# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'K. Caulton' _publ_contact_author_address ; Department of Chemistry Indiana University 800 E. Kirkwood Avenue Bloomington IN 47405 UNITED STATES OF AMERICA ; _publ_contact_author_email CAULTON@INDIANA.EDU _publ_section_title ; Reactivity of NO with an Osmium Polyhydride: Reductive Elimination and Reductive Nitrosylation on the Path from Odd- to Even-Electron Molecules ; loop_ _publ_author_name 'K. Caulton' 'Hongjun Fan.' 'Joo-Ho Lee.' 'Maren Pink' data_06013a _database_code_depnum_ccdc_archive 'CCDC 644903' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H53 N3 O2.50 OS P2 SI2' _chemical_formula_sum 'C22 H53 N3 O2.50 Os P2 Si2' _chemical_formula_weight 707.99 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' Si Si 0.0817 0.0704 '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' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P-42(1)c _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 23.2509(16) _cell_length_b 23.2509(16) _cell_length_c 11.4920(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6212.6(11) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 5557 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26.1 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 4.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6258 _exptl_absorpt_correction_T_max 0.8134 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 40 seconds each' _diffrn_measurement_method \w-scans _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99082 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6436 _reflns_number_gt 5810 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SIR-2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003), XTEL (loc. libr.)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _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^+8.9145P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(7) _refine_ls_number_reflns 6436 _refine_ls_number_parameters 310 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.080 _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 0.728419(8) 0.011728(7) 0.835561(18) 0.02170(5) Uani 1 1 d . . . H1OS H 0.7065 0.0731 0.7790 0.035(16) Uiso 1 1 d R A . O2 O 0.61541(19) -0.0020(2) 0.9422(4) 0.0535(12) Uani 1 1 d . . . N2 N 0.6613(2) 0.00122(19) 0.8989(4) 0.0294(10) Uani 1 1 d . A . O3 O 0.7793(5) -0.0545(3) 0.9181(9) 0.0393(11) Uani 0.50 1 d PDU A 1 N3 N 0.7662(4) -0.0997(3) 0.9684(8) 0.0393(11) Uani 0.50 1 d PDU A 1 O4 O 0.7198(4) -0.1046(3) 0.9744(7) 0.0393(11) Uani 0.50 1 d PDU A 1 O3D O 0.8138(4) -0.0708(3) 0.9409(7) 0.0393(11) Uani 0.50 1 d PU A 2 N3D N 0.7606(5) -0.0697(5) 0.9240(11) 0.0393(11) Uani 0.50 1 d PU A 2 P1 P 0.76300(6) 0.07186(6) 0.99456(12) 0.0278(3) Uani 1 1 d . A . P2 P 0.70400(6) -0.03460(5) 0.65172(13) 0.0279(3) Uani 1 1 d . A . Si1 Si 0.86747(5) 0.04189(6) 0.84284(16) 0.0283(3) Uani 1 1 d . . . Si2 Si 0.80955(7) 0.04191(7) 0.61068(13) 0.0313(3) Uani 1 1 d . . . N1 N 0.80721(19) 0.02990(19) 0.7582(4) 0.0267(10) Uani 1 1 d . A . C1 C 0.9170(3) -0.0211(3) 0.8528(7) 0.0523(17) Uani 1 1 d . A . H1A H 0.8958 -0.0544 0.8826 0.078 Uiso 1 1 calc R . . H1B H 0.9488 -0.0119 0.9057 0.078 Uiso 1 1 calc R . . H1C H 0.9323 -0.0299 0.7754 0.078 Uiso 1 1 calc R . . C2 C 0.9162(3) 0.1014(3) 0.7870(6) 0.0428(15) Uani 1 1 d . A . H2A H 0.9346 0.0889 0.7145 0.064 Uiso 1 1 calc R . . H2B H 0.9457 0.1098 0.8453 0.064 Uiso 1 1 calc R . . H2C H 0.8933 0.1360 0.7723 0.064 Uiso 1 1 calc R . . C3 C 0.8405(2) 0.0644(3) 0.9921(5) 0.0346(12) Uani 1 1 d . A . H3A H 0.8523 0.0353 1.0503 0.041 Uiso 1 1 calc R . . H3B H 0.8584 0.1015 1.0140 0.041 Uiso 1 1 calc R . . C4 C 0.7416(3) 0.0524(3) 1.1487(5) 0.0419(14) Uani 1 1 d . . . C5 C 0.7835(3) 0.0769(4) 1.2390(5) 0.058(2) Uani 1 1 d . A . H5A H 0.7704 0.0666 1.3173 0.087 Uiso 1 1 calc R . . H5B H 0.7850 0.1188 1.2315 0.087 Uiso 1 1 calc R . . H5C H 0.8219 0.0608 1.2258 0.087 Uiso 1 1 calc R . . C6 C 0.6803(3) 0.0731(3) 1.1774(6) 0.0527(17) Uani 1 1 d . A . H6A H 0.6699 0.0605 1.2559 0.079 Uiso 1 1 calc R . . H6B H 0.6532 0.0568 1.1210 0.079 Uiso 1 1 calc R . . H6C H 0.6789 0.1152 1.1733 0.079 Uiso 1 1 calc R . . C7 C 0.7427(3) -0.0123(3) 1.1617(6) 0.0493(16) Uani 1 1 d . A . H7A H 0.7360 -0.0226 1.2433 0.074 Uiso 1 1 calc R . . H7B H 0.7804 -0.0270 1.1372 0.074 Uiso 1 1 calc R . . H7C H 0.7126 -0.0294 1.1130 0.074 Uiso 1 1 calc R . . C8 C 0.7459(3) 0.1507(2) 0.9694(5) 0.0397(14) Uani 1 1 d . . . C9 C 0.6817(3) 0.1583(3) 0.9403(6) 0.0504(17) Uani 1 1 d . A . H9A H 0.6745 0.1982 0.9167 0.076 Uiso 1 1 calc R . . H9B H 0.6585 0.1492 1.0092 0.076 Uiso 1 1 calc R . . H9C H 0.6712 0.1323 0.8766 0.076 Uiso 1 1 calc R . . C10 C 0.7629(3) 0.1901(3) 1.0714(6) 0.0535(18) Uani 1 1 d . A . H10A H 0.7570 0.2304 1.0491 0.080 Uiso 1 1 calc R . . H10B H 0.8035 0.1840 1.0907 0.080 Uiso 1 1 calc R . . H10C H 0.7390 0.1811 1.1393 0.080 Uiso 1 1 calc R . . C11 C 0.7813(3) 0.1697(3) 0.8640(5) 0.0475(16) Uani 1 1 d . A . H11A H 0.7678 0.2074 0.8373 0.071 Uiso 1 1 calc R . . H11B H 0.7769 0.1416 0.8012 0.071 Uiso 1 1 calc R . . H11C H 0.8220 0.1724 0.8860 0.071 Uiso 1 1 calc R . . C12 C 0.8776(3) 0.0147(4) 0.5395(5) 0.0527(18) Uani 1 1 d . A . H12A H 0.9092 0.0414 0.5557 0.079 Uiso 1 1 calc R . . H12B H 0.8717 0.0119 0.4552 0.079 Uiso 1 1 calc R . . H12C H 0.8871 -0.0234 0.5707 0.079 Uiso 1 1 calc R . . C13 C 0.8026(3) 0.1192(3) 0.5686(5) 0.0425(15) Uani 1 1 d . A . H13A H 0.8347 0.1411 0.6017 0.064 Uiso 1 1 calc R . . H13B H 0.7662 0.1346 0.5985 0.064 Uiso 1 1 calc R . . H13C H 0.8033 0.1226 0.4836 0.064 Uiso 1 1 calc R . . C14 C 0.7449(3) 0.0056(3) 0.5454(4) 0.0343(14) Uani 1 1 d . A . H14A H 0.7197 0.0351 0.5097 0.041 Uiso 1 1 calc R . . H14B H 0.7577 -0.0208 0.4829 0.041 Uiso 1 1 calc R . . C15 C 0.7280(3) -0.1111(2) 0.6307(5) 0.0442(15) Uani 1 1 d . . . C16 C 0.6990(4) -0.1520(3) 0.7184(6) 0.063(2) Uani 1 1 d . A . H16A H 0.7134 -0.1912 0.7067 0.094 Uiso 1 1 calc R . . H16B H 0.6573 -0.1513 0.7066 0.094 Uiso 1 1 calc R . . H16C H 0.7079 -0.1394 0.7979 0.094 Uiso 1 1 calc R . . C17 C 0.7167(4) -0.1342(3) 0.5074(7) 0.073(2) Uani 1 1 d . A . H17A H 0.7379 -0.1702 0.4962 0.109 Uiso 1 1 calc R . . H17B H 0.7294 -0.1058 0.4500 0.109 Uiso 1 1 calc R . . H17C H 0.6754 -0.1414 0.4977 0.109 Uiso 1 1 calc R . . C18 C 0.7935(3) -0.1110(3) 0.6531(7) 0.0547(17) Uani 1 1 d . A . H18A H 0.8076 -0.1507 0.6552 0.082 Uiso 1 1 calc R . . H18B H 0.8014 -0.0924 0.7278 0.082 Uiso 1 1 calc R . . H18C H 0.8129 -0.0900 0.5906 0.082 Uiso 1 1 calc R . . C19 C 0.6264(3) -0.0255(3) 0.6062(5) 0.0371(13) Uani 1 1 d . . . C20 C 0.5873(3) -0.0682(3) 0.6696(7) 0.0507(15) Uani 1 1 d . A . H20A H 0.5470 -0.0583 0.6549 0.076 Uiso 1 1 calc R . . H20B H 0.5950 -0.0665 0.7534 0.076 Uiso 1 1 calc R . . H20C H 0.5950 -0.1072 0.6412 0.076 Uiso 1 1 calc R . . C21 C 0.6189(3) -0.0334(4) 0.4727(5) 0.060(2) Uani 1 1 d . A . H21A H 0.5784 -0.0282 0.4520 0.089 Uiso 1 1 calc R . . H21B H 0.6314 -0.0721 0.4504 0.089 Uiso 1 1 calc R . . H21C H 0.6423 -0.0047 0.4317 0.089 Uiso 1 1 calc R . . C22 C 0.6080(3) 0.0360(3) 0.6358(6) 0.0495(18) Uani 1 1 d . A . H22A H 0.5717 0.0448 0.5963 0.074 Uiso 1 1 calc R . . H22B H 0.6377 0.0630 0.6099 0.074 Uiso 1 1 calc R . . H22C H 0.6028 0.0396 0.7201 0.074 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 0.02272(9) 0.02263(9) 0.01976(8) 0.00037(8) 0.00018(10) -0.00233(7) O2 0.040(3) 0.075(3) 0.046(2) -0.010(3) 0.013(2) -0.022(2) N2 0.031(3) 0.031(2) 0.026(2) -0.0043(19) 0.0057(19) -0.0077(18) O3 0.065(3) 0.021(2) 0.0322(19) 0.0048(16) -0.012(2) 0.004(2) N3 0.065(3) 0.021(2) 0.0322(19) 0.0048(16) -0.012(2) 0.004(2) O4 0.065(3) 0.021(2) 0.0322(19) 0.0048(16) -0.012(2) 0.004(2) O3D 0.065(3) 0.021(2) 0.0322(19) 0.0048(16) -0.012(2) 0.004(2) N3D 0.065(3) 0.021(2) 0.0322(19) 0.0048(16) -0.012(2) 0.004(2) P1 0.0292(7) 0.0334(7) 0.0208(6) -0.0034(6) -0.0004(5) -0.0046(6) P2 0.0335(7) 0.0281(6) 0.0221(7) -0.0020(6) -0.0005(6) -0.0067(5) Si1 0.0235(6) 0.0332(7) 0.0282(7) 0.0044(7) -0.0015(7) -0.0031(5) Si2 0.0307(8) 0.0426(9) 0.0205(7) -0.0004(6) 0.0038(6) -0.0074(7) N1 0.023(2) 0.030(2) 0.027(2) 0.0021(18) 0.0031(18) -0.0022(18) C1 0.042(3) 0.047(4) 0.069(5) 0.010(4) -0.004(4) 0.007(3) C2 0.041(3) 0.049(4) 0.039(3) 0.005(3) 0.000(3) -0.012(3) C3 0.033(3) 0.047(3) 0.024(3) 0.004(2) -0.008(2) -0.006(2) C4 0.042(3) 0.064(4) 0.019(3) 0.000(3) -0.001(2) -0.006(3) C5 0.065(5) 0.089(5) 0.020(3) 0.001(3) -0.009(3) -0.028(4) C6 0.053(4) 0.075(4) 0.031(3) -0.005(3) 0.009(3) -0.005(3) C7 0.055(4) 0.067(4) 0.027(3) 0.010(4) -0.006(3) -0.002(3) C8 0.053(4) 0.035(3) 0.032(3) -0.006(2) -0.001(3) 0.004(3) C9 0.054(4) 0.044(4) 0.053(4) -0.007(3) -0.003(3) 0.018(3) C10 0.077(5) 0.042(4) 0.042(4) -0.014(3) 0.003(3) -0.009(3) C11 0.064(4) 0.035(3) 0.044(4) 0.002(3) 0.007(3) -0.005(3) C12 0.042(4) 0.079(5) 0.037(3) -0.009(3) 0.014(3) -0.009(4) C13 0.047(4) 0.052(4) 0.029(3) 0.008(3) -0.006(3) -0.015(3) C14 0.039(3) 0.048(3) 0.016(2) 0.002(3) 0.000(2) -0.005(3) C15 0.070(4) 0.024(3) 0.039(3) -0.008(2) 0.003(3) -0.005(3) C16 0.095(6) 0.037(4) 0.057(5) 0.009(3) -0.008(4) -0.005(4) C17 0.116(7) 0.050(4) 0.053(4) -0.025(4) -0.011(5) -0.001(4) C18 0.069(4) 0.046(4) 0.049(4) -0.007(4) 0.010(4) 0.018(3) C19 0.037(3) 0.044(3) 0.031(3) 0.005(3) -0.009(2) -0.013(3) C20 0.042(3) 0.065(4) 0.046(3) 0.005(4) -0.007(4) -0.024(3) C21 0.047(4) 0.097(6) 0.034(4) 0.008(4) -0.014(3) -0.032(4) C22 0.038(3) 0.057(4) 0.053(5) 0.009(3) -0.018(3) 0.000(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 N2 1.739(4) . ? Os1 N1 2.080(4) . ? Os1 O3 2.161(10) . ? Os1 N3D 2.275(12) . ? Os1 P1 2.4372(14) . ? Os1 P2 2.4385(15) . ? Os1 H1OS 1.6497 . ? O2 N2 1.179(6) . ? O3 N3 1.237(8) . ? N3 O4 1.089(8) . ? O3D N3D 1.252(16) . ? P1 C3 1.811(6) . ? P1 C4 1.895(6) . ? P1 C8 1.899(6) . ? P2 C14 1.808(6) . ? P2 C15 1.880(6) . ? P2 C19 1.891(6) . ? Si1 N1 1.728(5) . ? Si1 C1 1.866(6) . ? Si1 C2 1.899(6) . ? Si1 C3 1.900(6) . ? Si2 N1 1.720(5) . ? Si2 C13 1.869(7) . ? Si2 C14 1.881(6) . ? Si2 C12 1.890(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.513(9) . ? C4 C5 1.533(8) . ? C4 C6 1.540(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C11 1.530(8) . ? C8 C9 1.539(9) . ? C8 C10 1.539(8) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.538(9) . ? C15 C16 1.541(9) . ? C15 C18 1.543(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.529(8) . ? C19 C22 1.531(9) . ? C19 C21 1.554(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? 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 N2 Os1 N1 176.2(2) . . ? N2 Os1 O3 102.0(3) . . ? N1 Os1 O3 81.4(3) . . ? N2 Os1 N3D 89.5(4) . . ? N1 Os1 N3D 94.0(3) . . ? O3 Os1 N3D 14.3(4) . . ? N2 Os1 P1 93.61(14) . . ? N1 Os1 P1 85.02(13) . . ? O3 Os1 P1 84.2(3) . . ? N3D Os1 P1 91.9(3) . . ? N2 Os1 P2 95.25(14) . . ? N1 Os1 P2 85.68(13) . . ? O3 Os1 P2 101.1(3) . . ? N3D Os1 P2 95.5(3) . . ? P1 Os1 P2 168.46(5) . . ? N2 Os1 H1OS 90.5 . . ? N1 Os1 H1OS 85.9 . . ? O3 Os1 H1OS 163.5 . . ? N3D Os1 H1OS 176.2 . . ? P1 Os1 H1OS 84.3 . . ? P2 Os1 H1OS 88.2 . . ? O2 N2 Os1 175.5(5) . . ? N3 O3 Os1 132.5(9) . . ? O4 N3 O3 111.3(10) . . ? O3D N3D Os1 114.3(8) . . ? C3 P1 C4 104.6(3) . . ? C3 P1 C8 107.4(3) . . ? C4 P1 C8 108.5(3) . . ? C3 P1 Os1 105.2(2) . . ? C4 P1 Os1 118.5(2) . . ? C8 P1 Os1 111.76(19) . . ? C14 P2 C15 104.3(3) . . ? C14 P2 C19 104.9(3) . . ? C15 P2 C19 110.7(3) . . ? C14 P2 Os1 103.57(19) . . ? C15 P2 Os1 117.4(2) . . ? C19 P2 Os1 114.4(2) . . ? N1 Si1 C1 114.1(3) . . ? N1 Si1 C2 114.2(3) . . ? C1 Si1 C2 103.0(3) . . ? N1 Si1 C3 106.6(2) . . ? C1 Si1 C3 111.3(3) . . ? C2 Si1 C3 107.6(3) . . ? N1 Si2 C13 114.1(3) . . ? N1 Si2 C14 107.2(2) . . ? C13 Si2 C14 105.1(3) . . ? N1 Si2 C12 113.5(3) . . ? C13 Si2 C12 106.4(3) . . ? C14 Si2 C12 110.3(3) . . ? Si2 N1 Si1 120.2(3) . . ? Si2 N1 Os1 118.8(3) . . ? Si1 N1 Os1 120.4(2) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 Si1 111.7(3) . . ? P1 C3 H3A 109.3 . . ? Si1 C3 H3A 109.3 . . ? P1 C3 H3B 109.3 . . ? Si1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C7 C4 C5 107.0(6) . . ? C7 C4 C6 107.8(5) . . ? C5 C4 C6 109.1(6) . . ? C7 C4 P1 109.0(5) . . ? C5 C4 P1 112.2(4) . . ? C6 C4 P1 111.6(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 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 C8 C9 108.5(5) . . ? C11 C8 C10 107.0(5) . . ? C9 C8 C10 110.3(5) . . ? C11 C8 P1 106.6(4) . . ? C9 C8 P1 110.3(4) . . ? C10 C8 P1 113.9(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 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C14 Si2 112.5(3) . . ? P2 C14 H14A 109.1 . . ? Si2 C14 H14A 109.1 . . ? P2 C14 H14B 109.1 . . ? Si2 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C17 C15 C16 108.2(6) . . ? C17 C15 C18 108.9(6) . . ? C16 C15 C18 108.9(6) . . ? C17 C15 P2 113.4(5) . . ? C16 C15 P2 111.7(5) . . ? C18 C15 P2 105.7(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 109.5(6) . . ? C20 C19 C21 109.2(5) . . ? C22 C19 C21 107.3(6) . . ? C20 C19 P2 111.3(4) . . ? C22 C19 P2 108.0(4) . . ? C21 C19 P2 111.5(5) . . ? 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 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Os1 N2 O2 -14(7) . . . . ? O3 Os1 N2 O2 140(5) . . . . ? N3D Os1 N2 O2 147(5) . . . . ? P1 Os1 N2 O2 55(5) . . . . ? P2 Os1 N2 O2 -118(5) . . . . ? N2 Os1 O3 N3 20.4(11) . . . . ? N1 Os1 O3 N3 -161.3(11) . . . . ? N3D Os1 O3 N3 -9.4(16) . . . . ? P1 Os1 O3 N3 112.9(11) . . . . ? P2 Os1 O3 N3 -77.4(11) . . . . ? Os1 O3 N3 O4 -3.4(16) . . . . ? N2 Os1 N3D O3D -154.4(9) . . . . ? N1 Os1 N3D O3D 24.3(9) . . . . ? O3 Os1 N3D O3D -3.5(15) . . . . ? P1 Os1 N3D O3D -60.8(9) . . . . ? P2 Os1 N3D O3D 110.4(9) . . . . ? N2 Os1 P1 C3 154.5(3) . . . . ? N1 Os1 P1 C3 -29.0(2) . . . . ? O3 Os1 P1 C3 52.8(3) . . . . ? N3D Os1 P1 C3 64.9(4) . . . . ? P2 Os1 P1 C3 -65.4(3) . . . . ? N2 Os1 P1 C4 38.1(3) . . . . ? N1 Os1 P1 C4 -145.4(3) . . . . ? O3 Os1 P1 C4 -63.6(4) . . . . ? N3D Os1 P1 C4 -51.6(4) . . . . ? P2 Os1 P1 C4 178.2(3) . . . . ? N2 Os1 P1 C8 -89.2(3) . . . . ? N1 Os1 P1 C8 87.3(2) . . . . ? O3 Os1 P1 C8 169.1(3) . . . . ? N3D Os1 P1 C8 -178.9(4) . . . . ? P2 Os1 P1 C8 50.9(3) . . . . ? N2 Os1 P2 C14 146.3(3) . . . . ? N1 Os1 P2 C14 -30.0(2) . . . . ? O3 Os1 P2 C14 -110.4(3) . . . . ? N3D Os1 P2 C14 -123.7(4) . . . . ? P1 Os1 P2 C14 6.3(3) . . . . ? N2 Os1 P2 C15 -99.5(3) . . . . ? N1 Os1 P2 C15 84.2(3) . . . . ? O3 Os1 P2 C15 3.9(4) . . . . ? N3D Os1 P2 C15 -9.4(4) . . . . ? P1 Os1 P2 C15 120.5(3) . . . . ? N2 Os1 P2 C19 32.7(3) . . . . ? N1 Os1 P2 C19 -143.6(2) . . . . ? O3 Os1 P2 C19 136.1(3) . . . . ? N3D Os1 P2 C19 122.8(4) . . . . ? P1 Os1 P2 C19 -107.3(3) . . . . ? C13 Si2 N1 Si1 -79.4(4) . . . . ? C14 Si2 N1 Si1 164.8(3) . . . . ? C12 Si2 N1 Si1 42.8(4) . . . . ? C13 Si2 N1 Os1 92.4(3) . . . . ? C14 Si2 N1 Os1 -23.5(4) . . . . ? C12 Si2 N1 Os1 -145.5(3) . . . . ? C1 Si1 N1 Si2 -87.3(4) . . . . ? C2 Si1 N1 Si2 30.8(4) . . . . ? C3 Si1 N1 Si2 149.4(3) . . . . ? C1 Si1 N1 Os1 101.1(4) . . . . ? C2 Si1 N1 Os1 -140.8(3) . . . . ? C3 Si1 N1 Os1 -22.2(3) . . . . ? N2 Os1 N1 Si2 -72(3) . . . . ? O3 Os1 N1 Si2 134.2(4) . . . . ? N3D Os1 N1 Si2 127.5(4) . . . . ? P1 Os1 N1 Si2 -140.9(3) . . . . ? P2 Os1 N1 Si2 32.2(3) . . . . ? N2 Os1 N1 Si1 99(3) . . . . ? O3 Os1 N1 Si1 -54.1(3) . . . . ? N3D Os1 N1 Si1 -60.8(4) . . . . ? P1 Os1 N1 Si1 30.8(2) . . . . ? P2 Os1 N1 Si1 -156.1(3) . . . . ? C4 P1 C3 Si1 149.1(3) . . . . ? C8 P1 C3 Si1 -95.6(3) . . . . ? Os1 P1 C3 Si1 23.5(3) . . . . ? N1 Si1 C3 P1 -4.8(4) . . . . ? C1 Si1 C3 P1 -129.8(3) . . . . ? C2 Si1 C3 P1 118.1(3) . . . . ? C3 P1 C4 C7 -77.8(5) . . . . ? C8 P1 C4 C7 167.8(4) . . . . ? Os1 P1 C4 C7 38.9(5) . . . . ? C3 P1 C4 C5 40.5(6) . . . . ? C8 P1 C4 C5 -74.0(6) . . . . ? Os1 P1 C4 C5 157.2(4) . . . . ? C3 P1 C4 C6 163.3(4) . . . . ? C8 P1 C4 C6 48.8(5) . . . . ? Os1 P1 C4 C6 -80.0(5) . . . . ? C3 P1 C8 C11 48.4(5) . . . . ? C4 P1 C8 C11 161.1(4) . . . . ? Os1 P1 C8 C11 -66.4(4) . . . . ? C3 P1 C8 C9 166.1(4) . . . . ? C4 P1 C8 C9 -81.3(5) . . . . ? Os1 P1 C8 C9 51.2(5) . . . . ? C3 P1 C8 C10 -69.3(5) . . . . ? C4 P1 C8 C10 43.3(6) . . . . ? Os1 P1 C8 C10 175.8(4) . . . . ? C15 P2 C14 Si2 -99.2(4) . . . . ? C19 P2 C14 Si2 144.3(3) . . . . ? Os1 P2 C14 Si2 24.1(4) . . . . ? N1 Si2 C14 P2 -4.5(4) . . . . ? C13 Si2 C14 P2 -126.2(4) . . . . ? C12 Si2 C14 P2 119.5(4) . . . . ? C14 P2 C15 C17 -59.7(6) . . . . ? C19 P2 C15 C17 52.7(6) . . . . ? Os1 P2 C15 C17 -173.5(5) . . . . ? C14 P2 C15 C16 177.8(5) . . . . ? C19 P2 C15 C16 -69.9(5) . . . . ? Os1 P2 C15 C16 64.0(6) . . . . ? C14 P2 C15 C18 59.6(5) . . . . ? C19 P2 C15 C18 171.9(4) . . . . ? Os1 P2 C15 C18 -54.3(5) . . . . ? C14 P2 C19 C20 166.6(5) . . . . ? C15 P2 C19 C20 54.6(5) . . . . ? Os1 P2 C19 C20 -80.7(5) . . . . ? C14 P2 C19 C22 -73.2(5) . . . . ? C15 P2 C19 C22 174.9(4) . . . . ? Os1 P2 C19 C22 39.6(5) . . . . ? C14 P2 C19 C21 44.4(5) . . . . ? C15 P2 C19 C21 -67.5(5) . . . . ? Os1 P2 C19 C21 157.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.602 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.095 #===END