#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000360.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_5000360 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C26 H58 N2 O1 Os1 P2' _chemical_formula_moiety ? _chemical_formula_weight 666.937 _cell_length_a 8.8330(2) _cell_length_b 11.5202(3) _cell_length_c 16.0550(4) _cell_angle_alpha 103.6978 _cell_angle_beta 99.4508(12) _cell_angle_gamma 98.8901(12) _cell_volume 1533.49(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 113. _exptl_crystal_colour 'pale yellow' _exptl_crystal_description irregular _exptl_crystal_size_max .30 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .25 _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 4.2786 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_ambient_temperature 113. _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42598 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_min 2.38659 _diffrn_reflns_theta_max 32.5295 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _reflns_number_total 11137 _reflns_number_gt 9900 _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' 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' 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 98990 _refine_ls_number_parameters 522 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef 0.000000154(14) _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 0.0159 _refine_ls_wR_factor_ref 0.0134 _refine_ls_goodness_of_fit_ref 0.5487 _refine_ls_shift/su_max 0.0048 _refine_diff_density_max 2.43 _refine_diff_density_min -0.75 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 -0.346138(8) 0.024382(6) -0.218543(4) 0.01163(2) Uani 1 0 . N2 N -0.15541(19) -0.00834(15) -0.20111(10) 0.0167(5) Uani 1 0 . O3 O -0.02978(17) -0.03481(15) -0.18847(10) 0.0252(6) Uani 1 0 . C4 C -0.3409(2) 0.13632(18) -0.31503(13) 0.0169(6) Uani 1 0 . C5 C -0.1865(2) 0.20891(18) -0.31730(12) 0.0173(6) Uani 1 0 . C6 C -0.0646(3) 0.1368(2) -0.34525(16) 0.0241(7) Uani 1 0 . C7 C 0.0595(3) 0.2105(2) -0.37710(19) 0.0352(10) Uani 1 0 . C8 C 0.1129(3) 0.3353(2) -0.3141(2) 0.0381(10) Uani 1 0 . C9 C -0.0213(2) 0.4018(2) -0.30639(15) 0.0267(7) Uani 1 0 . N10 N -0.16740(19) 0.32527(16) -0.29913(11) 0.0209(6) Uani 1 0 . C11 C -0.0658(3) 0.4518(3) -0.38517(18) 0.0388(10) Uani 1 0 . C12 C 0.0250(4) 0.5104(2) -0.2240(2) 0.0423(10) Uani 1 0 . P13 P -0.32239(6) 0.19770(4) -0.09974(3) 0.01401(15) Uani 1 0 . C14 C -0.1240(2) 0.24308(19) -0.02811(13) 0.0193(6) Uani 1 0 . C15 C -0.0849(3) 0.1476(2) 0.01936(16) 0.0277(8) Uani 1 0 . C16 C -0.0004(3) 0.2722(2) -0.08070(16) 0.0253(7) Uani 1 0 . C17 C -0.3512(2) 0.33954(18) -0.13010(13) 0.0173(6) Uani 1 0 . C18 C -0.2788(3) 0.4605(2) -0.06125(16) 0.0257(8) Uani 1 0 . C19 C -0.5229(3) 0.3362(2) -0.16813(16) 0.0243(8) Uani 1 0 . C20 C -0.4499(3) 0.1691(2) -0.02225(13) 0.0210(7) Uani 1 0 . C21 C -0.6229(3) 0.1196(2) -0.06326(17) 0.0289(9) Uani 1 0 . C22 C -0.4323(4) 0.2764(3) 0.05821(17) 0.0351(10) Uani 1 0 . P23 P -0.47070(6) -0.15650(4) -0.32961(3) 0.01393(15) Uani 1 0 . C24 C -0.3873(2) -0.18078(19) -0.43023(13) 0.0191(6) Uani 1 0 . C25 C -0.2241(3) -0.2093(2) -0.41188(16) 0.0263(8) Uani 1 0 . C26 C -0.4865(3) -0.2706(2) -0.51455(15) 0.0273(8) Uani 1 0 . C27 C -0.4718(3) -0.29465(18) -0.28861(13) 0.0202(7) Uani 1 0 . C28 C -0.5364(3) -0.4168(2) -0.35730(17) 0.0332(9) Uani 1 0 . C29 C -0.3153(3) -0.2974(2) -0.23289(16) 0.0259(8) Uani 1 0 . C30 C -0.6817(2) -0.1677(2) -0.37255(14) 0.0227(7) Uani 1 0 . C31 C -0.7071(3) -0.0638(2) -0.41419(17) 0.0303(9) Uani 1 0 . C32 C -0.7808(3) -0.1717(3) -0.30355(19) 0.0338(9) Uani 1 0 . H1 H -0.521(3) 0.047(2) -0.2286(14) 0.024(6) Uiso 1 0 . H2 H -0.434(3) -0.048(2) -0.1555(16) 0.045(8) Uiso 1 0 . H3 H -0.383(2) 0.0797(19) -0.3751(14) 0.018(6) Uiso 1 0 . H4 H -0.417(2) 0.192(2) -0.3085(14) 0.018(6) Uiso 1 0 . H5 H -0.012(3) 0.111(2) -0.2970(17) 0.040(8) Uiso 1 0 . H6 H -0.118(3) 0.063(2) -0.3890(16) 0.032(7) Uiso 1 0 . H7 H 0.145(3) 0.171(2) -0.3817(16) 0.036(7) Uiso 1 0 . H8 H 0.017(3) 0.220(2) -0.4362(17) 0.043(8) Uiso 1 0 . H9 H 0.153(3) 0.330(2) -0.2567(18) 0.044(8) Uiso 1 0 . H10 H 0.196(3) 0.382(3) -0.3343(18) 0.054(9) Uiso 1 0 . H11 H 0.022(3) 0.511(3) -0.3919(17) 0.047(8) Uiso 1 0 . H12 H -0.091(3) 0.384(2) -0.4410(16) 0.031(7) Uiso 1 0 . H13 H -0.157(3) 0.493(3) -0.3820(18) 0.050(9) Uiso 1 0 . H14 H 0.054(3) 0.486(3) -0.1724(18) 0.048(9) Uiso 1 0 . H15 H 0.117(3) 0.561(3) -0.2306(18) 0.051(9) Uiso 1 0 . H16 H -0.063(3) 0.553(3) -0.2159(18) 0.050(9) Uiso 1 0 . H17 H -0.125(3) 0.315(2) 0.0131(14) 0.019(6) Uiso 1 0 . H18 H -0.151(3) 0.139(2) 0.0619(16) 0.029(7) Uiso 1 0 . H19 H -0.100(3) 0.066(2) -0.0203(16) 0.038(8) Uiso 1 0 . H20 H 0.021(3) 0.173(2) 0.0515(16) 0.038(7) Uiso 1 0 . H21 H 0.010(3) 0.201(2) -0.1210(15) 0.026(7) Uiso 1 0 . H22 H -0.026(3) 0.331(2) -0.1123(17) 0.041(8) Uiso 1 0 . H23 H 0.100(3) 0.307(2) -0.0413(16) 0.037(7) Uiso 1 0 . H24 H -0.298(2) 0.3369(19) -0.1770(14) 0.017(6) Uiso 1 0 . H25 H -0.160(3) 0.470(2) -0.0408(16) 0.036(7) Uiso 1 0 . H26 H -0.295(3) 0.525(2) -0.0854(16) 0.033(7) Uiso 1 0 . H27 H -0.328(3) 0.471(2) -0.0101(17) 0.036(7) Uiso 1 0 . H28 H -0.579(3) 0.355(2) -0.1229(15) 0.026(6) Uiso 1 0 . H29 H -0.528(3) 0.397(2) -0.1987(16) 0.033(7) Uiso 1 0 . H30 H -0.581(2) 0.256(2) -0.2091(14) 0.019(6) Uiso 1 0 . H31 H -0.411(2) 0.1070(19) -0.0041(13) 0.015(6) Uiso 1 0 . H32 H -0.671(3) 0.177(2) -0.0856(15) 0.030(7) Uiso 1 0 . H33 H -0.639(3) 0.051(2) -0.1110(17) 0.037(8) Uiso 1 0 . H34 H -0.673(3) 0.102(2) -0.0186(17) 0.040(8) Uiso 1 0 . H35 H -0.330(4) 0.307(3) 0.0872(19) 0.052(9) Uiso 1 0 . H36 H -0.481(3) 0.342(3) 0.0428(17) 0.045(8) Uiso 1 0 . H37 H -0.491(4) 0.243(3) 0.096(2) 0.061(10) Uiso 1 0 . H38 H -0.376(3) -0.106(2) -0.4416(14) 0.022(6) Uiso 1 0 . H39 H -0.226(3) -0.291(2) -0.4072(15) 0.030(7) Uiso 1 0 . H40 H -0.166(3) -0.195(2) -0.4563(17) 0.035(7) Uiso 1 0 . H41 H -0.159(3) -0.158(2) -0.3595(17) 0.037(8) Uiso 1 0 . H42 H -0.586(3) -0.255(2) -0.5332(16) 0.034(7) Uiso 1 0 . H43 H -0.429(3) -0.270(2) -0.5631(17) 0.043(8) Uiso 1 0 . H44 H -0.504(3) -0.351(2) -0.5091(15) 0.032(7) Uiso 1 0 . H45 H -0.542(3) -0.280(2) -0.2508(14) 0.020(6) Uiso 1 0 . H46 H -0.639(3) -0.419(2) -0.3958(17) 0.038(8) Uiso 1 0 . H47 H -0.469(3) -0.439(2) -0.3946(18) 0.043(8) Uiso 1 0 . H48 H -0.555(3) -0.482(2) -0.3270(17) 0.041(8) Uiso 1 0 . H49 H -0.325(3) -0.365(2) -0.2068(17) 0.041(8) Uiso 1 0 . H50 H -0.236(3) -0.302(2) -0.2660(16) 0.033(7) Uiso 1 0 . H51 H -0.278(3) -0.225(2) -0.1807(16) 0.030(7) Uiso 1 0 . H52 H -0.716(3) -0.244(2) -0.4167(14) 0.022(6) Uiso 1 0 . H53 H -0.673(3) 0.017(2) -0.3688(16) 0.034(7) Uiso 1 0 . H54 H -0.650(3) -0.061(2) -0.4631(17) 0.042(8) Uiso 1 0 . H55 H -0.818(3) -0.071(2) -0.4369(17) 0.043(8) Uiso 1 0 . H56 H -0.749(3) -0.091(2) -0.2539(16) 0.036(7) Uiso 1 0 . H57 H -0.883(3) -0.178(2) -0.3287(17) 0.045(8) Uiso 1 0 . H58 H -0.776(4) -0.236(3) -0.278(2) 0.064(10) Uiso 1 0 .