 1 1 calc R . . C37 C 0.76565(14) 1.02386(11) 0.80459(9) 0.0168(3) Uani 1 1 d . . . H37A H 0.7823 1.0167 0.7486 0.020 Uiso 1 1 calc R . . C38 C 0.69306(13) 0.95727(10) 0.86905(9) 0.0135(3) Uani 1 1 d . . . C39 C 0.55757(13) 0.78754(11) 0.94617(9) 0.0152(3) Uani 1 1 d . . . H39A H 0.4990 0.8294 0.9794 0.023 Uiso 1 1 calc R . . H39B H 0.6199 0.7603 0.9741 0.023 Uiso 1 1 calc R . . H39C H 0.5153 0.7346 0.9401 0.023 Uiso 1 1 calc R . . C40 C 0.46823(14) 0.76620(11) 0.65531(9) 0.0159(3) Uani 1 1 d . . . H40A H 0.5148 0.7087 0.6698 0.019 Uiso 1 1 calc R . . C41 C 0.34844(14) 0.76000(12) 0.65678(10) 0.0197(3) Uani 1 1 d . . . H41A H 0.3138 0.6984 0.6715 0.024 Uiso 1 1 calc R . . C42 C 0.27948(15) 0.84396(12) 0.63677(10) 0.0202(3) Uani 1 1 d . . . H42A H 0.1972 0.8400 0.6385 0.024 Uiso 1 1 calc R . . C43 C 0.33044(14) 0.93338(12) 0.61434(9) 0.0184(3) Uani 1 1 d . . . H43A H 0.2831 0.9907 0.6005 0.022 Uiso 1 1 calc R . . C44 C 0.45079(14) 0.93993(11) 0.61186(9) 0.0158(3) Uani 1 1 d . . . H44A H 0.4854 1.0016 0.5959 0.019 Uiso 1 1 calc R . . C45 C 0.52102(13) 0.85615(10) 0.63281(9) 0.0130(2) Uani 1 1 d . . . C46 C 0.87197(14) 0.87810(11) 0.48209(9) 0.0167(3) Uani 1 1 d . . . H46A H 0.9127 0.9035 0.5127 0.020 Uiso 1 1 calc R . . C47 C 0.92993(15) 0.87323(11) 0.39942(10) 0.0199(3) Uani 1 1 d . . . H47A H 1.0091 0.8967 0.3734 0.024 Uiso 1 1 calc R . . C48 C 0.87202(16) 0.83406(12) 0.35474(10) 0.0221(3) Uani 1 1 d . . . H48A H 0.9118 0.8303 0.2983 0.027 Uiso 1 1 calc R . . C49 C 0.75666(16) 0.80067(12) 0.39245(10) 0.0216(3) Uani 1 1 d . . . H49A H 0.7175 0.7731 0.3622 0.026 Uiso 1 1 calc R . . C50 C 0.69772(15) 0.80745(11) 0.47465(9) 0.0176(3) Uani 1 1 d . . . H50A H 0.6177 0.7855 0.4998 0.021 Uiso 1 1 calc R . . C51 C 0.75449(13) 0.84614(10) 0.52070(9) 0.0138(3) Uani 1 1 d . . . C52 C 0.69925(14) 0.99008(10) 0.61388(9) 0.0160(3) Uani 1 1 d . . . H52A H 0.6810 1.0236 0.5622 0.024 Uiso 1 1 calc R . . H52B H 0.7832 1.0008 0.6101 0.024 Uiso 1 1 calc R . . H52C H 0.6435 1.0157 0.6609 0.024 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 W1 0.00924(3) 0.00910(3) 0.00963(3) -0.00121(2) -0.00225(2) -0.00035(2) N1 0.0147(6) 0.0123(5) 0.0130(5) -0.0013(4) -0.0037(4) 0.0008(4) N2 0.0161(6) 0.0183(6) 0.0214(6) -0.0016(5) -0.0029(5) -0.0041(5) N3 0.0121(6) 0.0150(6) 0.0140(5) -0.0035(4) -0.0036(4) 0.0013(4) N4 0.0156(6) 0.0173(6) 0.0275(7) -0.0026(5) -0.0037(5) -0.0030(5) P1 0.01232(16) 0.01029(15) 0.01201(16) -0.00229(12) -0.00385(13) 0.00044(12) P2 0.01095(16) 0.01176(15) 0.01074(15) -0.00188(12) -0.00319(12) -0.00008(12) P3 0.01089(16) 0.01127(15) 0.01131(15) -0.00211(12) -0.00242(13) 0.00046(12) P4 0.01158(16) 0.01082(15) 0.01130(15) -0.00138(12) -0.00336(13) -0.00015(12) C1 0.0171(7) 0.0141(6) 0.0198(7) -0.0046(5) -0.0065(6) 0.0016(5) C2 0.0194(8) 0.0173(7) 0.0267(8) -0.0065(6) -0.0103(6) 0.0048(6) C3 0.0291(9) 0.0132(7) 0.0201(7) -0.0031(5) -0.0129(7) 0.0041(6) C4 0.0257(8) 0.0136(6) 0.0163(7) -0.0015(5) -0.0075(6) -0.0022(6) C5 0.0174(7) 0.0141(6) 0.0153(6) -0.0033(5) -0.0057(5) 0.0009(5) C6 0.0162(7) 0.0112(6) 0.0147(6) -0.0038(5) -0.0058(5) 0.0002(5) C7 0.0179(7) 0.0194(7) 0.0160(7) -0.0063(6) -0.0024(6) -0.0012(6) C8 0.0181(7) 0.0268(8) 0.0201(7) -0.0061(6) -0.0013(6) -0.0052(6) C9 0.0194(8) 0.0276(8) 0.0162(7) -0.0056(6) 0.0010(6) 0.0007(6) C10 0.0248(8) 0.0198(7) 0.0153(7) -0.0065(6) -0.0031(6) 0.0035(6) C11 0.0230(8) 0.0150(7) 0.0159(7) -0.0047(5) -0.0062(6) 0.0009(6) C12 0.0161(7) 0.0112(6) 0.0135(6) -0.0018(5) -0.0034(5) 0.0021(5) C13 0.0197(7) 0.0141(6) 0.0190(7) -0.0041(5) -0.0090(6) 0.0008(5) C14 0.0153(7) 0.0155(6) 0.0164(7) -0.0029(5) -0.0065(5) 0.0005(5) C15 0.0230(8) 0.0154(7) 0.0206(7) 0.0002(6) -0.0097(6) 0.0023(6) C16 0.0268(9) 0.0168(7) 0.0208(8) 0.0047(6) -0.0062(6) -0.0036(6) C17 0.0190(8) 0.0208(7) 0.0205(7) 0.0026(6) -0.0035(6) -0.0039(6) C18 0.0156(7) 0.0157(7) 0.0161(7) 0.0003(5) -0.0044(5) -0.0002(5) C19 0.0148(6) 0.0132(6) 0.0115(6) -0.0024(5) -0.0044(5) -0.0014(5) C20 0.0144(7) 0.0165(7) 0.0147(6) -0.0033(5) -0.0047(5) 0.0003(5) C21 0.0199(8) 0.0241(8) 0.0152(7) -0.0073(6) -0.0054(6) 0.0031(6) C22 0.0212(8) 0.0235(8) 0.0231(8) -0.0125(6) -0.0093(6) 0.0032(6) C23 0.0184(7) 0.0181(7) 0.0268(8) -0.0079(6) -0.0063(6) -0.0024(6) C24 0.0167(7) 0.0174(7) 0.0169(7) -0.0048(5) -0.0042(6) -0.0009(5) C25 0.0119(6) 0.0137(6) 0.0141(6) -0.0037(5) -0.0046(5) 0.0018(5) C26 0.0129(6) 0.0182(7) 0.0146(6) -0.0041(5) -0.0030(5) -0.0001(5) C27 0.0145(7) 0.0194(7) 0.0130(6) -0.0036(5) -0.0030(5) 0.0006(5) C28 0.0143(7) 0.0309(8) 0.0152(7) -0.0073(6) -0.0041(5) 0.0013(6) C29 0.0160(7) 0.0322(9) 0.0168(7) -0.0056(6) -0.0059(6) 0.0093(6) C30 0.0221(8) 0.0210(8) 0.0189(7) -0.0037(6) -0.0048(6) 0.0093(6) C31 0.0157(7) 0.0154(7) 0.0182(7) -0.0020(5) -0.0028(6) 0.0026(5) C32 0.0124(6) 0.0159(6) 0.0103(6) -0.0025(5) -0.0014(5) 0.0015(5) C33 0.0173(7) 0.0159(7) 0.0156(7) -0.0033(5) -0.0034(5) 0.0000(5) C34 0.0196(7) 0.0198(7) 0.0169(7) -0.0068(6) -0.0056(6) 0.0012(6) C35 0.0212(8) 0.0155(7) 0.0224(8) -0.0074(6) -0.0075(6) -0.0008(6) C36 0.0208(8) 0.0176(7) 0.0196(7) -0.0030(6) -0.0032(6) -0.0049(6) C37 0.0184(7) 0.0166(7) 0.0145(6) -0.0040(5) -0.0024(5) -0.0022(5) C38 0.0124(6) 0.0130(6) 0.0144(6) -0.0031(5) -0.0030(5) 0.0015(5) C39 0.0142(7) 0.0148(6) 0.0144(6) -0.0004(5) -0.0028(5) 0.0000(5) C40 0.0152(7) 0.0155(6) 0.0170(7) -0.0036(5) -0.0052(5) 0.0005(5) C41 0.0170(7) 0.0203(7) 0.0232(8) -0.0050(6) -0.0062(6) -0.0038(6) C42 0.0150(7) 0.0283(8) 0.0195(7) -0.0068(6) -0.0075(6) 0.0009(6) C43 0.0165(7) 0.0224(7) 0.0155(7) -0.0025(6) -0.0064(6) 0.0046(6) C44 0.0166(7) 0.0154(6) 0.0147(6) -0.0015(5) -0.0051(5) 0.0005(5) C45 0.0125(6) 0.0158(6) 0.0102(6) -0.0024(5) -0.0029(5) 0.0005(5) C46 0.0163(7) 0.0148(6) 0.0165(7) -0.0012(5) -0.0031(5) 0.0008(5) C47 0.0170(7) 0.0167(7) 0.0195(7) -0.0006(6) 0.0010(6) 0.0016(5) C48 0.0278(9) 0.0203(7) 0.0132(7) -0.0021(6) -0.0020(6) 0.0056(6) C49 0.0255(8) 0.0234(8) 0.0166(7) -0.0055(6) -0.0073(6) 0.0027(6) C50 0.0185(7) 0.0186(7) 0.0155(7) -0.0034(5) -0.0048(6) -0.0006(5) C51 0.0156(7) 0.0125(6) 0.0116(6) -0.0012(5) -0.0037(5) 0.0025(5) C52 0.0187(7) 0.0135(6) 0.0157(7) -0.0016(5) -0.0057(5) -0.0011(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 W1 N1 1.9908(13) . ? W1 N3 2.0011(13) . ? W1 P3 2.4706(4) . ? W1 P2 2.4710(4) . ? W1 P1 2.4760(4) . ? W1 P4 2.4763(4) . ? N1 N2 1.1336(18) . ? N3 N4 1.1322(18) . ? P1 C12 1.8363(15) . ? P1 C13 1.8390(15) . ? P1 C6 1.8504(14) . ? P2 C19 1.8373(15) . ? P2 C26 1.8403(15) . ? P2 C25 1.8538(14) . ? P3 C38 1.8357(15) . ? P3 C39 1.8434(15) . ? P3 C32 1.8490(14) . ? P4 C45 1.8323(15) . ? P4 C52 1.8402(15) . ? P4 C51 1.8516(15) . ? C1 C6 1.397(2) . ? C1 C2 1.398(2) . ? C1 H1A 0.9500 . ? C2 C3 1.381(2) . ? C2 H2A 0.9500 . ? C3 C4 1.388(2) . ? C3 H3A 0.9500 . ? C4 C5 1.389(2) . ? C4 H4A 0.9500 . ? C5 C6 1.395(2) . ? C5 H5A 0.9500 . ? C7 C8 1.388(2) . ? C7 C12 1.398(2) . ? C7 H7A 0.9500 . ? C8 C9 1.394(2) . ? C8 H8A 0.9500 . ? C9 C10 1.381(2) . ? C9 H9A 0.9500 . ? C10 C11 1.390(2) . ? C10 H10A 0.9500 . ? C11 C12 1.397(2) . ? C11 H11A 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.393(2) . ? C14 C15 1.394(2) . ? C14 H14A 0.9500 . ? C15 C16 1.382(2) . ? C15 H15A 0.9500 . ? C16 C17 1.392(2) . ? C16 H16A 0.9500 . ? C17 C18 1.386(2) . ? C17 H17A 0.9500 . ? C18 C19 1.398(2) . ? C18 H18A 0.9500 . ? C20 C21 1.389(2) . ? C20 C25 1.401(2) . ? C20 H20A 0.9500 . ? C21 C22 1.382(2) . ? C21 H21A 0.9500 . ? C22 C23 1.395(2) . ? C22 H22A 0.9500 . ? C23 C24 1.385(2) . ? C23 H23A 0.9500 . ? C24 C25 1.400(2) . ? C24 H24A 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.388(2) . ? C27 C32 1.401(2) . ? C27 H27A 0.9500 . ? C28 C29 1.390(2) . ? C28 H28A 0.9500 . ? C29 C30 1.384(3) . ? C29 H29A 0.9500 . ? C30 C31 1.393(2) . ? C30 H30A 0.9500 . ? C31 C32 1.397(2) . ? C31 H31A 0.9500 . ? C33 C34 1.391(2) . ? C33 C38 1.396(2) . ? C33 H33A 0.9500 . ? C34 C35 1.380(2) . ? C34 H34A 0.9500 . ? C35 C36 1.397(2) . ? C35 H35A 0.9500 . ? C36 C37 1.388(2) . ? C36 H36A 0.9500 . ? C37 C38 1.404(2) . ? C37 H37A 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.390(2) . ? C40 C45 1.398(2) . ? C40 H40A 0.9500 . ? C41 C42 1.388(2) . ? C41 H41A 0.9500 . ? C42 C43 1.382(2) . ? C42 H42A 0.9500 . ? C43 C44 1.392(2) . ? C43 H43A 0.9500 . ? C44 C45 1.398(2) . ? C44 H44A 0.9500 . ? C46 C47 1.390(2) . ? C46 C51 1.396(2) . ? C46 H46A 0.9500 . ? C47 C48 1.391(2) . ? C47 H47A 0.9500 . ? C48 C49 1.380(2) . ? C48 H48A 0.9500 . ? C49 C50 1.391(2) . ? C49 H49A 0.9500 . ? C50 C51 1.397(2) . ? C50 H50A 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? 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 W1 N3 179.35(5) . . ? N1 W1 P3 84.31(4) . . ? N3 W1 P3 95.26(4) . . ? N1 W1 P2 96.07(4) . . ? N3 W1 P2 84.42(4) . . ? P3 W1 P2 90.448(12) . . ? N1 W1 P1 83.99(4) . . ? N3 W1 P1 96.44(4) . . ? P3 W1 P1 168.294(12) . . ? P2 W1 P1 90.469(12) . . ? N1 W1 P4 95.32(4) . . ? N3 W1 P4 84.19(4) . . ? P3 W1 P4 90.991(12) . . ? P2 W1 P4 168.606(13) . . ? P1 W1 P4 90.411(12) . . ? N2 N1 W1 179.52(13) . . ? N4 N3 W1 179.40(13) . . ? C12 P1 C13 102.22(7) . . ? C12 P1 C6 100.47(7) . . ? C13 P1 C6 96.22(7) . . ? C12 P1 W1 121.66(5) . . ? C13 P1 W1 113.43(5) . . ? C6 P1 W1 118.74(5) . . ? C19 P2 C26 102.61(7) . . ? C19 P2 C25 99.56(6) . . ? C26 P2 C25 95.96(7) . . ? C19 P2 W1 120.98(5) . . ? C26 P2 W1 113.87(5) . . ? C25 P2 W1 119.74(5) . . ? C38 P3 C39 101.83(7) . . ? C38 P3 C32 100.65(7) . . ? C39 P3 C32 95.74(7) . . ? C38 P3 W1 121.31(5) . . ? C39 P3 W1 113.71(5) . . ? C32 P3 W1 119.36(5) . . ? C45 P4 C52 102.11(7) . . ? C45 P4 C51 99.43(7) . . ? C52 P4 C51 97.12(7) . . ? C45 P4 W1 120.75(5) . . ? C52 P4 W1 113.35(5) . . ? C51 P4 W1 120.15(5) . . ? C6 C1 C2 120.30(15) . . ? C6 C1 H1A 119.9 . . ? C2 C1 H1A 119.9 . . ? C3 C2 C1 120.26(15) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 120.00(14) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 119.77(15) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 121.09(14) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 118.55(13) . . ? C5 C6 P1 117.50(11) . . ? C1 C6 P1 123.95(12) . . ? C8 C7 C12 121.29(14) . . ? C8 C7 H7A 119.4 . . ? C12 C7 H7A 119.4 . . ? C7 C8 C9 119.55(16) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C10 C9 C8 119.78(15) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C9 C10 C11 120.61(15) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C10 C11 C12 120.50(15) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C11 C12 C7 118.26(14) . . ? C11 C12 P1 123.49(12) . . ? C7 C12 P1 118.25(11) . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 120.76(14) . . ? C19 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C16 C15 C14 120.54(14) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 119.40(15) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 119.94(15) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 121.35(14) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C14 C19 C18 117.99(13) . . ? C14 C19 P2 123.75(11) . . ? C18 C19 P2 118.23(11) . . ? C21 C20 C25 120.99(14) . . ? C21 C20 H20A 119.5 . . ? C25 C20 H20A 119.5 . . ? C22 C21 C20 120.10(15) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 119.68(14) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C24 C23 C22 120.29(15) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 120.72(15) . . ? C23 C24 H24A 119.6 . . ? C25 C24 H24A 119.6 . . ? C24 C25 C20 118.18(13) . . ? C24 C25 P2 118.94(11) . . ? C20 C25 P2 122.84(11) . . ? P2 C26 H26A 109.5 . . ? P2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 120.95(14) . . ? C28 C27 H27A 119.5 . . ? C32 C27 H27A 119.5 . . ? C27 C28 C29 119.94(16) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 119.81(14) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C31 120.33(15) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C30 C31 C32 120.60(15) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C31 C32 C27 118.34(13) . . ? C31 C32 P3 124.48(12) . . ? C27 C32 P3 117.15(11) . . ? C34 C33 C38 120.66(15) . . ? C34 C33 H33A 119.7 . . ? C38 C33 H33A 119.7 . . ? C35 C34 C33 120.70(14) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C36 119.48(14) . . ? C34 C35 H35A 120.3 . . ? C36 C35 H35A 120.3 . . ? C37 C36 C35 119.98(15) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 120.98(14) . . ? C36 C37 H37A 119.5 . . ? C38 C37 H37A 119.5 . . ? C33 C38 C37 118.18(14) . . ? C33 C38 P3 122.98(12) . . ? C37 C38 P3 118.84(11) . . ? P3 C39 H39A 109.5 . . ? P3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 120.77(14) . . ? C41 C40 H40A 119.6 . . ? C45 C40 H40A 119.6 . . ? C42 C41 C40 119.87(15) . . ? C42 C41 H41A 120.1 . . ? C40 C41 H41A 120.1 . . ? C43 C42 C41 120.01(15) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 120.37(14) . . ? C42 C43 H43A 119.8 . . ? C44 C43 H43A 119.8 . . ? C43 C44 C45 120.32(14) . . ? C43 C44 H44A 119.8 . . ? C45 C44 H44A 119.8 . . ? C40 C45 C44 118.65(13) . . ? C40 C45 P4 118.59(11) . . ? C44 C45 P4 122.74(11) . . ? C47 C46 C51 120.76(15) . . ? C47 C46 H46A 119.6 . . ? C51 C46 H46A 119.6 . . ? C46 C47 C48 119.99(15) . . ? C46 C47 H47A 120.0 . . ? C48 C47 H47A 120.0 . . ? C49 C48 C47 119.93(15) . . ? C49 C48 H48A 120.0 . . ? C47 C48 H48A 120.0 . . ? C48 C49 C50 120.03(15) . . ? C48 C49 H49A 120.0 . . ? C50 C49 H49A 120.0 . . ? C49 C50 C51 120.93(15) . . ? C49 C50 H50A 119.5 . . ? C51 C50 H50A 119.5 . . ? C46 C51 C50 118.34(14) . . ? C46 C51 P4 118.51(11) . . ? C50 C51 P4 123.14(12) . . ? P4 C52 H52A 109.5 . . ? P4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? P4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.996 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.089 #===END data_trans-W(N2)2(PPhNMePPh)2_(7-W) _database_code_depnum_ccdc_archive 'CCDC 854195' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H35 N3 O P2 W0.50' _chemical_formula_weight 619.48 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' W W -0.8490 6.8722 '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' _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 13.7790(6) _cell_length_b 14.3548(6) _cell_length_c 14.2441(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.0770(10) _cell_angle_gamma 90.00 _cell_volume 2764.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9782 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 33.16 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 2.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6612 _exptl_absorpt_correction_T_max 0.8059 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38991 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 33.28 _reflns_number_total 10506 _reflns_number_gt 7816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0256P)^2^+4.7490P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10506 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.0000 0.0000 0.0000 0.01229(3) Uani 1 2 d S . . N1 N 0.05385(15) 0.16066(14) 0.23799(15) 0.0182(4) Uani 1 1 d . . . N2 N -0.06158(14) 0.12097(15) -0.05447(14) 0.0175(4) Uani 1 1 d . . . N3 N -0.09240(18) 0.18803(16) -0.08419(18) 0.0285(5) Uani 1 1 d . . . P1 P -0.07160(4) 0.02148(4) 0.14251(4) 0.01509(11) Uani 1 1 d . . . P2 P 0.12990(4) 0.10817(4) 0.07893(4) 0.01432(10) Uani 1 1 d . . . C1 C -0.25833(16) 0.00184(17) 0.20026(16) 0.0171(4) Uani 1 1 d . . . H1A H -0.2226 -0.0228 0.2587 0.020 Uiso 1 1 calc R . . C2 C -0.36078(17) 0.00959(18) 0.18649(19) 0.0221(5) Uani 1 1 d . . . H2A H -0.3948 -0.0117 0.2344 0.026 Uiso 1 1 calc R . . C3 C -0.41314(18) 0.04849(18) 0.1026(2) 0.0235(5) Uani 1 1 d . . . H3A H -0.4830 0.0543 0.0932 0.028 Uiso 1 1 calc R . . C4 C -0.36306(18) 0.07893(18) 0.0324(2) 0.0229(5) Uani 1 1 d . . . H4A H -0.3986 0.1065 -0.0246 0.027 Uiso 1 1 calc R . . C5 C -0.26087(18) 0.06911(17) 0.04551(18) 0.0195(4) Uani 1 1 d . . . H5A H -0.2272 0.0893 -0.0031 0.023 Uiso 1 1 calc R . . C6 C -0.20748(17) 0.02986(16) 0.12929(17) 0.0165(4) Uani 1 1 d . . . C7 C 0.0398(2) -0.0473(2) 0.3163(2) 0.0279(6) Uani 1 1 d . . . H7A H 0.0755 0.0096 0.3200 0.033 Uiso 1 1 calc R . . C8 C 0.0649(2) -0.1138(2) 0.3874(2) 0.0326(6) Uani 1 1 d . . . H8A H 0.1176 -0.1018 0.4396 0.039 Uiso 1 1 calc R . . C9 C 0.0145(2) -0.19716(19) 0.3835(2) 0.0259(5) Uani 1 1 d . . . H9A H 0.0316 -0.2420 0.4330 0.031 Uiso 1 1 calc R . . C10 C -0.0612(2) -0.21469(18) 0.30699(19) 0.0235(5) Uani 1 1 d . . . H10A H -0.0960 -0.2721 0.3033 0.028 Uiso 1 1 calc R . . C11 C -0.08654(19) -0.14892(16) 0.23554(18) 0.0203(5) Uani 1 1 d . . . H11A H -0.1383 -0.1622 0.1828 0.024 Uiso 1 1 calc R . . C12 C -0.03775(17) -0.06369(16) 0.23931(17) 0.0169(4) Uani 1 1 d . . . C13 C -0.04908(17) 0.13126(17) 0.21185(18) 0.0196(4) Uani 1 1 d . . . H13A H -0.0871 0.1817 0.1740 0.024 Uiso 1 1 calc R . . H13B H -0.0757 0.1240 0.2712 0.024 Uiso 1 1 calc R . . C14 C 0.0633(2) 0.23063(18) 0.31396(19) 0.0247(5) Uani 1 1 d . . . H14A H 0.0381 0.2051 0.3684 0.037 Uiso 1 1 calc R . . H14B H 0.0251 0.2861 0.2899 0.037 Uiso 1 1 calc R . . H14C H 0.1331 0.2475 0.3345 0.037 Uiso 1 1 calc R . . C15 C 0.08829(17) 0.19903(15) 0.15541(17) 0.0175(4) Uani 1 1 d . . . H15A H 0.1438 0.2423 0.1781 0.021 Uiso 1 1 calc R . . H15B H 0.0341 0.2354 0.1164 0.021 Uiso 1 1 calc R . . C16 C 0.2454(2) -0.01922(17) 0.20059(19) 0.0234(5) Uani 1 1 d . . . H16A H 0.1911 -0.0604 0.1825 0.028 Uiso 1 1 calc R . . C17 C 0.3290(2) -0.0490(2) 0.2644(2) 0.0303(6) Uani 1 1 d . . . H17A H 0.3311 -0.1104 0.2896 0.036 Uiso 1 1 calc R . . C18 C 0.4086(2) 0.0092(2) 0.29135(19) 0.0297(6) Uani 1 1 d . . . H18A H 0.4665 -0.0126 0.3327 0.036 Uiso 1 1 calc R . . C19 C 0.4036(2) 0.1000(2) 0.2577(2) 0.0294(6) Uani 1 1 d . . . H19A H 0.4572 0.1415 0.2779 0.035 Uiso 1 1 calc R . . C20 C 0.32047(18) 0.13014(19) 0.19448(18) 0.0221(5) Uani 1 1 d . . . H20A H 0.3175 0.1926 0.1720 0.027 Uiso 1 1 calc R . . C21 C 0.24083(17) 0.07032(16) 0.16324(17) 0.0169(4) Uani 1 1 d . . . C22 C 0.13705(18) 0.27354(16) -0.02841(18) 0.0192(4) Uani 1 1 d . . . H22A H 0.0770 0.2894 -0.0089 0.023 Uiso 1 1 calc R . . C23 C 0.1759(2) 0.33348(17) -0.08831(19) 0.0228(5) Uani 1 1 d . . . H23A H 0.1428 0.3901 -0.1089 0.027 Uiso 1 1 calc R . . C24 C 0.2627(2) 0.31091(18) -0.11801(19) 0.0233(5) Uani 1 1 d . . . H24A H 0.2891 0.3517 -0.1593 0.028 Uiso 1 1 calc R . . C25 C 0.31098(19) 0.22875(18) -0.08746(18) 0.0220(5) Uani 1 1 d . . . H25A H 0.3704 0.2130 -0.1082 0.026 Uiso 1 1 calc R . . C26 C 0.27318(17) 0.16936(16) -0.02679(17) 0.0177(4) Uani 1 1 d . . . H26A H 0.3077 0.1136 -0.0055 0.021 Uiso 1 1 calc R . . C27 C 0.18474(16) 0.19023(15) 0.00371(17) 0.0160(4) Uani 1 1 d . . . O1 O 0.37847(16) 0.11849(17) 0.60074(16) 0.0377(5) Uani 1 1 d . . . C28 C 0.3757(2) 0.0864(2) 0.5053(2) 0.0293(6) Uani 1 1 d . . . H28A H 0.4126 0.0271 0.5061 0.035 Uiso 1 1 calc R . . H28B H 0.4062 0.1330 0.4687 0.035 Uiso 1 1 calc R . . C29 C 0.2678(2) 0.0719(3) 0.4595(2) 0.0402(8) Uani 1 1 d . . . H29A H 0.2552 0.0064 0.4391 0.048 Uiso 1 1 calc R . . H29B H 0.2483 0.1131 0.4032 0.048 Uiso 1 1 calc R . . C30 C 0.2122(2) 0.0972(3) 0.5382(2) 0.0363(7) Uani 1 1 d . . . H30A H 0.1502 0.1309 0.5122 0.044 Uiso 1 1 calc R . . H30B H 0.1964 0.0410 0.5727 0.044 Uiso 1 1 calc R . . C31 C 0.2848(2) 0.1592(2) 0.6025(2) 0.0328(6) Uani 1 1 d . . . H31A H 0.2816 0.2238 0.5777 0.039 Uiso 1 1 calc R . . H31B H 0.2713 0.1600 0.6683 0.039 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 W1 0.01273(5) 0.01134(5) 0.01363(5) -0.00019(5) 0.00462(4) -0.00057(4) N1 0.0197(9) 0.0176(9) 0.0184(9) -0.0043(7) 0.0067(8) -0.0031(7) N2 0.0108(8) 0.0255(10) 0.0164(9) -0.0018(8) 0.0032(7) -0.0052(7) N3 0.0292(11) 0.0244(11) 0.0321(13) -0.0025(10) 0.0067(10) -0.0010(9) P1 0.0142(2) 0.0168(3) 0.0149(3) -0.0010(2) 0.0046(2) -0.00080(18) P2 0.0152(2) 0.0124(2) 0.0161(3) -0.0001(2) 0.0048(2) -0.00066(19) C1 0.0156(9) 0.0209(10) 0.0154(9) -0.0026(9) 0.0047(7) -0.0009(9) C2 0.0159(9) 0.0301(13) 0.0223(11) -0.0036(10) 0.0088(8) -0.0018(9) C3 0.0173(10) 0.0243(12) 0.0296(13) -0.0053(10) 0.0062(10) -0.0001(8) C4 0.0200(11) 0.0219(11) 0.0260(12) 0.0005(10) 0.0026(10) 0.0035(9) C5 0.0193(10) 0.0197(11) 0.0203(11) 0.0009(9) 0.0057(9) 0.0001(8) C6 0.0177(10) 0.0151(9) 0.0178(10) -0.0018(8) 0.0058(8) -0.0006(8) C7 0.0242(12) 0.0279(13) 0.0286(14) 0.0067(11) -0.0021(11) -0.0073(10) C8 0.0268(13) 0.0391(16) 0.0271(14) 0.0110(12) -0.0071(11) -0.0073(11) C9 0.0264(12) 0.0271(13) 0.0234(12) 0.0082(10) 0.0026(10) 0.0015(10) C10 0.0281(12) 0.0180(11) 0.0247(12) 0.0016(9) 0.0053(10) 0.0011(9) C11 0.0246(11) 0.0169(10) 0.0185(11) -0.0006(9) 0.0021(9) 0.0006(8) C12 0.0162(9) 0.0194(10) 0.0159(10) 0.0011(8) 0.0049(8) 0.0004(8) C13 0.0182(10) 0.0190(10) 0.0234(12) -0.0045(9) 0.0083(9) -0.0018(8) C14 0.0296(13) 0.0236(12) 0.0226(12) -0.0077(10) 0.0096(10) -0.0054(10) C15 0.0201(10) 0.0136(9) 0.0205(11) -0.0019(8) 0.0080(9) -0.0019(8) C16 0.0291(12) 0.0194(11) 0.0205(11) -0.0005(9) 0.0016(10) 0.0009(9) C17 0.0424(16) 0.0226(12) 0.0243(13) 0.0021(10) 0.0023(12) 0.0115(11) C18 0.0231(11) 0.0466(17) 0.0187(11) 0.0029(12) 0.0023(9) 0.0140(12) C19 0.0190(11) 0.0471(17) 0.0216(12) 0.0060(12) 0.0027(10) -0.0038(11) C20 0.0195(10) 0.0279(12) 0.0185(11) 0.0038(10) 0.0027(9) -0.0041(9) C21 0.0177(10) 0.0173(10) 0.0161(10) 0.0002(8) 0.0042(8) 0.0011(8) C22 0.0208(10) 0.0170(10) 0.0204(11) 0.0012(9) 0.0050(9) -0.0003(8) C23 0.0296(12) 0.0156(10) 0.0230(12) 0.0042(9) 0.0044(10) -0.0013(9) C24 0.0283(12) 0.0220(11) 0.0209(11) 0.0030(9) 0.0080(10) -0.0082(9) C25 0.0207(11) 0.0257(12) 0.0206(11) -0.0013(10) 0.0067(9) -0.0062(9) C26 0.0184(10) 0.0175(10) 0.0172(10) -0.0008(8) 0.0035(8) -0.0017(8) C27 0.0174(10) 0.0131(9) 0.0181(10) -0.0004(8) 0.0047(8) -0.0032(7) O1 0.0280(10) 0.0548(14) 0.0282(11) -0.0037(10) -0.0003(9) 0.0015(10) C28 0.0244(12) 0.0352(15) 0.0285(14) 0.0023(12) 0.0059(11) 0.0006(11) C29 0.0261(14) 0.068(2) 0.0255(14) -0.0054(15) 0.0025(12) -0.0011(14) C30 0.0273(14) 0.054(2) 0.0275(14) -0.0040(14) 0.0054(12) -0.0058(13) C31 0.0366(15) 0.0298(14) 0.0325(15) -0.0013(12) 0.0077(13) -0.0008(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N2 2.021(2) . ? W1 N2 2.021(2) 3 ? W1 P1 2.4410(6) 3 ? W1 P1 2.4410(6) . ? W1 P2 2.4710(6) . ? W1 P2 2.4710(6) 3 ? N1 C15 1.458(3) . ? N1 C13 1.458(3) . ? N1 C14 1.464(3) . ? N2 N3 1.103(3) . ? P1 C12 1.835(2) . ? P1 C6 1.849(2) . ? P1 C13 1.854(2) . ? P2 C21 1.835(2) . ? P2 C27 1.849(2) . ? P2 C15 1.859(2) . ? C1 C2 1.392(3) . ? C1 C6 1.395(3) . ? C1 H1A 0.9500 . ? C2 C3 1.389(4) . ? C2 H2A 0.9500 . ? C3 C4 1.390(4) . ? C3 H3A 0.9500 . ? C4 C5 1.391(3) . ? C4 H4A 0.9500 . ? C5 C6 1.395(3) . ? C5 H5A 0.9500 . ? C7 C8 1.386(4) . ? C7 C12 1.397(3) . ? C7 H7A 0.9500 . ? C8 C9 1.379(4) . ? C8 H8A 0.9500 . ? C9 C10 1.378(4) . ? C9 H9A 0.9500 . ? C10 C11 1.383(3) . ? C10 H10A 0.9500 . ? C11 C12 1.392(3) . ? C11 H11A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.388(3) . ? C16 C17 1.390(4) . ? C16 H16A 0.9500 . ? C17 C18 1.374(4) . ? C17 H17A 0.9500 . ? C18 C19 1.387(4) . ? C18 H18A 0.9500 . ? C19 C20 1.383(4) . ? C19 H19A 0.9500 . ? C20 C21 1.397(3) . ? C20 H20A 0.9500 . ? C22 C23 1.390(3) . ? C22 C27 1.399(3) . ? C22 H22A 0.9500 . ? C23 C24 1.381(4) . ? C23 H23A 0.9500 . ? C24 C25 1.383(4) . ? C24 H24A 0.9500 . ? C25 C26 1.385(3) . ? C25 H25A 0.9500 . ? C26 C27 1.403(3) . ? C26 H26A 0.9500 . ? O1 C31 1.421(4) . ? O1 C28 1.429(4) . ? C28 C29 1.518(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.519(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.510(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? 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 W1 N2 180.0 . 3 ? N2 W1 P1 89.78(6) . 3 ? N2 W1 P1 90.22(6) 3 3 ? N2 W1 P1 90.22(6) . . ? N2 W1 P1 89.78(6) 3 . ? P1 W1 P1 180.0 3 . ? N2 W1 P2 81.30(5) . . ? N2 W1 P2 98.70(5) 3 . ? P1 W1 P2 94.85(2) 3 . ? P1 W1 P2 85.15(2) . . ? N2 W1 P2 98.70(5) . 3 ? N2 W1 P2 81.30(5) 3 3 ? P1 W1 P2 85.15(2) 3 3 ? P1 W1 P2 94.85(2) . 3 ? P2 W1 P2 180.0 . 3 ? C15 N1 C13 110.77(19) . . ? C15 N1 C14 109.90(19) . . ? C13 N1 C14 109.38(19) . . ? N3 N2 W1 177.9(2) . . ? C12 P1 C6 103.06(11) . . ? C12 P1 C13 100.00(11) . . ? C6 P1 C13 93.53(11) . . ? C12 P1 W1 117.11(8) . . ? C6 P1 W1 119.12(8) . . ? C13 P1 W1 119.83(8) . . ? C21 P2 C27 100.73(11) . . ? C21 P2 C15 97.82(11) . . ? C27 P2 C15 95.68(10) . . ? C21 P2 W1 123.44(8) . . ? C27 P2 W1 118.53(8) . . ? C15 P2 W1 115.43(8) . . ? C2 C1 C6 120.8(2) . . ? C2 C1 H1A 119.6 . . ? C6 C1 H1A 119.6 . . ? C3 C2 C1 119.9(2) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 119.8(2) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 120.1(2) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 118.7(2) . . ? C1 C6 P1 123.16(18) . . ? C5 C6 P1 118.07(18) . . ? C8 C7 C12 120.2(2) . . ? C8 C7 H7A 119.9 . . ? C12 C7 H7A 119.9 . . ? C9 C8 C7 121.0(2) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 119.2(2) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C12 121.3(2) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C11 C12 C7 118.0(2) . . ? C11 C12 P1 120.37(18) . . ? C7 C12 P1 121.57(19) . . ? N1 C13 P1 115.92(16) . . ? N1 C13 H13A 108.3 . . ? P1 C13 H13A 108.3 . . ? N1 C13 H13B 108.3 . . ? P1 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 P2 113.11(15) . . ? N1 C15 H15A 109.0 . . ? P2 C15 H15A 109.0 . . ? N1 C15 H15B 109.0 . . ? P2 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C21 C16 C17 120.4(3) . . ? C21 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C17 C18 C19 119.4(2) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 121.1(2) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C16 C21 C20 118.2(2) . . ? C16 C21 P2 119.73(18) . . ? C20 C21 P2 122.06(18) . . ? C23 C22 C27 121.2(2) . . ? C23 C22 H22A 119.4 . . ? C27 C22 H22A 119.4 . . ? C24 C23 C22 120.1(2) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 119.7(2) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 120.4(2) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C27 121.0(2) . . ? C25 C26 H26A 119.5 . . ? C27 C26 H26A 119.5 . . ? C22 C27 C26 117.6(2) . . ? C22 C27 P2 121.05(18) . . ? C26 C27 P2 121.31(17) . . ? C31 O1 C28 106.9(2) . . ? O1 C28 C29 107.4(2) . . ? O1 C28 H28A 110.2 . . ? C29 C28 H28A 110.2 . . ? O1 C28 H28B 110.2 . . ? C29 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? C28 C29 C30 104.0(2) . . ? C28 C29 H29A 111.0 . . ? C30 C29 H29A 111.0 . . ? C28 C29 H29B 111.0 . . ? C30 C29 H29B 111.0 . . ? H29A C29 H29B 109.0 . . ? C31 C30 C29 102.6(3) . . ? C31 C30 H30A 111.2 . . ? C29 C30 H30A 111.2 . . ? C31 C30 H30B 111.2 . . ? C29 C30 H30B 111.2 . . ? H30A C30 H30B 109.2 . . ? O1 C31 C30 104.2(2) . . ? O1 C31 H31A 110.9 . . ? C30 C31 H31A 110.9 . . ? O1 C31 H31B 110.9 . . ? C30 C31 H31B 110.9 . . ? H31A C31 H31B 108.9 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.649 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.127 #===END data_trans-MoBr2(PPhNBnPPh)2_(4) _database_code_depnum_ccdc_archive 'CCDC 854196' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H39 Br Mo0.50 N O P2' _chemical_formula_weight 703.51 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' Br Br -0.2901 2.4595 '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' O O 0.0106 0.0060 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9360(3) _cell_length_b 27.6368(7) _cell_length_c 9.1815(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.7040(10) _cell_angle_gamma 90.00 _cell_volume 3202.12(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9824 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 33.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7506 _exptl_absorpt_correction_T_max 0.8435 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 55072 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 33.33 _reflns_number_total 12313 _reflns_number_gt 10406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0297P)^2^+1.2242P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12313 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0609 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.0000 0.0000 0.5000 0.00851(3) Uani 1 2 d S . . Br1 Br 0.045685(10) 0.040064(4) 0.760441(13) 0.01297(3) Uani 1 1 d . . . N1 N 0.03062(8) 0.10850(4) 0.21214(11) 0.01191(18) Uani 1 1 d . . . P1 P 0.14490(2) 0.035924(11) 0.38310(3) 0.00974(5) Uani 1 1 d . . . P2 P -0.10836(2) 0.070954(11) 0.38086(3) 0.01023(6) Uani 1 1 d . . . C1 C 0.19485(11) 0.11403(5) 0.57751(14) 0.0159(2) Uani 1 1 d . . . H1A H 0.1305 0.1071 0.6023 0.019 Uiso 1 1 calc R . . C2 C 0.25423(12) 0.15347(5) 0.64269(15) 0.0194(3) Uani 1 1 d . . . H2A H 0.2284 0.1732 0.7086 0.023 Uiso 1 1 calc R . . C3 C 0.35137(11) 0.16346(5) 0.61007(15) 0.0193(3) Uani 1 1 d . . . H3A H 0.3922 0.1891 0.6569 0.023 Uiso 1 1 calc R . . C4 C 0.38747(11) 0.13503(5) 0.50709(16) 0.0187(2) Uani 1 1 d . . . H4A H 0.4525 0.1418 0.4841 0.022 Uiso 1 1 calc R . . C5 C 0.32676(10) 0.09653(5) 0.43821(15) 0.0155(2) Uani 1 1 d . . . H5A H 0.3503 0.0784 0.3666 0.019 Uiso 1 1 calc R . . C6 C 0.23086(9) 0.08479(4) 0.47535(13) 0.0119(2) Uani 1 1 d . . . C7 C 0.33692(10) -0.01512(4) 0.42365(14) 0.0135(2) Uani 1 1 d . . . H7A H 0.3511 -0.0014 0.5185 0.016 Uiso 1 1 calc R . . C8 C 0.41119(10) -0.04554(5) 0.38351(15) 0.0166(2) Uani 1 1 d . . . H8A H 0.4744 -0.0521 0.4512 0.020 Uiso 1 1 calc R . . C9 C 0.39119(11) -0.06618(5) 0.24229(15) 0.0182(2) Uani 1 1 d . . . H9A H 0.4409 -0.0866 0.2151 0.022 Uiso 1 1 calc R . . C10 C 0.29678(11) -0.05618(5) 0.14204(15) 0.0177(2) Uani 1 1 d . . . H10A H 0.2832 -0.0699 0.0473 0.021 Uiso 1 1 calc R . . C11 C 0.22199(10) -0.02564(5) 0.18239(14) 0.0144(2) Uani 1 1 d . . . H11A H 0.1589 -0.0192 0.1143 0.017 Uiso 1 1 calc R . . C12 C 0.24109(9) -0.00461(4) 0.32449(13) 0.0117(2) Uani 1 1 d . . . C13 C 0.09547(9) 0.06595(4) 0.20034(13) 0.0120(2) Uani 1 1 d . . . H13A H 0.1554 0.0756 0.1595 0.014 Uiso 1 1 calc R . . H13B H 0.0537 0.0430 0.1317 0.014 Uiso 1 1 calc R . . C14 C 0.03633(10) 0.14335(5) 0.09149(14) 0.0157(2) Uani 1 1 d . . . H14A H -0.0150 0.1690 0.0911 0.019 Uiso 1 1 calc R . . H14B H 0.0181 0.1269 -0.0041 0.019 Uiso 1 1 calc R . . C15 C 0.18269(11) 0.19766(5) 0.22690(15) 0.0187(2) Uani 1 1 d . . . H15A H 0.1392 0.2066 0.2907 0.022 Uiso 1 1 calc R . . C16 C 0.28423(12) 0.21682(5) 0.24775(17) 0.0222(3) Uani 1 1 d . . . H16A H 0.3083 0.2386 0.3250 0.027 Uiso 1 1 calc R . . C17 C 0.34956(12) 0.20359(5) 0.15399(17) 0.0232(3) Uani 1 1 d . . . H17A H 0.4176 0.2163 0.1684 0.028 Uiso 1 1 calc R . . C18 C 0.31374(12) 0.17136(6) 0.03871(17) 0.0239(3) Uani 1 1 d . . . H18A H 0.3577 0.1624 -0.0244 0.029 Uiso 1 1 calc R . . C19 C 0.21168(11) 0.15224(5) 0.01706(15) 0.0200(3) Uani 1 1 d . . . H19A H 0.1878 0.1307 -0.0609 0.024 Uiso 1 1 calc R . . C20 C 0.14542(10) 0.16518(5) 0.11122(14) 0.0155(2) Uani 1 1 d . . . C21 C -0.07955(10) 0.09521(4) 0.20555(13) 0.0129(2) Uani 1 1 d . . . H21A H -0.1005 0.0711 0.1277 0.015 Uiso 1 1 calc R . . H21B H -0.1234 0.1236 0.1764 0.015 Uiso 1 1 calc R . . C22 C -0.29220(10) 0.02122(5) 0.23952(14) 0.0164(2) Uani 1 1 d . . . H22A H -0.2467 -0.0049 0.2396 0.020 Uiso 1 1 calc R . . C23 C -0.39976(11) 0.01615(6) 0.17591(15) 0.0213(3) Uani 1 1 d . . . H23A H -0.4257 -0.0133 0.1341 0.026 Uiso 1 1 calc R . . C24 C -0.46834(11) 0.05467(6) 0.17448(16) 0.0252(3) Uani 1 1 d . . . H24A H -0.5403 0.0510 0.1335 0.030 Uiso 1 1 calc R . . C25 C -0.42906(11) 0.09874(6) 0.23458(16) 0.0240(3) Uani 1 1 d . . . H25A H -0.4747 0.1249 0.2324 0.029 Uiso 1 1 calc R . . C26 C -0.32164(10) 0.10405(5) 0.29818(15) 0.0181(2) Uani 1 1 d . . . H26A H -0.2959 0.1338 0.3377 0.022 Uiso 1 1 calc R . . C27 C -0.25202(10) 0.06512(5) 0.30315(13) 0.0133(2) Uani 1 1 d . . . C28 C -0.04181(12) 0.16572(5) 0.47412(16) 0.0203(3) Uani 1 1 d . . . H28A H -0.0087 0.1664 0.3940 0.024 Uiso 1 1 calc R . . C29 C -0.03183(13) 0.20508(5) 0.57086(19) 0.0272(3) Uani 1 1 d . . . H29A H 0.0080 0.2318 0.5552 0.033 Uiso 1 1 calc R . . C30 C -0.08121(13) 0.20443(5) 0.69054(18) 0.0270(3) Uani 1 1 d . . . H30A H -0.0744 0.2306 0.7555 0.032 Uiso 1 1 calc R . . C31 C -0.14071(12) 0.16456(5) 0.71268(16) 0.0230(3) Uani 1 1 d . . . H31A H -0.1743 0.1641 0.7924 0.028 Uiso 1 1 calc R . . C32 C -0.15049(11) 0.12531(5) 0.61670(15) 0.0179(2) Uani 1 1 d . . . H32A H -0.1905 0.0987 0.6328 0.021 Uiso 1 1 calc R . . C33 C -0.10104(10) 0.12534(4) 0.49632(13) 0.0135(2) Uani 1 1 d . . . O1 O 0.54001(10) 0.23092(4) 0.88006(13) 0.0345(3) Uani 1 1 d . . . C34 C 0.58207(15) 0.26163(6) 1.0035(2) 0.0313(3) Uani 1 1 d . . . H34A H 0.5257 0.2738 1.0479 0.038 Uiso 1 1 calc R . . H34B H 0.6187 0.2889 0.9716 0.038 Uiso 1 1 calc R . . C35 C 0.65855(14) 0.23087(6) 1.11472(19) 0.0310(3) Uani 1 1 d . . . H35A H 0.7150 0.2502 1.1740 0.037 Uiso 1 1 calc R . . H35B H 0.6225 0.2133 1.1804 0.037 Uiso 1 1 calc R . . C36 C 0.69973(14) 0.19715(7) 1.01075(18) 0.0319(4) Uani 1 1 d . . . H36A H 0.7536 0.2126 0.9683 0.038 Uiso 1 1 calc R . . H36B H 0.7284 0.1677 1.0613 0.038 Uiso 1 1 calc R . . C37 C 0.60084(14) 0.18735(6) 0.89373(18) 0.0286(3) Uani 1 1 d . . . H37A H 0.6184 0.1792 0.7993 0.034 Uiso 1 1 calc R . . H37B H 0.5614 0.1607 0.9239 0.034 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 0.00756(6) 0.00930(6) 0.00847(6) -0.00023(4) 0.00136(4) 0.00004(4) Br1 0.01376(6) 0.01401(5) 0.01088(5) -0.00218(4) 0.00215(4) -0.00157(4) N1 0.0101(4) 0.0125(4) 0.0133(4) 0.0027(3) 0.0031(3) 0.0003(3) P1 0.00833(12) 0.01088(12) 0.00989(12) -0.00011(9) 0.00174(10) -0.00021(10) P2 0.00894(13) 0.01086(12) 0.01080(12) 0.00071(10) 0.00198(10) 0.00044(10) C1 0.0161(6) 0.0162(5) 0.0161(5) -0.0014(4) 0.0054(4) -0.0032(4) C2 0.0237(7) 0.0177(6) 0.0176(6) -0.0045(4) 0.0064(5) -0.0042(5) C3 0.0191(6) 0.0160(6) 0.0211(6) -0.0023(5) 0.0004(5) -0.0051(5) C4 0.0122(5) 0.0157(6) 0.0281(7) -0.0003(5) 0.0042(5) -0.0029(4) C5 0.0127(5) 0.0144(5) 0.0201(6) -0.0002(4) 0.0049(4) -0.0010(4) C6 0.0108(5) 0.0117(5) 0.0127(5) 0.0002(4) 0.0012(4) -0.0008(4) C7 0.0121(5) 0.0146(5) 0.0137(5) 0.0014(4) 0.0028(4) -0.0002(4) C8 0.0111(5) 0.0177(6) 0.0206(6) 0.0006(4) 0.0025(4) 0.0016(4) C9 0.0161(6) 0.0168(6) 0.0238(6) -0.0024(5) 0.0085(5) 0.0022(5) C10 0.0188(6) 0.0195(6) 0.0164(5) -0.0035(4) 0.0069(5) 0.0009(5) C11 0.0138(5) 0.0160(5) 0.0131(5) -0.0012(4) 0.0022(4) 0.0005(4) C12 0.0109(5) 0.0122(5) 0.0126(5) 0.0002(4) 0.0038(4) -0.0006(4) C13 0.0112(5) 0.0137(5) 0.0116(5) 0.0011(4) 0.0035(4) 0.0011(4) C14 0.0142(5) 0.0169(5) 0.0157(5) 0.0063(4) 0.0028(4) 0.0005(4) C15 0.0205(6) 0.0148(5) 0.0209(6) 0.0016(5) 0.0051(5) -0.0001(5) C16 0.0231(7) 0.0163(6) 0.0250(7) 0.0016(5) 0.0005(5) -0.0039(5) C17 0.0174(6) 0.0214(6) 0.0298(7) 0.0072(5) 0.0027(5) -0.0044(5) C18 0.0184(6) 0.0295(7) 0.0260(7) 0.0033(6) 0.0096(5) -0.0034(5) C19 0.0194(6) 0.0230(6) 0.0188(6) 0.0008(5) 0.0067(5) -0.0042(5) C20 0.0146(6) 0.0149(5) 0.0168(5) 0.0052(4) 0.0026(4) -0.0004(4) C21 0.0100(5) 0.0157(5) 0.0124(5) 0.0025(4) 0.0016(4) 0.0002(4) C22 0.0132(5) 0.0217(6) 0.0144(5) -0.0007(4) 0.0031(4) -0.0020(5) C23 0.0139(6) 0.0323(7) 0.0172(6) -0.0038(5) 0.0024(5) -0.0064(5) C24 0.0111(6) 0.0453(9) 0.0181(6) -0.0009(6) 0.0006(5) -0.0016(6) C25 0.0134(6) 0.0348(8) 0.0232(6) 0.0039(6) 0.0028(5) 0.0071(5) C26 0.0137(6) 0.0204(6) 0.0197(6) 0.0033(5) 0.0024(5) 0.0033(5) C27 0.0100(5) 0.0188(5) 0.0112(5) 0.0030(4) 0.0024(4) 0.0003(4) C28 0.0212(6) 0.0165(6) 0.0252(6) -0.0035(5) 0.0091(5) -0.0028(5) C29 0.0287(8) 0.0173(6) 0.0376(8) -0.0098(6) 0.0114(6) -0.0063(6) C30 0.0300(8) 0.0207(7) 0.0296(7) -0.0122(6) 0.0047(6) 0.0012(6) C31 0.0284(7) 0.0228(7) 0.0190(6) -0.0039(5) 0.0077(5) 0.0053(6) C32 0.0199(6) 0.0161(6) 0.0183(6) -0.0006(4) 0.0055(5) 0.0024(5) C33 0.0129(5) 0.0125(5) 0.0147(5) -0.0006(4) 0.0022(4) 0.0027(4) O1 0.0317(6) 0.0356(6) 0.0330(6) 0.0017(5) -0.0001(5) 0.0115(5) C34 0.0389(9) 0.0212(7) 0.0379(9) -0.0003(6) 0.0170(7) 0.0049(6) C35 0.0275(8) 0.0378(9) 0.0283(8) -0.0065(6) 0.0077(6) 0.0000(7) C36 0.0262(8) 0.0417(9) 0.0277(7) 0.0014(7) 0.0056(6) 0.0132(7) C37 0.0337(9) 0.0235(7) 0.0290(7) -0.0024(6) 0.0078(6) 0.0021(6) _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 P2 2.5164(3) . ? Mo1 P2 2.5164(3) 3_556 ? Mo1 P1 2.5566(3) . ? Mo1 P1 2.5566(3) 3_556 ? Mo1 Br1 2.58297(12) . ? Mo1 Br1 2.58300(12) 3_556 ? N1 C21 1.4601(16) . ? N1 C13 1.4622(16) . ? N1 C14 1.4820(15) . ? P1 C6 1.8339(12) . ? P1 C12 1.8404(12) . ? P1 C13 1.8551(12) . ? P2 C33 1.8296(12) . ? P2 C27 1.8454(12) . ? P2 C21 1.8556(12) . ? C1 C2 1.3908(18) . ? C1 C6 1.3934(17) . ? C1 H1A 0.9300 . ? C2 C3 1.382(2) . ? C2 H2A 0.9300 . ? C3 C4 1.387(2) . ? C3 H3A 0.9300 . ? C4 C5 1.3894(18) . ? C4 H4A 0.9300 . ? C5 C6 1.3953(17) . ? C5 H5A 0.9300 . ? C7 C8 1.3861(18) . ? C7 C12 1.3977(16) . ? C7 H7A 0.9300 . ? C8 C9 1.3878(19) . ? C8 H8A 0.9300 . ? C9 C10 1.3859(19) . ? C9 H9A 0.9300 . ? C10 C11 1.3940(18) . ? C10 H10A 0.9300 . ? C11 C12 1.3998(17) . ? C11 H11A 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C20 1.5085(18) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.390(2) . ? C15 C20 1.3933(18) . ? C15 H15A 0.9300 . ? C16 C17 1.382(2) . ? C16 H16A 0.9300 . ? C17 C18 1.383(2) . ? C17 H17A 0.9300 . ? C18 C19 1.395(2) . ? C18 H18A 0.9300 . ? C19 C20 1.3913(19) . ? C19 H19A 0.9300 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.3926(18) . ? C22 C27 1.3964(18) . ? C22 H22A 0.9300 . ? C23 C24 1.384(2) . ? C23 H23A 0.9300 . ? C24 C25 1.387(2) . ? C24 H24A 0.9300 . ? C25 C26 1.3916(19) . ? C25 H25A 0.9300 . ? C26 C27 1.3974(18) . ? C26 H26A 0.9300 . ? C28 C29 1.3922(19) . ? C28 C33 1.3939(18) . ? C28 H28A 0.9300 . ? C29 C30 1.387(2) . ? C29 H29A 0.9300 . ? C30 C31 1.385(2) . ? C30 H30A 0.9300 . ? C31 C32 1.3857(19) . ? C31 H31A 0.9300 . ? C32 C33 1.3935(18) . ? C32 H32A 0.9300 . ? O1 C34 1.425(2) . ? O1 C37 1.4289(19) . ? C34 C35 1.517(2) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.512(2) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.503(2) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? 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 P2 Mo1 P2 180.0 . 3_556 ? P2 Mo1 P1 84.528(10) . . ? P2 Mo1 P1 95.471(10) 3_556 . ? P2 Mo1 P1 95.471(10) . 3_556 ? P2 Mo1 P1 84.529(10) 3_556 3_556 ? P1 Mo1 P1 180.0 . 3_556 ? P2 Mo1 Br1 93.471(8) . . ? P2 Mo1 Br1 86.528(7) 3_556 . ? P1 Mo1 Br1 100.520(7) . . ? P1 Mo1 Br1 79.481(7) 3_556 . ? P2 Mo1 Br1 86.529(7) . 3_556 ? P2 Mo1 Br1 93.472(8) 3_556 3_556 ? P1 Mo1 Br1 79.481(7) . 3_556 ? P1 Mo1 Br1 100.518(7) 3_556 3_556 ? Br1 Mo1 Br1 180.0 . 3_556 ? C21 N1 C13 111.43(10) . . ? C21 N1 C14 109.94(9) . . ? C13 N1 C14 110.09(10) . . ? C6 P1 C12 101.71(5) . . ? C6 P1 C13 98.15(5) . . ? C12 P1 C13 97.38(5) . . ? C6 P1 Mo1 121.21(4) . . ? C12 P1 Mo1 119.45(4) . . ? C13 P1 Mo1 114.50(4) . . ? C33 P2 C27 102.43(6) . . ? C33 P2 C21 102.19(6) . . ? C27 P2 C21 94.21(5) . . ? C33 P2 Mo1 115.81(4) . . ? C27 P2 Mo1 121.15(4) . . ? C21 P2 Mo1 117.37(4) . . ? C2 C1 C6 120.63(12) . . ? C2 C1 H1A 119.7 . . ? C6 C1 H1A 119.7 . . ? C3 C2 C1 120.38(13) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 119.54(12) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 120.18(13) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 120.72(12) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 118.45(11) . . ? C5 C6 P1 122.67(9) . . ? C1 C6 P1 118.65(9) . . ? C8 C7 C12 121.35(12) . . ? C8 C7 H7A 119.3 . . ? C12 C7 H7A 119.3 . . ? C7 C8 C9 120.00(12) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 119.64(12) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C9 C10 C11 120.40(12) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C10 C11 C12 120.57(12) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C7 C12 C11 118.05(11) . . ? C7 C12 P1 119.73(9) . . ? C11 C12 P1 122.22(9) . . ? N1 C13 P1 112.45(8) . . ? N1 C13 H13A 109.1 . . ? P1 C13 H13A 109.1 . . ? N1 C13 H13B 109.1 . . ? P1 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N1 C14 C20 111.67(10) . . ? N1 C14 H14A 109.3 . . ? C20 C14 H14A 109.3 . . ? N1 C14 H14B 109.3 . . ? C20 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C20 120.57(13) . . ? C16 C15 H15A 119.7 . . ? C20 C15 H15A 119.7 . . ? C17 C16 C15 120.15(13) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C18 C17 C16 119.96(13) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 120.02(14) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C20 120.48(13) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C15 C20 C19 118.82(12) . . ? C15 C20 C14 120.46(12) . . ? C19 C20 C14 120.69(12) . . ? N1 C21 P2 115.80(8) . . ? N1 C21 H21A 108.3 . . ? P2 C21 H21A 108.3 . . ? N1 C21 H21B 108.3 . . ? P2 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C23 C22 C27 120.56(13) . . ? C23 C22 H22A 119.7 . . ? C27 C22 H22A 119.7 . . ? C24 C23 C22 120.39(14) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.60(13) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C24 C25 C26 120.28(14) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C27 120.62(13) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C22 C27 C26 118.52(12) . . ? C22 C27 P2 119.22(10) . . ? C26 C27 P2 122.16(10) . . ? C29 C28 C33 120.61(13) . . ? C29 C28 H28A 119.7 . . ? C33 C28 H28A 119.7 . . ? C30 C29 C28 120.07(14) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C31 C30 C29 119.62(13) . . ? C31 C30 H30A 120.2 . . ? C29 C30 H30A 120.2 . . ? C30 C31 C32 120.37(14) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C31 C32 C33 120.69(13) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C32 C33 C28 118.64(12) . . ? C32 C33 P2 119.00(10) . . ? C28 C33 P2 122.22(10) . . ? C34 O1 C37 109.00(12) . . ? O1 C34 C35 106.28(12) . . ? O1 C34 H34A 110.5 . . ? C35 C34 H34A 110.5 . . ? O1 C34 H34B 110.5 . . ? C35 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? C36 C35 C34 100.87(13) . . ? C36 C35 H35A 111.6 . . ? C34 C35 H35A 111.6 . . ? C36 C35 H35B 111.6 . . ? C34 C35 H35B 111.6 . . ? H35A C35 H35B 109.4 . . ? C37 C36 C35 101.52(13) . . ? C37 C36 H36A 111.5 . . ? C35 C36 H36A 111.5 . . ? C37 C36 H36B 111.5 . . ? C35 C36 H36B 111.5 . . ? H36A C36 H36B 109.3 . . ? O1 C37 C36 106.06(13) . . ? O1 C37 H37A 110.5 . . ? C36 C37 H37A 110.5 . . ? O1 C37 H37B 110.5 . . ? C36 C37 H37B 110.5 . . ? H37A C37 H37B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.514 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.073 #===END data_trans-Mo(N2)2(PPhNMePPh)2_(7-Mo) _database_code_depnum_ccdc_archive 'CCDC 854197' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H27 Mo0.50 N3 P2' _chemical_formula_weight 503.43 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' _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 8.9918(5) _cell_length_b 13.9020(9) _cell_length_c 19.5071(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.521(3) _cell_angle_gamma 90.00 _cell_volume 2411.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8934 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 32.91 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.449 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9316 _exptl_absorpt_correction_T_max 0.9823 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42029 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_sigmaI/netI 0.1039 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 33.26 _reflns_number_total 9226 _reflns_number_gt 5847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0277P)^2^+0.7158P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9226 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.5000 1.0000 0.0000 0.00906(6) Uani 1 2 d S . . N1 N 0.83163(19) 0.90097(12) 0.14111(9) 0.0134(4) Uani 1 1 d . . . N2 N 0.3201(2) 0.98410(12) 0.05111(9) 0.0134(4) Uani 1 1 d . . . N3 N 0.2201(2) 0.97407(14) 0.07617(10) 0.0212(4) Uani 1 1 d . . . P1 P 0.68152(6) 1.06568(4) 0.09648(3) 0.01133(11) Uani 1 1 d . . . P2 P 0.59445(6) 0.84152(4) 0.04043(3) 0.01089(11) Uani 1 1 d . . . C1 C 0.7577(3) 1.10686(16) 0.23836(11) 0.0192(5) Uani 1 1 d . . . H1A H 0.8508 1.1282 0.2262 0.023 Uiso 1 1 calc R . . C2 C 0.7360(3) 1.10949(16) 0.30684(12) 0.0221(5) Uani 1 1 d . . . H2A H 0.8140 1.1318 0.3414 0.026 Uiso 1 1 calc R . . C3 C 0.6010(3) 1.07972(15) 0.32513(12) 0.0214(5) Uani 1 1 d . . . H3A H 0.5852 1.0828 0.3722 0.026 Uiso 1 1 calc R . . C4 C 0.4884(3) 1.04533(16) 0.27484(11) 0.0192(5) Uani 1 1 d . . . H4A H 0.3959 1.0238 0.2874 0.023 Uiso 1 1 calc R . . C5 C 0.5112(3) 1.04244(15) 0.20599(11) 0.0157(4) Uani 1 1 d . . . H5A H 0.4338 1.0189 0.1717 0.019 Uiso 1 1 calc R . . C6 C 0.6461(2) 1.07355(14) 0.18667(11) 0.0139(4) Uani 1 1 d . . . C7 C 0.8886(2) 1.19497(15) 0.04984(11) 0.0163(4) Uani 1 1 d . . . H7A H 0.9258 1.1400 0.0289 0.020 Uiso 1 1 calc R . . C8 C 0.9539(3) 1.28423(16) 0.04241(12) 0.0185(5) Uani 1 1 d . . . H8A H 1.0356 1.2899 0.0169 0.022 Uiso 1 1 calc R . . C9 C 0.8998(3) 1.36476(16) 0.07215(12) 0.0215(5) Uani 1 1 d . . . H9A H 0.9439 1.4259 0.0669 0.026 Uiso 1 1 calc R . . C10 C 0.7812(3) 1.35607(16) 0.10960(12) 0.0202(5) Uani 1 1 d . . . H10A H 0.7432 1.4114 0.1298 0.024 Uiso 1 1 calc R . . C11 C 0.7176(2) 1.26636(15) 0.11774(11) 0.0166(4) Uani 1 1 d . . . H11A H 0.6377 1.2608 0.1443 0.020 Uiso 1 1 calc R . . C12 C 0.7692(2) 1.18486(15) 0.08762(11) 0.0134(4) Uani 1 1 d . . . C13 C 0.8594(2) 0.99576(15) 0.11311(10) 0.0141(4) Uani 1 1 d . . . H13A H 0.9017 0.9882 0.0694 0.017 Uiso 1 1 calc R . . H13B H 0.9337 1.0309 0.1465 0.017 Uiso 1 1 calc R . . C14 C 0.9615(3) 0.86783(17) 0.19016(12) 0.0240(5) Uani 1 1 d . . . H14A H 0.9380 0.8057 0.2098 0.036 Uiso 1 1 calc R . . H14B H 0.9844 0.9150 0.2276 0.036 Uiso 1 1 calc R . . H14C H 1.0488 0.8606 0.1659 0.036 Uiso 1 1 calc R . . C15 C 0.7908(2) 0.83089(15) 0.08611(11) 0.0134(4) Uani 1 1 d . . . H15A H 0.8049 0.7655 0.1062 0.016 Uiso 1 1 calc R . . H15B H 0.8606 0.8379 0.0517 0.016 Uiso 1 1 calc R . . C16 C 0.6200(3) 0.64535(15) -0.00202(11) 0.0168(4) Uani 1 1 d . . . H16A H 0.6024 0.6277 0.0432 0.020 Uiso 1 1 calc R . . C17 C 0.6461(3) 0.57401(16) -0.04858(12) 0.0194(5) Uani 1 1 d . . . H17A H 0.6457 0.5083 -0.0353 0.023 Uiso 1 1 calc R . . C18 C 0.6728(3) 0.59891(17) -0.11430(12) 0.0207(5) Uani 1 1 d . . . H18A H 0.6889 0.5504 -0.1467 0.025 Uiso 1 1 calc R . . C19 C 0.6761(3) 0.69493(17) -0.13260(12) 0.0202(5) Uani 1 1 d . . . H19A H 0.6967 0.7123 -0.1773 0.024 Uiso 1 1 calc R . . C20 C 0.6494(2) 0.76596(16) -0.08608(11) 0.0152(4) Uani 1 1 d . . . H20A H 0.6520 0.8316 -0.0993 0.018 Uiso 1 1 calc R . . C21 C 0.6189(2) 0.74229(14) -0.02027(11) 0.0123(4) Uani 1 1 d . . . C22 C 0.5217(2) 0.80681(15) 0.17326(11) 0.0151(4) Uani 1 1 d . . . H22A H 0.6038 0.8482 0.1890 0.018 Uiso 1 1 calc R . . C23 C 0.4363(3) 0.76939(16) 0.22071(12) 0.0182(5) Uani 1 1 d . . . H23A H 0.4596 0.7855 0.2684 0.022 Uiso 1 1 calc R . . C24 C 0.3169(3) 0.70845(16) 0.19834(12) 0.0203(5) Uani 1 1 d . . . H24A H 0.2596 0.6816 0.2308 0.024 Uiso 1 1 calc R . . C25 C 0.2816(3) 0.68692(16) 0.12865(12) 0.0200(5) Uani 1 1 d . . . H25A H 0.1988 0.6460 0.1132 0.024 Uiso 1 1 calc R . . C26 C 0.3659(2) 0.72453(15) 0.08115(11) 0.0161(4) Uani 1 1 d . . . H26A H 0.3402 0.7095 0.0334 0.019 Uiso 1 1 calc R . . C27 C 0.4891(2) 0.78477(14) 0.10298(11) 0.0120(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.00844(11) 0.00890(11) 0.00983(11) -0.00031(10) 0.00132(8) 0.00008(10) N1 0.0133(9) 0.0124(9) 0.0136(9) 0.0001(7) -0.0013(7) 0.0003(7) N2 0.0170(9) 0.0106(9) 0.0115(8) -0.0011(6) -0.0021(7) -0.0013(7) N3 0.0165(10) 0.0258(11) 0.0213(10) -0.0044(8) 0.0021(8) -0.0014(8) P1 0.0104(2) 0.0116(3) 0.0119(3) -0.0013(2) 0.00125(19) -0.0004(2) P2 0.0108(3) 0.0103(2) 0.0115(3) 0.0002(2) 0.00168(19) 0.0003(2) C1 0.0230(12) 0.0183(11) 0.0158(11) -0.0008(9) 0.0018(9) -0.0017(9) C2 0.0307(14) 0.0191(12) 0.0149(11) -0.0022(9) -0.0015(9) -0.0012(10) C3 0.0387(15) 0.0125(10) 0.0144(11) 0.0022(9) 0.0079(10) 0.0046(10) C4 0.0227(12) 0.0176(11) 0.0192(12) 0.0008(9) 0.0093(9) 0.0042(9) C5 0.0181(11) 0.0140(10) 0.0153(11) 0.0012(8) 0.0029(8) 0.0030(9) C6 0.0176(11) 0.0100(10) 0.0138(10) -0.0006(8) 0.0008(8) 0.0001(8) C7 0.0148(11) 0.0150(10) 0.0194(11) -0.0021(9) 0.0035(9) 0.0012(8) C8 0.0138(10) 0.0214(12) 0.0207(11) 0.0007(9) 0.0037(9) -0.0026(9) C9 0.0201(12) 0.0133(11) 0.0307(13) -0.0011(10) 0.0021(10) -0.0053(9) C10 0.0195(12) 0.0139(11) 0.0269(13) -0.0041(9) 0.0027(10) 0.0008(9) C11 0.0127(10) 0.0179(11) 0.0187(11) -0.0028(9) 0.0010(8) -0.0009(8) C12 0.0117(10) 0.0145(10) 0.0128(10) 0.0000(8) -0.0016(8) -0.0028(8) C13 0.0113(9) 0.0137(9) 0.0162(9) -0.0012(9) -0.0015(7) -0.0005(9) C14 0.0245(13) 0.0193(12) 0.0242(13) 0.0023(10) -0.0091(10) -0.0001(10) C15 0.0122(10) 0.0127(10) 0.0152(10) 0.0001(8) 0.0020(8) 0.0019(8) C16 0.0211(11) 0.0154(11) 0.0139(10) -0.0012(8) 0.0023(8) 0.0009(9) C17 0.0242(12) 0.0123(10) 0.0217(12) -0.0020(9) 0.0040(9) 0.0021(9) C18 0.0199(12) 0.0215(12) 0.0206(12) -0.0079(10) 0.0027(9) 0.0033(9) C19 0.0215(12) 0.0256(12) 0.0145(11) -0.0014(9) 0.0059(9) 0.0012(10) C20 0.0135(10) 0.0165(11) 0.0156(10) 0.0001(9) 0.0016(8) 0.0000(8) C21 0.0103(10) 0.0130(10) 0.0129(10) -0.0005(8) -0.0001(8) 0.0027(8) C22 0.0152(11) 0.0138(10) 0.0168(11) -0.0010(8) 0.0044(8) -0.0012(8) C23 0.0219(12) 0.0182(11) 0.0153(11) -0.0017(9) 0.0058(9) 0.0014(9) C24 0.0210(12) 0.0208(12) 0.0212(12) 0.0027(9) 0.0097(9) -0.0004(9) C25 0.0180(12) 0.0191(11) 0.0238(12) -0.0009(10) 0.0057(10) -0.0040(9) C26 0.0154(11) 0.0162(11) 0.0163(11) 0.0016(9) 0.0008(8) -0.0010(9) C27 0.0128(10) 0.0079(9) 0.0157(10) 0.0014(8) 0.0039(8) 0.0020(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 2.0338(19) . ? Mo1 N2 2.0338(19) 3_675 ? Mo1 P2 2.4493(5) 3_675 ? Mo1 P2 2.4493(5) . ? Mo1 P1 2.4758(5) . ? Mo1 P1 2.4758(5) 3_675 ? N1 C15 1.455(3) . ? N1 C13 1.462(3) . ? N1 C14 1.470(3) . ? N2 N3 1.095(2) . ? P1 C6 1.837(2) . ? P1 C12 1.854(2) . ? P1 C13 1.859(2) . ? P2 C27 1.831(2) . ? P2 C21 1.852(2) . ? P2 C15 1.862(2) . ? C1 C2 1.379(3) . ? C1 C6 1.392(3) . ? C1 H1A 0.9500 . ? C2 C3 1.378(3) . ? C2 H2A 0.9500 . ? C3 C4 1.387(3) . ? C3 H3A 0.9500 . ? C4 C5 1.389(3) . ? C4 H4A 0.9500 . ? C5 C6 1.391(3) . ? C5 H5A 0.9500 . ? C7 C8 1.389(3) . ? C7 C12 1.397(3) . ? C7 H7A 0.9500 . ? C8 C9 1.382(3) . ? C8 H8A 0.9500 . ? C9 C10 1.384(3) . ? C9 H9A 0.9500 . ? C10 C11 1.391(3) . ? C10 H10A 0.9500 . ? C11 C12 1.387(3) . ? C11 H11A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.388(3) . ? C16 C21 1.394(3) . ? C16 H16A 0.9500 . ? C17 C18 1.383(3) . ? C17 H17A 0.9500 . ? C18 C19 1.383(3) . ? C18 H18A 0.9500 . ? C19 C20 1.386(3) . ? C19 H19A 0.9500 . ? C20 C21 1.391(3) . ? C20 H20A 0.9500 . ? C22 C23 1.388(3) . ? C22 C27 1.393(3) . ? C22 H22A 0.9500 . ? C23 C24 1.386(3) . ? C23 H23A 0.9500 . ? C24 C25 1.382(3) . ? C24 H24A 0.9500 . ? C25 C26 1.384(3) . ? C25 H25A 0.9500 . ? C26 C27 1.403(3) . ? C26 H26A 0.9500 . ? 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 N2 180.0 . 3_675 ? N2 Mo1 P2 89.58(5) . 3_675 ? N2 Mo1 P2 90.42(5) 3_675 3_675 ? N2 Mo1 P2 90.42(5) . . ? N2 Mo1 P2 89.58(5) 3_675 . ? P2 Mo1 P2 180.0 3_675 . ? N2 Mo1 P1 98.63(5) . . ? N2 Mo1 P1 81.37(5) 3_675 . ? P2 Mo1 P1 94.077(18) 3_675 . ? P2 Mo1 P1 85.924(18) . . ? N2 Mo1 P1 81.37(5) . 3_675 ? N2 Mo1 P1 98.63(5) 3_675 3_675 ? P2 Mo1 P1 85.924(18) 3_675 3_675 ? P2 Mo1 P1 94.075(18) . 3_675 ? P1 Mo1 P1 180.0 . 3_675 ? C15 N1 C13 111.49(16) . . ? C15 N1 C14 111.05(16) . . ? C13 N1 C14 111.24(17) . . ? N3 N2 Mo1 177.07(17) . . ? C6 P1 C12 99.93(9) . . ? C6 P1 C13 97.51(9) . . ? C12 P1 C13 96.72(10) . . ? C6 P1 Mo1 124.17(7) . . ? C12 P1 Mo1 120.02(7) . . ? C13 P1 Mo1 113.15(7) . . ? C27 P2 C21 103.14(9) . . ? C27 P2 C15 101.23(10) . . ? C21 P2 C15 93.03(9) . . ? C27 P2 Mo1 114.40(7) . . ? C21 P2 Mo1 122.17(7) . . ? C15 P2 Mo1 118.98(7) . . ? C2 C1 C6 121.3(2) . . ? C2 C1 H1A 119.3 . . ? C6 C1 H1A 119.3 . . ? C3 C2 C1 120.0(2) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 120.0(2) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C1 C6 C5 118.1(2) . . ? C1 C6 P1 120.31(17) . . ? C5 C6 P1 121.52(16) . . ? C8 C7 C12 121.0(2) . . ? C8 C7 H7A 119.5 . . ? C12 C7 H7A 119.5 . . ? C9 C8 C7 120.0(2) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 119.8(2) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C9 C10 C11 120.0(2) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 121.0(2) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C7 118.20(19) . . ? C11 C12 P1 121.15(16) . . ? C7 C12 P1 120.65(16) . . ? N1 C13 P1 110.27(14) . . ? N1 C13 H13A 109.6 . . ? P1 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? P1 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 P2 114.66(14) . . ? N1 C15 H15A 108.6 . . ? P2 C15 H15A 108.6 . . ? N1 C15 H15B 108.6 . . ? P2 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C21 121.3(2) . . ? C17 C16 H16A 119.4 . . ? C21 C16 H16A 119.4 . . ? C18 C17 C16 119.8(2) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C19 C18 C17 119.6(2) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C18 C19 C20 120.4(2) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C21 120.8(2) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C20 C21 C16 118.01(19) . . ? C20 C21 P2 118.17(15) . . ? C16 C21 P2 123.63(16) . . ? C23 C22 C27 121.1(2) . . ? C23 C22 H22A 119.4 . . ? C27 C22 H22A 119.4 . . ? C24 C23 C22 119.9(2) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C23 C24 C25 119.8(2) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C26 C25 C24 120.5(2) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 120.5(2) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C22 C27 C26 118.14(19) . . ? C22 C27 P2 120.45(16) . . ? C26 C27 P2 121.20(16) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.582 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.120 #===END data_[MoBr2(PEtNMePEt)]2 _database_code_depnum_ccdc_archive 'CCDC 854198' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H31 Br2 Mo N P2' _chemical_formula_weight 567.13 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' Br Br -0.2901 2.4595 '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 10.7168(4) _cell_length_b 13.4035(6) _cell_length_c 15.4417(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.0530(10) _cell_angle_gamma 90.00 _cell_volume 2160.77(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9345 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 34.17 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 4.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4408 _exptl_absorpt_correction_T_max 0.8420 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35063 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 34.17 _reflns_number_total 8815 _reflns_number_gt 7045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0295P)^2^+0.3386P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8815 _refine_ls_number_parameters 220 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.952077(13) 0.063648(11) 0.019323(9) 0.01179(3) Uani 1 1 d . . . Br1 Br 0.730664(16) 0.100751(14) -0.084750(11) 0.01779(4) Uani 1 1 d . . . Br2 Br 1.034093(17) 0.226290(13) -0.036179(11) 0.01767(4) Uani 1 1 d . . . N1 N 0.98391(14) -0.01179(12) 0.27827(9) 0.0183(3) Uani 1 1 d . . . P1 P 0.81536(4) -0.01584(3) 0.11343(3) 0.01444(8) Uani 1 1 d . . . P2 P 1.09393(4) 0.10559(4) 0.16897(3) 0.01620(9) Uani 1 1 d . . . C1 C 0.7224(5) 0.0831(11) 0.1531(9) 0.0244(7) Uani 0.803(4) 1 d PD A 1 H1A H 0.7813 0.1202 0.2009 0.029 Uiso 0.803(4) 1 calc PR A 1 H1B H 0.6925 0.1303 0.1034 0.029 Uiso 0.803(4) 1 calc PR A 1 C2 C 0.6062(3) 0.0512(2) 0.1884(2) 0.0333(6) Uani 0.803(4) 1 d PD A 1 H2A H 0.5671 0.1101 0.2090 0.050 Uiso 0.803(4) 1 calc PR A 1 H2B H 0.6335 0.0047 0.2380 0.050 Uiso 0.803(4) 1 calc PR A 1 H2C H 0.5436 0.0184 0.1409 0.050 Uiso 0.803(4) 1 calc PR A 1 C1' C 0.7290(19) 0.081(5) 0.159(4) 0.0244(7) Uani 0.197(4) 1 d PD A 2 H1'A H 0.7369 0.0663 0.2226 0.029 Uiso 0.197(4) 1 calc PR A 2 H1'B H 0.7728 0.1451 0.1548 0.029 Uiso 0.197(4) 1 calc PR A 2 C2' C 0.5884(10) 0.0947(9) 0.1165(8) 0.0333(6) Uani 0.197(4) 1 d PD A 2 H2'A H 0.5521 0.1449 0.1499 0.050 Uiso 0.197(4) 1 calc PR A 2 H2'B H 0.5433 0.0312 0.1173 0.050 Uiso 0.197(4) 1 calc PR A 2 H2'C H 0.5787 0.1170 0.0549 0.050 Uiso 0.197(4) 1 calc PR A 2 C3 C 0.69272(17) -0.10498(14) 0.05777(12) 0.0189(3) Uani 1 1 d . A . H3A H 0.6165 -0.0666 0.0273 0.023 Uiso 1 1 calc R . . H3B H 0.7261 -0.1400 0.0113 0.023 Uiso 1 1 calc R . . C4 C 0.6495(2) -0.18311(17) 0.11592(14) 0.0327(5) Uani 1 1 d . . . H4A H 0.5801 -0.2229 0.0799 0.049 Uiso 1 1 calc R A . H4B H 0.6189 -0.1501 0.1638 0.049 Uiso 1 1 calc R . . H4C H 0.7217 -0.2268 0.1416 0.049 Uiso 1 1 calc R . . C5 C 0.89791(18) -0.07849(13) 0.21674(11) 0.0182(3) Uani 1 1 d . A . H5A H 0.8331 -0.1058 0.2469 0.022 Uiso 1 1 calc R . . H5B H 0.9482 -0.1352 0.2015 0.022 Uiso 1 1 calc R . . C6 C 1.00883(18) -0.05391(15) 0.36891(11) 0.0210(4) Uani 1 1 d . . . H6A H 1.0776 -0.0148 0.4080 0.025 Uiso 1 1 calc R . . H6B H 1.0397 -0.1233 0.3673 0.025 Uiso 1 1 calc R . . C7 C 0.81992(19) 0.03249(14) 0.40626(12) 0.0231(4) Uani 1 1 d . . . H7A H 0.8422 0.0907 0.3780 0.028 Uiso 1 1 calc R . . C8 C 0.7154(2) 0.03461(16) 0.44535(13) 0.0271(4) Uani 1 1 d . . . H8A H 0.6662 0.0939 0.4432 0.033 Uiso 1 1 calc R . . C9 C 0.68276(19) -0.04919(17) 0.48747(13) 0.0276(4) Uani 1 1 d . . . H9A H 0.6113 -0.0477 0.5144 0.033 Uiso 1 1 calc R . . C10 C 0.75478(19) -0.13526(16) 0.49022(13) 0.0277(4) Uani 1 1 d . . . H10A H 0.7335 -0.1929 0.5197 0.033 Uiso 1 1 calc R . . C11 C 0.85755(18) -0.13742(14) 0.45013(12) 0.0217(4) Uani 1 1 d . . . H11A H 0.9055 -0.1972 0.4514 0.026 Uiso 1 1 calc R . . C12 C 0.89219(17) -0.05356(14) 0.40789(10) 0.0174(3) Uani 1 1 d . . . C13 C 1.10609(17) 0.00643(15) 0.25298(11) 0.0214(4) Uani 1 1 d . A . H13A H 1.1347 -0.0560 0.2292 0.026 Uiso 1 1 calc R . . H13B H 1.1716 0.0254 0.3066 0.026 Uiso 1 1 calc R . . C14 C 1.25960(16) 0.14305(15) 0.17314(11) 0.0195(3) Uani 1 1 d . A . H14A H 1.3027 0.0883 0.1482 0.023 Uiso 1 1 calc R . . H14B H 1.2583 0.2021 0.1344 0.023 Uiso 1 1 calc R . . C15 C 1.33935(19) 0.16831(18) 0.26574(13) 0.0323(5) Uani 1 1 d . . . H15A H 1.4178 0.2028 0.2603 0.049 Uiso 1 1 calc R A . H15B H 1.3617 0.1067 0.2999 0.049 Uiso 1 1 calc R . . H15C H 1.2896 0.2116 0.2964 0.049 Uiso 1 1 calc R . . C16 C 1.0361(2) 0.21023(16) 0.22671(15) 0.0306(5) Uani 1 1 d . A . H16A H 0.9445 0.1988 0.2256 0.037 Uiso 1 1 calc R . . H16B H 1.0833 0.2095 0.2897 0.037 Uiso 1 1 calc R . . C17 C 1.0496(3) 0.31354(17) 0.18892(14) 0.0399(6) Uani 1 1 d . . . H17A H 1.0139 0.3635 0.2229 0.060 Uiso 1 1 calc R A . H17B H 1.0032 0.3157 0.1265 0.060 Uiso 1 1 calc R . . H17C H 1.1404 0.3279 0.1930 0.060 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 0.01119(6) 0.01307(6) 0.01108(6) -0.00086(5) 0.00245(4) -0.00061(5) Br1 0.01386(8) 0.02027(9) 0.01768(7) 0.00173(6) 0.00027(6) 0.00136(6) Br2 0.01960(8) 0.01402(8) 0.01993(8) 0.00111(6) 0.00558(6) -0.00169(6) N1 0.0176(7) 0.0263(8) 0.0107(6) -0.0010(5) 0.0026(5) -0.0050(6) P1 0.01280(18) 0.0176(2) 0.01323(17) -0.00097(15) 0.00357(15) -0.00171(16) P2 0.01403(19) 0.0214(2) 0.01330(17) -0.00458(16) 0.00330(15) -0.00384(17) C1 0.0208(10) 0.0264(13) 0.028(2) -0.0054(13) 0.0102(11) 0.0020(11) C2 0.0228(12) 0.0404(16) 0.0407(14) -0.0128(12) 0.0156(11) -0.0019(11) C1' 0.0208(10) 0.0264(13) 0.028(2) -0.0054(13) 0.0102(11) 0.0020(11) C2' 0.0228(12) 0.0404(16) 0.0407(14) -0.0128(12) 0.0156(11) -0.0019(11) C3 0.0140(7) 0.0234(9) 0.0195(7) -0.0028(7) 0.0042(6) -0.0040(7) C4 0.0306(11) 0.0345(12) 0.0301(10) 0.0055(9) 0.0009(8) -0.0166(10) C5 0.0206(8) 0.0200(8) 0.0135(7) -0.0009(6) 0.0029(6) -0.0027(7) C6 0.0214(8) 0.0299(10) 0.0109(6) 0.0007(7) 0.0021(6) -0.0007(8) C7 0.0330(10) 0.0178(8) 0.0191(8) 0.0029(7) 0.0074(7) 0.0008(8) C8 0.0296(10) 0.0291(10) 0.0227(8) -0.0006(8) 0.0060(8) 0.0085(9) C9 0.0204(9) 0.0402(12) 0.0231(8) 0.0002(8) 0.0068(7) -0.0018(9) C10 0.0254(9) 0.0288(10) 0.0288(9) 0.0071(8) 0.0057(8) -0.0085(8) C11 0.0230(9) 0.0189(8) 0.0218(8) 0.0016(7) 0.0022(7) 0.0001(7) C12 0.0191(8) 0.0210(8) 0.0113(6) -0.0012(6) 0.0020(6) -0.0016(7) C13 0.0172(8) 0.0345(11) 0.0123(7) 0.0005(7) 0.0029(6) -0.0025(7) C14 0.0156(7) 0.0261(9) 0.0172(7) -0.0050(7) 0.0047(6) -0.0058(7) C15 0.0193(9) 0.0516(14) 0.0246(9) -0.0099(9) 0.0017(7) -0.0100(9) C16 0.0227(9) 0.0352(12) 0.0377(11) -0.0212(9) 0.0144(8) -0.0096(8) C17 0.0564(15) 0.0352(12) 0.0240(10) -0.0086(9) 0.0009(10) 0.0185(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo1 2.1445(3) 3_755 ? Mo1 P1 2.5209(4) . ? Mo1 P2 2.5259(4) . ? Mo1 Br2 2.5690(2) . ? Mo1 Br1 2.5957(2) . ? N1 C5 1.468(2) . ? N1 C13 1.469(2) . ? N1 C6 1.477(2) . ? P1 C1' 1.82(6) . ? P1 C3 1.8394(17) . ? P1 C5 1.8426(17) . ? P1 C1 1.844(14) . ? P2 C14 1.8322(18) . ? P2 C13 1.8411(19) . ? P2 C16 1.843(2) . ? C1 C2 1.529(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C1' C2' 1.512(19) . ? C1' H1'A 0.9900 . ? C1' H1'B 0.9900 . ? C2' H2'A 0.9800 . ? C2' H2'B 0.9800 . ? C2' H2'C 0.9800 . ? C3 C4 1.518(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C12 1.505(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.386(3) . ? C7 C8 1.387(3) . ? C7 H7A 0.9500 . ? C8 C9 1.382(3) . ? C8 H8A 0.9500 . ? C9 C10 1.383(3) . ? C9 H9A 0.9500 . ? C10 C11 1.380(3) . ? C10 H10A 0.9500 . ? C11 C12 1.391(3) . ? C11 H11A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.529(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.522(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 Mo1 Mo1 P1 101.622(14) 3_755 . ? Mo1 Mo1 P2 101.803(14) 3_755 . ? P1 Mo1 P2 82.806(15) . . ? Mo1 Mo1 Br2 111.150(10) 3_755 . ? P1 Mo1 Br2 146.941(13) . . ? P2 Mo1 Br2 86.317(12) . . ? Mo1 Mo1 Br1 114.107(10) 3_755 . ? P1 Mo1 Br1 82.461(12) . . ? P2 Mo1 Br1 143.215(13) . . ? Br2 Mo1 Br1 87.976(7) . . ? C5 N1 C13 113.33(14) . . ? C5 N1 C6 109.47(14) . . ? C13 N1 C6 109.53(13) . . ? C1' P1 C3 105.7(12) . . ? C1' P1 C5 100.3(16) . . ? C3 P1 C5 105.14(8) . . ? C1' P1 C1 3.2(17) . . ? C3 P1 C1 103.9(3) . . ? C5 P1 C1 103.3(4) . . ? C1' P1 Mo1 109.4(17) . . ? C3 P1 Mo1 116.88(6) . . ? C5 P1 Mo1 117.63(6) . . ? C1 P1 Mo1 108.4(4) . . ? C14 P2 C13 105.02(8) . . ? C14 P2 C16 101.74(9) . . ? C13 P2 C16 100.75(10) . . ? C14 P2 Mo1 118.12(6) . . ? C13 P2 Mo1 114.59(6) . . ? C16 P2 Mo1 114.42(7) . . ? C2 C1 P1 117.5(9) . . ? C2 C1 H1A 107.9 . . ? P1 C1 H1A 107.9 . . ? C2 C1 H1B 107.9 . . ? P1 C1 H1B 107.9 . . ? H1A C1 H1B 107.2 . . ? C2' C1' P1 118(4) . . ? C2' C1' H1'A 107.9 . . ? P1 C1' H1'A 107.9 . . ? C2' C1' H1'B 107.9 . . ? P1 C1' H1'B 107.9 . . ? H1'A C1' H1'B 107.2 . . ? C1' C2' H2'A 109.5 . . ? C1' C2' H2'B 109.5 . . ? H2'A C2' H2'B 109.5 . . ? C1' C2' H2'C 109.5 . . ? H2'A C2' H2'C 109.5 . . ? H2'B C2' H2'C 109.5 . . ? C4 C3 P1 116.93(13) . . ? C4 C3 H3A 108.1 . . ? P1 C3 H3A 108.1 . . ? C4 C3 H3B 108.1 . . ? P1 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 P1 113.03(12) . . ? N1 C5 H5A 109.0 . . ? P1 C5 H5A 109.0 . . ? N1 C5 H5B 109.0 . . ? P1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N1 C6 C12 112.91(15) . . ? N1 C6 H6A 109.0 . . ? C12 C6 H6A 109.0 . . ? N1 C6 H6B 109.0 . . ? C12 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C12 C7 C8 120.78(18) . . ? C12 C7 H7A 119.6 . . ? C8 C7 H7A 119.6 . . ? C9 C8 C7 120.21(19) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 119.56(19) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C11 C10 C9 120.00(19) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 121.17(18) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C7 C12 C11 118.26(17) . . ? C7 C12 C6 120.42(17) . . ? C11 C12 C6 121.24(17) . . ? N1 C13 P2 112.45(13) . . ? N1 C13 H13A 109.1 . . ? P2 C13 H13A 109.1 . . ? N1 C13 H13B 109.1 . . ? P2 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 P2 115.22(13) . . ? C15 C14 H14A 108.5 . . ? P2 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? P2 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 P2 115.81(15) . . ? C17 C16 H16A 108.3 . . ? P2 C16 H16A 108.3 . . ? C17 C16 H16B 108.3 . . ? P2 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.958 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.111 data_trans-MoBr2(PEtNBnPEt)2_(1) _database_code_depnum_ccdc_archive 'CCDC 854199' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H31 Br Mo0.50 N P2' _chemical_formula_weight 439.25 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' Br Br -0.2901 2.4595 '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 8.8246(4) _cell_length_b 10.0917(4) _cell_length_c 11.2789(5) _cell_angle_alpha 73.2370(10) _cell_angle_beta 84.9840(10) _cell_angle_gamma 85.1490(10) _cell_volume 956.22(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9902 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 33.17 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 2.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5597 _exptl_absorpt_correction_T_max 0.6787 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23040 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 33.19 _reflns_number_total 7248 _reflns_number_gt 6484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0232P)^2^+0.2565P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7248 _refine_ls_number_parameters 220 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0468 _refine_ls_wR_factor_gt 0.0451 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.5000 0.5000 0.5000 0.01095(3) Uani 1 2 d S . . Br1 Br 0.692404(11) 0.661594(11) 0.534554(10) 0.01641(3) Uani 1 1 d . . . N1 N 0.15800(10) 0.78983(9) 0.40552(8) 0.01471(15) Uani 1 1 d . . . P1 P 0.40925(3) 0.66672(3) 0.30513(2) 0.01391(5) Uani 1 1 d . . . P2 P 0.71740(3) 0.40047(3) 0.38886(2) 0.01196(5) Uani 1 1 d . . . C1 C 0.4687(3) 0.8487(3) 0.2480(3) 0.0169(4) Uani 0.630(4) 1 d PU A 1 H1B H 0.4004 0.9019 0.1833 0.020 Uiso 0.630(4) 1 calc PR A 1 H1C H 0.4537 0.8908 0.3177 0.020 Uiso 0.630(4) 1 calc PR A 1 C2 C 0.6334(2) 0.86463(18) 0.19444(18) 0.0205(4) Uani 0.630(4) 1 d PU A 1 H2A H 0.6529 0.9633 0.1642 0.031 Uiso 0.630(4) 1 calc PR A 1 H2B H 0.6502 0.8230 0.1255 0.031 Uiso 0.630(4) 1 calc PR A 1 H2C H 0.7027 0.8178 0.2592 0.031 Uiso 0.630(4) 1 calc PR A 1 C1' C 0.5149(5) 0.8216(5) 0.2573(5) 0.0167(7) Uani 0.370(4) 1 d PU A 2 H1'A H 0.4862 0.8748 0.3180 0.020 Uiso 0.370(4) 1 calc PR A 2 H1'B H 0.6243 0.7919 0.2651 0.020 Uiso 0.370(4) 1 calc PR A 2 C2' C 0.4996(4) 0.9208(3) 0.1293(3) 0.0250(8) Uani 0.370(4) 1 d PU A 2 H2'A H 0.5482 1.0064 0.1237 0.038 Uiso 0.370(4) 1 calc PR A 2 H2'B H 0.3913 0.9425 0.1142 0.038 Uiso 0.370(4) 1 calc PR A 2 H2'C H 0.5491 0.8780 0.0671 0.038 Uiso 0.370(4) 1 calc PR A 2 C3 C 0.41905(13) 0.60018(13) 0.16782(11) 0.0218(2) Uani 1 1 d . A . H3A H 0.5275 0.5747 0.1494 0.026 Uiso 1 1 calc R . . H3B H 0.3651 0.5133 0.1923 0.026 Uiso 1 1 calc R . . C4 C 0.35693(19) 0.6901(2) 0.04715(13) 0.0451(4) Uani 1 1 d . . . H4A H 0.3676 0.6381 -0.0146 0.068 Uiso 1 1 calc R A . H4B H 0.4141 0.7738 0.0163 0.068 Uiso 1 1 calc R . . H4C H 0.2490 0.7165 0.0619 0.068 Uiso 1 1 calc R . . C5 C 0.20426(12) 0.72019(11) 0.30977(10) 0.01716(19) Uani 1 1 d . A . H5A H 0.1796 0.7835 0.2279 0.021 Uiso 1 1 calc R . . H5B H 0.1449 0.6372 0.3251 0.021 Uiso 1 1 calc R . . C6 C 0.03082(12) 0.89366(10) 0.36607(11) 0.01727(19) Uani 1 1 d . . . H6A H -0.0143 0.9240 0.4382 0.021 Uiso 1 1 calc R . . H6B H -0.0492 0.8509 0.3358 0.021 Uiso 1 1 calc R . . C7 C 0.19569(13) 1.09614(11) 0.28629(11) 0.01878(19) Uani 1 1 d . . . H7A H 0.2359 1.0721 0.3657 0.023 Uiso 1 1 calc R . . C8 C 0.24923(14) 1.20847(11) 0.19344(11) 0.0210(2) Uani 1 1 d . . . H8A H 0.3259 1.2606 0.2093 0.025 Uiso 1 1 calc R . . C9 C 0.19079(15) 1.24469(12) 0.07746(11) 0.0239(2) Uani 1 1 d . . . H9A H 0.2278 1.3212 0.0136 0.029 Uiso 1 1 calc R . . C10 C 0.07825(15) 1.16899(13) 0.05501(12) 0.0256(2) Uani 1 1 d . . . H10A H 0.0375 1.1940 -0.0242 0.031 Uiso 1 1 calc R . . C11 C 0.02472(14) 1.05637(12) 0.14824(11) 0.0217(2) Uani 1 1 d . . . H11A H -0.0528 1.0052 0.1323 0.026 Uiso 1 1 calc R . . C12 C 0.08356(12) 1.01798(10) 0.26463(10) 0.01642(18) Uani 1 1 d . . . C13 C 0.88262(11) 0.30914(10) 0.47503(10) 0.01607(18) Uani 1 1 d . . . H13A H 0.9458 0.2591 0.4227 0.019 Uiso 1 1 calc R . . H13B H 0.9457 0.3789 0.4895 0.019 Uiso 1 1 calc R . . C14 C 0.67408(13) 0.27702(11) 0.30524(11) 0.01844(19) Uani 1 1 d . A . H14A H 0.5828 0.3146 0.2582 0.022 Uiso 1 1 calc R . . H14B H 0.7603 0.2710 0.2442 0.022 Uiso 1 1 calc R . . C15 C 0.64533(15) 0.13074(12) 0.38719(12) 0.0234(2) Uani 1 1 d . . . H15A H 0.6162 0.0746 0.3360 0.035 Uiso 1 1 calc R A . H15B H 0.5629 0.1353 0.4503 0.035 Uiso 1 1 calc R . . H15C H 0.7384 0.0885 0.4279 0.035 Uiso 1 1 calc R . . C16 C 0.82554(12) 0.52986(11) 0.26864(10) 0.01617(18) Uani 1 1 d . A . H16A H 0.7540 0.5821 0.2061 0.019 Uiso 1 1 calc R . . H16B H 0.8603 0.5966 0.3083 0.019 Uiso 1 1 calc R . . C17 C 0.96413(13) 0.47776(12) 0.19974(12) 0.0224(2) Uani 1 1 d . . . H17A H 1.0087 0.5565 0.1376 0.034 Uiso 1 1 calc R A . H17B H 0.9325 0.4124 0.1585 0.034 Uiso 1 1 calc R . . H17C H 1.0400 0.4310 0.2590 0.034 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 0.00806(5) 0.01519(5) 0.00995(5) -0.00393(4) -0.00065(4) -0.00130(4) Br1 0.01245(5) 0.02113(5) 0.01800(5) -0.00822(4) -0.00108(4) -0.00467(3) N1 0.0157(4) 0.0138(3) 0.0140(4) -0.0030(3) -0.0030(3) 0.0017(3) P1 0.01344(11) 0.01689(11) 0.01140(11) -0.00333(9) -0.00110(9) -0.00314(8) P2 0.01051(10) 0.01341(10) 0.01172(11) -0.00329(8) -0.00058(8) -0.00054(8) C1 0.0142(12) 0.0152(10) 0.0195(10) -0.0025(8) 0.0002(9) -0.0002(8) C2 0.0169(8) 0.0186(8) 0.0237(9) -0.0028(6) 0.0023(6) -0.0036(6) C1' 0.015(2) 0.0145(17) 0.0191(16) -0.0021(13) -0.0015(16) -0.0013(13) C2' 0.0316(17) 0.0176(13) 0.0209(15) 0.0017(11) 0.0014(13) -0.0028(11) C3 0.0201(5) 0.0322(6) 0.0149(5) -0.0096(4) -0.0016(4) -0.0010(4) C4 0.0356(8) 0.0821(13) 0.0159(6) -0.0161(7) -0.0084(5) 0.0205(8) C5 0.0183(5) 0.0174(4) 0.0171(5) -0.0069(4) -0.0066(4) 0.0037(3) C6 0.0159(4) 0.0154(4) 0.0191(5) -0.0030(4) -0.0024(4) 0.0018(3) C7 0.0218(5) 0.0170(4) 0.0178(5) -0.0049(4) -0.0044(4) 0.0004(4) C8 0.0238(5) 0.0169(4) 0.0218(5) -0.0050(4) -0.0005(4) -0.0015(4) C9 0.0304(6) 0.0199(5) 0.0184(5) -0.0018(4) 0.0008(4) 0.0002(4) C10 0.0335(6) 0.0241(5) 0.0169(5) -0.0017(4) -0.0067(5) 0.0010(5) C11 0.0237(5) 0.0204(5) 0.0211(5) -0.0050(4) -0.0074(4) 0.0011(4) C12 0.0171(4) 0.0141(4) 0.0174(5) -0.0041(4) -0.0028(4) 0.0030(3) C13 0.0127(4) 0.0162(4) 0.0176(5) -0.0019(4) -0.0021(4) -0.0006(3) C14 0.0206(5) 0.0194(4) 0.0173(5) -0.0082(4) -0.0023(4) -0.0007(4) C15 0.0296(6) 0.0177(5) 0.0256(6) -0.0090(4) -0.0039(5) -0.0036(4) C16 0.0136(4) 0.0166(4) 0.0153(5) -0.0011(3) 0.0018(3) 0.0009(3) C17 0.0180(5) 0.0255(5) 0.0213(5) -0.0055(4) 0.0066(4) -0.0009(4) _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 P2 2.4981(3) 2_666 ? Mo1 P2 2.4981(3) . ? Mo1 P1 2.4999(3) . ? Mo1 P1 2.5000(3) 2_666 ? Mo1 Br1 2.57771(12) 2_666 ? Mo1 Br1 2.57773(13) . ? N1 C5 1.4625(14) . ? N1 C13 1.4632(14) 2_666 ? N1 C6 1.4748(13) . ? P1 C1' 1.810(5) . ? P1 C5 1.8441(11) . ? P1 C3 1.8503(12) . ? P1 C1 1.867(3) . ? P2 C14 1.8464(11) . ? P2 C16 1.8486(11) . ? P2 C13 1.8503(10) . ? C1 C2 1.528(3) . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C1' C2' 1.510(6) . ? C1' H1'A 0.9900 . ? C1' H1'B 0.9900 . ? C2' H2'A 0.9800 . ? C2' H2'B 0.9800 . ? C2' H2'C 0.9800 . ? C3 C4 1.5200(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C12 1.5091(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.3872(16) . ? C7 C12 1.3951(15) . ? C7 H7A 0.9500 . ? C8 C9 1.3860(17) . ? C8 H8A 0.9500 . ? C9 C10 1.3849(18) . ? C9 H9A 0.9500 . ? C10 C11 1.3910(17) . ? C10 H10A 0.9500 . ? C11 C12 1.3909(16) . ? C11 H11A 0.9500 . ? C13 N1 1.4632(14) 2_666 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.5274(16) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.5286(15) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 P2 Mo1 P2 180.0 2_666 . ? P2 Mo1 P1 86.488(9) 2_666 . ? P2 Mo1 P1 93.513(9) . . ? P2 Mo1 P1 93.512(9) 2_666 2_666 ? P2 Mo1 P1 86.487(9) . 2_666 ? P1 Mo1 P1 180.000(1) . 2_666 ? P2 Mo1 Br1 86.189(7) 2_666 2_666 ? P2 Mo1 Br1 93.811(7) . 2_666 ? P1 Mo1 Br1 85.195(7) . 2_666 ? P1 Mo1 Br1 94.806(7) 2_666 2_666 ? P2 Mo1 Br1 93.811(7) 2_666 . ? P2 Mo1 Br1 86.189(7) . . ? P1 Mo1 Br1 94.805(7) . . ? P1 Mo1 Br1 85.195(7) 2_666 . ? Br1 Mo1 Br1 179.999(1) 2_666 . ? C5 N1 C13 111.74(8) . 2_666 ? C5 N1 C6 110.55(8) . . ? C13 N1 C6 110.73(8) 2_666 . ? C1' P1 C5 108.13(14) . . ? C1' P1 C3 105.56(16) . . ? C5 P1 C3 98.41(5) . . ? C1' P1 C1 14.70(11) . . ? C5 P1 C1 93.60(9) . . ? C3 P1 C1 106.45(10) . . ? C1' P1 Mo1 112.10(15) . . ? C5 P1 Mo1 115.37(4) . . ? C3 P1 Mo1 116.01(4) . . ? C1 P1 Mo1 122.45(9) . . ? C14 P2 C16 102.81(5) . . ? C14 P2 C13 101.84(5) . . ? C16 P2 C13 96.86(5) . . ? C14 P2 Mo1 117.61(4) . . ? C16 P2 Mo1 114.82(3) . . ? C13 P2 Mo1 119.64(4) . . ? C2 C1 P1 115.32(16) . . ? C2 C1 H1B 108.4 . . ? P1 C1 H1B 108.4 . . ? C2 C1 H1C 108.4 . . ? P1 C1 H1C 108.4 . . ? H1B C1 H1C 107.5 . . ? C2' C1' P1 119.9(3) . . ? C2' C1' H1'A 107.4 . . ? P1 C1' H1'A 107.4 . . ? C2' C1' H1'B 107.4 . . ? P1 C1' H1'B 107.4 . . ? H1'A C1' H1'B 106.9 . . ? C1' C2' H2'A 109.5 . . ? C1' C2' H2'B 109.5 . . ? H2'A C2' H2'B 109.5 . . ? C1' C2' H2'C 109.5 . . ? H2'A C2' H2'C 109.5 . . ? H2'B C2' H2'C 109.5 . . ? C4 C3 P1 120.10(10) . . ? C4 C3 H3A 107.3 . . ? P1 C3 H3A 107.3 . . ? C4 C3 H3B 107.3 . . ? P1 C3 H3B 107.3 . . ? H3A C3 H3B 106.9 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 P1 113.01(7) . . ? N1 C5 H5A 109.0 . . ? P1 C5 H5A 109.0 . . ? N1 C5 H5B 109.0 . . ? P1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N1 C6 C12 111.37(9) . . ? N1 C6 H6A 109.4 . . ? C12 C6 H6A 109.4 . . ? N1 C6 H6B 109.4 . . ? C12 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C12 120.88(10) . . ? C8 C7 H7A 119.6 . . ? C12 C7 H7A 119.6 . . ? C9 C8 C7 119.99(11) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 119.78(11) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C9 C10 C11 120.15(11) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C12 120.66(11) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C11 C12 C7 118.54(10) . . ? C11 C12 C6 121.68(10) . . ? C7 C12 C6 119.77(10) . . ? N1 C13 P2 114.33(7) 2_666 . ? N1 C13 H13A 108.7 2_666 . ? P2 C13 H13A 108.7 . . ? N1 C13 H13B 108.7 2_666 . ? P2 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C15 C14 P2 115.14(8) . . ? C15 C14 H14A 108.5 . . ? P2 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? P2 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 P2 118.08(8) . . ? C17 C16 H16A 107.8 . . ? P2 C16 H16A 107.8 . . ? C17 C16 H16B 107.8 . . ? P2 C16 H16B 107.8 . . ? H16A C16 H16B 107.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.508 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.061 #===END data_trans-Mo(N2)2(PEtNMePEt)2_(trans-6) _database_code_depnum_ccdc_archive 'CCDC 854200' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H54 Mo N6 P4' _chemical_formula_weight 622.53 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.534(3) _cell_length_b 18.737(6) _cell_length_c 19.610(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.308(10) _cell_angle_gamma 90.00 _cell_volume 3102.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 33.22 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8809 _exptl_absorpt_correction_T_max 0.9745 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 57244 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 33.44 _reflns_number_total 11948 _reflns_number_gt 9248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0313P)^2^+0.6525P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11948 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.243118(13) 0.267250(6) 0.383428(6) 0.01100(3) Uani 1 1 d . . . N1 N 0.49792(15) 0.20513(8) 0.56557(7) 0.0255(3) Uani 1 1 d . . . N2 N -0.01764(14) 0.32711(6) 0.20036(6) 0.0158(2) Uani 1 1 d . . . N3 N 0.06882(14) 0.24968(6) 0.44115(6) 0.0159(2) Uani 1 1 d . . . N4 N -0.02709(16) 0.23954(7) 0.47310(7) 0.0237(3) Uani 1 1 d . . . N5 N 0.42164(14) 0.28467(6) 0.32802(6) 0.0141(2) Uani 1 1 d . . . N6 N 0.52319(15) 0.29405(7) 0.29926(7) 0.0212(3) Uani 1 1 d . . . P1 P 0.37681(4) 0.159453(19) 0.43243(2) 0.01671(7) Uani 1 1 d . . . P2 P 0.40129(4) 0.32417(2) 0.482669(19) 0.01680(7) Uani 1 1 d . . . P3 P 0.10508(4) 0.373234(17) 0.333498(19) 0.01252(7) Uani 1 1 d . . . P4 P 0.08592(4) 0.209993(18) 0.283973(18) 0.01252(7) Uani 1 1 d . . . C1 C 0.29389(18) 0.06906(8) 0.41372(9) 0.0236(3) Uani 1 1 d . . . H1A H 0.3015 0.0569 0.3652 0.028 Uiso 1 1 calc R . . H1B H 0.3583 0.0341 0.4435 0.028 Uiso 1 1 calc R . . C2 C 0.12060(19) 0.06270(8) 0.42548(10) 0.0292(4) Uani 1 1 d . . . H2A H 0.0795 0.0157 0.4100 0.044 Uiso 1 1 calc R . . H2B H 0.0576 0.0999 0.3993 0.044 Uiso 1 1 calc R . . H2C H 0.1140 0.0684 0.4747 0.044 Uiso 1 1 calc R . . C3 C 0.58503(17) 0.14733(8) 0.41882(9) 0.0239(3) Uani 1 1 d . . . H3A H 0.5880 0.1500 0.3686 0.029 Uiso 1 1 calc R . . H3B H 0.6460 0.1886 0.4401 0.029 Uiso 1 1 calc R . . C4 C 0.6720(2) 0.08057(11) 0.44519(15) 0.0586(8) Uani 1 1 d . . . H4A H 0.7843 0.0852 0.4404 0.088 Uiso 1 1 calc R . . H4B H 0.6268 0.0394 0.4184 0.088 Uiso 1 1 calc R . . H4C H 0.6615 0.0737 0.4939 0.088 Uiso 1 1 calc R . . C5 C 0.39750(19) 0.15109(9) 0.52721(8) 0.0251(3) Uani 1 1 d . . . H5A H 0.2908 0.1536 0.5413 0.030 Uiso 1 1 calc R . . H5B H 0.4417 0.1034 0.5404 0.030 Uiso 1 1 calc R . . C6 C 0.5382(2) 0.18147(12) 0.63718(9) 0.0393(5) Uani 1 1 d . . . H6A H 0.6098 0.2162 0.6628 0.059 Uiso 1 1 calc R . . H6B H 0.5905 0.1348 0.6382 0.059 Uiso 1 1 calc R . . H6C H 0.4414 0.1776 0.6584 0.059 Uiso 1 1 calc R . . C7 C 0.41893(18) 0.27425(9) 0.56496(8) 0.0250(3) Uani 1 1 d . . . H7A H 0.4775 0.3043 0.6016 0.030 Uiso 1 1 calc R . . H7B H 0.3112 0.2667 0.5768 0.030 Uiso 1 1 calc R . . C8 C 0.61094(17) 0.34366(9) 0.47464(8) 0.0220(3) Uani 1 1 d . . . H8A H 0.6534 0.3021 0.4520 0.026 Uiso 1 1 calc R . . H8B H 0.6121 0.3848 0.4430 0.026 Uiso 1 1 calc R . . C9 C 0.72481(18) 0.36014(10) 0.53930(9) 0.0286(4) Uani 1 1 d . . . H9A H 0.8285 0.3726 0.5268 0.043 Uiso 1 1 calc R . . H9B H 0.7355 0.3182 0.5694 0.043 Uiso 1 1 calc R . . H9C H 0.6842 0.4003 0.5635 0.043 Uiso 1 1 calc R . . C10 C 0.34542(18) 0.41038(9) 0.51911(9) 0.0254(3) Uani 1 1 d . . . H10A H 0.4188 0.4202 0.5620 0.031 Uiso 1 1 calc R . . H10B H 0.3589 0.4489 0.4859 0.031 Uiso 1 1 calc R . . C11 C 0.17536(19) 0.41249(10) 0.53532(9) 0.0299(4) Uani 1 1 d . . . H11A H 0.1494 0.4612 0.5481 0.045 Uiso 1 1 calc R . . H11B H 0.1654 0.3801 0.5737 0.045 Uiso 1 1 calc R . . H11C H 0.1024 0.3976 0.4946 0.045 Uiso 1 1 calc R . . C12 C -0.10098(16) 0.38526(7) 0.35081(8) 0.0166(3) Uani 1 1 d . . . H12A H -0.1531 0.3379 0.3469 0.020 Uiso 1 1 calc R . . H12B H -0.0963 0.4008 0.3993 0.020 Uiso 1 1 calc R . . C13 C -0.20700(18) 0.43709(8) 0.30609(10) 0.0273(4) Uani 1 1 d . . . H13A H -0.3094 0.4405 0.3229 0.041 Uiso 1 1 calc R . . H13B H -0.2232 0.4200 0.2583 0.041 Uiso 1 1 calc R . . H13C H -0.1569 0.4842 0.3081 0.041 Uiso 1 1 calc R . . C14 C 0.18302(17) 0.46454(7) 0.35095(8) 0.0180(3) Uani 1 1 d . . . H14A H 0.1132 0.4989 0.3227 0.022 Uiso 1 1 calc R . . H14B H 0.1805 0.4762 0.4000 0.022 Uiso 1 1 calc R . . C15 C 0.35270(17) 0.47342(8) 0.33518(9) 0.0216(3) Uani 1 1 d . . . H15A H 0.3915 0.5212 0.3491 0.032 Uiso 1 1 calc R . . H15B H 0.3540 0.4672 0.2856 0.032 Uiso 1 1 calc R . . H15C H 0.4212 0.4375 0.3607 0.032 Uiso 1 1 calc R . . C16 C 0.08234(17) 0.38128(7) 0.23840(7) 0.0166(3) Uani 1 1 d . . . H16A H 0.0374 0.4289 0.2252 0.020 Uiso 1 1 calc R . . H16B H 0.1887 0.3790 0.2240 0.020 Uiso 1 1 calc R . . C17 C -0.06215(19) 0.35072(9) 0.12897(8) 0.0245(3) Uani 1 1 d . . . H17A H -0.1300 0.3146 0.1034 0.037 Uiso 1 1 calc R . . H17B H 0.0335 0.3573 0.1074 0.037 Uiso 1 1 calc R . . H17C H -0.1198 0.3960 0.1284 0.037 Uiso 1 1 calc R . . C18 C 0.06283(18) 0.25843(7) 0.20058(7) 0.0177(3) Uani 1 1 d . . . H18A H 0.1692 0.2663 0.1875 0.021 Uiso 1 1 calc R . . H18B H 0.0030 0.2277 0.1649 0.021 Uiso 1 1 calc R . . C19 C 0.14819(17) 0.12497(7) 0.24776(8) 0.0179(3) Uani 1 1 d . . . H19A H 0.1323 0.0855 0.2796 0.022 Uiso 1 1 calc R . . H19B H 0.0804 0.1155 0.2033 0.022 Uiso 1 1 calc R . . C20 C 0.32169(17) 0.12607(8) 0.23621(9) 0.0214(3) Uani 1 1 d . . . H20A H 0.3518 0.0787 0.2212 0.032 Uiso 1 1 calc R . . H20B H 0.3888 0.1388 0.2793 0.032 Uiso 1 1 calc R . . H20C H 0.3356 0.1614 0.2007 0.032 Uiso 1 1 calc R . . C21 C -0.12502(16) 0.19382(8) 0.29120(8) 0.0178(3) Uani 1 1 d . . . H21A H -0.1309 0.1792 0.3393 0.021 Uiso 1 1 calc R . . H21B H -0.1813 0.2400 0.2837 0.021 Uiso 1 1 calc R . . C22 C -0.21633(19) 0.13950(10) 0.24414(10) 0.0323(4) Uani 1 1 d . . . H22A H -0.3288 0.1420 0.2491 0.048 Uiso 1 1 calc R . . H22B H -0.1760 0.0916 0.2566 0.048 Uiso 1 1 calc R . . H22C H -0.2034 0.1497 0.1963 0.048 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 0.00968(5) 0.01347(5) 0.00990(5) -0.00008(4) 0.00161(4) 0.00043(4) N1 0.0182(6) 0.0453(8) 0.0129(6) 0.0077(6) 0.0016(5) 0.0028(6) N2 0.0168(5) 0.0191(5) 0.0109(6) 0.0015(4) -0.0003(4) -0.0005(4) N3 0.0157(5) 0.0176(5) 0.0140(6) 0.0003(4) 0.0004(4) 0.0023(4) N4 0.0216(6) 0.0289(7) 0.0216(7) 0.0030(5) 0.0070(5) 0.0016(5) N5 0.0146(5) 0.0155(5) 0.0115(5) -0.0007(4) -0.0010(4) 0.0008(4) N6 0.0196(6) 0.0270(6) 0.0175(6) 0.0003(5) 0.0042(5) -0.0016(5) P1 0.01422(16) 0.01978(16) 0.01692(19) 0.00658(14) 0.00493(14) 0.00355(13) P2 0.01178(16) 0.02698(18) 0.01151(17) -0.00411(14) 0.00125(13) -0.00034(13) P3 0.01140(15) 0.01213(14) 0.01408(17) -0.00083(12) 0.00205(12) -0.00008(11) P4 0.01232(15) 0.01299(14) 0.01251(16) -0.00208(12) 0.00270(12) -0.00091(12) C1 0.0232(7) 0.0196(6) 0.0297(9) 0.0076(6) 0.0096(6) 0.0044(6) C2 0.0266(8) 0.0217(7) 0.0415(11) 0.0038(7) 0.0128(7) -0.0027(6) C3 0.0158(7) 0.0301(7) 0.0275(9) 0.0119(6) 0.0085(6) 0.0073(6) C4 0.0277(10) 0.0469(12) 0.108(2) 0.0430(13) 0.0315(12) 0.0219(9) C5 0.0220(7) 0.0358(8) 0.0183(8) 0.0114(6) 0.0057(6) 0.0035(6) C6 0.0261(9) 0.0743(14) 0.0167(8) 0.0164(9) 0.0005(7) 0.0048(9) C7 0.0176(7) 0.0455(9) 0.0122(7) -0.0006(6) 0.0038(5) -0.0007(6) C8 0.0130(6) 0.0373(8) 0.0157(7) -0.0033(6) 0.0016(5) -0.0016(6) C9 0.0165(7) 0.0434(9) 0.0251(9) -0.0113(7) 0.0007(6) -0.0043(7) C10 0.0169(7) 0.0354(8) 0.0230(8) -0.0144(7) -0.0003(6) 0.0002(6) C11 0.0219(8) 0.0441(10) 0.0242(9) -0.0092(7) 0.0050(6) 0.0055(7) C12 0.0139(6) 0.0161(6) 0.0202(7) 0.0001(5) 0.0039(5) 0.0012(5) C13 0.0165(7) 0.0253(7) 0.0401(10) 0.0104(7) 0.0043(7) 0.0050(6) C14 0.0170(6) 0.0127(6) 0.0244(8) -0.0027(5) 0.0036(6) -0.0010(5) C15 0.0171(7) 0.0197(6) 0.0285(9) -0.0029(6) 0.0047(6) -0.0044(5) C16 0.0182(6) 0.0163(6) 0.0153(7) 0.0014(5) 0.0026(5) -0.0015(5) C17 0.0253(8) 0.0307(8) 0.0162(8) 0.0054(6) -0.0012(6) 0.0000(6) C18 0.0209(7) 0.0187(6) 0.0136(7) -0.0021(5) 0.0031(5) -0.0009(5) C19 0.0182(7) 0.0153(6) 0.0213(7) -0.0050(5) 0.0062(5) -0.0018(5) C20 0.0187(7) 0.0201(6) 0.0269(8) -0.0054(6) 0.0092(6) -0.0006(5) C21 0.0138(6) 0.0225(6) 0.0171(7) -0.0038(5) 0.0030(5) -0.0023(5) C22 0.0175(7) 0.0452(10) 0.0354(10) -0.0203(8) 0.0079(7) -0.0111(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N5 2.0215(13) . ? Mo1 N3 2.0220(14) . ? Mo1 P3 2.4406(7) . ? Mo1 P1 2.4470(7) . ? Mo1 P2 2.4469(6) . ? Mo1 P4 2.4491(6) . ? N1 C7 1.459(2) . ? N1 C6 1.465(2) . ? N1 C5 1.463(2) . ? N2 C18 1.4584(18) . ? N2 C16 1.4597(18) . ? N2 C17 1.4649(19) . ? N3 N4 1.1166(18) . ? N5 N6 1.1140(17) . ? P1 C5 1.8480(17) . ? P1 C3 1.8486(16) . ? P1 C1 1.8519(17) . ? P2 C8 1.8549(16) . ? P2 C7 1.8524(17) . ? P2 C10 1.8564(16) . ? P3 C14 1.8496(14) . ? P3 C16 1.8529(16) . ? P3 C12 1.8522(15) . ? P4 C21 1.8509(15) . ? P4 C19 1.8531(15) . ? P4 C18 1.8557(16) . ? C1 C2 1.534(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.507(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.514(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.530(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.517(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.533(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.530(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.512(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 N5 Mo1 N3 178.48(5) . . ? N5 Mo1 P3 90.60(4) . . ? N3 Mo1 P3 90.32(4) . . ? N5 Mo1 P1 89.98(4) . . ? N3 Mo1 P1 89.12(4) . . ? P3 Mo1 P1 178.800(13) . . ? N5 Mo1 P2 89.15(4) . . ? N3 Mo1 P2 89.52(4) . . ? P3 Mo1 P2 98.23(2) . . ? P1 Mo1 P2 82.83(2) . . ? N5 Mo1 P4 90.65(4) . . ? N3 Mo1 P4 90.68(4) . . ? P3 Mo1 P4 81.95(2) . . ? P1 Mo1 P4 97.00(2) . . ? P2 Mo1 P4 179.731(14) . . ? C7 N1 C6 108.70(14) . . ? C7 N1 C5 112.00(12) . . ? C6 N1 C5 108.80(14) . . ? C18 N2 C16 111.83(11) . . ? C18 N2 C17 109.05(12) . . ? C16 N2 C17 109.28(11) . . ? N4 N3 Mo1 179.56(12) . . ? N6 N5 Mo1 177.88(11) . . ? C5 P1 C3 100.41(8) . . ? C5 P1 C1 95.74(8) . . ? C3 P1 C1 101.93(7) . . ? C5 P1 Mo1 115.87(5) . . ? C3 P1 Mo1 116.62(5) . . ? C1 P1 Mo1 122.28(6) . . ? C8 P2 C7 102.44(7) . . ? C8 P2 C10 99.54(7) . . ? C7 P2 C10 95.58(8) . . ? C8 P2 Mo1 116.51(5) . . ? C7 P2 Mo1 116.03(6) . . ? C10 P2 Mo1 122.86(5) . . ? C14 P3 C16 95.37(7) . . ? C14 P3 C12 100.32(6) . . ? C16 P3 C12 102.15(7) . . ? C14 P3 Mo1 122.59(5) . . ? C16 P3 Mo1 116.38(5) . . ? C12 P3 Mo1 116.19(5) . . ? C21 P4 C19 102.98(6) . . ? C21 P4 C18 99.61(7) . . ? C19 P4 C18 94.74(7) . . ? C21 P4 Mo1 115.95(5) . . ? C19 P4 Mo1 121.83(5) . . ? C18 P4 Mo1 117.63(5) . . ? C2 C1 P1 112.98(11) . . ? C2 C1 H1A 109.0 . . ? P1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? P1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 119.23(12) . . ? C4 C3 H3A 107.5 . . ? P1 C3 H3A 107.5 . . ? C4 C3 H3B 107.5 . . ? P1 C3 H3B 107.5 . . ? H3A C3 H3B 107.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 P1 114.98(11) . . ? N1 C5 H5A 108.5 . . ? P1 C5 H5A 108.5 . . ? N1 C5 H5B 108.5 . . ? P1 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 P2 115.76(11) . . ? N1 C7 H7A 108.3 . . ? P2 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? P2 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 P2 118.64(12) . . ? C9 C8 H8A 107.7 . . ? P2 C8 H8A 107.7 . . ? C9 C8 H8B 107.7 . . ? P2 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P2 113.98(11) . . ? C11 C10 H10A 108.8 . . ? P2 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? P2 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 P3 118.33(11) . . ? C13 C12 H12A 107.7 . . ? P3 C12 H12A 107.7 . . ? C13 C12 H12B 107.7 . . ? P3 C12 H12B 107.7 . . ? H12A C12 H12B 107.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 P3 112.83(10) . . ? C15 C14 H14A 109.0 . . ? P3 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? P3 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 P3 115.23(10) . . ? N2 C16 H16A 108.5 . . ? P3 C16 H16A 108.5 . . ? N2 C16 H16B 108.5 . . ? P3 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 P4 115.10(10) . . ? N2 C18 H18A 108.5 . . ? P4 C18 H18A 108.5 . . ? N2 C18 H18B 108.5 . . ? P4 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C20 C19 P4 112.48(9) . . ? C20 C19 H19A 109.1 . . ? P4 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? P4 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P4 118.98(11) . . ? C22 C21 H21A 107.6 . . ? P4 C21 H21A 107.6 . . ? C22 C21 H21B 107.6 . . ? P4 C21 H21B 107.6 . . ? H21A C21 H21B 107.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 33.44 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.686 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.084 #===END data_cis-Mo(N2)2(PEtNMePEt)2_(cis-6) _database_code_depnum_ccdc_archive 'CCDC 854201' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H54 Mo N6 P4' _chemical_formula_weight 622.53 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.7747(13) _cell_length_b 10.2104(7) _cell_length_c 15.5500(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.199(2) _cell_angle_gamma 90.00 _cell_volume 3079.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9888 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 33.27 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8801 _exptl_absorpt_correction_T_max 0.9495 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 55672 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 33.33 _reflns_number_total 11885 _reflns_number_gt 9273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0307P)^2^+0.4918P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11885 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.247634(6) 0.471372(12) 0.402026(7) 0.00994(3) Uani 1 1 d . . . N1 N 0.15699(6) 0.38728(13) 0.60353(8) 0.0149(2) Uani 1 1 d . . . N2 N 0.36642(6) 0.80420(12) 0.41441(8) 0.0151(2) Uani 1 1 d . . . N3 N 0.21669(6) 0.48049(13) 0.26991(8) 0.0152(2) Uani 1 1 d . . . N4 N 0.20231(7) 0.47995(16) 0.19643(9) 0.0246(3) Uani 1 1 d . . . N5 N 0.26129(6) 0.27852(13) 0.38405(8) 0.0138(2) Uani 1 1 d . . . N6 N 0.26670(7) 0.17107(14) 0.37204(9) 0.0215(3) Uani 1 1 d . . . P1 P 0.283922(18) 0.43446(4) 0.56096(2) 0.01203(7) Uani 1 1 d . . . P2 P 0.131077(18) 0.41749(4) 0.42489(2) 0.01190(7) Uani 1 1 d . . . P3 P 0.232655(19) 0.70988(4) 0.41323(2) 0.01310(7) Uani 1 1 d . . . P4 P 0.361691(18) 0.53541(4) 0.37717(2) 0.01218(7) Uani 1 1 d . . . C1 C 0.30773(8) 0.26472(15) 0.59642(9) 0.0168(3) Uani 1 1 d . . . H1A H 0.3094 0.2584 0.6603 0.020 Uiso 1 1 calc R . . H1B H 0.2709 0.2050 0.5671 0.020 Uiso 1 1 calc R . . C2 C 0.37654(8) 0.21730(17) 0.57723(10) 0.0222(3) Uani 1 1 d . . . H2A H 0.3837 0.1255 0.5951 0.033 Uiso 1 1 calc R . . H2B H 0.4140 0.2709 0.6100 0.033 Uiso 1 1 calc R . . H2C H 0.3761 0.2251 0.5143 0.033 Uiso 1 1 calc R . . C3 C 0.35631(7) 0.52873(16) 0.62495(9) 0.0162(3) Uani 1 1 d . . . H3A H 0.3974 0.5119 0.5989 0.019 Uiso 1 1 calc R . . H3B H 0.3450 0.6228 0.6161 0.019 Uiso 1 1 calc R . . C4 C 0.37726(8) 0.50542(17) 0.72376(10) 0.0216(3) Uani 1 1 d . . . H4A H 0.4182 0.5578 0.7473 0.032 Uiso 1 1 calc R . . H4B H 0.3876 0.4124 0.7348 0.032 Uiso 1 1 calc R . . H4C H 0.3393 0.5312 0.7525 0.032 Uiso 1 1 calc R . . C5 C 0.22041(7) 0.46165(15) 0.63252(9) 0.0148(3) Uani 1 1 d . . . H5A H 0.2412 0.4357 0.6932 0.018 Uiso 1 1 calc R . . H5B H 0.2092 0.5561 0.6329 0.018 Uiso 1 1 calc R . . C6 C 0.12439(8) 0.35407(18) 0.67754(10) 0.0213(3) Uani 1 1 d . . . H6A H 0.0833 0.3008 0.6568 0.032 Uiso 1 1 calc R . . H6B H 0.1111 0.4347 0.7043 0.032 Uiso 1 1 calc R . . H6C H 0.1569 0.3046 0.7212 0.032 Uiso 1 1 calc R . . C7 C 0.10899(7) 0.45241(15) 0.53325(9) 0.0146(3) Uani 1 1 d . . . H7A H 0.1105 0.5481 0.5436 0.018 Uiso 1 1 calc R . . H7B H 0.0615 0.4218 0.5334 0.018 Uiso 1 1 calc R . . C8 C 0.05321(7) 0.49027(16) 0.35640(9) 0.0163(3) Uani 1 1 d . . . H8A H 0.0128 0.4685 0.3826 0.020 Uiso 1 1 calc R . . H8B H 0.0582 0.5868 0.3575 0.020 Uiso 1 1 calc R . . C9 C 0.03911(8) 0.44410(18) 0.26077(10) 0.0210(3) Uani 1 1 d . . . H9A H -0.0005 0.4918 0.2276 0.032 Uiso 1 1 calc R . . H9B H 0.0291 0.3500 0.2585 0.032 Uiso 1 1 calc R . . H9C H 0.0797 0.4609 0.2350 0.032 Uiso 1 1 calc R . . C10 C 0.10868(7) 0.24209(15) 0.41813(10) 0.0161(3) Uani 1 1 d . . . H10A H 0.1142 0.2104 0.3597 0.019 Uiso 1 1 calc R . . H10B H 0.1432 0.1955 0.4622 0.019 Uiso 1 1 calc R . . C11 C 0.03712(8) 0.19975(17) 0.43148(12) 0.0243(3) Uani 1 1 d . . . H11A H 0.0317 0.1052 0.4218 0.036 Uiso 1 1 calc R . . H11B H 0.0017 0.2463 0.3897 0.036 Uiso 1 1 calc R . . H11C H 0.0321 0.2207 0.4914 0.036 Uiso 1 1 calc R . . C12 C 0.20585(7) 0.79914(16) 0.30856(9) 0.0170(3) Uani 1 1 d . . . H12A H 0.2103 0.8943 0.3204 0.020 Uiso 1 1 calc R . . H12B H 0.2379 0.7763 0.2692 0.020 Uiso 1 1 calc R . . C13 C 0.13239(8) 0.77066(17) 0.26104(10) 0.0216(3) Uani 1 1 d . . . H13A H 0.1231 0.8179 0.2051 0.032 Uiso 1 1 calc R . . H13B H 0.0999 0.7994 0.2974 0.032 Uiso 1 1 calc R . . H13C H 0.1270 0.6764 0.2501 0.032 Uiso 1 1 calc R . . C14 C 0.17272(8) 0.77635(16) 0.48032(10) 0.0188(3) Uani 1 1 d . . . H14A H 0.1280 0.7310 0.4621 0.023 Uiso 1 1 calc R . . H14B H 0.1908 0.7515 0.5420 0.023 Uiso 1 1 calc R . . C15 C 0.15830(9) 0.92316(17) 0.47855(11) 0.0256(3) Uani 1 1 d . . . H15A H 0.1233 0.9421 0.5136 0.038 Uiso 1 1 calc R . . H15B H 0.1415 0.9514 0.4179 0.038 Uiso 1 1 calc R . . H15C H 0.2008 0.9704 0.5030 0.038 Uiso 1 1 calc R . . C16 C 0.30810(7) 0.81359(15) 0.45944(9) 0.0159(3) Uani 1 1 d . . . H16A H 0.2928 0.9060 0.4580 0.019 Uiso 1 1 calc R . . H16B H 0.3242 0.7892 0.5217 0.019 Uiso 1 1 calc R . . C17 C 0.41307(8) 0.91461(16) 0.44112(10) 0.0199(3) Uani 1 1 d . . . H17A H 0.3881 0.9970 0.4264 0.030 Uiso 1 1 calc R . . H17B H 0.4518 0.9100 0.4103 0.030 Uiso 1 1 calc R . . H17C H 0.4306 0.9107 0.5045 0.030 Uiso 1 1 calc R . . C18 C 0.40507(7) 0.68195(15) 0.43309(9) 0.0153(3) Uani 1 1 d . . . H18A H 0.4139 0.6665 0.4972 0.018 Uiso 1 1 calc R . . H18B H 0.4503 0.6924 0.4156 0.018 Uiso 1 1 calc R . . C19 C 0.43702(7) 0.42553(16) 0.40530(10) 0.0170(3) Uani 1 1 d . . . H19A H 0.4788 0.4735 0.3970 0.020 Uiso 1 1 calc R . . H19B H 0.4432 0.4015 0.4680 0.020 Uiso 1 1 calc R . . C20 C 0.43054(8) 0.30062(16) 0.35060(11) 0.0208(3) Uani 1 1 d . . . H20A H 0.4695 0.2426 0.3729 0.031 Uiso 1 1 calc R . . H20B H 0.4307 0.3228 0.2893 0.031 Uiso 1 1 calc R . . H20C H 0.3873 0.2562 0.3544 0.031 Uiso 1 1 calc R . . C21 C 0.36371(8) 0.57635(17) 0.26142(9) 0.0180(3) Uani 1 1 d . . . H21A H 0.3467 0.4990 0.2252 0.022 Uiso 1 1 calc R . . H21B H 0.3302 0.6480 0.2433 0.022 Uiso 1 1 calc R . . C22 C 0.43220(8) 0.61761(19) 0.23808(11) 0.0260(4) Uani 1 1 d . . . H22A H 0.4254 0.6354 0.1751 0.039 Uiso 1 1 calc R . . H22B H 0.4660 0.5470 0.2534 0.039 Uiso 1 1 calc R . . H22C H 0.4491 0.6968 0.2709 0.039 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 0.01039(5) 0.01129(6) 0.00821(5) 0.00005(4) 0.00199(4) 0.00120(4) N1 0.0152(5) 0.0188(7) 0.0114(5) 0.0026(4) 0.0043(4) 0.0017(5) N2 0.0176(6) 0.0127(6) 0.0148(5) 0.0003(4) 0.0020(4) -0.0025(5) N3 0.0123(5) 0.0194(7) 0.0143(5) 0.0004(5) 0.0032(4) 0.0003(5) N4 0.0209(6) 0.0388(9) 0.0137(6) 0.0008(6) 0.0024(5) -0.0015(6) N5 0.0118(5) 0.0174(6) 0.0120(5) -0.0006(4) 0.0016(4) 0.0007(5) N6 0.0204(6) 0.0194(7) 0.0247(7) -0.0038(5) 0.0042(5) 0.0009(5) P1 0.01314(16) 0.01363(18) 0.00932(15) 0.00072(12) 0.00217(12) 0.00184(13) P2 0.01150(15) 0.01358(18) 0.01086(15) 0.00034(13) 0.00276(12) 0.00145(13) P3 0.01474(16) 0.01219(18) 0.01225(15) 0.00152(13) 0.00229(12) 0.00205(13) P4 0.01138(15) 0.01428(18) 0.01096(15) -0.00063(13) 0.00234(12) 0.00016(13) C1 0.0212(7) 0.0148(7) 0.0140(6) 0.0027(5) 0.0029(5) 0.0031(6) C2 0.0259(8) 0.0216(8) 0.0190(7) 0.0023(6) 0.0041(6) 0.0085(7) C3 0.0164(6) 0.0180(7) 0.0132(6) 0.0005(5) 0.0003(5) -0.0012(6) C4 0.0229(7) 0.0271(9) 0.0131(6) -0.0007(6) -0.0006(6) 0.0001(6) C5 0.0160(6) 0.0182(7) 0.0105(6) 0.0000(5) 0.0031(5) 0.0022(6) C6 0.0210(7) 0.0279(9) 0.0168(7) 0.0070(6) 0.0076(6) 0.0002(6) C7 0.0155(6) 0.0169(7) 0.0122(6) 0.0007(5) 0.0043(5) 0.0021(5) C8 0.0136(6) 0.0197(8) 0.0159(6) 0.0028(5) 0.0032(5) 0.0034(5) C9 0.0154(7) 0.0308(10) 0.0157(7) 0.0004(6) 0.0003(5) 0.0005(6) C10 0.0148(6) 0.0161(7) 0.0176(6) -0.0011(5) 0.0036(5) -0.0002(5) C11 0.0191(7) 0.0202(8) 0.0349(9) -0.0009(7) 0.0083(7) -0.0035(6) C12 0.0176(7) 0.0167(7) 0.0159(6) 0.0047(5) 0.0016(5) 0.0019(6) C13 0.0193(7) 0.0212(8) 0.0222(7) 0.0071(6) -0.0010(6) 0.0018(6) C14 0.0227(7) 0.0163(8) 0.0186(7) 0.0018(6) 0.0072(6) 0.0045(6) C15 0.0328(9) 0.0179(8) 0.0279(8) -0.0012(7) 0.0105(7) 0.0064(7) C16 0.0185(7) 0.0130(7) 0.0155(6) 0.0000(5) 0.0013(5) 0.0015(5) C17 0.0232(7) 0.0172(8) 0.0184(7) 0.0002(6) 0.0013(6) -0.0059(6) C18 0.0147(6) 0.0160(7) 0.0149(6) 0.0004(5) 0.0021(5) -0.0010(5) C19 0.0129(6) 0.0189(8) 0.0185(7) -0.0021(6) 0.0017(5) 0.0013(6) C20 0.0186(7) 0.0192(8) 0.0254(8) -0.0056(6) 0.0064(6) 0.0027(6) C21 0.0164(7) 0.0253(8) 0.0127(6) 0.0001(6) 0.0043(5) -0.0015(6) C22 0.0213(8) 0.0378(11) 0.0211(8) 0.0029(7) 0.0097(6) -0.0044(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N5 2.0143(13) . ? Mo1 N3 2.0287(12) . ? Mo1 P4 2.4500(4) . ? Mo1 P2 2.4617(4) . ? Mo1 P3 2.4635(4) . ? Mo1 P1 2.4650(4) . ? N1 C7 1.4611(18) . ? N1 C5 1.4605(19) . ? N1 C6 1.4640(18) . ? N2 C16 1.4641(18) . ? N2 C17 1.4648(19) . ? N2 C18 1.4630(19) . ? N3 N4 1.1226(17) . ? N5 N6 1.1216(18) . ? P1 C3 1.8473(15) . ? P1 C1 1.8516(15) . ? P1 C5 1.8535(14) . ? P2 C10 1.8430(16) . ? P2 C8 1.8494(15) . ? P2 C7 1.8554(14) . ? P3 C12 1.8508(15) . ? P3 C14 1.8532(15) . ? P3 C16 1.8566(15) . ? P4 C19 1.8483(15) . ? P4 C18 1.8549(15) . ? P4 C21 1.8558(14) . ? C1 C2 1.527(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.530(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.533(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.532(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.525(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.525(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.525(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.528(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 N5 Mo1 N3 85.79(5) . . ? N5 Mo1 P4 94.97(3) . . ? N3 Mo1 P4 86.21(3) . . ? N5 Mo1 P2 87.48(3) . . ? N3 Mo1 P2 92.86(3) . . ? P4 Mo1 P2 177.296(14) . . ? N5 Mo1 P3 175.82(3) . . ? N3 Mo1 P3 90.54(4) . . ? P4 Mo1 P3 82.780(13) . . ? P2 Mo1 P3 94.698(13) . . ? N5 Mo1 P1 88.22(3) . . ? N3 Mo1 P1 173.82(4) . . ? P4 Mo1 P1 95.815(13) . . ? P2 Mo1 P1 85.378(12) . . ? P3 Mo1 P1 95.501(13) . . ? C7 N1 C5 112.85(12) . . ? C7 N1 C6 111.86(11) . . ? C5 N1 C6 111.14(12) . . ? C16 N2 C17 108.98(12) . . ? C16 N2 C18 112.99(11) . . ? C17 N2 C18 108.93(12) . . ? N4 N3 Mo1 175.93(13) . . ? N6 N5 Mo1 177.54(12) . . ? C3 P1 C1 101.64(7) . . ? C3 P1 C5 98.22(7) . . ? C1 P1 C5 97.13(7) . . ? C3 P1 Mo1 120.31(5) . . ? C1 P1 Mo1 116.71(5) . . ? C5 P1 Mo1 118.67(5) . . ? C10 P2 C8 101.17(7) . . ? C10 P2 C7 98.18(7) . . ? C8 P2 C7 97.43(6) . . ? C10 P2 Mo1 115.49(5) . . ? C8 P2 Mo1 121.68(5) . . ? C7 P2 Mo1 118.71(5) . . ? C12 P3 C14 102.09(7) . . ? C12 P3 C16 97.52(7) . . ? C14 P3 C16 97.29(7) . . ? C12 P3 Mo1 116.26(5) . . ? C14 P3 Mo1 120.05(5) . . ? C16 P3 Mo1 119.51(5) . . ? C19 P4 C18 95.77(7) . . ? C19 P4 C21 101.42(7) . . ? C18 P4 C21 100.24(7) . . ? C19 P4 Mo1 121.67(5) . . ? C18 P4 Mo1 119.83(5) . . ? C21 P4 Mo1 114.02(5) . . ? C2 C1 P1 115.03(11) . . ? C2 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 119.36(11) . . ? C4 C3 H3A 107.5 . . ? P1 C3 H3A 107.5 . . ? C4 C3 H3B 107.5 . . ? P1 C3 H3B 107.5 . . ? H3A C3 H3B 107.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 P1 112.22(9) . . ? N1 C5 H5A 109.2 . . ? P1 C5 H5A 109.2 . . ? N1 C5 H5B 109.2 . . ? P1 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 P2 111.01(9) . . ? N1 C7 H7A 109.4 . . ? P2 C7 H7A 109.4 . . ? N1 C7 H7B 109.4 . . ? P2 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 P2 114.16(10) . . ? C9 C8 H8A 108.7 . . ? P2 C8 H8A 108.7 . . ? C9 C8 H8B 108.7 . . ? P2 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P2 118.98(11) . . ? C11 C10 H10A 107.6 . . ? P2 C10 H10A 107.6 . . ? C11 C10 H10B 107.6 . . ? P2 C10 H10B 107.6 . . ? H10A C10 H10B 107.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 P3 114.55(10) . . ? C13 C12 H12A 108.6 . . ? P3 C12 H12A 108.6 . . ? C13 C12 H12B 108.6 . . ? P3 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 P3 119.18(11) . . ? C15 C14 H14A 107.5 . . ? P3 C14 H14A 107.5 . . ? C15 C14 H14B 107.5 . . ? P3 C14 H14B 107.5 . . ? H14A C14 H14B 107.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 P3 115.21(10) . . ? N2 C16 H16A 108.5 . . ? P3 C16 H16A 108.5 . . ? N2 C16 H16B 108.5 . . ? P3 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 P4 114.77(10) . . ? N2 C18 H18A 108.6 . . ? P4 C18 H18A 108.6 . . ? N2 C18 H18B 108.6 . . ? P4 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C20 C19 P4 113.53(10) . . ? C20 C19 H19A 108.9 . . ? P4 C19 H19A 108.9 . . ? C20 C19 H19B 108.9 . . ? P4 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P4 118.66(11) . . ? C22 C21 H21A 107.6 . . ? P4 C21 H21A 107.6 . . ? C22 C21 H21B 107.6 . . ? P4 C21 H21B 107.6 . . ? H21A C21 H21B 107.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 33.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.910 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.092 #===END data_trans-Mo(N2)2(PPhNBnPPh)2_(8) _database_code_depnum_ccdc_archive 'CCDC 854202' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H31 Mo0.50 N3 P2' _chemical_formula_weight 579.52 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.123(4) _cell_length_b 16.082(3) _cell_length_c 15.539(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.277(8) _cell_angle_gamma 90.00 _cell_volume 5646.4(17) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6161 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 28.09 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.394 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9254 _exptl_absorpt_correction_T_max 0.9844 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 51596 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 33.26 _reflns_number_total 10782 _reflns_number_gt 7228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0388P)^2^+1.5250P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10782 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.2500 0.2500 0.5000 0.00954(5) Uani 1 2 d S . . N1 N 0.40268(7) 0.11898(10) 0.53647(10) 0.0129(3) Uani 1 1 d . . . N2 N 0.25660(7) 0.18989(10) 0.61629(11) 0.0143(3) Uani 1 1 d . . . N3 N 0.26272(8) 0.15585(11) 0.68015(11) 0.0196(4) Uani 1 1 d . . . P1 P 0.28380(2) 0.11965(3) 0.44478(3) 0.01146(10) Uani 1 1 d . . . P2 P 0.14318(2) 0.22230(3) 0.44342(3) 0.01103(9) Uani 1 1 d . . . C1 C 0.21123(8) 0.00390(12) 0.50402(13) 0.0171(4) Uani 1 1 d . . . H1A H 0.2132 0.0418 0.5515 0.020 Uiso 1 1 calc R . . C2 C 0.18053(9) -0.07036(14) 0.50347(14) 0.0229(4) Uani 1 1 d . . . H2A H 0.1617 -0.0831 0.5505 0.027 Uiso 1 1 calc R . . C3 C 0.17731(9) -0.12598(13) 0.43465(15) 0.0244(5) Uani 1 1 d . . . H3A H 0.1562 -0.1767 0.4345 0.029 Uiso 1 1 calc R . . C4 C 0.20479(9) -0.10770(13) 0.36595(15) 0.0223(4) Uani 1 1 d . . . H4A H 0.2026 -0.1459 0.3187 0.027 Uiso 1 1 calc R . . C5 C 0.23559(8) -0.03344(12) 0.36616(13) 0.0170(4) Uani 1 1 d . . . H5A H 0.2543 -0.0211 0.3189 0.020 Uiso 1 1 calc R . . C6 C 0.23922(8) 0.02339(12) 0.43531(13) 0.0143(4) Uani 1 1 d . . . C7 C 0.36093(9) 0.09869(13) 0.32458(14) 0.0190(4) Uani 1 1 d . . . H7A H 0.3902 0.0791 0.3728 0.023 Uiso 1 1 calc R . . C8 C 0.37370(10) 0.10387(14) 0.24096(14) 0.0256(5) Uani 1 1 d . . . H8A H 0.4117 0.0878 0.2326 0.031 Uiso 1 1 calc R . . C9 C 0.33155(11) 0.13213(14) 0.17018(14) 0.0261(5) Uani 1 1 d . . . H9A H 0.3403 0.1344 0.1132 0.031 Uiso 1 1 calc R . . C10 C 0.27655(10) 0.15717(14) 0.18246(14) 0.0237(5) Uani 1 1 d . . . H10A H 0.2478 0.1778 0.1342 0.028 Uiso 1 1 calc R . . C11 C 0.26371(9) 0.15188(13) 0.26564(13) 0.0189(4) Uani 1 1 d . . . H11A H 0.2259 0.1688 0.2737 0.023 Uiso 1 1 calc R . . C12 C 0.30545(8) 0.12218(12) 0.33760(12) 0.0135(4) Uani 1 1 d . . . C13 C 0.34850(8) 0.06908(12) 0.51709(12) 0.0143(4) Uani 1 1 d . . . H13A H 0.3376 0.0544 0.5735 0.017 Uiso 1 1 calc R . . H13B H 0.3570 0.0166 0.4889 0.017 Uiso 1 1 calc R . . C14 C 0.45363(8) 0.06470(12) 0.56966(13) 0.0161(4) Uani 1 1 d . . . H14A H 0.4497 0.0135 0.5335 0.019 Uiso 1 1 calc R . . H14B H 0.4532 0.0483 0.6309 0.019 Uiso 1 1 calc R . . C15 C 0.56128(9) 0.09087(14) 0.63608(14) 0.0214(4) Uani 1 1 d . . . H15A H 0.5567 0.0603 0.6865 0.026 Uiso 1 1 calc R . . C16 C 0.61683(9) 0.12101(14) 0.63064(16) 0.0273(5) Uani 1 1 d . . . H16A H 0.6501 0.1105 0.6770 0.033 Uiso 1 1 calc R . . C17 C 0.62357(10) 0.16624(14) 0.55770(16) 0.0280(5) Uani 1 1 d . . . H17A H 0.6615 0.1861 0.5533 0.034 Uiso 1 1 calc R . . C18 C 0.57472(10) 0.18252(14) 0.49099(16) 0.0259(5) Uani 1 1 d . . . H18A H 0.5792 0.2148 0.4416 0.031 Uiso 1 1 calc R . . C19 C 0.51941(9) 0.15218(13) 0.49572(14) 0.0194(4) Uani 1 1 d . . . H19A H 0.4862 0.1635 0.4495 0.023 Uiso 1 1 calc R . . C20 C 0.51225(8) 0.10516(12) 0.56803(13) 0.0167(4) Uani 1 1 d . . . C21 C 0.09959(8) 0.31602(12) 0.39864(12) 0.0138(4) Uani 1 1 d . . . H21A H 0.1169 0.3398 0.3510 0.017 Uiso 1 1 calc R . . H21B H 0.0586 0.2985 0.3721 0.017 Uiso 1 1 calc R . . C22 C 0.10428(8) 0.07398(12) 0.34770(13) 0.0157(4) Uani 1 1 d . . . H22A H 0.1063 0.0485 0.4034 0.019 Uiso 1 1 calc R . . C23 C 0.08729(9) 0.02715(13) 0.27125(13) 0.0188(4) Uani 1 1 d . . . H23A H 0.0780 -0.0300 0.2755 0.023 Uiso 1 1 calc R . . C24 C 0.08368(9) 0.06235(13) 0.18915(13) 0.0197(4) Uani 1 1 d . . . H24A H 0.0720 0.0298 0.1373 0.024 Uiso 1 1 calc R . . C25 C 0.09739(9) 0.14573(13) 0.18352(13) 0.0192(4) Uani 1 1 d . . . H25A H 0.0947 0.1708 0.1275 0.023 Uiso 1 1 calc R . . C26 C 0.11504(8) 0.19304(12) 0.25972(12) 0.0154(4) Uani 1 1 d . . . H26A H 0.1249 0.2500 0.2550 0.018 Uiso 1 1 calc R . . C27 C 0.11847(8) 0.15806(12) 0.34329(12) 0.0126(3) Uani 1 1 d . . . C28 C 0.03856(8) 0.15177(12) 0.48264(13) 0.0168(4) Uani 1 1 d . . . H28A H 0.0253 0.1440 0.4210 0.020 Uiso 1 1 calc R . . C29 C 0.00175(9) 0.12995(13) 0.53910(13) 0.0196(4) Uani 1 1 d . . . H29A H -0.0359 0.1059 0.5161 0.024 Uiso 1 1 calc R . . C30 C 0.02008(9) 0.14344(13) 0.62924(13) 0.0205(4) Uani 1 1 d . . . H30A H -0.0053 0.1295 0.6678 0.025 Uiso 1 1 calc R . . C31 C 0.07527(9) 0.17720(13) 0.66270(13) 0.0180(4) Uani 1 1 d . . . H31A H 0.0877 0.1870 0.7242 0.022 Uiso 1 1 calc R . . C32 C 0.11264(8) 0.19689(12) 0.60637(12) 0.0152(4) Uani 1 1 d . . . H32A H 0.1509 0.2188 0.6299 0.018 Uiso 1 1 calc R . . C33 C 0.09462(8) 0.18483(11) 0.51549(12) 0.0129(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.00895(9) 0.01045(10) 0.00947(10) -0.00044(9) 0.00254(7) -0.00017(9) N1 0.0104(7) 0.0128(8) 0.0154(8) -0.0019(6) 0.0021(6) 0.0010(6) N2 0.0106(7) 0.0138(8) 0.0188(8) -0.0052(6) 0.0039(6) -0.0012(6) N3 0.0184(8) 0.0230(9) 0.0168(8) 0.0017(7) 0.0025(7) 0.0004(7) P1 0.0106(2) 0.0120(2) 0.0122(2) -0.00074(18) 0.00337(17) -0.00030(17) P2 0.0099(2) 0.0118(2) 0.0114(2) -0.00015(17) 0.00239(17) -0.00004(17) C1 0.0158(9) 0.0171(10) 0.0189(10) 0.0007(8) 0.0051(8) -0.0008(7) C2 0.0188(10) 0.0240(11) 0.0262(11) 0.0074(9) 0.0058(9) -0.0033(8) C3 0.0218(10) 0.0163(10) 0.0342(13) 0.0038(9) 0.0042(9) -0.0063(8) C4 0.0214(10) 0.0158(10) 0.0283(12) -0.0041(8) 0.0022(9) -0.0022(8) C5 0.0152(9) 0.0135(9) 0.0231(10) -0.0029(8) 0.0056(8) -0.0018(7) C6 0.0102(8) 0.0128(9) 0.0197(10) -0.0002(7) 0.0022(7) 0.0006(7) C7 0.0182(9) 0.0202(10) 0.0195(10) -0.0014(8) 0.0064(8) 0.0018(8) C8 0.0246(11) 0.0319(12) 0.0251(11) -0.0041(9) 0.0157(9) -0.0001(9) C9 0.0375(13) 0.0276(12) 0.0169(10) -0.0029(9) 0.0142(10) -0.0049(10) C10 0.0296(11) 0.0270(12) 0.0136(10) -0.0009(8) 0.0026(8) -0.0024(9) C11 0.0189(9) 0.0211(10) 0.0168(10) -0.0034(8) 0.0041(8) -0.0022(8) C12 0.0145(8) 0.0125(9) 0.0144(9) -0.0030(7) 0.0054(7) -0.0017(7) C13 0.0132(8) 0.0126(9) 0.0167(9) -0.0012(7) 0.0023(7) 0.0007(7) C14 0.0139(8) 0.0152(9) 0.0190(10) 0.0006(8) 0.0029(7) 0.0038(7) C15 0.0182(9) 0.0260(11) 0.0193(10) -0.0056(9) 0.0023(8) 0.0061(8) C16 0.0147(9) 0.0308(12) 0.0327(13) -0.0130(10) -0.0032(9) 0.0070(9) C17 0.0155(10) 0.0246(12) 0.0454(14) -0.0125(11) 0.0103(10) 0.0000(9) C18 0.0208(10) 0.0205(11) 0.0397(13) -0.0022(10) 0.0141(10) 0.0012(9) C19 0.0151(9) 0.0194(10) 0.0235(11) -0.0020(8) 0.0039(8) 0.0029(8) C20 0.0138(8) 0.0154(9) 0.0211(10) -0.0061(8) 0.0044(7) 0.0048(7) C21 0.0136(8) 0.0133(9) 0.0141(9) -0.0014(7) 0.0022(7) 0.0011(7) C22 0.0159(9) 0.0156(9) 0.0149(9) 0.0009(7) 0.0013(7) 0.0000(7) C23 0.0191(9) 0.0143(9) 0.0219(10) -0.0036(8) 0.0016(8) -0.0028(8) C24 0.0192(9) 0.0222(11) 0.0162(10) -0.0062(8) 0.0007(8) -0.0011(8) C25 0.0191(9) 0.0237(11) 0.0145(9) -0.0006(8) 0.0028(8) 0.0002(8) C26 0.0146(8) 0.0151(9) 0.0166(9) -0.0019(7) 0.0039(7) -0.0024(7) C27 0.0085(7) 0.0148(9) 0.0138(9) -0.0009(7) 0.0008(6) 0.0000(7) C28 0.0143(9) 0.0199(10) 0.0157(9) 0.0005(8) 0.0022(7) -0.0010(8) C29 0.0125(8) 0.0238(11) 0.0224(10) 0.0025(8) 0.0035(8) -0.0024(8) C30 0.0165(9) 0.0258(11) 0.0209(10) 0.0064(9) 0.0080(8) 0.0002(8) C31 0.0188(9) 0.0217(10) 0.0143(9) 0.0033(8) 0.0050(8) -0.0006(8) C32 0.0139(8) 0.0145(9) 0.0169(9) 0.0003(7) 0.0027(7) -0.0004(7) C33 0.0128(8) 0.0112(9) 0.0156(9) 0.0011(7) 0.0050(7) 0.0013(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 2.0263(17) . ? Mo1 N2 2.0263(17) 7_556 ? Mo1 P1 2.4549(6) 7_556 ? Mo1 P1 2.4549(6) . ? Mo1 P2 2.4798(6) . ? Mo1 P2 2.4798(6) 7_556 ? N1 C21 1.461(2) 7_556 ? N1 C13 1.464(2) . ? N1 C14 1.469(2) . ? N2 N3 1.116(2) . ? P1 C12 1.8387(19) . ? P1 C6 1.8483(19) . ? P1 C13 1.8566(19) . ? P2 C33 1.8473(18) . ? P2 C27 1.8538(19) . ? P2 C21 1.8637(19) . ? C1 C2 1.388(3) . ? C1 C6 1.397(3) . ? C1 H1A 0.9500 . ? C2 C3 1.384(3) . ? C2 H2A 0.9500 . ? C3 C4 1.385(3) . ? C3 H3A 0.9500 . ? C4 C5 1.390(3) . ? C4 H4A 0.9500 . ? C5 C6 1.399(3) . ? C5 H5A 0.9500 . ? C7 C12 1.393(3) . ? C7 C8 1.395(3) . ? C7 H7A 0.9500 . ? C8 C9 1.382(3) . ? C8 H8A 0.9500 . ? C9 C10 1.385(3) . ? C9 H9A 0.9500 . ? C10 C11 1.389(3) . ? C10 H10A 0.9500 . ? C11 C12 1.397(3) . ? C11 H11A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C20 1.508(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.392(3) . ? C15 C20 1.395(3) . ? C15 H15A 0.9500 . ? C16 C17 1.383(3) . ? C16 H16A 0.9500 . ? C17 C18 1.386(3) . ? C17 H17A 0.9500 . ? C18 C19 1.385(3) . ? C18 H18A 0.9500 . ? C19 C20 1.393(3) . ? C19 H19A 0.9500 . ? C21 N1 1.461(2) 7_556 ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.391(3) . ? C22 C27 1.397(3) . ? C22 H22A 0.9500 . ? C23 C24 1.382(3) . ? C23 H23A 0.9500 . ? C24 C25 1.385(3) . ? C24 H24A 0.9500 . ? C25 C26 1.394(3) . ? C25 H25A 0.9500 . ? C26 C27 1.402(3) . ? C26 H26A 0.9500 . ? C28 C29 1.391(3) . ? C28 C33 1.394(3) . ? C28 H28A 0.9500 . ? C29 C30 1.392(3) . ? C29 H29A 0.9500 . ? C30 C31 1.382(3) . ? C30 H30A 0.9500 . ? C31 C32 1.391(3) . ? C31 H31A 0.9500 . ? C32 C33 1.398(3) . ? C32 H32A 0.9500 . ? 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 N2 180.0 . 7_556 ? N2 Mo1 P1 93.72(5) . 7_556 ? N2 Mo1 P1 86.28(5) 7_556 7_556 ? N2 Mo1 P1 86.28(5) . . ? N2 Mo1 P1 93.72(5) 7_556 . ? P1 Mo1 P1 180.0 7_556 . ? N2 Mo1 P2 96.37(5) . . ? N2 Mo1 P2 83.63(5) 7_556 . ? P1 Mo1 P2 84.847(17) 7_556 . ? P1 Mo1 P2 95.153(17) . . ? N2 Mo1 P2 83.63(5) . 7_556 ? N2 Mo1 P2 96.37(5) 7_556 7_556 ? P1 Mo1 P2 95.152(17) 7_556 7_556 ? P1 Mo1 P2 84.848(17) . 7_556 ? P2 Mo1 P2 180.0 . 7_556 ? C21 N1 C13 112.30(14) 7_556 . ? C21 N1 C14 109.06(15) 7_556 . ? C13 N1 C14 109.51(15) . . ? N3 N2 Mo1 176.91(15) . . ? C12 P1 C6 101.60(9) . . ? C12 P1 C13 102.61(9) . . ? C6 P1 C13 92.59(8) . . ? C12 P1 Mo1 117.77(6) . . ? C6 P1 Mo1 121.97(6) . . ? C13 P1 Mo1 115.98(6) . . ? C33 P2 C27 102.04(8) . . ? C33 P2 C21 98.05(8) . . ? C27 P2 C21 95.26(8) . . ? C33 P2 Mo1 122.12(6) . . ? C27 P2 Mo1 120.24(6) . . ? C21 P2 Mo1 113.95(6) . . ? C2 C1 C6 120.51(19) . . ? C2 C1 H1A 119.7 . . ? C6 C1 H1A 119.7 . . ? C3 C2 C1 120.28(19) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 120.02(19) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 119.9(2) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.66(19) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 118.59(18) . . ? C1 C6 P1 117.92(14) . . ? C5 C6 P1 123.34(14) . . ? C12 C7 C8 120.20(19) . . ? C12 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 120.5(2) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 119.91(19) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 C11 119.6(2) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C10 C11 C12 121.19(19) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C7 C12 C11 118.52(18) . . ? C7 C12 P1 124.21(15) . . ? C11 C12 P1 117.25(14) . . ? N1 C13 P1 115.37(13) . . ? N1 C13 H13A 108.4 . . ? P1 C13 H13A 108.4 . . ? N1 C13 H13B 108.4 . . ? P1 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? N1 C14 C20 113.23(16) . . ? N1 C14 H14A 108.9 . . ? C20 C14 H14A 108.9 . . ? N1 C14 H14B 108.9 . . ? C20 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C20 120.6(2) . . ? C16 C15 H15A 119.7 . . ? C20 C15 H15A 119.7 . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 119.8(2) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C19 C18 C17 120.6(2) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 120.2(2) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C15 118.94(19) . . ? C19 C20 C14 120.59(18) . . ? C15 C20 C14 120.30(19) . . ? N1 C21 P2 114.64(13) 7_556 . ? N1 C21 H21A 108.6 7_556 . ? P2 C21 H21A 108.6 . . ? N1 C21 H21B 108.6 7_556 . ? P2 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C27 120.60(18) . . ? C23 C22 H22A 119.7 . . ? C27 C22 H22A 119.7 . . ? C24 C23 C22 121.16(19) . . ? C24 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? C23 C24 C25 119.03(19) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? C24 C25 C26 120.30(19) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C27 121.11(18) . . ? C25 C26 H26A 119.4 . . ? C27 C26 H26A 119.4 . . ? C22 C27 C26 117.80(17) . . ? C22 C27 P2 122.14(14) . . ? C26 C27 P2 120.03(14) . . ? C29 C28 C33 120.76(18) . . ? C29 C28 H28A 119.6 . . ? C33 C28 H28A 119.6 . . ? C28 C29 C30 119.94(19) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 119.94(18) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.00(19) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C33 120.83(18) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? C28 C33 C32 118.49(17) . . ? C28 C33 P2 122.70(14) . . ? C32 C33 P2 118.56(14) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 33.26 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.535 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.105 #===END data_trans-W(N2)2(PMePh2)4_preSQUEEZE _database_code_depnum_ccdc_archive 'CCDC 863033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H64 N4 O1.50 P4 W' _chemical_formula_weight 1148.86 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' W W -0.8490 6.8722 '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' _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 11.5609(4) _cell_length_b 14.1387(5) _cell_length_c 17.2056(6) _cell_angle_alpha 77.0490(10) _cell_angle_beta 72.3200(10) _cell_angle_gamma 83.3430(10) _cell_volume 2607.89(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9781 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 33.22 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 2.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6222 _exptl_absorpt_correction_T_max 0.7017 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56743 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 33.38 _reflns_number_total 19916 _reflns_number_gt 18095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. This is the solution before SQUEEZE was used on the data removing the density of 1.5 molecules of THF solvent. ; _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^)+(0.1000P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19916 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.2204 _refine_ls_wR_factor_gt 0.2133 _refine_ls_goodness_of_fit_ref 1.835 _refine_ls_restrained_S_all 1.835 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.758188(14) 0.760586(11) 0.743483(9) 0.00911(7) Uani 1 1 d . . . N1 N 0.6200(4) 0.6719(3) 0.7897(3) 0.0139(7) Uani 1 1 d . . . N2 N 0.5432(4) 0.6218(3) 0.8144(3) 0.0185(8) Uani 1 1 d . . . N3 N 0.8944(4) 0.8507(3) 0.6975(3) 0.0137(7) Uani 1 1 d . . . N4 N 0.9719(4) 0.9026(4) 0.6707(3) 0.0205(9) Uani 1 1 d . . . P1 P 0.85244(11) 0.63862(9) 0.65651(7) 0.0112(2) Uani 1 1 d . . . P2 P 0.86993(11) 0.68372(9) 0.84499(7) 0.0109(2) Uani 1 1 d . . . P3 P 0.63007(11) 0.85965(9) 0.84250(7) 0.0108(2) Uani 1 1 d . . . P4 P 0.68028(11) 0.85907(9) 0.62975(7) 0.0108(2) Uani 1 1 d . . . C1 C 1.0266(5) 0.4844(4) 0.6879(3) 0.0164(9) Uani 1 1 d . . . H1A H 1.0867 0.5227 0.6461 0.020 Uiso 1 1 calc R . . C2 C 1.0605(5) 0.3926(4) 0.7298(3) 0.0198(9) Uani 1 1 d . . . H2A H 1.1436 0.3705 0.7179 0.024 Uiso 1 1 calc R . . C3 C 0.9725(5) 0.3346(4) 0.7883(3) 0.0196(9) Uani 1 1 d . . . H3A H 0.9947 0.2723 0.8159 0.024 Uiso 1 1 calc R . . C4 C 0.8513(5) 0.3685(4) 0.8063(3) 0.0187(9) Uani 1 1 d . . . H4A H 0.7903 0.3284 0.8452 0.022 Uiso 1 1 calc R . . C5 C 0.8190(5) 0.4610(3) 0.7675(3) 0.0153(8) Uani 1 1 d . . . H5A H 0.7365 0.4846 0.7823 0.018 Uiso 1 1 calc R . . C6 C 0.9060(4) 0.5191(3) 0.7073(3) 0.0130(7) Uani 1 1 d . . . C7 C 1.0746(5) 0.7184(4) 0.5674(3) 0.0180(9) Uani 1 1 d . . . H7A H 1.0693 0.7366 0.6183 0.022 Uiso 1 1 calc R . . C8 C 1.1745(5) 0.7438(4) 0.4990(3) 0.0219(10) Uani 1 1 d . . . H8A H 1.2356 0.7809 0.5025 0.026 Uiso 1 1 calc R . . C9 C 1.1841(5) 0.7138(4) 0.4240(3) 0.0229(10) Uani 1 1 d . . . H9A H 1.2526 0.7292 0.3769 0.027 Uiso 1 1 calc R . . C10 C 1.0933(5) 0.6624(4) 0.4201(3) 0.0217(10) Uani 1 1 d . . . H10A H 1.0985 0.6429 0.3698 0.026 Uiso 1 1 calc R . . C11 C 0.9931(5) 0.6384(4) 0.4895(3) 0.0179(9) Uani 1 1 d . . . H11A H 0.9317 0.6018 0.4858 0.022 Uiso 1 1 calc R . . C12 C 0.9818(4) 0.6667(3) 0.5629(3) 0.0140(8) Uani 1 1 d . . . C13 C 0.7459(5) 0.5923(4) 0.6156(3) 0.0166(8) Uani 1 1 d . . . H13A H 0.7809 0.5320 0.5966 0.025 Uiso 1 1 calc R . . H13B H 0.7306 0.6407 0.5688 0.025 Uiso 1 1 calc R . . H13C H 0.6692 0.5792 0.6596 0.025 Uiso 1 1 calc R . . C14 C 0.9143(4) 0.4921(3) 0.9318(3) 0.0147(8) Uani 1 1 d . . . H14A H 0.9985 0.5021 0.9072 0.018 Uiso 1 1 calc R . . C15 C 0.8783(5) 0.4050(4) 0.9860(3) 0.0193(9) Uani 1 1 d . . . H15A H 0.9381 0.3561 0.9971 0.023 Uiso 1 1 calc R . . C16 C 0.7584(5) 0.3887(4) 1.0234(3) 0.0234(10) Uani 1 1 d . . . H16A H 0.7346 0.3305 1.0628 0.028 Uiso 1 1 calc R . . C17 C 0.6697(5) 0.4595(4) 1.0030(3) 0.0233(10) Uani 1 1 d . . . H17A H 0.5856 0.4476 1.0257 0.028 Uiso 1 1 calc R . . C18 C 0.7074(4) 0.5478(4) 0.9486(3) 0.0160(8) Uani 1 1 d . . . H18A H 0.6482 0.5964 0.9360 0.019 Uiso 1 1 calc R . . C19 C 0.8300(4) 0.5647(3) 0.9129(3) 0.0120(7) Uani 1 1 d . . . C20 C 0.8285(4) 0.7197(4) 1.0092(3) 0.0143(8) Uani 1 1 d . . . H20A H 0.7804 0.6644 1.0286 0.017 Uiso 1 1 calc R . . C21 C 0.8443(5) 0.7683(4) 1.0654(3) 0.0195(9) Uani 1 1 d . . . H21A H 0.8064 0.7467 1.1231 0.023 Uiso 1 1 calc R . . C22 C 0.9156(5) 0.8493(4) 1.0389(4) 0.0211(10) Uani 1 1 d . . . H22A H 0.9286 0.8818 1.0781 0.025 Uiso 1 1 calc R . . C23 C 0.9667(5) 0.8809(4) 0.9545(3) 0.0202(9) Uani 1 1 d . . . H23A H 1.0151 0.9360 0.9356 0.024 Uiso 1 1 calc R . . C24 C 0.9489(4) 0.8340(4) 0.8964(3) 0.0168(8) Uani 1 1 d . . . H24A H 0.9820 0.8586 0.8386 0.020 Uiso 1 1 calc R . . C25 C 0.8818(4) 0.7500(3) 0.9238(3) 0.0131(7) Uani 1 1 d . . . C26 C 1.0350(4) 0.6667(4) 0.7975(3) 0.0145(8) Uani 1 1 d . . . H26A H 1.0740 0.6372 0.8410 0.022 Uiso 1 1 calc R . . H26B H 1.0689 0.7299 0.7688 0.022 Uiso 1 1 calc R . . H26C H 1.0498 0.6241 0.7574 0.022 Uiso 1 1 calc R . . C27 C 0.3963(4) 0.8617(4) 0.8270(3) 0.0150(8) Uani 1 1 d . . . H27A H 0.4114 0.7932 0.8349 0.018 Uiso 1 1 calc R . . C28 C 0.2859(5) 0.9015(4) 0.8175(3) 0.0201(9) Uani 1 1 d . . . H28A H 0.2249 0.8603 0.8203 0.024 Uiso 1 1 calc R . . C29 C 0.2628(5) 1.0019(4) 0.8038(3) 0.0222(10) Uani 1 1 d . . . H29A H 0.1867 1.0294 0.7968 0.027 Uiso 1 1 calc R . . C30 C 0.3536(5) 1.0615(4) 0.8004(3) 0.0228(10) Uani 1 1 d . . . H30A H 0.3391 1.1301 0.7904 0.027 Uiso 1 1 calc R . . C31 C 0.4635(5) 1.0221(4) 0.8112(3) 0.0174(9) Uani 1 1 d . . . H31A H 0.5238 1.0636 0.8093 0.021 Uiso 1 1 calc R . . C32 C 0.4871(4) 0.9211(3) 0.8251(3) 0.0132(8) Uani 1 1 d . . . C33 C 0.6690(5) 0.9691(4) 0.9508(3) 0.0178(9) Uani 1 1 d . . . H33A H 0.6175 0.9263 0.9951 0.021 Uiso 1 1 calc R . . C34 C 0.7210(5) 1.0449(4) 0.9674(3) 0.0184(9) Uani 1 1 d . . . H34A H 0.7069 1.0515 1.0233 0.022 Uiso 1 1 calc R . . C35 C 0.7926(5) 1.1101(4) 0.9027(3) 0.0184(9) Uani 1 1 d . . . H35A H 0.8267 1.1614 0.9145 0.022 Uiso 1 1 calc R . . C36 C 0.8139(5) 1.1004(4) 0.8221(3) 0.0204(9) Uani 1 1 d . . . H36A H 0.8621 1.1455 0.7779 0.024 Uiso 1 1 calc R . . C37 C 0.7652(5) 1.0243(4) 0.8042(3) 0.0178(9) Uani 1 1 d . . . H37A H 0.7806 1.0180 0.7481 0.021 Uiso 1 1 calc R . . C38 C 0.6935(4) 0.9574(3) 0.8690(3) 0.0146(8) Uani 1 1 d . . . C39 C 0.5578(4) 0.7874(3) 0.9461(3) 0.0153(8) Uani 1 1 d . . . H39A H 0.5084 0.8308 0.9822 0.023 Uiso 1 1 calc R . . H39B H 0.6207 0.7525 0.9706 0.023 Uiso 1 1 calc R . . H39C H 0.5058 0.7407 0.9407 0.023 Uiso 1 1 calc R . . C40 C 0.4690(4) 0.7663(4) 0.6552(3) 0.0157(8) Uani 1 1 d . . . H40A H 0.5160 0.7090 0.6697 0.019 Uiso 1 1 calc R . . C41 C 0.3484(5) 0.7595(4) 0.6567(3) 0.0202(9) Uani 1 1 d . . . H41A H 0.3140 0.6978 0.6713 0.024 Uiso 1 1 calc R . . C42 C 0.2790(5) 0.8439(4) 0.6365(3) 0.0203(10) Uani 1 1 d . . . H42A H 0.1967 0.8400 0.6385 0.024 Uiso 1 1 calc R . . C43 C 0.3307(5) 0.9339(4) 0.6136(3) 0.0179(9) Uani 1 1 d . . . H43A H 0.2838 0.9914 0.5995 0.022 Uiso 1 1 calc R . . C44 C 0.4513(4) 0.9396(4) 0.6113(3) 0.0156(8) Uani 1 1 d . . . H44A H 0.4865 1.0011 0.5950 0.019 Uiso 1 1 calc R . . C45 C 0.5204(4) 0.8562(3) 0.6325(3) 0.0127(7) Uani 1 1 d . . . C46 C 0.8730(4) 0.8779(4) 0.4818(3) 0.0160(8) Uani 1 1 d . . . H46A H 0.9141 0.9026 0.5125 0.019 Uiso 1 1 calc R . . C47 C 0.9301(5) 0.8736(4) 0.4007(3) 0.0194(9) Uani 1 1 d . . . H47A H 1.0092 0.8972 0.3749 0.023 Uiso 1 1 calc R . . C48 C 0.8705(5) 0.8333(4) 0.3538(3) 0.0215(10) Uani 1 1 d . . . H48A H 0.9095 0.8300 0.2972 0.026 Uiso 1 1 calc R . . C49 C 0.7573(5) 0.8001(4) 0.3925(3) 0.0210(10) Uani 1 1 d . . . H49A H 0.7184 0.7713 0.3628 0.025 Uiso 1 1 calc R . . C50 C 0.6969(5) 0.8073(4) 0.4747(3) 0.0175(9) Uani 1 1 d . . . H50A H 0.6167 0.7857 0.4996 0.021 Uiso 1 1 calc R . . C51 C 0.7541(4) 0.8464(3) 0.5210(3) 0.0130(8) Uani 1 1 d . . . C52 C 0.6996(4) 0.9901(3) 0.6132(3) 0.0160(8) Uani 1 1 d . . . H52A H 0.6946 1.0218 0.5574 0.024 Uiso 1 1 calc R . . H52B H 0.7792 1.0002 0.6184 0.024 Uiso 1 1 calc R . . H52C H 0.6354 1.0182 0.6550 0.024 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 W1 0.00874(9) 0.00870(9) 0.00925(9) -0.00113(6) -0.00216(6) -0.00035(6) N1 0.0131(17) 0.0132(17) 0.0135(17) -0.0014(14) -0.0029(14) 0.0013(14) N2 0.0152(19) 0.0159(19) 0.022(2) -0.0017(16) -0.0033(16) -0.0019(15) N3 0.0124(17) 0.0131(17) 0.0162(18) -0.0026(14) -0.0056(14) 0.0010(14) N4 0.016(2) 0.018(2) 0.027(2) -0.0032(17) -0.0039(17) -0.0046(16) P1 0.0121(5) 0.0097(5) 0.0118(5) -0.0020(4) -0.0040(4) 0.0005(4) P2 0.0111(5) 0.0111(5) 0.0104(5) -0.0015(4) -0.0035(4) -0.0005(4) P3 0.0105(5) 0.0105(5) 0.0106(5) -0.0023(4) -0.0021(4) 0.0007(4) P4 0.0110(5) 0.0103(5) 0.0108(5) -0.0014(4) -0.0035(4) 0.0002(4) C1 0.017(2) 0.014(2) 0.020(2) -0.0053(17) -0.0058(17) 0.0011(16) C2 0.021(2) 0.015(2) 0.024(2) -0.0047(18) -0.010(2) 0.0055(18) C3 0.027(3) 0.014(2) 0.021(2) -0.0055(17) -0.012(2) 0.0060(18) C4 0.025(2) 0.013(2) 0.018(2) -0.0009(16) -0.0094(19) -0.0017(17) C5 0.019(2) 0.0121(19) 0.015(2) -0.0020(15) -0.0074(17) 0.0009(16) C6 0.0139(19) 0.0109(18) 0.0145(19) -0.0027(14) -0.0050(15) 0.0010(14) C7 0.017(2) 0.020(2) 0.016(2) -0.0051(17) -0.0009(17) -0.0027(17) C8 0.015(2) 0.028(3) 0.021(2) -0.005(2) -0.0010(18) -0.0044(19) C9 0.020(2) 0.027(3) 0.017(2) -0.0049(19) 0.0011(18) 0.002(2) C10 0.026(3) 0.021(2) 0.016(2) -0.0060(18) -0.0037(19) 0.0021(19) C11 0.023(2) 0.015(2) 0.016(2) -0.0044(16) -0.0055(18) 0.0017(17) C12 0.015(2) 0.0111(18) 0.0133(19) -0.0024(15) -0.0019(15) 0.0023(15) C13 0.020(2) 0.014(2) 0.018(2) -0.0045(16) -0.0068(17) 0.0011(16) C14 0.0142(19) 0.0131(19) 0.017(2) -0.0013(15) -0.0072(16) 0.0010(15) C15 0.020(2) 0.015(2) 0.022(2) 0.0010(17) -0.0086(19) 0.0010(17) C16 0.029(3) 0.017(2) 0.021(2) 0.0034(18) -0.008(2) -0.0034(19) C17 0.020(2) 0.021(2) 0.023(2) 0.0063(19) -0.0037(19) -0.0034(19) C18 0.015(2) 0.015(2) 0.016(2) 0.0011(16) -0.0053(16) -0.0001(16) C19 0.0147(19) 0.0112(18) 0.0113(17) -0.0028(14) -0.0046(15) -0.0014(14) C20 0.0130(19) 0.016(2) 0.0132(19) -0.0034(16) -0.0027(15) 0.0015(15) C21 0.022(2) 0.023(2) 0.014(2) -0.0074(18) -0.0048(18) 0.0014(19) C22 0.023(2) 0.019(2) 0.025(2) -0.0123(19) -0.007(2) 0.0004(18) C23 0.020(2) 0.020(2) 0.025(2) -0.0077(19) -0.0082(19) -0.0059(18) C24 0.017(2) 0.017(2) 0.017(2) -0.0063(16) -0.0029(16) -0.0016(16) C25 0.0128(19) 0.0124(18) 0.0141(19) -0.0027(15) -0.0047(15) 0.0011(14) C26 0.0124(19) 0.017(2) 0.0146(19) -0.0046(16) -0.0033(15) 0.0001(15) C27 0.0123(19) 0.020(2) 0.0118(18) -0.0037(16) -0.0024(15) 0.0011(16) C28 0.016(2) 0.029(3) 0.016(2) -0.0063(19) -0.0044(17) -0.0008(18) C29 0.016(2) 0.029(3) 0.022(2) -0.004(2) -0.0083(18) 0.0081(19) C30 0.021(2) 0.021(2) 0.021(2) -0.0031(19) -0.0013(19) 0.0070(19) C31 0.015(2) 0.014(2) 0.020(2) -0.0001(17) -0.0045(17) 0.0036(16) C32 0.0121(18) 0.0152(19) 0.0109(18) -0.0036(15) -0.0016(14) 0.0025(15) C33 0.023(2) 0.015(2) 0.015(2) -0.0014(16) -0.0050(18) -0.0035(17) C34 0.020(2) 0.020(2) 0.018(2) -0.0071(18) -0.0073(18) 0.0015(17) C35 0.020(2) 0.015(2) 0.022(2) -0.0059(17) -0.0078(19) -0.0011(17) C36 0.023(2) 0.017(2) 0.020(2) -0.0030(18) -0.0032(19) -0.0062(18) C37 0.019(2) 0.017(2) 0.015(2) -0.0035(16) -0.0007(17) -0.0032(17) C38 0.0133(19) 0.0118(19) 0.016(2) -0.0019(15) -0.0018(16) 0.0006(15) C39 0.015(2) 0.0136(19) 0.015(2) -0.0013(15) -0.0026(16) 0.0008(15) C40 0.015(2) 0.015(2) 0.017(2) -0.0023(16) -0.0043(16) -0.0006(15) C41 0.017(2) 0.022(2) 0.023(2) -0.0035(19) -0.0080(18) -0.0033(18) C42 0.014(2) 0.030(3) 0.020(2) -0.009(2) -0.0062(17) -0.0002(18) C43 0.019(2) 0.019(2) 0.016(2) -0.0019(17) -0.0075(17) 0.0034(17) C44 0.016(2) 0.015(2) 0.0150(19) -0.0018(15) -0.0061(16) 0.0017(16) C45 0.0116(18) 0.0152(19) 0.0104(17) -0.0020(14) -0.0024(14) -0.0004(14) C46 0.015(2) 0.016(2) 0.0143(19) -0.0019(16) -0.0014(16) -0.0004(16) C47 0.018(2) 0.018(2) 0.017(2) -0.0035(17) 0.0026(17) 0.0006(17) C48 0.020(2) 0.023(2) 0.018(2) 0.0019(18) -0.0056(18) 0.0008(19) C49 0.024(2) 0.021(2) 0.016(2) -0.0052(18) -0.0043(19) 0.0039(19) C50 0.022(2) 0.017(2) 0.015(2) -0.0022(16) -0.0071(18) -0.0038(17) C51 0.0149(19) 0.0138(19) 0.0099(17) -0.0016(14) -0.0044(15) 0.0024(15) C52 0.019(2) 0.0118(19) 0.017(2) -0.0013(15) -0.0057(17) -0.0024(16) _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 W1 N1 2.000(4) . ? W1 N3 1.996(5) . ? W1 P2 2.4687(11) . ? W1 P3 2.4727(12) . ? W1 P1 2.4761(12) . ? W1 P4 2.4774(11) . ? N1 N2 1.119(6) . ? N3 N4 1.142(6) . ? P1 C12 1.837(5) . ? P1 C13 1.834(5) . ? P1 C6 1.851(5) . ? P2 C19 1.839(5) . ? P2 C26 1.844(5) . ? P2 C25 1.857(5) . ? P3 C38 1.838(5) . ? P3 C39 1.843(5) . ? P3 C32 1.851(4) . ? P4 C52 1.840(5) . ? P4 C45 1.839(5) . ? P4 C51 1.846(4) . ? C1 C6 1.388(7) . ? C1 C2 1.412(7) . ? C1 H1A 0.9500 . ? C2 C3 1.386(8) . ? C2 H2A 0.9500 . ? C3 C4 1.391(7) . ? C3 H3A 0.9500 . ? C4 C5 1.394(6) . ? C4 H4A 0.9500 . ? C5 C6 1.392(7) . ? C5 H5A 0.9500 . ? C7 C8 1.389(7) . ? C7 C12 1.397(7) . ? C7 H7A 0.9500 . ? C8 C9 1.416(7) . ? C8 H8A 0.9500 . ? C9 C10 1.370(8) . ? C9 H9A 0.9500 . ? C10 C11 1.396(7) . ? C10 H10A 0.9500 . ? C11 C12 1.374(6) . ? C11 H11A 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.388(7) . ? C14 C19 1.386(6) . ? C14 H14A 0.9500 . ? C15 C16 1.362(8) . ? C15 H15A 0.9500 . ? C16 C17 1.414(7) . ? C16 H16A 0.9500 . ? C17 C18 1.406(7) . ? C17 H17A 0.9500 . ? C18 C19 1.388(7) . ? C18 H18A 0.9500 . ? C20 C21 1.370(7) . ? C20 C25 1.397(7) . ? C20 H20A 0.9500 . ? C21 C22 1.398(8) . ? C21 H21A 0.9500 . ? C22 C23 1.382(8) . ? C22 H22A 0.9500 . ? C23 C24 1.391(6) . ? C23 H23A 0.9500 . ? C24 C25 1.404(7) . ? C24 H24A 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.375(7) . ? C27 C32 1.407(7) . ? C27 H27A 0.9500 . ? C28 C29 1.393(8) . ? C28 H28A 0.9500 . ? C29 C30 1.401(8) . ? C29 H29A 0.9500 . ? C30 C31 1.376(7) . ? C30 H30A 0.9500 . ? C31 C32 1.402(7) . ? C31 H31A 0.9500 . ? C33 C34 1.407(7) . ? C33 C38 1.393(6) . ? C33 H33A 0.9500 . ? C34 C35 1.390(7) . ? C34 H34A 0.9500 . ? C35 C36 1.370(7) . ? C35 H35A 0.9500 . ? C36 C37 1.401(7) . ? C36 H36A 0.9500 . ? C37 C38 1.404(7) . ? C37 H37A 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.392(7) . ? C40 C41 1.401(7) . ? C40 H40A 0.9500 . ? C41 C42 1.397(7) . ? C41 H41A 0.9500 . ? C42 C43 1.392(8) . ? C42 H42A 0.9500 . ? C43 C44 1.395(7) . ? C43 H43A 0.9500 . ? C44 C45 1.389(6) . ? C44 H44A 0.9500 . ? C46 C47 1.362(6) . ? C46 C51 1.410(7) . ? C46 H46A 0.9500 . ? C47 C48 1.444(8) . ? C47 H47A 0.9500 . ? C48 C49 1.360(8) . ? C48 H48A 0.9500 . ? C49 C50 1.396(7) . ? C49 H49A 0.9500 . ? C50 C51 1.406(7) . ? C50 H50A 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? 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 W1 N3 179.20(13) . . ? N1 W1 P2 96.03(12) . . ? N3 W1 P2 84.46(12) . . ? N1 W1 P3 84.13(12) . . ? N3 W1 P3 95.24(12) . . ? P2 W1 P3 90.45(4) . . ? N1 W1 P1 84.25(12) . . ? N3 W1 P1 96.38(12) . . ? P2 W1 P1 90.44(4) . . ? P3 W1 P1 168.38(4) . . ? N1 W1 P4 95.32(12) . . ? N3 W1 P4 84.19(12) . . ? P2 W1 P4 168.64(4) . . ? P3 W1 P4 90.96(4) . . ? P1 W1 P4 90.44(4) . . ? N2 N1 W1 179.0(4) . . ? N4 N3 W1 179.5(5) . . ? C12 P1 C13 101.7(2) . . ? C12 P1 C6 100.8(2) . . ? C13 P1 C6 96.7(2) . . ? C12 P1 W1 121.59(15) . . ? C13 P1 W1 113.67(16) . . ? C6 P1 W1 118.40(15) . . ? C19 P2 C26 102.8(2) . . ? C19 P2 C25 99.1(2) . . ? C26 P2 C25 96.0(2) . . ? C19 P2 W1 121.15(15) . . ? C26 P2 W1 113.55(15) . . ? C25 P2 W1 119.98(14) . . ? C38 P3 C39 102.0(2) . . ? C38 P3 C32 100.8(2) . . ? C39 P3 C32 95.6(2) . . ? C38 P3 W1 121.19(15) . . ? C39 P3 W1 113.54(15) . . ? C32 P3 W1 119.50(14) . . ? C52 P4 C45 102.2(2) . . ? C52 P4 C51 96.7(2) . . ? C45 P4 C51 99.3(2) . . ? C52 P4 W1 113.55(16) . . ? C45 P4 W1 120.88(15) . . ? C51 P4 W1 120.19(14) . . ? C6 C1 C2 120.5(5) . . ? C6 C1 H1A 119.8 . . ? C2 C1 H1A 119.8 . . ? C3 C2 C1 120.0(5) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C4 C3 C2 119.5(5) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 120.8(4) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C1 C6 C5 118.9(4) . . ? C1 C6 P1 123.8(4) . . ? C5 C6 P1 117.3(3) . . ? C8 C7 C12 121.4(4) . . ? C8 C7 H7A 119.3 . . ? C12 C7 H7A 119.3 . . ? C7 C8 C9 119.1(5) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 119.2(5) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C9 C10 C11 120.7(5) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C12 C11 C10 121.2(5) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C11 C12 C7 118.3(5) . . ? C11 C12 P1 123.8(4) . . ? C7 C12 P1 117.9(3) . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 121.4(5) . . ? C15 C14 H14A 119.3 . . ? C19 C14 H14A 119.3 . . ? C16 C15 C14 120.8(5) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 119.3(5) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C18 C17 C16 119.2(5) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18A 119.5 . . ? C17 C18 H18A 119.5 . . ? C14 C19 C18 118.3(4) . . ? C14 C19 P2 124.2(4) . . ? C18 C19 P2 117.5(3) . . ? C21 C20 C25 121.1(5) . . ? C21 C20 H20A 119.4 . . ? C25 C20 H20A 119.4 . . ? C20 C21 C22 120.9(5) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C23 C22 C21 118.3(4) . . ? C23 C22 H22A 120.8 . . ? C21 C22 H22A 120.8 . . ? C24 C23 C22 121.5(5) . . ? C24 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? C23 C24 C25 119.6(5) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C20 C25 C24 118.4(4) . . ? C20 C25 P2 123.1(4) . . ? C24 C25 P2 118.5(4) . . ? P2 C26 H26A 109.5 . . ? P2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 120.8(5) . . ? C28 C27 H27A 119.6 . . ? C32 C27 H27A 119.6 . . ? C29 C28 C27 120.6(5) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 118.8(5) . . ? C28 C29 H29A 120.6 . . ? C30 C29 H29A 120.6 . . ? C31 C30 C29 120.9(5) . . ? C31 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? C30 C31 C32 120.4(5) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C31 C32 C27 118.4(4) . . ? C31 C32 P3 124.3(4) . . ? C27 C32 P3 117.2(3) . . ? C34 C33 C38 119.5(5) . . ? C34 C33 H33A 120.2 . . ? C38 C33 H33A 120.2 . . ? C35 C34 C33 120.6(4) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C36 C35 C34 119.9(5) . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C37 120.4(5) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C38 C37 C36 120.2(4) . . ? C38 C37 H37A 119.9 . . ? C36 C37 H37A 119.9 . . ? C37 C38 C33 119.2(5) . . ? C37 C38 P3 118.7(4) . . ? C33 C38 P3 122.1(4) . . ? P3 C39 H39A 109.5 . . ? P3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 120.5(4) . . ? C45 C40 H40A 119.8 . . ? C41 C40 H40A 119.8 . . ? C42 C41 C40 119.6(5) . . ? C42 C41 H41A 120.2 . . ? C40 C41 H41A 120.2 . . ? C43 C42 C41 119.9(5) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C44 C43 C42 120.0(4) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C45 120.5(5) . . ? C43 C44 H44A 119.7 . . ? C45 C44 H44A 119.7 . . ? C44 C45 C40 119.5(4) . . ? C44 C45 P4 122.5(4) . . ? C40 C45 P4 118.0(3) . . ? C47 C46 C51 121.3(5) . . ? C47 C46 H46A 119.3 . . ? C51 C46 H46A 119.3 . . ? C46 C47 C48 120.0(5) . . ? C46 C47 H47A 120.0 . . ? C48 C47 H47A 120.0 . . ? C49 C48 C47 118.6(5) . . ? C49 C48 H48A 120.7 . . ? C47 C48 H48A 120.7 . . ? C48 C49 C50 121.5(5) . . ? C48 C49 H49A 119.2 . . ? C50 C49 H49A 119.2 . . ? C49 C50 C51 120.4(5) . . ? C49 C50 H50A 119.8 . . ? C51 C50 H50A 119.8 . . ? C50 C51 C46 118.1(4) . . ? C50 C51 P4 123.1(4) . . ? C46 C51 P4 118.8(3) . . ? P4 C52 H52A 109.5 . . ? P4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? P4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 11.481 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.302