#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000359.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_5000359 ## 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C58 H70 B F24 N O3 Os P2' _[local]_cod_chemical_formula_sum_orig 'C58 H70 B1 F24 N1 O3 Os1 P2' _chemical_formula_moiety ? _chemical_formula_weight 1548.15 _cell_length_a 15.183(2) _cell_length_b 17.785(3) _cell_length_c 24.578(4) _cell_angle_alpha 90 _cell_angle_beta 97.412(4) _cell_angle_gamma 90 _cell_volume 6581.5(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 113 _exptl_crystal_colour yellow _exptl_crystal_description 'small fragment' _exptl_crystal_size_max .23 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .11 _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 2.0948 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z x,1/2-y,1/2+z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_ambient_temperature 113 _diffrn_measurement_device_type 'Bruker AXS Smart6000' _diffrn_measurement_method 'omega scans' _diffrn_detector 'Smart 6000 CCD' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3 _diffrn_reflns_av_R_equivalents 3959 _diffrn_reflns_theta_min 2.02578 _diffrn_reflns_theta_max 27.6665 _diffrn_reflns_theta_full 27.6665 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _reflns_number_total 15093 _reflns_number_gt 3959 _reflns_threshold_expression 'Fo^2^> 2.33\s(Fo^2^)' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source OS Os -1.816 7.605 'International Tables Vol. IV (1974) Table 2.2B' P P 0.09 0.095 'International Tables Vol. IV (1974) Table 2.2B' F F 0.014 0.01 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' B B 0 0.001 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 3959 _refine_ls_number_parameters 782 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef -0.000000003(10) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.0552 _refine_ls_goodness_of_fit_ref 1.0819 _refine_ls_shift/su_max 0.3486 _refine_diff_density_max 2.22 _refine_diff_density_min -1.53 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_disorder_group _atom_site_disorder_assembly OS1 OS 0.2898(3) 0.30529(18) 0.37691(15) 0.0217(9) Uani 0.477(19) 0 . P2 P 0.3013(4) 0.1998(3) 0.43981(19) 0.068(2) Uani 1 0 . C3 C 0.4221(16) 0.1657(10) 0.4489(9) 0.082(10) Uani 1 0 . C4 C 0.4825(18) 0.2258(11) 0.4707(9) 0.114(12) Uani 1 0 . C5 C 0.4348(18) 0.0905(14) 0.4814(11) 0.144(14) Uani 1 0 . C6 C 0.2420(16) 0.1165(10) 0.4195(10) 0.071(10) Uani 1 0 . C7 C 0.139(2) 0.1319(15) 0.4134(12) 0.152(17) Uani 1 0 . C8 C 0.261(2) 0.0773(11) 0.3724(13) 0.123(15) Uani 1 0 . C9 C 0.242(4) 0.215(3) 0.497(2) 0.089(16) Uiso 0.45 0 . C10 C 0.230(4) 0.2889(17) 0.5168(11) 0.27(3) Uani 1 0 . C11 C 0.253(3) 0.1565(17) 0.5449(13) 0.24(3) Uani 1 0 . P12 P 0.2126(4) 0.3777(2) 0.30386(18) 0.0460(19) Uani 1 0 . C13 C 0.0945(15) 0.3698(11) 0.2929(9) 0.082(9) Uani 1 0 . C14 C 0.0526(17) 0.3049(16) 0.2977(16) 0.193(19) Uani 1 0 . C15 C 0.0440(15) 0.4247(14) 0.2526(10) 0.116(12) Uani 1 0 . C16 C 0.2625(13) 0.3622(9) 0.2387(7) 0.060(8) Uani 1 0 . C17 C 0.2383(13) 0.4217(10) 0.1942(7) 0.067(8) Uani 1 0 . C18 C 0.235(2) 0.2861(12) 0.2137(9) 0.125(14) Uani 1 0 . C19 C 0.2299(16) 0.4778(9) 0.3151(7) 0.065(9) Uani 1 0 . C20 C 0.3287(15) 0.5018(10) 0.3210(8) 0.085(10) Uani 1 0 . C21 C 0.1888(18) 0.5045(10) 0.3666(10) 0.108(12) Uani 1 0 . N22 N 0.3329(11) 0.3705(7) 0.4202(6) 0.062(7) Uani 1 0 . O23 O 0.3721(11) 0.4141(7) 0.4537(5) 0.088(7) Uani 1 0 . O24 O 0.4078(10) 0.2779(6) 0.3345(5) 0.078(6) Uani 1 0 . C25 C 0.4790(16) 0.3311(9) 0.3310(8) 0.078(10) Uani 1 0 . C26 C 0.5496(18) 0.2850(12) 0.3078(11) 0.112(13) Uani 1 0 . C27 C 0.5275(17) 0.2101(13) 0.3010(9) 0.099(11) Uani 1 0 . C28 C 0.4285(19) 0.2127(11) 0.3010(8) 0.092(11) Uani 1 0 . B29 B 0.7392(13) 0.2849(8) 0.1387(6) 0.032(7) Uani 1 0 . C30 C 0.7878(11) 0.3343(7) 0.0930(6) 0.032(6) Uani 1 0 . C31 C 0.7368(12) 0.3546(7) 0.0419(6) 0.040(7) Uani 1 0 . C32 C 0.7779(16) 0.3997(9) 0.0043(6) 0.057(8) Uani 1 0 . C33 C 0.8622(14) 0.4185(10) 0.0124(7) 0.060(8) Uani 1 0 . C34 C 0.9100(12) 0.3983(10) 0.0609(7) 0.053(7) Uani 1 0 . C35 C 0.8724(11) 0.3587(9) 0.0998(6) 0.044(7) Uani 1 0 . C36 C 0.7177(16) 0.4176(10) -0.0472(9) 0.067(10) Uani 1 0 . F37 F 0.7564(11) 0.4634(6) -0.0808(4) 0.111(7) Uani 1 0 . F38 F 0.6911(10) 0.3578(6) -0.0765(4) 0.108(6) Uani 1 0 . F39 F 0.6454(12) 0.4523(9) -0.0389(5) 0.146(9) Uani 1 0 . C40 C 1.0109(17) 0.4193(14) 0.0723(10) 0.083(11) Uani 1 0 . F41 F 1.0531(9) 0.3622(8) 0.0988(6) 0.120(7) Uani 1 0 . F42 F 1.0209(8) 0.4785(6) 0.0977(6) 0.129(7) Uani 1 0 . F43 F 1.0430(8) 0.4211(7) 0.0240(6) 0.100(6) Uani 1 0 . C44 C 0.6963(11) 0.3499(8) 0.1762(6) 0.033(6) Uani 1 0 . C45 C 0.6134(11) 0.3801(7) 0.1592(6) 0.031(6) Uani 1 0 . C46 C 0.5771(11) 0.4376(8) 0.1890(6) 0.036(6) Uani 1 0 . C47 C 0.6218(14) 0.4644(8) 0.2337(7) 0.054(5) Uiso 1 0 . C48 C 0.7045(13) 0.4374(9) 0.2514(7) 0.057(8) Uani 1 0 . C49 C 0.7422(14) 0.3796(8) 0.2222(7) 0.059(8) Uani 1 0 . C50 C 0.4901(15) 0.4633(10) 0.1729(9) 0.064(9) Uani 1 0 . F51 F 0.4492(8) 0.4977(8) 0.2077(5) 0.113(6) Uani 1 0 . F52 F 0.4371(9) 0.4200(8) 0.1430(7) 0.151(8) Uani 1 0 . F53 F 0.4938(10) 0.5213(10) 0.1343(7) 0.157(9) Uani 1 0 . C54 C 0.773(4) 0.4726(17) 0.2988(15) 0.29(3) Uani 1 0 . F55 F 0.8406(11) 0.4462(7) 0.3140(5) 0.101(7) Uani 1 0 . F56 F 0.7449(9) 0.5358(6) 0.3142(5) 0.106(6) Uani 1 0 . F57 F 0.7295(15) 0.4334(11) 0.3485(6) 0.188(11) Uani 1 0 . C58 C 0.8137(12) 0.2327(8) 0.1756(6) 0.040(7) Uani 1 0 . C59 C 0.7988(13) 0.2109(7) 0.2271(7) 0.054(7) Uani 1 0 . C60 C 0.9297(15) 0.1429(9) 0.2441(9) 0.065(9) Uani 1 0 . C61 C 0.8915(12) 0.2050(8) 0.1562(7) 0.051(7) Uani 1 0 . C62 C 0.843(2) 0.1463(17) 0.3171(11) 0.113(15) Uani 1 0 . F63 F 0.7576(16) 0.1154(9) 0.3145(5) 0.158(10) Uani 1 0 . F64 F 0.8399(16) 0.2059(8) 0.3475(5) 0.223(14) Uani 1 0 . F65 F 0.8902(16) 0.1015(10) 0.3441(8) 0.235(14) Uani 1 0 . C66 C 0.9469(15) 0.1602(11) 0.1923(12) 0.083(11) Uani 1 0 . F67 F 1.0190(10) 0.0649(7) 0.1447(6) 0.137(7) Uani 1 0 . F68 F 1.0952(11) 0.1187(9) 0.2161(8) 0.177(9) Uani 1 0 . F69 F 1.0672(10) 0.1784(8) 0.1413(8) 0.155(9) Uani 1 0 . C70 C 0.6673(10) 0.2241(7) 0.1098(6) 0.031(5) Uani 1 0 . C71 C 0.6832(10) 0.1844(7) 0.0639(6) 0.032(6) Uani 1 0 . C72 C 0.6227(11) 0.1310(7) 0.0376(5) 0.032(6) Uani 1 0 . C73 C 0.5496(12) 0.1129(7) 0.0630(7) 0.043(7) Uani 1 0 . C74 C 0.5355(11) 0.1509(8) 0.1089(6) 0.034(6) Uani 1 0 . C75 C 0.5912(10) 0.2041(8) 0.1318(5) 0.030(5) Uani 1 0 . C76 C 0.6429(14) 0.0957(9) -0.0139(7) 0.054(8) Uani 1 0 . F77 F 0.6627(8) 0.1452(5) -0.0514(4) 0.068(5) Uani 1 0 . F78 F 0.5757(8) 0.0521(5) -0.0374(4) 0.070(4) Uani 1 0 . F79 F 0.7150(9) 0.0489(5) -0.0058(4) 0.083(5) Uani 1 0 . C80 C 0.4577(14) 0.1301(9) 0.1375(9) 0.057(9) Uani 1 0 . F81 F 0.4132(8) 0.1884(7) 0.1511(5) 0.094(5) Uani 1 0 . F82 F 0.3959(8) 0.0897(7) 0.1054(4) 0.107(6) Uani 1 0 . F83 F 0.4765(9) 0.0933(7) 0.1832(5) 0.115(6) Uani 1 0 . O84 O 0.906(2) 0.1754(16) 0.0156(13) 0.115(11) Uiso 0.5 0 . C85 C 0.919(3) 0.2172(18) -0.0259(16) 0.068(12) Uiso 0.5 0 . C86 C 0.964(3) 0.175(2) -0.0603(17) 0.089(14) Uiso 0.5 0 . C87 C 0.975(3) 0.107(2) -0.0411(18) 0.088(13) Uiso 0.5 0 . C88 C 0.944(4) 0.108(3) 0.003(2) 0.120(18) Uiso 0.5 0 . C89 C 0.8554(17) 0.1659(10) 0.2611(9) 0.073(6) Uiso 1 0 . C90 C 1.025(3) 0.1325(17) 0.1742(13) 0.122(10) Uiso 1 0 . OS91A OS 0.2638(10) 0.2997(3) 0.3808(3) 0.109(2) Uani 0.539(19) 0 . C92A C 0.298(3) 0.2336(19) 0.5136(15) 0.060(10) Uiso 0.55 0 . H1 H 0.4341 0.1578 0.411 0.0063 Uiso 1 0 . H2 H 0.5439 0.2118 0.4708 0.0063 Uiso 1 0 . H3 H 0.4745 0.2726 0.4497 0.0063 Uiso 1 0 . H4 H 0.4746 0.2384 0.5078 0.0063 Uiso 1 0 . H5 H 0.3853 0.0499 0.461 0.0063 Uiso 1 0 . H6 H 0.4859 0.0632 0.4787 0.0063 Uiso 1 0 . H7 H 0.4172 0.0898 0.5161 0.0063 Uiso 1 0 . H8 H 0.256 0.0795 0.4503 0.0063 Uiso 1 0 . H9 H 0.127 0.1601 0.3823 0.0063 Uiso 1 0 . H10 H 0.1106 0.0843 0.4106 0.0063 Uiso 1 0 . H11 H 0.1293 0.1566 0.4455 0.0063 Uiso 1 0 . H12 H 0.2458 0.1037 0.3407 0.0063 Uiso 1 0 . H13 H 0.3235 0.0619 0.3753 0.0063 Uiso 1 0 . H14 H 0.2286 0.028 0.3689 0.0063 Uiso 1 0 . H15 H 0.1603 0.2003 0.4819 0.0063 Uiso 1 0 . H16 H 0.2804 0.3018 0.5312 0.0063 Uiso 1 0 . H17 H 0.2008 0.322 0.4875 0.0063 Uiso 1 0 . H18 H 0.1839 0.293 0.5448 0.0063 Uiso 1 0 . H19 H 0.2525 0.1063 0.534 0.0063 Uiso 1 0 . H20 H 0.3133 0.1694 0.5615 0.0063 Uiso 1 0 . H21 H 0.2168 0.1611 0.5751 0.0063 Uiso 1 0 . H22 H 0.0844 0.3966 0.329 0.0063 Uiso 1 0 . H23 H -0.0026 0.3201 0.3178 0.0063 Uiso 1 0 . H24 H 0.0407 0.2811 0.2715 0.0063 Uiso 1 0 . H25 H 0.0873 0.2785 0.3314 0.0063 Uiso 1 0 . H26 H 0.0738 0.4702 0.2471 0.0063 Uiso 1 0 . H27 H 0.028 0.4011 0.2171 0.0063 Uiso 1 0 . H28 H -0.0151 0.4403 0.2634 0.0063 Uiso 1 0 . H29 H 0.328 0.3629 0.249 0.0063 Uiso 1 0 . H30 H 0.2688 0.4124 0.1616 0.0063 Uiso 1 0 . H31 H 0.176 0.421 0.181 0.0063 Uiso 1 0 . H32 H 0.254 0.4719 0.2057 0.0063 Uiso 1 0 . H33 H 0.1764 0.2831 0.2042 0.0063 Uiso 1 0 . H34 H 0.2692 0.2749 0.1847 0.0063 Uiso 1 0 . H35 H 0.2539 0.2466 0.2425 0.0063 Uiso 1 0 . H36 H 0.2021 0.5052 0.2849 0.0063 Uiso 1 0 . H37 H 0.3563 0.4872 0.2888 0.0063 Uiso 1 0 . H38 H 0.3375 0.555 0.3252 0.0063 Uiso 1 0 . H39 H 0.3638 0.4779 0.3519 0.0063 Uiso 1 0 . H40 H 0.1899 0.5564 0.3733 0.0063 Uiso 1 0 . H41 H 0.1255 0.4886 0.3637 0.0063 Uiso 1 0 . H42 H 0.216 0.4795 0.4004 0.0063 Uiso 1 0 . H43 H 0.4606 0.3747 0.3078 0.0063 Uiso 1 0 . H44 H 0.5023 0.3527 0.3665 0.0063 Uiso 1 0 . H45 H 0.5584 0.308 0.2728 0.0063 Uiso 1 0 . H46 H 0.6039 0.2904 0.3316 0.0063 Uiso 1 0 . H47 H 0.5422 0.1918 0.2648 0.0063 Uiso 1 0 . H48 H 0.5583 0.1791 0.3277 0.0063 Uiso 1 0 . H49 H 0.4085 0.1662 0.3182 0.0063 Uiso 1 0 . H50 H 0.3956 0.2144 0.2652 0.0063 Uiso 1 0 . H51 H 0.6753 0.3377 0.0335 0.0063 Uiso 1 0 . H52 H 0.8939 0.4454 -0.0152 0.0063 Uiso 1 0 . H53 H 0.9078 0.3489 0.1361 0.0063 Uiso 1 0 . H54 H 0.5787 0.3597 0.1262 0.0063 Uiso 1 0 . H55 H 0.5924 0.5035 0.2525 0.0063 Uiso 1 0 . H56 H 0.8017 0.3615 0.2362 0.0063 Uiso 1 0 . H57 H 0.7417 0.2296 0.2405 0.0063 Uiso 1 0 . H58 H 0.9735 0.1143 0.2662 0.0063 Uiso 1 0 . H59 H 0.9034 0.2213 0.117 0.0063 Uiso 1 0 . H60 H 0.739 0.1944 0.0483 0.0063 Uiso 1 0 . H61 H 0.5091 0.0727 0.0475 0.0063 Uiso 1 0 . H62 H 0.5779 0.2309 0.1651 0.0063 Uiso 1 0 . H63 H 0.962 0.257 -0.0121 0.0063 Uiso 1 0 . H64 H 0.8698 0.24 -0.0448 0.0063 Uiso 1 0 . H65 H 1.0186 0.1986 -0.0689 0.0063 Uiso 1 0 . H66 H 0.9261 0.1748 -0.0981 0.0063 Uiso 1 0 . H67 H 1.039 0.0881 -0.0361 0.0063 Uiso 1 0 . H68 H 0.9469 0.064 -0.0657 0.0063 Uiso 1 0 . H69 H 0.9041 0.0599 0.0037 0.0063 Uiso 1 0 . H70 H 0.994 0.09 0.0327 0.0063 Uiso 1 0 . _cod_database_code 5000359