#------------------------------------------------------------------------------ #$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/00/00/1000004.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_1000004 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H30 Cu I P2' _chemical_formula_weight 630.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.899(5) _cell_length_b 11.729(5) _cell_length_c 12.259(5) _cell_angle_alpha 103.442(5) _cell_angle_beta 96.291(5) _cell_angle_gamma 95.560(5) _cell_volume 1364.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 2.063 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4319 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0104 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.18 _reflns_number_total 4319 _reflns_number_gt 4039 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1038P)^2^+0.5590P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4319 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _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 Cu Cu 0.45979(5) 0.36869(4) 0.37830(4) 0.03768(18) Uani 1 1 d . . . I I 0.59748(3) 0.401507(19) 0.59219(2) 0.03931(16) Uani 1 1 d . . . P1 P 0.25033(11) 0.26261(8) 0.34169(9) 0.0350(3) Uani 1 1 d . . . P2 P 0.61789(11) 0.31869(8) 0.26291(9) 0.0346(3) Uani 1 1 d . . . C1 C 0.1306(5) 0.3224(4) 0.4381(4) 0.0457(10) Uani 1 1 d . . . H1A H 0.1436 0.4080 0.4537 0.055 Uiso 1 1 calc R . . H1B H 0.0375 0.2950 0.4014 0.055 Uiso 1 1 calc R . . C2 C 0.1502(7) 0.2857(5) 0.5496(4) 0.0614(14) Uani 1 1 d . . . H2A H 0.2461 0.2773 0.5673 0.074 Uiso 1 1 calc R . . H2B H 0.0979 0.2088 0.5396 0.074 Uiso 1 1 calc R . . C3 C 0.8932(5) 0.6277(4) 0.3485(4) 0.0522(12) Uani 1 1 d . . . H3A H 0.9249 0.6726 0.2969 0.063 Uiso 1 1 calc R . . H3B H 0.9700 0.5917 0.3758 0.063 Uiso 1 1 calc R . . C4 C 0.7807(6) 0.5293(4) 0.2824(6) 0.0672(16) Uani 1 1 d . . . H4A H 0.6924 0.5552 0.2957 0.081 Uiso 1 1 calc R . . H4B H 0.7865 0.5185 0.2022 0.081 Uiso 1 1 calc R . . C5 C 0.7856(4) 0.4111(3) 0.3112(4) 0.0408(9) Uani 1 1 d . . . H5A H 0.8083 0.4230 0.3924 0.049 Uiso 1 1 calc R . . H5B H 0.8561 0.3711 0.2749 0.049 Uiso 1 1 calc R . . C111 C 0.2344(5) 0.1059(3) 0.3378(4) 0.0403(10) Uani 1 1 d . . . C112 C 0.3504(5) 0.0526(4) 0.3598(5) 0.0513(12) Uani 1 1 d . . . H112 H 0.4363 0.0973 0.3755 0.062 Uiso 1 1 calc R . . C113 C 0.3393(6) -0.0674(5) 0.3587(5) 0.0640(15) Uani 1 1 d . . . H113 H 0.4170 -0.1030 0.3732 0.077 Uiso 1 1 calc R . . C114 C 0.2122(6) -0.1313(4) 0.3358(4) 0.0579(14) Uani 1 1 d . . . H114 H 0.2039 -0.2115 0.3338 0.069 Uiso 1 1 calc R . . C115 C 0.0973(6) -0.0799(4) 0.3160(4) 0.0544(13) Uani 1 1 d . . . H115 H 0.0117 -0.1247 0.3025 0.065 Uiso 1 1 calc R . . C116 C 0.1074(5) 0.0384(4) 0.3160(4) 0.0496(11) Uani 1 1 d . . . H116 H 0.0287 0.0728 0.3012 0.060 Uiso 1 1 calc R . . C121 C 0.1605(5) 0.2642(4) 0.2020(4) 0.0423(10) Uani 1 1 d . . . C122 C 0.1443(7) 0.1686(5) 0.1068(5) 0.0648(15) Uani 1 1 d . . . H122 H 0.1749 0.0979 0.1144 0.078 Uiso 1 1 calc R . . C123 C 0.0836(8) 0.1762(7) 0.0011(5) 0.082(2) Uani 1 1 d . . . H123 H 0.0713 0.1106 -0.0603 0.098 Uiso 1 1 calc R . . C124 C 0.0422(7) 0.2812(7) -0.0119(5) 0.082(2) Uani 1 1 d . . . H124 H 0.0032 0.2874 -0.0825 0.099 Uiso 1 1 calc R . . C125 C 0.0587(7) 0.3784(7) 0.0811(5) 0.0761(17) Uani 1 1 d . . . H125 H 0.0301 0.4494 0.0723 0.091 Uiso 1 1 calc R . . C126 C 0.1175(5) 0.3702(5) 0.1866(4) 0.0540(12) Uani 1 1 d . . . H126 H 0.1284 0.4359 0.2478 0.065 Uiso 1 1 calc R . . C211 C 0.6606(5) 0.1694(4) 0.2559(4) 0.0406(10) Uani 1 1 d . . . C212 C 0.7280(5) 0.1443(4) 0.3525(4) 0.0461(10) Uani 1 1 d . . . H212 H 0.7583 0.2051 0.4168 0.055 Uiso 1 1 calc R . . C213 C 0.7501(5) 0.0290(4) 0.3529(5) 0.0538(12) Uani 1 1 d . . . H213 H 0.7948 0.0128 0.4173 0.065 Uiso 1 1 calc R . . C214 C 0.7053(6) -0.0615(4) 0.2573(5) 0.0621(14) Uani 1 1 d . . . H214 H 0.7214 -0.1382 0.2580 0.074 Uiso 1 1 calc R . . C215 C 0.6366(7) -0.0402(4) 0.1600(6) 0.0749(18) Uani 1 1 d . . . H215 H 0.6073 -0.1014 0.0958 0.090 Uiso 1 1 calc R . . C216 C 0.6131(6) 0.0747(4) 0.1613(5) 0.0613(14) Uani 1 1 d . . . H216 H 0.5644 0.0896 0.0979 0.074 Uiso 1 1 calc R . . C221 C 0.5787(5) 0.3204(3) 0.1136(3) 0.0387(10) Uani 1 1 d . . . C222 C 0.4558(5) 0.3528(4) 0.0746(4) 0.0456(11) Uani 1 1 d . . . H222 H 0.3917 0.3706 0.1240 0.055 Uiso 1 1 calc R . . C223 C 0.4258(6) 0.3593(4) -0.0379(4) 0.0577(13) Uani 1 1 d . . . H223 H 0.3415 0.3799 -0.0628 0.069 Uiso 1 1 calc R . . C224 C 0.5184(7) 0.3357(5) -0.1103(4) 0.0662(16) Uani 1 1 d . . . H224 H 0.4990 0.3405 -0.1850 0.079 Uiso 1 1 calc R . . C225 C 0.6427(7) 0.3044(5) -0.0719(5) 0.0688(16) Uani 1 1 d . . . H225 H 0.7070 0.2891 -0.1216 0.083 Uiso 1 1 calc R . . C226 C 0.6743(6) 0.2950(5) 0.0378(4) 0.0573(13) Uani 1 1 d . . . H226 H 0.7579 0.2721 0.0612 0.069 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 Cu 0.0422(4) 0.0266(3) 0.0447(3) 0.0082(2) 0.0095(2) 0.0040(2) I 0.0550(3) 0.0241(2) 0.0421(2) 0.01200(13) 0.00604(15) 0.01226(14) P1 0.0399(6) 0.0227(5) 0.0433(6) 0.0097(4) 0.0067(5) 0.0037(4) P2 0.0422(7) 0.0222(5) 0.0410(5) 0.0088(4) 0.0091(5) 0.0053(4) C1 0.053(3) 0.037(2) 0.055(2) 0.0180(19) 0.015(2) 0.0143(19) C2 0.095(4) 0.043(3) 0.057(3) 0.020(2) 0.029(3) 0.023(3) C3 0.063(3) 0.032(2) 0.060(3) 0.0066(19) 0.024(2) -0.006(2) C4 0.074(4) 0.033(2) 0.092(4) 0.024(3) -0.008(3) -0.006(2) C5 0.048(3) 0.0259(19) 0.050(2) 0.0105(17) 0.0094(19) 0.0040(17) C111 0.049(3) 0.0217(18) 0.053(2) 0.0122(16) 0.011(2) 0.0042(17) C112 0.053(3) 0.036(2) 0.071(3) 0.019(2) 0.018(2) 0.012(2) C113 0.078(4) 0.040(3) 0.088(4) 0.031(3) 0.027(3) 0.026(3) C114 0.089(4) 0.027(2) 0.062(3) 0.013(2) 0.021(3) 0.009(2) C115 0.069(3) 0.029(2) 0.063(3) 0.013(2) 0.008(2) -0.009(2) C116 0.052(3) 0.028(2) 0.070(3) 0.017(2) 0.009(2) 0.0023(19) C121 0.041(2) 0.039(2) 0.048(2) 0.0162(18) 0.0061(19) -0.0012(18) C122 0.082(4) 0.054(3) 0.054(3) 0.010(2) 0.004(3) -0.003(3) C123 0.104(5) 0.085(5) 0.047(3) 0.008(3) 0.007(3) -0.010(4) C124 0.084(5) 0.111(6) 0.058(3) 0.042(4) -0.003(3) 0.001(4) C125 0.077(4) 0.096(5) 0.071(4) 0.045(4) 0.008(3) 0.028(4) C126 0.055(3) 0.055(3) 0.057(3) 0.023(2) 0.008(2) 0.013(2) C211 0.045(3) 0.025(2) 0.055(3) 0.0116(18) 0.014(2) 0.0093(17) C212 0.058(3) 0.033(2) 0.052(2) 0.0130(18) 0.013(2) 0.0138(19) C213 0.058(3) 0.040(2) 0.070(3) 0.022(2) 0.009(2) 0.015(2) C214 0.081(4) 0.028(2) 0.080(4) 0.013(2) 0.016(3) 0.016(2) C215 0.112(5) 0.026(2) 0.077(4) 0.002(2) -0.005(3) 0.007(3) C216 0.086(4) 0.026(2) 0.067(3) 0.009(2) -0.003(3) 0.004(2) C221 0.055(3) 0.0237(19) 0.039(2) 0.0080(15) 0.0107(19) 0.0043(17) C222 0.061(3) 0.028(2) 0.051(2) 0.0152(18) 0.010(2) 0.005(2) C223 0.080(4) 0.041(3) 0.053(3) 0.020(2) -0.001(3) 0.005(2) C224 0.109(5) 0.045(3) 0.043(3) 0.016(2) 0.008(3) -0.011(3) C225 0.087(4) 0.066(3) 0.052(3) 0.009(3) 0.029(3) -0.004(3) C226 0.063(3) 0.056(3) 0.055(3) 0.010(2) 0.020(2) 0.010(2) _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 1.321 _refine_diff_density_min -1.563 _refine_diff_density_rms 0.258 _cod_database_code 1000004