CIF文件详解.doc

data_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 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 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(7)
_cell_length_c 10.044(7)
_cell_angle_alpha 90.00
_cell_angle_beta 105.94(3)
_cell_angle_gamma 90.00
_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θ值
_cell_measurement_theta_max 20.48 用于确定晶胞的衍射点的最大θ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 'SADABS; 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λ
_diffrn_radiation_type 'MoK\a' 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_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
_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
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 1.68 结构精修时最小θ角
_diffrn_reflns_theta_max 27.74 结构精修时最大θ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2σ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 '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_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_details 结构精修过程中一些细节的说明
;
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 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/[\s^2^(Fo^2^)+(0.05P)^2^+0.88P] where P=(Fo^2^+2Fc^2^)/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_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
_refine_ls_number_parameters 349 参加结构精修的参数数目
_refine_ls_number_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
_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_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 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) 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(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 . . .
C11 C 0.5998(4) 0.5425(4) 0.0516(4) 0.0438(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) 0.0427(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 01743 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 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) 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) 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 calc 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) 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 calc 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) 00423(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) Uani 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 . . .
O1 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) 0.0440(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) -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) -0.014(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) 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(17) -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) 0.037(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 0.047(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) 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)
N4 0.055(2) 0.0406(19) 0.0303(17) -0.0039(15) 0.0093(16) -0.0081(17)
N5 0.0338(17) 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
;
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 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) . ?
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 0.9300 . ?
C10 O1 1.228(5) . ?
C10 N2 1.432(5) . ?
C10 C11 1.437(6) . ?
C11 C15 1.393(6) . ?
C11 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 C21 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) . ?