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xuanshaoxie捐助贵宾 (小有名气)
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[求助]
求助精修一个晶体 已有2人参与
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求帮忙精修一个晶体（溶剂：水；盐：硝酸铅；配体H2bta（附图）），修了几天修蒙圈了。。。求路过帮忙看看。 非常感谢！！！  http://pan.baidu.com/s/1o8vpFrs  BTA.png@lich666 [ Last edited by linhua0402313 on 2016-9-1 at 09:39 ] |
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xuanshaoxie
捐助贵宾 (小有名气)
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10楼2016-09-01 08:43:28
匿名
用户注销 (知名作家)
精修问题可私信
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★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ...
感谢参与，应助指数 +1
xuanshaoxie: 金币+100, ★★★很有帮助, 谢谢 2016-09-01 17:34:12
感谢参与，应助指数 +1
xuanshaoxie: 金币+100, ★★★很有帮助, 谢谢 2016-09-01 17:34:12
 本帖仅楼主可见 |
» 本帖已获得的红花（最新10朵）
xuanshaoxie2楼2016-08-30 16:37:22
xuanshaoxie
捐助贵宾 (小有名气)
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3楼2016-08-30 17:09:20
匿名
用户注销 (知名作家)
精修问题可私信
- CMEI: 2
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- 专业: 药物分析
- 管辖: 晶体
4楼2016-08-30 19:42:47
xuanshaoxie
捐助贵宾 (小有名气)
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5楼2016-08-30 20:16:19
羊倌
至尊木虫 (正式写手)
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- 专业: 动物生理及行为学
【答案】应助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ...
感谢参与，应助指数 +1
xuanshaoxie: 金币+100, ★★★很有帮助 2016-09-01 20:01:42
感谢参与，应助指数 +1
xuanshaoxie: 金币+100, ★★★很有帮助 2016-09-01 20:01:42
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data_xb8444_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H16 Cu N18 O7 Pb' _chemical_formula_weight 699.08 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' 'Pb' 'Pb' -3.3944 10.1111 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8365(12) _cell_length_b 12.453(2) _cell_length_c 13.026(2) _cell_angle_alpha 110.877(2) _cell_angle_beta 103.778(3) _cell_angle_gamma 100.585(3) _cell_volume 961.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 9.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2831 _exptl_absorpt_correction_T_max 0.4081 _exptl_absorpt_process_details 'SADABS, Sheldrick,2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 4636 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3318 _reflns_number_gt 3030 _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^)+(0.0902P)^2^+4.8503P] 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 SHELXL _refine_ls_extinction_coef 0.0040(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3318 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 C1 C 0.7672(13) 0.4530(8) 0.7696(8) 0.0165(17) Uani 1 1 d . . . C2 C 0.7147(14) 0.4568(8) 0.9469(8) 0.0179(18) Uani 1 1 d . . . C3 C 0.4498(15) -0.0392(7) 0.6913(8) 0.0187(19) Uani 1 1 d . . . C4 C 0.2814(14) -0.0106(8) 0.5225(8) 0.0196(19) Uani 1 1 d . . . N1 N 0.6525(13) 0.3392(7) 0.7017(7) 0.0232(17) Uani 1 1 d . . . N2 N 0.6823(14) 0.3149(7) 0.5988(7) 0.0276(19) Uani 1 1 d . . . N3 N 0.8093(14) 0.4117(7) 0.6050(8) 0.0287(19) Uani 1 1 d . . . N4 N 0.8631(14) 0.5008(7) 0.7125(7) 0.0254(18) Uani 1 1 d . . . N5 N 0.7838(13) 0.5139(7) 0.8834(7) 0.0240(18) Uani 1 1 d . . . H5 H 0.8394 0.5907 0.9165 0.029 Uiso 1 1 calc R . . N6 N 0.7553(13) 0.5148(7) 1.0616(7) 0.0243(17) Uani 1 1 d . . . N7 N 0.6604(13) 0.4293(7) 1.0899(7) 0.0266(18) Uani 1 1 d . . . N8 N 0.5698(13) 0.3279(7) 0.9996(7) 0.0247(17) Uani 1 1 d . . . N9 N 0.6035(13) 0.3429(7) 0.9065(7) 0.0237(17) Uani 1 1 d . . . N10 N 0.5041(13) 0.0750(7) 0.7690(7) 0.0205(16) Uani 1 1 d . . . N11 N 0.5984(14) 0.0737(7) 0.8723(7) 0.0268(18) Uani 1 1 d . . . N12 N 0.6045(14) -0.0340(8) 0.8543(7) 0.0295(19) Uani 1 1 d . . . N13 N 0.5059(14) -0.1108(7) 0.7402(7) 0.0273(18) Uani 1 1 d . . . N14 N 0.3468(13) -0.0820(7) 0.5737(7) 0.0217(17) Uani 1 1 d . . . H14 H 0.3226 -0.1570 0.5307 0.026 Uiso 1 1 calc R . . N15 N 0.1697(13) -0.0553(7) 0.4093(7) 0.0250(18) Uani 1 1 d . . . N16 N 0.1363(14) 0.0435(8) 0.3949(7) 0.0293(19) Uani 1 1 d . . . N17 N 0.2220(14) 0.1389(8) 0.4920(7) 0.0285(19) Uani 1 1 d . . . N18 N 0.3166(13) 0.1064(7) 0.5752(7) 0.0222(17) Uani 1 1 d . . . O1 O 0.1761(13) 0.2670(9) 0.7426(9) 0.064(3) Uani 1 1 d . . . H1A H 0.1960 0.3268 0.8184 0.096 Uiso 1 1 d R . . H1B H 0.0665 0.1962 0.7249 0.096 Uiso 1 1 d R . . O2 O 0.7111(11) 0.7051(6) 0.7047(7) 0.0350(18) Uani 1 1 d . . . H2A H 0.6997 0.7854 0.7287 0.053 Uiso 1 1 d R . . H2B H 0.6495 0.6664 0.7462 0.053 Uiso 1 1 d R . . O3 O 1.0333(11) 0.7551(6) 0.9456(6) 0.0306(16) Uani 1 1 d . . . H3A H 1.1665 0.7662 0.9996 0.046 Uiso 1 1 d R . . H3C H 0.9909 0.8267 0.9720 0.046 Uiso 1 1 d R . . O4 O 1.0550(13) 0.9227(7) 0.7978(7) 0.0379(19) Uani 1 1 d . . . H4A H 0.9946 0.9314 0.7278 0.057 Uiso 1 1 d R . . H4B H 1.1955 0.9769 0.8378 0.057 Uiso 1 1 d R . . O5 O 0.9237(13) 0.6653(7) 0.5281(7) 0.0409(19) Uani 1 1 d . . . H5B H 0.9931 0.6136 0.4862 0.061 Uiso 1 1 d R . . H5C H 0.9498 0.7388 0.5183 0.061 Uiso 1 1 d R . . Pb1 Pb 1.06930(5) 0.71299(3) 0.74747(3) 0.0257(2) Uani 1 1 d . . . Cu1 Cu 0.4725(2) 0.22102(10) 0.74133(10) 0.0246(3) Uani 1 1 d . . . O6 O 0.7532(11) 0.8658(7) 1.0058(6) 0.0298(16) Uani 1 1 d . . . H6WA H 0.6656 0.8028 0.9969 0.036 Uiso 1 1 d R . . H6WB H 0.7058 0.8883 0.9535 0.036 Uiso 1 1 d R . . O7 O 0.3520(14) 0.5522(8) 0.6803(8) 0.046(2) Uani 1 1 d . . . H7WE H 0.3677 0.4873 0.6438 0.055 Uiso 1 1 d R . . H7WD H 0.3430 0.5548 0.7465 0.055 Uiso 1 1 d 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 C1 0.015(4) 0.012(4) 0.024(4) 0.007(4) 0.008(4) 0.004(3) C2 0.014(4) 0.013(4) 0.028(5) 0.008(4) 0.007(4) 0.007(3) C3 0.026(5) 0.005(4) 0.025(5) 0.004(4) 0.011(4) 0.005(3) C4 0.020(4) 0.014(4) 0.019(4) 0.002(4) 0.006(4) 0.000(3) N1 0.026(4) 0.017(4) 0.025(4) 0.006(3) 0.012(4) 0.005(3) N2 0.040(5) 0.020(4) 0.024(4) 0.009(3) 0.014(4) 0.008(4) N3 0.040(5) 0.014(4) 0.032(5) 0.009(4) 0.015(4) 0.004(4) N4 0.035(5) 0.012(4) 0.024(4) 0.004(3) 0.008(4) 0.004(3) N5 0.031(4) 0.011(4) 0.026(4) 0.004(3) 0.010(4) 0.003(3) N6 0.025(4) 0.022(4) 0.024(4) 0.008(3) 0.007(4) 0.007(3) N7 0.030(4) 0.022(4) 0.027(4) 0.008(4) 0.009(4) 0.011(4) N8 0.027(4) 0.024(4) 0.033(5) 0.017(4) 0.014(4) 0.013(3) N9 0.027(4) 0.018(4) 0.023(4) 0.007(3) 0.005(3) 0.008(3) N10 0.030(4) 0.009(4) 0.018(4) 0.004(3) 0.004(3) 0.005(3) N11 0.036(5) 0.019(4) 0.023(4) 0.009(3) 0.004(4) 0.008(4) N12 0.039(5) 0.028(5) 0.022(4) 0.011(4) 0.004(4) 0.018(4) N13 0.039(5) 0.017(4) 0.029(4) 0.011(4) 0.012(4) 0.013(4) N14 0.032(4) 0.008(4) 0.020(4) 0.004(3) 0.004(3) 0.006(3) N15 0.031(4) 0.017(4) 0.020(4) 0.003(3) 0.006(4) 0.005(3) N16 0.030(5) 0.031(5) 0.027(5) 0.014(4) 0.006(4) 0.010(4) N17 0.035(5) 0.024(4) 0.023(4) 0.012(4) 0.002(4) 0.008(4) N18 0.025(4) 0.018(4) 0.024(4) 0.011(3) 0.006(3) 0.007(3) O1 0.027(4) 0.058(6) 0.063(6) -0.019(5) 0.005(4) 0.017(4) O2 0.023(4) 0.022(4) 0.062(5) 0.013(4) 0.019(4) 0.013(3) O3 0.027(4) 0.018(3) 0.036(4) 0.004(3) 0.001(3) 0.009(3) O4 0.047(5) 0.025(4) 0.034(4) 0.012(3) -0.003(4) 0.013(3) O5 0.052(5) 0.034(4) 0.048(5) 0.016(4) 0.029(4) 0.021(4) Pb1 0.0255(3) 0.0185(3) 0.0350(3) 0.01115(18) 0.01316(18) 0.00666(16) Cu1 0.0336(7) 0.0166(6) 0.0210(6) 0.0085(5) 0.0054(5) 0.0053(5) O6 0.029(4) 0.032(4) 0.034(4) 0.018(3) 0.009(3) 0.013(3) O7 0.044(5) 0.036(5) 0.053(5) 0.016(4) 0.019(4) 0.001(4) _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 C1 N4 1.321(12) . ? C1 N1 1.332(12) . ? C1 N5 1.368(12) . ? C2 N9 1.322(12) . ? C2 N6 1.337(12) . ? C2 N5 1.377(12) . ? C3 N13 1.327(13) . ? C3 N10 1.337(11) . ? C3 N14 1.375(12) . ? C4 N18 1.316(12) . ? C4 N15 1.338(12) . ? C4 N14 1.366(12) . ? N1 N2 1.339(11) . ? N1 Cu1 2.031(8) . ? N2 N3 1.314(12) . ? N3 N4 1.351(11) . ? N4 Pb1 2.577(8) . ? N5 H5 0.8600 . ? N6 N7 1.353(12) . ? N7 N8 1.291(12) . ? N8 N9 1.355(11) . ? N9 Cu1 1.998(8) . ? N10 N11 1.354(12) . ? N10 Cu1 2.014(8) . ? N11 N12 1.287(12) . ? N12 N13 1.361(12) . ? N14 H14 0.8600 . ? N15 N16 1.360(12) . ? N16 N17 1.294(12) . ? N17 N18 1.353(12) . ? N18 Cu1 1.999(8) . ? O1 Cu1 2.207(8) . ? O1 H1A 0.9600 . ? O1 H1B 0.9600 . ? O2 Pb1 2.354(7) . ? O2 H2A 0.9600 . ? O2 H2B 0.9600 . ? O3 Pb1 2.526(8) . ? O3 H3A 0.9600 . ? O3 H3C 0.9600 . ? O4 Pb1 2.483(7) . ? O4 H4A 0.9600 . ? O4 H4B 0.9600 . ? O5 Pb1 2.593(9) . ? O5 H5B 0.9600 . ? O5 H5C 0.9600 . ? O6 H6WA 0.8467 . ? O6 H6WB 0.8433 . ? O7 H7WE 0.8199 . ? O7 H7WD 0.8692 . ? 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 N4 C1 N1 111.1(8) . . ? N4 C1 N5 123.8(8) . . ? N1 C1 N5 125.1(8) . . ? N9 C2 N6 111.7(8) . . ? N9 C2 N5 126.6(8) . . ? N6 C2 N5 121.8(8) . . ? N13 C3 N10 112.2(8) . . ? N13 C3 N14 122.0(8) . . ? N10 C3 N14 125.8(8) . . ? N18 C4 N15 112.3(9) . . ? N18 C4 N14 125.8(8) . . ? N15 C4 N14 121.9(8) . . ? C1 N1 N2 105.8(8) . . ? C1 N1 Cu1 128.8(6) . . ? N2 N1 Cu1 125.4(6) . . ? N3 N2 N1 108.8(8) . . ? N2 N3 N4 109.1(8) . . ? C1 N4 N3 105.3(7) . . ? C1 N4 Pb1 136.5(6) . . ? N3 N4 Pb1 117.6(6) . . ? C1 N5 C2 122.5(8) . . ? C1 N5 H5 118.8 . . ? C2 N5 H5 118.8 . . ? C2 N6 N7 103.4(8) . . ? N8 N7 N6 111.2(8) . . ? N7 N8 N9 108.0(8) . . ? C2 N9 N8 105.7(8) . . ? C2 N9 Cu1 128.6(7) . . ? N8 N9 Cu1 125.2(6) . . ? C3 N10 N11 104.7(7) . . ? C3 N10 Cu1 128.7(7) . . ? N11 N10 Cu1 126.4(6) . . ? N12 N11 N10 108.6(8) . . ? N11 N12 N13 111.1(8) . . ? C3 N13 N12 103.2(7) . . ? C4 N14 C3 122.8(7) . . ? C4 N14 H14 118.6 . . ? C3 N14 H14 118.6 . . ? C4 N15 N16 103.0(8) . . ? N17 N16 N15 110.9(8) . . ? N16 N17 N18 108.3(8) . . ? C4 N18 N17 105.5(8) . . ? C4 N18 Cu1 130.3(7) . . ? N17 N18 Cu1 124.2(6) . . ? Cu1 O1 H1A 109.3 . . ? Cu1 O1 H1B 109.4 . . ? H1A O1 H1B 109.5 . . ? Pb1 O2 H2A 109.3 . . ? Pb1 O2 H2B 109.0 . . ? H2A O2 H2B 109.5 . . ? Pb1 O3 H3A 109.4 . . ? Pb1 O3 H3C 109.4 . . ? H3A O3 H3C 109.5 . . ? Pb1 O4 H4A 109.4 . . ? Pb1 O4 H4B 109.1 . . ? H4A O4 H4B 109.5 . . ? Pb1 O5 H5B 109.4 . . ? Pb1 O5 H5C 109.4 . . ? H5B O5 H5C 109.5 . . ? O2 Pb1 O4 73.1(3) . . ? O2 Pb1 O3 80.2(3) . . ? O4 Pb1 O3 82.8(2) . . ? O2 Pb1 N4 73.1(3) . . ? O4 Pb1 N4 144.1(3) . . ? O3 Pb1 N4 79.8(2) . . ? O2 Pb1 O5 73.0(3) . . ? O4 Pb1 O5 89.8(2) . . ? O3 Pb1 O5 153.2(3) . . ? N4 Pb1 O5 91.8(3) . . ? N9 Cu1 N18 174.1(3) . . ? N9 Cu1 N10 97.7(3) . . ? N18 Cu1 N10 86.2(3) . . ? N9 Cu1 N1 86.2(3) . . ? N18 Cu1 N1 94.4(3) . . ? N10 Cu1 N1 134.1(3) . . ? N9 Cu1 O1 88.1(3) . . ? N18 Cu1 O1 86.1(3) . . ? N10 Cu1 O1 117.6(4) . . ? N1 Cu1 O1 108.2(4) . . ? H6WA O6 H6WB 110.3 . . ? H7WE O7 H7WD 108.7 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 6.150 _refine_diff_density_min -1.974 _refine_diff_density_rms 0.252 |
6楼2016-08-30 22:18:59
羊倌
至尊木虫 (正式写手)
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【答案】应助回帖
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data_xb8444_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H16 Cu N18 O7 Pb' _chemical_formula_weight 699.08 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' 'Pb' 'Pb' -3.3944 10.1111 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8365(12) _cell_length_b 12.453(2) _cell_length_c 13.026(2) _cell_angle_alpha 110.877(2) _cell_angle_beta 103.778(3) _cell_angle_gamma 100.585(3) _cell_volume 961.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 9.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2831 _exptl_absorpt_correction_T_max 0.4081 _exptl_absorpt_process_details 'SADABS, Sheldrick,2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 4636 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3318 _reflns_number_gt 3030 _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^)+(0.0902P)^2^+4.8503P] 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 SHELXL _refine_ls_extinction_coef 0.0040(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3318 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 C1 C 0.7672(13) 0.4530(8) 0.7696(8) 0.0165(17) Uani 1 1 d . . . C2 C 0.7147(14) 0.4568(8) 0.9469(8) 0.0179(18) Uani 1 1 d . . . C3 C 0.4498(15) -0.0392(7) 0.6913(8) 0.0187(19) Uani 1 1 d . . . C4 C 0.2814(14) -0.0106(8) 0.5225(8) 0.0196(19) Uani 1 1 d . . . N1 N 0.6525(13) 0.3392(7) 0.7017(7) 0.0232(17) Uani 1 1 d . . . N2 N 0.6823(14) 0.3149(7) 0.5988(7) 0.0276(19) Uani 1 1 d . . . N3 N 0.8093(14) 0.4117(7) 0.6050(8) 0.0287(19) Uani 1 1 d . . . N4 N 0.8631(14) 0.5008(7) 0.7125(7) 0.0254(18) Uani 1 1 d . . . N5 N 0.7838(13) 0.5139(7) 0.8834(7) 0.0240(18) Uani 1 1 d . . . H5 H 0.8394 0.5907 0.9165 0.029 Uiso 1 1 calc R . . N6 N 0.7553(13) 0.5148(7) 1.0616(7) 0.0243(17) Uani 1 1 d . . . N7 N 0.6604(13) 0.4293(7) 1.0899(7) 0.0266(18) Uani 1 1 d . . . N8 N 0.5698(13) 0.3279(7) 0.9996(7) 0.0247(17) Uani 1 1 d . . . N9 N 0.6035(13) 0.3429(7) 0.9065(7) 0.0237(17) Uani 1 1 d . . . N10 N 0.5041(13) 0.0750(7) 0.7690(7) 0.0205(16) Uani 1 1 d . . . N11 N 0.5984(14) 0.0737(7) 0.8723(7) 0.0268(18) Uani 1 1 d . . . N12 N 0.6045(14) -0.0340(8) 0.8543(7) 0.0295(19) Uani 1 1 d . . . N13 N 0.5059(14) -0.1108(7) 0.7402(7) 0.0273(18) Uani 1 1 d . . . N14 N 0.3468(13) -0.0820(7) 0.5737(7) 0.0217(17) Uani 1 1 d . . . H14 H 0.3226 -0.1570 0.5307 0.026 Uiso 1 1 calc R . . N15 N 0.1697(13) -0.0553(7) 0.4093(7) 0.0250(18) Uani 1 1 d . . . N16 N 0.1363(14) 0.0435(8) 0.3949(7) 0.0293(19) Uani 1 1 d . . . N17 N 0.2220(14) 0.1389(8) 0.4920(7) 0.0285(19) Uani 1 1 d . . . N18 N 0.3166(13) 0.1064(7) 0.5752(7) 0.0222(17) Uani 1 1 d . . . O1 O 0.1761(13) 0.2670(9) 0.7426(9) 0.064(3) Uani 1 1 d . . . H1A H 0.1960 0.3268 0.8184 0.096 Uiso 1 1 d R . . H1B H 0.0665 0.1962 0.7249 0.096 Uiso 1 1 d R . . O2 O 0.7111(11) 0.7051(6) 0.7047(7) 0.0350(18) Uani 1 1 d . . . H2A H 0.6997 0.7854 0.7287 0.053 Uiso 1 1 d R . . H2B H 0.6495 0.6664 0.7462 0.053 Uiso 1 1 d R . . O3 O 1.0333(11) 0.7551(6) 0.9456(6) 0.0306(16) Uani 1 1 d . . . H3A H 1.1665 0.7662 0.9996 0.046 Uiso 1 1 d R . . H3C H 0.9909 0.8267 0.9720 0.046 Uiso 1 1 d R . . O4 O 1.0550(13) 0.9227(7) 0.7978(7) 0.0379(19) Uani 1 1 d . . . H4A H 0.9946 0.9314 0.7278 0.057 Uiso 1 1 d R . . H4B H 1.1955 0.9769 0.8378 0.057 Uiso 1 1 d R . . O5 O 0.9237(13) 0.6653(7) 0.5281(7) 0.0409(19) Uani 1 1 d . . . H5B H 0.9931 0.6136 0.4862 0.061 Uiso 1 1 d R . . H5C H 0.9498 0.7388 0.5183 0.061 Uiso 1 1 d R . . Pb1 Pb 1.06930(5) 0.71299(3) 0.74747(3) 0.0257(2) Uani 1 1 d . . . Cu1 Cu 0.4725(2) 0.22102(10) 0.74133(10) 0.0246(3) Uani 1 1 d . . . O6 O 0.7532(11) 0.8658(7) 1.0058(6) 0.0298(16) Uani 1 1 d . . . H6WA H 0.6656 0.8028 0.9969 0.036 Uiso 1 1 d R . . H6WB H 0.7058 0.8883 0.9535 0.036 Uiso 1 1 d R . . O7 O 0.3520(14) 0.5522(8) 0.6803(8) 0.046(2) Uani 1 1 d . . . H7WE H 0.3677 0.4873 0.6438 0.055 Uiso 1 1 d R . . H7WD H 0.3430 0.5548 0.7465 0.055 Uiso 1 1 d 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 C1 0.015(4) 0.012(4) 0.024(4) 0.007(4) 0.008(4) 0.004(3) C2 0.014(4) 0.013(4) 0.028(5) 0.008(4) 0.007(4) 0.007(3) C3 0.026(5) 0.005(4) 0.025(5) 0.004(4) 0.011(4) 0.005(3) C4 0.020(4) 0.014(4) 0.019(4) 0.002(4) 0.006(4) 0.000(3) N1 0.026(4) 0.017(4) 0.025(4) 0.006(3) 0.012(4) 0.005(3) N2 0.040(5) 0.020(4) 0.024(4) 0.009(3) 0.014(4) 0.008(4) N3 0.040(5) 0.014(4) 0.032(5) 0.009(4) 0.015(4) 0.004(4) N4 0.035(5) 0.012(4) 0.024(4) 0.004(3) 0.008(4) 0.004(3) N5 0.031(4) 0.011(4) 0.026(4) 0.004(3) 0.010(4) 0.003(3) N6 0.025(4) 0.022(4) 0.024(4) 0.008(3) 0.007(4) 0.007(3) N7 0.030(4) 0.022(4) 0.027(4) 0.008(4) 0.009(4) 0.011(4) N8 0.027(4) 0.024(4) 0.033(5) 0.017(4) 0.014(4) 0.013(3) N9 0.027(4) 0.018(4) 0.023(4) 0.007(3) 0.005(3) 0.008(3) N10 0.030(4) 0.009(4) 0.018(4) 0.004(3) 0.004(3) 0.005(3) N11 0.036(5) 0.019(4) 0.023(4) 0.009(3) 0.004(4) 0.008(4) N12 0.039(5) 0.028(5) 0.022(4) 0.011(4) 0.004(4) 0.018(4) N13 0.039(5) 0.017(4) 0.029(4) 0.011(4) 0.012(4) 0.013(4) N14 0.032(4) 0.008(4) 0.020(4) 0.004(3) 0.004(3) 0.006(3) N15 0.031(4) 0.017(4) 0.020(4) 0.003(3) 0.006(4) 0.005(3) N16 0.030(5) 0.031(5) 0.027(5) 0.014(4) 0.006(4) 0.010(4) N17 0.035(5) 0.024(4) 0.023(4) 0.012(4) 0.002(4) 0.008(4) N18 0.025(4) 0.018(4) 0.024(4) 0.011(3) 0.006(3) 0.007(3) O1 0.027(4) 0.058(6) 0.063(6) -0.019(5) 0.005(4) 0.017(4) O2 0.023(4) 0.022(4) 0.062(5) 0.013(4) 0.019(4) 0.013(3) O3 0.027(4) 0.018(3) 0.036(4) 0.004(3) 0.001(3) 0.009(3) O4 0.047(5) 0.025(4) 0.034(4) 0.012(3) -0.003(4) 0.013(3) O5 0.052(5) 0.034(4) 0.048(5) 0.016(4) 0.029(4) 0.021(4) Pb1 0.0255(3) 0.0185(3) 0.0350(3) 0.01115(18) 0.01316(18) 0.00666(16) Cu1 0.0336(7) 0.0166(6) 0.0210(6) 0.0085(5) 0.0054(5) 0.0053(5) O6 0.029(4) 0.032(4) 0.034(4) 0.018(3) 0.009(3) 0.013(3) O7 0.044(5) 0.036(5) 0.053(5) 0.016(4) 0.019(4) 0.001(4) _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 C1 N4 1.321(12) . ? C1 N1 1.332(12) . ? C1 N5 1.368(12) . ? C2 N9 1.322(12) . ? C2 N6 1.337(12) . ? C2 N5 1.377(12) . ? C3 N13 1.327(13) . ? C3 N10 1.337(11) . ? C3 N14 1.375(12) . ? C4 N18 1.316(12) . ? C4 N15 1.338(12) . ? C4 N14 1.366(12) . ? N1 N2 1.339(11) . ? N1 Cu1 2.031(8) . ? N2 N3 1.314(12) . ? N3 N4 1.351(11) . ? N4 Pb1 2.577(8) . ? N5 H5 0.8600 . ? N6 N7 1.353(12) . ? N7 N8 1.291(12) . ? N8 N9 1.355(11) . ? N9 Cu1 1.998(8) . ? N10 N11 1.354(12) . ? N10 Cu1 2.014(8) . ? N11 N12 1.287(12) . ? N12 N13 1.361(12) . ? N14 H14 0.8600 . ? N15 N16 1.360(12) . ? N16 N17 1.294(12) . ? N17 N18 1.353(12) . ? N18 Cu1 1.999(8) . ? O1 Cu1 2.207(8) . ? O1 H1A 0.9600 . ? O1 H1B 0.9600 . ? O2 Pb1 2.354(7) . ? O2 H2A 0.9600 . ? O2 H2B 0.9600 . ? O3 Pb1 2.526(8) . ? O3 H3A 0.9600 . ? O3 H3C 0.9600 . ? O4 Pb1 2.483(7) . ? O4 H4A 0.9600 . ? O4 H4B 0.9600 . ? O5 Pb1 2.593(9) . ? O5 H5B 0.9600 . ? O5 H5C 0.9600 . ? O6 H6WA 0.8467 . ? O6 H6WB 0.8433 . ? O7 H7WE 0.8199 . ? O7 H7WD 0.8692 . ? 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 N4 C1 N1 111.1(8) . . ? N4 C1 N5 123.8(8) . . ? N1 C1 N5 125.1(8) . . ? N9 C2 N6 111.7(8) . . ? N9 C2 N5 126.6(8) . . ? N6 C2 N5 121.8(8) . . ? N13 C3 N10 112.2(8) . . ? N13 C3 N14 122.0(8) . . ? N10 C3 N14 125.8(8) . . ? N18 C4 N15 112.3(9) . . ? N18 C4 N14 125.8(8) . . ? N15 C4 N14 121.9(8) . . ? C1 N1 N2 105.8(8) . . ? C1 N1 Cu1 128.8(6) . . ? N2 N1 Cu1 125.4(6) . . ? N3 N2 N1 108.8(8) . . ? N2 N3 N4 109.1(8) . . ? C1 N4 N3 105.3(7) . . ? C1 N4 Pb1 136.5(6) . . ? N3 N4 Pb1 117.6(6) . . ? C1 N5 C2 122.5(8) . . ? C1 N5 H5 118.8 . . ? C2 N5 H5 118.8 . . ? C2 N6 N7 103.4(8) . . ? N8 N7 N6 111.2(8) . . ? N7 N8 N9 108.0(8) . . ? C2 N9 N8 105.7(8) . . ? C2 N9 Cu1 128.6(7) . . ? N8 N9 Cu1 125.2(6) . . ? C3 N10 N11 104.7(7) . . ? C3 N10 Cu1 128.7(7) . . ? N11 N10 Cu1 126.4(6) . . ? N12 N11 N10 108.6(8) . . ? N11 N12 N13 111.1(8) . . ? C3 N13 N12 103.2(7) . . ? C4 N14 C3 122.8(7) . . ? C4 N14 H14 118.6 . . ? C3 N14 H14 118.6 . . ? C4 N15 N16 103.0(8) . . ? N17 N16 N15 110.9(8) . . ? N16 N17 N18 108.3(8) . . ? C4 N18 N17 105.5(8) . . ? C4 N18 Cu1 130.3(7) . . ? N17 N18 Cu1 124.2(6) . . ? Cu1 O1 H1A 109.3 . . ? Cu1 O1 H1B 109.4 . . ? H1A O1 H1B 109.5 . . ? Pb1 O2 H2A 109.3 . . ? Pb1 O2 H2B 109.0 . . ? H2A O2 H2B 109.5 . . ? Pb1 O3 H3A 109.4 . . ? Pb1 O3 H3C 109.4 . . ? H3A O3 H3C 109.5 . . ? Pb1 O4 H4A 109.4 . . ? Pb1 O4 H4B 109.1 . . ? H4A O4 H4B 109.5 . . ? Pb1 O5 H5B 109.4 . . ? Pb1 O5 H5C 109.4 . . ? H5B O5 H5C 109.5 . . ? O2 Pb1 O4 73.1(3) . . ? O2 Pb1 O3 80.2(3) . . ? O4 Pb1 O3 82.8(2) . . ? O2 Pb1 N4 73.1(3) . . ? O4 Pb1 N4 144.1(3) . . ? O3 Pb1 N4 79.8(2) . . ? O2 Pb1 O5 73.0(3) . . ? O4 Pb1 O5 89.8(2) . . ? O3 Pb1 O5 153.2(3) . . ? N4 Pb1 O5 91.8(3) . . ? N9 Cu1 N18 174.1(3) . . ? N9 Cu1 N10 97.7(3) . . ? N18 Cu1 N10 86.2(3) . . ? N9 Cu1 N1 86.2(3) . . ? N18 Cu1 N1 94.4(3) . . ? N10 Cu1 N1 134.1(3) . . ? N9 Cu1 O1 88.1(3) . . ? N18 Cu1 O1 86.1(3) . . ? N10 Cu1 O1 117.6(4) . . ? N1 Cu1 O1 108.2(4) . . ? H6WA O6 H6WB 110.3 . . ? H7WE O7 H7WD 108.7 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 6.150 _refine_diff_density_min -1.974 _refine_diff_density_rms 0.252 |
7楼2016-08-30 22:19:16
羊倌
至尊木虫 (正式写手)
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【答案】应助回帖
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PLAT183_ALERT_1_A Missing _cell_measurement_reflns_used value .... Please Do ! PLAT184_ALERT_1_A Missing _cell_measurement_theta_min value ...... Please Do ! PLAT185_ALERT_1_A Missing _cell_measurement_theta_max value ...... Please Do ! --------------------------------------------------------------------------------Alert level C DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75 _refine_diff_density_max given = 6.150 Test value = 6.150 DIFMX02_ALERT_1_C The maximum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full value Low . 0.979 Note PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.12 Report -------------------------------------------------------------------------------- |
8楼2016-08-30 22:20:14
xuanshaoxie
捐助贵宾 (小有名气)
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9楼2016-08-31 09:07:25