晶体表填写说明.doc

1、CIF文件填写说明data_CIF文件填写示例 （标题） _audit_creation_method SHELXL-97 产生CIF的程序名称_chemical_name_systematic化合物的系统命名; catena-(bis(m8-Oxalato)-(m3-oxalato)-bis(m2-aqua)-aqua-iron(iii)-tripotassium); _chemical_name_common 化合物的俗名_chemical_melting_point 化合物的熔点_chemical_formula_moiety 化合物的化学式 1 C6 H6 Fe K3 O15 _che

2、mical_formula_sum C6 H6 Fe K3 O15 _chemical_formula_weight 491.26 化合物的化学式量 2 loop_ _atom_type_symbol 原子散射因子参数数据来源 _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

3、0.0000 0.0000 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 Fe Fe 0.3463 0.8444 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 _symmetry_cell

4、_setting Monoclinic 晶系名称 6_symmetry_space_group_name_H-M P2(1)/c 空间群名称 7loop_ _symmetry_equiv_pos_as_xyz 晶胞中等效坐标 x, y, z -x, y+1/2, -z+1/2 -x, -y, -z x, -y-1/2, z-1/2 _cell_length_a 7.7521(6) 晶胞参数 8_cell_length_b 19.9071(15) 9_cell_length_c 10.3352(8) 10_cell_angle_alpha 90.00 11_cell_angle_beta 107

5、.7170(10) 12_cell_angle_gamma 90.00 13_cell_volume 1519.3(2) 晶胞体积 14_cell_formula_units_Z 4 晶胞包含的分子数 15_cell_measurement_temperature 273(2) 测量晶胞时的温度 4_cell_measurement_reflns_used 4257 用于确定晶胞的衍射点数_cell_measurement_theta_min 2.76 用于确定晶胞的衍射点的最小值 _cell_measurement_theta_max 28.00 用于确定晶胞的衍射点的最大值 _exptl_

6、crystal_description block 被测单晶样品的外观形状_exptl_crystal_colour colourless被测单晶样品的外观颜色_exptl_crystal_size_max 0.30 被测单晶样品的外观尺寸 3_exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? 被测单晶样品的测量密度_exptl_crystal_density_diffrn 2.148 被测单晶样品的计算密度 16_exptl_crystal_density_method

7、 not measured 测量单晶样品密度方法_exptl_crystal_F_000 980 单胞中电子数 17_exptl_absorpt_coefficient_mu 1.896 单胞的线性吸收系数 18_exptl_absorpt_correction_type multi-scan 吸收校正方法_exptl_absorpt_correction_T_min 0.59 最小透过率_exptl_absorpt_correction_T_max 0.66 最大透过率_exptl_absorpt_process_details SADABS; Bruker, 2000 吸收校正所用方法及其

8、文献 _exptl_special_details 实验细节描述; ? ; _diffrn_ambient_temperature 273(2) 衍射实验温度_diffrn_radiation_wavelength 0.71073 X射线波长 5_diffrn_radiation_type MoKa 衍射光源种类_diffrn_radiation_source sealed tube X光管类型_diffrn_radiation_monochromator graphite 单色器类型_diffrn_measurement_device_type Bruker Smart Aepex CCD

9、衍射仪型号_diffrn_measurement_method phi and omega scans 收集衍射数据的扫描方式_diffrn_standards_number ? 设置标准衍射点数_diffrn_standards_interval_count ? 标准衍射测量的间隔_diffrn_standards_decay_% ? 测量过程中衍射强度衰减百分率_diffrn_reflns_number 8209衍射实验中收集的总衍射点数 20a_diffrn_reflns_av_R_equivalents 0.0370等效点平均标准偏差 20b_diffrn_reflns_av_sigm

10、aI/netI 0.0481平均背景强度与平均衍射强度之比_diffrn_reflns_limit_h_min -9 最小与最大衍射指标范围_diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.05 结构精修时最小角 19a_diffrn_reflns_theta_max 26.00 结构精修时最大

11、角 19b_reflns_number_total 2995 独立衍射点数 21_reflns_number_gt 2227独立衍射点中强度大于2的衍射点数 22_reflns_threshold_expression 2sigma(I) _computing_data_collection SMART, (Bruker, 2000) 收集衍射数据所用程序_computing_cell_refinement SMART 精修晶胞参数所用程序_computing_data_reduction SAINT (Bruker, 2000)衍射数据还原所用程序_computing_structure_s

12、olution SHELXTL (Bruker, 2000)解析粗结构所用程序_computing_structure_refinement SHELXTL结构精修所用程序_computing_molecular_graphics SHELXTL发表论文作图所用程序_computing_publication_material SHELXTL 发表论文制作数据表格所用程序 _refine_special_details结构精修过程中一些细节的说明; Refinement of F2 against ALL reflections. The weighted R-factor wR and go

13、odness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistic

14、ally 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 基于F2的结构精修_refine_ls_matrix_type full精修矩阵类型_refine_ls_weighting_scheme calc 权重方案_refine_ls_weighting_details 权重方案表达式 calc w=1/s2(Fo2)+(0.0546P)2 where P=(Fo2+2F

15、c2)/3 _atom_sites_solution_primary direct解析粗结构的方法_atom_sites_solution_secondary difmap进一步解析结构的方法_atom_sites_solution_hydrogens geom获得氢原子的方法_refine_ls_hydrogen_treatment mixed结构精修中氢原子的处理方法_refine_ls_extinction_method none消光校正方案_refine_ls_extinction_coef 消光校正系数_refine_ls_number_reflns 2995参加结构精修的衍射点数

16、23a_refine_ls_number_parameters 244参加结构精修的参数数目 23c_refine_ls_number_restraints 0结构精修中几何限制数目 23b_refine_ls_R_factor_all 0.0641对全部衍射点的R1值 26a_refine_ls_R_factor_gt 0.0475对可观察衍射点的R1值 25a_refine_ls_wR_factor_ref 0.1071对全部衍射点的wR2值 26b_refine_ls_wR_factor_gt 0.1036对可观察衍射点的wR2值 25b_refine_ls_goodness_of_fi

17、t_ref 1.058对可观察衍射点的S值 24_refine_ls_restrained_S_all 1.058对全部衍射点的S值_refine_ls_shift/su_max 0.000最后精修过程的漂移值_refine_ls_shift/su_mean 0.000最后精修过程的平均漂移值 loop_ 结构中各原子坐标, 各向同性振动参数, 原子占有率等 _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_eq

18、uiv _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 0.2152(5) 0.44531(17) 0.5109(4) 0.0230(7) Uani 1 1 d . . . C2 C 0.0285(5) 0.41233(17) 0.5021(4) 0.0220(7) Uani 1

19、1 d . . . .H15A H 0.623(7) 0.346(3) 0.607(6) 0.054 Uiso 1 1 d . . . H15B H 0.534(7) 0.301(3) 0.514(5) 0.054 Uiso 1 1 d . . . loop_ 原子各向异性振动参数(又叫热参数或各向异性温度因子) _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_sit

20、e_aniso_U_12 C1 0.0215(16) 0.0225(18) 0.0283(19) -0.0027(15) 0.0125(15) 0.0034(14) C2 0.0222(17) 0.0236(18) 0.0228(18) -0.0045(14) 0.0107(15) 0.0004(14) .O14 0.0412(17) 0.0393(17) 0.0350(17) 0.0057(13) 0.0129(14) 0.0022(14) O15 0.0431(18) 0.0438(18) 0.0475(19) 0.0163(16) 0.0130(15) -0.0041(15) _geom

21、_special_details 分子几何中需要说明的问题; 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 cel

22、l 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_ 分子中原子间键长列表 _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom

23、_bond_publ_flag C1 O2 1.220(4) . ? C1 O1 1.293(4) . ? .O15 H15A 0.86(6) . ? O15 H15B 0.91(6) . ? loop_ 分子中原子间键角列表 _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 O2 C1

24、O1 126.4(3) . . ? O2 C1 C2 121.0(3) . . ? .K1 O15 H15B 128(3) . . ? H15A O15 H15B 99(5) . . ? loop_ 氢键列表 _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond

25、_site_symmetry_A O13 H13C O11 0.82(6) 2.47(6) 3.215(4) 153(5) 1_655 O14 H14A O6 0.80(5) 2.15(5) 2.798(5) 138(5) 1_455 _diffrn_measured_fraction_theta_max 0.999 对于最大衍射角衍射数据收集完备率_diffrn_reflns_theta_full 26.00 在结构精修中使用的最大衍射角_diffrn_measured_fraction_theta_full 0.999 整个衍射数据的完备率_refine_diff_density_max

26、0.394差值傅立叶图中最大残余电子密度峰值 27a_refine_diff_density_min -0.671差值傅立叶图中最小残余电子密度谷值 27b_refine_diff_density_rms 0.098差值傅立叶图中平均残余电子密度Table S1 Crystallographic Data for 2a, 3a3b and 4a4bCompound2achemical formulaC14H22B10NO2S3Co 1formula weight499.54 2crystal size (mm)0.180.150.12 3temperature (K)296(2) 4radiation0.71073 5crystal systemMonoclinic 6space groupP2(1)/c 7a()16.778(4) 8b()14.901(3) 9c()9.602(2) 10()90.00 11()102.633(3) 12()90.00 13V(3)2342.4(9) 14Z4 15 (calc) (g/cm3)1.416 16F (000)1016 17absorp.coeff. (mm-1)1.013 18 range (deg)1.85 to 26.0 19reflns colle