CIF文件详解.doc

1、1data_NJU_audit_creation_method SHELXL-97 产生 CIF 的程序名称_chemical_name_systematic 化合物的系统命名; ? ; _chemical_name_common ? 化合物的俗名_chemical_melting_point ? 化合物的熔点_chemical_formula_moiety C15 H13 N3 O 化合物的化学式_chemical_formula_sum C15 H13 N3 O _chemical_formula_weight 251.28 化合物的化学式量loop_ _atom_type_symbol

2、构成化合物的原子散射因子来源_atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 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 0.0000 International

3、Tables Vol C Tables 4.2.6.8 and 6.1.1.4 O O 0.0106 0.0000 International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 _symmetry_cell_setting Triclinic 晶系名称_symmetry_space_group_name_H-M Pc 空间群名称loop_ _symmetry_equiv_pos_as_xyz x, y, z x, -y, z+1/2 晶胞中等效坐标_cell_length_a 12.608(8) 晶胞参数_cell_length_b 11.023(

4、7) _cell_length_c 10.044(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.94(3) _cell_angle_gamma 90.00 2_cell_volume 1342.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) 测量晶胞时的温度_cell_measurement_reflns_used 940 用于确定晶胞的衍射点数 _cell_measurement_theta_min 2.50 用于确定晶胞的衍射点的最小 值 _cell_me

5、asurement_theta_max 20.48 用于确定晶胞的衍射点的最大 值 _exptl_crystal_description block 被测单晶的外观形状_exptl_crystal_colour colourless 被测单晶的外观颜色_exptl_crystal_size_max 0.30 被测单晶的外观尺寸_exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? 被测单晶的测量密度_exptl_crystal_density_diffrn 1.244 被测单

6、晶的计算密度_exptl_crystal_density_method not measured 测量单晶密度方法_exptl_crystal_F_000 528 单胞中电子数_exptl_absorpt_coefficient_mu 0.081 单胞的线性吸收系数_exptl_absorpt_correction_type multi-scan 吸收校正方法 ）_exptl_absorpt_correction_T_min 0.98 最小透过率_exptl_absorpt_correction_T_max 0.98 最大透过率_exptl_absorpt_process_details SA

7、DABS; Bruker, 2000 吸收校正所用方法及其文献_exptl_special_details; ? （实验细节描述）; _diffrn_ambient_temperature 291(2) 衍射实验时温度_diffrn_radiation_wavelength 0.71073 衍射线波长 _diffrn_radiation_type MoKa 衍射光源_diffrn_radiation_source sealed tube X-光管类型_diffrn_radiation_monochromator graphite 单色器类型_diffrn_measurement_device_

8、type Bruker Smart Apex CCD area detector 衍射仪型号_diffrn_measurement_method phi and omega scans 收集衍射数据的方式_diffrn_detector_area_resol_mean ? _diffrn_standards_number ? 设置标准衍射点数_diffrn_standards_interval_count ? 标准衍射测量衍射点间隔_diffrn_standards_interval_time ? 标准衍射测量时间间隔_diffrn_standards_decay_% ? 测量过程中是否有衰减

9、_diffrn_reflns_number 11645 总衍射点数_diffrn_reflns_av_R_equivalents 0.0437 等效点平均标准误差_diffrn_reflns_av_sigmaI/netI 0.0321 平均背景强度与平均衍射强度之比_diffrn_reflns_limit_h_min -16 衍射指标范围_diffrn_reflns_limit_h_max 16 3_diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn

10、_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.68 结构精修时最小 角_diffrn_reflns_theta_max 27.74 结构精修时最大 角_reflns_number_total 3110 独立衍射点数_reflns_number_gt 2784 独立衍射点中强度大于 2 的衍射点数_reflns_threshold_expression 2sigma(I) _computing_data_collection SMART (Bruker, 2000) 收集衍射数据所用程序_computing_cell_refinement S

11、MART 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_solution 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_

12、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 goodness 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

13、 is not relevant to the choice of reflections for refinement. R-factors based on F2 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 基于 F2 的结构精修_refine_ls_matrix_type full 精修矩阵类型_refine_ls_weight

14、ing_scheme calc 权重方案_refine_ls_weighting_details 权重方案表达式calc w=1/s2(Fo2)+(0.05P)2+0.88P where P=(Fo2+2Fc2)/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_refin

15、e_ls_extinction_method none 消光校正方案_refine_ls_extinction_coef ? 消光校正系数_refine_ls_abs_structure_details 处理绝对构型方法和参考文献Flack H D (1983), Acta Cryst. A39, 876-881 _refine_ls_abs_structure_Flack 10(10) 绝对构型参数_refine_ls_number_reflns 3110 参加结构精修的衍射点数4_refine_ls_number_parameters 349 参加结构精修的参数数目_refine_ls_n

16、umber_restraints 2 结构精修中几何限制数目_refine_ls_R_factor_all 0.0675 对全部衍射点的 R1 值_refine_ls_R_factor_gt 0.0593 对可观察衍射点的 R1 值_refine_ls_wR_factor_ref 0.1338 对全部衍射点的 wR2 值_refine_ls_wR_factor_gt 0.1302 对可观察衍射点的 wR2 值_refine_ls_goodness_of_fit_ref 1.012 对可观察衍射点的 S 值_refine_ls_restrained_S_all 1.011 对全部衍射点的 S 值

17、_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_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_

18、multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.2011(4) 0.4816(5) 0.8674(5) 0.0472(10) Uani 1 1 d . . . H1 H 1.2238 0.5562 0.8420 0.057 Uiso 1 1 calc R . . C2 C 1.2551(4) 0.4303(4) 0.9917(5) 0.0457(10) Uani 1 1 d . . . H2 H

19、1.3139 0.4716 1.0505 0.055 Uiso 1 1 calc R . . C3 C 1.2239(4) 0.3174(4) 1.0323(5) 0.0417(9) Uani 1 1 d . . . H3 H 1.2609 0.2838 1.1173 0.050 Uiso 1 1 calc R . . C4 C 1.1362(4) 0.2566(4) 0.9422(4) 0.0418(10) Uani 1 1 d . . . H4 H 1.1148 0.1809 0.9666 0.050 Uiso 1 1 calc R . . C5 C 1.0805(4) 0.3081(5)

20、 0.8167(4) 0.0469(11) Uani 1 1 d . . . H5 H 1.0219 0.2672 0.7571 0.056 Uiso 1 1 calc R . . C6 C 1.1126(3) 0.4217(4) 0.7798(5) 0.0421(9) Uani 1 1 d . . . C7 C 1.0508(3) 0.4875(4) 0.6585(5) 0.0426(10) Uani 1 1 d . . . H7 H 1.0694 0.5672 0.6446 0.051 Uiso 1 1 calc R . . C8 C 0.9646(4) 0.4321(4) 0.5637(

21、5) 0.0436(10) Uani 1 1 d . . . H8 H 0.9451 0.3521 0.5747 0.052 Uiso 1 1 calc R . . C9 C 0.9049(4) 0.5050(4) 0.4446(4) 0.0435(10) Uani 1 1 d . . . H9 H 0.9175 0.5870 0.4333 0.052 Uiso 1 1 calc R . . C10 C 0.6810(4) 0.4686(4) 0.1451(4) 0.0391(9) Uani 1 1 d . . . 5C11 C 0.5998(4) 0.5425(4) 0.0516(4) 0.

22、0438(10) Uani 1 1 d . . . C12 C 0.5471(3) 0.5017(4) -0.0823(4) 0.0356(8) Uani 1 1 d . . . H12 H 0.5587 0.4233 -0.1093 0.043 Uiso 1 1 calc R . . C13 C 0.4793(4) 0.5778(4) -0.1716(5) 0.0413(9) Uani 1 1 d . . . H13 H 0.4438 0.5497 -0.2599 0.050 Uiso 1 1 calc R . . C14 C 0.5136(4) 0.7372(4) -0.0082(4) 0

23、.0427(9) Uani 1 1 d . . . H14 H 0.5025 0.8165 0.0165 0.051 Uiso 1 1 calc R . . C15 C 0.5845(3) 0.6620(4) 0.0872(4) 0.0432(10) Uani 1 1 d . . . H15 H 0.6216 0.6914 0.1743 0.052 Uiso 1 1 calc R . . C16 C 0.4052(4) 0.0511(4) -0.2985(4) 0.0424(9) Uani 1 1 d . . . H16 H 0.4482 -0.0181 -0.2728 0.051 Uiso

24、1 1 calc R . . C17 C 0.3238(3) 0.0544(4) -0.4232(4) 0.0400(9) Uani 1 1 d . . . H17 H 0.3127 -0.0128 -0.4814 0.048 Uiso 1 1 calc R . . C18 C 0.2588(4) 0.1560(4) -0.4623(5) 0.0455(10) Uani 1 1 d . . . H18 H 0.2039 0.1569 -0.5459 0.055 Uiso 1 1 calc R . . C19 C 0.2761(4) 0.2580(4) -0.3752(4) 0.0417(9)

25、Uani 1 1 d . . . H19 H 0.2328 0.3269 -0.4015 0.050 Uiso 1 1 calc R . . C20 C 0.3577(3) 0.2565(4) -0.2498(4) 0.0356(8) Uani 1 1 d . . . H20 H 0.3689 0.3242 -0.1923 0.043 Uiso 1 1 calc R . . C21 C 0.4226(4) 0.1536(4) -0.2104(4) 0.0462(10) Uani 1 1 d . . . C22 C 0.5026(4) 0.1586(4) -0.0775(5) 0.0462(10

26、) Uani 1 1 d . . . H22 H 0.5019 0.2227 -0.0175 0.055 Uiso 1 1 calc R . . C23 C 0.5807(4) 0.0677(4) -0.0391(4) 0.0433(10) Uani 1 1 d . . . H23 H 0.5931 0.0067 -0.0970 0.052 Uiso 1 1 calc R . . C24 C 0.6411(3) 0.0828(4) 0.1081(4) 0.0398(9) Uani 1 1 d . . . H24 H 0.6423 0.1533 0.1594 0.048 Uiso 1 1 cal

27、c R . . C25 C 0.8300(4) -0.1108(5) 0.3489(5) 0.0502(11) Uani 1 1 d . . . C26 C 0.8954(4) -0.0909(4) 0.4904(5) 0.0441(10) Uani 1 1 d . . . C27 C 0.9750(4) -0.0014(4) 0.5288(5) 0.0405(9) Uani 1 1 d . . . H27 H 0.9822 0.0570 0.4650 0.049 Uiso 1 1 calc R . . C28 C 1.0442(4) 0.0012(5) 0.6632(5) 0.0505(11

28、) Uani 1 1 d . . . H28 H 1.0965 0.0623 0.6904 0.061 Uiso 1 1 calc R . . C29 C 0.9555(3) -0.1774(4) 0.7183(4) 0.0421(9) Uani 1 1 d . . . H29 H 0.9483 -0.2360 0.7819 0.051 Uiso 1 1 calc R . . C30 C 0.8865(3) -0.1796(3) 0.5848(4) 0.0337(8) Uani 1 1 d . . . H30 H 0.8341 -0.2407 0.5582 0.040 Uiso 1 1 cal

29、c R . . N1 N 0.8334(3) 0.4414(3) 0.3586(4) 0.0397(8) Uani 1 1 d . . . N2 N 0.7663(3) 0.5206(4) 0.2548(4) 0.0423(9) Uani 1 1 d . . . H2A H 0.777(4) 0.598(5) 0.259(5) 0.051 Uiso 1 1 d . . . N3 N 0.4603(3) 0.6964(3) -0.1372(3) 0.0392(8) Uani 1 1 d . . . N4 N 0.6918(3) -0.0162(3) 0.1548(4) 0.0424(8) Uan

30、i 1 1 d . . . N5 N 0.7800(3) -0.0023(3) 0.2797(3) 0.0368(8) Uani 1 1 d . . . H5A H 0.833(4) 0.042(4) 0.259(5) 0.044 Uiso 1 1 d . . . N6 N 1.0342(3) -0.0891(4) 0.7569(4) 0.0491(9) Uani 1 1 d . . . 6O1 O 0.6774(2) 0.3578(3) 0.1322(3) 0.0434(7) Uani 1 1 d . . . O2 O 0.8172(2) -0.2090(3) 0.2914(3) 0.044

31、0(7) Uani 1 1 d . . . loop_ 原子各向异性振动参数_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 0.042(2) 0.052(3) 0.051(3) 0.004(2) 0.019(2) -0.006(2) C2 0.042(2) 0.048(2) 0.049(3) -0.011(2) 0.017(2)

32、-0.0034(19) C3 0.043(2) 0.044(2) 0.043(2) -0.0022(18) 0.0214(19) 0.0020(18) C4 0.048(2) 0.042(2) 0.042(2) 0.0100(17) 0.0227(19) -0.0146(18) C5 0.037(2) 0.071(3) 0.035(2) -0.010(2) 0.0134(17) -0.014(2) C6 0.0332(18) 0.050(2) 0.046(2) -0.0088(19) 0.0149(17) 0.0070(18) C7 0.037(2) 0.043(2) 0.054(3) -0.

33、014(2) 0.0238(19) 0.0071(18) C8 0.040(2) 0.041(2) 0.053(3) 0.0057(19) 0.0167(19) 0.0142(18) C9 0.051(2) 0.050(2) 0.0264(19) -0.0123(18) 0.0053(17) 0.003(2) C10 0.044(2) 0.036(2) 0.040(2) 0.0063(17) 0.0151(17) -0.0233(18) C11 0.054(3) 0.041(2) 0.038(2) -0.0013(18) 0.0163(19) -0.006(2) C12 0.0331(19)

34、0.038(2) 0.043(2) -0.0088(16) 0.0221(16) 0.0074(16) C13 0.042(2) 0.046(2) 0.040(2) -0.0042(18) 0.0172(18) -0.0041(19) C14 0.048(2) 0.042(2) 0.037(2) -0.0103(18) 0.0103(18) -0.0053(19) C15 0.041(2) 0.056(3) 0.032(2) -0.0133(18) 0.0092(17) -0.0076(19) C16 0.051(2) 0.045(2) 0.031(2) 0.0038(17) 0.0121(1

35、7) -0.005(2) C17 0.036(2) 0.046(2) 0.036(2) -0.0079(17) 0.0074(17) -0.0121(17) C18 0.047(2) 0.047(2) 0.043(2) -0.013(2) 0.0108(19) -0.0120(19) C19 0.049(2) 0.043(2) 0.034(2) -0.0051(17) 0.0128(18) -0.0036(19) C20 0.0386(19) 0.036(2) 0.037(2) 0.0037(16) 0.0175(16) -0.0144(16) C21 0.055(3) 0.051(3) 0.

36、037(2) 0.0099(19) 0.0198(19) -0.004(2) C22 0.046(2) 0.044(2) 0.051(3) -0.0061(19) 0.018(2) 0.0147(19) C23 0.044(2) 0.045(2) 0.040(2) -0.0135(18) 0.0095(18) 0.0018(19) C24 0.0314(18) 0.052(2) 0.037(2) -0.0110(18) 0.0113(16) -0.0043(17) C25 0.050(2) 0.052(3) 0.054(3) 0.003(2) 0.022(2) 0.013(2) C26 0.0

37、47(2) 0.045(2) 0.049(3) 0.005(2) 0.028(2) 0.003(2) C27 0.038(2) 0.046(2) 0.044(2) 0.0012(18) 0.0225(18) 0.0001(17) C28 0.050(2) 0.063(3) 0.038(2) -0.009(2) 0.0126(19) -0.011(2) C29 0.040(2) 0.047(2) 0.044(2) -0.0077(18) 0.0202(18) 0.0067(18) C30 0.0285(16) 0.0339(19) 0.044(2) -0.0027(16) 0.0190(15)

38、0.0102(14) N1 0.0374(17) 0.0327(17) 0.0451(19) 0.0001(14) 0.0045(14) -0.0052(14) N2 0.0305(17) 0.045(2) 0.0435(19) 0.0138(16) -0.0034(14) -0.0151(15) N3 0.0488(19) 0.0410(19) 0.0321(17) 0.0002(15) 0.0182(14) 0.0031(16) 7N4 0.055(2) 0.0406(19) 0.0303(17) -0.0039(15) 0.0093(16) -0.0081(17) N5 0.0338(1

39、7) 0.0399(18) 0.0350(18) -0.0011(14) 0.0064(14) -0.0151(14) N6 0.043(2) 0.062(2) 0.049(2) -0.0041(19) 0.0230(17) -0.0020(18) O1 0.0396(15) 0.0449(17) 0.0474(17) -0.0059(13) 0.0152(13) -0.0096(13) O2 0.0434(15) 0.0455(17) 0.0413(16) 0.0034(14) 0.0084(12) 0.0001(13) _geom_special_details 分子几何中需要说明的问题;

40、 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 whe

41、n 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 分子中原子间键长列表_geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.369(7)

42、. ? C1 C6 1.385(7) . ? C1 H1 0.9300 . ? C2 C3 1.400(6) . ? C2 H2 0.9300 . ? C3 C4 1.394(6) . ? C3 H3 0.9300 . ? C4 C5 1.386(6) . ? C4 H4 0.9300 . ? C5 C6 1.397(7) . ? C5 H5 0.9300 . ? C6 C7 1.447(7) . ? C7 C8 1.375(7) . ? C7 H7 0.9300 . ? C8 C9 1.467(6) . ? C8 H8 0.9300 . ? C9 N1 1.273(5) . ? C9 H9

43、0.9300 . ? C10 O1 1.228(5) . ? C10 N2 1.432(5) . ? C10 C11 1.437(6) . ? C11 C15 1.393(6) . ? 8C11 C12 1.400(6) . ? C12 C13 1.347(6) . ? C12 H12 0.9300 . ? C13 N3 1.390(6) . ? C13 H13 0.9300 . ? C14 N3 1.362(5) . ? C14 C15 1.390(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.385(6) . ? C16 C2

44、1 1.415(7) . ? C16 H16 0.9300 . ? C17 C18 1.379(7) . ? C17 H17 0.9300 . ? C18 C19 1.405(6) . ? C18 H18 0.9300 . ? C19 C20 1.391(6) . ? C19 H19 0.9300 . ? C20 C21 1.391(6) . ? C20 H20 0.9300 . ? C21 C22 1.437(6) . ? C22 C23 1.383(6) . ? C22 H22 0.9300 . ? C23 C24 1.475(6) . ? C23 H23 0.9300 . ? C24 N

45、4 1.287(6) . ? C24 H24 0.9300 . ? C25 O2 1.216(6) . ? C25 N5 1.439(6) . ? C25 C26 1.451(7) . ? C26 C27 1.385(6) . ? C26 C30 1.388(6) . ? C27 C28 1.391(7) . ? C27 H27 0.9300 . ? C28 N6 1.399(7) . ? C28 H28 0.9300 . ? C29 N6 1.368(6) . ? C29 C30 1.384(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? N1 N2

46、 1.442(5) . ? N2 H2A 0.86(5) . ? N4 N5 1.437(5) . ? N5 H5A 0.90(5) . ? 9loop_ _geom_angle_atom_site_label_1 分子中原子间键角列表_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 C2 C1 C6 119.7(5) . . ? C2 C1 H1

47、 120.1 . . ? C6 C1 H1 120.1 . . ? C1 C2 C3 121.6(4) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C4 C3 C2 118.4(4) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.9(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 120.0(4) . . ? C1 C6 C7 116.7(5) . . ? C5 C6 C7 123.0(4) . . ? C8 C7 C6 120.0(4) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 116.9(4) . . ? C7 C8 H8 121.5 . . ? C9 C8 H8 121.5 . . ? N1 C9 C8 111.1(4) . . ? N1 C9 H9 124.4 . . ? C8 C9 H9 124