Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_method Xtal3.6 _audit_creation_date 00-12-19 _audit_update_record ? _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_title ; Syntheses, structures and redox properties of some complexes containing the Os(dppe)Cp* fragment, including {Os(dppe)Cp*}2(?-C?CC?C). ; loop_ _publ_author_name 'Paul Low' 'M. Bruce' 'Karine Costuas' 'Thomas Davin' 'J. Halet' 'Kathy A. Kramarczuk' ; B.Nicholson ; 'Gary J. Perkins' 'Rachel L. Roberts' 'Brian W. Skelton' 'Mark E. Smith' 'Allan H. White' #===END data_br764 _database_code_depnum_ccdc_archive 'CCDC 282444' _audit_creation_method Xtal3.6 _audit_creation_date 00-10-01 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C36 H39 Br1 Os1 P2' _chemical_formula_moiety 'C36 H39 Br1 Os1 P2' _chemical_formula_weight 803.76 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.1670(10) _cell_length_b 17.764(2) _cell_length_c 16.792(2) _cell_angle_alpha 90.00000 _cell_angle_beta 109.387(2) _cell_angle_gamma 90.00000 _cell_volume 3142.2(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6085 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 26.4 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 5.456 _exptl_crystal_description prism _exptl_crystal_size_max .12 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour gold _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .59 _exptl_absorpt_correction_T_max .77 _diffrn_reflns_number 61533 _reflns_number_total 16020 _reflns_Friedel_coverage 0 _reflns_number_gt 10876 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .054 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .03 _refine_ls_wR_factor_ref .024 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_number_reflns 10876 _refine_ls_number_parameters 361 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .018 _refine_diff_density_min -1.062 _refine_diff_density_max 1.985 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 144 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 156 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 4 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' Os ? 0 4 -1.816 7.605 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Os .223468(8) .675672(5) .827760(6) .01570(3) Uani ? ? 1.00000 ? ? Br .23327(3) .535249(15) .869084(19) .03078(13) Uani ? ? 1.00000 ? ? P1 .43958(6) .66491(4) .88178(4) .0205(3) Uani ? ? 1.00000 ? ? C111 .5256(2) .59402(16) .84211(16) .0280(12) Uani ? ? 1.00000 ? ? C112 .6041(3) .53976(17) .8926(2) .0365(15) Uani ? ? 1.00000 ? ? C113 .6726(3) .49051(18) .8602(2) .0436(17) Uani ? ? 1.00000 ? ? C114 .6625(3) .4941(2) .7771(2) .0457(17) Uani ? ? 1.00000 ? ? C115 .5851(4) .5467(3) .7260(2) .070(2) Uani ? ? 1.00000 ? ? C116 .5165(4) .5960(2) .7588(2) .065(2) Uani ? ? 1.00000 ? ? C121 .5378(3) .74872(17) .88173(16) .0300(13) Uani ? ? 1.00000 ? ? C122 .4795(3) .81608(17) .85165(18) .0372(14) Uani ? ? 1.00000 ? ? C123 .5486(4) .8811(2) .8506(2) .060(2) Uani ? ? 1.00000 ? ? C124 .6766(5) .8788(3) .8805(3) .072(3) Uani ? ? 1.00000 ? ? C125 .7388(3) .8134(3) .9128(3) .070(3) Uani ? ? 1.00000 ? ? C126 .6708(3) .7459(2) .9133(2) .0491(18) Uani ? ? 1.00000 ? ? C1 .4843(2) .64237(16) .99527(16) .0272(12) Uani ? ? 1.00000 ? ? C2 .4128(2) .69406(15) 1.03637(15) .0256(11) Uani ? ? 1.00000 ? ? P2 .24897(6) .71269(4) .96229(4) .0177(3) Uani ? ? 1.00000 ? ? C211 .1462(2) .67426(15) 1.01835(15) .0229(10) Uani ? ? 1.00000 ? ? C212 .0506(3) .62375(15) .98047(18) .0292(12) Uani ? ? 1.00000 ? ? C213 -.0249(3) .59533(16) 1.0253(2) .0397(16) Uani ? ? 1.00000 ? ? C214 -.0042(3) .61707(18) 1.1073(2) .0432(17) Uani ? ? 1.00000 ? ? C215 .0896(3) .66875(18) 1.14525(19) .0387(15) Uani ? ? 1.00000 ? ? C216 .1649(3) .69686(16) 1.10106(17) .0322(13) Uani ? ? 1.00000 ? ? C221 .2292(2) .81379(13) .97885(14) .0205(10) Uani ? ? 1.00000 ? ? C222 .1141(3) .84232(15) .98031(18) .0292(12) Uani ? ? 1.00000 ? ? C223 .0922(3) .91890(18) .9803(2) .0418(16) Uani ? ? 1.00000 ? ? C224 .1875(3) .96900(16) .9812(2) .0406(15) Uani ? ? 1.00000 ? ? C225 .3041(3) .94210(16) .98359(18) .0342(14) Uani ? ? 1.00000 ? ? C226 .3245(3) .86544(15) .98181(16) .0268(12) Uani ? ? 1.00000 ? ? C01 .1315(3) .77281(16) .74562(16) .0317(13) Uani ? ? 1.00000 ? ? C011 .1445(4) .85670(18) .7549(2) .0510(17) Uani ? ? 1.00000 ? ? C02 .1910(2) .72518(15) .69993(15) .0267(12) Uani ? ? 1.00000 ? ? C021 .2821(3) .75137(19) .65757(17) .0396(16) Uani ? ? 1.00000 ? ? C03 .1331(2) .65303(15) .69022(15) .0246(11) Uani ? ? 1.00000 ? ? C031 .1569(3) .58710(17) .64158(17) .0361(14) Uani ? ? 1.00000 ? ? C04 .0332(2) .65662(17) .72818(16) .0296(12) Uani ? ? 1.00000 ? ? C041 -.0595(3) .5958(2) .7255(2) .0484(18) Uani ? ? 1.00000 ? ? C05 .0333(2) .72959(18) .76085(16) .0324(13) Uani ? ? 1.00000 ? ? C051 -.0642(3) .7598(2) .7970(2) .058(2) Uani ? ? 1.00000 ? ? H112 .61145 .53690 .95162 .04500 Uiso ? ? 1.00000 ? ? H113 .72747 .45343 .89662 .05500 Uiso ? ? 1.00000 ? ? H114 .70969 .46019 .75376 .05700 Uiso ? ? 1.00000 ? ? H115 .57584 .54793 .66722 .08600 Uiso ? ? 1.00000 ? ? H116 .46316 .63327 .72208 .08000 Uiso ? ? 1.00000 ? ? H122 .38814 .81823 .83115 .04800 Uiso ? ? 1.00000 ? ? H123 .50439 .92766 .82830 .08100 Uiso ? ? 1.00000 ? ? H124 .72408 .92341 .87946 .08300 Uiso ? ? 1.00000 ? ? H125 .82920 .81479 .93454 .08900 Uiso ? ? 1.00000 ? ? H126 .71566 .69883 .93574 .06400 Uiso ? ? 1.00000 ? ? H1a .46211 .59101 1.00175 .03400 Uiso ? ? 1.00000 ? ? H1b .57332 .64810 1.02170 .03400 Uiso ? ? 1.00000 ? ? H2a .45787 .74089 1.05081 .03200 Uiso ? ? 1.00000 ? ? H2b .40820 .67178 1.08695 .03200 Uiso ? ? 1.00000 ? ? H212 .03394 .60925 .92232 .03600 Uiso ? ? 1.00000 ? ? H213 -.09126 .56008 .99905 .05000 Uiso ? ? 1.00000 ? ? H214 -.05433 .59619 1.13845 .05200 Uiso ? ? 1.00000 ? ? H215 .10269 .68474 1.20185 .04700 Uiso ? ? 1.00000 ? ? H216 .23037 .73229 1.12804 .04000 Uiso ? ? 1.00000 ? ? H222 .04852 .80765 .98150 .03700 Uiso ? ? 1.00000 ? ? H223 .01024 .93781 .97771 .05100 Uiso ? ? 1.00000 ? ? H224 .17333 1.02229 .98060 .04900 Uiso ? ? 1.00000 ? ? H225 .37219 .97658 .98714 .04200 Uiso ? ? 1.00000 ? ? H226 .40598 .84718 .98242 .03200 Uiso ? ? 1.00000 ? ? H011a .07226 .87985 .71591 .07500 Uiso ? ? 1.00000 ? ? H011b .21830 .87145 .74020 .07500 Uiso ? ? 1.00000 ? ? H011c .15790 .87205 .81142 .07500 Uiso ? ? 1.00000 ? ? H021a .32737 .70905 .64456 .05900 Uiso ? ? 1.00000 ? ? H021b .34490 .78468 .69330 .05900 Uiso ? ? 1.00000 ? ? H021c .23995 .77695 .60642 .05900 Uiso ? ? 1.00000 ? ? H031a .20204 .60272 .60569 .05300 Uiso ? ? 1.00000 ? ? H031b .07761 .56529 .60781 .05300 Uiso ? ? 1.00000 ? ? H031c .20479 .54966 .67935 .05300 Uiso ? ? 1.00000 ? ? H041a -.13408 .60110 .67751 .06900 Uiso ? ? 1.00000 ? ? H041b -.02298 .54702 .72218 .06900 Uiso ? ? 1.00000 ? ? H041c -.08287 .59650 .77514 .06900 Uiso ? ? 1.00000 ? ? H051a -.09280 .71739 .82317 .08800 Uiso ? ? 1.00000 ? ? H051b -.02482 .79484 .84009 .08800 Uiso ? ? 1.00000 ? ? H051c -.13394 .78238 .75485 .08800 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os .01346(4) .01815(4) .01436(3) .00007(4) .00311(3) -.00176(4) Br .03826(15) .01872(12) .04129(16) -.00142(11) .02114(13) -.00023(11) P1 .0151(3) .0281(4) .0174(3) .0017(2) .0042(2) -.0006(2) C111 .0187(12) .0364(16) .0273(13) .0049(11) .0055(10) -.0050(11) C112 .0388(17) .0358(17) .0409(17) .0091(13) .0212(14) .0073(13) C113 .0402(18) .0356(17) .060(2) .0121(14) .0238(16) .0052(15) C114 .0314(16) .051(2) .056(2) .0097(15) .0167(15) -.0174(17) C115 .064(3) .113(4) .0316(18) .050(3) .0128(17) -.011(2) C116 .060(2) .101(3) .0277(16) .054(2) .0083(16) -.0020(18) C121 .0247(14) .0471(18) .0230(12) -.0137(12) .0141(10) -.0131(12) C122 .0504(18) .0358(17) .0318(14) -.0200(15) .0223(13) -.0098(13) C123 .095(3) .048(2) .054(2) -.040(2) .049(2) -.0221(17) C124 .092(4) .080(3) .069(3) -.055(3) .060(3) -.042(2) C125 .037(2) .126(4) .060(2) -.046(2) .0319(18) -.054(3) C126 .0259(16) .080(3) .0436(18) -.0145(16) .0152(14) -.0290(18) C1 .0214(12) .0367(15) .0203(12) .0082(11) .0025(10) .0023(11) C2 .0213(12) .0360(15) .0168(11) .0021(10) .0027(9) -.0006(10) P2 .0168(3) .0202(3) .0157(3) -.0005(2) .0050(2) -.0007(2) C211 .0248(12) .0221(11) .0249(11) .0012(11) .0126(9) .0041(11) C212 .0318(15) .0220(13) .0389(15) -.0027(11) .0187(12) -.0047(11) C213 .0422(18) .0238(15) .066(2) -.0065(13) .0359(17) -.0046(14) C214 .053(2) .0307(17) .065(2) .0038(15) .0451(18) .0093(15) C215 .0497(18) .0420(18) .0338(15) .0058(15) .0265(14) .0067(14) C216 .0354(15) .0404(17) .0237(13) -.0039(13) .0136(12) .0035(11) C221 .0231(11) .0219(13) .0161(10) -.0022(10) .0060(8) -.0026(9) C222 .0269(13) .0243(14) .0376(15) -.0020(10) .0121(12) -.0061(11) C223 .0414(18) .0318(16) .057(2) .0063(14) .0228(16) -.0076(15) C224 .058(2) .0209(14) .0419(17) -.0001(14) .0151(15) -.0074(13) C225 .0433(18) .0283(15) .0301(15) -.0121(13) .0109(13) -.0022(12) C226 .0287(14) .0294(14) .0227(12) -.0049(11) .0093(11) -.0013(10) C01 .0373(16) .0326(15) .0172(12) .0124(13) -.0016(11) .0005(10) C011 .071(2) .0343(17) .0305(16) .0179(17) -.0063(16) .0015(13) C02 .0266(13) .0332(15) .0166(11) .0044(11) .0021(10) .0037(10) C021 .0471(19) .047(2) .0244(15) -.0028(15) .0113(13) .0091(13) C03 .0178(11) .0366(15) .0175(11) .0020(10) .0033(9) -.0058(10) C031 .0362(16) .0436(18) .0261(14) .0037(14) .0070(12) -.0124(13) C04 .0172(12) .0485(18) .0194(11) -.0016(11) .0012(9) -.0082(11) C041 .0295(16) .078(3) .0365(17) -.0219(17) .0095(13) -.0258(17) C05 .0222(13) .0516(19) .0171(11) .0152(13) -.0020(10) -.0069(12) C051 .0367(18) .097(3) .0288(16) .036(2) -.0034(13) -.0178(18) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Os Br . . 2.5818(4) ? Os P1 . . 2.2870(6) ? Os P2 . . 2.2780(7) ? Os C01 . . 2.235(3) ? Os C02 . . 2.235(3) ? Os C03 . . 2.229(2) ? Os C04 . . 2.251(2) ? Os C05 . . 2.260(3) ? P1 C111 . . 1.838(3) ? P1 C121 . . 1.849(3) ? P1 C1 . . 1.846(3) ? C111 C112 . . 1.387(4) ? C111 C116 . . 1.369(5) ? C112 C113 . . 1.386(5) ? C112 H112 . . .968 ? C113 C114 . . 1.364(5) ? C113 H113 . . .966 ? C114 C115 . . 1.366(5) ? C114 H114 . . .965 ? C115 C116 . . 1.391(6) ? C115 H115 . . .958 ? C116 H116 . . .964 ? C121 C122 . . 1.376(4) ? C121 C126 . . 1.402(4) ? C122 C123 . . 1.392(5) ? C122 H122 . . .963 ? C123 C124 . . 1.349(7) ? C123 H123 . . .973 ? C124 C125 . . 1.370(7) ? C124 H124 . . .956 ? C125 C126 . . 1.422(6) ? C125 H125 . . .953 ? C126 H126 . . .983 ? C1 C2 . . 1.524(4) ? C1 H1a . . .961 ? C1 H1b . . .950 ? C2 P2 . . 1.869(2) ? C2 H2a . . .961 ? C2 H2b . . .954 ? P2 C211 . . 1.840(3) ? P2 C221 . . 1.842(2) ? C211 C212 . . 1.378(4) ? C211 C216 . . 1.393(4) ? C212 C213 . . 1.398(5) ? C212 H212 . . .966 ? C213 C214 . . 1.374(5) ? C213 H213 . . .959 ? C214 C215 . . 1.379(4) ? C214 H214 . . .959 ? C215 C216 . . 1.386(5) ? C215 H215 . . .956 ? C216 H216 . . .957 ? C221 C222 . . 1.389(4) ? C221 C226 . . 1.394(4) ? C222 C223 . . 1.382(4) ? C222 H222 . . .962 ? C223 C224 . . 1.383(5) ? C223 H223 . . .962 ? C224 C225 . . 1.375(5) ? C224 H224 . . .959 ? C225 C226 . . 1.383(4) ? C225 H225 . . .962 ? C226 H226 . . .962 ? C01 C011 . . 1.500(4) ? C01 C02 . . 1.444(4) ? C01 C05 . . 1.429(4) ? C011 H011a . . .948 ? C011 H011b . . .971 ? C011 H011c . . .950 ? C02 C021 . . 1.496(5) ? C02 C03 . . 1.420(4) ? C021 H021a . . .971 ? C021 H021b . . .961 ? C021 H021c . . .947 ? C03 C031 . . 1.501(4) ? C03 C04 . . 1.459(4) ? C031 H031a . . .946 ? C031 H031b . . .960 ? C031 H031c . . .952 ? C04 C041 . . 1.487(5) ? C04 C05 . . 1.407(4) ? C041 H041a . . .952 ? C041 H041b . . .967 ? C041 H041c . . .952 ? C05 C051 . . 1.509(5) ? C051 H051a . . .978 ? C051 H051b . . .946 ? C051 H051c . . .950 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br Os P1 . . . 82.395(17) ? Br Os P2 . . . 91.843(19) ? Br Os C01 . . . 151.84(7) ? Br Os C02 . . . 128.11(7) ? Br Os C03 . . . 93.92(7) ? Br Os C04 . . . 89.99(8) ? Br Os C05 . . . 119.49(8) ? P1 Os P2 . . . 82.11(2) ? P1 Os C01 . . . 121.18(8) ? P1 Os C02 . . . 103.14(7) ? P1 Os C03 . . . 116.81(7) ? P1 Os C04 . . . 153.35(8) ? P1 Os C05 . . . 157.90(8) ? P2 Os C01 . . . 105.64(7) ? P2 Os C02 . . . 139.98(7) ? P2 Os C03 . . . 160.80(7) ? P2 Os C04 . . . 123.81(8) ? P2 Os C05 . . . 99.10(7) ? C01 Os C02 . . . 37.70(11) ? C01 Os C03 . . . 62.78(10) ? C01 Os C04 . . . 61.99(10) ? C01 Os C05 . . . 37.08(11) ? C02 Os C03 . . . 37.10(10) ? C02 Os C04 . . . 62.20(10) ? C02 Os C05 . . . 61.94(11) ? C03 Os C04 . . . 38.01(11) ? C03 Os C05 . . . 62.22(10) ? C04 Os C05 . . . 36.36(11) ? Os P1 C111 . . . 121.56(8) ? Os P1 C121 . . . 118.72(9) ? Os P1 C1 . . . 108.41(9) ? C111 P1 C121 . . . 99.77(14) ? C111 P1 C1 . . . 103.33(13) ? C121 P1 C1 . . . 102.58(12) ? P1 C111 C112 . . . 123.7(2) ? P1 C111 C116 . . . 118.8(2) ? C112 C111 C116 . . . 117.4(3) ? C111 C112 C113 . . . 121.2(3) ? C111 C112 H112 . . . 119.0 ? C113 C112 H112 . . . 119.9 ? C112 C113 C114 . . . 120.2(3) ? C112 C113 H113 . . . 119.9 ? C114 C113 H113 . . . 119.9 ? C113 C114 C115 . . . 119.6(4) ? C113 C114 H114 . . . 121.1 ? C115 C114 H114 . . . 119.3 ? C114 C115 C116 . . . 119.9(3) ? C114 C115 H115 . . . 119.4 ? C116 C115 H115 . . . 120.6 ? C111 C116 C115 . . . 121.6(3) ? C111 C116 H116 . . . 119.5 ? C115 C116 H116 . . . 118.9 ? P1 C121 C122 . . . 119.4(2) ? P1 C121 C126 . . . 121.6(2) ? C122 C121 C126 . . . 118.9(3) ? C121 C122 C123 . . . 121.9(3) ? C121 C122 H122 . . . 118.8 ? C123 C122 H122 . . . 119.2 ? C122 C123 C124 . . . 119.6(4) ? C122 C123 H123 . . . 119.8 ? C124 C123 H123 . . . 120.5 ? C123 C124 C125 . . . 120.5(4) ? C123 C124 H124 . . . 119.6 ? C125 C124 H124 . . . 119.9 ? C124 C125 C126 . . . 121.1(4) ? C124 C125 H125 . . . 117.6 ? C126 C125 H125 . . . 121.3 ? C121 C126 C125 . . . 117.9(3) ? C121 C126 H126 . . . 121.1 ? C125 C126 H126 . . . 120.9 ? P1 C1 C2 . . . 109.50(17) ? P1 C1 H1a . . . 109.34 ? P1 C1 H1b . . . 110.0 ? C2 C1 H1a . . . 109.1 ? C2 C1 H1b . . . 110.4 ? H1a C1 H1b . . . 108.5 ? C1 C2 P2 . . . 110.46(15) ? C1 C2 H2a . . . 109.1 ? C1 C2 H2b . . . 110.2 ? P2 C2 H2a . . . 109.24 ? P2 C2 H2b . . . 109.6 ? H2a C2 H2b . . . 108.2 ? Os P2 C2 . . . 112.42(9) ? Os P2 C211 . . . 120.42(8) ? Os P2 C221 . . . 116.70(8) ? C2 P2 C211 . . . 103.46(11) ? C2 P2 C221 . . . 102.24(11) ? C211 P2 C221 . . . 99.10(12) ? P2 C211 C212 . . . 121.6(2) ? P2 C211 C216 . . . 119.4(2) ? C212 C211 C216 . . . 119.0(3) ? C211 C212 C213 . . . 120.0(3) ? C211 C212 H212 . . . 120.0 ? C213 C212 H212 . . . 120.0 ? C212 C213 C214 . . . 120.5(3) ? C212 C213 H213 . . . 120.1 ? C214 C213 H213 . . . 119.5 ? C213 C214 C215 . . . 120.0(4) ? C213 C214 H214 . . . 120.2 ? C215 C214 H214 . . . 119.8 ? C214 C215 C216 . . . 119.7(3) ? C214 C215 H215 . . . 120.0 ? C216 C215 H215 . . . 120.4 ? C211 C216 C215 . . . 120.9(3) ? C211 C216 H216 . . . 120.0 ? C215 C216 H216 . . . 119.2 ? P2 C221 C222 . . . 121.1(2) ? P2 C221 C226 . . . 121.3(2) ? C222 C221 C226 . . . 117.3(2) ? C221 C222 C223 . . . 121.6(3) ? C221 C222 H222 . . . 118.8 ? C223 C222 H222 . . . 119.6 ? C222 C223 C224 . . . 119.8(3) ? C222 C223 H223 . . . 120.6 ? C224 C223 H223 . . . 119.5 ? C223 C224 C225 . . . 119.6(3) ? C223 C224 H224 . . . 120.7 ? C225 C224 H224 . . . 119.6 ? C224 C225 C226 . . . 120.2(3) ? C224 C225 H225 . . . 120.1 ? C226 C225 H225 . . . 119.7 ? C221 C226 C225 . . . 121.3(3) ? C221 C226 H226 . . . 119.1 ? C225 C226 H226 . . . 119.6 ? Os C01 C011 . . . 133.93(17) ? Os C01 C02 . . . 71.16(15) ? Os C01 C05 . . . 72.40(16) ? C011 C01 C02 . . . 126.2(3) ? C011 C01 C05 . . . 124.7(3) ? C02 C01 C05 . . . 107.2(2) ? C01 C011 H011a . . . 109.2 ? C01 C011 H011b . . . 107.6 ? C01 C011 H011c . . . 111.5 ? H011a C011 H011b . . . 107.9 ? H011a C011 H011c . . . 112.4 ? H011b C011 H011c . . . 108.1 ? Os C02 C01 . . . 71.14(15) ? Os C02 C021 . . . 131.29(17) ? Os C02 C03 . . . 71.20(15) ? C01 C02 C021 . . . 125.2(3) ? C01 C02 C03 . . . 108.5(3) ? C021 C02 C03 . . . 125.5(3) ? C02 C021 H021a . . . 110.7 ? C02 C021 H021b . . . 111.4 ? C02 C021 H021c . . . 111.7 ? H021a C021 H021b . . . 106.9 ? H021a C021 H021c . . . 107.9 ? H021b C021 H021c . . . 108.1 ? Os C03 C02 . . . 71.70(14) ? Os C03 C031 . . . 127.14(17) ? Os C03 C04 . . . 71.83(14) ? C02 C03 C031 . . . 127.6(3) ? C02 C03 C04 . . . 107.2(2) ? C031 C03 C04 . . . 124.8(3) ? C03 C031 H031a . . . 110.2 ? C03 C031 H031b . . . 109.9 ? C03 C031 H031c . . . 110.1 ? H031a C031 H031b . . . 108.9 ? H031a C031 H031c . . . 109.2 ? H031b C031 H031c . . . 108.4 ? Os C04 C03 . . . 70.16(13) ? Os C04 C041 . . . 127.4(2) ? Os C04 C05 . . . 72.15(14) ? C03 C04 C041 . . . 125.5(3) ? C03 C04 C05 . . . 108.0(2) ? C041 C04 C05 . . . 126.3(3) ? C04 C041 H041a . . . 110.9 ? C04 C041 H041b . . . 110.5 ? C04 C041 H041c . . . 110.7 ? H041a C041 H041b . . . 107.9 ? H041a C041 H041c . . . 108.8 ? H041b C041 H041c . . . 107.9 ? Os C05 C01 . . . 70.52(15) ? Os C05 C04 . . . 71.49(15) ? Os C05 C051 . . . 129.42(18) ? C01 C05 C04 . . . 109.1(3) ? C01 C05 C051 . . . 125.4(3) ? C04 C05 C051 . . . 125.2(3) ? C05 C051 H051a . . . 107.1 ? C05 C051 H051b . . . 109.1 ? C05 C051 H051c . . . 111.9 ? H051a C051 H051b . . . 107.5 ? H051a C051 H051c . . . 110.5 ? H051b C051 H051c . . . 110.5 ? _exptl_crystal_F_000 1584 _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 30 _reflns_limit_l_min -28 _reflns_limit_l_max 26 _reflns_number_observed ? _reflns_d_resolution_high .584 _reflns_d_resolution_low 10.508 _diffrn_reflns_av_sigmaI/netI .108 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .062 _refine_ls_wR_factor_all .027 _refine_ls_goodness_of_fit_all .929 _refine_ls_shift/su_mean .001 #===END #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_br767 _database_code_depnum_ccdc_archive 'CCDC 617825' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C38 H42 F6 N Os P3' _chemical_formula_moiety 'C38 H42 N Os P2, F6 P' _chemical_formula_weight 909.87 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 11.4255(6) _cell_length_b 17.3798(8) _cell_length_c 19.1554(9) _cell_angle_alpha 90.00000 _cell_angle_beta 104.3830(10) _cell_angle_gamma 90.00000 _cell_volume 3684.5(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 36.8 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 3.65 _exptl_crystal_description prism _exptl_crystal_size_max .17 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .06 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .56 _exptl_absorpt_correction_T_max .80 _diffrn_reflns_number 76147 _reflns_number_total 19329 _reflns_Friedel_coverage 0 _reflns_number_gt 13760 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .044 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .027 _refine_ls_wR_factor_ref .024 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_number_reflns 13760 _refine_ls_number_parameters 442 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/(sig^2(F) + .0004F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .046 _refine_diff_density_min -1.085 _refine_diff_density_max 1.907 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 152 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 168 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 24 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 4 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 12 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Os ? 0 4 -1.816 7.605 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Os .073558(6) .520721(4) .763025(4) .01482(3) Uani ? ? 1.00000 ? ? P1 .02827(5) .62383(3) .68575(3) .0176(2) Uani ? ? 1.00000 ? ? C111 .13626(17) .63961(11) .63037(10) .0207(8) Uani ? ? 1.00000 ? ? C112 .1918(2) .71048(12) .62571(12) .0272(9) Uani ? ? 1.00000 ? ? C113 .2780(2) .71807(14) .58612(13) .0349(11) Uani ? ? 1.00000 ? ? C114 .3089(2) .65550(16) .55045(12) .0367(12) Uani ? ? 1.00000 ? ? C115 .2569(2) .58473(15) .55528(12) .0342(11) Uani ? ? 1.00000 ? ? C116 .1719(2) .57691(12) .59534(11) .0271(9) Uani ? ? 1.00000 ? ? C121 -.12004(18) .62986(11) .62172(11) .0219(8) Uani ? ? 1.00000 ? ? C122 -.13699(19) .61389(12) .54825(11) .0255(9) Uani ? ? 1.00000 ? ? C123 -.2515(2) .61844(13) .50195(12) .0316(10) Uani ? ? 1.00000 ? ? C124 -.3504(2) .63784(14) .52738(13) .0357(11) Uani ? ? 1.00000 ? ? C125 -.3355(2) .65344(14) .59995(14) .0349(11) Uani ? ? 1.00000 ? ? C126 -.2215(2) .64883(12) .64699(12) .0274(9) Uani ? ? 1.00000 ? ? C1 .03562(19) .71412(11) .73698(11) .0225(8) Uani ? ? 1.00000 ? ? C2 .14053(18) .70727(11) .80409(11) .0225(8) Uani ? ? 1.00000 ? ? P2 .11691(5) .61650(3) .84839(3) .0180(2) Uani ? ? 1.00000 ? ? C211 .24990(18) .60605(11) .92364(11) .0225(8) Uani ? ? 1.00000 ? ? C212 .3566(2) .64578(15) .92762(13) .0350(11) Uani ? ? 1.00000 ? ? C213 .4556(2) .63499(17) .98613(15) .0471(14) Uani ? ? 1.00000 ? ? C214 .4492(2) .58517(17) 1.04081(14) .0442(13) Uani ? ? 1.00000 ? ? C215 .3434(2) .54533(16) 1.03730(13) .0414(13) Uani ? ? 1.00000 ? ? C216 .2445(2) .55563(14) .97956(12) .0316(10) Uani ? ? 1.00000 ? ? C221 .00049(18) .64624(10) .89280(10) .0200(8) Uani ? ? 1.00000 ? ? C222 -.12023(19) .63026(11) .86022(11) .0234(8) Uani ? ? 1.00000 ? ? C223 -.2118(2) .65643(12) .89003(12) .0280(10) Uani ? ? 1.00000 ? ? C224 -.1835(2) .69891(13) .95281(12) .0298(10) Uani ? ? 1.00000 ? ? C225 -.0642(2) .71582(13) .98551(11) .0300(10) Uani ? ? 1.00000 ? ? C226 .02761(19) .69012(12) .95583(11) .0250(9) Uani ? ? 1.00000 ? ? N01 .24934(15) .53137(8) .76074(9) .0203(7) Uani ? ? 1.00000 ? ? C01 .3472(2) .53445(11) .75888(12) .0267(9) Uani ? ? 1.00000 ? ? C02 .4735(2) .53947(16) .75518(18) .0493(15) Uani ? ? 1.00000 ? ? C101 .09331(18) .40055(10) .80448(11) .0213(8) Uani ? ? 1.00000 ? ? C1011 .2033(2) .36738(12) .85550(13) .0321(10) Uani ? ? 1.00000 ? ? C102 -.00974(18) .43365(10) .82258(11) .0214(8) Uani ? ? 1.00000 ? ? C1021 -.0324(2) .43677(12) .89609(13) .0329(11) Uani ? ? 1.00000 ? ? C103 -.09652(18) .45348(11) .75696(12) .0231(8) Uani ? ? 1.00000 ? ? C1031 -.2271(2) .47344(13) .75062(15) .0365(11) Uani ? ? 1.00000 ? ? C104 -.04848(19) .42983(11) .69808(11) .0233(8) Uani ? ? 1.00000 ? ? C1041 -.1180(2) .42941(13) .62060(12) .0368(11) Uani ? ? 1.00000 ? ? C105 .06765(19) .39783(10) .72613(11) .0223(8) Uani ? ? 1.00000 ? ? C1051 .1469(2) .36236(12) .68343(13) .0345(11) Uani ? ? 1.00000 ? ? P .49093(6) .79503(3) .79371(4) .0329(3) Uani ? ? 1.00000 ? ? F1 .59575(15) .76763(10) .75811(10) .0618(11) Uani ? ? 1.00000 ? ? F2 .56216(16) .87221(9) .82162(11) .0671(11) Uani ? ? 1.00000 ? ? F3 .38619(13) .82103(8) .83059(9) .0471(8) Uani ? ? 1.00000 ? ? F4 .41928(14) .71720(8) .76722(9) .0516(9) Uani ? ? 1.00000 ? ? F5 .55579(15) .75320(10) .86770(9) .0615(10) Uani ? ? 1.00000 ? ? F6 .42458(17) .83688(11) .72168(9) .0651(11) Uani ? ? 1.00000 ? ? H112 .16867 .75437 .64968 .03400 Uiso ? ? 1.00000 ? ? H113 .31597 .76674 .58387 .04300 Uiso ? ? 1.00000 ? ? H114 .36784 .66040 .52234 .04600 Uiso ? ? 1.00000 ? ? H115 .27914 .54106 .53067 .04300 Uiso ? ? 1.00000 ? ? H116 .13566 .52771 .59851 .03300 Uiso ? ? 1.00000 ? ? H122 -.06946 .59912 .52953 .03200 Uiso ? ? 1.00000 ? ? H123 -.26153 .60866 .45134 .04100 Uiso ? ? 1.00000 ? ? H124 -.42959 .63977 .49500 .04500 Uiso ? ? 1.00000 ? ? H125 -.40409 .66798 .61755 .04400 Uiso ? ? 1.00000 ? ? H126 -.21232 .65874 .69754 .03500 Uiso ? ? 1.00000 ? ? H1a .04844 .75642 .70796 .02800 Uiso ? ? 1.00000 ? ? H1b -.03826 .72197 .75055 .02800 Uiso ? ? 1.00000 ? ? H2a .14142 .74949 .83577 .02800 Uiso ? ? 1.00000 ? ? H2b .21593 .70567 .79090 .02800 Uiso ? ? 1.00000 ? ? H212 .36199 .68106 .88984 .04400 Uiso ? ? 1.00000 ? ? H213 .52851 .66292 .98938 .05900 Uiso ? ? 1.00000 ? ? H214 .51766 .57731 1.08097 .05400 Uiso ? ? 1.00000 ? ? H215 .33838 .51074 1.07512 .05100 Uiso ? ? 1.00000 ? ? H216 .17201 .52701 .97754 .03900 Uiso ? ? 1.00000 ? ? H222 -.13981 .60056 .81639 .03000 Uiso ? ? 1.00000 ? ? H223 -.29482 .64528 .86695 .03500 Uiso ? ? 1.00000 ? ? H224 -.24676 .71683 .97350 .03600 Uiso ? ? 1.00000 ? ? H225 -.04432 .74537 1.02942 .03700 Uiso ? ? 1.00000 ? ? H226 .11038 .70247 .97810 .03100 Uiso ? ? 1.00000 ? ? H1011a .26870 .36620 .83271 .04700 Uiso ? ? 1.00000 ? ? H1011b .18669 .31629 .86813 .04700 Uiso ? ? 1.00000 ? ? H1011c .22583 .39817 .89786 .04700 Uiso ? ? 1.00000 ? ? H1021a .04037 .42427 .93183 .05000 Uiso ? ? 1.00000 ? ? H1021b -.09320 .40069 .89998 .05000 Uiso ? ? 1.00000 ? ? H1021c -.05723 .48694 .90588 .05000 Uiso ? ? 1.00000 ? ? H1031a -.25173 .51393 .71615 .05500 Uiso ? ? 1.00000 ? ? H1031b -.27697 .42982 .73529 .05500 Uiso ? ? 1.00000 ? ? H1031c -.23742 .49031 .79590 .05500 Uiso ? ? 1.00000 ? ? H1041a -.16818 .38492 .61077 .05500 Uiso ? ? 1.00000 ? ? H1041b -.16857 .47418 .61051 .05500 Uiso ? ? 1.00000 ? ? H1041c -.06449 .42967 .58979 .05500 Uiso ? ? 1.00000 ? ? H1051a .12588 .30983 .67412 .05200 Uiso ? ? 1.00000 ? ? H1051b .13610 .38889 .63850 .05200 Uiso ? ? 1.00000 ? ? H1051c .22957 .36630 .70919 .05200 Uiso ? ? 1.00000 ? ? H02a .50638 .58969 .76847 .07300 Uiso ? ? 1.00000 ? ? H02b .52304 .50255 .78563 .07300 Uiso ? ? 1.00000 ? ? H02c .47984 .52925 .70717 .07300 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os .01462(3) .01284(3) .01701(3) -.00034(3) .00394(2) -.00019(3) P1 .0169(2) .0153(2) .0198(2) -.00031(17) .00332(18) .00124(17) C111 .0169(9) .0251(9) .0190(9) -.0004(7) .0023(7) .0044(7) C112 .0245(10) .0287(10) .0281(11) -.0045(8) .0059(8) .0051(8) C113 .0261(12) .0439(13) .0347(13) -.0100(10) .0074(10) .0083(10) C114 .0235(11) .0610(16) .0264(11) -.0047(11) .0074(9) .0062(11) C115 .0302(12) .0469(14) .0263(11) .0030(10) .0086(9) -.0033(10) C116 .0278(11) .0306(10) .0241(10) -.0007(9) .0084(8) -.0007(8) C121 .0197(9) .0180(8) .0257(10) -.0005(7) .0014(8) .0056(7) C122 .0226(10) .0261(10) .0265(10) -.0019(8) .0037(8) .0026(8) C123 .0279(11) .0352(11) .0274(11) -.0063(9) -.0014(9) .0044(9) C124 .0210(11) .0432(13) .0376(13) -.0002(10) -.0027(9) .0113(11) C125 .0202(11) .0410(13) .0427(14) .0022(9) .0060(10) .0073(11) C126 .0228(10) .0288(10) .0296(11) .0003(8) .0050(8) .0044(8) C1 .0255(10) .0154(8) .0274(10) .0009(7) .0078(8) .0002(7) C2 .0243(10) .0167(8) .0259(10) -.0041(7) .0048(8) -.0029(7) P2 .0173(2) .0171(2) .0192(2) -.00111(18) .00390(18) -.00231(17) C211 .0203(9) .0243(9) .0224(9) .0012(7) .0040(7) -.0046(7) C212 .0243(11) .0456(13) .0332(12) -.0062(10) .0036(9) .0019(10) C213 .0228(12) .0661(18) .0478(16) -.0099(12) .0002(11) .0015(14) C214 .0261(12) .0645(18) .0354(14) .0019(12) -.0049(10) .0030(13) C215 .0349(14) .0524(15) .0314(13) .0034(12) -.0021(10) .0098(11) C216 .0254(11) .0358(12) .0305(11) -.0016(9) .0013(9) .0048(9) C221 .0215(9) .0181(8) .0209(9) .0022(7) .0063(7) .0003(7) C222 .0234(10) .0213(9) .0253(10) -.0000(7) .0056(8) -.0022(7) C223 .0213(10) .0262(10) .0370(12) .0020(8) .0081(9) .0010(9) C224 .0300(12) .0287(10) .0342(12) .0092(9) .0150(10) .0027(9) C225 .0366(13) .0299(10) .0226(10) .0089(9) .0056(9) -.0038(8) C226 .0242(10) .0262(9) .0228(10) .0037(8) .0021(8) -.0040(8) N01 .0213(8) .0175(7) .0214(8) .0010(6) .0042(6) .0007(6) C01 .0210(10) .0242(10) .0341(11) .0016(7) .0052(8) -.0004(8) C02 .0214(12) .0482(16) .081(2) .0012(11) .0182(13) -.0026(14) C101 .0241(10) .0129(7) .0268(10) -.0012(7) .0057(8) .0010(7) C1011 .0332(12) .0226(9) .0370(13) .0065(9) .0018(10) .0039(9) C102 .0245(10) .0156(8) .0263(10) -.0031(7) .0104(8) .0019(7) C1021 .0454(14) .0242(10) .0359(12) -.0032(10) .0227(11) .0026(9) C103 .0183(9) .0158(8) .0347(11) -.0032(7) .0056(8) .0010(8) C1031 .0189(10) .0255(10) .0640(17) -.0039(9) .0081(10) -.0034(11) C104 .0260(10) .0158(8) .0254(10) -.0042(7) .0013(8) -.0009(7) C1041 .0466(15) .0275(11) .0295(12) -.0121(10) -.0037(10) -.0018(9) C105 .0272(10) .0144(8) .0272(10) -.0023(7) .0104(8) -.0020(7) C1051 .0464(15) .0205(9) .0434(14) .0005(9) .0240(12) -.0062(9) P .0227(3) .0273(3) .0469(4) -.0011(2) .0049(3) .0022(3) F1 .0475(11) .0614(11) .0861(14) -.0042(8) .0343(10) -.0129(9) F2 .0614(12) .0490(10) .0972(14) -.0285(9) .0317(11) -.0239(10) F3 .0368(8) .0410(8) .0667(11) .0098(7) .0191(8) .0074(7) F4 .0469(10) .0339(8) .0735(11) -.0127(7) .0138(8) -.0075(8) F5 .0476(10) .0700(12) .0573(11) .0257(9) -.0048(8) .0077(9) F6 .0828(14) .0572(11) .0514(11) .0209(10) .0094(10) .0182(8) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Os P1 . . 2.2999(5) ? Os P2 . . 2.2996(5) ? Os N01 . . 2.0282(18) ? Os C101 . . 2.2258(18) ? Os C102 . . 2.244(2) ? Os C103 . . 2.246(2) ? Os C104 . . 2.2639(18) ? Os C105 . . 2.2454(18) ? P1 C111 . . 1.837(2) ? P1 C121 . . 1.8315(19) ? P1 C1 . . 1.842(2) ? C111 C112 . . 1.399(3) ? C111 C116 . . 1.392(3) ? C112 C113 . . 1.390(4) ? C112 H112 . . .961 ? C113 C114 . . 1.377(4) ? C113 H113 . . .957 ? C114 C115 . . 1.379(4) ? C114 H114 . . .964 ? C115 C116 . . 1.386(4) ? C115 H115 . . .960 ? C116 H116 . . .958 ? C121 C122 . . 1.400(3) ? C121 C126 . . 1.401(3) ? C122 C123 . . 1.389(3) ? C122 H122 . . .963 ? C123 C124 . . 1.379(4) ? C123 H123 . . .963 ? C124 C125 . . 1.385(4) ? C124 H124 . . .962 ? C125 C126 . . 1.390(3) ? C125 H125 . . .961 ? C126 H126 . . .963 ? C1 C2 . . 1.529(3) ? C1 H1a . . .955 ? C1 H1b . . .953 ? C2 P2 . . 1.843(2) ? C2 H2a . . .951 ? C2 H2b . . .957 ? P2 C211 . . 1.8252(18) ? P2 C221 . . 1.823(2) ? C211 C212 . . 1.387(3) ? C211 C216 . . 1.397(3) ? C212 C213 . . 1.393(3) ? C212 H212 . . .962 ? C213 C214 . . 1.375(4) ? C213 H213 . . .953 ? C214 C215 . . 1.380(4) ? C214 H214 . . .961 ? C215 C216 . . 1.382(3) ? C215 H215 . . .954 ? C216 H216 . . .958 ? C221 C222 . . 1.393(3) ? C221 C226 . . 1.396(3) ? C222 C223 . . 1.388(3) ? C222 H222 . . .963 ? C223 C224 . . 1.379(3) ? C223 H223 . . .961 ? C224 C225 . . 1.383(3) ? C224 H224 . . .959 ? C225 C226 . . 1.386(3) ? C225 H225 . . .963 ? C226 H226 . . .960 ? N01 C01 . . 1.128(3) ? C01 C02 . . 1.465(4) ? C02 H02a . . .959 ? C02 H02b . . .953 ? C02 H02c . . .957 ? C101 C1011 . . 1.502(3) ? C101 C102 . . 1.428(3) ? C101 C105 . . 1.457(3) ? C1011 H1011a . . .954 ? C1011 H1011b . . .952 ? C1011 H1011c . . .953 ? C102 C1021 . . 1.495(3) ? C102 C103 . . 1.436(3) ? C1021 H1021a . . .961 ? C1021 H1021b . . .953 ? C1021 H1021c . . .950 ? C103 C1031 . . 1.507(3) ? C103 C104 . . 1.432(3) ? C1031 H1031a . . .958 ? C1031 H1031b . . .950 ? C1031 H1031c . . .950 ? C104 C1041 . . 1.499(3) ? C104 C105 . . 1.416(3) ? C1041 H1041a . . .953 ? C1041 H1041b . . .960 ? C1041 H1041c . . .949 ? C105 C1051 . . 1.496(4) ? C1051 H1051a . . .950 ? C1051 H1051b . . .957 ? C1051 H1051c . . .953 ? P F1 . . 1.591(2) ? P F2 . . 1.5910(18) ? P F3 . . 1.5985(19) ? P F4 . . 1.5972(16) ? P F5 . . 1.6015(18) ? P F6 . . 1.5773(17) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 Os P2 . . . 82.410(18) ? P1 Os N01 . . . 88.89(4) ? P1 Os C101 . . . 161.33(5) ? P1 Os C102 . . . 142.80(5) ? P1 Os C103 . . . 108.59(5) ? P1 Os C104 . . . 100.41(5) ? P1 Os C105 . . . 123.65(5) ? P2 Os N01 . . . 84.82(4) ? P2 Os C101 . . . 116.15(5) ? P2 Os C102 . . . 99.80(5) ? P2 Os C103 . . . 116.37(6) ? P2 Os C104 . . . 152.91(6) ? P2 Os C105 . . . 153.73(5) ? N01 Os C101 . . . 94.59(7) ? N01 Os C102 . . . 128.30(6) ? N01 Os C103 . . . 153.53(7) ? N01 Os C104 . . . 121.99(7) ? N01 Os C105 . . . 91.86(7) ? C101 Os C102 . . . 37.27(8) ? C101 Os C103 . . . 62.61(7) ? C101 Os C104 . . . 62.31(7) ? C101 Os C105 . . . 38.02(7) ? C102 Os C103 . . . 37.31(7) ? C102 Os C104 . . . 61.82(7) ? C102 Os C105 . . . 62.31(8) ? C103 Os C104 . . . 37.02(8) ? C103 Os C105 . . . 62.02(8) ? C104 Os C105 . . . 36.59(7) ? Os P1 C111 . . . 114.34(6) ? Os P1 C121 . . . 119.89(7) ? Os P1 C1 . . . 110.35(7) ? C111 P1 C121 . . . 104.31(9) ? C111 P1 C1 . . . 103.43(10) ? C121 P1 C1 . . . 102.72(9) ? P1 C111 C112 . . . 123.31(16) ? P1 C111 C116 . . . 118.69(16) ? C112 C111 C116 . . . 117.8(2) ? C111 C112 C113 . . . 120.8(2) ? C111 C112 H112 . . . 119.0 ? C113 C112 H112 . . . 120.1 ? C112 C113 C114 . . . 120.0(2) ? C112 C113 H113 . . . 120.0 ? C114 C113 H113 . . . 120.1 ? C113 C114 C115 . . . 120.2(2) ? C113 C114 H114 . . . 120.6 ? C115 C114 H114 . . . 119.2 ? C114 C115 C116 . . . 119.8(2) ? C114 C115 H115 . . . 120.1 ? C116 C115 H115 . . . 120.1 ? C111 C116 C115 . . . 121.3(2) ? C111 C116 H116 . . . 119.0 ? C115 C116 H116 . . . 119.7 ? P1 C121 C122 . . . 122.40(17) ? P1 C121 C126 . . . 119.27(15) ? C122 C121 C126 . . . 118.30(17) ? C121 C122 C123 . . . 120.3(2) ? C121 C122 H122 . . . 120.24 ? C123 C122 H122 . . . 119.5 ? C122 C123 C124 . . . 120.9(2) ? C122 C123 H123 . . . 119.4 ? C124 C123 H123 . . . 119.8 ? C123 C124 C125 . . . 119.7(2) ? C123 C124 H124 . . . 120.2 ? C125 C124 H124 . . . 120.1 ? C124 C125 C126 . . . 120.1(2) ? C124 C125 H125 . . . 119.7 ? C126 C125 H125 . . . 120.2 ? C121 C126 C125 . . . 120.8(2) ? C121 C126 H126 . . . 119.8 ? C125 C126 H126 . . . 119.4 ? P1 C1 C2 . . . 107.71(13) ? P1 C1 H1a . . . 109.82 ? P1 C1 H1b . . . 109.95 ? C2 C1 H1a . . . 110.36 ? C2 C1 H1b . . . 110.1 ? H1a C1 H1b . . . 108.85 ? C1 C2 P2 . . . 106.25(13) ? C1 C2 H2a . . . 111.01 ? C1 C2 H2b . . . 110.5 ? P2 C2 H2a . . . 110.27 ? P2 C2 H2b . . . 109.95 ? H2a C2 H2b . . . 108.88 ? Os P2 C2 . . . 108.82(7) ? Os P2 C211 . . . 118.66(7) ? Os P2 C221 . . . 118.94(6) ? C2 P2 C211 . . . 105.10(9) ? C2 P2 C221 . . . 100.34(9) ? C211 P2 C221 . . . 102.74(9) ? P2 C211 C212 . . . 122.82(16) ? P2 C211 C216 . . . 118.76(16) ? C212 C211 C216 . . . 118.42(18) ? C211 C212 C213 . . . 120.3(2) ? C211 C212 H212 . . . 119.7 ? C213 C212 H212 . . . 120.0 ? C212 C213 C214 . . . 120.8(2) ? C212 C213 H213 . . . 120.4 ? C214 C213 H213 . . . 118.8 ? C213 C214 C215 . . . 119.4(2) ? C213 C214 H214 . . . 120.8 ? C215 C214 H214 . . . 119.8 ? C214 C215 C216 . . . 120.4(2) ? C214 C215 H215 . . . 119.7 ? C216 C215 H215 . . . 119.9 ? C211 C216 C215 . . . 120.8(2) ? C211 C216 H216 . . . 119.8 ? C215 C216 H216 . . . 119.4 ? P2 C221 C222 . . . 119.37(15) ? P2 C221 C226 . . . 121.83(15) ? C222 C221 C226 . . . 118.6(2) ? C221 C222 C223 . . . 120.95(19) ? C221 C222 H222 . . . 119.1 ? C223 C222 H222 . . . 119.9 ? C222 C223 C224 . . . 119.8(2) ? C222 C223 H223 . . . 120.2 ? C224 C223 H223 . . . 120.0 ? C223 C224 C225 . . . 120.0(2) ? C223 C224 H224 . . . 119.8 ? C225 C224 H224 . . . 120.2 ? C224 C225 C226 . . . 120.5(2) ? C224 C225 H225 . . . 120.1 ? C226 C225 H225 . . . 119.4 ? C221 C226 C225 . . . 120.19(19) ? C221 C226 H226 . . . 119.3 ? C225 C226 H226 . . . 120.5 ? Os N01 C01 . . . 177.42(15) ? N01 C01 C02 . . . 178.8(2) ? C01 C02 H02a . . . 111.5 ? C01 C02 H02b . . . 111.9 ? C01 C02 H02c . . . 110.3 ? H02a C02 H02b . . . 108.4 ? H02a C02 H02c . . . 107.8 ? H02b C02 H02c . . . 106.7 ? Os C101 C1011 . . . 125.90(14) ? Os C101 C102 . . . 72.07(11) ? Os C101 C105 . . . 71.72(10) ? C1011 C101 C102 . . . 127.1(2) ? C1011 C101 C105 . . . 125.4(2) ? C102 C101 C105 . . . 107.22(16) ? C101 C1011 H1011a . . . 109.5 ? C101 C1011 H1011b . . . 109.6 ? C101 C1011 H1011c . . . 110.1 ? H1011a C1011 H1011b . . . 108.9 ? H1011a C1011 H1011c . . . 109.0 ? H1011b C1011 H1011c . . . 109.6 ? Os C102 C101 . . . 70.66(12) ? Os C102 C1021 . . . 130.47(14) ? Os C102 C103 . . . 71.40(12) ? C101 C102 C1021 . . . 126.11(17) ? C101 C102 C103 . . . 108.40(19) ? C1021 C102 C103 . . . 124.9(2) ? C102 C1021 H1021a . . . 110.0 ? C102 C1021 H1021b . . . 110.5 ? C102 C1021 H1021c . . . 110.4 ? H1021a C1021 H1021b . . . 108.3 ? H1021a C1021 H1021c . . . 108.3 ? H1021b C1021 H1021c . . . 109.2 ? Os C103 C102 . . . 71.29(11) ? Os C103 C1031 . . . 135.32(14) ? Os C103 C104 . . . 72.18(12) ? C102 C103 C1031 . . . 125.5(2) ? C102 C103 C104 . . . 107.70(17) ? C1031 C103 C104 . . . 124.62(19) ? C103 C1031 H1031a . . . 109.9 ? C103 C1031 H1031b . . . 110.3 ? C103 C1031 H1031c . . . 110.0 ? H1031a C1031 H1031b . . . 108.8 ? H1031a C1031 H1031c . . . 108.7 ? H1031b C1031 H1031c . . . 109.1 ? Os C104 C103 . . . 70.80(11) ? Os C104 C1041 . . . 130.53(15) ? Os C104 C105 . . . 70.99(11) ? C103 C104 C1041 . . . 124.7(2) ? C103 C104 C105 . . . 108.69(17) ? C1041 C104 C105 . . . 126.1(2) ? C104 C1041 H1041a . . . 110.1 ? C104 C1041 H1041b . . . 109.9 ? C104 C1041 H1041c . . . 110.5 ? H1041a C1041 H1041b . . . 108.4 ? H1041a C1041 H1041c . . . 109.2 ? H1041b C1041 H1041c . . . 108.6 ? Os C105 C101 . . . 70.26(10) ? Os C105 C104 . . . 72.41(11) ? Os C105 C1051 . . . 126.10(15) ? C101 C105 C104 . . . 107.9(2) ? C101 C105 C1051 . . . 125.63(18) ? C104 C105 C1051 . . . 126.30(19) ? C105 C1051 H1051a . . . 109.9 ? C105 C1051 H1051b . . . 109.4 ? C105 C1051 H1051c . . . 110.1 ? H1051a C1051 H1051b . . . 108.9 ? H1051a C1051 H1051c . . . 109.8 ? H1051b C1051 H1051c . . . 108.7 ? F1 P F2 . . . 91.13(11) ? F1 P F3 . . . 178.79(11) ? F1 P F4 . . . 89.50(10) ? F1 P F5 . . . 90.65(10) ? F1 P F6 . . . 90.71(11) ? F2 P F3 . . . 89.42(10) ? F2 P F4 . . . 178.91(11) ? F2 P F5 . . . 89.98(9) ? F2 P F6 . . . 89.99(10) ? F3 P F4 . . . 89.94(9) ? F3 P F5 . . . 88.27(9) ? F3 P F6 . . . 90.37(10) ? F4 P F5 . . . 89.12(9) ? F4 P F6 . . . 90.89(9) ? F5 P F6 . . . 178.64(11) ? _exptl_crystal_F_000 1808 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 29 _reflns_limit_l_min -32 _reflns_limit_l_max 31 _reflns_number_observed ? _reflns_d_resolution_high .582 _reflns_d_resolution_low 11.043 _diffrn_reflns_av_sigmaI/netI .088 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .054 _refine_ls_wR_factor_all .026 _refine_ls_goodness_of_fit_all .962 _refine_ls_shift/su_mean .001 #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_br770 _database_code_depnum_ccdc_archive 'CCDC 617826' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C45.5 H45.5 Os P2' _chemical_formula_moiety 'C44 H44 Os P2, 1/4(C6 H6)' _chemical_formula_weight 844.51 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 11.9922(6) _cell_length_b 17.8922(8) _cell_length_c 19.8242(9) _cell_angle_alpha 114.7640(10) _cell_angle_beta 90.6820(10) _cell_angle_gamma 103.1450(10) _cell_volume 3733.5(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6269 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 36.5 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 3.532 _exptl_crystal_description plate _exptl_crystal_size_max .24 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .59 _exptl_absorpt_correction_T_max .83 _diffrn_reflns_number 77398 _reflns_number_total 38378 _reflns_Friedel_coverage 0 _reflns_number_gt 23364 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .049 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .038 _refine_ls_wR_factor_ref .024 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_number_reflns 23364 _refine_ls_number_parameters 875 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .037 _refine_diff_density_min -3.001 _refine_diff_density_max 2.977 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics 'xtal PIG' _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 182 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 182 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Os ? 0 4 -1.816 7.605 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Os1 .828597(10) .726457(7) .461137(6) .01397(4) Uani ? ? 1.00000 ? ? Os2 .467946(10) .753154(7) .977366(6) .01503(4) Uani ? ? 1.00000 ? ? P11 1.00223(6) .81460(5) .52141(4) .0163(3) Uani ? ? 1.00000 ? ? C1111 1.1292(2) .79458(17) .47443(15) .0181(11) Uani ? ? 1.00000 ? ? C1112 1.1702(2) .82932(18) .42525(16) .0212(12) Uani ? ? 1.00000 ? ? C1113 1.2661(3) .81173(19) .38921(16) .0253(13) Uani ? ? 1.00000 ? ? C1114 1.3222(2) .7577(2) .39985(16) .0259(13) Uani ? ? 1.00000 ? ? C1115 1.2830(3) .7211(2) .44675(18) .0288(14) Uani ? ? 1.00000 ? ? C1116 1.1880(2) .73950(19) .48338(17) .0247(13) Uani ? ? 1.00000 ? ? C1121 1.0534(2) .83140(17) .61615(15) .0175(11) Uani ? ? 1.00000 ? ? C1122 .9792(2) .79964(18) .65618(16) .0232(12) Uani ? ? 1.00000 ? ? C1123 1.0163(3) .8125(2) .72829(17) .0333(15) Uani ? ? 1.00000 ? ? C1124 1.1277(3) .8561(2) .75949(17) .0348(15) Uani ? ? 1.00000 ? ? C1125 1.2027(3) .8883(2) .72066(17) .0322(14) Uani ? ? 1.00000 ? ? C1126 1.1661(3) .87719(18) .64939(17) .0261(13) Uani ? ? 1.00000 ? ? C110 1.0012(2) .92378(17) .53703(16) .0188(11) Uani ? ? 1.00000 ? ? C120 .8896(2) .94100(17) .56911(16) .0204(12) Uani ? ? 1.00000 ? ? P12 .76637(6) .84650(5) .51815(4) .0161(3) Uani ? ? 1.00000 ? ? C1211 .6876(2) .87950(18) .45941(15) .0177(11) Uani ? ? 1.00000 ? ? C1212 .6482(2) .82413(18) .38427(16) .0213(12) Uani ? ? 1.00000 ? ? C1213 .5906(3) .8493(2) .33944(17) .0270(13) Uani ? ? 1.00000 ? ? C1214 .5720(3) .9291(2) .36811(18) .0310(15) Uani ? ? 1.00000 ? ? C1215 .6097(3) .9850(2) .44261(18) .0311(15) Uani ? ? 1.00000 ? ? C1216 .6668(3) .96001(19) .48800(17) .0249(13) Uani ? ? 1.00000 ? ? C1221 .6696(2) .85224(17) .59055(15) .0179(11) Uani ? ? 1.00000 ? ? C1222 .7130(3) .8657(2) .66144(17) .0264(13) Uani ? ? 1.00000 ? ? C1223 .6389(3) .8630(2) .71460(17) .0343(15) Uani ? ? 1.00000 ? ? C1224 .5220(3) .8458(2) .69780(18) .0349(15) Uani ? ? 1.00000 ? ? C1225 .4780(3) .8328(2) .62772(18) .0323(14) Uani ? ? 1.00000 ? ? C1226 .5506(2) .83642(18) .57476(16) .0238(12) Uani ? ? 1.00000 ? ? C11 .8786(2) .76927(17) .38365(15) .0178(11) Uani ? ? 1.00000 ? ? C12 .9085(2) .79734(18) .33944(16) .0220(12) Uani ? ? 1.00000 ? ? C121 .9545(2) .83705(18) .29208(15) .0203(11) Uani ? ? 1.00000 ? ? C122 .9009(3) .89177(19) .27733(16) .0255(13) Uani ? ? 1.00000 ? ? C123 .9471(3) .9299(2) .23225(19) .0386(17) Uani ? ? 1.00000 ? ? C124 1.0456(3) .9144(2) .2010(2) .0485(19) Uani ? ? 1.00000 ? ? C125 1.0986(3) .8595(2) .2140(2) .0436(18) Uani ? ? 1.00000 ? ? C126 1.0537(3) .8213(2) .25862(17) .0292(14) Uani ? ? 1.00000 ? ? C101 .8342(2) .59138(17) .39397(16) .0213(12) Uani ? ? 1.00000 ? ? C1011 .9224(3) .5610(2) .3422(2) .0374(15) Uani ? ? 1.00000 ? ? C102 .8379(2) .60717(17) .47110(17) .0225(12) Uani ? ? 1.00000 ? ? C1021 .9284(3) .5923(2) .5138(2) .0346(15) Uani ? ? 1.00000 ? ? C103 .7332(2) .62679(17) .49701(15) .0204(11) Uani ? ? 1.00000 ? ? C1031 .6917(3) .6341(2) .57013(17) .0321(14) Uani ? ? 1.00000 ? ? C104 .6633(2) .62223(17) .43589(16) .0178(11) Uani ? ? 1.00000 ? ? C1041 .5410(3) .6270(2) .43419(18) .0280(13) Uani ? ? 1.00000 ? ? C105 .7256(2) .60040(17) .37216(15) .0209(11) Uani ? ? 1.00000 ? ? C1051 .6816(3) .5815(2) .29364(17) .0309(14) Uani ? ? 1.00000 ? ? P21 .30276(7) .66015(5) .97561(4) .0174(3) Uani ? ? 1.00000 ? ? C2111 .1677(2) .66733(18) .93763(16) .0208(12) Uani ? ? 1.00000 ? ? C2112 .1261(3) .6229(2) .86137(17) .0320(14) Uani ? ? 1.00000 ? ? C2113 .0266(3) .6350(2) .83469(19) .0429(17) Uani ? ? 1.00000 ? ? C2114 -.0320(3) .6884(2) .8823(2) .0423(17) Uani ? ? 1.00000 ? ? C2115 .0077(3) .7320(2) .9574(2) .0335(15) Uani ? ? 1.00000 ? ? C2116 .1065(3) .7213(2) .98477(17) .0279(13) Uani ? ? 1.00000 ? ? C2121 .2565(2) .65003(18) 1.06012(16) .0201(12) Uani ? ? 1.00000 ? ? C2122 .3241(3) .69879(18) 1.12880(16) .0240(13) Uani ? ? 1.00000 ? ? C2123 .2906(3) .6910(2) 1.19297(17) .0318(15) Uani ? ? 1.00000 ? ? C2124 .1900(3) .6344(2) 1.18962(18) .0321(15) Uani ? ? 1.00000 ? ? C2125 .1221(3) .5836(2) 1.1209(2) .0360(16) Uani ? ? 1.00000 ? ? C2126 .1554(3) .5913(2) 1.05721(17) .0280(13) Uani ? ? 1.00000 ? ? C210 .3152(2) .55218(17) .91704(16) .0227(12) Uani ? ? 1.00000 ? ? C220 .4318(3) .54602(18) .94245(17) .0253(13) Uani ? ? 1.00000 ? ? P22 .54451(7) .64017(5) .95129(4) .0187(3) Uani ? ? 1.00000 ? ? C2211 .6102(2) .60157(19) .86297(16) .0234(12) Uani ? ? 1.00000 ? ? C2212 .6461(3) .6565(2) .83044(17) .0267(13) Uani ? ? 1.00000 ? ? C2213 .6953(3) .6316(2) .76371(18) .0347(15) Uani ? ? 1.00000 ? ? C2214 .7067(3) .5501(2) .72815(18) .0425(17) Uani ? ? 1.00000 ? ? C2215 .6720(3) .4936(2) .75944(18) .0442(17) Uani ? ? 1.00000 ? ? C2216 .6244(3) .5189(2) .82675(18) .0333(15) Uani ? ? 1.00000 ? ? C2221 .6560(3) .64748(17) 1.02015(16) .0219(12) Uani ? ? 1.00000 ? ? C2222 .6321(3) .6738(2) 1.09447(17) .0274(13) Uani ? ? 1.00000 ? ? C2223 .7131(3) .6831(2) 1.14930(17) .0320(15) Uani ? ? 1.00000 ? ? C2224 .8188(3) .66659(19) 1.13191(18) .0324(14) Uani ? ? 1.00000 ? ? C2225 .8431(3) .6417(2) 1.05956(19) .0322(14) Uani ? ? 1.00000 ? ? C2226 .7620(3) .6312(2) 1.00323(17) .0262(13) Uani ? ? 1.00000 ? ? C21 .4126(2) .70204(17) .86740(15) .0181(11) Uani ? ? 1.00000 ? ? C22 .3828(2) .67825(18) .80174(16) .0207(12) Uani ? ? 1.00000 ? ? C221 .3463(2) .65485(17) .72472(15) .0199(11) Uani ? ? 1.00000 ? ? C222 .4048(3) .61064(18) .66690(17) .0246(13) Uani ? ? 1.00000 ? ? C223 .3690(3) .59068(19) .59312(16) .0292(14) Uani ? ? 1.00000 ? ? C224 .2741(3) .6133(2) .57592(17) .0321(14) Uani ? ? 1.00000 ? ? C225 .2151(3) .6569(2) .63231(18) .0359(16) Uani ? ? 1.00000 ? ? C226 .2501(3) .6771(2) .70573(17) .0289(14) Uani ? ? 1.00000 ? ? C201 .4535(3) .88074(17) .99129(16) .0218(12) Uani ? ? 1.00000 ? ? C2011 .3648(3) .8949(2) .94687(18) .0311(14) Uani ? ? 1.00000 ? ? C202 .4477(3) .87976(17) 1.06289(16) .0229(12) Uani ? ? 1.00000 ? ? C2021 .3526(3) .89839(19) 1.11108(18) .0321(15) Uani ? ? 1.00000 ? ? C203 .5545(3) .86866(17) 1.08640(16) .0229(12) Uani ? ? 1.00000 ? ? C2031 .5920(3) .8797(2) 1.16327(17) .0339(14) Uani ? ? 1.00000 ? ? C204 .6281(2) .86363(17) 1.02860(16) .0233(12) Uani ? ? 1.00000 ? ? C2041 .7510(3) .8601(2) 1.03371(18) .0321(14) Uani ? ? 1.00000 ? ? C205 .5663(3) .87156(17) .97039(16) .0227(12) Uani ? ? 1.00000 ? ? C2051 .6132(3) .8787(2) .90310(17) .0322(15) Uani ? ? 1.00000 ? ? C01 .9711(3) .0722(2) .0487(2) .0432(18) Uani ? ? 1.00000 ? ? C02 1.0424(3) .0371(2) .0746(2) .0410(17) Uani ? ? 1.00000 ? ? C03 1.0708(3) -.0346(2) .0258(2) .0442(19) Uani ? ? 1.00000 ? ? H1112 1.13057 .86614 .41662 .02700 Uiso ? ? 1.00000 ? ? H1113 1.29393 .83735 .35657 .03300 Uiso ? ? 1.00000 ? ? H1114 1.38815 .74488 .37472 .03300 Uiso ? ? 1.00000 ? ? H1115 1.32142 .68289 .45442 .03700 Uiso ? ? 1.00000 ? ? H1116 1.16122 .71411 .51671 .03200 Uiso ? ? 1.00000 ? ? H1122 .90169 .76815 .63385 .02900 Uiso ? ? 1.00000 ? ? H1123 .96356 .79062 .75595 .04200 Uiso ? ? 1.00000 ? ? H1124 1.15485 .86366 .80854 .04400 Uiso ? ? 1.00000 ? ? H1125 1.28108 .91875 .74243 .04100 Uiso ? ? 1.00000 ? ? H1126 1.21867 .90063 .62287 .03400 Uiso ? ? 1.00000 ? ? H110a 1.06724 .96353 .57069 .02400 Uiso ? ? 1.00000 ? ? H110b 1.00444 .92808 .49050 .02400 Uiso ? ? 1.00000 ? ? H120a .87589 .98923 .56475 .02500 Uiso ? ? 1.00000 ? ? H120b .89765 .95304 .62101 .02500 Uiso ? ? 1.00000 ? ? H1212 .66136 .76841 .36425 .02800 Uiso ? ? 1.00000 ? ? H1213 .56311 .81003 .28795 .03500 Uiso ? ? 1.00000 ? ? H1214 .53320 .94634 .33641 .03900 Uiso ? ? 1.00000 ? ? H1215 .59727 1.04137 .46308 .04000 Uiso ? ? 1.00000 ? ? H1216 .69148 .99848 .53978 .03100 Uiso ? ? 1.00000 ? ? H1222 .79474 .87761 .67393 .03300 Uiso ? ? 1.00000 ? ? H1223 .67106 .87458 .76364 .04300 Uiso ? ? 1.00000 ? ? H1224 .47167 .84218 .73417 .04300 Uiso ? ? 1.00000 ? ? H1225 .39534 .82073 .61558 .04100 Uiso ? ? 1.00000 ? ? H1226 .51913 .82836 .52674 .03100 Uiso ? ? 1.00000 ? ? H122 .83144 .90264 .29850 .03300 Uiso ? ? 1.00000 ? ? H123 .90966 .96801 .22327 .04900 Uiso ? ? 1.00000 ? ? H124 1.07752 .94082 .16954 .06100 Uiso ? ? 1.00000 ? ? H125 1.16781 .84804 .19129 .05600 Uiso ? ? 1.00000 ? ? H126 1.09057 .78296 .26699 .03800 Uiso ? ? 1.00000 ? ? H1011a .99336 .57448 .37189 .05800 Uiso ? ? 1.00000 ? ? H1011b .93337 .59162 .31199 .05800 Uiso ? ? 1.00000 ? ? H1011c .89604 .50185 .31069 .05800 Uiso ? ? 1.00000 ? ? H1021a .99219 .58573 .48547 .05200 Uiso ? ? 1.00000 ? ? H1021b .89649 .54075 .51784 .05200 Uiso ? ? 1.00000 ? ? H1021c .95298 .63930 .56142 .05200 Uiso ? ? 1.00000 ? ? H1031a .65662 .68106 .59110 .04700 Uiso ? ? 1.00000 ? ? H1031b .75351 .64296 .60528 .04700 Uiso ? ? 1.00000 ? ? H1031c .63460 .58422 .56259 .04700 Uiso ? ? 1.00000 ? ? H1041a .49042 .57150 .41677 .04100 Uiso ? ? 1.00000 ? ? H1041b .52534 .65139 .40141 .04100 Uiso ? ? 1.00000 ? ? H1041c .52549 .66187 .48319 .04100 Uiso ? ? 1.00000 ? ? H1051a .73965 .60637 .27174 .04700 Uiso ? ? 1.00000 ? ? H1051b .65771 .52159 .26365 .04700 Uiso ? ? 1.00000 ? ? H1051c .61633 .60419 .29487 .04700 Uiso ? ? 1.00000 ? ? H2112 .16666 .58449 .82765 .04100 Uiso ? ? 1.00000 ? ? H2113 -.00173 .60360 .78200 .05400 Uiso ? ? 1.00000 ? ? H2114 -.10072 .69542 .86267 .05200 Uiso ? ? 1.00000 ? ? H2115 -.03340 .77031 .99101 .04200 Uiso ? ? 1.00000 ? ? H2116 .13354 .75103 1.03776 .03600 Uiso ? ? 1.00000 ? ? H2122 .39588 .73864 1.13155 .02900 Uiso ? ? 1.00000 ? ? H2123 .33814 .72636 1.24037 .04100 Uiso ? ? 1.00000 ? ? H2124 .16666 .63025 1.23424 .04300 Uiso ? ? 1.00000 ? ? H2125 .05199 .54206 1.11772 .04400 Uiso ? ? 1.00000 ? ? H2126 .10816 .55613 1.00984 .03700 Uiso ? ? 1.00000 ? ? H210a .30986 .54091 .86539 .02800 Uiso ? ? 1.00000 ? ? H210b .25355 .51079 .92278 .02800 Uiso ? ? 1.00000 ? ? H220a .42982 .54377 .99004 .03100 Uiso ? ? 1.00000 ? ? H220b .44954 .49535 .90734 .03100 Uiso ? ? 1.00000 ? ? H2212 .63777 .71386 .85519 .03500 Uiso ? ? 1.00000 ? ? H2213 .72170 .67156 .74329 .04500 Uiso ? ? 1.00000 ? ? H2214 .73783 .53135 .68107 .05300 Uiso ? ? 1.00000 ? ? H2215 .68059 .43640 .73445 .05600 Uiso ? ? 1.00000 ? ? H2216 .60073 .47927 .84875 .04300 Uiso ? ? 1.00000 ? ? H2222 .55851 .68506 1.10723 .03400 Uiso ? ? 1.00000 ? ? H2223 .69575 .70133 1.20026 .04100 Uiso ? ? 1.00000 ? ? H2224 .87411 .67287 1.17103 .04300 Uiso ? ? 1.00000 ? ? H2225 .91768 .63128 1.04742 .04200 Uiso ? ? 1.00000 ? ? H2226 .77884 .61256 .95248 .03400 Uiso ? ? 1.00000 ? ? H222 .47161 .59430 .67803 .03000 Uiso ? ? 1.00000 ? ? H223 .41027 .55991 .55351 .03600 Uiso ? ? 1.00000 ? ? H224 .24917 .59939 .52483 .04000 Uiso ? ? 1.00000 ? ? H225 .14968 .67414 .62035 .04500 Uiso ? ? 1.00000 ? ? H226 .20710 .70701 .74457 .03600 Uiso ? ? 1.00000 ? ? H2011a .36779 .86316 .89464 .04700 Uiso ? ? 1.00000 ? ? H2011b .29023 .87639 .95863 .04700 Uiso ? ? 1.00000 ? ? H2011c .38037 .95354 .95834 .04700 Uiso ? ? 1.00000 ? ? H2021a .38110 .94931 1.15561 .05000 Uiso ? ? 1.00000 ? ? H2021b .29209 .90573 1.08432 .05000 Uiso ? ? 1.00000 ? ? H2021c .32144 .85234 1.12355 .05000 Uiso ? ? 1.00000 ? ? H2031a .53513 .84472 1.17807 .05100 Uiso ? ? 1.00000 ? ? H2031b .66308 .86446 1.16379 .05100 Uiso ? ? 1.00000 ? ? H2031c .60235 .93755 1.19834 .05100 Uiso ? ? 1.00000 ? ? H2041a .77623 .84291 .98535 .04800 Uiso ? ? 1.00000 ? ? H2041b .79826 .91410 1.06665 .04800 Uiso ? ? 1.00000 ? ? H2041c .75800 .81936 1.05244 .04800 Uiso ? ? 1.00000 ? ? H2051a .60841 .93033 .90264 .04500 Uiso ? ? 1.00000 ? ? H2051b .69182 .87565 .90289 .04500 Uiso ? ? 1.00000 ? ? H2051c .56957 .83214 .85851 .04500 Uiso ? ? 1.00000 ? ? H01 .95049 .12270 .08262 .05300 Uiso ? ? 1.00000 ? ? H02 1.07151 .06310 .12696 .06200 Uiso ? ? 1.00000 ? ? H03 1.12028 -.05922 .04380 .06600 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os1 .01402(5) .01480(5) .01328(5) .00342(4) .00214(4) .00640(4) Os2 .01761(6) .01421(5) .01281(5) .00267(4) .00137(4) .00612(4) P11 .0153(4) .0177(4) .0166(4) .0044(3) .0022(3) .0080(3) C1111 .0114(13) .0163(14) .0194(15) .0029(11) -.0037(11) .0014(11) C1112 .0201(15) .0228(16) .0227(16) .0072(12) .0037(13) .0109(13) C1113 .0263(17) .0293(17) .0234(16) .0074(14) .0110(14) .0139(14) C1114 .0203(16) .0360(19) .0205(16) .0109(14) .0081(13) .0092(14) C1115 .0221(17) .039(2) .037(2) .0181(15) .0111(15) .0220(16) C1116 .0202(16) .0310(18) .0310(18) .0085(13) .0069(14) .0200(15) C1121 .0189(15) .0176(14) .0171(14) .0068(12) .0026(12) .0073(12) C1122 .0229(16) .0255(16) .0215(16) .0072(13) .0045(13) .0097(13) C1123 .041(2) .043(2) .0191(17) .0112(17) .0090(15) .0156(15) C1124 .048(2) .039(2) .0161(16) .0213(18) -.0017(16) .0055(15) C1125 .0318(19) .0305(18) .0235(17) .0095(15) -.0086(15) .0011(14) C1126 .0261(17) .0221(16) .0265(17) .0038(13) .0004(14) .0084(14) C110 .0171(14) .0192(14) .0209(15) .0048(12) .0033(12) .0094(12) C120 .0216(15) .0196(15) .0192(15) .0051(12) .0038(12) .0077(12) P12 .0157(4) .0176(4) .0163(4) .0051(3) .0029(3) .0083(3) C1211 .0137(14) .0250(15) .0198(15) .0063(12) .0046(11) .0141(12) C1212 .0161(15) .0277(17) .0230(16) .0066(12) .0044(12) .0131(13) C1213 .0208(16) .043(2) .0227(17) .0077(15) .0032(13) .0198(15) C1214 .0260(18) .048(2) .035(2) .0150(16) .0048(15) .0308(17) C1215 .032(2) .035(2) .038(2) .0173(16) .0113(16) .0226(16) C1216 .0265(17) .0268(17) .0270(17) .0129(14) .0052(14) .0138(14) C1221 .0229(15) .0150(14) .0168(14) .0072(12) .0037(12) .0067(11) C1222 .0241(17) .0365(19) .0251(17) .0102(14) .0062(14) .0182(15) C1223 .039(2) .049(2) .0201(17) .0160(18) .0085(15) .0176(16) C1224 .039(2) .039(2) .031(2) .0121(17) .0186(17) .0173(16) C1225 .0203(17) .038(2) .036(2) .0065(15) .0077(15) .0133(16) C1226 .0219(16) .0246(16) .0233(16) .0056(13) .0059(13) .0087(13) C11 .0134(14) .0203(15) .0193(15) .0027(11) .0014(11) .0090(12) C12 .0191(15) .0251(16) .0181(15) .0052(13) .0016(12) .0061(13) C121 .0205(15) .0227(15) .0142(14) -.0005(12) .0000(12) .0078(12) C122 .0282(17) .0268(17) .0213(16) .0068(14) .0032(14) .0104(14) C123 .053(2) .033(2) .036(2) .0096(18) .0021(18) .0217(17) C124 .060(3) .059(3) .037(2) .001(2) .013(2) .037(2) C125 .039(2) .065(3) .036(2) .016(2) .0185(18) .030(2) C126 .0321(19) .036(2) .0236(17) .0104(15) .0092(15) .0154(15) C101 .0210(15) .0143(14) .0251(16) .0048(12) .0065(13) .0050(12) C1011 .034(2) .0262(18) .042(2) .0106(15) .0101(17) .0030(16) C102 .0227(16) .0144(14) .0283(17) .0014(12) -.0046(13) .0092(13) C1021 .0297(19) .0257(18) .050(2) .0066(15) -.0082(17) .0190(17) C103 .0266(16) .0154(14) .0175(15) -.0011(12) -.0008(13) .0087(12) C1031 .040(2) .0293(18) .0228(17) -.0056(15) -.0003(15) .0146(15) C104 .0150(14) .0145(13) .0238(16) .0006(11) .0022(12) .0098(12) C1041 .0214(16) .0271(17) .035(2) .0029(14) .0012(14) .0151(15) C105 .0223(16) .0183(15) .0173(15) .0009(12) -.0006(12) .0055(12) C1051 .040(2) .0262(17) .0175(16) -.0008(15) -.0006(15) .0059(13) P21 .0190(4) .0168(4) .0151(4) .0039(3) .0021(3) .0060(3) C2111 .0136(14) .0273(16) .0223(16) .0051(12) .0023(12) .0116(13) C2112 .0245(18) .044(2) .0243(18) .0076(16) .0029(14) .0126(16) C2113 .027(2) .068(3) .029(2) .0106(19) -.0043(16) .018(2) C2114 .025(2) .062(3) .052(2) .0134(18) -.0010(18) .035(2) C2115 .0270(18) .038(2) .045(2) .0142(16) .0094(16) .0232(17) C2116 .0278(18) .0288(18) .0282(18) .0066(14) .0037(14) .0138(15) C2121 .0216(15) .0214(15) .0196(15) .0063(12) .0043(12) .0106(12) C2122 .0283(17) .0226(16) .0219(16) .0082(13) .0041(14) .0095(13) C2123 .039(2) .037(2) .0216(17) .0140(16) .0082(15) .0127(15) C2124 .038(2) .044(2) .0290(18) .0173(17) .0144(16) .0252(16) C2125 .032(2) .042(2) .043(2) .0070(16) .0163(17) .0278(18) C2126 .0267(17) .0311(18) .0253(17) .0004(14) .0033(14) .0149(15) C210 .0238(16) .0166(15) .0222(16) .0009(12) -.0004(13) .0055(12) C220 .0310(18) .0166(15) .0279(17) .0070(13) .0037(14) .0087(13) P22 .0200(4) .0182(4) .0178(4) .0050(3) .0010(3) .0077(3) C2211 .0216(16) .0287(17) .0188(15) .0119(13) -.0006(13) .0066(13) C2212 .0222(16) .0354(19) .0242(17) .0097(14) .0032(14) .0134(15) C2213 .0255(18) .058(2) .0262(18) .0128(17) .0059(15) .0224(17) C2214 .035(2) .068(3) .0224(18) .025(2) .0063(16) .0122(18) C2215 .048(2) .048(2) .029(2) .028(2) .0020(18) .0015(18) C2216 .041(2) .034(2) .0265(18) .0192(17) .0047(16) .0097(15) C2221 .0277(17) .0159(14) .0218(16) .0029(12) -.0023(13) .0094(12) C2222 .0320(19) .0275(17) .0249(17) .0110(14) .0030(15) .0119(14) C2223 .046(2) .0313(19) .0190(16) .0120(16) -.0014(15) .0105(14) C2224 .041(2) .0203(16) .033(2) .0015(15) -.0138(16) .0124(15) C2225 .0230(17) .0311(19) .044(2) -.0003(14) -.0082(16) .0223(17) C2226 .0239(17) .0287(17) .0274(17) .0049(14) -.0013(14) .0145(14) C21 .0178(14) .0164(14) .0212(15) .0061(11) .0031(12) .0083(12) C22 .0239(16) .0202(15) .0204(15) .0069(12) .0039(13) .0103(12) C221 .0222(15) .0211(15) .0170(14) .0019(12) -.0014(12) .0105(12) C222 .0268(17) .0223(16) .0240(17) .0037(13) -.0008(14) .0108(13) C223 .042(2) .0231(16) .0177(16) -.0001(15) .0059(15) .0088(13) C224 .038(2) .0303(18) .0234(17) -.0071(15) -.0094(15) .0161(15) C225 .036(2) .045(2) .033(2) .0077(17) -.0049(16) .0258(18) C226 .0303(18) .0331(19) .0268(18) .0109(15) .0028(15) .0148(15) C201 .0296(17) .0126(14) .0228(16) .0047(12) .0036(13) .0076(12) C2011 .038(2) .0232(17) .033(2) .0099(15) .0000(16) .0127(15) C202 .0277(17) .0118(14) .0248(16) .0026(12) .0084(14) .0050(12) C2021 .043(2) .0208(16) .032(2) .0119(15) .0140(17) .0090(14) C203 .0305(17) .0146(14) .0179(15) -.0027(12) -.0012(13) .0062(12) C2031 .049(2) .0237(17) .0177(16) -.0089(15) -.0081(15) .0078(14) C204 .0225(16) .0172(15) .0250(16) -.0032(12) -.0014(13) .0087(13) C2041 .0248(18) .0313(19) .036(2) -.0037(14) -.0004(15) .0158(16) C205 .0294(17) .0182(15) .0176(15) -.0016(13) .0015(13) .0090(12) C2051 .044(2) .0296(18) .0269(18) .0066(16) .0101(16) .0176(15) C01 .060(3) .040(2) .041(2) .023(2) .025(2) .0224(18) C02 .045(2) .044(2) .036(2) .0059(18) .0066(18) .0217(18) C03 .046(2) .060(3) .051(2) .030(2) .020(2) .038(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Os1 P11 . . 2.2625(7) ? Os1 P12 . . 2.2721(8) ? Os1 C11 . . 2.026(3) ? Os1 C101 . . 2.236(3) ? Os1 C102 . . 2.251(4) ? Os1 C103 . . 2.269(3) ? Os1 C104 . . 2.274(2) ? Os1 C105 . . 2.252(2) ? Os2 P21 . . 2.2682(8) ? Os2 P22 . . 2.2752(9) ? Os2 C21 . . 2.012(3) ? Os2 C201 . . 2.230(3) ? Os2 C202 . . 2.260(3) ? Os2 C203 . . 2.291(2) ? Os2 C204 . . 2.274(2) ? Os2 C205 . . 2.238(3) ? P11 C1111 . . 1.821(3) ? P11 C1121 . . 1.847(3) ? P11 C110 . . 1.848(3) ? C1111 C1112 . . 1.399(5) ? C1111 C1116 . . 1.399(5) ? C1112 C1113 . . 1.388(4) ? C1112 H1112 . . .961 ? C1113 C1114 . . 1.376(5) ? C1113 H1113 . . .961 ? C1114 C1115 . . 1.377(6) ? C1114 H1114 . . .960 ? C1115 C1116 . . 1.387(4) ? C1115 H1115 . . .965 ? C1116 H1116 . . .968 ? C1121 C1122 . . 1.381(5) ? C1121 C1126 . . 1.399(4) ? C1122 C1123 . . 1.399(5) ? C1122 H1122 . . .960 ? C1123 C1124 . . 1.371(4) ? C1123 H1123 . . .964 ? C1124 C1125 . . 1.373(5) ? C1124 H1124 . . .965 ? C1125 C1126 . . 1.392(5) ? C1125 H1125 . . .963 ? C1126 H1126 . . .960 ? C110 C120 . . 1.528(4) ? C110 H110a . . .955 ? C110 H110b . . .958 ? C120 P12 . . 1.860(2) ? C120 H120a . . .952 ? C120 H120b . . .958 ? P12 C1211 . . 1.844(4) ? P12 C1221 . . 1.841(3) ? C1211 C1212 . . 1.399(4) ? C1211 C1216 . . 1.394(4) ? C1212 C1213 . . 1.390(5) ? C1212 H1212 . . .958 ? C1213 C1214 . . 1.370(5) ? C1213 H1213 . . .964 ? C1214 C1215 . . 1.388(4) ? C1214 H1214 . . .963 ? C1215 C1216 . . 1.392(6) ? C1215 H1215 . . .966 ? C1216 H1216 . . .961 ? C1221 C1222 . . 1.395(5) ? C1221 C1226 . . 1.395(4) ? C1222 C1223 . . 1.396(5) ? C1222 H1222 . . .960 ? C1223 C1224 . . 1.370(5) ? C1223 H1223 . . .960 ? C1224 C1225 . . 1.385(5) ? C1224 H1224 . . .959 ? C1225 C1226 . . 1.384(5) ? C1225 H1225 . . .970 ? C1226 H1226 . . .959 ? C11 C12 . . 1.202(5) ? C12 C121 . . 1.443(5) ? C121 C122 . . 1.406(5) ? C121 C126 . . 1.396(4) ? C122 C123 . . 1.386(6) ? C122 H122 . . .960 ? C123 C124 . . 1.370(6) ? C123 H123 . . .969 ? C124 C125 . . 1.389(7) ? C124 H124 . . .964 ? C125 C126 . . 1.374(6) ? C125 H125 . . .971 ? C126 H126 . . .962 ? C101 C1011 . . 1.513(5) ? C101 C102 . . 1.432(5) ? C101 C105 . . 1.432(5) ? C1011 H1011a . . .951 ? C1011 H1011b . . .959 ? C1011 H1011c . . .948 ? C102 C1021 . . 1.505(5) ? C102 C103 . . 1.424(4) ? C1021 H1021a . . .954 ? C1021 H1021b . . .951 ? C1021 H1021c . . .949 ? C103 C1031 . . 1.501(5) ? C103 C104 . . 1.428(5) ? C1031 H1031a . . .964 ? C1031 H1031b . . .949 ? C1031 H1031c . . .947 ? C104 C1041 . . 1.489(4) ? C104 C105 . . 1.431(4) ? C1041 H1041a . . .952 ? C1041 H1041b . . .960 ? C1041 H1041c . . .958 ? C105 C1051 . . 1.508(5) ? C1051 H1051a . . .948 ? C1051 H1051b . . .952 ? C1051 H1051c . . .957 ? P21 C2111 . . 1.831(3) ? P21 C2121 . . 1.838(3) ? P21 C210 . . 1.833(3) ? C2111 C2112 . . 1.400(4) ? C2111 C2116 . . 1.388(4) ? C2112 C2113 . . 1.396(6) ? C2112 H2112 . . .965 ? C2113 C2114 . . 1.366(5) ? C2113 H2113 . . .967 ? C2114 C2115 . . 1.375(5) ? C2114 H2114 . . .963 ? C2115 C2116 . . 1.382(5) ? C2115 H2115 . . .967 ? C2116 H2116 . . .968 ? C2121 C2122 . . 1.389(4) ? C2121 C2126 . . 1.394(4) ? C2122 C2123 . . 1.391(5) ? C2122 H2122 . . .969 ? C2123 C2124 . . 1.368(5) ? C2123 H2123 . . .966 ? C2124 C2125 . . 1.394(4) ? C2124 H2124 . . .958 ? C2125 C2126 . . 1.381(5) ? C2125 H2125 . . .969 ? C2126 H2126 . . .964 ? C210 C220 . . 1.523(5) ? C210 H210a . . .955 ? C210 H210b . . .965 ? C220 P22 . . 1.846(3) ? C220 H220a . . .961 ? C220 H220b . . .956 ? P22 C2211 . . 1.852(3) ? P22 C2221 . . 1.842(3) ? C2211 C2212 . . 1.383(5) ? C2211 C2216 . . 1.400(5) ? C2212 C2213 . . 1.393(5) ? C2212 H2212 . . .964 ? C2213 C2214 . . 1.369(5) ? C2213 H2213 . . .958 ? C2214 C2215 . . 1.385(6) ? C2214 H2214 . . .962 ? C2215 C2216 . . 1.393(5) ? C2215 H2215 . . .964 ? C2216 H2216 . . .971 ? C2221 C2222 . . 1.402(4) ? C2221 C2226 . . 1.382(4) ? C2222 C2223 . . 1.379(5) ? C2222 H2222 . . .963 ? C2223 C2224 . . 1.382(5) ? C2223 H2223 . . .964 ? C2224 C2225 . . 1.369(5) ? C2224 H2224 . . .967 ? C2225 C2226 . . 1.395(5) ? C2225 H2225 . . .967 ? C2226 H2226 . . .959 ? C21 C22 . . 1.208(4) ? C22 C221 . . 1.437(4) ? C221 C222 . . 1.394(4) ? C221 C226 . . 1.398(5) ? C222 C223 . . 1.389(5) ? C222 H222 . . .966 ? C223 C224 . . 1.376(5) ? C223 H223 . . .967 ? C224 C225 . . 1.377(5) ? C224 H224 . . .962 ? C225 C226 . . 1.379(5) ? C225 H225 . . .967 ? C226 H226 . . .967 ? C201 C2011 . . 1.502(5) ? C201 C202 . . 1.429(5) ? C201 C205 . . 1.444(4) ? C2011 H2011a . . .956 ? C2011 H2011b . . .948 ? C2011 H2011c . . .947 ? C202 C2021 . . 1.502(5) ? C202 C203 . . 1.442(5) ? C2021 H2021a . . .951 ? C2021 H2021b . . .958 ? C2021 H2021c . . .955 ? C203 C2031 . . 1.501(5) ? C203 C204 . . 1.440(4) ? C2031 H2031a . . .953 ? C2031 H2031b . . .953 ? C2031 H2031c . . .953 ? C204 C2041 . . 1.494(5) ? C204 C205 . . 1.437(5) ? C2041 H2041a . . .953 ? C2041 H2041b . . .946 ? C2041 H2041c . . .964 ? C205 C2051 . . 1.497(5) ? C2051 H2051a . . .943 ? C2051 H2051b . . .956 ? C2051 H2051c . . .961 ? C01 C02 . . 1.376(6) ? C01 H01 . . .963 ? C01 C03 . '2 755' 1.372(5) ? C02 C03 . . 1.365(5) ? C02 H02 . . .963 ? C03 H03 . . .958 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P11 Os1 P12 . . . 83.35(3) ? P11 Os1 C11 . . . 81.17(7) ? P11 Os1 C101 . . . 113.54(8) ? P11 Os1 C102 . . . 101.28(7) ? P11 Os1 C103 . . . 121.32(8) ? P11 Os1 C104 . . . 157.93(9) ? P11 Os1 C105 . . . 149.05(8) ? P12 Os1 C11 . . . 86.30(9) ? P12 Os1 C101 . . . 163.07(8) ? P12 Os1 C102 . . . 141.94(8) ? P12 Os1 C103 . . . 109.14(8) ? P12 Os1 C104 . . . 102.12(8) ? P12 Os1 C105 . . . 126.45(9) ? C11 Os1 C101 . . . 97.17(12) ? C11 Os1 C102 . . . 131.74(11) ? C11 Os1 C103 . . . 153.20(9) ? C11 Os1 C104 . . . 120.24(11) ? C11 Os1 C105 . . . 91.64(11) ? C101 Os1 C102 . . . 37.22(12) ? C101 Os1 C103 . . . 61.89(11) ? C101 Os1 C104 . . . 61.82(10) ? C101 Os1 C105 . . . 37.21(11) ? C102 Os1 C103 . . . 36.73(11) ? C102 Os1 C104 . . . 61.30(11) ? C102 Os1 C105 . . . 61.74(12) ? C103 Os1 C104 . . . 36.64(11) ? C103 Os1 C105 . . . 61.56(11) ? C104 Os1 C105 . . . 36.87(10) ? P21 Os2 P22 . . . 83.35(3) ? P21 Os2 C21 . . . 81.62(8) ? P21 Os2 C201 . . . 116.66(8) ? P21 Os2 C202 . . . 103.12(8) ? P21 Os2 C203 . . . 120.77(8) ? P21 Os2 C204 . . . 157.05(8) ? P21 Os2 C205 . . . 153.00(9) ? P22 Os2 C21 . . . 87.16(9) ? P22 Os2 C201 . . . 159.43(8) ? P22 Os2 C202 . . . 147.93(9) ? P22 Os2 C203 . . . 112.98(9) ? P22 Os2 C204 . . . 101.13(9) ? P22 Os2 C205 . . . 121.73(9) ? C21 Os2 C201 . . . 90.99(12) ? C21 Os2 C202 . . . 124.71(13) ? C21 Os2 C203 . . . 150.30(13) ? C21 Os2 C204 . . . 120.86(12) ? C21 Os2 C205 . . . 89.27(11) ? C201 Os2 C202 . . . 37.12(12) ? C201 Os2 C203 . . . 62.34(12) ? C201 Os2 C204 . . . 62.56(11) ? C201 Os2 C205 . . . 37.72(11) ? C202 Os2 C203 . . . 36.93(12) ? C202 Os2 C204 . . . 61.54(10) ? C202 Os2 C205 . . . 61.81(11) ? C203 Os2 C204 . . . 36.76(11) ? C203 Os2 C205 . . . 61.82(11) ? C204 Os2 C205 . . . 37.13(13) ? Os1 P11 C1111 . . . 117.66(8) ? Os1 P11 C1121 . . . 121.56(10) ? Os1 P11 C110 . . . 108.32(9) ? C1111 P11 C1121 . . . 100.37(14) ? C1111 P11 C110 . . . 105.18(14) ? C1121 P11 C110 . . . 101.63(13) ? P11 C1111 C1112 . . . 122.7(3) ? P11 C1111 C1116 . . . 120.8(3) ? C1112 C1111 C1116 . . . 116.4(3) ? C1111 C1112 C1113 . . . 121.5(3) ? C1111 C1112 H1112 . . . 118.7 ? C1113 C1112 H1112 . . . 119.9 ? C1112 C1113 C1114 . . . 120.5(3) ? C1112 C1113 H1113 . . . 120.1 ? C1114 C1113 H1113 . . . 119.4 ? C1113 C1114 C1115 . . . 119.6(3) ? C1113 C1114 H1114 . . . 120.9 ? C1115 C1114 H1114 . . . 119.5 ? C1114 C1115 C1116 . . . 119.8(4) ? C1114 C1115 H1115 . . . 120.3 ? C1116 C1115 H1115 . . . 119.9 ? C1111 C1116 C1115 . . . 122.2(4) ? C1111 C1116 H1116 . . . 118.3 ? C1115 C1116 H1116 . . . 119.5 ? P11 C1121 C1122 . . . 120.0(2) ? P11 C1121 C1126 . . . 121.4(3) ? C1122 C1121 C1126 . . . 118.6(3) ? C1121 C1122 C1123 . . . 120.7(3) ? C1121 C1122 H1122 . . . 119.2 ? C1123 C1122 H1122 . . . 120.0 ? C1122 C1123 C1124 . . . 119.9(3) ? C1122 C1123 H1123 . . . 120.1 ? C1124 C1123 H1123 . . . 120.0 ? C1123 C1124 C1125 . . . 120.2(3) ? C1123 C1124 H1124 . . . 120.5 ? C1125 C1124 H1124 . . . 119.2 ? C1124 C1125 C1126 . . . 120.3(3) ? C1124 C1125 H1125 . . . 120.3 ? C1126 C1125 H1125 . . . 119.3 ? C1121 C1126 C1125 . . . 120.1(3) ? C1121 C1126 H1126 . . . 120.0 ? C1125 C1126 H1126 . . . 119.9 ? P11 C110 C120 . . . 107.6(2) ? P11 C110 H110a . . . 109.7 ? P11 C110 H110b . . . 109.5 ? C120 C110 H110a . . . 111.2 ? C120 C110 H110b . . . 110.4 ? H110a C110 H110b . . . 108.4 ? C110 C120 P12 . . . 110.14(16) ? C110 C120 H120a . . . 109.5 ? C110 C120 H120b . . . 108.9 ? P12 C120 H120a . . . 109.9 ? P12 C120 H120b . . . 109.6 ? H120a C120 H120b . . . 108.7 ? Os1 P12 C120 . . . 111.02(10) ? Os1 P12 C1211 . . . 118.34(8) ? Os1 P12 C1221 . . . 118.29(11) ? C120 P12 C1211 . . . 103.51(14) ? C120 P12 C1221 . . . 102.67(12) ? C1211 P12 C1221 . . . 100.89(14) ? P12 C1211 C1212 . . . 120.5(2) ? P12 C1211 C1216 . . . 121.3(2) ? C1212 C1211 C1216 . . . 118.2(3) ? C1211 C1212 C1213 . . . 120.7(3) ? C1211 C1212 H1212 . . . 118.8 ? C1213 C1212 H1212 . . . 120.5 ? C1212 C1213 C1214 . . . 120.4(3) ? C1212 C1213 H1213 . . . 119.5 ? C1214 C1213 H1213 . . . 120.0 ? C1213 C1214 C1215 . . . 119.9(4) ? C1213 C1214 H1214 . . . 119.9 ? C1215 C1214 H1214 . . . 120.2 ? C1214 C1215 C1216 . . . 120.0(3) ? C1214 C1215 H1215 . . . 120.3 ? C1216 C1215 H1215 . . . 119.7 ? C1211 C1216 C1215 . . . 120.8(3) ? C1211 C1216 H1216 . . . 119.5 ? C1215 C1216 H1216 . . . 119.7 ? P12 C1221 C1222 . . . 120.2(2) ? P12 C1221 C1226 . . . 121.5(2) ? C1222 C1221 C1226 . . . 118.1(3) ? C1221 C1222 C1223 . . . 120.6(3) ? C1221 C1222 H1222 . . . 119.7 ? C1223 C1222 H1222 . . . 119.8 ? C1222 C1223 C1224 . . . 120.7(3) ? C1222 C1223 H1223 . . . 119.0 ? C1224 C1223 H1223 . . . 120.3 ? C1223 C1224 C1225 . . . 119.2(3) ? C1223 C1224 H1224 . . . 120.0 ? C1225 C1224 H1224 . . . 120.8 ? C1224 C1225 C1226 . . . 120.8(3) ? C1224 C1225 H1225 . . . 119.5 ? C1226 C1225 H1225 . . . 119.7 ? C1221 C1226 C1225 . . . 120.7(3) ? C1221 C1226 H1226 . . . 119.4 ? C1225 C1226 H1226 . . . 120.0 ? Os1 C11 C12 . . . 177.9(2) ? C11 C12 C121 . . . 174.1(3) ? C12 C121 C122 . . . 121.6(3) ? C12 C121 C126 . . . 120.6(3) ? C122 C121 C126 . . . 117.8(3) ? C121 C122 C123 . . . 120.7(3) ? C121 C122 H122 . . . 119.7 ? C123 C122 H122 . . . 119.6 ? C122 C123 C124 . . . 120.4(4) ? C122 C123 H123 . . . 119.5 ? C124 C123 H123 . . . 120.1 ? C123 C124 C125 . . . 119.7(4) ? C123 C124 H124 . . . 120.3 ? C125 C124 H124 . . . 120.0 ? C124 C125 C126 . . . 120.4(4) ? C124 C125 H125 . . . 119.6 ? C126 C125 H125 . . . 120.0 ? C121 C126 C125 . . . 121.0(4) ? C121 C126 H126 . . . 119.1 ? C125 C126 H126 . . . 119.9 ? Os1 C101 C1011 . . . 126.6(2) ? Os1 C101 C102 . . . 71.96(16) ? Os1 C101 C105 . . . 72.01(16) ? C1011 C101 C102 . . . 126.5(3) ? C1011 C101 C105 . . . 125.6(3) ? C102 C101 C105 . . . 107.6(3) ? C101 C1011 H1011a . . . 108.3 ? C101 C1011 H1011b . . . 108.0 ? C101 C1011 H1011c . . . 110.6 ? H1011a C1011 H1011b . . . 108.6 ? H1011a C1011 H1011c . . . 112.0 ? H1011b C1011 H1011c . . . 109.3 ? Os1 C102 C101 . . . 70.8(2) ? Os1 C102 C1021 . . . 129.74(18) ? Os1 C102 C103 . . . 72.3(2) ? C101 C102 C1021 . . . 125.5(3) ? C101 C102 C103 . . . 108.4(3) ? C1021 C102 C103 . . . 125.5(3) ? C102 C1021 H1021a . . . 107.8 ? C102 C1021 H1021b . . . 108.0 ? C102 C1021 H1021c . . . 110.4 ? H1021a C1021 H1021b . . . 109.0 ? H1021a C1021 H1021c . . . 109.6 ? H1021b C1021 H1021c . . . 112.0 ? Os1 C103 C102 . . . 70.94(19) ? Os1 C103 C1031 . . . 131.71(18) ? Os1 C103 C104 . . . 71.86(18) ? C102 C103 C1031 . . . 126.6(3) ? C102 C103 C104 . . . 108.0(3) ? C1031 C103 C104 . . . 124.4(3) ? C103 C1031 H1031a . . . 110.5 ? C103 C1031 H1031b . . . 111.2 ? C103 C1031 H1031c . . . 110.1 ? H1031a C1031 H1031b . . . 108.4 ? H1031a C1031 H1031c . . . 107.0 ? H1031b C1031 H1031c . . . 109.5 ? Os1 C104 C103 . . . 71.50(15) ? Os1 C104 C1041 . . . 129.7(2) ? Os1 C104 C105 . . . 70.74(14) ? C103 C104 C1041 . . . 126.7(3) ? C103 C104 C105 . . . 108.0(3) ? C1041 C104 C105 . . . 124.7(3) ? C104 C1041 H1041a . . . 110.2 ? C104 C1041 H1041b . . . 110.5 ? C104 C1041 H1041c . . . 110.3 ? H1041a C1041 H1041b . . . 108.5 ? H1041a C1041 H1041c . . . 109.1 ? H1041b C1041 H1041c . . . 108.1 ? Os1 C105 C101 . . . 70.78(13) ? Os1 C105 C104 . . . 72.39(13) ? Os1 C105 C1051 . . . 126.9(2) ? C101 C105 C104 . . . 108.0(3) ? C101 C105 C1051 . . . 125.1(3) ? C104 C105 C1051 . . . 126.6(3) ? C105 C1051 H1051a . . . 110.6 ? C105 C1051 H1051b . . . 110.2 ? C105 C1051 H1051c . . . 109.4 ? H1051a C1051 H1051b . . . 109.4 ? H1051a C1051 H1051c . . . 108.9 ? H1051b C1051 H1051c . . . 108.1 ? Os2 P21 C2111 . . . 117.61(12) ? Os2 P21 C2121 . . . 122.75(8) ? Os2 P21 C210 . . . 107.93(10) ? C2111 P21 C2121 . . . 99.50(15) ? C2111 P21 C210 . . . 105.56(13) ? C2121 P21 C210 . . . 101.29(15) ? P21 C2111 C2112 . . . 122.1(2) ? P21 C2111 C2116 . . . 119.5(2) ? C2112 C2111 C2116 . . . 118.3(3) ? C2111 C2112 C2113 . . . 119.7(3) ? C2111 C2112 H2112 . . . 119.8 ? C2113 C2112 H2112 . . . 120.5 ? C2112 C2113 C2114 . . . 120.8(3) ? C2112 C2113 H2113 . . . 119.0 ? C2114 C2113 H2113 . . . 120.2 ? C2113 C2114 C2115 . . . 120.0(4) ? C2113 C2114 H2114 . . . 119.2 ? C2115 C2114 H2114 . . . 120.7 ? C2114 C2115 C2116 . . . 120.0(3) ? C2114 C2115 H2115 . . . 120.0 ? C2116 C2115 H2115 . . . 120.0 ? C2111 C2116 C2115 . . . 121.2(3) ? C2111 C2116 H2116 . . . 118.8 ? C2115 C2116 H2116 . . . 120.0 ? P21 C2121 C2122 . . . 120.6(2) ? P21 C2121 C2126 . . . 121.5(2) ? C2122 C2121 C2126 . . . 117.8(3) ? C2121 C2122 C2123 . . . 121.1(3) ? C2121 C2122 H2122 . . . 118.9 ? C2123 C2122 H2122 . . . 119.9 ? C2122 C2123 C2124 . . . 120.4(3) ? C2122 C2123 H2123 . . . 119.8 ? C2124 C2123 H2123 . . . 119.7 ? C2123 C2124 C2125 . . . 119.3(3) ? C2123 C2124 H2124 . . . 120.0 ? C2125 C2124 H2124 . . . 120.7 ? C2124 C2125 C2126 . . . 120.2(3) ? C2124 C2125 H2125 . . . 119.9 ? C2126 C2125 H2125 . . . 119.8 ? C2121 C2126 C2125 . . . 121.0(3) ? C2121 C2126 H2126 . . . 119.0 ? C2125 C2126 H2126 . . . 120.0 ? P21 C210 C220 . . . 107.25(16) ? P21 C210 H210a . . . 110.8 ? P21 C210 H210b . . . 110.2 ? C220 C210 H210a . . . 110.5 ? C220 C210 H210b . . . 110.5 ? H210a C210 H210b . . . 107.8 ? C210 C220 P22 . . . 109.4(2) ? C210 C220 H220a . . . 109.8 ? C210 C220 H220b . . . 110.5 ? P22 C220 H220a . . . 109.45 ? P22 C220 H220b . . . 109.7 ? H220a C220 H220b . . . 108.0 ? Os2 P22 C220 . . . 110.43(11) ? Os2 P22 C2211 . . . 117.15(13) ? Os2 P22 C2221 . . . 118.84(9) ? C220 P22 C2211 . . . 103.84(13) ? C220 P22 C2221 . . . 102.16(16) ? C2211 P22 C2221 . . . 102.42(14) ? P22 C2211 C2212 . . . 118.7(2) ? P22 C2211 C2216 . . . 123.2(3) ? C2212 C2211 C2216 . . . 118.1(3) ? C2211 C2212 C2213 . . . 121.8(3) ? C2211 C2212 H2212 . . . 118.8 ? C2213 C2212 H2212 . . . 119.3 ? C2212 C2213 C2214 . . . 119.5(4) ? C2212 C2213 H2213 . . . 120.1 ? C2214 C2213 H2213 . . . 120.4 ? C2213 C2214 C2215 . . . 120.0(3) ? C2213 C2214 H2214 . . . 120.5 ? C2215 C2214 H2214 . . . 119.5 ? C2214 C2215 C2216 . . . 120.5(3) ? C2214 C2215 H2215 . . . 119.8 ? C2216 C2215 H2215 . . . 119.7 ? C2211 C2216 C2215 . . . 120.0(4) ? C2211 C2216 H2216 . . . 119.7 ? C2215 C2216 H2216 . . . 120.3 ? P22 C2221 C2222 . . . 117.4(2) ? P22 C2221 C2226 . . . 124.0(2) ? C2222 C2221 C2226 . . . 118.6(3) ? C2221 C2222 C2223 . . . 120.4(3) ? C2221 C2222 H2222 . . . 119.7 ? C2223 C2222 H2222 . . . 119.8 ? C2222 C2223 C2224 . . . 120.6(3) ? C2222 C2223 H2223 . . . 119.7 ? C2224 C2223 H2223 . . . 119.7 ? C2223 C2224 C2225 . . . 119.3(3) ? C2223 C2224 H2224 . . . 119.4 ? C2225 C2224 H2224 . . . 121.3 ? C2224 C2225 C2226 . . . 120.9(3) ? C2224 C2225 H2225 . . . 119.5 ? C2226 C2225 H2225 . . . 119.6 ? C2221 C2226 C2225 . . . 120.1(3) ? C2221 C2226 H2226 . . . 119.3 ? C2225 C2226 H2226 . . . 120.6 ? Os2 C21 C22 . . . 174.4(3) ? C21 C22 C221 . . . 176.6(3) ? C22 C221 C222 . . . 122.0(3) ? C22 C221 C226 . . . 120.2(3) ? C222 C221 C226 . . . 117.8(3) ? C221 C222 C223 . . . 120.7(3) ? C221 C222 H222 . . . 120.0 ? C223 C222 H222 . . . 119.3 ? C222 C223 C224 . . . 120.3(3) ? C222 C223 H223 . . . 119.9 ? C224 C223 H223 . . . 119.8 ? C223 C224 C225 . . . 119.8(3) ? C223 C224 H224 . . . 120.4 ? C225 C224 H224 . . . 119.8 ? C224 C225 C226 . . . 120.3(4) ? C224 C225 H225 . . . 119.8 ? C226 C225 H225 . . . 119.9 ? C221 C226 C225 . . . 121.1(3) ? C221 C226 H226 . . . 119.7 ? C225 C226 H226 . . . 119.2 ? Os2 C201 C2011 . . . 124.48(17) ? Os2 C201 C202 . . . 72.60(19) ? Os2 C201 C205 . . . 71.47(18) ? C2011 C201 C202 . . . 128.0(3) ? C2011 C201 C205 . . . 124.9(3) ? C202 C201 C205 . . . 107.0(3) ? C201 C2011 H2011a . . . 109.5 ? C201 C2011 H2011b . . . 109.7 ? C201 C2011 H2011c . . . 109.6 ? H2011a C2011 H2011b . . . 109.2 ? H2011a C2011 H2011c . . . 109.2 ? H2011b C2011 H2011c . . . 109.7 ? Os2 C202 C201 . . . 70.28(16) ? Os2 C202 C2021 . . . 129.1(2) ? Os2 C202 C203 . . . 72.71(15) ? C201 C202 C2021 . . . 125.9(3) ? C201 C202 C203 . . . 109.2(3) ? C2021 C202 C203 . . . 124.5(3) ? C202 C2021 H2021a . . . 109.9 ? C202 C2021 H2021b . . . 109.3 ? C202 C2021 H2021c . . . 110.6 ? H2021a C2021 H2021b . . . 108.8 ? H2021a C2021 H2021c . . . 109.7 ? H2021b C2021 H2021c . . . 108.5 ? Os2 C203 C202 . . . 70.36(13) ? Os2 C203 C2031 . . . 133.8(2) ? Os2 C203 C204 . . . 70.98(13) ? C202 C203 C2031 . . . 126.0(3) ? C202 C203 C204 . . . 107.2(3) ? C2031 C203 C204 . . . 125.5(3) ? C203 C2031 H2031a . . . 110.4 ? C203 C2031 H2031b . . . 110.1 ? C203 C2031 H2031c . . . 109.8 ? H2031a C2031 H2031b . . . 109.0 ? H2031a C2031 H2031c . . . 108.6 ? H2031b C2031 H2031c . . . 108.9 ? Os2 C204 C203 . . . 72.26(14) ? Os2 C204 C2041 . . . 128.1(2) ? Os2 C204 C205 . . . 70.08(15) ? C203 C204 C2041 . . . 124.7(3) ? C203 C204 C205 . . . 108.0(3) ? C2041 C204 C205 . . . 127.0(3) ? C204 C2041 H2041a . . . 109.7 ? C204 C2041 H2041b . . . 110.2 ? C204 C2041 H2041c . . . 109.8 ? H2041a C2041 H2041b . . . 109.6 ? H2041a C2041 H2041c . . . 108.8 ? H2041b C2041 H2041c . . . 108.7 ? Os2 C205 C201 . . . 70.81(17) ? Os2 C205 C204 . . . 72.79(18) ? Os2 C205 C2051 . . . 127.14(17) ? C201 C205 C204 . . . 108.5(3) ? C201 C205 C2051 . . . 124.7(3) ? C204 C205 C2051 . . . 126.5(3) ? C205 C2051 H2051a . . . 110.6 ? C205 C2051 H2051b . . . 110.2 ? C205 C2051 H2051c . . . 109.5 ? H2051a C2051 H2051b . . . 109.5 ? H2051a C2051 H2051c . . . 108.9 ? H2051b C2051 H2051c . . . 108.1 ? C02 C01 H01 . . . 120.2 ? C02 C01 C03 . . '2 755' 119.6(3) ? H01 C01 C03 . . '2 755' 120.1 ? C01 C02 C03 . . . 119.5(3) ? C01 C02 H02 . . . 119.8 ? C03 C02 H02 . . . 120.7 ? C02 C03 H03 . . . 119.7 ? C02 C03 C01 . . '2 755' 120.8(4) ? H03 C03 C01 . . '2 755' 119.5 ? _exptl_crystal_F_000 1698 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min -30 _reflns_limit_k_max 29 _reflns_limit_l_min -33 _reflns_limit_l_max 33 _reflns_number_observed ? _reflns_d_resolution_high .582 _reflns_d_resolution_low 15.568 _diffrn_reflns_av_sigmaI/netI .156 _diffrn_reflns_theta_min 1.3 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .084 _refine_ls_wR_factor_all .026 _refine_ls_goodness_of_fit_all .966 _refine_ls_shift/su_mean .002 #===END #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_br776z _database_code_depnum_ccdc_archive 'CCDC 617827' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C38 H40 Os1 P2' _chemical_formula_moiety 'C38 H40 Os1 P2' _chemical_formula_weight 748.89 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 11.1341(5) _cell_length_b 16.7364(8) _cell_length_c 18.1183(8) _cell_angle_alpha 88.6890(10) _cell_angle_beta 88.9600(10) _cell_angle_gamma 70.9060(10) _cell_volume 3189.5(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.56 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 24.4 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 4.124 _exptl_crystal_description cuboid _exptl_crystal_size_max .18 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour pale_yellow _exptl_crystal_F_000 1496 _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .54 _exptl_absorpt_correction_T_max .70 _diffrn_reflns_number 66158 _reflns_number_total 11193 _reflns_Friedel_coverage 0 _reflns_number_gt 9206 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .063 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .042 _refine_ls_wR_factor_ref .051 _refine_ls_goodness_of_fit_ref 1.454 _refine_ls_number_reflns 8967 _refine_ls_number_parameters 740 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/(sig^2(F) + .0005F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .02 _refine_diff_density_min -1.565 _refine_diff_density_max 5.419 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics 'xtal PIG' _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 152 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 160 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 0 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Os ? 0 4 -1.816 7.605 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Os1 .24249(3) 1.17488(2) .18661(2) .0159(2) Uani ? ? 1.00000 ? ? Os2 .26552(3) .33143(2) .68005(2) .0157(2) Uani ? ? 1.00000 ? ? P11 .45359(18) 1.11694(12) .16351(11) .0193(13) Uani ? ? 1.00000 ? ? C1111 .5721(7) 1.1095(5) .2357(4) .024(6) Uani ? ? 1.00000 ? ? C1112 .5335(8) 1.1342(5) .3054(5) .031(6) Uani ? ? 1.00000 ? ? C1113 .6251(10) 1.1273(6) .3610(5) .041(8) Uani ? ? 1.00000 ? ? C1114 .7514(8) 1.0957(5) .3416(5) .035(7) Uani ? ? 1.00000 ? ? C1115 .7911(8) 1.0698(6) .2713(5) .038(7) Uani ? ? 1.00000 ? ? C1116 .7013(8) 1.0775(5) .2182(5) .030(6) Uani ? ? 1.00000 ? ? C1121 .5306(7) 1.1558(5) .0868(5) .027(6) Uani ? ? 1.00000 ? ? C1122 .6012(8) 1.1048(6) .0322(4) .033(7) Uani ? ? 1.00000 ? ? C1123 .6689(8) 1.1353(6) -.0204(5) .035(7) Uani ? ? 1.00000 ? ? C1124 .6637(9) 1.2172(6) -.0194(5) .043(7) Uani ? ? 1.00000 ? ? C1125 .5922(13) 1.2691(6) .0329(8) .083(12) Uani ? ? 1.00000 ? ? C1126 .5263(11) 1.2383(6) .0860(7) .065(9) Uani ? ? 1.00000 ? ? C110 .4877(7) 1.0038(5) .1416(5) .025(6) Uani ? ? 1.00000 ? ? C120 .4225(7) .9652(5) .2000(4) .023(5) Uani ? ? 1.00000 ? ? P12 .26141(18) 1.04046(12) .22093(10) .0169(13) Uani ? ? 1.00000 ? ? C1211 .2440(7) 1.0181(4) .3200(4) .019(5) Uani ? ? 1.00000 ? ? C1212 .1352(8) 1.0072(5) .3498(4) .030(6) Uani ? ? 1.00000 ? ? C1213 .1184(9) 1.0013(6) .4253(5) .041(7) Uani ? ? 1.00000 ? ? C1214 .2107(9) 1.0052(6) .4738(5) .041(7) Uani ? ? 1.00000 ? ? C1215 .3217(8) 1.0136(5) .4446(5) .033(6) Uani ? ? 1.00000 ? ? C1216 .3390(8) 1.0203(5) .3691(4) .027(6) Uani ? ? 1.00000 ? ? C1221 .1555(7) .9885(5) .1812(4) .022(5) Uani ? ? 1.00000 ? ? C1222 .0654(7) 1.0301(5) .1310(4) .023(6) Uani ? ? 1.00000 ? ? C1223 -.0094(8) .9880(6) .0993(4) .036(7) Uani ? ? 1.00000 ? ? C1224 .0061(9) .9055(6) .1163(5) .040(8) Uani ? ? 1.00000 ? ? C1225 .0949(9) .8626(6) .1675(5) .039(7) Uani ? ? 1.00000 ? ? C1226 .1728(8) .9024(5) .2010(4) .027(6) Uani ? ? 1.00000 ? ? C11 .2380(7) 1.1457(5) .0795(4) .025(6) Uani ? ? 1.00000 ? ? C12 .2363(8) 1.1353(6) .0166(5) .034(7) Uani ? ? 1.00000 ? ? C101 .1510(7) 1.3146(4) .1650(4) .024(5) Uani ? ? 1.00000 ? ? C1011 .1646(9) 1.3621(5) .0971(5) .038(7) Uani ? ? 1.00000 ? ? C102 .0523(7) 1.2764(5) .1775(5) .032(6) Uani ? ? 1.00000 ? ? C1021 -.0504(8) 1.2790(6) .1261(6) .047(8) Uani ? ? 1.00000 ? ? C103 .0665(8) 1.2444(5) .2530(5) .029(6) Uani ? ? 1.00000 ? ? C1031 -.0248(9) 1.2094(6) .2930(6) .045(7) Uani ? ? 1.00000 ? ? C104 .1703(8) 1.2614(5) .2861(4) .029(6) Uani ? ? 1.00000 ? ? C1041 .2006(10) 1.2506(6) .3672(5) .049(8) Uani ? ? 1.00000 ? ? C105 .2201(8) 1.3053(5) .2317(4) .025(6) Uani ? ? 1.00000 ? ? C1051 .3209(9) 1.3451(6) .2459(5) .042(7) Uani ? ? 1.00000 ? ? P21 .05071(18) .37948(12) .67633(11) .0195(13) Uani ? ? 1.00000 ? ? C2111 -.0403(7) .3749(5) .7622(5) .027(6) Uani ? ? 1.00000 ? ? C2112 .0258(8) .3442(5) .8274(5) .033(6) Uani ? ? 1.00000 ? ? C2113 -.0381(9) .3413(6) .8932(5) .040(7) Uani ? ? 1.00000 ? ? C2114 -.1694(10) .3693(6) .8941(5) .049(9) Uani ? ? 1.00000 ? ? C2115 -.2374(8) .4016(6) .8305(5) .039(7) Uani ? ? 1.00000 ? ? C2116 -.1723(8) .4032(6) .7645(5) .039(7) Uani ? ? 1.00000 ? ? C2121 -.0350(7) .3372(5) .6107(4) .025(6) Uani ? ? 1.00000 ? ? C2122 -.0735(9) .3769(6) .5423(5) .039(7) Uani ? ? 1.00000 ? ? C2123 -.1397(10) .3421(7) .4934(5) .047(8) Uani ? ? 1.00000 ? ? C2124 -.1629(10) .2680(7) .5107(6) .051(9) Uani ? ? 1.00000 ? ? C2125 -.1234(10) .2291(6) .5793(6) .051(9) Uani ? ? 1.00000 ? ? C2126 -.0625(9) .2644(6) .6284(5) .038(7) Uani ? ? 1.00000 ? ? C210 -.0015(7) .4938(5) .6557(5) .027(6) Uani ? ? 1.00000 ? ? C220 .0704(7) .5356(5) .7036(4) .023(5) Uani ? ? 1.00000 ? ? P22 .23819(18) .46448(12) .71624(10) .0169(13) Uani ? ? 1.00000 ? ? C2211 .2662(7) .4795(4) .8148(4) .020(5) Uani ? ? 1.00000 ? ? C2212 .3813(8) .4851(5) .8380(4) .028(6) Uani ? ? 1.00000 ? ? C2213 .4065(9) .4850(6) .9123(5) .043(8) Uani ? ? 1.00000 ? ? C2214 .3163(9) .4834(6) .9638(5) .042(8) Uani ? ? 1.00000 ? ? C2215 .2008(9) .4802(5) .9431(4) .033(7) Uani ? ? 1.00000 ? ? C2216 .1747(8) .4783(5) .8684(4) .028(6) Uani ? ? 1.00000 ? ? C2221 .3332(8) .5247(5) .6735(4) .026(6) Uani ? ? 1.00000 ? ? C2222 .4279(8) .4891(5) .6218(4) .030(6) Uani ? ? 1.00000 ? ? C2223 .4991(9) .5361(7) .5915(5) .045(8) Uani ? ? 1.00000 ? ? C2224 .4766(10) .6187(6) .6121(5) .045(8) Uani ? ? 1.00000 ? ? C2225 .3830(9) .6563(6) .6628(5) .037(7) Uani ? ? 1.00000 ? ? C2226 .3150(8) .6074(5) .6933(6) .041(7) Uani ? ? 1.00000 ? ? C21 .2479(7) .3757(5) .5734(4) .024(6) Uani ? ? 1.00000 ? ? C22 .2402(8) .3976(6) .5117(5) .036(7) Uani ? ? 1.00000 ? ? C201 .3496(8) .1940(4) .6551(4) .026(6) Uani ? ? 1.00000 ? ? C2011 .3105(9) .1468(6) .5958(6) .044(7) Uani ? ? 1.00000 ? ? C202 .4507(8) .2312(5) .6480(5) .035(6) Uani ? ? 1.00000 ? ? C2021 .5284(10) .2316(6) .5802(6) .053(8) Uani ? ? 1.00000 ? ? C203 .4666(7) .2623(5) .7189(5) .033(6) Uani ? ? 1.00000 ? ? C2031 .5673(9) .2988(6) .7396(7) .056(8) Uani ? ? 1.00000 ? ? C204 .3792(8) .2439(5) .7699(4) .027(6) Uani ? ? 1.00000 ? ? C2041 .3797(10) .2537(6) .8527(5) .051(8) Uani ? ? 1.00000 ? ? C205 .3056(7) .2011(5) .7301(5) .027(6) Uani ? ? 1.00000 ? ? C2051 .2201(9) .1582(5) .7624(5) .038(7) Uani ? ? 1.00000 ? ? H1112 .44324 1.15769 .31669 .03900 Uiso ? ? 1.00000 ? ? H1113 .60100 1.14459 .41086 .05000 Uiso ? ? 1.00000 ? ? H1114 .81426 1.09098 .37979 .04400 Uiso ? ? 1.00000 ? ? H1115 .88024 1.04531 .25851 .04600 Uiso ? ? 1.00000 ? ? H1116 .72748 1.06093 .16812 .03800 Uiso ? ? 1.00000 ? ? H1122 .60279 1.04637 .03091 .03900 Uiso ? ? 1.00000 ? ? H1123 .72036 1.09742 -.05766 .04100 Uiso ? ? 1.00000 ? ? H1124 .71156 1.23821 -.05453 .05700 Uiso ? ? 1.00000 ? ? H1125 .58796 1.32821 .03416 .09200 Uiso ? ? 1.00000 ? ? H1126 .47702 1.27646 .12387 .07800 Uiso ? ? 1.00000 ? ? H110a .45544 .99910 .09319 .02800 Uiso ? ? 1.00000 ? ? H110b .57747 .97509 .14034 .02800 Uiso ? ? 1.00000 ? ? H120a .47202 .95328 .24416 .02800 Uiso ? ? 1.00000 ? ? H120b .41519 .91305 .18333 .02800 Uiso ? ? 1.00000 ? ? H1212 .07042 1.00333 .31733 .03700 Uiso ? ? 1.00000 ? ? H1213 .04294 .99380 .44558 .04700 Uiso ? ? 1.00000 ? ? H1214 .19953 1.00101 .52632 .05000 Uiso ? ? 1.00000 ? ? H1215 .38723 1.01553 .47819 .04200 Uiso ? ? 1.00000 ? ? H1216 .41730 1.02713 .34958 .03200 Uiso ? ? 1.00000 ? ? H1222 .05294 1.08824 .11756 .02900 Uiso ? ? 1.00000 ? ? H1223 -.07453 1.01810 .06611 .04500 Uiso ? ? 1.00000 ? ? H1224 -.04529 .87849 .09084 .04600 Uiso ? ? 1.00000 ? ? H1225 .10473 .80430 .17916 .05100 Uiso ? ? 1.00000 ? ? H1226 .23699 .87264 .23728 .03500 Uiso ? ? 1.00000 ? ? H12 .23594 1.12517 -.03618 .04800 Uiso ? ? 1.00000 ? ? H1011a .22898 1.38690 .10245 .05600 Uiso ? ? 1.00000 ? ? H1011b .08549 1.40642 .08715 .05600 Uiso ? ? 1.00000 ? ? H1011c .18430 1.32584 .05542 .05600 Uiso ? ? 1.00000 ? ? H1021a -.11343 1.33380 .12430 .06600 Uiso ? ? 1.00000 ? ? H1021b -.08911 1.23821 .13933 .06600 Uiso ? ? 1.00000 ? ? H1021c -.01591 1.26693 .07623 .06600 Uiso ? ? 1.00000 ? ? H1031a .01471 1.17745 .33546 .06000 Uiso ? ? 1.00000 ? ? H1031b -.04893 1.17226 .26106 .06000 Uiso ? ? 1.00000 ? ? H1031c -.09893 1.25392 .30836 .06000 Uiso ? ? 1.00000 ? ? H1041a .12921 1.28746 .39307 .07200 Uiso ? ? 1.00000 ? ? H1041b .27102 1.27273 .37366 .07200 Uiso ? ? 1.00000 ? ? H1041c .21904 1.19422 .38518 .07200 Uiso ? ? 1.00000 ? ? H1051a .37124 1.34508 .20269 .06100 Uiso ? ? 1.00000 ? ? H1051b .37796 1.31338 .28413 .06100 Uiso ? ? 1.00000 ? ? H1051c .28456 1.40162 .26211 .06100 Uiso ? ? 1.00000 ? ? H2112 .11814 .32363 .82684 .04000 Uiso ? ? 1.00000 ? ? H2113 .00794 .32125 .93804 .04900 Uiso ? ? 1.00000 ? ? H2114 -.21373 .36550 .93926 .06100 Uiso ? ? 1.00000 ? ? H2115 -.32886 .42248 .83238 .05100 Uiso ? ? 1.00000 ? ? H2116 -.21909 .42399 .71988 .04600 Uiso ? ? 1.00000 ? ? H2122 -.05668 .42902 .52898 .04700 Uiso ? ? 1.00000 ? ? H2123 -.16990 .37017 .44768 .05900 Uiso ? ? 1.00000 ? ? H2124 -.20572 .24323 .47675 .05900 Uiso ? ? 1.00000 ? ? H2125 -.14041 .17704 .59292 .06100 Uiso ? ? 1.00000 ? ? H2126 -.03950 .23742 .67613 .04300 Uiso ? ? 1.00000 ? ? H210a .01536 .50299 .60508 .03400 Uiso ? ? 1.00000 ? ? H210b -.09071 .51727 .66488 .03400 Uiso ? ? 1.00000 ? ? H220a .02844 .54716 .75142 .03000 Uiso ? ? 1.00000 ? ? H220b .06914 .58825 .68194 .03000 Uiso ? ? 1.00000 ? ? H2212 .44370 .48843 .80168 .03700 Uiso ? ? 1.00000 ? ? H2213 .48927 .48534 .92758 .05500 Uiso ? ? 1.00000 ? ? H2214 .33301 .48464 1.01659 .05000 Uiso ? ? 1.00000 ? ? H2215 .13785 .47906 .98049 .03900 Uiso ? ? 1.00000 ? ? H2216 .09382 .47567 .85303 .03300 Uiso ? ? 1.00000 ? ? H2222 .44360 .43144 .60685 .03700 Uiso ? ? 1.00000 ? ? H2223 .56473 .51188 .55571 .05200 Uiso ? ? 1.00000 ? ? H2224 .52836 .64932 .58986 .05400 Uiso ? ? 1.00000 ? ? H2225 .36492 .71517 .67540 .04700 Uiso ? ? 1.00000 ? ? H2226 .25305 .63113 .73295 .05200 Uiso ? ? 1.00000 ? ? H22 .23190 .41659 .45980 .05500 Uiso ? ? 1.00000 ? ? H2011a .38027 .09722 .58488 .06400 Uiso ? ? 1.00000 ? ? H2011b .23595 .13341 .61319 .06400 Uiso ? ? 1.00000 ? ? H2011c .28840 .18086 .55150 .06400 Uiso ? ? 1.00000 ? ? H2021a .58068 .26435 .59041 .07500 Uiso ? ? 1.00000 ? ? H2021b .57910 .17480 .57134 .07500 Uiso ? ? 1.00000 ? ? H2021c .47416 .25733 .53874 .07500 Uiso ? ? 1.00000 ? ? H2031a .64870 .25859 .72767 .08000 Uiso ? ? 1.00000 ? ? H2031b .55773 .34893 .70960 .08000 Uiso ? ? 1.00000 ? ? H2031c .56318 .31114 .79008 .08000 Uiso ? ? 1.00000 ? ? H2041a .44983 .21450 .87692 .07400 Uiso ? ? 1.00000 ? ? H2041b .37073 .30947 .86781 .07400 Uiso ? ? 1.00000 ? ? H2041c .30350 .24596 .87318 .07400 Uiso ? ? 1.00000 ? ? H2051a .13421 .18696 .74885 .05700 Uiso ? ? 1.00000 ? ? H2051b .24404 .10127 .74709 .05700 Uiso ? ? 1.00000 ? ? H2051c .22455 .15822 .81558 .05700 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os1 .01240(16) .01339(16) .01868(17) .00020(12) .00109(11) .00129(11) Os2 .01222(16) .01296(16) .01962(17) -.00071(12) -.00049(12) -.00124(11) P11 .0128(10) .0180(10) .0247(11) -.0022(8) .0002(8) .0018(8) C1111 .022(4) .014(4) .037(5) -.008(3) -.007(3) .005(3) C1112 .038(5) .014(4) .046(5) -.015(4) -.008(4) .006(4) C1113 .063(7) .036(5) .031(5) -.026(5) -.005(5) .001(4) C1114 .027(5) .033(5) .055(6) -.022(4) -.016(4) .017(4) C1115 .027(5) .044(6) .046(6) -.015(4) -.016(4) .014(4) C1116 .026(5) .034(5) .034(5) -.013(4) -.006(4) .008(4) C1121 .015(4) .027(4) .038(5) -.005(4) -.004(3) .006(4) C1122 .035(5) .039(5) .025(5) -.014(4) .005(4) -.002(4) C1123 .032(5) .048(6) .029(5) -.019(5) -.000(4) .005(4) C1124 .031(5) .046(6) .051(6) -.014(5) .020(4) .010(5) C1125 .105(11) .028(6) .116(11) -.025(7) .069(9) .001(6) C1126 .071(8) .023(5) .089(9) -.003(5) .059(7) .001(5) C110 .016(4) .017(4) .040(5) -.001(3) .003(4) -.004(3) C120 .013(4) .018(4) .035(5) -.003(3) .000(3) .003(3) P12 .0141(10) .0164(10) .0183(10) -.0022(8) .0009(8) -.0006(7) C1211 .023(4) .010(4) .023(4) -.004(3) -.001(3) .001(3) C1212 .029(5) .035(5) .024(4) -.009(4) .000(4) .001(4) C1213 .035(5) .061(7) .030(5) -.022(5) .008(4) .002(4) C1214 .051(6) .045(6) .022(5) -.010(5) .002(4) .006(4) C1215 .033(5) .029(5) .033(5) -.006(4) -.008(4) -.003(4) C1216 .028(5) .027(4) .027(4) -.011(4) -.004(4) .004(3) C1221 .020(4) .025(4) .022(4) -.010(4) .005(3) -.004(3) C1222 .017(4) .035(5) .019(4) -.012(4) .001(3) .002(3) C1223 .025(5) .067(7) .020(4) -.022(5) .001(4) -.000(4) C1224 .039(6) .062(6) .034(5) -.035(5) .009(4) -.014(4) C1225 .034(5) .043(6) .047(6) -.021(5) .006(4) -.011(4) C1226 .035(5) .031(5) .012(4) -.008(4) .004(3) -.003(3) C11 .014(4) .026(4) .031(5) -.002(3) -.003(3) -.000(3) C12 .031(5) .039(5) .033(5) -.014(4) -.008(4) .006(4) C101 .017(4) .010(4) .039(5) .003(3) .005(3) .003(3) C1011 .037(5) .029(5) .042(6) -.006(4) .008(4) .017(4) C102 .012(4) .011(4) .065(6) .005(3) -.002(4) .003(4) C1021 .021(5) .032(5) .083(8) -.002(4) -.014(5) -.006(5) C103 .023(4) .010(4) .047(5) .003(3) .015(4) -.001(3) C1031 .037(6) .031(5) .062(7) -.006(4) .024(5) -.001(5) C104 .035(5) .020(4) .025(4) -.001(4) .008(4) -.008(3) C1041 .066(7) .033(5) .032(5) .003(5) .012(5) -.004(4) C105 .024(4) .018(4) .029(4) -.001(4) .003(3) .002(3) C1051 .041(6) .031(5) .057(6) -.014(5) .002(5) -.009(4) P21 .0137(10) .0170(10) .0261(11) -.0025(8) -.0005(8) .0005(8) C2111 .019(4) .020(4) .046(5) -.010(4) .008(4) -.011(4) C2112 .031(5) .031(5) .039(5) -.016(4) .003(4) -.003(4) C2113 .052(6) .038(5) .037(5) -.027(5) .012(4) -.009(4) C2114 .058(7) .058(7) .050(6) -.043(6) .032(5) -.027(5) C2115 .025(5) .049(6) .053(6) -.025(5) .021(4) -.022(5) C2116 .027(5) .037(5) .054(6) -.011(4) .007(4) -.014(4) C2121 .013(4) .024(4) .036(5) -.005(3) -.005(3) -.003(3) C2122 .051(6) .048(6) .030(5) -.031(5) .004(4) -.006(4) C2123 .051(6) .071(7) .029(5) -.035(6) -.010(4) .005(5) C2124 .044(6) .064(7) .053(6) -.027(6) .001(5) -.023(5) C2125 .054(7) .037(6) .068(7) -.023(5) -.015(5) .001(5) C2126 .042(6) .036(5) .041(5) -.021(5) -.017(4) .005(4) C210 .018(4) .019(4) .040(5) .000(4) -.006(3) -.001(3) C220 .022(4) .012(4) .031(5) .000(3) -.005(3) .000(3) P22 .0159(10) .0150(9) .0191(10) -.0040(8) .0001(8) -.0005(7) C2211 .023(4) .010(4) .022(4) .000(3) .002(3) -.003(3) C2212 .026(5) .030(5) .025(4) -.004(4) -.004(3) -.004(3) C2213 .035(5) .059(7) .039(6) -.019(5) -.012(4) -.002(5) C2214 .047(6) .049(6) .031(5) -.016(5) -.006(4) -.003(4) C2215 .046(6) .028(5) .023(5) -.008(4) .005(4) .003(3) C2216 .032(5) .023(4) .026(4) -.004(4) -.000(4) -.001(3) C2221 .027(5) .026(4) .030(5) -.015(4) -.008(4) -.000(3) C2222 .035(5) .042(5) .017(4) -.020(4) .005(4) -.005(4) C2223 .042(6) .070(7) .034(5) -.033(6) .011(4) -.013(5) C2224 .057(7) .064(7) .032(5) -.046(6) -.006(5) .008(5) C2225 .045(6) .040(5) .030(5) -.021(5) .001(4) .004(4) C2226 .023(5) .027(5) .070(7) -.005(4) -.001(4) -.011(4) C21 .018(4) .021(4) .034(5) -.008(3) .003(3) -.006(3) C22 .033(5) .046(6) .033(5) -.017(5) .002(4) -.006(4) C201 .026(5) .010(4) .037(5) .001(3) -.005(4) -.009(3) C2011 .038(6) .027(5) .061(7) -.001(4) -.012(5) -.016(4) C202 .024(5) .025(5) .053(6) -.002(4) .005(4) -.010(4) C2021 .041(6) .045(6) .069(7) -.009(5) .026(5) -.012(5) C203 .013(4) .014(4) .064(6) .007(3) -.013(4) -.010(4) C2031 .019(5) .027(5) .116(10) .001(4) -.028(5) -.005(5) C204 .032(5) .018(4) .023(4) .002(4) -.010(4) -.001(3) C2041 .063(7) .034(5) .039(6) .006(5) -.026(5) .005(4) C205 .019(4) .010(4) .040(5) .008(3) .003(4) .004(3) C2051 .039(6) .022(5) .052(6) -.009(4) .003(4) .007(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Os1 P11 . . 2.2653(19) ? Os1 P12 . . 2.263(2) ? Os1 C11 . . 2.017(8) ? Os1 C101 . . 2.252(7) ? Os1 C102 . . 2.245(7) ? Os1 C103 . . 2.265(8) ? Os1 C104 . . 2.302(8) ? Os1 C105 . . 2.283(8) ? Os2 P21 . . 2.262(2) ? Os2 P22 . . 2.258(2) ? Os2 C21 . . 2.043(8) ? Os2 C201 . . 2.235(7) ? Os2 C202 . . 2.268(7) ? Os2 C203 . . 2.274(7) ? Os2 C204 . . 2.270(7) ? Os2 C205 . . 2.251(7) ? P11 C1111 . . 1.849(8) ? P11 C1121 . . 1.837(9) ? P11 C110 . . 1.856(8) ? C1111 C1112 . . 1.355(11) ? C1111 C1116 . . 1.394(11) ? C1112 C1113 . . 1.423(13) ? C1112 H1112 . . .972 ? C1113 C1114 . . 1.373(13) ? C1113 H1113 . . .961 ? C1114 C1115 . . 1.372(13) ? C1114 H1114 . . .978 ? C1115 C1116 . . 1.374(13) ? C1115 H1115 . . .968 ? C1116 H1116 . . .967 ? C1121 C1122 . . 1.377(11) ? C1121 C1126 . . 1.365(13) ? C1122 C1123 . . 1.392(13) ? C1122 H1122 . . .974 ? C1123 C1124 . . 1.355(14) ? C1123 H1123 . . .976 ? C1124 C1125 . . 1.359(15) ? C1124 H1124 . . .954 ? C1125 C1126 . . 1.390(19) ? C1125 H1125 . . .975 ? C1126 H1126 . . .978 ? C110 C120 . . 1.521(12) ? C110 H110a . . .968 ? C110 H110b . . .957 ? C120 P12 . . 1.862(7) ? C120 H120a . . .960 ? C120 H120b . . .958 ? P12 C1211 . . 1.845(7) ? P12 C1221 . . 1.843(9) ? C1211 C1212 . . 1.382(12) ? C1211 C1216 . . 1.405(12) ? C1212 C1213 . . 1.382(12) ? C1212 H1212 . . .959 ? C1213 C1214 . . 1.383(14) ? C1213 H1213 . . .955 ? C1214 C1215 . . 1.383(14) ? C1214 H1214 . . .962 ? C1215 C1216 . . 1.384(11) ? C1215 H1215 . . .969 ? C1216 H1216 . . .975 ? C1221 C1222 . . 1.367(10) ? C1221 C1226 . . 1.428(12) ? C1222 C1223 . . 1.393(14) ? C1222 H1222 . . .962 ? C1223 C1224 . . 1.362(15) ? C1223 H1223 . . .951 ? C1224 C1225 . . 1.376(12) ? C1224 H1224 . . .965 ? C1225 C1226 . . 1.407(14) ? C1225 H1225 . . .964 ? C1226 H1226 . . .980 ? C11 C12 . . 1.159(12) ? C12 H12 . . .975 ? C101 C1011 . . 1.482(12) ? C101 C102 . . 1.453(13) ? C101 C105 . . 1.423(11) ? C1011 H1011a . . .946 ? C1011 H1011b . . .965 ? C1011 H1011c . . .956 ? C102 C1021 . . 1.477(14) ? C102 C103 . . 1.450(12) ? C1021 H1021a . . .956 ? C1021 H1021b . . .944 ? C1021 H1021c . . .973 ? C103 C1031 . . 1.498(14) ? C103 C104 . . 1.423(13) ? C1031 H1031a . . .955 ? C1031 H1031b . . .961 ? C1031 H1031c . . .956 ? C104 C1041 . . 1.506(12) ? C104 C105 . . 1.425(12) ? C1041 H1041a . . .955 ? C1041 H1041b . . .980 ? C1041 H1041c . . .949 ? C105 C1051 . . 1.508(15) ? C1051 H1051a . . .955 ? C1051 H1051b . . .972 ? C1051 H1051c . . .951 ? P21 C2111 . . 1.856(9) ? P21 C2121 . . 1.830(9) ? P21 C210 . . 1.840(8) ? C2111 C2112 . . 1.399(12) ? C2111 C2116 . . 1.389(12) ? C2112 C2113 . . 1.385(13) ? C2112 H2112 . . .972 ? C2113 C2114 . . 1.382(14) ? C2113 H2113 . . .962 ? C2114 C2115 . . 1.388(13) ? C2114 H2114 . . .959 ? C2115 C2116 . . 1.392(13) ? C2115 H2115 . . .963 ? C2116 H2116 . . .965 ? C2121 C2122 . . 1.399(11) ? C2121 C2126 . . 1.379(13) ? C2122 C2123 . . 1.412(16) ? C2122 H2122 . . .975 ? C2123 C2124 . . 1.374(17) ? C2123 H2123 . . .954 ? C2124 C2125 . . 1.400(14) ? C2124 H2124 . . .963 ? C2125 C2126 . . 1.382(16) ? C2125 H2125 . . .976 ? C2126 H2126 . . .965 ? C210 C220 . . 1.518(13) ? C210 H210a . . .951 ? C210 H210b . . .955 ? C220 P22 . . 1.872(7) ? C220 H220a . . .970 ? C220 H220b . . .952 ? P22 C2211 . . 1.856(8) ? P22 C2221 . . 1.835(9) ? C2211 C2212 . . 1.387(12) ? C2211 C2216 . . 1.399(11) ? C2212 C2213 . . 1.380(12) ? C2212 H2212 . . .962 ? C2213 C2214 . . 1.364(14) ? C2213 H2213 . . .969 ? C2214 C2215 . . 1.365(15) ? C2214 H2214 . . .980 ? C2215 C2216 . . 1.393(11) ? C2215 H2215 . . .971 ? C2216 H2216 . . .962 ? C2221 C2222 . . 1.386(11) ? C2221 C2226 . . 1.386(12) ? C2222 C2223 . . 1.387(15) ? C2222 H2222 . . .967 ? C2223 C2224 . . 1.381(15) ? C2223 H2223 . . .958 ? C2224 C2225 . . 1.375(12) ? C2224 H2224 . . .965 ? C2225 C2226 . . 1.386(15) ? C2225 H2225 . . .971 ? C2226 H2226 . . .982 ? C21 C22 . . 1.165(12) ? C22 H22 . . .982 ? C201 C2011 . . 1.501(14) ? C201 C202 . . 1.456(14) ? C201 C205 . . 1.430(11) ? C2011 H2011a . . .954 ? C2011 H2011b . . .973 ? C2011 H2011c . . .961 ? C202 C2021 . . 1.491(14) ? C202 C203 . . 1.432(13) ? C2021 H2021a . . .943 ? C2021 H2021b . . .949 ? C2021 H2021c . . .973 ? C203 C2031 . . 1.498(14) ? C203 C204 . . 1.432(12) ? C2031 H2031a . . .959 ? C2031 H2031b . . .966 ? C2031 H2031c . . .940 ? C204 C2041 . . 1.512(12) ? C204 C205 . . 1.460(13) ? C2041 H2041a . . .948 ? C2041 H2041b . . .952 ? C2041 H2041c . . .965 ? C205 C2051 . . 1.473(14) ? C2051 H2051a . . .953 ? C2051 H2051b . . .949 ? C2051 H2051c . . .965 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P11 Os1 P12 . . . 82.68(7) ? P11 Os1 C11 . . . 80.3(2) ? P11 Os1 C101 . . . 118.1(2) ? P11 Os1 C102 . . . 154.2(2) ? P11 Os1 C103 . . . 156.2(2) ? P11 Os1 C104 . . . 120.5(2) ? P11 Os1 C105 . . . 104.4(2) ? P12 Os1 C11 . . . 90.4(2) ? P12 Os1 C101 . . . 159.3(2) ? P12 Os1 C102 . . . 121.9(2) ? P12 Os1 C103 . . . 99.2(2) ? P12 Os1 C104 . . . 108.9(2) ? P12 Os1 C105 . . . 143.1(2) ? C11 Os1 C101 . . . 93.4(3) ? C11 Os1 C102 . . . 91.2(3) ? C11 Os1 C103 . . . 123.3(3) ? C11 Os1 C104 . . . 152.5(3) ? C11 Os1 C105 . . . 126.4(3) ? C101 Os1 C102 . . . 37.7(3) ? C101 Os1 C103 . . . 61.9(3) ? C101 Os1 C104 . . . 61.7(3) ? C101 Os1 C105 . . . 36.6(3) ? C102 Os1 C103 . . . 37.5(3) ? C102 Os1 C104 . . . 62.2(3) ? C102 Os1 C105 . . . 61.5(3) ? C103 Os1 C104 . . . 36.3(3) ? C103 Os1 C105 . . . 60.2(3) ? C104 Os1 C105 . . . 36.2(3) ? P21 Os2 P22 . . . 82.88(7) ? P21 Os2 C21 . . . 82.4(2) ? P21 Os2 C201 . . . 113.3(2) ? P21 Os2 C202 . . . 148.5(3) ? P21 Os2 C203 . . . 160.8(2) ? P21 Os2 C204 . . . 124.1(2) ? P21 Os2 C205 . . . 102.2(2) ? P22 Os2 C21 . . . 88.2(2) ? P22 Os2 C201 . . . 163.4(2) ? P22 Os2 C202 . . . 127.3(3) ? P22 Os2 C203 . . . 101.3(2) ? P22 Os2 C204 . . . 106.4(2) ? P22 Os2 C205 . . . 139.1(2) ? C21 Os2 C201 . . . 97.3(3) ? C21 Os2 C202 . . . 89.1(3) ? C21 Os2 C203 . . . 116.3(3) ? C21 Os2 C204 . . . 150.5(3) ? C21 Os2 C205 . . . 132.7(3) ? C201 Os2 C202 . . . 37.7(3) ? C201 Os2 C203 . . . 62.2(3) ? C201 Os2 C204 . . . 62.2(3) ? C201 Os2 C205 . . . 37.2(3) ? C202 Os2 C203 . . . 36.7(3) ? C202 Os2 C204 . . . 61.6(3) ? C202 Os2 C205 . . . 62.5(3) ? C203 Os2 C204 . . . 36.7(3) ? C203 Os2 C205 . . . 62.3(3) ? C204 Os2 C205 . . . 37.7(3) ? Os1 P11 C1111 . . . 121.3(2) ? Os1 P11 C1121 . . . 121.2(2) ? Os1 P11 C110 . . . 108.4(3) ? C1111 P11 C1121 . . . 98.7(4) ? C1111 P11 C110 . . . 101.3(3) ? C1121 P11 C110 . . . 103.0(4) ? P11 C1111 C1112 . . . 120.1(6) ? P11 C1111 C1116 . . . 119.5(6) ? C1112 C1111 C1116 . . . 120.3(8) ? C1111 C1112 C1113 . . . 119.9(8) ? C1111 C1112 H1112 . . . 119.6 ? C1113 C1112 H1112 . . . 120.5 ? C1112 C1113 C1114 . . . 118.0(8) ? C1112 C1113 H1113 . . . 122.1 ? C1114 C1113 H1113 . . . 119.9 ? C1113 C1114 C1115 . . . 122.4(9) ? C1113 C1114 H1114 . . . 118.0 ? C1115 C1114 H1114 . . . 119.6 ? C1114 C1115 C1116 . . . 118.8(8) ? C1114 C1115 H1115 . . . 121.9 ? C1116 C1115 H1115 . . . 119.3 ? C1111 C1116 C1115 . . . 120.6(8) ? C1111 C1116 H1116 . . . 119.4 ? C1115 C1116 H1116 . . . 120.0 ? P11 C1121 C1122 . . . 123.6(7) ? P11 C1121 C1126 . . . 118.8(7) ? C1122 C1121 C1126 . . . 117.4(9) ? C1121 C1122 C1123 . . . 121.5(9) ? C1121 C1122 H1122 . . . 118.4 ? C1123 C1122 H1122 . . . 120.2 ? C1122 C1123 C1124 . . . 119.9(8) ? C1122 C1123 H1123 . . . 119.9 ? C1124 C1123 H1123 . . . 120.2 ? C1123 C1124 C1125 . . . 119.6(10) ? C1123 C1124 H1124 . . . 120.4 ? C1125 C1124 H1124 . . . 120.0 ? C1124 C1125 C1126 . . . 120.4(10) ? C1124 C1125 H1125 . . . 120.3 ? C1126 C1125 H1125 . . . 119.3 ? C1121 C1126 C1125 . . . 121.2(9) ? C1121 C1126 H1126 . . . 119.8 ? C1125 C1126 H1126 . . . 119.0 ? P11 C110 C120 . . . 108.0(5) ? P11 C110 H110a . . . 109.8 ? P11 C110 H110b . . . 110.3 ? C120 C110 H110a . . . 110.1 ? C120 C110 H110b . . . 111.3 ? H110a C110 H110b . . . 107.4 ? C110 C120 P12 . . . 109.7(5) ? C110 C120 H120a . . . 109.6 ? C110 C120 H120b . . . 110.7 ? P12 C120 H120a . . . 109.4 ? P12 C120 H120b . . . 109.6 ? H120a C120 H120b . . . 108.0 ? Os1 P12 C120 . . . 112.2(3) ? Os1 P12 C1211 . . . 117.7(2) ? Os1 P12 C1221 . . . 119.9(2) ? C120 P12 C1211 . . . 101.5(3) ? C120 P12 C1221 . . . 102.7(3) ? C1211 P12 C1221 . . . 100.2(4) ? P12 C1211 C1212 . . . 122.8(6) ? P12 C1211 C1216 . . . 119.4(6) ? C1212 C1211 C1216 . . . 117.6(7) ? C1211 C1212 C1213 . . . 121.4(8) ? C1211 C1212 H1212 . . . 119.1 ? C1213 C1212 H1212 . . . 119.5 ? C1212 C1213 C1214 . . . 121.1(9) ? C1212 C1213 H1213 . . . 121.0 ? C1214 C1213 H1213 . . . 117.8 ? C1213 C1214 C1215 . . . 118.0(8) ? C1213 C1214 H1214 . . . 121.4 ? C1215 C1214 H1214 . . . 120.5 ? C1214 C1215 C1216 . . . 121.3(8) ? C1214 C1215 H1215 . . . 118.5 ? C1216 C1215 H1215 . . . 120.2 ? C1211 C1216 C1215 . . . 120.5(8) ? C1211 C1216 H1216 . . . 119.3 ? C1215 C1216 H1216 . . . 120.1 ? P12 C1221 C1222 . . . 120.7(7) ? P12 C1221 C1226 . . . 119.0(6) ? C1222 C1221 C1226 . . . 120.2(8) ? C1221 C1222 C1223 . . . 119.5(8) ? C1221 C1222 H1222 . . . 120.6 ? C1223 C1222 H1222 . . . 119.9 ? C1222 C1223 C1224 . . . 121.7(8) ? C1222 C1223 H1223 . . . 119.0 ? C1224 C1223 H1223 . . . 119.3 ? C1223 C1224 C1225 . . . 119.9(10) ? C1223 C1224 H1224 . . . 118.3 ? C1225 C1224 H1224 . . . 121.8 ? C1224 C1225 C1226 . . . 120.5(9) ? C1224 C1225 H1225 . . . 119.2 ? C1226 C1225 H1225 . . . 120.3 ? C1221 C1226 C1225 . . . 118.2(7) ? C1221 C1226 H1226 . . . 120.2 ? C1225 C1226 H1226 . . . 121.7 ? Os1 C11 C12 . . . 174.4(8) ? C11 C12 H12 . . . 178.7 ? Os1 C101 C1011 . . . 126.5(5) ? Os1 C101 C102 . . . 70.9(4) ? Os1 C101 C105 . . . 72.9(4) ? C1011 C101 C102 . . . 124.6(8) ? C1011 C101 C105 . . . 127.7(8) ? C102 C101 C105 . . . 107.4(7) ? C101 C1011 H1011a . . . 110.9 ? C101 C1011 H1011b . . . 109.7 ? C101 C1011 H1011c . . . 110.8 ? H1011a C1011 H1011b . . . 108.5 ? H1011a C1011 H1011c . . . 109.2 ? H1011b C1011 H1011c . . . 107.6 ? Os1 C102 C101 . . . 71.4(4) ? Os1 C102 C1021 . . . 126.8(6) ? Os1 C102 C103 . . . 72.0(4) ? C101 C102 C1021 . . . 126.2(8) ? C101 C102 C103 . . . 106.2(7) ? C1021 C102 C103 . . . 127.2(8) ? C102 C1021 H1021a . . . 111.3 ? C102 C1021 H1021b . . . 111.2 ? C102 C1021 H1021c . . . 109.9 ? H1021a C1021 H1021b . . . 109.5 ? H1021a C1021 H1021c . . . 107.0 ? H1021b C1021 H1021c . . . 107.8 ? Os1 C103 C102 . . . 70.5(4) ? Os1 C103 C1031 . . . 128.7(5) ? Os1 C103 C104 . . . 73.3(4) ? C102 C103 C1031 . . . 124.8(8) ? C102 C103 C104 . . . 109.7(8) ? C1031 C103 C104 . . . 125.0(8) ? C103 C1031 H1031a . . . 110.0 ? C103 C1031 H1031b . . . 109.6 ? C103 C1031 H1031c . . . 110.7 ? H1031a C1031 H1031b . . . 108.2 ? H1031a C1031 H1031c . . . 108.8 ? H1031b C1031 H1031c . . . 109.5 ? Os1 C104 C103 . . . 70.4(4) ? Os1 C104 C1041 . . . 132.7(5) ? Os1 C104 C105 . . . 71.2(4) ? C103 C104 C1041 . . . 124.8(9) ? C103 C104 C105 . . . 106.5(7) ? C1041 C104 C105 . . . 127.5(9) ? C104 C1041 H1041a . . . 107.2 ? C104 C1041 H1041b . . . 105.7 ? C104 C1041 H1041c . . . 113.8 ? H1041a C1041 H1041b . . . 106.6 ? H1041a C1041 H1041c . . . 110.2 ? H1041b C1041 H1041c . . . 112.9 ? Os1 C105 C101 . . . 70.5(4) ? Os1 C105 C104 . . . 72.6(5) ? Os1 C105 C1051 . . . 129.1(5) ? C101 C105 C104 . . . 110.2(8) ? C101 C105 C1051 . . . 124.9(8) ? C104 C105 C1051 . . . 124.6(7) ? C105 C1051 H1051a . . . 111.4 ? C105 C1051 H1051b . . . 110.2 ? C105 C1051 H1051c . . . 111.5 ? H1051a C1051 H1051b . . . 107.3 ? H1051a C1051 H1051c . . . 108.7 ? H1051b C1051 H1051c . . . 107.6 ? Os2 P21 C2111 . . . 118.7(3) ? Os2 P21 C2121 . . . 120.9(2) ? Os2 P21 C210 . . . 108.3(3) ? C2111 P21 C2121 . . . 100.2(4) ? C2111 P21 C210 . . . 101.9(3) ? C2121 P21 C210 . . . 104.5(4) ? P21 C2111 C2112 . . . 119.1(6) ? P21 C2111 C2116 . . . 122.2(6) ? C2112 C2111 C2116 . . . 118.7(8) ? C2111 C2112 C2113 . . . 121.2(8) ? C2111 C2112 H2112 . . . 120.0 ? C2113 C2112 H2112 . . . 118.9 ? C2112 C2113 C2114 . . . 119.1(8) ? C2112 C2113 H2113 . . . 120.7 ? C2114 C2113 H2113 . . . 120.1 ? C2113 C2114 C2115 . . . 120.9(9) ? C2113 C2114 H2114 . . . 119.2 ? C2115 C2114 H2114 . . . 119.9 ? C2114 C2115 C2116 . . . 119.5(8) ? C2114 C2115 H2115 . . . 119.9 ? C2116 C2115 H2115 . . . 120.6 ? C2111 C2116 C2115 . . . 120.6(8) ? C2111 C2116 H2116 . . . 119.6 ? C2115 C2116 H2116 . . . 119.8 ? P21 C2121 C2122 . . . 121.5(7) ? P21 C2121 C2126 . . . 119.8(6) ? C2122 C2121 C2126 . . . 118.7(9) ? C2121 C2122 C2123 . . . 119.6(10) ? C2121 C2122 H2122 . . . 120.2 ? C2123 C2122 H2122 . . . 120.2 ? C2122 C2123 C2124 . . . 121.2(9) ? C2122 C2123 H2123 . . . 120.1 ? C2124 C2123 H2123 . . . 118.7 ? C2123 C2124 C2125 . . . 118.4(10) ? C2123 C2124 H2124 . . . 121.3 ? C2125 C2124 H2124 . . . 120.3 ? C2124 C2125 C2126 . . . 120.7(10) ? C2124 C2125 H2125 . . . 119.6 ? C2126 C2125 H2125 . . . 119.7 ? C2121 C2126 C2125 . . . 121.4(8) ? C2121 C2126 H2126 . . . 119.8 ? C2125 C2126 H2126 . . . 118.8 ? P21 C210 C220 . . . 109.5(5) ? P21 C210 H210a . . . 109.5 ? P21 C210 H210b . . . 109.2 ? C220 C210 H210a . . . 109.3 ? C220 C210 H210b . . . 110.3 ? H210a C210 H210b . . . 108.9 ? C210 C220 P22 . . . 110.4(5) ? C210 C220 H220a . . . 109.0 ? C210 C220 H220b . . . 110.1 ? P22 C220 H220a . . . 109.3 ? P22 C220 H220b . . . 110.3 ? H220a C220 H220b . . . 107.6 ? Os2 P22 C220 . . . 111.9(3) ? Os2 P22 C2211 . . . 117.4(2) ? Os2 P22 C2221 . . . 120.1(2) ? C220 P22 C2211 . . . 102.3(3) ? C220 P22 C2221 . . . 103.6(3) ? C2211 P22 C2221 . . . 99.2(4) ? P22 C2211 C2212 . . . 121.3(6) ? P22 C2211 C2216 . . . 120.1(6) ? C2212 C2211 C2216 . . . 118.4(7) ? C2211 C2212 C2213 . . . 120.4(8) ? C2211 C2212 H2212 . . . 119.3 ? C2213 C2212 H2212 . . . 120.3 ? C2212 C2213 C2214 . . . 120.4(9) ? C2212 C2213 H2213 . . . 119.4 ? C2214 C2213 H2213 . . . 120.2 ? C2213 C2214 C2215 . . . 120.9(9) ? C2213 C2214 H2214 . . . 120.7 ? C2215 C2214 H2214 . . . 118.4 ? C2214 C2215 C2216 . . . 119.5(8) ? C2214 C2215 H2215 . . . 119.7 ? C2216 C2215 H2215 . . . 120.7 ? C2211 C2216 C2215 . . . 120.3(8) ? C2211 C2216 H2216 . . . 119.3 ? C2215 C2216 H2216 . . . 120.4 ? P22 C2221 C2222 . . . 121.7(7) ? P22 C2221 C2226 . . . 120.9(6) ? C2222 C2221 C2226 . . . 117.4(9) ? C2221 C2222 C2223 . . . 120.1(8) ? C2221 C2222 H2222 . . . 119.7 ? C2223 C2222 H2222 . . . 120.2 ? C2222 C2223 C2224 . . . 120.6(8) ? C2222 C2223 H2223 . . . 120.6 ? C2224 C2223 H2223 . . . 118.8 ? C2223 C2224 C2225 . . . 120.9(10) ? C2223 C2224 H2224 . . . 118.2 ? C2225 C2224 H2224 . . . 120.9 ? C2224 C2225 C2226 . . . 117.3(9) ? C2224 C2225 H2225 . . . 120.6 ? C2226 C2225 H2225 . . . 122.2 ? C2221 C2226 C2225 . . . 123.7(8) ? C2221 C2226 H2226 . . . 117.5 ? C2225 C2226 H2226 . . . 118.7 ? Os2 C21 C22 . . . 177.2(7) ? C21 C22 H22 . . . 178.8 ? Os2 C201 C2011 . . . 127.3(5) ? Os2 C201 C202 . . . 72.4(4) ? Os2 C201 C205 . . . 72.0(4) ? C2011 C201 C202 . . . 125.1(8) ? C2011 C201 C205 . . . 126.0(8) ? C202 C201 C205 . . . 108.5(8) ? C201 C2011 H2011a . . . 108.6 ? C201 C2011 H2011b . . . 108.3 ? C201 C2011 H2011c . . . 110.8 ? H2011a C2011 H2011b . . . 112.2 ? H2011a C2011 H2011c . . . 108.6 ? H2011b C2011 H2011c . . . 108.4 ? Os2 C202 C201 . . . 69.9(4) ? Os2 C202 C2021 . . . 126.4(6) ? Os2 C202 C203 . . . 71.9(4) ? C201 C202 C2021 . . . 125.9(9) ? C201 C202 C203 . . . 107.5(8) ? C2021 C202 C203 . . . 126.5(9) ? C202 C2021 H2021a . . . 107.0 ? C202 C2021 H2021b . . . 107.4 ? C202 C2021 H2021c . . . 110.7 ? H2021a C2021 H2021b . . . 110.1 ? H2021a C2021 H2021c . . . 109.0 ? H2021b C2021 H2021c . . . 112.5 ? Os2 C203 C202 . . . 71.4(4) ? Os2 C203 C2031 . . . 128.5(5) ? Os2 C203 C204 . . . 71.5(4) ? C202 C203 C2031 . . . 126.5(9) ? C202 C203 C204 . . . 108.6(8) ? C2031 C203 C204 . . . 124.6(9) ? C203 C2031 H2031a . . . 108.3 ? C203 C2031 H2031b . . . 108.6 ? C203 C2031 H2031c . . . 111.6 ? H2031a C2031 H2031b . . . 107.3 ? H2031a C2031 H2031c . . . 109.9 ? H2031b C2031 H2031c . . . 110.9 ? Os2 C204 C203 . . . 71.8(4) ? Os2 C204 C2041 . . . 131.2(5) ? Os2 C204 C205 . . . 70.4(4) ? C203 C204 C2041 . . . 125.1(9) ? C203 C204 C205 . . . 108.2(7) ? C2041 C204 C205 . . . 126.0(8) ? C204 C2041 H2041a . . . 114.6 ? C204 C2041 H2041b . . . 114.2 ? C204 C2041 H2041c . . . 108.4 ? H2041a C2041 H2041b . . . 109.5 ? H2041a C2041 H2041c . . . 107.4 ? H2041b C2041 H2041c . . . 101.7 ? Os2 C205 C201 . . . 70.8(4) ? Os2 C205 C204 . . . 71.9(4) ? Os2 C205 C2051 . . . 131.4(5) ? C201 C205 C204 . . . 107.2(7) ? C201 C205 C2051 . . . 124.9(8) ? C204 C205 C2051 . . . 126.9(8) ? C205 C2051 H2051a . . . 110.8 ? C205 C2051 H2051b . . . 111.0 ? C205 C2051 H2051c . . . 109.5 ? H2051a C2051 H2051b . . . 109.3 ? H2051a C2051 H2051c . . . 107.9 ? H2051b C2051 H2051c . . . 108.2 ? _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min -18 _reflns_limit_k_max 19 _reflns_limit_l_min -21 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .842 _reflns_d_resolution_low 18.047 _diffrn_reflns_av_sigmaI/netI .053 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .061 _refine_ls_wR_factor_all .063 _refine_ls_goodness_of_fit_all 1.603 _refine_ls_shift/su_mean .001 #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_br778 _database_code_depnum_ccdc_archive 'CCDC 617828' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C39 H45 F6 O1 Os1 P3' _chemical_formula_moiety 'C38 H41 Os P2, F6 P, C H4 O' _chemical_formula_weight 926.90 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.7240(10) _cell_length_b 17.360(2) _cell_length_c 18.500(2) _cell_angle_alpha 90.00000 _cell_angle_beta 103.300(2) _cell_angle_gamma 90.00000 _cell_volume 3664.3(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.68 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7325 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 36.2 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 3.673 _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .13 _exptl_crystal_size_rad ? _exptl_crystal_colour pale_yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .46 _exptl_absorpt_correction_T_max .70 _diffrn_reflns_number 76389 _reflns_number_total 19252 _reflns_Friedel_coverage 0 _reflns_number_gt 13371 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .054 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .035 _refine_ls_wR_factor_ref .035 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_number_reflns 13371 _refine_ls_number_parameters 615 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/(sig^2(F) + .0003F^2) ; _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .019 _refine_diff_density_min -1.813 _refine_diff_density_max 2.559 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 156 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 180 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 24 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Os ? 0 4 -1.816 7.605 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 12 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Os .676866(8) .540641(6) .780883(5) .01446(4) Uani ? ? 1.00000 ? ? P1 .79532(6) .55442(4) .69784(4) .0159(3) Uani ? ? 1.00000 ? ? C111 .8053(2) .47783(15) .63268(14) .0177(10) Uani ? ? 1.00000 ? ? C112 .7186(3) .42116(17) .61607(16) .0230(12) Uani ? ? 1.00000 ? ? C113 .7189(3) .36815(17) .55968(17) .0279(13) Uani ? ? 1.00000 ? ? C114 .8074(3) .36986(19) .52109(17) .0295(14) Uani ? ? 1.00000 ? ? C115 .8932(3) .4248(2) .53702(18) .0294(14) Uani ? ? 1.00000 ? ? C116 .8921(2) .48029(18) .59149(16) .0229(12) Uani ? ? 1.00000 ? ? C121 .9474(2) .58091(16) .73859(15) .0190(11) Uani ? ? 1.00000 ? ? C122 1.0153(3) .5307(2) .78907(18) .0299(14) Uani ? ? 1.00000 ? ? C123 1.1278(3) .5508(2) .8269(2) .0365(17) Uani ? ? 1.00000 ? ? C124 1.1733(3) .6217(2) .8143(2) .0364(16) Uani ? ? 1.00000 ? ? C125 1.1085(3) .6702(2) .7623(3) .0432(19) Uani ? ? 1.00000 ? ? C126 .9962(3) .6501(2) .7242(2) .0354(16) Uani ? ? 1.00000 ? ? C10 .7358(2) .63395(16) .63516(15) .0193(11) Uani ? ? 1.00000 ? ? C20 .6051(2) .61697(17) .60581(15) .0191(11) Uani ? ? 1.00000 ? ? P2 .53849(6) .59479(4) .68459(4) .0157(3) Uani ? ? 1.00000 ? ? C211 .4098(2) .53663(16) .64475(14) .0185(10) Uani ? ? 1.00000 ? ? C212 .3088(2) .54482(19) .67148(15) .0229(12) Uani ? ? 1.00000 ? ? C213 .2151(3) .4946(2) .64984(18) .0296(15) Uani ? ? 1.00000 ? ? C214 .2196(3) .4364(2) .59995(17) .0294(14) Uani ? ? 1.00000 ? ? C215 .3175(3) .4288(2) .57113(17) .0271(13) Uani ? ? 1.00000 ? ? C216 .4129(3) .47796(17) .59307(15) .0220(12) Uani ? ? 1.00000 ? ? C221 .4705(2) .68578(16) .70239(15) .0203(11) Uani ? ? 1.00000 ? ? C222 .4782(3) .71313(18) .77396(17) .0275(14) Uani ? ? 1.00000 ? ? C223 .4202(3) .7807(2) .7852(2) .0361(17) Uani ? ? 1.00000 ? ? C224 .3562(3) .8215(2) .7259(2) .0361(17) Uani ? ? 1.00000 ? ? C225 .3473(3) .7950(2) .6546(2) .0362(16) Uani ? ? 1.00000 ? ? C226 .4034(3) .7277(2) .64279(19) .0296(14) Uani ? ? 1.00000 ? ? C1 .7374(3) .6398(2) .81420(15) .0265(13) Uani ? ? 1.00000 ? ? C2 .7787(4) .6989(3) .8394(3) .043(2) Uani ? ? 1.00000 ? ? C01 .6631(3) .50808(17) .89696(15) .0219(12) Uani ? ? 1.00000 ? ? C011 .6673(4) .5619(2) .96067(18) .0360(17) Uani ? ? 1.00000 ? ? C02 .5619(2) .47974(17) .84655(15) .0218(12) Uani ? ? 1.00000 ? ? C021 .4387(3) .4954(3) .8525(2) .0351(17) Uani ? ? 1.00000 ? ? C03 .5983(2) .42172(16) .80092(15) .0208(11) Uani ? ? 1.00000 ? ? C031 .5159(3) .3680(2) .7513(2) .0333(16) Uani ? ? 1.00000 ? ? C04 .7225(3) .41556(16) .82314(15) .0213(12) Uani ? ? 1.00000 ? ? C041 .7961(3) .3556(2) .7979(2) .0304(15) Uani ? ? 1.00000 ? ? C05 .7633(2) .47018(16) .88203(15) .0206(11) Uani ? ? 1.00000 ? ? C051 .8846(3) .4758(3) .9304(2) .0366(17) Uani ? ? 1.00000 ? ? P .58695(8) .28234(5) .98495(5) .0287(4) Uani ? ? 1.00000 ? ? F1 .7000(2) .25442(14) 1.04569(14) .0606(14) Uani ? ? 1.00000 ? ? F2 .5579(2) .19407(12) .96446(13) .0476(12) Uani ? ? 1.00000 ? ? F3 .6189(2) .36936(12) 1.00652(13) .0557(13) Uani ? ? 1.00000 ? ? F4 .6621(2) .28618(12) .92343(13) .0491(12) Uani ? ? 1.00000 ? ? F5 .4744(2) .30949(15) .92513(14) .0620(15) Uani ? ? 1.00000 ? ? F6 .5110(2) .27766(14) 1.04589(13) .0588(14) Uani ? ? 1.00000 ? ? C0 .9522(8) .3051(4) 1.0166(5) .122(6) Uani ? ? 1.00000 ? ? O0 .9534(4) .2409(3) 1.0544(3) .113(3) Uani ? ? 1.00000 ? ? H112 .660(3) .4210(18) .6470(17) .017(8) Uiso ? ? 1.00000 ? ? H113 .654(3) .331(2) .548(2) .049(12) Uiso ? ? 1.00000 ? ? H114 .804(3) .333(2) .481(2) .040(11) Uiso ? ? 1.00000 ? ? H115 .948(3) .427(2) .513(2) .030(10) Uiso ? ? 1.00000 ? ? H116 .945(3) .516(2) .599(2) .035(10) Uiso ? ? 1.00000 ? ? H122 .994(4) .479(3) .801(3) .071(15) Uiso ? ? 1.00000 ? ? H123 1.167(5) .511(3) .852(3) .085(18) Uiso ? ? 1.00000 ? ? H124 1.243(3) .631(2) .843(2) .044(11) Uiso ? ? 1.00000 ? ? H125 1.135(4) .717(2) .754(2) .052(13) Uiso ? ? 1.00000 ? ? H126 .953(3) .689(2) .692(2) .044(11) Uiso ? ? 1.00000 ? ? H10a .744(3) .6805(18) .6627(17) .019(8) Uiso ? ? 1.00000 ? ? H10b .779(3) .6369(18) .5969(18) .023(8) Uiso ? ? 1.00000 ? ? H20a .595(3) .575(2) .5754(18) .024(9) Uiso ? ? 1.00000 ? ? H20b .563(3) .658(2) .5743(18) .026(9) Uiso ? ? 1.00000 ? ? H212 .303(3) .585(2) .704(2) .034(10) Uiso ? ? 1.00000 ? ? H213 .144(3) .497(2) .668(2) .037(10) Uiso ? ? 1.00000 ? ? H214 .159(3) .399(2) .585(2) .033(10) Uiso ? ? 1.00000 ? ? H215 .319(3) .3919(18) .5357(17) .018(8) Uiso ? ? 1.00000 ? ? H216 .484(3) .4678(18) .575(2) .029(10) Uiso ? ? 1.00000 ? ? H222 .521(3) .684(2) .815(2) .041(11) Uiso ? ? 1.00000 ? ? H223 .434(3) .794(2) .833(2) .044(11) Uiso ? ? 1.00000 ? ? H224 .326(3) .867(3) .732(2) .053(13) Uiso ? ? 1.00000 ? ? H225 .301(3) .809(2) .616(2) .036(11) Uiso ? ? 1.00000 ? ? H226 .398(3) .719(2) .600(2) .029(10) Uiso ? ? 1.00000 ? ? H2a .848(4) .700(2) .853(2) .040(12) Uiso ? ? 1.00000 ? ? H2b .737(4) .724(3) .842(3) .060(18) Uiso ? ? 1.00000 ? ? H011a .750(4) .595(2) .972(2) .056(13) Uiso ? ? 1.00000 ? ? H011b .604(4) .598(2) .959(2) .056(13) Uiso ? ? 1.00000 ? ? H011c .666(3) .530(2) 1.005(2) .032(10) Uiso ? ? 1.00000 ? ? H021a .411(4) .456(2) .888(2) .049(12) Uiso ? ? 1.00000 ? ? H021b .387(4) .481(2) .813(3) .051(13) Uiso ? ? 1.00000 ? ? H021c .419(4) .549(2) .868(2) .054(13) Uiso ? ? 1.00000 ? ? H031a .539(3) .349(2) .714(2) .040(11) Uiso ? ? 1.00000 ? ? H031b .443(4) .396(2) .729(2) .057(13) Uiso ? ? 1.00000 ? ? H031c .499(4) .326(2) .778(2) .052(12) Uiso ? ? 1.00000 ? ? H041a .863(4) .379(3) .781(3) .081(16) Uiso ? ? 1.00000 ? ? H041b .762(5) .323(3) .751(3) .098(19) Uiso ? ? 1.00000 ? ? H041c .826(4) .322(2) .839(2) .055(13) Uiso ? ? 1.00000 ? ? H051a .940(3) .440(2) .912(2) .043(11) Uiso ? ? 1.00000 ? ? H051b .883(5) .444(3) .973(3) .081(17) Uiso ? ? 1.00000 ? ? H051c .905(5) .528(3) .936(3) .078(17) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os .01513(4) .01655(4) .01193(4) -.00097(4) .00357(3) -.00002(4) P1 .0144(3) .0185(3) .0151(3) -.0018(2) .0040(2) -.0005(2) C111 .0197(12) .0175(12) .0157(11) .0006(9) .0039(9) -.0008(9) C112 .0260(14) .0237(14) .0199(13) -.0039(11) .0066(11) -.0011(11) C113 .0381(17) .0198(14) .0247(14) -.0045(12) .0047(12) -.0044(11) C114 .0398(17) .0279(16) .0212(13) .0033(13) .0081(12) -.0068(12) C115 .0239(14) .0417(19) .0239(14) .0060(13) .0085(12) -.0052(13) C116 .0173(12) .0286(15) .0231(13) -.0021(11) .0055(10) -.0034(11) C121 .0163(11) .0215(13) .0195(12) -.0005(10) .0045(9) -.0028(10) C122 .0183(12) .040(2) .0304(15) -.0026(12) .0027(11) .0087(14) C123 .0193(13) .057(2) .0312(17) .0040(15) .0023(12) .0096(16) C124 .0162(13) .049(2) .042(2) .0013(14) .0020(13) -.0197(17) C125 .0235(16) .0228(16) .078(3) -.0055(13) .0002(17) -.0071(18) C126 .0207(14) .0232(15) .058(2) -.0031(12) .0007(14) .0049(15) C10 .0202(12) .0184(13) .0205(12) .0002(10) .0075(10) .0014(10) C20 .0173(11) .0245(13) .0163(11) .0010(10) .0051(9) .0036(10) P2 .0154(3) .0187(3) .0133(3) .0002(2) .0039(2) -.0000(2) C211 .0160(10) .0249(13) .0149(10) -.0022(10) .0038(8) .0003(10) C212 .0167(11) .0338(15) .0190(12) -.0011(12) .0056(9) -.0014(12) C213 .0184(13) .044(2) .0260(15) -.0052(13) .0052(11) .0030(13) C214 .0244(14) .0385(17) .0232(14) -.0136(13) .0008(11) .0017(12) C215 .0285(15) .0310(16) .0205(13) -.0082(13) .0029(11) -.0049(12) C216 .0215(13) .0278(14) .0177(12) -.0027(10) .0063(10) -.0020(10) C221 .0194(12) .0196(13) .0224(13) .0026(10) .0061(10) .0000(10) C222 .0330(16) .0278(16) .0228(14) .0087(13) .0088(12) .0023(12) C223 .048(2) .0344(18) .0296(17) .0087(16) .0164(15) -.0059(14) C224 .0400(18) .0257(16) .044(2) .0111(14) .0130(16) -.0028(15) C225 .0393(19) .0331(18) .0335(18) .0135(15) .0030(15) .0059(14) C226 .0346(16) .0288(16) .0237(15) .0075(13) .0034(13) .0002(12) C1 .0264(14) .0410(18) .0129(11) .0137(13) .0060(10) .0031(11) C2 .038(2) .050(3) .041(2) -.002(2) .0113(18) .0100(19) C01 .0259(13) .0273(14) .0134(11) .0010(11) .0065(10) .0020(10) C011 .054(2) .0382(19) .0182(14) .0036(17) .0128(15) -.0042(13) C02 .0209(12) .0281(14) .0182(12) .0024(10) .0080(10) .0078(10) C021 .0234(15) .051(2) .0341(18) .0060(15) .0125(14) .0163(17) C03 .0232(13) .0220(13) .0175(12) -.0032(10) .0051(10) .0047(10) C031 .040(2) .0319(18) .0261(16) -.0154(15) .0044(14) .0047(14) C04 .0278(14) .0194(13) .0195(12) .0013(11) .0109(11) .0041(10) C041 .0378(18) .0256(16) .0318(17) .0086(14) .0160(14) .0058(13) C05 .0219(12) .0228(14) .0155(11) -.0006(10) .0014(9) .0032(9) C051 .0260(15) .053(2) .0257(16) -.0013(15) -.0044(13) .0077(15) P .0419(5) .0230(4) .0248(4) .0063(3) .0153(3) .0027(3) F1 .0566(15) .0542(15) .0622(16) .0084(12) -.0041(13) .0127(13) F2 .0653(15) .0325(12) .0522(14) -.0107(11) .0283(12) -.0025(10) F3 .095(2) .0258(11) .0501(14) .0002(12) .0237(13) -.0070(10) F4 .0720(16) .0315(11) .0601(15) -.0032(11) .0485(13) .0018(10) F5 .0575(15) .0718(18) .0519(15) .0189(13) .0031(12) .0221(13) F6 .0862(19) .0575(15) .0471(14) .0193(14) .0451(14) .0115(12) C0 .146(7) .084(5) .155(8) .043(5) .075(6) .051(5) O0 .086(3) .109(4) .145(4) -.014(3) .031(3) -.036(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Os P1 . . 2.3081(8) ? Os P2 . . 2.3151(6) ? Os C1 . . 1.910(3) ? Os C01 . . 2.262(3) ? Os C02 . . 2.272(3) ? Os C03 . . 2.325(3) ? Os C04 . . 2.328(3) ? Os C05 . . 2.270(3) ? P1 C111 . . 1.817(3) ? P1 C121 . . 1.827(3) ? P1 C10 . . 1.835(3) ? C111 C112 . . 1.397(4) ? C111 C116 . . 1.405(4) ? C112 C113 . . 1.392(4) ? C112 H112 . . .99(3) ? C113 C114 . . 1.388(5) ? C113 H113 . . .98(4) ? C114 C115 . . 1.369(5) ? C114 H114 . . .97(4) ? C115 C116 . . 1.396(5) ? C115 H115 . . .86(4) ? C116 H116 . . .87(4) ? C121 C122 . . 1.388(4) ? C121 C126 . . 1.383(4) ? C122 C123 . . 1.388(4) ? C122 H122 . . .97(5) ? C123 C124 . . 1.382(6) ? C123 H123 . . .90(5) ? C124 C125 . . 1.370(5) ? C124 H124 . . .88(4) ? C125 C126 . . 1.388(5) ? C125 H125 . . .89(4) ? C126 H126 . . .97(4) ? C10 C20 . . 1.532(4) ? C10 H10a . . .95(3) ? C10 H10b . . .97(4) ? C20 P2 . . 1.845(3) ? C20 H20a . . .92(3) ? C20 H20b . . .98(3) ? P2 C211 . . 1.824(3) ? P2 C221 . . 1.833(3) ? C211 C212 . . 1.391(4) ? C211 C216 . . 1.403(4) ? C212 C213 . . 1.388(4) ? C212 H212 . . .93(4) ? C213 C214 . . 1.377(5) ? C213 H213 . . .97(4) ? C214 C215 . . 1.379(5) ? C214 H214 . . .96(3) ? C215 C216 . . 1.391(4) ? C215 H215 . . .92(3) ? C216 H216 . . .98(4) ? C221 C222 . . 1.390(4) ? C221 C226 . . 1.402(4) ? C222 C223 . . 1.395(5) ? C222 H222 . . .96(4) ? C223 C224 . . 1.374(5) ? C223 H223 . . .89(4) ? C224 C225 . . 1.380(5) ? C224 H224 . . .88(5) ? C225 C226 . . 1.382(5) ? C225 H225 . . .83(3) ? C226 H226 . . .80(4) ? C1 C2 . . 1.183(6) ? C2 H2a . . .80(4) ? C2 H2b . . .66(5) ? C01 C011 . . 1.496(5) ? C01 C02 . . 1.417(4) ? C01 C05 . . 1.428(4) ? C011 H011a . . 1.10(4) ? C011 H011b . . .96(4) ? C011 H011c . . .99(4) ? C02 C021 . . 1.499(5) ? C02 C03 . . 1.440(4) ? C021 H021a . . 1.04(4) ? C021 H021b . . .87(4) ? C021 H021c . . 1.01(4) ? C03 C031 . . 1.496(4) ? C03 C04 . . 1.424(4) ? C031 H031a . . .86(4) ? C031 H031b . . .98(4) ? C031 H031c . . .92(4) ? C04 C041 . . 1.494(5) ? C04 C05 . . 1.441(4) ? C041 H041a . . .99(5) ? C041 H041b . . 1.03(5) ? C041 H041c . . .96(4) ? C05 C051 . . 1.498(4) ? C051 H051a . . 1.01(4) ? C051 H051b . . .97(6) ? C051 H051c . . .94(5) ? P F1 . . 1.603(2) ? P F2 . . 1.596(2) ? P F3 . . 1.585(2) ? P F4 . . 1.593(3) ? P F5 . . 1.586(2) ? P F6 . . 1.592(3) ? C0 O0 . . 1.315(10) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published P1 Os P2 . . . 82.42(3) ? P1 Os C1 . . . 83.42(10) ? P1 Os C01 . . . 147.47(7) ? P1 Os C02 . . . 157.78(8) ? P1 Os C03 . . . 121.29(8) ? P1 Os C04 . . . 101.13(8) ? P1 Os C05 . . . 112.43(8) ? P2 Os C1 . . . 91.43(8) ? P2 Os C01 . . . 129.91(8) ? P2 Os C02 . . . 101.75(7) ? P2 Os C03 . . . 104.47(6) ? P2 Os C04 . . . 134.70(6) ? P2 Os C05 . . . 162.59(8) ? C1 Os C01 . . . 91.22(11) ? C1 Os C02 . . . 117.98(12) ? C1 Os C03 . . . 151.72(11) ? C1 Os C04 . . . 133.85(10) ? C1 Os C05 . . . 99.05(10) ? C01 Os C02 . . . 36.43(10) ? C01 Os C03 . . . 60.61(10) ? C01 Os C04 . . . 60.61(11) ? C01 Os C05 . . . 36.74(11) ? C02 Os C03 . . . 36.49(11) ? C02 Os C04 . . . 60.35(11) ? C02 Os C05 . . . 61.04(10) ? C03 Os C04 . . . 35.64(10) ? C03 Os C05 . . . 60.55(9) ? C04 Os C05 . . . 36.49(9) ? Os P1 C111 . . . 120.43(10) ? Os P1 C121 . . . 115.51(10) ? Os P1 C10 . . . 107.39(10) ? C111 P1 C121 . . . 104.60(13) ? C111 P1 C10 . . . 101.81(12) ? C121 P1 C10 . . . 105.34(13) ? P1 C111 C112 . . . 120.4(2) ? P1 C111 C116 . . . 120.2(2) ? C112 C111 C116 . . . 118.9(3) ? C111 C112 C113 . . . 120.2(3) ? C111 C112 H112 . . . 116.2(17) ? C113 C112 H112 . . . 123.5(17) ? C112 C113 C114 . . . 120.2(3) ? C112 C113 H113 . . . 117(3) ? C114 C113 H113 . . . 123(3) ? C113 C114 C115 . . . 120.2(3) ? C113 C114 H114 . . . 118(2) ? C115 C114 H114 . . . 122(2) ? C114 C115 C116 . . . 120.5(3) ? C114 C115 H115 . . . 121(2) ? C116 C115 H115 . . . 118(2) ? C111 C116 C115 . . . 119.9(3) ? C111 C116 H116 . . . 121(3) ? C115 C116 H116 . . . 119(3) ? P1 C121 C122 . . . 118.3(2) ? P1 C121 C126 . . . 123.2(2) ? C122 C121 C126 . . . 118.5(3) ? C121 C122 C123 . . . 120.9(3) ? C121 C122 H122 . . . 126(3) ? C123 C122 H122 . . . 113(3) ? C122 C123 C124 . . . 119.8(3) ? C122 C123 H123 . . . 112(3) ? C124 C123 H123 . . . 127(3) ? C123 C124 C125 . . . 119.6(3) ? C123 C124 H124 . . . 114(3) ? C125 C124 H124 . . . 127(3) ? C124 C125 C126 . . . 120.7(3) ? C124 C125 H125 . . . 121(2) ? C126 C125 H125 . . . 118(2) ? C121 C126 C125 . . . 120.5(3) ? C121 C126 H126 . . . 124(2) ? C125 C126 H126 . . . 116(2) ? P1 C10 C20 . . . 106.5(2) ? P1 C10 H10a . . . 108.9(18) ? P1 C10 H10b . . . 108.3(18) ? C20 C10 H10a . . . 108.9(19) ? C20 C10 H10b . . . 114.0(17) ? H10a C10 H10b . . . 110(3) ? C10 C20 P2 . . . 109.31(18) ? C10 C20 H20a . . . 110(2) ? C10 C20 H20b . . . 113(2) ? P2 C20 H20a . . . 107(2) ? P2 C20 H20b . . . 112(2) ? H20a C20 H20b . . . 104(3) ? Os P2 C20 . . . 110.09(9) ? Os P2 C211 . . . 117.02(9) ? Os P2 C221 . . . 117.93(9) ? C20 P2 C211 . . . 104.92(12) ? C20 P2 C221 . . . 104.04(14) ? C211 P2 C221 . . . 101.30(12) ? P2 C211 C212 . . . 119.5(2) ? P2 C211 C216 . . . 121.9(2) ? C212 C211 C216 . . . 118.3(3) ? C211 C212 C213 . . . 121.0(3) ? C211 C212 H212 . . . 120(2) ? C213 C212 H212 . . . 119(2) ? C212 C213 C214 . . . 120.3(3) ? C212 C213 H213 . . . 124(2) ? C214 C213 H213 . . . 116(2) ? C213 C214 C215 . . . 119.5(3) ? C213 C214 H214 . . . 123(2) ? C215 C214 H214 . . . 117(2) ? C214 C215 C216 . . . 120.9(3) ? C214 C215 H215 . . . 119(2) ? C216 C215 H215 . . . 120(2) ? C211 C216 C215 . . . 119.9(3) ? C211 C216 H216 . . . 121.0(19) ? C215 C216 H216 . . . 118.8(19) ? P2 C221 C222 . . . 122.0(2) ? P2 C221 C226 . . . 119.6(2) ? C222 C221 C226 . . . 118.3(3) ? C221 C222 C223 . . . 120.1(3) ? C221 C222 H222 . . . 119(2) ? C223 C222 H222 . . . 121(2) ? C222 C223 C224 . . . 120.7(3) ? C222 C223 H223 . . . 112(2) ? C224 C223 H223 . . . 127(2) ? C223 C224 C225 . . . 119.9(4) ? C223 C224 H224 . . . 122(3) ? C225 C224 H224 . . . 118(3) ? C224 C225 C226 . . . 119.9(3) ? C224 C225 H225 . . . 128(3) ? C226 C225 H225 . . . 111(3) ? C221 C226 C225 . . . 121.1(3) ? C221 C226 H226 . . . 126(2) ? C225 C226 H226 . . . 113(2) ? Os C1 C2 . . . 175.4(3) ? C1 C2 H2a . . . 116(3) ? C1 C2 H2b . . . 110(4) ? H2a C2 H2b . . . 133(5) ? Os C01 C011 . . . 126.5(2) ? Os C01 C02 . . . 72.16(16) ? Os C01 C05 . . . 71.93(16) ? C011 C01 C02 . . . 127.3(3) ? C011 C01 C05 . . . 124.1(3) ? C02 C01 C05 . . . 108.3(2) ? C01 C011 H011a . . . 110(2) ? C01 C011 H011b . . . 120(2) ? C01 C011 H011c . . . 107(2) ? H011a C011 H011b . . . 108(3) ? H011a C011 H011c . . . 108(3) ? H011b C011 H011c . . . 103(4) ? Os C02 C01 . . . 71.40(17) ? Os C02 C021 . . . 130.9(2) ? Os C02 C03 . . . 73.76(18) ? C01 C02 C021 . . . 124.3(3) ? C01 C02 C03 . . . 108.2(2) ? C021 C02 C03 . . . 126.2(3) ? C02 C021 H021a . . . 112(2) ? C02 C021 H021b . . . 112(3) ? C02 C021 H021c . . . 118(3) ? Os C03 C02 . . . 69.75(16) ? Os C03 C031 . . . 132.8(2) ? Os C03 C04 . . . 72.31(16) ? C02 C03 C031 . . . 124.0(3) ? C02 C03 C04 . . . 107.7(2) ? C031 C03 C04 . . . 127.1(3) ? C03 C031 H031a . . . 117(3) ? C03 C031 H031b . . . 109(2) ? C03 C031 H031c . . . 110(2) ? Os C04 C03 . . . 72.06(16) ? Os C04 C041 . . . 130.5(2) ? Os C04 C05 . . . 69.56(15) ? C03 C04 C041 . . . 126.0(3) ? C03 C04 C05 . . . 108.0(3) ? C041 C04 C05 . . . 125.5(3) ? C04 C041 H041a . . . 111(3) ? C04 C041 H041b . . . 120(3) ? C04 C041 H041c . . . 108(3) ? Os C05 C01 . . . 71.33(15) ? Os C05 C04 . . . 73.95(15) ? Os C05 C051 . . . 129.7(2) ? C01 C05 C04 . . . 107.7(2) ? C01 C05 C051 . . . 124.4(3) ? C04 C05 C051 . . . 126.8(3) ? C05 C051 H051a . . . 111(2) ? C05 C051 H051b . . . 105(3) ? C05 C051 H051c . . . 108(3) ? F1 P F2 . . . 88.45(12) ? F1 P F3 . . . 90.14(13) ? F1 P F4 . . . 90.56(14) ? F1 P F5 . . . 179.52(17) ? F1 P F6 . . . 89.73(14) ? F2 P F3 . . . 178.57(13) ? F2 P F4 . . . 89.62(13) ? F2 P F5 . . . 91.26(13) ? F2 P F6 . . . 89.75(14) ? F3 P F4 . . . 90.15(14) ? F3 P F5 . . . 90.15(13) ? F3 P F6 . . . 90.49(15) ? F4 P F5 . . . 89.82(14) ? F4 P F6 . . . 179.31(13) ? F5 P F6 . . . 89.89(14) ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1848 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 29 _reflns_limit_l_min -31 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .583 _reflns_d_resolution_low 12.466 _diffrn_reflns_av_sigmaI/netI .103 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .069 _refine_ls_wR_factor_all .04 _refine_ls_goodness_of_fit_all .98 _refine_ls_shift/su_mean .0005 #===END #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_br779 _database_code_depnum_ccdc_archive 'CCDC 617829' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C81 H90 Os2 P4' _chemical_formula_moiety 'C76 H78 Os2 P4, C5 H12' _chemical_formula_weight 1567.91 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 10.971(2) _cell_length_b 17.958(3) _cell_length_c 17.855(3) _cell_angle_alpha 88.677(4) _cell_angle_beta 85.690(4) _cell_angle_gamma 87.946(4) _cell_volume 3504.8(10) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 37.6 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 3.756 _exptl_crystal_description prism _exptl_crystal_size_max .3 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour red _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .50 _exptl_absorpt_correction_T_max .70 _diffrn_reflns_number 72480 _reflns_number_total 36104 _reflns_Friedel_coverage 0 _reflns_number_gt 23919 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 38.0 _diffrn_reflns_theta_full 38 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .041 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .036 _refine_ls_wR_factor_ref .038 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_number_reflns 23919 _refine_ls_number_parameters 772 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/(sig^2(F) + .0005F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .014 _refine_diff_density_min -3.244 _refine_diff_density_max 2.093 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 162 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 180 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Os ? 0 4 -1.816 7.605 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Os1 .589670(11) .637540(6) .278423(6) .01657(6) Uani ? ? 1.00000 ? ? Os2 .662819(10) .201507(6) .293007(6) .01470(5) Uani ? ? 1.00000 ? ? C1 .6018(3) .52558(17) .28268(17) .0204(15) Uani ? ? 1.00000 ? ? C2 .6127(3) .45780(17) .28728(17) .0212(15) Uani ? ? 1.00000 ? ? C3 .6332(3) .38159(17) .29104(17) .0202(15) Uani ? ? 1.00000 ? ? C4 .6474(3) .31365(16) .29252(16) .0181(14) Uani ? ? 1.00000 ? ? P11 .78503(8) .62256(5) .23018(5) .0208(4) Uani ? ? 1.00000 ? ? C1111 .8707(3) .70332(19) .19315(18) .0254(17) Uani ? ? 1.00000 ? ? C1112 .8127(3) .7729(2) .1885(2) .0285(18) Uani ? ? 1.00000 ? ? C1113 .8760(4) .8341(2) .1581(2) .044(3) Uani ? ? 1.00000 ? ? C1114 .9963(4) .8252(2) .1316(2) .045(3) Uani ? ? 1.00000 ? ? C1115 1.0558(4) .7569(3) .1350(2) .044(3) Uani ? ? 1.00000 ? ? C1116 .9943(3) .6957(2) .1659(2) .034(2) Uani ? ? 1.00000 ? ? C1121 .8926(3) .58005(18) .29346(18) .0237(16) Uani ? ? 1.00000 ? ? C1122 .9609(3) .6256(2) .3355(2) .0294(19) Uani ? ? 1.00000 ? ? C1123 1.0322(3) .5952(2) .3902(2) .035(2) Uani ? ? 1.00000 ? ? C1124 1.0344(3) .5196(2) .4046(2) .037(2) Uani ? ? 1.00000 ? ? C1125 .9678(3) .4737(2) .3638(2) .039(2) Uani ? ? 1.00000 ? ? C1126 .8968(3) .5037(2) .3086(2) .033(2) Uani ? ? 1.00000 ? ? C11 .7935(3) .5613(2) .1466(2) .0291(18) Uani ? ? 1.00000 ? ? C12 .6690(3) .55545(18) .11515(18) .0260(17) Uani ? ? 1.00000 ? ? P12 .55416(8) .62286(4) .15717(4) .0201(4) Uani ? ? 1.00000 ? ? C1211 .5650(3) .70538(18) .09534(17) .0248(17) Uani ? ? 1.00000 ? ? C1212 .6662(3) .7167(2) .0451(2) .033(2) Uani ? ? 1.00000 ? ? C1213 .6795(4) .7838(2) .0047(2) .043(3) Uani ? ? 1.00000 ? ? C1214 .5889(4) .8392(2) .0142(2) .042(2) Uani ? ? 1.00000 ? ? C1215 .4876(4) .8284(2) .0628(2) .043(2) Uani ? ? 1.00000 ? ? C1216 .4757(4) .7620(2) .10366(19) .033(2) Uani ? ? 1.00000 ? ? C1221 .4094(3) .58556(17) .13341(19) .0252(17) Uani ? ? 1.00000 ? ? C1222 .3648(3) .5970(2) .0628(2) .034(2) Uani ? ? 1.00000 ? ? C1223 .2524(4) .5687(2) .0478(2) .042(2) Uani ? ? 1.00000 ? ? C1224 .1847(4) .5289(2) .1020(3) .042(2) Uani ? ? 1.00000 ? ? C1225 .2294(4) .5171(2) .1722(3) .043(3) Uani ? ? 1.00000 ? ? C1226 .3405(3) .5446(2) .1873(2) .032(2) Uani ? ? 1.00000 ? ? P21 .73064(7) .21988(4) .17245(4) .0181(4) Uani ? ? 1.00000 ? ? C2111 .7680(3) .13634(17) .11687(16) .0218(15) Uani ? ? 1.00000 ? ? C2112 .6781(3) .1006(2) .0821(2) .030(2) Uani ? ? 1.00000 ? ? C2113 .7026(4) .0330(2) .0468(2) .039(2) Uani ? ? 1.00000 ? ? C2114 .8165(4) .0000(2) .0460(2) .040(2) Uani ? ? 1.00000 ? ? C2115 .9068(4) .0343(2) .0796(2) .042(2) Uani ? ? 1.00000 ? ? C2116 .8837(3) .1020(2) .1149(2) .034(2) Uani ? ? 1.00000 ? ? C2121 .8706(3) .27151(18) .14897(18) .0241(16) Uani ? ? 1.00000 ? ? C2122 .9168(4) .2789(2) .0744(2) .038(2) Uani ? ? 1.00000 ? ? C2123 1.0264(4) .3140(3) .0566(2) .047(3) Uani ? ? 1.00000 ? ? C2124 1.0907(4) .3418(2) .1134(3) .044(3) Uani ? ? 1.00000 ? ? C2125 1.0439(4) .3361(2) .1873(2) .039(2) Uani ? ? 1.00000 ? ? C2126 .9326(3) .3023(2) .2046(2) .0299(19) Uani ? ? 1.00000 ? ? C21 .6153(3) .2738(2) .11983(19) .0292(18) Uani ? ? 1.00000 ? ? C22 .4882(3) .27746(19) .16074(18) .0252(17) Uani ? ? 1.00000 ? ? P22 .47847(7) .21631(4) .24565(4) .0176(4) Uani ? ? 1.00000 ? ? C2211 .4020(3) .13505(18) .21225(17) .0225(16) Uani ? ? 1.00000 ? ? C2212 .4648(3) .06661(19) .20724(18) .0274(18) Uani ? ? 1.00000 ? ? C2213 .4120(4) .0051(2) .1781(2) .035(2) Uani ? ? 1.00000 ? ? C2214 .2959(4) .0133(2) .1526(2) .041(2) Uani ? ? 1.00000 ? ? C2215 .2332(4) .0813(3) .1561(2) .042(2) Uani ? ? 1.00000 ? ? C2216 .2845(3) .1417(2) .1862(2) .030(2) Uani ? ? 1.00000 ? ? C2221 .3539(3) .25900(18) .30618(17) .0219(15) Uani ? ? 1.00000 ? ? C2222 .2774(3) .2134(2) .35180(18) .0258(17) Uani ? ? 1.00000 ? ? C2223 .1899(3) .2450(2) .40424(19) .0294(19) Uani ? ? 1.00000 ? ? C2224 .1772(3) .3216(2) .4107(2) .032(2) Uani ? ? 1.00000 ? ? C2225 .2523(3) .3666(2) .3654(2) .032(2) Uani ? ? 1.00000 ? ? C2226 .3410(3) .33603(19) .3136(2) .0260(17) Uani ? ? 1.00000 ? ? C101 .5690(3) .64814(18) .40272(17) .0235(16) Uani ? ? 1.00000 ? ? C1011 .6317(4) .5979(2) .4570(2) .037(2) Uani ? ? 1.00000 ? ? C102 .6085(3) .71797(18) .37164(17) .0249(17) Uani ? ? 1.00000 ? ? C1021 .7203(4) .7575(2) .3908(2) .034(2) Uani ? ? 1.00000 ? ? C103 .5171(3) .74879(17) .32636(17) .0238(16) Uani ? ? 1.00000 ? ? C1031 .5114(4) .82699(19) .2940(2) .035(2) Uani ? ? 1.00000 ? ? C104 .4180(3) .69805(17) .33015(17) .0235(16) Uani ? ? 1.00000 ? ? C1041 .2962(3) .7118(2) .2988(2) .033(2) Uani ? ? 1.00000 ? ? C105 .4490(3) .63643(18) .37720(17) .0226(16) Uani ? ? 1.00000 ? ? C1051 .3709(3) .5735(2) .4024(2) .033(2) Uani ? ? 1.00000 ? ? C201 .7734(3) .20022(18) .39409(17) .0236(16) Uani ? ? 1.00000 ? ? C2011 .8360(4) .2670(2) .4215(2) .036(2) Uani ? ? 1.00000 ? ? C202 .6498(3) .1821(2) .41681(17) .0276(18) Uani ? ? 1.00000 ? ? C2021 .5659(4) .2249(3) .4730(2) .046(3) Uani ? ? 1.00000 ? ? C203 .6270(3) .1132(2) .38266(18) .0271(18) Uani ? ? 1.00000 ? ? C2031 .5156(4) .0682(2) .4005(2) .043(2) Uani ? ? 1.00000 ? ? C204 .7343(3) .08978(17) .33748(18) .0248(17) Uani ? ? 1.00000 ? ? C2041 .7573(4) .0163(2) .3004(2) .041(2) Uani ? ? 1.00000 ? ? C205 .8254(3) .14425(17) .34560(17) .0226(16) Uani ? ? 1.00000 ? ? C2051 .9570(3) .1358(2) .3163(2) .033(2) Uani ? ? 1.00000 ? ? C01 .8829(7) .0787(5) .7033(5) .042(2) Uiso ? ? .50000 ? ? C02 .8127(16) .0360(11) .6682(10) .159(8) Uiso ? ? .50000 ? ? C03 .8891(11) .0662(7) .6086(7) .225(6) Uiso ? ? 1.00000 ? ? C04 .793(2) .0672(12) .5560(15) .282(16) Uiso ? ? .50000 ? ? C05 .7927(9) -.0129(5) .5221(6) .156(4) Uiso ? ? 1.00000 ? ? C01' .9911(12) .1608(8) .6102(8) .090(4) Uiso ? ? .50000 ? ? C02' .8929(9) .1284(5) .5736(5) .052(2) Uiso ? ? .50000 ? ? C04' .7795(14) .0165(9) .5959(10) .127(6) Uiso ? ? .50000 ? ? H1112 .72908 .77888 .20677 .03600 Uiso ? ? 1.00000 ? ? H1113 .83368 .88238 .15516 .05600 Uiso ? ? 1.00000 ? ? H1114 1.04151 .86661 .11036 .05900 Uiso ? ? 1.00000 ? ? H1115 1.14069 .75069 .11630 .05300 Uiso ? ? 1.00000 ? ? H1116 1.03564 .64712 .16825 .04200 Uiso ? ? 1.00000 ? ? H1122 .96083 .67883 .32510 .03600 Uiso ? ? 1.00000 ? ? H1123 1.07862 .62702 .41898 .04400 Uiso ? ? 1.00000 ? ? H1124 1.08302 .49882 .44304 .04700 Uiso ? ? 1.00000 ? ? H1125 .97034 .42010 .37334 .04900 Uiso ? ? 1.00000 ? ? H1126 .84913 .47085 .28034 .04100 Uiso ? ? 1.00000 ? ? H11a .84999 .58114 .10857 .03600 Uiso ? ? 1.00000 ? ? H11b .82373 .51259 .16102 .03600 Uiso ? ? 1.00000 ? ? H12a .64040 .50573 .12524 .03200 Uiso ? ? 1.00000 ? ? H12b .67701 .56327 .06213 .03200 Uiso ? ? 1.00000 ? ? H1212 .72835 .67745 .03804 .04000 Uiso ? ? 1.00000 ? ? H1213 .75132 .79046 -.02995 .05300 Uiso ? ? 1.00000 ? ? H1214 .59793 .88622 -.01356 .05200 Uiso ? ? 1.00000 ? ? H1215 .42354 .86726 .06771 .05300 Uiso ? ? 1.00000 ? ? H1216 .40247 .75507 .13775 .04300 Uiso ? ? 1.00000 ? ? H1222 .41118 .62573 .02412 .04400 Uiso ? ? 1.00000 ? ? H1223 .21995 .57713 -.00035 .05100 Uiso ? ? 1.00000 ? ? H1224 .10748 .50979 .09134 .05300 Uiso ? ? 1.00000 ? ? H1225 .18191 .48929 .21056 .05400 Uiso ? ? 1.00000 ? ? H1226 .37117 .53464 .23640 .04100 Uiso ? ? 1.00000 ? ? H2112 .59621 .12377 .08281 .03800 Uiso ? ? 1.00000 ? ? H2113 .63704 .00953 .02293 .04900 Uiso ? ? 1.00000 ? ? H2114 .83275 -.04728 .02147 .04900 Uiso ? ? 1.00000 ? ? H2115 .98843 .01144 .07839 .05300 Uiso ? ? 1.00000 ? ? H2116 .94813 .12520 .13866 .04200 Uiso ? ? 1.00000 ? ? H2122 .87053 .26027 .03501 .04700 Uiso ? ? 1.00000 ? ? H2123 1.05911 .31786 .00498 .05600 Uiso ? ? 1.00000 ? ? H2124 1.16626 .36502 .10076 .05300 Uiso ? ? 1.00000 ? ? H2125 1.08800 .35527 .22678 .04800 Uiso ? ? 1.00000 ? ? H2126 .89838 .30017 .25591 .03700 Uiso ? ? 1.00000 ? ? H21a .64316 .32356 .11112 .03700 Uiso ? ? 1.00000 ? ? H21b .61074 .25138 .07200 .03700 Uiso ? ? 1.00000 ? ? H22a .42975 .26231 .12742 .03100 Uiso ? ? 1.00000 ? ? H22b .46836 .32752 .17497 .03100 Uiso ? ? 1.00000 ? ? H2212 .54588 .06116 .22371 .03500 Uiso ? ? 1.00000 ? ? H2213 .45554 -.04262 .17615 .04400 Uiso ? ? 1.00000 ? ? H2214 .25916 -.02886 .13114 .04800 Uiso ? ? 1.00000 ? ? H2215 .15308 .08606 .13801 .05300 Uiso ? ? 1.00000 ? ? H2216 .23957 .18867 .18874 .03800 Uiso ? ? 1.00000 ? ? H2222 .28448 .16015 .34668 .03300 Uiso ? ? 1.00000 ? ? H2223 .13824 .21356 .43604 .03700 Uiso ? ? 1.00000 ? ? H2224 .11636 .34334 .44544 .03800 Uiso ? ? 1.00000 ? ? H2225 .24320 .42001 .37065 .03900 Uiso ? ? 1.00000 ? ? H2226 .39372 .36772 .28371 .03300 Uiso ? ? 1.00000 ? ? H1011a .61030 .54746 .45135 .05600 Uiso ? ? 1.00000 ? ? H1011b .61025 .61229 .50730 .05600 Uiso ? ? 1.00000 ? ? H1011c .71879 .60075 .44782 .05600 Uiso ? ? 1.00000 ? ? H1021a .76280 .77930 .34702 .05100 Uiso ? ? 1.00000 ? ? H1021b .77579 .72617 .41592 .05100 Uiso ? ? 1.00000 ? ? H1021c .69632 .79895 .42207 .05100 Uiso ? ? 1.00000 ? ? H1031a .49268 .86210 .33295 .05200 Uiso ? ? 1.00000 ? ? H1031b .45021 .83185 .25884 .05200 Uiso ? ? 1.00000 ? ? H1031c .58837 .83872 .26867 .05200 Uiso ? ? 1.00000 ? ? H1041a .26158 .66595 .28779 .04900 Uiso ? ? 1.00000 ? ? H1041b .30546 .74122 .25306 .04900 Uiso ? ? 1.00000 ? ? H1041c .24220 .73791 .33363 .04900 Uiso ? ? 1.00000 ? ? H1051a .33041 .58196 .45061 .05000 Uiso ? ? 1.00000 ? ? H1051b .41843 .52779 .40450 .05000 Uiso ? ? 1.00000 ? ? H1051c .30993 .56676 .36745 .05000 Uiso ? ? 1.00000 ? ? H2011a .91783 .26924 .39716 .05400 Uiso ? ? 1.00000 ? ? H2011b .84287 .26316 .47413 .05400 Uiso ? ? 1.00000 ? ? H2011c .79284 .31166 .40953 .05400 Uiso ? ? 1.00000 ? ? H2021a .56406 .27652 .46143 .06900 Uiso ? ? 1.00000 ? ? H2021b .59014 .21670 .52279 .06900 Uiso ? ? 1.00000 ? ? H2021c .48433 .20713 .47268 .06900 Uiso ? ? 1.00000 ? ? H2031a .49303 .04672 .35458 .06500 Uiso ? ? 1.00000 ? ? H2031b .44989 .09982 .41934 .06500 Uiso ? ? 1.00000 ? ? H2031c .53188 .02878 .43513 .06500 Uiso ? ? 1.00000 ? ? H2041a .81193 -.01455 .32755 .06200 Uiso ? ? 1.00000 ? ? H2041b .79250 .02341 .25023 .06200 Uiso ? ? 1.00000 ? ? H2041c .68217 -.00879 .29838 .06200 Uiso ? ? 1.00000 ? ? H2051a 1.00701 .11959 .35549 .04900 Uiso ? ? 1.00000 ? ? H2051b .98606 .18218 .29602 .04900 Uiso ? ? 1.00000 ? ? H2051c .96597 .10016 .27727 .04900 Uiso ? ? 1.00000 ? ? H01a .85586 .07781 .75666 .07600 Uiso ? ? .50000 ? ? H01b .88091 .12907 .68647 .07600 Uiso ? ? .50000 ? ? H01c .96636 .06007 .69972 .07600 Uiso ? ? .50000 ? ? H02a .82129 -.01277 .67932 .28800 Uiso ? ? .50000 ? ? H02b .73326 .05553 .66855 .28800 Uiso ? ? .50000 ? ? H03a .94351 .02304 .58892 .33400 Uiso ? ? .50000 ? ? H03b .92831 .10514 .61415 .33400 Uiso ? ? .50000 ? ? H04a .79581 .11168 .52514 .38300 Uiso ? ? .50000 ? ? H04b .70880 .08045 .58992 .38300 Uiso ? ? .50000 ? ? H05a .72878 -.01436 .48667 .23500 Uiso ? ? .50000 ? ? H05b .78212 -.04987 .55773 .23500 Uiso ? ? .50000 ? ? H05c .86914 -.01863 .49295 .23500 Uiso ? ? .50000 ? ? H01'a 1.00408 .20905 .60257 .20400 Uiso ? ? .50000 ? ? H01'b 1.06207 .12965 .61207 .20400 Uiso ? ? .50000 ? ? H01'c .96210 .15919 .67113 .20400 Uiso ? ? .50000 ? ? H02'a .91347 .12483 .52200 .08400 Uiso ? ? .50000 ? ? H02'b .81350 .15437 .58105 .08400 Uiso ? ? .50000 ? ? H03'a .89122 .06813 .66037 .33400 Uiso ? ? .50000 ? ? H03'b .95769 .03294 .58929 .33400 Uiso ? ? .50000 ? ? H04'a .69866 .05196 .59690 .19300 Uiso ? ? .50000 ? ? H04'b .75667 -.02105 .62872 .19300 Uiso ? ? .50000 ? ? H05'a .72263 -.03791 .50750 .23500 Uiso ? ? .50000 ? ? H05'b .86121 -.04510 .51940 .23500 Uiso ? ? .50000 ? ? H05'c .80699 .02761 .48464 .23500 Uiso ? ? .50000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os1 .02069(6) .01333(5) .01555(5) .00219(4) -.00153(4) -.00083(4) Os2 .01645(5) .01343(5) .01401(5) .00089(4) -.00001(4) -.00173(4) C1 .0220(14) .0181(13) .0211(14) .0018(11) -.0033(11) -.0008(11) C2 .0220(14) .0190(14) .0226(14) .0025(11) -.0029(11) -.0004(11) C3 .0204(14) .0181(13) .0221(14) .0014(11) -.0022(11) -.0020(11) C4 .0212(14) .0156(12) .0174(13) .0004(10) -.0004(10) -.0026(10) P11 .0225(4) .0189(4) .0207(4) .0026(3) -.0008(3) -.0015(3) C1111 .0285(16) .0261(16) .0215(15) -.0018(13) -.0019(12) -.0000(12) C1112 .0318(18) .0255(16) .0279(17) -.0036(14) -.0005(14) .0007(13) C1113 .059(3) .031(2) .042(2) -.007(2) -.003(2) .0098(17) C1114 .054(3) .042(2) .039(2) -.019(2) -.001(2) .0109(18) C1115 .038(2) .060(3) .035(2) -.018(2) .0030(17) .002(2) C1116 .0313(19) .038(2) .0321(19) -.0019(16) .0022(15) .0012(15) C1121 .0198(14) .0252(15) .0252(15) .0050(12) .0003(12) .0010(12) C1122 .0290(17) .0312(18) .0280(17) .0029(14) -.0038(14) -.0010(14) C1123 .0285(18) .050(2) .0267(17) .0045(17) -.0049(14) -.0059(16) C1124 .0264(18) .052(2) .0305(18) .0106(17) -.0010(14) .0095(17) C1125 .0255(18) .037(2) .054(2) .0061(15) -.0022(17) .0197(18) C1126 .0216(16) .0302(18) .047(2) .0028(14) -.0041(15) .0080(16) C11 .0293(17) .0281(17) .0289(17) .0056(14) .0024(14) -.0091(13) C12 .0305(17) .0242(16) .0226(15) .0056(13) .0004(13) -.0063(12) P12 .0256(4) .0167(3) .0179(3) .0018(3) -.0030(3) -.0018(3) C1211 .0350(18) .0233(15) .0173(14) -.0035(13) -.0089(12) -.0010(11) C1212 .038(2) .035(2) .0275(17) -.0021(16) -.0069(15) .0062(15) C1213 .055(3) .044(2) .032(2) -.016(2) -.0124(18) .0112(17) C1214 .069(3) .0267(19) .032(2) -.0134(19) -.015(2) .0037(15) C1215 .081(3) .0197(16) .0285(19) .0107(19) -.009(2) -.0047(14) C1216 .052(2) .0231(16) .0224(16) .0052(16) -.0014(15) -.0019(13) C1221 .0290(17) .0181(14) .0287(16) .0023(12) -.0040(13) -.0047(12) C1222 .037(2) .034(2) .0315(18) .0009(16) -.0110(15) -.0083(15) C1223 .045(2) .037(2) .045(2) .0065(18) -.023(2) -.0149(18) C1224 .031(2) .035(2) .063(3) .0004(16) -.017(2) -.016(2) C1225 .038(2) .039(2) .054(3) -.0134(18) -.008(2) -.001(2) C1226 .034(2) .0291(18) .0345(19) -.0045(15) -.0054(15) .0002(15) P21 .0205(4) .0171(3) .0164(3) .0004(3) .0009(3) -.0018(3) C2111 .0283(16) .0228(15) .0142(13) -.0001(12) .0004(11) -.0043(11) C2112 .0335(19) .0311(18) .0272(17) -.0018(15) -.0015(14) -.0103(14) C2113 .054(3) .036(2) .0292(19) -.0118(18) -.0020(17) -.0142(16) C2114 .063(3) .0280(19) .0280(18) .0040(18) .0037(18) -.0100(15) C2115 .048(2) .039(2) .039(2) .0164(18) -.0011(18) -.0137(17) C2116 .0320(19) .035(2) .035(2) .0096(15) -.0032(15) -.0151(15) C2121 .0233(15) .0242(15) .0241(15) -.0057(12) .0056(12) -.0009(12) C2122 .038(2) .050(2) .0256(18) -.0162(18) .0058(15) -.0006(16) C2123 .044(2) .059(3) .036(2) -.020(2) .0141(18) -.001(2) C2124 .036(2) .041(2) .055(3) -.0171(18) .012(2) -.002(2) C2125 .036(2) .038(2) .043(2) -.0148(17) .0053(17) -.0123(17) C2126 .0304(18) .0270(17) .0320(18) -.0063(14) .0035(14) -.0069(14) C21 .0317(18) .0313(18) .0229(15) .0078(14) .0033(13) .0082(13) C22 .0245(15) .0289(17) .0222(15) .0025(13) -.0037(12) .0027(12) P22 .0182(3) .0170(3) .0176(3) .0004(3) -.0013(3) -.0016(3) C2211 .0235(15) .0233(15) .0206(14) -.0026(12) .0002(11) -.0037(11) C2212 .0344(18) .0247(16) .0230(15) -.0027(14) -.0007(13) -.0011(12) C2213 .041(2) .0274(18) .038(2) -.0056(16) -.0024(17) -.0070(15) C2214 .044(2) .040(2) .040(2) -.0178(18) -.0016(18) -.0140(17) C2215 .035(2) .056(3) .036(2) -.0102(19) -.0028(17) -.0171(19) C2216 .0253(17) .036(2) .0298(17) -.0025(14) -.0026(13) -.0096(14) C2221 .0176(13) .0262(15) .0221(14) .0031(11) -.0033(11) -.0045(12) C2222 .0239(15) .0289(17) .0242(15) .0009(13) .0010(12) -.0026(13) C2223 .0212(15) .043(2) .0237(16) .0007(14) -.0012(12) -.0026(14) C2224 .0197(15) .045(2) .0296(17) .0090(15) -.0048(13) -.0114(15) C2225 .0241(16) .0312(18) .041(2) .0067(14) -.0050(15) -.0140(15) C2226 .0195(15) .0256(16) .0328(17) .0021(12) -.0012(13) -.0053(13) C101 .0315(17) .0224(15) .0162(13) .0022(13) -.0004(12) -.0007(11) C1011 .045(2) .043(2) .0224(17) .0030(18) -.0079(15) .0061(15) C102 .0311(17) .0247(16) .0187(14) -.0009(13) .0015(12) -.0060(12) C1021 .038(2) .034(2) .0309(18) -.0094(16) -.0014(15) -.0118(15) C103 .0349(18) .0163(13) .0191(14) .0036(12) .0035(12) -.0024(11) C1031 .052(2) .0173(15) .034(2) .0056(15) .0033(17) -.0023(13) C104 .0266(16) .0210(14) .0221(14) .0069(12) .0002(12) -.0033(11) C1041 .0273(17) .035(2) .0350(19) .0115(15) -.0006(14) -.0002(15) C105 .0226(15) .0235(15) .0206(14) .0014(12) .0038(11) -.0017(11) C1051 .0334(19) .0309(19) .0344(19) -.0032(15) .0079(15) .0020(15) C201 .0265(16) .0270(16) .0180(14) .0020(13) -.0068(12) -.0026(12) C2011 .041(2) .035(2) .034(2) .0000(16) -.0170(16) -.0066(15) C202 .0282(17) .039(2) .0147(13) .0078(14) .0000(12) .0021(13) C2021 .041(2) .076(3) .0194(17) .016(2) .0034(16) -.0064(18) C203 .0280(17) .0297(17) .0230(15) .0002(13) -.0020(13) .0109(13) C2031 .035(2) .052(3) .041(2) -.0122(18) -.0027(17) .026(2) C204 .0296(17) .0195(14) .0252(15) .0037(12) -.0040(13) .0039(12) C2041 .050(2) .0175(16) .057(3) .0048(16) -.014(2) .0005(16) C205 .0232(15) .0217(14) .0226(14) .0041(12) -.0023(12) .0009(11) C2051 .0230(16) .035(2) .041(2) .0061(14) -.0019(15) -.0007(16) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Os1 C1 . . 2.010(3) ? Os1 P11 . . 2.2583(9) ? Os1 P12 . . 2.2515(9) ? Os1 C101 . . 2.226(3) ? Os1 C102 . . 2.255(3) ? Os1 C103 . . 2.285(3) ? Os1 C104 . . 2.285(3) ? Os1 C105 . . 2.255(3) ? Os2 C4 . . 2.015(3) ? Os2 P21 . . 2.2451(8) ? Os2 P22 . . 2.2548(9) ? Os2 C201 . . 2.248(3) ? Os2 C202 . . 2.224(3) ? Os2 C203 . . 2.250(3) ? Os2 C204 . . 2.276(3) ? Os2 C205 . . 2.279(3) ? C1 C2 . . 1.220(4) ? C2 C3 . . 1.380(4) ? C3 C4 . . 1.224(4) ? P11 C1111 . . 1.840(3) ? P11 C1121 . . 1.830(3) ? P11 C11 . . 1.869(4) ? C1111 C1112 . . 1.386(5) ? C1111 C1116 . . 1.409(5) ? C1112 C1113 . . 1.398(5) ? C1112 H1112 . . .953 ? C1113 C1114 . . 1.373(6) ? C1113 H1113 . . .971 ? C1114 C1115 . . 1.370(6) ? C1114 H1114 . . .964 ? C1115 C1116 . . 1.392(6) ? C1115 H1115 . . .969 ? C1116 H1116 . . .970 ? C1121 C1122 . . 1.396(5) ? C1121 C1126 . . 1.392(5) ? C1122 C1123 . . 1.387(5) ? C1122 H1122 . . .970 ? C1123 C1124 . . 1.377(6) ? C1123 H1123 . . .960 ? C1124 C1125 . . 1.376(6) ? C1124 H1124 . . .960 ? C1125 C1126 . . 1.388(6) ? C1125 H1125 . . .974 ? C1126 H1126 . . .975 ? C11 C12 . . 1.523(5) ? C11 H11a . . .956 ? C11 H11b . . .961 ? C12 P12 . . 1.846(3) ? C12 H12a . . .966 ? C12 H12b . . .952 ? P12 C1211 . . 1.829(3) ? P12 C1221 . . 1.828(4) ? C1211 C1212 . . 1.391(5) ? C1211 C1216 . . 1.390(5) ? C1212 C1213 . . 1.395(6) ? C1212 H1212 . . .967 ? C1213 C1214 . . 1.385(6) ? C1213 H1213 . . .974 ? C1214 C1215 . . 1.375(6) ? C1214 H1214 . . .973 ? C1215 C1216 . . 1.388(5) ? C1215 H1215 . . .973 ? C1216 H1216 . . .980 ? C1221 C1222 . . 1.395(5) ? C1221 C1226 . . 1.391(5) ? C1222 C1223 . . 1.396(6) ? C1222 H1222 . . .976 ? C1223 C1224 . . 1.377(6) ? C1223 H1223 . . .962 ? C1224 C1225 . . 1.389(6) ? C1224 H1224 . . .960 ? C1225 C1226 . . 1.379(6) ? C1225 H1225 . . .969 ? C1226 H1226 . . .973 ? P21 C2111 . . 1.835(3) ? P21 C2121 . . 1.838(3) ? P21 C21 . . 1.862(4) ? C2111 C2112 . . 1.388(5) ? C2111 C2116 . . 1.390(5) ? C2112 C2113 . . 1.389(5) ? C2112 H2112 . . .976 ? C2113 C2114 . . 1.363(6) ? C2113 H2113 . . .977 ? C2114 C2115 . . 1.368(6) ? C2114 H2114 . . .969 ? C2115 C2116 . . 1.388(6) ? C2115 H2115 . . .971 ? C2116 H2116 . . .963 ? C2121 C2122 . . 1.394(5) ? C2121 C2126 . . 1.381(5) ? C2122 C2123 . . 1.390(6) ? C2122 H2122 . . .970 ? C2123 C2124 . . 1.391(6) ? C2123 H2123 . . .965 ? C2124 C2125 . . 1.381(6) ? C2124 H2124 . . .951 ? C2125 C2126 . . 1.395(5) ? C2125 H2125 . . .961 ? C2126 H2126 . . .964 ? C21 C22 . . 1.525(5) ? C21 H21a . . .961 ? C21 H21b . . .958 ? C22 P22 . . 1.850(3) ? C22 H22a . . .958 ? C22 H22b . . .953 ? P22 C2211 . . 1.842(3) ? P22 C2221 . . 1.835(3) ? C2211 C2212 . . 1.389(5) ? C2211 C2216 . . 1.402(5) ? C2212 C2213 . . 1.394(5) ? C2212 H2212 . . .958 ? C2213 C2214 . . 1.387(6) ? C2213 H2213 . . .966 ? C2214 C2215 . . 1.380(6) ? C2214 H2214 . . .970 ? C2215 C2216 . . 1.378(6) ? C2215 H2215 . . .959 ? C2216 H2216 . . .962 ? C2221 C2222 . . 1.398(4) ? C2221 C2226 . . 1.394(5) ? C2222 C2223 . . 1.404(5) ? C2222 H2222 . . .962 ? C2223 C2224 . . 1.384(5) ? C2223 H2223 . . .960 ? C2224 C2225 . . 1.379(5) ? C2224 H2224 . . .956 ? C2225 C2226 . . 1.397(5) ? C2225 H2225 . . .968 ? C2226 H2226 . . .952 ? C101 C1011 . . 1.498(5) ? C101 C102 . . 1.428(5) ? C101 C105 . . 1.449(5) ? C1011 H1011a . . .953 ? C1011 H1011b . . .950 ? C1011 H1011c . . .960 ? C102 C1021 . . 1.504(5) ? C102 C103 . . 1.424(5) ? C1021 H1021a . . .962 ? C1021 H1021b . . .945 ? C1021 H1021c . . .958 ? C103 C1031 . . 1.507(5) ? C103 C104 . . 1.441(5) ? C1031 H1031a . . .955 ? C1031 H1031b . . .954 ? C1031 H1031c . . .955 ? C104 C1041 . . 1.497(5) ? C104 C105 . . 1.421(4) ? C1041 H1041a . . .950 ? C1041 H1041b . . .962 ? C1041 H1041c . . .947 ? C105 C1051 . . 1.484(5) ? C1051 H1051a . . .951 ? C1051 H1051b . . .958 ? C1051 H1051c . . .961 ? C201 C2011 . . 1.512(5) ? C201 C202 . . 1.432(5) ? C201 C205 . . 1.418(4) ? C2011 H2011a . . .969 ? C2011 H2011b . . .950 ? C2011 H2011c . . .944 ? C202 C2021 . . 1.513(5) ? C202 C203 . . 1.430(5) ? C2021 H2021a . . .945 ? C2021 H2021b . . .953 ? C2021 H2021c . . .961 ? C203 C2031 . . 1.500(5) ? C203 C204 . . 1.433(5) ? C2031 H2031a . . .966 ? C2031 H2031b . . .948 ? C2031 H2031c . . .951 ? C204 C2041 . . 1.494(5) ? C204 C205 . . 1.440(5) ? C2041 H2041a . . .953 ? C2041 H2041b . . .956 ? C2041 H2041c . . .957 ? C205 C2051 . . 1.502(5) ? C2051 H2051a . . .955 ? C2051 H2051b . . .956 ? C2051 H2051c . . .955 ? C01 C02 . . 1.31(2) ? C01 H01a . . .977 ? C01 H01b . . .946 ? C01 H01c . . .962 ? C02 C03 . . 1.42(2) ? C02 H02a . . .897 ? C02 H02b . . .927 ? C03 C04 . . 1.46(3) ? C03 C02' . . 1.269(15) ? C03 C04' . . 1.56(2) ? C03 H03a . . 1.013 ? C03 H03b . . .846 ? C03 H03'a . . .929 ? C03 H03'b . . .989 ? C04 C05 . . 1.57(3) ? C04 H04a . . .96 ? C04 H04b . . 1.09 ? C05 C04' . . 1.43(2) ? C05 H05a . . .981 ? C05 H05b . . .913 ? C05 H05c . . .957 ? C05 H05'a . . .960 ? C05 H05'b . . .931 ? C05 H05'c . . .986 ? C01' C02' . . 1.447(17) ? C01' H01'a . . .888 ? C01' H01'b . . .945 ? C01' H01'c . . 1.111 ? C02' H02'a . . .935 ? C02' H02'b . . .974 ? C04' H04'a . . 1.073 ? C04' H04'b . . .912 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 Os1 P11 . . . 81.79(9) ? C1 Os1 P12 . . . 84.72(9) ? C1 Os1 C101 . . . 93.96(12) ? C1 Os1 C102 . . . 128.39(12) ? C1 Os1 C103 . . . 151.15(11) ? C1 Os1 C104 . . . 119.57(12) ? C1 Os1 C105 . . . 89.92(12) ? P11 Os1 P12 . . . 81.18(3) ? P11 Os1 C101 . . . 114.42(9) ? P11 Os1 C102 . . . 101.94(9) ? P11 Os1 C103 . . . 121.23(9) ? P11 Os1 C104 . . . 157.89(8) ? P11 Os1 C105 . . . 150.58(8) ? P12 Os1 C101 . . . 164.05(9) ? P12 Os1 C102 . . . 146.88(8) ? P12 Os1 C103 . . . 113.98(8) ? P12 Os1 C104 . . . 104.98(8) ? P12 Os1 C105 . . . 126.32(9) ? C101 Os1 C102 . . . 37.17(11) ? C101 Os1 C103 . . . 61.87(11) ? C101 Os1 C104 . . . 61.94(12) ? C101 Os1 C105 . . . 37.73(12) ? C102 Os1 C103 . . . 36.56(12) ? C102 Os1 C104 . . . 61.24(12) ? C102 Os1 C105 . . . 61.84(12) ? C103 Os1 C104 . . . 36.75(12) ? C103 Os1 C105 . . . 61.42(11) ? C104 Os1 C105 . . . 36.47(11) ? C4 Os2 P21 . . . 83.19(8) ? C4 Os2 P22 . . . 81.03(9) ? C4 Os2 C201 . . . 91.50(12) ? C4 Os2 C202 . . . 98.07(12) ? C4 Os2 C203 . . . 133.21(12) ? C4 Os2 C204 . . . 152.97(12) ? C4 Os2 C205 . . . 118.82(12) ? P21 Os2 P22 . . . 82.66(3) ? P21 Os2 C201 . . . 127.28(8) ? P21 Os2 C202 . . . 164.38(9) ? P21 Os2 C203 . . . 143.57(9) ? P21 Os2 C204 . . . 110.73(8) ? P21 Os2 C205 . . . 103.77(8) ? P22 Os2 C201 . . . 148.28(8) ? P22 Os2 C202 . . . 112.94(9) ? P22 Os2 C203 . . . 101.90(9) ? P22 Os2 C204 . . . 122.60(9) ? P22 Os2 C205 . . . 159.47(8) ? C201 Os2 C202 . . . 37.35(12) ? C201 Os2 C203 . . . 61.60(12) ? C201 Os2 C204 . . . 61.54(12) ? C201 Os2 C205 . . . 36.49(11) ? C202 Os2 C203 . . . 37.27(13) ? C202 Os2 C204 . . . 62.28(12) ? C202 Os2 C205 . . . 61.90(12) ? C203 Os2 C204 . . . 36.91(12) ? C203 Os2 C205 . . . 61.35(12) ? C204 Os2 C205 . . . 36.87(12) ? Os1 C1 C2 . . . 177.4(3) ? C1 C2 C3 . . . 176.2(3) ? C2 C3 C4 . . . 177.4(3) ? Os2 C4 C3 . . . 177.2(3) ? Os1 P11 C1111 . . . 120.44(11) ? Os1 P11 C1121 . . . 115.91(10) ? Os1 P11 C11 . . . 110.51(11) ? C1111 P11 C1121 . . . 100.92(15) ? C1111 P11 C11 . . . 101.71(15) ? C1121 P11 C11 . . . 105.47(15) ? P11 C1111 C1112 . . . 120.2(3) ? P11 C1111 C1116 . . . 121.3(3) ? C1112 C1111 C1116 . . . 118.4(3) ? C1111 C1112 C1113 . . . 120.6(3) ? C1111 C1112 H1112 . . . 119.3 ? C1113 C1112 H1112 . . . 120.1 ? C1112 C1113 C1114 . . . 119.9(4) ? C1112 C1113 H1113 . . . 119.4 ? C1114 C1113 H1113 . . . 120.7 ? C1113 C1114 C1115 . . . 120.8(4) ? C1113 C1114 H1114 . . . 121.2 ? C1115 C1114 H1114 . . . 118.0 ? C1114 C1115 C1116 . . . 119.9(4) ? C1114 C1115 H1115 . . . 120.7 ? C1116 C1115 H1115 . . . 119.3 ? C1111 C1116 C1115 . . . 120.3(3) ? C1111 C1116 H1116 . . . 119.2 ? C1115 C1116 H1116 . . . 120.5 ? P11 C1121 C1122 . . . 119.6(2) ? P11 C1121 C1126 . . . 121.6(3) ? C1122 C1121 C1126 . . . 118.3(3) ? C1121 C1122 C1123 . . . 120.8(3) ? C1121 C1122 H1122 . . . 119.7 ? C1123 C1122 H1122 . . . 119.5 ? C1122 C1123 C1124 . . . 120.0(4) ? C1122 C1123 H1123 . . . 120.2 ? C1124 C1123 H1123 . . . 119.8 ? C1123 C1124 C1125 . . . 120.1(4) ? C1123 C1124 H1124 . . . 119.8 ? C1125 C1124 H1124 . . . 120.1 ? C1124 C1125 C1126 . . . 120.2(4) ? C1124 C1125 H1125 . . . 120.2 ? C1126 C1125 H1125 . . . 119.6 ? C1121 C1126 C1125 . . . 120.7(3) ? C1121 C1126 H1126 . . . 119.7 ? C1125 C1126 H1126 . . . 119.6 ? P11 C11 C12 . . . 111.6(2) ? P11 C11 H11a . . . 109.1 ? P11 C11 H11b . . . 108.9 ? C12 C11 H11a . . . 109.3 ? C12 C11 H11b . . . 109.7 ? H11a C11 H11b . . . 108.1 ? C11 C12 P12 . . . 112.5(2) ? C11 C12 H12a . . . 108.7 ? C11 C12 H12b . . . 109.5 ? P12 C12 H12a . . . 108.6 ? P12 C12 H12b . . . 109.4 ? H12a C12 H12b . . . 108.0 ? Os1 P12 C12 . . . 108.80(11) ? Os1 P12 C1211 . . . 117.11(11) ? Os1 P12 C1221 . . . 119.79(11) ? C12 P12 C1211 . . . 104.76(15) ? C12 P12 C1221 . . . 103.03(15) ? C1211 P12 C1221 . . . 101.56(15) ? P12 C1211 C1212 . . . 122.0(3) ? P12 C1211 C1216 . . . 119.2(2) ? C1212 C1211 C1216 . . . 118.5(3) ? C1211 C1212 C1213 . . . 121.2(3) ? C1211 C1212 H1212 . . . 119.4 ? C1213 C1212 H1212 . . . 119.4 ? C1212 C1213 C1214 . . . 119.0(4) ? C1212 C1213 H1213 . . . 119.7 ? C1214 C1213 H1213 . . . 121.3 ? C1213 C1214 C1215 . . . 120.5(4) ? C1213 C1214 H1214 . . . 119.4 ? C1215 C1214 H1214 . . . 120.1 ? C1214 C1215 C1216 . . . 120.3(4) ? C1214 C1215 H1215 . . . 119.5 ? C1216 C1215 H1215 . . . 120.2 ? C1211 C1216 C1215 . . . 120.5(3) ? C1211 C1216 H1216 . . . 120.2 ? C1215 C1216 H1216 . . . 119.2 ? P12 C1221 C1222 . . . 122.2(3) ? P12 C1221 C1226 . . . 119.3(3) ? C1222 C1221 C1226 . . . 118.4(3) ? C1221 C1222 C1223 . . . 120.1(3) ? C1221 C1222 H1222 . . . 120.0 ? C1223 C1222 H1222 . . . 119.9 ? C1222 C1223 C1224 . . . 120.8(4) ? C1222 C1223 H1223 . . . 120.8 ? C1224 C1223 H1223 . . . 118.5 ? C1223 C1224 C1225 . . . 119.2(4) ? C1223 C1224 H1224 . . . 120.3 ? C1225 C1224 H1224 . . . 120.5 ? C1224 C1225 C1226 . . . 120.4(4) ? C1224 C1225 H1225 . . . 119.4 ? C1226 C1225 H1225 . . . 120.2 ? C1221 C1226 C1225 . . . 121.1(4) ? C1221 C1226 H1226 . . . 119.8 ? C1225 C1226 H1226 . . . 119.1 ? Os2 P21 C2111 . . . 116.78(10) ? Os2 P21 C2121 . . . 120.14(11) ? Os2 P21 C21 . . . 111.15(11) ? C2111 P21 C2121 . . . 99.35(14) ? C2111 P21 C21 . . . 104.93(15) ? C2121 P21 C21 . . . 102.45(15) ? P21 C2111 C2112 . . . 120.9(2) ? P21 C2111 C2116 . . . 121.3(3) ? C2112 C2111 C2116 . . . 117.5(3) ? C2111 C2112 C2113 . . . 121.3(3) ? C2111 C2112 H2112 . . . 118.8 ? C2113 C2112 H2112 . . . 119.8 ? C2112 C2113 C2114 . . . 120.3(4) ? C2112 C2113 H2113 . . . 119.0 ? C2114 C2113 H2113 . . . 120.7 ? C2113 C2114 C2115 . . . 119.5(4) ? C2113 C2114 H2114 . . . 119.7 ? C2115 C2114 H2114 . . . 120.8 ? C2114 C2115 C2116 . . . 120.9(4) ? C2114 C2115 H2115 . . . 119.7 ? C2116 C2115 H2115 . . . 119.4 ? C2111 C2116 C2115 . . . 120.6(4) ? C2111 C2116 H2116 . . . 119.6 ? C2115 C2116 H2116 . . . 119.9 ? P21 C2121 C2122 . . . 120.1(3) ? P21 C2121 C2126 . . . 120.9(2) ? C2122 C2121 C2126 . . . 119.0(3) ? C2121 C2122 C2123 . . . 120.5(4) ? C2121 C2122 H2122 . . . 119.1 ? C2123 C2122 H2122 . . . 120.4 ? C2122 C2123 C2124 . . . 119.9(4) ? C2122 C2123 H2123 . . . 120.2 ? C2124 C2123 H2123 . . . 119.9 ? C2123 C2124 C2125 . . . 119.9(4) ? C2123 C2124 H2124 . . . 119.3 ? C2125 C2124 H2124 . . . 120.8 ? C2124 C2125 C2126 . . . 119.9(4) ? C2124 C2125 H2125 . . . 120.2 ? C2126 C2125 H2125 . . . 119.9 ? C2121 C2126 C2125 . . . 120.7(3) ? C2121 C2126 H2126 . . . 119.5 ? C2125 C2126 H2126 . . . 119.8 ? P21 C21 C22 . . . 113.5(2) ? P21 C21 H21a . . . 108.4 ? P21 C21 H21b . . . 108.6 ? C22 C21 H21a . . . 109.0 ? C22 C21 H21b . . . 109.2 ? H21a C21 H21b . . . 107.9 ? C21 C22 P22 . . . 112.0(2) ? C21 C22 H22a . . . 109.0 ? C21 C22 H22b . . . 109.3 ? P22 C22 H22a . . . 108.8 ? P22 C22 H22b . . . 109.0 ? H22a C22 H22b . . . 108.6 ? Os2 P22 C22 . . . 110.65(11) ? Os2 P22 C2211 . . . 120.06(11) ? Os2 P22 C2221 . . . 117.35(11) ? C22 P22 C2211 . . . 101.86(15) ? C22 P22 C2221 . . . 104.13(14) ? C2211 P22 C2221 . . . 100.60(14) ? P22 C2211 C2212 . . . 119.6(3) ? P22 C2211 C2216 . . . 121.5(3) ? C2212 C2211 C2216 . . . 118.7(3) ? C2211 C2212 C2213 . . . 121.0(3) ? C2211 C2212 H2212 . . . 120.1 ? C2213 C2212 H2212 . . . 119.0 ? C2212 C2213 C2214 . . . 119.0(3) ? C2212 C2213 H2213 . . . 120.4 ? C2214 C2213 H2213 . . . 120.5 ? C2213 C2214 C2215 . . . 120.6(4) ? C2213 C2214 H2214 . . . 119.7 ? C2215 C2214 H2214 . . . 119.7 ? C2214 C2215 C2216 . . . 120.3(4) ? C2214 C2215 H2215 . . . 119.5 ? C2216 C2215 H2215 . . . 120.2 ? C2211 C2216 C2215 . . . 120.3(3) ? C2211 C2216 H2216 . . . 120.1 ? C2215 C2216 H2216 . . . 119.5 ? P22 C2221 C2222 . . . 119.4(2) ? P22 C2221 C2226 . . . 121.5(2) ? C2222 C2221 C2226 . . . 118.8(3) ? C2221 C2222 C2223 . . . 120.3(3) ? C2221 C2222 H2222 . . . 119.6 ? C2223 C2222 H2222 . . . 120.1 ? C2222 C2223 C2224 . . . 120.5(3) ? C2222 C2223 H2223 . . . 120.2 ? C2224 C2223 H2223 . . . 119.4 ? C2223 C2224 C2225 . . . 119.2(3) ? C2223 C2224 H2224 . . . 120.7 ? C2225 C2224 H2224 . . . 120.1 ? C2224 C2225 C2226 . . . 121.1(3) ? C2224 C2225 H2225 . . . 118.5 ? C2226 C2225 H2225 . . . 120.4 ? C2221 C2226 C2225 . . . 120.2(3) ? C2221 C2226 H2226 . . . 119.7 ? C2225 C2226 H2226 . . . 120.2 ? Os1 C101 C1011 . . . 124.6(2) ? Os1 C101 C102 . . . 72.52(17) ? Os1 C101 C105 . . . 72.24(17) ? C1011 C101 C102 . . . 127.8(3) ? C1011 C101 C105 . . . 124.7(3) ? C102 C101 C105 . . . 107.3(3) ? C101 C1011 H1011a . . . 110.6 ? C101 C1011 H1011b . . . 110.8 ? C101 C1011 H1011c . . . 109.8 ? H1011a C1011 H1011b . . . 109.2 ? H1011a C1011 H1011c . . . 108.3 ? H1011b C1011 H1011c . . . 108.1 ? Os1 C102 C101 . . . 70.31(18) ? Os1 C102 C1021 . . . 128.6(2) ? Os1 C102 C103 . . . 72.87(18) ? C101 C102 C1021 . . . 125.9(3) ? C101 C102 C103 . . . 108.8(3) ? C1021 C102 C103 . . . 124.9(3) ? C102 C1021 H1021a . . . 112.0 ? C102 C1021 H1021b . . . 112.8 ? C102 C1021 H1021c . . . 109.6 ? H1021a C1021 H1021b . . . 108.8 ? H1021a C1021 H1021c . . . 104.6 ? H1021b C1021 H1021c . . . 108.7 ? Os1 C103 C102 . . . 70.57(18) ? Os1 C103 C1031 . . . 133.0(2) ? Os1 C103 C104 . . . 71.63(17) ? C102 C103 C1031 . . . 126.2(3) ? C102 C103 C104 . . . 107.7(3) ? C1031 C103 C104 . . . 124.9(3) ? C103 C1031 H1031a . . . 110.6 ? C103 C1031 H1031b . . . 110.5 ? C103 C1031 H1031c . . . 110.1 ? H1031a C1031 H1031b . . . 108.7 ? H1031a C1031 H1031c . . . 108.5 ? H1031b C1031 H1031c . . . 108.4 ? Os1 C104 C103 . . . 71.62(17) ? Os1 C104 C1041 . . . 129.5(2) ? Os1 C104 C105 . . . 70.63(17) ? C103 C104 C1041 . . . 126.2(3) ? C103 C104 C105 . . . 108.2(3) ? C1041 C104 C105 . . . 125.1(3) ? C104 C1041 H1041a . . . 110.3 ? C104 C1041 H1041b . . . 110.1 ? C104 C1041 H1041c . . . 110.2 ? H1041a C1041 H1041b . . . 108.4 ? H1041a C1041 H1041c . . . 109.1 ? H1041b C1041 H1041c . . . 108.6 ? Os1 C105 C101 . . . 70.03(17) ? Os1 C105 C104 . . . 72.90(17) ? Os1 C105 C1051 . . . 126.5(2) ? C101 C105 C104 . . . 108.0(3) ? C101 C105 C1051 . . . 124.4(3) ? C104 C105 C1051 . . . 127.5(3) ? C105 C1051 H1051a . . . 111.5 ? C105 C1051 H1051b . . . 110.9 ? C105 C1051 H1051c . . . 110.1 ? H1051a C1051 H1051b . . . 108.7 ? H1051a C1051 H1051c . . . 108.3 ? H1051b C1051 H1051c . . . 107.1 ? Os2 C201 C2011 . . . 124.5(2) ? Os2 C201 C202 . . . 70.43(18) ? Os2 C201 C205 . . . 72.95(18) ? C2011 C201 C202 . . . 124.0(3) ? C2011 C201 C205 . . . 127.2(3) ? C202 C201 C205 . . . 108.8(3) ? C201 C2011 H2011a . . . 109.6 ? C201 C2011 H2011b . . . 110.7 ? C201 C2011 H2011c . . . 110.8 ? H2011a C2011 H2011b . . . 107.8 ? H2011a C2011 H2011c . . . 108.0 ? H2011b C2011 H2011c . . . 109.9 ? Os2 C202 C201 . . . 72.23(17) ? Os2 C202 C2021 . . . 125.6(2) ? Os2 C202 C203 . . . 72.33(18) ? C201 C202 C2021 . . . 125.2(3) ? C201 C202 C203 . . . 107.2(3) ? C2021 C202 C203 . . . 127.4(3) ? C202 C2021 H2021a . . . 111.4 ? C202 C2021 H2021b . . . 111.1 ? C202 C2021 H2021c . . . 109.4 ? H2021a C2021 H2021b . . . 109.6 ? H2021a C2021 H2021c . . . 108.6 ? H2021b C2021 H2021c . . . 106.6 ? Os2 C203 C202 . . . 70.40(18) ? Os2 C203 C2031 . . . 129.7(3) ? Os2 C203 C204 . . . 72.52(18) ? C202 C203 C2031 . . . 124.9(3) ? C202 C203 C204 . . . 108.8(3) ? C2031 C203 C204 . . . 125.8(3) ? C203 C2031 H2031a . . . 108.5 ? C203 C2031 H2031b . . . 109.5 ? C203 C2031 H2031c . . . 110.9 ? H2031a C2031 H2031b . . . 108.3 ? H2031a C2031 H2031c . . . 108.4 ? H2031b C2031 H2031c . . . 111.2 ? Os2 C204 C203 . . . 70.57(18) ? Os2 C204 C2041 . . . 131.3(3) ? Os2 C204 C205 . . . 71.71(18) ? C203 C204 C2041 . . . 126.9(3) ? C203 C204 C205 . . . 107.1(3) ? C2041 C204 C205 . . . 125.1(3) ? C204 C2041 H2041a . . . 110.6 ? C204 C2041 H2041b . . . 110.2 ? C204 C2041 H2041c . . . 110.2 ? H2041a C2041 H2041b . . . 108.7 ? H2041a C2041 H2041c . . . 108.6 ? H2041b C2041 H2041c . . . 108.4 ? Os2 C205 C201 . . . 70.56(18) ? Os2 C205 C204 . . . 71.42(18) ? Os2 C205 C2051 . . . 130.4(2) ? C201 C205 C204 . . . 108.2(3) ? C201 C205 C2051 . . . 126.7(3) ? C204 C205 C2051 . . . 124.6(3) ? C205 C2051 H2051a . . . 110.8 ? C205 C2051 H2051b . . . 110.6 ? C205 C2051 H2051c . . . 110.4 ? H2051a C2051 H2051b . . . 108.5 ? H2051a C2051 H2051c . . . 108.5 ? H2051b C2051 H2051c . . . 107.9 ? C02 C01 H01a . . . 108.5 ? C02 C01 H01b . . . 114.0 ? C02 C01 H01c . . . 111.4 ? H01a C01 H01b . . . 107.6 ? H01a C01 H01c . . . 106.3 ? H01b C01 H01c . . . 108.8 ? C01 C02 C03 . . . 77.5(12) ? C01 C02 H02a . . . 114.7 ? C01 C02 H02b . . . 111.7 ? C03 C02 H02a . . . 118.3 ? C03 C02 H02b . . . 112.0 ? H02a C02 H02b . . . 116 ? C02 C03 C04 . . . 93.4(14) ? C02 C03 H03a . . . 105.7 ? C02 C03 H03b . . . 121.1 ? C04 C03 H03a . . . 101.0 ? C04 C03 H03b . . . 119.7 ? C02' C03 C04' . . . 116.9(11) ? C02' C03 H03'a . . . 115.7 ? C02' C03 H03'b . . . 110.0 ? C04' C03 H03'a . . . 105.0 ? C04' C03 H03'b . . . 99.9 ? H03a C03 H03b . . . 112.8 ? H03'a C03 H03'b . . . 107.9 ? C03 C04 C05 . . . 107.2(15) ? C03 C04 H04a . . . 111 ? C03 C04 H04b . . . 105 ? C05 C04 H04a . . . 122 ? C05 C04 H04b . . . 111.8 ? H04a C04 H04b . . . 98 ? C04 C05 H05a . . . 109.4 ? C04 C05 H05b . . . 113.4 ? C04 C05 H05c . . . 105.2 ? C04' C05 H05'a . . . 114.7 ? C04' C05 H05'b . . . 107.7 ? C04' C05 H05'c . . . 110.2 ? H05a C05 H05b . . . 110.0 ? H05a C05 H05c . . . 106.4 ? H05b C05 H05c . . . 112.1 ? H05'a C05 H05'b . . . 110.3 ? H05'a C05 H05'c . . . 105.7 ? H05'b C05 H05'c . . . 108.0 ? C02' C01' H01'a . . . 118.4 ? C02' C01' H01'b . . . 114.3 ? C02' C01' H01'c . . . 105.5 ? H01'a C01' H01'b . . . 115.6 ? H01'a C01' H01'c . . . 101.2 ? H01'b C01' H01'c . . . 97.6 ? C03 C02' C01' . . . 99.2(10) ? C03 C02' H02'a . . . 114.1 ? C03 C02' H02'b . . . 109.1 ? C01' C02' H02'a . . . 110.3 ? C01' C02' H02'b . . . 115.4 ? H02'a C02' H02'b . . . 108.6 ? C03 C04' C05 . . . 110.0 ? C03 C04' H04'a . . . 107.6 ? C03 C04' H04'b . . . 121.9 ? C05 C04' H04'a . . . 105.1 ? C05 C04' H04'b . . . 108.2 ? H04'a C04' H04'b . . . 102.5 ? _exptl_crystal_F_000 1576 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min -30 _reflns_limit_k_max 30 _reflns_limit_l_min -30 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .577 _reflns_d_resolution_low 17.738 _diffrn_reflns_av_sigmaI/netI .119 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 13 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .075 _refine_ls_wR_factor_all .042 _refine_ls_goodness_of_fit_all .987 _refine_ls_shift/su_mean .001