#------------------------------------------------------------------------------ #$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/02/4000245.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_4000245 loop_ _publ_author_name 'Stephen Lee' 'Banglin Chen' 'Daniel C. Fredrickson' 'Francis J. DiSalvo' 'Emil Lobkovsky' 'Judith A. Adams' _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm020651p _journal_year 2003 _chemical_formula_sum 'C30 H27 I11.5 S6' _chemical_formula_weight 2039.23 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 107.217(6) _cell_angle_beta 95.966(6) _cell_angle_gamma 94.088(6) _cell_formula_units_Z 2 _cell_length_a 10.845(2) _cell_length_b 12.758(2) _cell_length_c 17.660(3) _cell_measurement_temperature 173(2) _cell_volume 2307.9(7) _diffrn_ambient_temperature 173(2) _diffrn_measurement_device_type 'Bruker 1K CCD area detector' _diffrn_measurement_method '0.3 deg. omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 18671 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.12 _exptl_absorpt_coefficient_mu 8.012 _exptl_absorpt_correction_T_max 0.6901 _exptl_absorpt_correction_T_min 0.1973 _exptl_absorpt_correction_type SADABS _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.934 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'flat rod' _exptl_crystal_F_000 1825 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 430 _refine_ls_number_reflns 9232 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0595 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1308 _refine_ls_wR_factor_ref 0.1431 _reflns_number_gt 6503 _reflns_number_total 9232 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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_original_sg_symbol_H-M P-1 _cod_original_formula_sum 'C30 H27 I11.50 S6' _cod_database_code 4000245 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 I1 I 0.0000 0.0000 0.0000 0.0267(2) Uani 1 2 d S . . I2 I 0.24958(7) 0.06696(6) 0.09158(4) 0.02700(18) Uani 1 1 d . . . I3 I 0.00470(8) 0.18292(7) 0.23548(5) 0.0355(2) Uani 1 1 d . . . I4 I -0.08448(7) 0.29645(6) 0.38112(5) 0.0309(2) Uani 1 1 d . . . I5 I -0.17633(8) 0.41692(7) 0.53424(5) 0.0363(2) Uani 1 1 d . . . I6 I -0.33851(7) 0.06727(6) 0.07587(4) 0.02549(18) Uani 1 1 d . . . I7 I -0.40139(7) 0.18113(6) 0.22178(5) 0.03034(19) Uani 1 1 d . . . I8 I 0.28480(9) 0.26330(7) 0.32856(5) 0.0379(2) Uani 1 1 d . . . I9 I 0.51705(9) 0.33424(7) 0.41970(5) 0.0380(2) Uani 1 1 d . . . I10 I 0.14160(8) 0.79275(7) 0.40066(5) 0.0388(2) Uani 1 1 d . . . I11 I 0.12162(10) 0.98205(8) 0.35789(7) 0.0586(3) Uani 1 1 d . . . I12 I -1.49615(9) -0.09828(9) -0.48374(6) 0.0595(3) Uani 1 1 d . . . S1 S -0.2041(3) 0.5790(2) 0.36873(18) 0.0312(7) Uani 1 1 d . . . S2 S -0.2305(3) 0.9454(2) 0.26845(19) 0.0329(7) Uani 1 1 d . . . S3 S -0.1469(3) 0.6162(2) -0.13510(17) 0.0281(7) Uani 1 1 d . . . S4 S -0.1463(3) 0.2435(2) -0.03943(18) 0.0301(7) Uani 1 1 d . . . S5 S -0.5296(3) 0.4846(2) 0.25359(17) 0.0281(7) Uani 1 1 d . . . S6 S -0.5388(3) 0.8530(2) 0.15271(18) 0.0289(7) Uani 1 1 d . . . C1 C -0.2112(10) 0.6426(8) 0.2949(6) 0.021(2) Uani 1 1 d . . . C2 C -0.2191(10) 0.7549(9) 0.3109(6) 0.023(2) Uani 1 1 d . . . H2A H -0.2248 0.7983 0.3641 0.028 Uiso 1 1 calc R . . C3 C -0.2189(9) 0.8056(8) 0.2518(6) 0.019(2) Uani 1 1 d . . . C4 C -0.2091(10) 0.7421(8) 0.1710(6) 0.021(2) Uani 1 1 d . . . C5 C -0.2037(10) 0.7878(8) 0.1094(7) 0.025(3) Uani 1 1 d . . . H5A H -0.2101 0.8646 0.1203 0.030 Uiso 1 1 calc R . . C6 C -0.1896(11) 0.7269(9) 0.0335(7) 0.028(3) Uani 1 1 d . . . H6A H -0.1866 0.7623 -0.0067 0.034 Uiso 1 1 calc R . . C7 C -0.1796(9) 0.6143(8) 0.0138(6) 0.021(2) Uani 1 1 d . . . C8 C -0.1596(10) 0.5475(9) -0.0649(6) 0.020(2) Uani 1 1 d . . . C9 C -0.1505(10) 0.4359(9) -0.0795(6) 0.025(3) Uani 1 1 d . . . H9A H -0.1370 0.3932 -0.1314 0.030 Uiso 1 1 calc R . . C10 C -0.1603(9) 0.3842(8) -0.0217(6) 0.021(2) Uani 1 1 d . . . C11 C -0.1795(9) 0.4463(8) 0.0589(6) 0.018(2) Uani 1 1 d . . . C12 C -0.1870(10) 0.3978(9) 0.1191(6) 0.024(2) Uani 1 1 d . . . H12A H -0.1821 0.3208 0.1079 0.028 Uiso 1 1 calc R . . C13 C -0.2015(10) 0.4601(8) 0.1944(6) 0.023(2) Uani 1 1 d . . . H13A H -0.2087 0.4247 0.2343 0.028 Uiso 1 1 calc R . . C14 C -0.2064(9) 0.5743(9) 0.2150(6) 0.020(2) Uani 1 1 d . . . C15 C -0.2024(9) 0.6256(8) 0.1545(6) 0.018(2) Uani 1 1 d . . . C16 C -0.1864(9) 0.5610(8) 0.0750(6) 0.020(2) Uani 1 1 d . . . C17 C -0.2044(12) 0.6906(10) 0.4592(7) 0.038(3) Uani 1 1 d . . . H17A H -0.2004 0.6618 0.5049 0.057 Uiso 1 1 calc R . . H17B H -0.2810 0.7263 0.4558 0.057 Uiso 1 1 calc R . . H17C H -0.1320 0.7447 0.4662 0.057 Uiso 1 1 calc R . . C18 C -0.2318(13) 0.9993(10) 0.3747(7) 0.043(3) Uani 1 1 d . . . H18A H -0.2388 1.0788 0.3893 0.064 Uiso 1 1 calc R . . H18B H -0.1543 0.9863 0.4026 0.064 Uiso 1 1 calc R . . H18C H -0.3030 0.9622 0.3899 0.064 Uiso 1 1 calc R . . C19 C -0.1292(11) 0.5075(9) -0.2246(6) 0.030(3) Uani 1 1 d . . . H19A H -0.1209 0.5388 -0.2685 0.045 Uiso 1 1 calc R . . H19B H -0.2027 0.4527 -0.2389 0.045 Uiso 1 1 calc R . . H19C H -0.0545 0.4720 -0.2150 0.045 Uiso 1 1 calc R . . C20 C -0.1191(11) 0.1987(9) -0.1410(7) 0.034(3) Uani 1 1 d . . . H20A H -0.1102 0.1195 -0.1570 0.051 Uiso 1 1 calc R . . H20B H -0.0426 0.2393 -0.1472 0.051 Uiso 1 1 calc R . . H20C H -0.1897 0.2124 -0.1749 0.051 Uiso 1 1 calc R . . C21 C -0.5284(9) 0.5494(8) 0.1797(6) 0.018(2) Uani 1 1 d . . . C22 C -0.5331(10) 0.6624(9) 0.1934(6) 0.025(3) Uani 1 1 d . . . H22A H -0.5410 0.7063 0.2461 0.030 Uiso 1 1 calc R . . C23 C -0.5271(9) 0.7136(8) 0.1369(6) 0.020(2) Uani 1 1 d . . . C24 C -0.5127(9) 0.6479(8) 0.0564(6) 0.018(2) Uani 1 1 d . . . C25 C -0.5032(10) 0.6961(9) -0.0061(6) 0.024(2) Uani 1 1 d . . . H25A H -0.5075 0.7731 0.0043 0.029 Uiso 1 1 calc R . . C26 C -0.4880(10) 0.6329(9) -0.0802(6) 0.026(3) Uani 1 1 d . . . H26A H -0.4793 0.6679 -0.1202 0.031 Uiso 1 1 calc R . . C27 C -0.4844(10) 0.5184(8) -0.1010(6) 0.021(2) Uani 1 1 d . . . C28 C -0.5064(9) 0.5332(8) 0.0397(5) 0.014(2) Uani 1 1 d . . . C30 C -0.5392(12) 0.5966(10) 0.3433(6) 0.037(3) Uani 1 1 d . . . H30A H -0.5406 0.5676 0.3888 0.056 Uiso 1 1 calc R . . H30B H -0.6157 0.6312 0.3364 0.056 Uiso 1 1 calc R . . H30C H -0.4667 0.6514 0.3533 0.056 Uiso 1 1 calc R . . C31 C -0.5629(13) 0.9045(10) 0.2571(7) 0.040(3) Uani 1 1 d . . . H31A H -0.5711 0.9837 0.2712 0.059 Uiso 1 1 calc R . . H31B H -0.4914 0.8920 0.2909 0.059 Uiso 1 1 calc R . . H31C H -0.6390 0.8655 0.2654 0.059 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 I1 0.0352(6) 0.0250(5) 0.0256(6) 0.0131(4) 0.0096(5) 0.0088(4) I2 0.0324(4) 0.0256(4) 0.0247(4) 0.0097(3) 0.0036(3) 0.0055(3) I3 0.0372(5) 0.0399(5) 0.0303(4) 0.0116(4) 0.0093(4) -0.0009(4) I4 0.0298(4) 0.0310(4) 0.0340(4) 0.0160(3) -0.0008(3) -0.0015(3) I5 0.0425(5) 0.0372(5) 0.0307(4) 0.0106(4) 0.0101(4) 0.0049(4) I6 0.0264(4) 0.0256(4) 0.0277(4) 0.0137(3) 0.0021(3) 0.0020(3) I7 0.0347(4) 0.0308(4) 0.0302(4) 0.0139(3) 0.0086(3) 0.0081(3) I8 0.0573(6) 0.0318(4) 0.0293(4) 0.0116(3) 0.0200(4) 0.0050(4) I9 0.0537(5) 0.0333(4) 0.0285(4) 0.0101(3) 0.0131(4) 0.0016(4) I10 0.0300(4) 0.0425(5) 0.0413(5) 0.0086(4) 0.0073(4) 0.0020(4) I11 0.0592(6) 0.0489(6) 0.0789(8) 0.0283(5) 0.0270(6) 0.0148(5) I12 0.0457(6) 0.0597(6) 0.0589(6) -0.0047(5) -0.0019(5) 0.0227(5) S1 0.0421(18) 0.0323(16) 0.0277(16) 0.0191(13) 0.0093(14) 0.0103(13) S2 0.0423(18) 0.0215(14) 0.0360(17) 0.0093(13) 0.0102(14) 0.0009(13) S3 0.0401(17) 0.0266(15) 0.0224(15) 0.0132(12) 0.0093(13) 0.0034(13) S4 0.0393(17) 0.0203(14) 0.0361(17) 0.0146(12) 0.0106(14) 0.0046(12) S5 0.0343(16) 0.0314(15) 0.0258(15) 0.0180(13) 0.0085(13) 0.0041(13) S6 0.0385(17) 0.0204(14) 0.0312(16) 0.0107(12) 0.0109(13) 0.0044(12) C1 0.026(6) 0.022(5) 0.021(6) 0.014(4) 0.010(5) 0.001(4) C2 0.023(6) 0.032(6) 0.016(5) 0.008(5) 0.008(5) 0.006(5) C3 0.017(5) 0.013(5) 0.029(6) 0.006(4) 0.007(5) -0.001(4) C4 0.023(5) 0.020(5) 0.025(6) 0.014(5) 0.008(5) 0.001(4) C5 0.027(6) 0.015(5) 0.037(7) 0.013(5) 0.005(5) 0.002(4) C6 0.035(7) 0.029(6) 0.024(6) 0.013(5) 0.001(5) 0.003(5) C7 0.021(5) 0.020(5) 0.020(6) 0.008(4) 0.003(4) -0.007(4) C8 0.021(5) 0.027(6) 0.016(5) 0.016(4) 0.003(4) -0.004(4) C9 0.022(6) 0.033(6) 0.018(6) 0.006(5) 0.007(5) -0.001(5) C10 0.014(5) 0.022(5) 0.031(6) 0.014(5) 0.001(5) 0.001(4) C11 0.013(5) 0.023(5) 0.024(6) 0.015(5) 0.003(4) 0.001(4) C12 0.028(6) 0.023(6) 0.025(6) 0.014(5) 0.011(5) 0.002(5) C13 0.032(6) 0.023(6) 0.019(6) 0.014(5) 0.002(5) -0.003(5) C14 0.011(5) 0.027(6) 0.028(6) 0.018(5) 0.005(4) 0.004(4) C15 0.019(5) 0.023(5) 0.013(5) 0.010(4) 0.004(4) -0.003(4) C16 0.017(5) 0.019(5) 0.025(6) 0.012(4) 0.002(4) 0.000(4) C17 0.047(8) 0.048(8) 0.026(7) 0.022(6) 0.000(6) 0.006(6) C18 0.064(9) 0.026(6) 0.043(8) 0.013(6) 0.028(7) -0.004(6) C19 0.034(7) 0.041(7) 0.022(6) 0.018(5) 0.008(5) 0.002(5) C20 0.037(7) 0.028(6) 0.039(7) 0.006(6) 0.024(6) 0.010(5) C21 0.016(5) 0.019(5) 0.027(6) 0.019(4) 0.002(4) 0.004(4) C22 0.019(5) 0.039(7) 0.016(5) 0.003(5) 0.004(5) 0.006(5) C23 0.017(5) 0.020(5) 0.029(6) 0.015(5) 0.004(5) 0.002(4) C24 0.016(5) 0.021(5) 0.019(5) 0.008(4) 0.006(4) 0.002(4) C25 0.028(6) 0.024(6) 0.024(6) 0.011(5) 0.003(5) 0.003(5) C26 0.031(6) 0.029(6) 0.022(6) 0.015(5) 0.000(5) 0.004(5) C27 0.029(6) 0.022(5) 0.018(5) 0.015(4) 0.004(5) -0.004(5) C28 0.016(5) 0.017(5) 0.010(5) 0.007(4) 0.000(4) 0.001(4) C30 0.045(8) 0.050(8) 0.017(6) 0.012(6) 0.006(5) 0.005(6) C31 0.051(8) 0.032(7) 0.037(7) 0.010(6) 0.014(6) -0.003(6)