晶体表填写说明

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'

_chemical_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' 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_setting 'Monoclinic' 晶系名称 6

_symmetry_space_group_name_H-M 'P2(1)/c' 空间群名称 7

loop_

_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 107.7170(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θ值

_cell_measurement_theta_max 28.00 用于确定晶胞的衍射点的最大θ值

_exptl_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 '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λ 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' 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_sigmaI/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θ角 19a

_diffrn_reflns_theta_max 26.00 结构精修时最大θ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2σ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_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^)+(0.0546P)^2^] 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_number_reflns 2995 参加结构精修的衍射点数 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_fit_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_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 0.2152(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 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_site_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_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_ 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_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 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_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θ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θ

_diffrn_measured_fraction_theta_full 0.999 整个衍射数据的完备率

_refine_diff_density_max 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, 3a–3b and 4a–4b

Compound

chemical formula

formula weight

crystal size (mm)

temperature (K)

radiation

crystal system

space group

a(Å)

b(Å)

c(Å)

α(°)

β(°)

γ(°)

V(Å3)

Z

ρ(calc) (g/cm3)

F (000)

. (mm-1)

θ range (deg)

reflns collected

indep. reflns

Refns obs. [I＞2σ(I)]

data/restr/paras

GOF

R1/wR2

[I＞2σ(I)]

R1/wR2

(all data)

larg peak and hole(e/Å3)

2a

C14H22B10NO2S3Co 1

499.54 2

0.18×0.15×0.12 3

296(2) 4

0.71073 5

Monoclinic 6

P2(1)/c 7

16.778(4) 8

14.901(3) 9

9.602(2) 10

90.00 11

102.633(3) 12

90.00 13

2342.4(9) 14

4 15

1.416 16

1016 17

1.013 18

1.85 to 26.0 19

12549 (Rint = 0.0796) 20

4600 21

3219 22

4600/0/337 23a/23b/23c

0.894 24

0.0393/0.0830 25a/25b

0.0570/0.0875 26a/26b

0.294/-0.286 27a/27b