#------------------------------------------------------------------------------ #$Date: 2008-03-16 12:50:27 +0000 (Sun, 16 Mar 2008) $ #$Revision: 279 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000328.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_5000328 ## 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C19 H44 O2 Os1 P2' _chemical_formula_moiety ? _chemical_formula_weight 556.735 _cell_length_a 7.811(2) _cell_length_b 14.936(4) _cell_length_c 20.130(5) _cell_angle_alpha 90 _cell_angle_beta 95.755(15) _cell_angle_gamma 90 _cell_volume 2336.7(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 94 _cell_measurement_theta_min 11.52 _cell_measurement_theta_max 12.39 _cell_measurement_temperature 102 _exptl_crystal_colour orange/red _exptl_crystal_description irregular _exptl_crystal_size_max .30 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .18 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 5.6025 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.277 _exptl_absorpt_correction_T_max 0.391 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 102 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10155 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_min 3.03794 _diffrn_reflns_theta_max 27.5213 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 4 _diffrn_standards_decay_% -0.2 _diffrn_standards_interval_count 1000 _reflns_number_total 5358 _reflns_number_gt 4193 _reflns_threshold_expression F^2^>2.33\s(F^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' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 '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 4458 _refine_ls_number_parameters 218 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef 0.00000029(3) _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)+(.03F)^2^ _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0355 _refine_ls_goodness_of_fit_ref 1.3745 _refine_ls_shift/su_max 0.0089 _refine_diff_density_max 3.08 _refine_diff_density_min -1.83 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 0.42801(3) 0.358012(15) 0.118380(11) 0.01367(7) Uani 1 0 . P2 P 0.5338(2) 0.27168(10) 0.03296(7) 0.0144(4) Uani 1 0 . C3 C 0.6873(9) 0.3343(4) -0.0120(3) 0.024(2) Uani 1 0 . C4 C 0.3618(8) 0.2439(4) -0.0357(3) 0.0209(19) Uani 1 0 . C5 C 0.2452(9) 0.1687(5) -0.0141(3) 0.029(2) Uani 1 0 . C6 C 0.4241(10) 0.2211(5) -0.1029(3) 0.031(2) Uani 1 0 . C7 C 0.2512(10) 0.3286(5) -0.0459(4) 0.036(2) Uani 1 0 . C8 C 0.6612(8) 0.1700(4) 0.0603(3) 0.0205(18) Uani 1 0 . C9 C 0.7072(10) 0.1101(5) 0.0020(4) 0.033(2) Uani 1 0 . C10 C 0.5664(9) 0.1122(5) 0.1073(4) 0.030(2) Uani 1 0 . C11 C 0.8280(9) 0.2015(5) 0.0982(4) 0.032(2) Uani 1 0 . P12 P 0.3278(2) 0.45511(10) 0.19897(8) 0.0162(4) Uani 1 0 . C13 C 0.4130(9) 0.5680(4) 0.1933(3) 0.026(2) Uani 1 0 . C14 C 0.0896(8) 0.4750(5) 0.1833(3) 0.024(2) Uani 1 0 . C15 C -0.0115(9) 0.3986(5) 0.2108(4) 0.033(2) Uani 1 0 . C16 C 0.0502(9) 0.4771(5) 0.1069(4) 0.034(2) Uani 1 0 . C17 C 0.0291(9) 0.5634(5) 0.2114(4) 0.034(2) Uani 1 0 . C18 C 0.3908(8) 0.4252(4) 0.2882(3) 0.0195(18) Uani 1 0 . C19 C 0.5859(9) 0.4422(5) 0.3007(3) 0.030(2) Uani 1 0 . C20 C 0.3607(9) 0.3258(5) 0.3015(3) 0.026(2) Uani 1 0 . C21 C 0.3024(9) 0.4805(5) 0.3383(3) 0.027(2) Uani 1 0 . C22 C 0.3025(7) 0.2658(4) 0.1454(3) 0.0170(18) Uani 1 0 . O23 O 0.2168(6) 0.2077(3) 0.1631(2) 0.0256(15) Uani 1 0 . O24 O 0.5035(7) 0.4718(3) 0.0753(2) 0.0323(16) Uani 1 0 . H1 H 0.782 0.352 0.018 0.0365 Uiso 1 0 . H2 H 0.7261 0.2973 -0.046 0.0365 Uiso 1 0 . H3 H 0.632 0.3858 -0.0321 0.0365 Uiso 1 0 . H4 H 0.2074 0.1836 0.0279 0.0413 Uiso 1 0 . H5 H 0.1483 0.1628 -0.0464 0.0413 Uiso 1 0 . H6 H 0.3077 0.1145 -0.0107 0.0413 Uiso 1 0 . H7 H 0.4911 0.168 -0.0985 0.043 Uiso 1 0 . H8 H 0.3278 0.2121 -0.1348 0.043 Uiso 1 0 . H9 H 0.492 0.2689 -0.1167 0.043 Uiso 1 0 . H10 H 0.3197 0.3763 -0.0594 0.0478 Uiso 1 0 . H11 H 0.1584 0.3178 -0.079 0.0478 Uiso 1 0 . H12 H 0.2071 0.3437 -0.0049 0.0478 Uiso 1 0 . H13 H 0.6046 0.087 -0.0208 0.0455 Uiso 1 0 . H14 H 0.7668 0.1449 -0.0277 0.0455 Uiso 1 0 . H15 H 0.7783 0.0623 0.0192 0.0455 Uiso 1 0 . H16 H 0.5404 0.1467 0.1444 0.0428 Uiso 1 0 . H17 H 0.4622 0.0907 0.0838 0.0428 Uiso 1 0 . H18 H 0.6364 0.0627 0.122 0.0428 Uiso 1 0 . H19 H 0.8935 0.1512 0.1142 0.0446 Uiso 1 0 . H20 H 0.8912 0.2354 0.069 0.0446 Uiso 1 0 . H21 H 0.8027 0.2378 0.1346 0.0446 Uiso 1 0 . H22 H 0.535 0.566 0.2002 0.0387 Uiso 1 0 . H23 H 0.3786 0.5916 0.1502 0.0387 Uiso 1 0 . H24 H 0.3697 0.6045 0.2262 0.0387 Uiso 1 0 . H25 H -0.1313 0.4072 0.199 0.0453 Uiso 1 0 . H26 H 0.0225 0.3431 0.1928 0.0453 Uiso 1 0 . H27 H 0.0105 0.3967 0.2582 0.0453 Uiso 1 0 . H28 H -0.0686 0.4865 0.0946 0.0462 Uiso 1 0 . H29 H 0.1134 0.5253 0.0886 0.0462 Uiso 1 0 . H30 H 0.085 0.4225 0.0878 0.0462 Uiso 1 0 . H31 H 0.0487 0.5623 0.2589 0.0476 Uiso 1 0 . H32 H 0.0905 0.6117 0.1948 0.0476 Uiso 1 0 . H33 H -0.0908 0.5709 0.1987 0.0476 Uiso 1 0 . H34 H 0.6253 0.4266 0.3454 0.0427 Uiso 1 0 . H35 H 0.644 0.4064 0.2709 0.0427 Uiso 1 0 . H36 H 0.6086 0.5034 0.2933 0.0427 Uiso 1 0 . H37 H 0.2405 0.3139 0.297 0.0392 Uiso 1 0 . H38 H 0.415 0.2905 0.2706 0.0392 Uiso 1 0 . H39 H 0.4073 0.3112 0.3458 0.0392 Uiso 1 0 . H40 H 0.3448 0.4625 0.3827 0.039 Uiso 1 0 . H41 H 0.3284 0.5419 0.3329 0.039 Uiso 1 0 . H42 H 0.1827 0.4712 0.3319 0.039 Uiso 1 0 . H43 H 0.49 0.48 0.02 0.038 Uiso 1 0 . H44 H 0.5908 0.4061 0.181 0.038 Uiso 1 0 .