#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4060268.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_4060268 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C41 H30 O5 P2 W' _chemical_formula_weight 848.44 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8844(1) _cell_length_b 17.7818(2) _cell_length_c 17.5881(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.9127(3) _cell_angle_gamma 90.00 _cell_volume 3402.18(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 3.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.578 _exptl_absorpt_correction_T_max 0.710 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24819 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7816 _reflns_number_gt 5874 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7816 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.167784(16) 0.196252(10) 0.479542(10) 0.02029(9) Uani 1 1 d . . . P1 P 0.22127(11) 0.31772(7) 0.40946(7) 0.0201(3) Uani 1 1 d . . . P2 P 0.17159(11) 0.10983(7) 0.36232(7) 0.0210(3) Uani 1 1 d . . . O1 O 0.2162(3) 0.2734(2) 0.6371(2) 0.0393(9) Uani 1 1 d . . . O2 O -0.1024(3) 0.2605(2) 0.4743(2) 0.0376(9) Uani 1 1 d . . . O3 O 0.0424(4) 0.0670(2) 0.5701(3) 0.0539(12) Uani 1 1 d . . . O4 O 0.3573(3) 0.16765(19) 0.46274(19) 0.0248(7) Uani 1 1 d . . . O5 O 0.5719(4) 0.2841(2) 0.5336(3) 0.0488(11) Uani 1 1 d . . . C1 C 0.1985(4) 0.2463(3) 0.5780(3) 0.0258(11) Uani 1 1 d . . . C2 C -0.0035(5) 0.2373(3) 0.4757(3) 0.0260(11) Uani 1 1 d . . . C3 C 0.0886(5) 0.1132(3) 0.5362(3) 0.0335(12) Uani 1 1 d . . . C4 C 0.3224(4) 0.1123(3) 0.5071(3) 0.0270(11) Uani 1 1 d . . . H4A H 0.3566 0.1141 0.5605 0.032 Uiso 1 1 calc R . . C5 C 0.3066(4) 0.0354(3) 0.4743(3) 0.0258(11) Uani 1 1 d . . . C6 C 0.3545(4) -0.0270(3) 0.5129(3) 0.0321(12) Uani 1 1 d . . . H6A H 0.3943 -0.0209 0.5614 0.039 Uiso 1 1 calc R . . C7 C 0.3441(5) -0.0981(3) 0.4808(4) 0.0411(14) Uani 1 1 d . . . H7A H 0.3773 -0.1405 0.5072 0.049 Uiso 1 1 calc R . . C8 C 0.2858(5) -0.1073(3) 0.4106(3) 0.0394(14) Uani 1 1 d . . . H8A H 0.2796 -0.1561 0.3887 0.047 Uiso 1 1 calc R . . C9 C 0.2364(5) -0.0460(3) 0.3719(3) 0.0332(12) Uani 1 1 d . . . H9A H 0.1961 -0.0529 0.3236 0.040 Uiso 1 1 calc R . . C10 C 0.2452(4) 0.0257(3) 0.4031(3) 0.0238(10) Uani 1 1 d . . . C11 C 0.0295(4) 0.0774(3) 0.3143(3) 0.0244(10) Uani 1 1 d . . . C12 C 0.0289(5) 0.0372(3) 0.2459(3) 0.0302(12) Uani 1 1 d . . . H12A H 0.1046 0.0238 0.2242 0.036 Uiso 1 1 calc R . . C13 C -0.0804(5) 0.0169(3) 0.2097(3) 0.0370(13) Uani 1 1 d . . . H13A H -0.0795 -0.0102 0.1632 0.044 Uiso 1 1 calc R . . C14 C -0.1920(5) 0.0357(3) 0.2409(3) 0.0406(14) Uani 1 1 d . . . H14A H -0.2673 0.0224 0.2155 0.049 Uiso 1 1 calc R . . C15 C -0.1921(5) 0.0738(3) 0.3088(3) 0.0369(13) Uani 1 1 d . . . H15A H -0.2681 0.0863 0.3306 0.044 Uiso 1 1 calc R . . C16 C -0.0824(4) 0.0945(3) 0.3460(3) 0.0290(11) Uani 1 1 d . . . H16A H -0.0840 0.1203 0.3932 0.035 Uiso 1 1 calc R . . C17 C 0.2691(4) 0.1339(3) 0.2821(3) 0.0221(10) Uani 1 1 d . . . C18 C 0.2208(4) 0.1613(3) 0.2134(3) 0.0262(11) Uani 1 1 d . . . H18A H 0.1347 0.1688 0.2071 0.031 Uiso 1 1 calc R . . C19 C 0.2971(5) 0.1778(3) 0.1536(3) 0.0297(12) Uani 1 1 d . . . H19A H 0.2630 0.1957 0.1066 0.036 Uiso 1 1 calc R . . C20 C 0.4223(5) 0.1681(3) 0.1630(3) 0.0320(12) Uani 1 1 d . . . H20A H 0.4744 0.1791 0.1222 0.038 Uiso 1 1 calc R . . C21 C 0.4722(4) 0.1425(3) 0.2313(3) 0.0290(11) Uani 1 1 d . . . H21A H 0.5588 0.1369 0.2376 0.035 Uiso 1 1 calc R . . C22 C 0.3968(4) 0.1249(3) 0.2909(3) 0.0254(11) Uani 1 1 d . . . H22A H 0.4317 0.1067 0.3377 0.031 Uiso 1 1 calc R . . C23 C 0.4800(5) 0.2955(3) 0.4940(3) 0.0320(12) Uani 1 1 d . . . H23A H 0.4034 0.2992 0.5181 0.038 Uiso 1 1 calc R . . C24 C 0.4806(5) 0.3039(3) 0.4106(3) 0.0285(11) Uani 1 1 d . . . C25 C 0.5934(5) 0.3013(3) 0.3747(4) 0.0368(14) Uani 1 1 d . . . H25A H 0.6664 0.2917 0.4042 0.044 Uiso 1 1 calc R . . C26 C 0.6005(5) 0.3124(3) 0.2977(4) 0.0437(16) Uani 1 1 d . . . H26A H 0.6780 0.3114 0.2745 0.052 Uiso 1 1 calc R . . C27 C 0.4946(5) 0.3251(3) 0.2542(4) 0.0388(14) Uani 1 1 d . . . H27A H 0.4995 0.3330 0.2009 0.047 Uiso 1 1 calc R . . C28 C 0.3807(5) 0.3265(3) 0.2880(3) 0.0276(11) Uani 1 1 d . . . H28A H 0.3082 0.3341 0.2575 0.033 Uiso 1 1 calc R . . C29 C 0.3723(4) 0.3168(2) 0.3658(3) 0.0239(11) Uani 1 1 d . . . C30 C 0.1111(4) 0.3445(3) 0.3328(3) 0.0209(10) Uani 1 1 d . . . C31 C 0.0332(4) 0.2896(3) 0.3019(3) 0.0252(11) Uani 1 1 d . . . H31A H 0.0420 0.2390 0.3184 0.030 Uiso 1 1 calc R . . C32 C -0.0573(5) 0.3075(3) 0.2472(3) 0.0312(12) Uani 1 1 d . . . H32A H -0.1086 0.2692 0.2258 0.037 Uiso 1 1 calc R . . C33 C -0.0720(5) 0.3812(3) 0.2242(3) 0.0329(12) Uani 1 1 d . . . H33A H -0.1358 0.3943 0.1885 0.039 Uiso 1 1 calc R . . C34 C 0.0055(5) 0.4355(3) 0.2530(3) 0.0347(13) Uani 1 1 d . . . H34A H -0.0029 0.4857 0.2352 0.042 Uiso 1 1 calc R . . C35 C 0.0966(4) 0.4186(3) 0.3080(3) 0.0272(11) Uani 1 1 d . . . H35A H 0.1483 0.4572 0.3283 0.033 Uiso 1 1 calc R . . C36 C 0.2246(5) 0.4053(3) 0.4658(3) 0.0264(11) Uani 1 1 d . . . C37 C 0.1338(5) 0.4177(3) 0.5149(3) 0.0343(13) Uani 1 1 d . . . H37A H 0.0734 0.3800 0.5217 0.041 Uiso 1 1 calc R . . C38 C 0.1267(5) 0.4850(3) 0.5560(3) 0.0395(14) Uani 1 1 d . . . H38A H 0.0634 0.4925 0.5911 0.047 Uiso 1 1 calc R . . C39 C 0.2127(6) 0.5399(3) 0.5448(4) 0.0473(16) Uani 1 1 d . . . H39A H 0.2080 0.5862 0.5716 0.057 Uiso 1 1 calc R . . C40 C 0.3058(6) 0.5286(3) 0.4949(4) 0.0459(16) Uani 1 1 d . . . H40A H 0.3651 0.5669 0.4878 0.055 Uiso 1 1 calc R . . C41 C 0.3136(5) 0.4611(3) 0.4545(3) 0.0357(13) Uani 1 1 d . . . H41A H 0.3778 0.4531 0.4202 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.02093(13) 0.01987(13) 0.02017(12) 0.00098(8) 0.00233(7) 0.00048(8) P1 0.0192(6) 0.0196(6) 0.0215(6) -0.0001(5) 0.0009(5) -0.0001(5) P2 0.0213(6) 0.0186(6) 0.0230(6) -0.0005(5) 0.0020(5) 0.0000(5) O1 0.038(2) 0.051(2) 0.028(2) -0.0080(19) -0.0021(17) 0.0087(19) O2 0.025(2) 0.045(2) 0.043(2) -0.0050(19) 0.0023(17) 0.0058(17) O3 0.055(3) 0.040(2) 0.068(3) 0.025(2) 0.029(2) 0.001(2) O4 0.0228(17) 0.0257(17) 0.0261(19) 0.0018(15) 0.0024(14) 0.0021(14) O5 0.036(2) 0.051(3) 0.057(3) 0.003(2) -0.021(2) -0.0024(19) C1 0.023(3) 0.029(3) 0.025(3) 0.001(2) 0.001(2) 0.004(2) C2 0.031(3) 0.025(3) 0.022(3) -0.001(2) 0.005(2) -0.002(2) C3 0.031(3) 0.035(3) 0.035(3) 0.003(2) 0.010(2) 0.005(2) C4 0.024(3) 0.032(3) 0.025(3) 0.000(2) -0.003(2) 0.006(2) C5 0.022(2) 0.023(2) 0.033(3) 0.001(2) 0.007(2) -0.001(2) C6 0.030(3) 0.035(3) 0.032(3) 0.012(2) 0.003(2) 0.004(2) C7 0.041(3) 0.029(3) 0.055(4) 0.014(3) 0.008(3) 0.007(3) C8 0.048(3) 0.021(3) 0.050(4) 0.000(3) 0.007(3) 0.005(2) C9 0.035(3) 0.025(3) 0.040(3) -0.004(2) 0.003(2) -0.001(2) C10 0.023(2) 0.021(2) 0.029(3) 0.004(2) 0.008(2) 0.000(2) C11 0.025(2) 0.020(2) 0.029(3) 0.002(2) 0.001(2) -0.003(2) C12 0.028(3) 0.027(3) 0.036(3) -0.006(2) 0.002(2) -0.003(2) C13 0.039(3) 0.036(3) 0.036(3) -0.007(3) -0.004(2) -0.011(3) C14 0.032(3) 0.048(3) 0.041(4) 0.001(3) -0.007(3) -0.016(3) C15 0.024(3) 0.051(4) 0.036(3) 0.004(3) 0.004(2) -0.010(3) C16 0.026(3) 0.032(3) 0.029(3) 0.001(2) 0.001(2) -0.004(2) C17 0.023(2) 0.021(2) 0.023(3) -0.003(2) 0.0029(19) -0.0001(19) C18 0.021(2) 0.028(3) 0.030(3) 0.000(2) 0.002(2) 0.002(2) C19 0.029(3) 0.034(3) 0.026(3) 0.003(2) -0.001(2) 0.001(2) C20 0.034(3) 0.037(3) 0.026(3) -0.002(2) 0.010(2) 0.000(2) C21 0.024(3) 0.030(3) 0.033(3) 0.003(2) 0.003(2) 0.001(2) C22 0.026(3) 0.025(3) 0.026(3) 0.001(2) -0.002(2) 0.002(2) C23 0.024(3) 0.024(3) 0.047(3) 0.001(2) -0.009(2) -0.004(2) C24 0.024(3) 0.020(2) 0.041(3) 0.000(2) 0.001(2) -0.001(2) C25 0.020(3) 0.029(3) 0.061(4) -0.002(3) 0.003(3) -0.003(2) C26 0.031(3) 0.032(3) 0.070(5) -0.003(3) 0.025(3) -0.005(2) C27 0.042(3) 0.032(3) 0.043(4) 0.001(3) 0.015(3) -0.003(3) C28 0.028(3) 0.021(2) 0.034(3) 0.003(2) 0.005(2) 0.001(2) C29 0.021(2) 0.018(2) 0.033(3) -0.001(2) 0.003(2) -0.0015(19) C30 0.021(2) 0.024(2) 0.019(2) -0.001(2) 0.0024(18) 0.004(2) C31 0.029(3) 0.021(2) 0.025(3) 0.000(2) -0.001(2) 0.001(2) C32 0.029(3) 0.034(3) 0.030(3) -0.006(2) -0.002(2) 0.000(2) C33 0.032(3) 0.048(3) 0.019(3) 0.003(2) -0.005(2) 0.007(2) C34 0.038(3) 0.031(3) 0.036(3) 0.011(2) 0.001(2) 0.006(2) C35 0.029(3) 0.027(3) 0.025(3) 0.002(2) 0.000(2) 0.000(2) C36 0.043(3) 0.015(2) 0.020(3) 0.000(2) -0.012(2) -0.002(2) C37 0.034(3) 0.023(3) 0.045(3) 0.002(2) -0.015(3) 0.004(2) C38 0.047(3) 0.039(3) 0.032(3) -0.013(3) -0.005(3) 0.017(3) C39 0.062(4) 0.027(3) 0.050(4) -0.019(3) -0.024(3) 0.015(3) C40 0.055(4) 0.022(3) 0.059(4) -0.008(3) -0.015(3) -0.009(3) C41 0.036(3) 0.026(3) 0.044(4) -0.001(2) -0.003(3) -0.004(2)