#------------------------------------------------------------------------------ #$Date: 2014-07-23 10:49:31 +0100 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/01/4060142.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_4060142 _journal_name_full Organometallics _journal_year 2005 _chemical_formula_sum 'C41 H42 P Rh' _chemical_formula_weight 668.63 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 91.8700(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.6680(10) _cell_length_b 19.3790(10) _cell_length_c 18.8010(10) _cell_measurement_reflns_used 251 _cell_measurement_temperature 150.0(1) _cell_measurement_theta_max 20.0 _cell_measurement_theta_min 3.0 _cell_volume 3156.5(4) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ? _computing_publication_material ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150.0(1) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 14887 _diffrn_reflns_theta_max 29.95 _diffrn_reflns_theta_min 2.76 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_T_max 0.9292 _exptl_absorpt_correction_T_min 0.8859 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1392 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 403 _refine_ls_number_reflns 9120 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0400 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.1033 _reflns_number_gt 6967 _reflns_number_total 9120 _reflns_threshold_expression >2sigma(I) _[local]_cod_cif_authors_sg_H-M P21/n _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4060142 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' 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 Rh1 Rh 0.111610(16) 0.194056(9) 0.290725(8) 0.01831(6) Uani 1 1 d . . . P1 P 0.42353(6) 0.12788(3) 0.31239(3) 0.01956(12) Uani 1 1 d . . . C1 C 0.3050(2) 0.16529(12) 0.38163(11) 0.0194(4) Uani 1 1 d . . . C2 C 0.1631(2) 0.13388(11) 0.39651(10) 0.0188(4) Uani 1 1 d . . . C3 C 0.0782(2) 0.09389(11) 0.34400(10) 0.0188(4) Uani 1 1 d . . . H3 H -0.0165 0.0744 0.3581 0.023 Uiso 1 1 calc R . . C4 C 0.1221(2) 0.08061(12) 0.27282(11) 0.0196(4) Uani 1 1 d . . . C5 C 0.2641(2) 0.10783(12) 0.24955(10) 0.0192(4) Uani 1 1 d . . . C6 C 0.4938(2) 0.04148(12) 0.34791(11) 0.0234(5) Uani 1 1 d . . . C7 C 0.6105(3) 0.05687(15) 0.40881(15) 0.0391(6) Uani 1 1 d . . . H7A H 0.5574 0.0787 0.4481 0.059 Uiso 1 1 calc R . . H7B H 0.6904 0.0880 0.3919 0.059 Uiso 1 1 calc R . . H7C H 0.6583 0.0137 0.4254 0.059 Uiso 1 1 calc R . . C8 C 0.5787(3) 0.00826(14) 0.28668(13) 0.0334(6) Uani 1 1 d . . . H8A H 0.6268 -0.0349 0.3030 0.050 Uiso 1 1 calc R . . H8B H 0.6586 0.0398 0.2705 0.050 Uiso 1 1 calc R . . H8C H 0.5052 -0.0014 0.2472 0.050 Uiso 1 1 calc R . . C9 C 0.3727(2) -0.00847(13) 0.37481(13) 0.0309(5) Uani 1 1 d . . . H9A H 0.4232 -0.0511 0.3913 0.046 Uiso 1 1 calc R . . H9B H 0.2981 -0.0192 0.3361 0.046 Uiso 1 1 calc R . . H9C H 0.3189 0.0128 0.4143 0.046 Uiso 1 1 calc R . . C10 C 0.3742(2) 0.22294(12) 0.42468(11) 0.0199(4) Uani 1 1 d . . . C11 C 0.5335(2) 0.23485(13) 0.42676(12) 0.0266(5) Uani 1 1 d . . . H11 H 0.5986 0.2045 0.4017 0.032 Uiso 1 1 calc R . . C12 C 0.5989(2) 0.28948(14) 0.46417(13) 0.0300(5) Uani 1 1 d . . . H12 H 0.7074 0.2961 0.4641 0.036 Uiso 1 1 calc R . . C13 C 0.5089(3) 0.33439(14) 0.50152(13) 0.0309(5) Uani 1 1 d . . . H13 H 0.5542 0.3714 0.5280 0.037 Uiso 1 1 calc R . . C14 C 0.3505(3) 0.32432(14) 0.49959(13) 0.0310(5) Uani 1 1 d . . . H14 H 0.2861 0.3552 0.5243 0.037 Uiso 1 1 calc R . . C15 C 0.2853(2) 0.26987(13) 0.46210(12) 0.0256(5) Uani 1 1 d . . . H15 H 0.1764 0.2641 0.4617 0.031 Uiso 1 1 calc R . . C16 C 0.0903(2) 0.14007(11) 0.46748(10) 0.0194(4) Uani 1 1 d . . . C17 C 0.1789(2) 0.12534(13) 0.52916(11) 0.0247(5) Uani 1 1 d . . . H17 H 0.2850 0.1141 0.5256 0.030 Uiso 1 1 calc R . . C18 C 0.1132(3) 0.12705(13) 0.59541(12) 0.0289(5) Uani 1 1 d . . . H18 H 0.1739 0.1163 0.6369 0.035 Uiso 1 1 calc R . . C19 C -0.0413(3) 0.14441(13) 0.60100(12) 0.0293(5) Uani 1 1 d . . . H19 H -0.0854 0.1469 0.6465 0.035 Uiso 1 1 calc R . . C20 C -0.1308(2) 0.15801(13) 0.54075(12) 0.0282(5) Uani 1 1 d . . . H20 H -0.2367 0.1696 0.5447 0.034 Uiso 1 1 calc R . . C21 C -0.0657(2) 0.15474(12) 0.47401(12) 0.0240(5) Uani 1 1 d . . . H21 H -0.1286 0.1626 0.4325 0.029 Uiso 1 1 calc R . . C22 C 0.0127(2) 0.03874(12) 0.22704(11) 0.0207(4) Uani 1 1 d . . . C23 C -0.0701(2) 0.06667(13) 0.16950(12) 0.0275(5) Uani 1 1 d . . . H23 H -0.0632 0.1146 0.1595 0.033 Uiso 1 1 calc R . . C24 C -0.1629(3) 0.02430(15) 0.12662(12) 0.0344(6) Uani 1 1 d . . . H24 H -0.2202 0.0437 0.0876 0.041 Uiso 1 1 calc R . . C25 C -0.1729(3) -0.04527(14) 0.13991(12) 0.0319(6) Uani 1 1 d . . . H25 H -0.2339 -0.0740 0.1092 0.038 Uiso 1 1 calc R . . C26 C -0.0940(2) -0.07332(14) 0.19793(12) 0.0308(5) Uani 1 1 d . . . H26 H -0.1020 -0.1212 0.2079 0.037 Uiso 1 1 calc R . . C27 C -0.0034(2) -0.03124(13) 0.24149(12) 0.0261(5) Uani 1 1 d . . . H27 H 0.0488 -0.0505 0.2820 0.031 Uiso 1 1 calc R . . C28 C 0.3155(2) 0.10088(12) 0.17408(11) 0.0218(5) Uani 1 1 d . . . C29 C 0.4045(2) 0.15387(14) 0.14506(12) 0.0280(5) Uani 1 1 d . . . H29 H 0.4294 0.1935 0.1729 0.034 Uiso 1 1 calc R . . C30 C 0.4566(3) 0.14913(15) 0.07611(13) 0.0351(6) Uani 1 1 d . . . H30 H 0.5136 0.1861 0.0568 0.042 Uiso 1 1 calc R . . C31 C 0.4265(3) 0.09150(16) 0.03587(12) 0.0382(7) Uani 1 1 d . . . H31 H 0.4630 0.0884 -0.0111 0.046 Uiso 1 1 calc R . . C32 C 0.3427(3) 0.03798(16) 0.06389(13) 0.0375(6) Uani 1 1 d . . . H32 H 0.3216 -0.0020 0.0360 0.045 Uiso 1 1 calc R . . C33 C 0.2884(2) 0.04212(14) 0.13300(12) 0.0288(5) Uani 1 1 d . . . H33 H 0.2327 0.0046 0.1520 0.035 Uiso 1 1 calc R . . C34 C 0.1114(2) 0.25313(13) 0.19529(12) 0.0251(5) Uani 1 1 d . . . H34 H 0.154(3) 0.2219(14) 0.1589(13) 0.030 Uiso 1 1 d . . . C35 C 0.2118(3) 0.28359(13) 0.24638(12) 0.0246(5) Uani 1 1 d . . . H35 H 0.314(3) 0.2739(14) 0.2437(13) 0.030 Uiso 1 1 d . . . C36 C 0.1760(3) 0.34696(14) 0.28968(13) 0.0318(5) Uani 1 1 d . . . H36A H 0.1846 0.3884 0.2593 0.038 Uiso 1 1 calc R . . H36B H 0.2531 0.3512 0.3294 0.038 Uiso 1 1 calc R . . C37 C 0.0128(3) 0.34423(13) 0.32002(13) 0.0296(5) Uani 1 1 d . . . H37A H 0.0116 0.3715 0.3646 0.035 Uiso 1 1 calc R . . H37B H -0.0617 0.3654 0.2855 0.035 Uiso 1 1 calc R . . C38 C -0.0366(2) 0.27087(13) 0.33518(12) 0.0241(5) Uani 1 1 d . . . H38 H -0.039(3) 0.2603(14) 0.3812(13) 0.029 Uiso 1 1 d . . . C39 C -0.1246(2) 0.22954(13) 0.28786(12) 0.0256(5) Uani 1 1 d . . . H39 H -0.181(3) 0.1922(13) 0.3093(14) 0.031 Uiso 1 1 d . . . C40 C -0.1766(2) 0.25181(14) 0.21395(13) 0.0313(6) Uani 1 1 d . . . H40A H -0.2610 0.2859 0.2175 0.038 Uiso 1 1 calc R . . H40B H -0.2179 0.2113 0.1874 0.038 Uiso 1 1 calc R . . C41 C -0.0444(3) 0.28383(14) 0.17268(13) 0.0304(5) Uani 1 1 d . . . H41A H -0.0633 0.2759 0.1211 0.036 Uiso 1 1 calc R . . H41B H -0.0423 0.3343 0.1809 0.036 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 Rh1 0.01650(9) 0.02023(10) 0.01834(9) 0.00068(7) 0.00236(6) 0.00034(6) P1 0.0163(2) 0.0220(3) 0.0205(3) -0.0016(2) 0.00238(19) -0.0001(2) C1 0.0181(9) 0.0218(12) 0.0185(10) -0.0011(9) 0.0012(7) 0.0001(9) C2 0.0178(9) 0.0205(11) 0.0182(10) 0.0014(8) 0.0010(7) 0.0009(8) C3 0.0156(9) 0.0212(12) 0.0196(10) 0.0025(8) 0.0004(7) -0.0015(8) C4 0.0197(9) 0.0173(11) 0.0217(10) -0.0007(9) -0.0010(7) -0.0001(8) C5 0.0193(9) 0.0206(12) 0.0178(10) -0.0008(8) 0.0023(7) 0.0013(8) C6 0.0204(10) 0.0240(12) 0.0258(11) -0.0028(9) -0.0008(8) 0.0029(9) C7 0.0384(13) 0.0312(15) 0.0462(16) -0.0019(12) -0.0197(11) 0.0050(11) C8 0.0318(11) 0.0293(15) 0.0393(14) -0.0047(11) 0.0064(10) 0.0091(11) C9 0.0293(11) 0.0270(14) 0.0365(13) 0.0067(11) 0.0009(9) 0.0031(10) C10 0.0185(9) 0.0210(12) 0.0201(10) 0.0017(9) 0.0006(7) -0.0013(9) C11 0.0203(10) 0.0267(13) 0.0329(12) -0.0043(10) 0.0029(8) -0.0001(9) C12 0.0199(10) 0.0351(15) 0.0349(13) -0.0046(11) 0.0002(9) -0.0039(10) C13 0.0315(12) 0.0304(14) 0.0309(13) -0.0073(11) -0.0002(9) -0.0097(11) C14 0.0277(11) 0.0333(15) 0.0324(13) -0.0106(11) 0.0075(9) -0.0020(10) C15 0.0206(10) 0.0269(13) 0.0294(12) -0.0048(10) 0.0037(8) -0.0007(9) C16 0.0210(9) 0.0210(12) 0.0164(10) -0.0010(8) 0.0030(7) -0.0024(8) C17 0.0208(10) 0.0288(13) 0.0245(11) 0.0000(10) 0.0003(8) 0.0026(9) C18 0.0346(12) 0.0319(14) 0.0201(11) 0.0013(10) 0.0003(9) 0.0005(11) C19 0.0398(13) 0.0277(14) 0.0210(11) -0.0006(10) 0.0109(9) -0.0006(11) C20 0.0239(10) 0.0300(14) 0.0314(12) 0.0046(10) 0.0093(9) 0.0021(10) C21 0.0202(10) 0.0266(13) 0.0252(11) 0.0022(10) 0.0007(8) -0.0033(9) C22 0.0176(9) 0.0266(12) 0.0180(10) -0.0023(9) 0.0029(7) -0.0023(9) C23 0.0312(11) 0.0258(13) 0.0252(11) 0.0017(10) -0.0032(9) -0.0023(10) C24 0.0394(13) 0.0377(16) 0.0253(12) 0.0028(11) -0.0123(9) -0.0062(12) C25 0.0330(12) 0.0347(15) 0.0278(12) -0.0063(11) -0.0026(9) -0.0114(11) C26 0.0293(11) 0.0261(14) 0.0370(14) -0.0014(11) 0.0012(9) -0.0085(10) C27 0.0263(10) 0.0263(13) 0.0254(11) 0.0022(10) -0.0025(8) -0.0006(10) C28 0.0177(9) 0.0281(13) 0.0197(10) 0.0009(9) 0.0015(7) 0.0050(9) C29 0.0269(11) 0.0301(14) 0.0275(12) 0.0033(10) 0.0090(9) 0.0034(10) C30 0.0284(12) 0.0485(18) 0.0290(13) 0.0148(12) 0.0106(9) 0.0116(12) C31 0.0302(12) 0.064(2) 0.0204(11) 0.0009(12) 0.0051(9) 0.0188(13) C32 0.0315(12) 0.0507(19) 0.0302(13) -0.0151(12) -0.0015(10) 0.0112(12) C33 0.0261(11) 0.0347(15) 0.0257(12) -0.0034(10) 0.0022(8) 0.0042(10) C34 0.0292(11) 0.0257(13) 0.0208(11) 0.0061(9) 0.0068(8) 0.0048(10) C35 0.0237(10) 0.0229(12) 0.0278(12) 0.0061(10) 0.0087(9) -0.0022(10) C36 0.0354(13) 0.0253(14) 0.0346(13) 0.0031(11) 0.0021(10) -0.0026(11) C37 0.0313(11) 0.0257(14) 0.0318(13) -0.0002(10) 0.0043(9) 0.0047(10) C38 0.0240(10) 0.0250(13) 0.0237(11) 0.0015(10) 0.0059(8) 0.0072(9) C39 0.0159(9) 0.0309(14) 0.0302(12) 0.0040(10) 0.0040(8) 0.0040(9) C40 0.0233(11) 0.0357(15) 0.0345(13) 0.0007(11) -0.0031(9) 0.0096(10) C41 0.0340(12) 0.0326(14) 0.0244(12) 0.0056(11) 0.0000(9) 0.0070(11) _journal_paper_doi 10.1021/om049261y