#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/04/4000431.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_4000431 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm0493997 _journal_year 2004 _chemical_formula_moiety 'C28 H56 O4 Zn4' _chemical_formula_sum 'C28 H56 O4 Zn4' _chemical_formula_weight 718.21 _chemical_name_common '(6) Zn4(OMPec)4(Et)4' _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 97.350(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.166(3) _cell_length_b 19.155(8) _cell_length_c 10.522(4) _cell_measurement_temperature 168(2) _cell_volume 1632.4(11) _diffrn_ambient_temperature 168(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'CCD area detector' _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 0.71073 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 11739 _diffrn_reflns_theta_max 25.69 _diffrn_reflns_theta_min 1.95 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 2.931 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 752 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 329 _refine_ls_number_reflns 6029 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.993 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0481 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1002 _refine_ls_wR_factor_ref 0.1119 _reflns_number_gt 4550 _reflns_number_total 6029 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'NONE' changed to 'none' 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 P21 _cod_database_code 4000431 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -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 Zn1 Zn 0.24298(10) 0.09869(4) 0.83254(7) 0.0346(2) Uani 1 1 d . . . Zn2 Zn 0.02072(10) 0.09455(5) 0.57145(7) 0.0380(2) Uani 1 1 d . . . Zn3 Zn 0.34833(11) 0.17634(4) 0.59573(8) 0.0353(2) Uani 1 1 d . . . Zn4 Zn 0.05767(10) 0.23100(4) 0.72978(8) 0.0340(2) Uani 1 1 d . . . O1 O 0.2654(5) 0.0788(2) 0.6403(4) 0.0303(11) Uani 1 1 d . . . O2 O 0.3004(6) 0.1991(2) 0.7828(4) 0.0269(10) Uani 1 1 d . . . O3 O 0.1004(6) 0.1960(2) 0.5483(4) 0.0312(11) Uani 1 1 d . . . O4 O 0.0046(6) 0.1274(2) 0.7580(4) 0.0312(11) Uani 1 1 d . . . C1 C 0.3135(11) 0.0337(4) 0.9745(8) 0.048(2) Uani 1 1 d . . . H1A H 0.2387 -0.0071 0.9629 0.058 Uiso 1 1 calc R . . H1B H 0.4248 0.0168 0.9620 0.058 Uiso 1 1 calc R . . C2 C 0.3216(13) 0.0549(5) 1.1081(8) 0.066(3) Uani 1 1 d . . . H2A H 0.4034 0.0923 1.1258 0.099 Uiso 1 1 calc R . . H2B H 0.3538 0.0149 1.1637 0.099 Uiso 1 1 calc R . . H2C H 0.2132 0.0719 1.1246 0.099 Uiso 1 1 calc R . . C3 C -0.1463(12) 0.0370(6) 0.4706(12) 0.080(3) Uani 1 1 d . . . H3A H -0.1795 0.0009 0.5295 0.096 Uiso 1 1 calc R . . H3B H -0.2438 0.0674 0.4481 0.096 Uiso 1 1 calc R . . C4 C -0.1198(17) 0.0018(7) 0.3563(10) 0.108(5) Uani 1 1 d . . . H4A H -0.0400 0.0280 0.3129 0.162 Uiso 1 1 calc R . . H4B H -0.2244 -0.0018 0.2996 0.162 Uiso 1 1 calc R . . H4C H -0.0766 -0.0451 0.3774 0.162 Uiso 1 1 calc R . . C5 C 0.5490(10) 0.1999(4) 0.5196(8) 0.0450(19) Uani 1 1 d . . . H5A H 0.5878 0.2463 0.5525 0.054 Uiso 1 1 calc R . . H5B H 0.6356 0.1656 0.5508 0.054 Uiso 1 1 calc R . . C6 C 0.5345(11) 0.2019(4) 0.3732(7) 0.049(2) Uani 1 1 d . . . H6A H 0.5021 0.1557 0.3387 0.073 Uiso 1 1 calc R . . H6B H 0.6413 0.2149 0.3469 0.073 Uiso 1 1 calc R . . H6C H 0.4509 0.2363 0.3403 0.073 Uiso 1 1 calc R . . C7 C -0.0814(10) 0.3128(4) 0.7567(8) 0.048(2) Uani 1 1 d . . . H7A H -0.0906 0.3410 0.6773 0.058 Uiso 1 1 calc R . . H7B H -0.1934 0.2951 0.7649 0.058 Uiso 1 1 calc R . . C8 C -0.0348(13) 0.3607(5) 0.8648(10) 0.075(3) Uani 1 1 d . . . H8A H -0.0319 0.3350 0.9457 0.112 Uiso 1 1 calc R . . H8B H -0.1160 0.3985 0.8625 0.112 Uiso 1 1 calc R . . H8C H 0.0745 0.3804 0.8583 0.112 Uiso 1 1 calc R . . C9 C 0.3587(9) 0.0189(4) 0.6084(7) 0.0343(17) Uani 1 1 d . . . H9 H 0.4741 0.0236 0.6526 0.041 Uiso 1 1 calc R . . C10 C 0.2883(15) -0.0503(4) 0.6494(10) 0.070(3) Uani 1 1 d . . . H10A H 0.3189 -0.0587 0.7422 0.084 Uiso 1 1 calc R . . H10B H 0.1665 -0.0514 0.6292 0.084 Uiso 1 1 calc R . . C11 C 0.3693(16) -0.1033(5) 0.5696(11) 0.086(4) Uani 1 1 d . . . H11A H 0.2924 -0.1423 0.5441 0.103 Uiso 1 1 calc R . . H11B H 0.4701 -0.1226 0.6195 0.103 Uiso 1 1 calc R . . C12 C 0.4135(12) -0.0648(5) 0.4499(10) 0.064(3) Uani 1 1 d . . . H12A H 0.5331 -0.0689 0.4439 0.077 Uiso 1 1 calc R . . H12B H 0.3513 -0.0846 0.3713 0.077 Uiso 1 1 calc R . . C13 C 0.3662(11) 0.0115(5) 0.4660(8) 0.052(2) Uani 1 1 d . . . H13A H 0.4502 0.0431 0.4376 0.062 Uiso 1 1 calc R . . H13B H 0.2577 0.0219 0.4163 0.062 Uiso 1 1 calc R . . C14 C 0.4146(9) 0.2425(4) 0.8588(7) 0.0382(18) Uani 1 1 d . . . H14 H 0.5264 0.2205 0.8652 0.046 Uiso 1 1 calc R . . C15 C 0.3713(13) 0.2538(5) 0.9919(8) 0.060(3) Uani 1 1 d . . . H15A H 0.4051 0.2134 1.0478 0.072 Uiso 1 1 calc R . . H15B H 0.2512 0.2616 0.9906 0.072 Uiso 1 1 calc R . . C16 C 0.4712(17) 0.3204(6) 1.0378(10) 0.088(4) Uani 1 1 d . . . H16A H 0.4082 0.3493 1.0926 0.105 Uiso 1 1 calc R . . H16B H 0.5779 0.3074 1.0877 0.105 Uiso 1 1 calc R . . C17 C 0.4993(13) 0.3596(5) 0.9196(10) 0.070(3) Uani 1 1 d . . . H17A H 0.6190 0.3666 0.9173 0.084 Uiso 1 1 calc R . . H17B H 0.4454 0.4059 0.9184 0.084 Uiso 1 1 calc R . . C18 C 0.4250(10) 0.3163(4) 0.8037(8) 0.046(2) Uani 1 1 d . . . H18A H 0.3142 0.3338 0.7689 0.055 Uiso 1 1 calc R . . H18B H 0.4972 0.3172 0.7349 0.055 Uiso 1 1 calc R . . C19 C 0.0319(9) 0.2389(4) 0.4426(7) 0.0414(18) Uani 1 1 d . . . H19 H -0.0865 0.2491 0.4505 0.050 Uiso 1 1 calc R . . C20 C 0.0439(12) 0.2052(4) 0.3154(7) 0.053(2) Uani 1 1 d . . . H20A H -0.0417 0.1688 0.2962 0.063 Uiso 1 1 calc R . . H20B H 0.1541 0.1841 0.3131 0.063 Uiso 1 1 calc R . . C21 C 0.0152(14) 0.2665(6) 0.2207(9) 0.077(3) Uani 1 1 d . . . H21A H 0.0713 0.2581 0.1441 0.093 Uiso 1 1 calc R . . H21B H -0.1042 0.2734 0.1930 0.093 Uiso 1 1 calc R . . C22 C 0.0873(14) 0.3280(5) 0.2936(9) 0.073(3) Uani 1 1 d . . . H22A H 0.0084 0.3675 0.2842 0.087 Uiso 1 1 calc R . . H22B H 0.1901 0.3428 0.2607 0.087 Uiso 1 1 calc R . . C23 C 0.1244(11) 0.3070(4) 0.4349(8) 0.053(2) Uani 1 1 d . . . H23A H 0.2444 0.3003 0.4599 0.063 Uiso 1 1 calc R . . H23B H 0.0840 0.3428 0.4911 0.063 Uiso 1 1 calc R . . C24 C -0.1352(9) 0.1095(4) 0.8197(7) 0.0389(18) Uani 1 1 d . . . H24 H -0.2371 0.1267 0.7659 0.047 Uiso 1 1 calc R . . C25 C -0.1526(14) 0.0313(5) 0.8402(10) 0.069(3) Uani 1 1 d . . . H25A H -0.2406 0.0116 0.7769 0.083 Uiso 1 1 calc R . . H25B H -0.0476 0.0070 0.8318 0.083 Uiso 1 1 calc R . . C26 C -0.1969(17) 0.0238(6) 0.9743(14) 0.110(5) Uani 1 1 d . . . H26A H -0.1024 0.0044 1.0318 0.132 Uiso 1 1 calc R . . H26B H -0.2922 -0.0081 0.9747 0.132 Uiso 1 1 calc R . . C27 C -0.2408(13) 0.0967(7) 1.0195(11) 0.085(3) Uani 1 1 d . . . H27A H -0.3582 0.1081 0.9921 0.102 Uiso 1 1 calc R . . H27B H -0.2170 0.1013 1.1138 0.102 Uiso 1 1 calc R . . C28 C -0.1275(13) 0.1418(6) 0.9523(8) 0.064(3) Uani 1 1 d . . . H28A H -0.0135 0.1406 0.9975 0.077 Uiso 1 1 calc R . . H28B H -0.1665 0.1908 0.9468 0.077 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 Zn1 0.0420(5) 0.0276(4) 0.0339(4) 0.0031(4) 0.0042(3) 0.0010(4) Zn2 0.0436(5) 0.0290(4) 0.0402(4) -0.0033(4) 0.0014(4) -0.0016(4) Zn3 0.0413(5) 0.0289(4) 0.0371(5) 0.0000(4) 0.0098(4) 0.0007(4) Zn4 0.0373(5) 0.0266(4) 0.0388(5) -0.0010(4) 0.0075(3) 0.0010(4) O1 0.033(3) 0.024(3) 0.035(3) 0.0005(19) 0.009(2) 0.0006(19) O2 0.031(3) 0.024(2) 0.026(2) -0.0067(18) 0.003(2) -0.0021(19) O3 0.038(3) 0.028(3) 0.027(2) 0.0030(19) 0.002(2) 0.000(2) O4 0.036(3) 0.026(3) 0.031(3) 0.003(2) 0.001(2) -0.003(2) C1 0.056(5) 0.041(5) 0.049(5) 0.015(4) 0.009(4) 0.003(4) C2 0.088(8) 0.051(6) 0.054(6) 0.010(4) -0.007(5) 0.002(5) C3 0.050(6) 0.072(7) 0.119(9) -0.046(7) 0.012(6) -0.009(5) C4 0.137(12) 0.122(11) 0.063(7) -0.032(7) 0.006(7) -0.062(9) C5 0.046(5) 0.035(4) 0.054(5) -0.001(4) 0.010(4) -0.001(3) C6 0.053(5) 0.050(5) 0.044(5) -0.002(4) 0.011(4) -0.005(4) C7 0.049(5) 0.037(5) 0.057(5) -0.006(4) 0.002(4) 0.008(4) C8 0.068(7) 0.062(7) 0.094(8) -0.019(6) 0.010(6) 0.007(5) C9 0.036(4) 0.019(3) 0.046(4) -0.006(3) 0.001(3) 0.008(3) C10 0.110(9) 0.028(5) 0.075(7) -0.004(4) 0.020(6) -0.001(5) C11 0.122(11) 0.039(6) 0.092(9) -0.021(5) -0.001(7) 0.026(6) C12 0.059(6) 0.058(6) 0.078(7) -0.031(5) 0.017(5) 0.001(5) C13 0.057(5) 0.059(6) 0.044(5) -0.021(4) 0.022(4) -0.008(4) C14 0.027(4) 0.041(5) 0.047(4) -0.009(4) 0.007(3) -0.003(3) C15 0.091(7) 0.048(5) 0.040(5) 0.000(4) 0.002(5) 0.000(5) C16 0.126(10) 0.067(7) 0.065(7) -0.024(6) -0.006(7) -0.029(7) C17 0.070(7) 0.045(6) 0.099(9) -0.028(6) 0.031(6) -0.018(5) C18 0.046(5) 0.033(4) 0.064(6) -0.013(4) 0.031(4) -0.007(3) C19 0.043(4) 0.042(5) 0.040(4) 0.008(4) 0.005(3) 0.008(4) C20 0.065(6) 0.061(6) 0.032(4) -0.006(4) 0.007(4) -0.004(4) C21 0.083(8) 0.096(9) 0.054(6) 0.022(6) 0.015(5) 0.002(6) C22 0.104(8) 0.055(6) 0.064(6) 0.028(5) 0.030(6) 0.019(6) C23 0.062(6) 0.033(4) 0.067(6) 0.004(4) 0.020(5) 0.002(4) C24 0.031(4) 0.039(5) 0.046(4) 0.010(3) 0.003(3) -0.004(3) C25 0.080(7) 0.046(5) 0.077(7) 0.016(5) -0.014(6) -0.022(5) C26 0.094(9) 0.081(9) 0.165(14) 0.070(9) 0.057(9) 0.030(7) C27 0.069(7) 0.098(9) 0.094(8) 0.020(8) 0.035(6) -0.008(8) C28 0.069(6) 0.082(7) 0.044(5) 0.017(5) 0.018(4) 0.014(5)