# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 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 'Gusev, Dmitry G.' ;Wilfrid Laurier University Department of Chemistry 75 University Avenue West Waterloo, Ontario N2L 3C5 Canada ; _publ_contact_author_address ;Wilfrid Laurier University Department of Chemistry 75 University Avenue West Waterloo, Ontario N2L 3C5 Canada ; _publ_contact_author_email dgoussev@wlu.ca _publ_contact_author_fax 1-519-746-0677 _publ_contact_author_phone '1-519-884-1970, 2736' _publ_contact_author_name 'Professor Dmitri G. Goussev (Gusev)' data_k0649 _database_code_depnum_ccdc_archive 'CCDC 815356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H40 Cl N Os P2' _chemical_formula_sum 'C16 H40 Cl N Os P2' _chemical_formula_weight 534.08 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' Cl Cl 0.1484 0.1585 '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' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.4821(5) _cell_length_b 13.5764(6) _cell_length_c 14.3947(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.339(2) _cell_angle_gamma 90.00 _cell_volume 2200.13(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 12132 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 6.059 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.279 _exptl_absorpt_correction_T_max 0.442 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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-Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12132 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3864 _reflns_number_gt 3235 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL V6.1(Sheldrick, 2001)' _computing_molecular_graphics 'SHELXTL V6.1' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0524P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3864 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Os1 Os 0.565202(17) 0.377875(14) 0.710908(14) 0.02364(12) Uani 1 1 d . . . H1OS H 0.618(4) 0.273(4) 0.725(4) 0.028 Uiso 1 1 d . . . H2OS H 0.580(4) 0.429(4) 0.810(3) 0.028 Uiso 1 1 d . . . H3OS H 0.610(4) 0.329(4) 0.806(4) 0.028 Uiso 1 1 d . . . Cl1 Cl 0.55135(12) 0.35132(9) 0.53690(9) 0.0295(3) Uani 1 1 d . . . P1 P 0.74204(13) 0.46059(10) 0.71886(10) 0.0288(3) Uani 1 1 d . . . P2 P 0.36853(12) 0.33326(10) 0.69419(10) 0.0294(3) Uani 1 1 d . . . N1 N 0.4902(4) 0.5208(3) 0.6607(3) 0.0297(10) Uani 1 1 d . . . H1C H 0.4857 0.5208 0.5955 0.036 Uiso 1 1 calc R . . C1 C 0.2908(5) 0.4467(4) 0.6420(5) 0.0406(14) Uani 1 1 d . . . H1A H 0.2759 0.4425 0.5719 0.049 Uiso 1 1 calc R . . H1B H 0.2133 0.4526 0.6618 0.049 Uiso 1 1 calc R . . C2 C 0.3667(5) 0.5369(4) 0.6749(4) 0.0377(14) Uani 1 1 d . . . H2A H 0.3323 0.5954 0.6386 0.045 Uiso 1 1 calc R . . H2B H 0.3675 0.5491 0.7429 0.045 Uiso 1 1 calc R . . C3 C 0.5685(5) 0.6047(4) 0.6981(4) 0.0354(15) Uani 1 1 d . . . H3A H 0.5719 0.6118 0.7670 0.042 Uiso 1 1 calc R . . H3B H 0.5363 0.6665 0.6666 0.042 Uiso 1 1 calc R . . C4 C 0.6924(5) 0.5861(4) 0.6795(4) 0.0360(13) Uani 1 1 d . . . H4A H 0.7483 0.6353 0.7140 0.043 Uiso 1 1 calc R . . H4B H 0.6918 0.5932 0.6109 0.043 Uiso 1 1 calc R . . C5 C 0.8364(5) 0.4285(4) 0.6326(4) 0.0360(13) Uani 1 1 d . . . H5A H 0.7836 0.4359 0.5689 0.043 Uiso 1 1 calc R . . C6 C 0.9398(6) 0.4982(5) 0.6316(5) 0.0566(18) Uani 1 1 d . . . H6A H 0.9841 0.4763 0.5837 0.085 Uiso 1 1 calc R . . H6B H 0.9924 0.4982 0.6941 0.085 Uiso 1 1 calc R . . H6C H 0.9094 0.5649 0.6163 0.085 Uiso 1 1 calc R . . C7 C 0.8743(6) 0.3215(5) 0.6384(5) 0.0477(16) Uani 1 1 d . . . H7A H 0.9233 0.3085 0.5911 0.072 Uiso 1 1 calc R . . H7B H 0.8038 0.2792 0.6259 0.072 Uiso 1 1 calc R . . H7C H 0.9205 0.3075 0.7018 0.072 Uiso 1 1 calc R . . C8 C 0.8467(5) 0.4804(4) 0.8318(4) 0.0354(13) Uani 1 1 d . . . H8A H 0.9153 0.5190 0.8176 0.043 Uiso 1 1 calc R . . C9 C 0.7911(6) 0.5408(4) 0.9015(4) 0.0478(16) Uani 1 1 d . . . H9A H 0.8497 0.5503 0.9602 0.072 Uiso 1 1 calc R . . H9B H 0.7220 0.5057 0.9154 0.072 Uiso 1 1 calc R . . H9C H 0.7661 0.6050 0.8734 0.072 Uiso 1 1 calc R . . C10 C 0.8952(7) 0.3839(4) 0.8761(5) 0.0509(18) Uani 1 1 d . . . H10A H 0.9507 0.3971 0.9358 0.076 Uiso 1 1 calc R . . H10B H 0.9368 0.3491 0.8326 0.076 Uiso 1 1 calc R . . H10C H 0.8296 0.3431 0.8886 0.076 Uiso 1 1 calc R . . C11 C 0.3029(5) 0.3027(5) 0.7979(4) 0.0426(15) Uani 1 1 d . . . H11A H 0.2224 0.2740 0.7738 0.051 Uiso 1 1 calc R . . C12 C 0.3758(6) 0.2264(5) 0.8609(4) 0.0468(16) Uani 1 1 d . . . H12A H 0.3383 0.2121 0.9150 0.070 Uiso 1 1 calc R . . H12B H 0.4561 0.2519 0.8839 0.070 Uiso 1 1 calc R . . H12C H 0.3801 0.1659 0.8246 0.070 Uiso 1 1 calc R . . C13 C 0.2876(9) 0.3906(5) 0.8583(6) 0.073(3) Uani 1 1 d . . . H13A H 0.2527 0.3694 0.9119 0.109 Uiso 1 1 calc R . . H13B H 0.2351 0.4387 0.8203 0.109 Uiso 1 1 calc R . . H13C H 0.3652 0.4209 0.8821 0.109 Uiso 1 1 calc R . . C14 C 0.3066(5) 0.2396(4) 0.6042(4) 0.0358(13) Uani 1 1 d . . . H14A H 0.3335 0.2593 0.5448 0.043 Uiso 1 1 calc R . . C15 C 0.1714(5) 0.2337(5) 0.5779(6) 0.061(2) Uani 1 1 d . . . H15A H 0.1483 0.1827 0.5297 0.091 Uiso 1 1 calc R . . H15B H 0.1396 0.2974 0.5528 0.091 Uiso 1 1 calc R . . H15C H 0.1396 0.2173 0.6344 0.091 Uiso 1 1 calc R . . C16 C 0.3592(6) 0.1393(4) 0.6295(5) 0.0482(17) Uani 1 1 d . . . H16A H 0.3250 0.0919 0.5803 0.072 Uiso 1 1 calc R . . H16B H 0.3414 0.1185 0.6904 0.072 Uiso 1 1 calc R . . H16C H 0.4455 0.1422 0.6343 0.072 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 Os1 0.02637(16) 0.02264(16) 0.02343(16) 0.00151(8) 0.00858(10) 0.00096(8) Cl1 0.0335(7) 0.0312(6) 0.0249(7) -0.0008(5) 0.0082(6) 0.0004(6) P1 0.0316(7) 0.0281(7) 0.0270(8) 0.0020(6) 0.0064(6) -0.0051(6) P2 0.0262(7) 0.0298(7) 0.0353(8) 0.0057(6) 0.0132(6) 0.0038(6) N1 0.035(2) 0.029(2) 0.029(2) 0.0004(19) 0.015(2) 0.001(2) C1 0.027(3) 0.044(3) 0.054(4) 0.012(3) 0.017(3) 0.011(3) C2 0.042(3) 0.031(3) 0.045(3) 0.009(3) 0.020(3) 0.015(3) C3 0.052(4) 0.023(3) 0.031(3) 0.000(2) 0.009(3) 0.000(2) C4 0.041(3) 0.029(3) 0.035(3) 0.006(3) 0.001(3) -0.009(3) C5 0.033(3) 0.045(3) 0.032(3) 0.002(3) 0.012(3) -0.009(3) C6 0.046(4) 0.070(5) 0.060(5) 0.006(4) 0.023(3) -0.016(4) C7 0.050(4) 0.056(4) 0.044(4) -0.005(3) 0.027(3) 0.004(3) C8 0.039(3) 0.033(3) 0.034(3) 0.004(3) 0.006(3) -0.007(3) C9 0.061(4) 0.043(3) 0.035(3) -0.009(3) -0.001(3) 0.005(3) C10 0.058(4) 0.055(4) 0.035(4) -0.001(3) -0.003(3) 0.010(3) C11 0.042(3) 0.053(4) 0.041(4) 0.002(3) 0.026(3) 0.006(3) C12 0.049(4) 0.061(4) 0.033(3) 0.009(3) 0.014(3) -0.007(3) C13 0.129(8) 0.055(4) 0.057(5) -0.006(3) 0.074(6) 0.009(4) C14 0.029(3) 0.042(3) 0.036(3) 0.004(3) 0.008(3) 0.002(3) C15 0.032(3) 0.061(4) 0.084(5) -0.003(4) 0.000(3) -0.006(3) C16 0.059(4) 0.036(3) 0.047(4) -0.009(3) 0.006(3) 0.001(3) _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 Os1 H3OS 1.52(5) . ? Os1 H1OS 1.55(5) . ? Os1 H2OS 1.56(5) . ? Os1 N1 2.187(4) . ? Os1 P1 2.3034(14) . ? Os1 P2 2.3044(14) . ? Os1 Cl1 2.5045(13) . ? P1 C8 1.842(6) . ? P1 C4 1.850(6) . ? P1 C5 1.853(6) . ? P2 C11 1.847(6) . ? P2 C14 1.855(6) . ? P2 C1 1.863(6) . ? N1 C3 1.486(7) . ? N1 C2 1.488(6) . ? C1 C2 1.524(8) . ? C3 C4 1.519(8) . ? C5 C7 1.514(9) . ? C5 C6 1.520(8) . ? C8 C10 1.514(8) . ? C8 C9 1.529(8) . ? C11 C13 1.507(8) . ? C11 C12 1.517(8) . ? C14 C16 1.505(8) . ? C14 C15 1.525(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 H3OS Os1 H1OS 55(2) . . ? H3OS Os1 H2OS 54(3) . . ? H1OS Os1 H2OS 109(3) . . ? H3OS Os1 N1 136.5(19) . . ? H1OS Os1 N1 168.2(19) . . ? H2OS Os1 N1 82.9(18) . . ? H3OS Os1 P1 91.5(19) . . ? H1OS Os1 P1 97.0(18) . . ? H2OS Os1 P1 78.5(18) . . ? N1 Os1 P1 82.54(12) . . ? H3OS Os1 P2 97.7(19) . . ? H1OS Os1 P2 97.1(18) . . ? H2OS Os1 P2 98.2(18) . . ? N1 Os1 P2 83.35(12) . . ? P1 Os1 P2 165.81(5) . . ? H3OS Os1 Cl1 141.7(19) . . ? H1OS Os1 Cl1 86.7(19) . . ? H2OS Os1 Cl1 161.8(18) . . ? N1 Os1 Cl1 81.58(12) . . ? P1 Os1 Cl1 90.11(5) . . ? P2 Os1 Cl1 89.40(5) . . ? C8 P1 C4 104.2(3) . . ? C8 P1 C5 105.0(3) . . ? C4 P1 C5 101.4(3) . . ? C8 P1 Os1 122.07(19) . . ? C4 P1 Os1 102.60(19) . . ? C5 P1 Os1 118.55(19) . . ? C11 P2 C14 104.4(3) . . ? C11 P2 C1 105.8(3) . . ? C14 P2 C1 101.4(3) . . ? C11 P2 Os1 121.5(2) . . ? C14 P2 Os1 119.12(18) . . ? C1 P2 Os1 101.94(18) . . ? C3 N1 C2 111.2(4) . . ? C3 N1 Os1 112.9(3) . . ? C2 N1 Os1 114.1(3) . . ? C2 C1 P2 109.8(4) . . ? N1 C2 C1 109.9(4) . . ? N1 C3 C4 109.2(4) . . ? C3 C4 P1 110.0(4) . . ? C7 C5 C6 112.4(5) . . ? C7 C5 P1 112.9(4) . . ? C6 C5 P1 114.9(4) . . ? C10 C8 C9 110.8(5) . . ? C10 C8 P1 111.6(4) . . ? C9 C8 P1 111.9(4) . . ? C13 C11 C12 108.0(6) . . ? C13 C11 P2 113.7(4) . . ? C12 C11 P2 111.8(4) . . ? C16 C14 C15 110.7(5) . . ? C16 C14 P2 111.7(4) . . ? C15 C14 P2 116.1(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C Cl1 0.93 2.61 3.074(4) 111.3 . N1 H1C Cl1 0.93 2.55 3.286(4) 136.3 3_666 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.858 _refine_diff_density_min -2.907 _refine_diff_density_rms 0.256 # Attachment '- Complex4.cif' data_k07138 _database_code_depnum_ccdc_archive 'CCDC 815357' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H48 N Os P3' _chemical_formula_sum 'C19 H48 N Os P3' _chemical_formula_weight 573.69 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' P P 0.1023 0.0942 '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' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.2733(4) _cell_length_b 9.7158(2) _cell_length_c 16.9733(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.9870(11) _cell_angle_gamma 90.00 _cell_volume 2463.79(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 14955 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 5.374 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.490 _exptl_absorpt_correction_T_max 0.588 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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-Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14955 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5590 _reflns_number_gt 4183 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL V6.1(Sheldrick, 2001)' _computing_molecular_graphics 'SHELXTL V6.1' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0428P)^2^+1.3756P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5590 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 Os1 Os 0.762312(14) 0.16024(2) 0.520751(14) 0.01780(9) Uani 1 1 d . . . H1OS H 0.847(4) 0.205(5) 0.475(4) 0.024(15) Uiso 1 1 d . . . H2OS H 0.683(5) 0.104(8) 0.572(5) 0.07(2) Uiso 1 1 d . . . P1 P 0.71459(10) 0.01096(15) 0.41471(9) 0.0201(3) Uani 1 1 d . . . P2 P 0.84158(10) 0.25497(15) 0.63824(10) 0.0207(3) Uani 1 1 d . . . P3 P 0.68011(10) 0.34434(14) 0.47320(10) 0.0208(3) Uani 1 1 d . . . N1 N 0.8377(3) -0.0272(5) 0.5718(3) 0.0232(11) Uani 1 1 d . . . H1 H 0.7996 -0.0748 0.5983 0.028 Uiso 1 1 calc R . . C1 C 0.7732(4) -0.1528(5) 0.4479(4) 0.0257(14) Uani 1 1 d . . . H1A H 0.7334 -0.2141 0.4713 0.031 Uiso 1 1 calc R . . H1B H 0.7891 -0.2003 0.4012 0.031 Uiso 1 1 calc R . . C2 C 0.8565(4) -0.1221(6) 0.5099(4) 0.0275(14) Uani 1 1 d . . . H2A H 0.8814 -0.2090 0.5357 0.033 Uiso 1 1 calc R . . H2B H 0.9019 -0.0806 0.4831 0.033 Uiso 1 1 calc R . . C3 C 0.9183(4) 0.0001(6) 0.6325(4) 0.0282(14) Uani 1 1 d . . . H3A H 0.9661 0.0331 0.6058 0.034 Uiso 1 1 calc R . . H3B H 0.9391 -0.0866 0.6610 0.034 Uiso 1 1 calc R . . C4 C 0.9023(4) 0.1060(6) 0.6929(4) 0.0272(14) Uani 1 1 d . . . H4A H 0.9602 0.1370 0.7259 0.033 Uiso 1 1 calc R . . H4B H 0.8664 0.0652 0.7293 0.033 Uiso 1 1 calc R . . C5 C 0.7454(4) 0.0321(6) 0.3148(3) 0.0249(13) Uani 1 1 d . . . H5A H 0.7271 -0.0540 0.2834 0.030 Uiso 1 1 calc R . . C6 C 0.8469(4) 0.0484(7) 0.3226(4) 0.0360(16) Uani 1 1 d . . . H6A H 0.8604 0.0586 0.2689 0.054 Uiso 1 1 calc R . . H6B H 0.8775 -0.0332 0.3489 0.054 Uiso 1 1 calc R . . H6C H 0.8675 0.1303 0.3549 0.054 Uiso 1 1 calc R . . C7 C 0.6955(5) 0.1513(6) 0.2669(4) 0.0317(15) Uani 1 1 d . . . H7A H 0.7131 0.1582 0.2147 0.048 Uiso 1 1 calc R . . H7B H 0.7104 0.2373 0.2969 0.048 Uiso 1 1 calc R . . H7C H 0.6309 0.1351 0.2582 0.048 Uiso 1 1 calc R . . C8 C 0.5959(4) -0.0505(6) 0.3831(4) 0.0277(14) Uani 1 1 d . . . H8A H 0.5582 0.0333 0.3677 0.033 Uiso 1 1 calc R . . C9 C 0.5758(5) -0.1482(6) 0.3106(5) 0.0367(17) Uani 1 1 d . . . H9A H 0.5122 -0.1732 0.2995 0.055 Uiso 1 1 calc R . . H9B H 0.6122 -0.2315 0.3227 0.055 Uiso 1 1 calc R . . H9C H 0.5900 -0.1024 0.2634 0.055 Uiso 1 1 calc R . . C10 C 0.5630(4) -0.1177(7) 0.4539(4) 0.0368(17) Uani 1 1 d . . . H10A H 0.5009 -0.1480 0.4358 0.055 Uiso 1 1 calc R . . H10B H 0.5664 -0.0506 0.4976 0.055 Uiso 1 1 calc R . . H10C H 0.6009 -0.1972 0.4735 0.055 Uiso 1 1 calc R . . C11 C 0.7890(4) 0.3320(6) 0.7187(4) 0.0255(14) Uani 1 1 d . . . H11A H 0.7638 0.4231 0.6979 0.031 Uiso 1 1 calc R . . C12 C 0.7100(4) 0.2442(6) 0.7323(4) 0.0338(16) Uani 1 1 d . . . H12A H 0.6835 0.2864 0.7743 0.051 Uiso 1 1 calc R . . H12B H 0.7312 0.1514 0.7492 0.051 Uiso 1 1 calc R . . H12C H 0.6648 0.2386 0.6821 0.051 Uiso 1 1 calc R . . C13 C 0.8528(5) 0.3597(7) 0.7991(4) 0.0360(16) Uani 1 1 d . . . H13A H 0.8194 0.3999 0.8369 0.054 Uiso 1 1 calc R . . H13B H 0.8996 0.4239 0.7909 0.054 Uiso 1 1 calc R . . H13C H 0.8804 0.2730 0.8211 0.054 Uiso 1 1 calc R . . C14 C 0.9358(4) 0.3795(6) 0.6409(4) 0.0253(14) Uani 1 1 d . . . H14A H 0.9691 0.3862 0.6981 0.030 Uiso 1 1 calc R . . C15 C 1.0023(4) 0.3307(6) 0.5906(5) 0.0351(17) Uani 1 1 d . . . H15A H 1.0503 0.3989 0.5939 0.053 Uiso 1 1 calc R . . H15B H 0.9713 0.3198 0.5344 0.053 Uiso 1 1 calc R . . H15C H 1.0281 0.2423 0.6115 0.053 Uiso 1 1 calc R . . C16 C 0.9030(4) 0.5239(6) 0.6142(4) 0.0352(16) Uani 1 1 d . . . H16A H 0.9545 0.5851 0.6167 0.053 Uiso 1 1 calc R . . H16B H 0.8653 0.5588 0.6500 0.053 Uiso 1 1 calc R . . H16C H 0.8681 0.5205 0.5588 0.053 Uiso 1 1 calc R . . C17 C 0.6451(4) 0.4660(6) 0.5447(4) 0.0349(16) Uani 1 1 d . . . H17A H 0.6100 0.5407 0.5147 0.052 Uiso 1 1 calc R . . H17B H 0.6983 0.5044 0.5804 0.052 Uiso 1 1 calc R . . H17C H 0.6086 0.4173 0.5770 0.052 Uiso 1 1 calc R . . C18 C 0.5693(4) 0.3194(6) 0.4077(4) 0.0298(15) Uani 1 1 d . . . H18A H 0.5420 0.4092 0.3920 0.045 Uiso 1 1 calc R . . H18B H 0.5311 0.2672 0.4368 0.045 Uiso 1 1 calc R . . H18C H 0.5757 0.2684 0.3594 0.045 Uiso 1 1 calc R . . C19 C 0.7244(5) 0.4711(6) 0.4106(4) 0.0332(16) Uani 1 1 d . . . H19A H 0.6805 0.5448 0.3948 0.050 Uiso 1 1 calc R . . H19B H 0.7360 0.4256 0.3622 0.050 Uiso 1 1 calc R . . H19C H 0.7803 0.5102 0.4414 0.050 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 Os1 0.01848(14) 0.01635(14) 0.01868(14) 0.00036(9) 0.00413(10) 0.00226(9) P1 0.0206(8) 0.0199(8) 0.0197(8) -0.0012(6) 0.0039(7) 0.0015(6) P2 0.0196(8) 0.0222(8) 0.0206(9) -0.0005(6) 0.0046(7) 0.0021(6) P3 0.0235(8) 0.0177(8) 0.0202(8) 0.0013(6) 0.0021(7) 0.0031(6) N1 0.026(3) 0.018(2) 0.026(3) 0.002(2) 0.007(2) 0.006(2) C1 0.029(3) 0.019(3) 0.029(4) 0.000(3) 0.004(3) 0.004(2) C2 0.033(4) 0.024(3) 0.027(4) -0.001(3) 0.009(3) 0.005(3) C3 0.028(3) 0.027(3) 0.026(4) -0.001(3) -0.003(3) 0.007(3) C4 0.029(4) 0.031(3) 0.020(3) 0.004(3) 0.001(3) 0.006(3) C5 0.029(3) 0.030(3) 0.015(3) -0.005(3) 0.002(3) 0.001(3) C6 0.036(4) 0.052(4) 0.022(4) 0.000(3) 0.011(3) 0.004(3) C7 0.038(4) 0.033(4) 0.024(4) 0.006(3) 0.005(3) 0.003(3) C8 0.023(3) 0.027(3) 0.031(4) -0.001(3) 0.001(3) -0.002(3) C9 0.033(4) 0.035(4) 0.039(4) -0.009(3) 0.002(3) -0.008(3) C10 0.030(4) 0.037(4) 0.046(5) 0.000(3) 0.012(3) -0.003(3) C11 0.026(3) 0.031(3) 0.020(3) 0.000(3) 0.005(3) -0.001(3) C12 0.036(4) 0.035(4) 0.034(4) -0.005(3) 0.015(3) -0.008(3) C13 0.032(4) 0.049(4) 0.025(4) -0.006(3) 0.003(3) 0.006(3) C14 0.021(3) 0.033(3) 0.021(3) -0.008(3) 0.001(3) -0.001(3) C15 0.020(3) 0.042(4) 0.045(5) -0.008(3) 0.009(3) -0.002(3) C16 0.032(4) 0.034(4) 0.042(4) 0.006(3) 0.012(3) -0.004(3) C17 0.036(4) 0.037(4) 0.029(4) -0.005(3) 0.000(3) 0.018(3) C18 0.023(3) 0.034(4) 0.029(4) 0.001(3) -0.001(3) 0.010(3) C19 0.051(4) 0.021(3) 0.026(4) 0.002(3) 0.004(3) 0.005(3) _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 Os1 H1OS 1.70(6) . ? Os1 H2OS 1.72(7) . ? Os1 N1 2.231(4) . ? Os1 P3 2.2374(14) . ? Os1 P2 2.2993(16) . ? Os1 P1 2.3087(15) . ? P1 C1 1.855(5) . ? P1 C5 1.863(6) . ? P1 C8 1.878(6) . ? P2 C4 1.859(6) . ? P2 C14 1.874(6) . ? P2 C11 1.878(6) . ? P3 C18 1.838(6) . ? P3 C19 1.845(6) . ? P3 C17 1.851(6) . ? N1 C3 1.456(7) . ? N1 C2 1.470(7) . ? C1 C2 1.503(9) . ? C3 C4 1.508(8) . ? C5 C7 1.525(8) . ? C5 C6 1.537(8) . ? C8 C9 1.534(9) . ? C8 C10 1.541(9) . ? C11 C13 1.527(9) . ? C11 C12 1.535(8) . ? C14 C16 1.526(8) . ? C14 C15 1.531(8) . ? 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 H1OS Os1 H2OS 175(3) . . ? H1OS Os1 N1 90.2(18) . . ? H2OS Os1 N1 85(2) . . ? H1OS Os1 P3 93.2(18) . . ? H2OS Os1 P3 92(2) . . ? N1 Os1 P3 176.56(13) . . ? H1OS Os1 P2 88.8(19) . . ? H2OS Os1 P2 89(2) . . ? N1 Os1 P2 81.59(13) . . ? P3 Os1 P2 98.50(5) . . ? H1OS Os1 P1 87.2(19) . . ? H2OS Os1 P1 93(2) . . ? N1 Os1 P1 81.01(13) . . ? P3 Os1 P1 99.11(5) . . ? P2 Os1 P1 162.13(5) . . ? C1 P1 C5 100.0(3) . . ? C1 P1 C8 101.0(3) . . ? C5 P1 C8 100.7(3) . . ? C1 P1 Os1 104.3(2) . . ? C5 P1 Os1 122.82(19) . . ? C8 P1 Os1 123.5(2) . . ? C4 P2 C14 100.9(3) . . ? C4 P2 C11 101.0(3) . . ? C14 P2 C11 99.6(3) . . ? C4 P2 Os1 103.9(2) . . ? C14 P2 Os1 122.9(2) . . ? C11 P2 Os1 124.3(2) . . ? C18 P3 C19 98.1(3) . . ? C18 P3 C17 97.2(3) . . ? C19 P3 C17 98.2(3) . . ? C18 P3 Os1 119.3(2) . . ? C19 P3 Os1 119.7(2) . . ? C17 P3 Os1 119.4(2) . . ? C3 N1 C2 111.0(5) . . ? C3 N1 Os1 114.7(3) . . ? C2 N1 Os1 113.3(4) . . ? C2 C1 P1 109.1(4) . . ? N1 C2 C1 111.3(5) . . ? N1 C3 C4 111.9(5) . . ? C3 C4 P2 109.1(4) . . ? C7 C5 C6 110.5(5) . . ? C7 C5 P1 112.1(4) . . ? C6 C5 P1 111.9(4) . . ? C9 C8 C10 108.7(5) . . ? C9 C8 P1 116.5(5) . . ? C10 C8 P1 111.3(4) . . ? C13 C11 C12 109.8(5) . . ? C13 C11 P2 115.5(4) . . ? C12 C11 P2 110.9(4) . . ? C16 C14 C15 109.5(5) . . ? C16 C14 P2 112.5(4) . . ? C15 C14 P2 112.5(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 4.022 _refine_diff_density_min -2.186 _refine_diff_density_rms 0.208