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ycheng1银虫 (正式写手)
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【求助】求帮忙节结构已有1人参与
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求好心人帮忙解结构：原料是均苯三酸，氯化铜，水，乙腈 数据间一下连接 http://g.zhubajie.com/urllink.php?id=926695794hs8s68noq2415v |
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wsyy163
银虫 (正式写手)
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溶剂分子好像不太容易处理 data_fm-3m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H Cl Cu K Li N Na O' _chemical_formula_weight 211.05 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y, x+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'y, -x+1/2, z+1/2' '-y, x+1/2, z+1/2' 'x, z+1/2, -y+1/2' '-x, z+1/2, y+1/2' '-x, -z+1/2, -y+1/2' 'x, -z+1/2, y+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' '-z, y+1/2, x+1/2' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1/2, x, -z+1/2' '-y+1/2, -x, -z+1/2' 'y+1/2, -x, z+1/2' '-y+1/2, x, z+1/2' 'x+1/2, z, -y+1/2' '-x+1/2, z, y+1/2' '-x+1/2, -z, -y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' '-z+1/2, y, x+1/2' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, -z' '-y+1/2, -x+1/2, -z' 'y+1/2, -x+1/2, z' '-y+1/2, x+1/2, z' 'x+1/2, z+1/2, -y' '-x+1/2, z+1/2, y' '-x+1/2, -z+1/2, -y' 'x+1/2, -z+1/2, y' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' '-z+1/2, y+1/2, x' '-z+1/2, -y+1/2, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' '-x, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' '-z, -x+1/2, -y+1/2' '-z, x+1/2, y+1/2' 'z, x+1/2, -y+1/2' 'z, -x+1/2, y+1/2' '-y, -z+1/2, -x+1/2' 'y, -z+1/2, x+1/2' '-y, z+1/2, x+1/2' 'y, z+1/2, -x+1/2' '-y, -x+1/2, z+1/2' 'y, x+1/2, z+1/2' '-y, x+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' '-x, -z+1/2, y+1/2' 'x, -z+1/2, -y+1/2' 'x, z+1/2, y+1/2' '-x, z+1/2, -y+1/2' '-z, -y+1/2, x+1/2' '-z, y+1/2, -x+1/2' 'z, -y+1/2, -x+1/2' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' '-z+1/2, -x, -y+1/2' '-z+1/2, x, y+1/2' 'z+1/2, x, -y+1/2' 'z+1/2, -x, y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/2, -z, x+1/2' '-y+1/2, z, x+1/2' 'y+1/2, z, -x+1/2' '-y+1/2, -x, z+1/2' 'y+1/2, x, z+1/2' '-y+1/2, x, -z+1/2' 'y+1/2, -x, -z+1/2' '-x+1/2, -z, y+1/2' 'x+1/2, -z, -y+1/2' 'x+1/2, z, y+1/2' '-x+1/2, z, -y+1/2' '-z+1/2, -y, x+1/2' '-z+1/2, y, -x+1/2' 'z+1/2, -y, -x+1/2' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-z+1/2, -x+1/2, -y' '-z+1/2, x+1/2, y' 'z+1/2, x+1/2, -y' 'z+1/2, -x+1/2, y' '-y+1/2, -z+1/2, -x' 'y+1/2, -z+1/2, x' '-y+1/2, z+1/2, x' 'y+1/2, z+1/2, -x' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' '-y+1/2, x+1/2, -z' 'y+1/2, -x+1/2, -z' '-x+1/2, -z+1/2, y' 'x+1/2, -z+1/2, -y' 'x+1/2, z+1/2, y' '-x+1/2, z+1/2, -y' '-z+1/2, -y+1/2, x' '-z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, -x' 'z+1/2, y+1/2, x' _cell_length_a 26.3339(6) _cell_length_b 26.3339(6) _cell_length_c 26.3339(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18261.9(7) _cell_formula_units_Z 228 _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 4.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 23028 _exptl_absorpt_coefficient_mu 8.853 _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 0.71073 _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 60763 _diffrn_reflns_av_R_equivalents 0.1024 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.82 _reflns_number_total 1142 _reflns_number_gt 1023 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1000P)^2^+0.0200P] 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 1142 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1350 _refine_ls_R_factor_gt 0.1274 _refine_ls_wR_factor_ref 0.3935 _refine_ls_wR_factor_gt 0.3891 _refine_ls_goodness_of_fit_ref 3.220 _refine_ls_restrained_S_all 3.220 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.017 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 Cu2 Cu 0.21454(4) 0.5000 0.28546(4) 0.0272(8) Uani 1 4 d S . 3 O1 O 0.2569(2) 0.5528(2) 0.3168(2) 0.0461(16) Uani 1 1 d . A 3 O2 O 0.1549(4) 0.5000 0.3451(4) 0.090(5) Uani 1 4 d S B 3 C3 C 0.3648(3) 0.6352(3) 0.3005(4) 0.036(2) Uani 1 2 d S A 3 H3 H 0.3797 0.6203 0.2721 0.044 Uiso 1 2 calc SR A 3 C1 C 0.2965(3) 0.5692(4) 0.2965(3) 0.037(2) Uani 1 2 d S A 3 C2 C 0.3213(3) 0.6138(4) 0.3213(3) 0.036(2) Uani 1 2 d S A 3 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 Cu2 0.0280(9) 0.0254(10) 0.0280(9) 0.000 0.0094(6) 0.000 O1 0.047(3) 0.045(3) 0.047(3) -0.014(2) 0.015(3) -0.017(3) O2 0.083(7) 0.105(13) 0.083(7) 0.000 0.039(9) 0.000 C3 0.038(3) 0.038(3) 0.033(5) -0.007(3) 0.007(3) -0.007(4) C1 0.039(3) 0.032(5) 0.039(3) -0.001(3) -0.007(4) -0.001(3) C2 0.037(3) 0.032(5) 0.037(3) -0.006(3) -0.001(4) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu2 O1 1.964(5) 72_565 ? Cu2 O1 1.964(5) . ? Cu2 O1 1.964(5) 166 ? Cu2 O1 1.964(5) 99_565 ? Cu2 O2 2.219(15) . ? Cu2 Cu2 2.641(3) 145_565 ? O1 C1 1.249(7) . ? C3 C2 1.389(7) 12_665 ? C3 C2 1.389(7) . ? C1 O1 1.250(7) 120 ? C1 C2 1.495(14) . ? C2 C3 1.389(7) 6_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu2 O1 168.0(3) 72_565 . ? O1 Cu2 O1 90.2(4) 72_565 166 ? O1 Cu2 O1 88.6(4) . 166 ? O1 Cu2 O1 88.6(4) 72_565 99_565 ? O1 Cu2 O1 90.2(4) . 99_565 ? O1 Cu2 O1 168.0(3) 166 99_565 ? O1 Cu2 O2 95.98(16) 72_565 . ? O1 Cu2 O2 95.99(16) . . ? O1 Cu2 O2 95.98(16) 166 . ? O1 Cu2 O2 95.99(16) 99_565 . ? O1 Cu2 Cu2 84.01(16) 72_565 145_565 ? O1 Cu2 Cu2 84.01(16) . 145_565 ? O1 Cu2 Cu2 84.01(16) 166 145_565 ? O1 Cu2 Cu2 84.01(16) 99_565 145_565 ? O2 Cu2 Cu2 179.992(1) . 145_565 ? C1 O1 Cu2 122.6(6) . . ? C2 C3 C2 120.9(10) 12_665 . ? O1 C1 O1 126.5(11) . 120 ? O1 C1 C2 116.7(5) . . ? O1 C1 C2 116.7(5) 120 . ? C3 C2 C3 119.1(10) 6_566 . ? C3 C2 C1 120.4(5) 6_566 . ? C3 C2 C1 120.4(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 11.576 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.330 |
2楼2010-06-13 00:47:28