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至尊木虫 (知名作家)

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[求助] Checkcif时，发现晶体有一个B类错误，求修正方法，谢谢啦已有1人参与

非晶体学专业，投稿时Checkcif了一下，发现晶体有一个B类错误，求修正方法，要是能把C类错误也纠正一下，就更好了，谢谢啦。

cif文件如下所示。

data_shelx

_audit_creation_method          SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common          ?
_chemical_melting_point          ?
_chemical_formula_moiety       ?
_chemical_formula_sum
'C39 H36 Cl3 N3 O6 S2'
_chemical_formula_weight       813.18

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'
'S'  'S' 0.1246 0.1234
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl'  'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting          Triclinic
_symmetry_space_group_name_H-M P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.092(2)
_cell_length_b                   12.945(2)
_cell_length_c                   13.599(3)
_cell_angle_alpha                98.723(3)
_cell_angle_beta                112.832(4)
_cell_angle_gamma                96.192(2)
_cell_volume                   1906.5(6)
_cell_formula_units_Z          2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used          6625
_cell_measurement_theta_min          3.0
_cell_measurement_theta_max          27.5

_exptl_crystal_description       Prism
_exptl_crystal_colour          Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas    ?
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             844
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_type MULTI-SCAN
_exptl_absorpt_correction_T_min 0.9241
_exptl_absorpt_correction_T_max 0.9535
_exptl_absorpt_process_details 'REQAB (Rigaku, 1998)'

_exptl_special_details
;
?
;

_diffrn_ambient_temperature    113(2)
_diffrn_radiation_wavelength    0.71073
_diffrn_radiation_type          MoK\a
_diffrn_radiation_source       'rotating anode'
_diffrn_radiation_monochromator multilayer
_diffrn_measurement_device_type 'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_detector_area_resol_mean  5.814
_diffrn_standards_number       0
_diffrn_standards_interval_count  0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_%       0
_diffrn_reflns_number          24660
_diffrn_reflns_av_R_equivalents 0.0382
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min       3.02
_diffrn_reflns_theta_max       27.54
_reflns_number_total             8618
_reflns_number_gt                7864
_reflns_threshold_expression    >2sigma(I)

_computing_data_collection 'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_cell_refinement 'CrystalClear-SM Expert 2.1 b42'
_computing_data_reduction    'CrystalClear-SM Expert 2.1 b42'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material 'CrystalStructure 4.1 (Rigaku, 2014)'

_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^)+(0.0667P)^2^+1.1766P] 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    CONSTR
_refine_ls_extinction_method    none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns       8618
_refine_ls_number_parameters    508
_refine_ls_number_restraints    54
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt          0.0416
_refine_ls_wR_factor_ref       0.1207
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_restrained_S_all    1.039
_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
S1 S 1.08752(3) 0.23603(3) 0.12298(3) 0.02274(10) Uani 1 1 d . . .
S2 S 0.76520(3) 0.39727(3) -0.09566(3) 0.02232(10) Uani 1 1 d . . .
O1 O 1.21331(10) 0.23771(10) 0.19219(10) 0.0290(3) Uani 1 1 d . . .
O2 O 1.05736(11) 0.24898(11) 0.01242(10) 0.0303(3) Uani 1 1 d . . .
O3 O 0.65714(10) 0.39662(10) -0.07467(10) 0.0276(2) Uani 1 1 d . . .
O4 O 0.79191(11) 0.47476(11) -0.15281(10) 0.0334(3) Uani 1 1 d . . .
O5 O 1.30790(11) 0.19688(10) 0.45064(10) 0.0308(3) Uani 1 1 d . . .
O6 O 0.92824(11) 0.54743(9) 0.26017(10) 0.0285(2) Uani 1 1 d . . .
N1 N 1.42181(12) 0.35624(12) 0.56294(11) 0.0250(3) Uani 1 1 d . . .
N2 N 0.89891(11) 0.31148(10) 0.27071(10) 0.0198(3) Uani 1 1 d . . .
N3 N 0.71806(12) 0.49668(11) 0.18579(11) 0.0252(3) Uani 1 1 d . . .
C1 C 1.51926(15) 0.31483(17) 0.63931(14) 0.0323(4) Uani 1 1 d . . .
H1A H 1.5067 0.3151 0.7063 0.049 Uiso 1 1 calc R . .
H1B H 1.5979 0.3595 0.6567 0.049 Uiso 1 1 calc R . .
H1C H 1.5189 0.2419 0.6064 0.049 Uiso 1 1 calc R . .
C2 C 1.41536(14) 0.46448(14) 0.57030(13) 0.0241(3) Uani 1 1 d . . .
C3 C 1.49621(16) 0.55082(16) 0.64794(14) 0.0324(4) Uani 1 1 d . . .
H3 H 1.5667 0.5418 0.7069 0.039 Uiso 1 1 calc R . .
C4 C 1.46940(18) 0.65108(16) 0.63552(16) 0.0372(4) Uani 1 1 d . . .
H4 H 1.5231 0.7122 0.6866 0.045 Uiso 1 1 calc R . .
C5 C 1.36558(18) 0.66345(15) 0.54979(17) 0.0357(4) Uani 1 1 d . . .
H5 H 1.3494 0.7329 0.5433 0.043 Uiso 1 1 calc R . .
C6 C 1.28413(16) 0.57526(14) 0.47259(15) 0.0283(3) Uani 1 1 d . . .
H6 H 1.2126 0.5840 0.4145 0.034 Uiso 1 1 calc R . .
C7 C 1.31069(13) 0.47586(13) 0.48339(12) 0.0222(3) Uani 1 1 d . . .
C8 C 1.24719(13) 0.36762(12) 0.41135(12) 0.0207(3) Uani 1 1 d . . .
H8 H 1.2540 0.3642 0.3400 0.025 Uiso 1 1 calc R . .
C9 C 1.32561(13) 0.29387(13) 0.47382(13) 0.0234(3) Uani 1 1 d . . .
C10 C 1.11452(13) 0.33979(12) 0.38993(12) 0.0201(3) Uani 1 1 d . . .
C11 C 1.08642(14) 0.32832(14) 0.48709(13) 0.0247(3) Uani 1 1 d . . .
H11A H 1.1036 0.3993 0.5346 0.030 Uiso 1 1 calc R . .
H11B H 1.1404 0.2841 0.5300 0.030 Uiso 1 1 calc R . .
C12 C 0.95330(15) 0.27730(14) 0.45258(14) 0.0274(3) Uani 1 1 d . . .
H12A H 0.9414 0.2001 0.4235 0.033 Uiso 1 1 calc R . .
H12B H 0.9328 0.2867 0.5168 0.033 Uiso 1 1 calc R . .
C13 C 0.86950(14) 0.32823(14) 0.36564(14) 0.0262(3) Uani 1 1 d . . .
H13A H 0.7833 0.2960 0.3445 0.031 Uiso 1 1 calc R . .
H13B H 0.8806 0.4053 0.3946 0.031 Uiso 1 1 calc R . .
C14 C 1.02381(13) 0.33051(11) 0.29117(12) 0.0184(3) Uani 1 1 d . . .
C15 C 1.03055(12) 0.34026(12) 0.18424(12) 0.0187(3) Uani 1 1 d . . .
H15 H 1.0816 0.4104 0.1944 0.022 Uiso 1 1 calc R . .
C16 C 0.89669(12) 0.33900(12) 0.10373(12) 0.0187(3) Uani 1 1 d . . .
H16 H 0.8619 0.2658 0.0573 0.022 Uiso 1 1 calc R . .
C17 C 0.82968(13) 0.35909(12) 0.17996(12) 0.0195(3) Uani 1 1 d . . .
C18 C 0.69448(13) 0.31592(13) 0.13281(13) 0.0226(3) Uani 1 1 d . . .
C19 C 0.63083(15) 0.21308(14) 0.09261(15) 0.0296(3) Uani 1 1 d . . .
H19 H 0.6722 0.1550 0.0902 0.036 Uiso 1 1 calc R . .
C20 C 0.50289(16) 0.19617(18) 0.05521(16) 0.0382(4) Uani 1 1 d . . .
H20 H 0.4571 0.1259 0.0269 0.046 Uiso 1 1 calc R . .
C21 C 0.44354(15) 0.28106(19) 0.05938(16) 0.0390(4) Uani 1 1 d . . .
H21 H 0.3571 0.2680 0.0336 0.047 Uiso 1 1 calc R . .
C22 C 0.50721(15) 0.38540(17) 0.10047(14) 0.0324(4) Uani 1 1 d . . .
H22 H 0.4661 0.4436 0.1028 0.039 Uiso 1 1 calc R . .
C23 C 0.63329(14) 0.40049(14) 0.13780(13) 0.0247(3) Uani 1 1 d . . .
C24 C 0.83528(14) 0.47980(12) 0.21541(13) 0.0225(3) Uani 1 1 d . . .
C25 C 0.68675(18) 0.60067(15) 0.20468(16) 0.0348(4) Uani 1 1 d . . .
H25A H 0.6560 0.6056 0.2618 0.052 Uiso 1 1 calc R . .
H25B H 0.6236 0.6110 0.1371 0.052 Uiso 1 1 calc R . .
H25C H 0.7595 0.6556 0.2279 0.052 Uiso 1 1 calc R . .
C26 C 0.89653(13) 0.41620(13) 0.02934(12) 0.0223(3) Uani 1 1 d . . .
H26A H 0.9684 0.4124 0.0119 0.027 Uiso 1 1 calc R . .
H26B H 0.9078 0.4891 0.0711 0.027 Uiso 1 1 calc R . .
C27 C 0.75749(15) 0.27022(15) -0.16948(14) 0.0311(4) Uani 1 1 d . . .
C28 C 0.8283(2) 0.2604(2) -0.22990(16) 0.0472(5) Uani 1 1 d . . .
H28 H 0.8831 0.3199 -0.2280 0.057 Uiso 1 1 calc R . .
C29 C 0.8160(3) 0.1613(3) -0.2926(2) 0.0706(9) Uani 1 1 d . . .
H29 H 0.8624 0.1527 -0.3349 0.085 Uiso 1 1 calc R . .
C30 C 0.7374(3) 0.0754(3) -0.2942(2) 0.0753(11) Uani 1 1 d . . .
H30 H 0.7305 0.0080 -0.3372 0.090 Uiso 1 1 calc R . .
C31 C 0.6679(2) 0.08589(19) -0.2338(2) 0.0631(8) Uani 1 1 d . . .
H31 H 0.6138 0.0259 -0.2356 0.076 Uiso 1 1 calc R . .
C32 C 0.67748(18) 0.18494(15) -0.17006(16) 0.0406(5) Uani 1 1 d . . .
H32 H 0.6304 0.1934 -0.1284 0.049 Uiso 1 1 calc R . .
C33 C 0.99738(14) 0.11817(13) 0.11984(14) 0.0252(3) Uani 1 1 d . . .
C34 C 0.89877(15) 0.06741(14) 0.02221(14) 0.0290(3) Uani 1 1 d . . .
H34 H 0.8829 0.0941 -0.0423 0.035 Uiso 1 1 calc R . .
C35 C 0.82451(16) -0.02248(15) 0.02114(17) 0.0355(4) Uani 1 1 d . . .
H35 H 0.7576 -0.0584 -0.0447 0.043 Uiso 1 1 calc R . .
C36 C 0.84769(19) -0.05975(16) 0.11550(19) 0.0415(5) Uani 1 1 d . . .
H36 H 0.7959 -0.1209 0.1145 0.050 Uiso 1 1 calc R . .
C37 C 0.9462(2) -0.00877(15) 0.21230(18) 0.0401(4) Uani 1 1 d . . .
H37 H 0.9609 -0.0351 0.2769 0.048 Uiso 1 1 calc R . .
C38 C 1.02304(17) 0.08048(14) 0.21493(15) 0.0318(4) Uani 1 1 d . . .
H38 H 1.0915 0.1148 0.2803 0.038 Uiso 1 1 calc R . .
Cl1 Cl 0.6606(5) 0.8580(3) 0.2613(4) 0.0610(9) Uani 0.572(14) 1 d PDU A 1
Cl2 Cl 0.8588(3) 0.9693(5) 0.4662(4) 0.0693(11) Uani 0.572(14) 1 d PDU A 1
Cl3 Cl 0.6636(3) 1.0663(2) 0.3656(5) 0.0921(12) Uani 0.572(14) 1 d PDU A 1
Cl1' Cl 0.6476(6) 0.8714(5) 0.2513(5) 0.0634(12) Uani 0.428(14) 1 d PDU A 2
Cl2' Cl 0.8590(3) 0.9502(7) 0.4546(6) 0.0695(15) Uani 0.428(14) 1 d PDU A 2
Cl3' Cl 0.6484(7) 1.0602(4) 0.3922(6) 0.118(2) Uani 0.428(14) 1 d PDU A 2
C39 C 0.7006(2) 0.94190(16) 0.38714(19) 0.0459(5) Uani 1 1 d D . .

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
S1 0.01399(17) 0.0316(2) 0.02000(19) 0.00078(14) 0.00508(14) 0.00737(14)
S2 0.01622(17) 0.0297(2) 0.01958(18) 0.00766(14) 0.00415(14) 0.00727(14)
O1 0.0137(5) 0.0413(7) 0.0273(6) 0.0006(5) 0.0047(4) 0.0100(5)
O2 0.0250(6) 0.0441(7) 0.0222(6) 0.0032(5) 0.0105(5) 0.0101(5)
O3 0.0176(5) 0.0391(6) 0.0264(6) 0.0099(5) 0.0072(4) 0.0100(5)
O4 0.0257(6) 0.0448(7) 0.0288(6) 0.0180(6) 0.0066(5) 0.0066(5)
O5 0.0275(6) 0.0303(6) 0.0332(6) 0.0085(5) 0.0094(5) 0.0090(5)
O6 0.0259(6) 0.0259(6) 0.0297(6) 0.0019(5) 0.0093(5) 0.0027(4)
N1 0.0145(6) 0.0383(7) 0.0197(6) 0.0088(6) 0.0032(5) 0.0059(5)
N2 0.0121(5) 0.0279(6) 0.0200(6) 0.0064(5) 0.0059(5) 0.0066(5)
N3 0.0220(6) 0.0307(7) 0.0241(7) 0.0055(5) 0.0087(5) 0.0130(5)
C1 0.0166(7) 0.0547(11) 0.0259(8) 0.0178(8) 0.0045(6) 0.0108(7)
C2 0.0160(7) 0.0366(8) 0.0188(7) 0.0041(6) 0.0077(6) 0.0010(6)
C3 0.0218(8) 0.0483(10) 0.0214(8) -0.0012(7) 0.0092(6) -0.0053(7)
C4 0.0343(9) 0.0401(10) 0.0335(9) -0.0080(8) 0.0204(8) -0.0100(8)
C5 0.0398(10) 0.0291(8) 0.0455(11) 0.0020(8) 0.0284(9) 0.0022(7)
C6 0.0259(8) 0.0310(8) 0.0320(9) 0.0066(7) 0.0161(7) 0.0057(6)
C7 0.0159(6) 0.0295(8) 0.0205(7) 0.0034(6) 0.0082(6) 0.0017(6)
C8 0.0141(6) 0.0273(7) 0.0184(7) 0.0044(6) 0.0042(5) 0.0048(5)
C9 0.0156(6) 0.0333(8) 0.0213(7) 0.0076(6) 0.0064(6) 0.0069(6)
C10 0.0148(6) 0.0245(7) 0.0195(7) 0.0043(5) 0.0057(5) 0.0041(5)
C11 0.0195(7) 0.0338(8) 0.0199(7) 0.0065(6) 0.0069(6) 0.0048(6)
C12 0.0213(7) 0.0378(9) 0.0263(8) 0.0123(7) 0.0110(6) 0.0062(6)
C13 0.0195(7) 0.0382(9) 0.0258(8) 0.0101(7) 0.0120(6) 0.0099(6)
C14 0.0131(6) 0.0218(7) 0.0201(7) 0.0034(5) 0.0068(5) 0.0042(5)
C15 0.0119(6) 0.0247(7) 0.0174(7) 0.0030(5) 0.0039(5) 0.0054(5)
C16 0.0115(6) 0.0241(7) 0.0182(7) 0.0040(5) 0.0034(5) 0.0050(5)
C17 0.0131(6) 0.0234(7) 0.0202(7) 0.0041(5) 0.0050(5) 0.0044(5)
C18 0.0126(6) 0.0333(8) 0.0213(7) 0.0064(6) 0.0056(5) 0.0058(6)
C19 0.0182(7) 0.0348(9) 0.0320(9) 0.0056(7) 0.0076(6) 0.0018(6)
C20 0.0185(8) 0.0515(11) 0.0358(10) 0.0045(8) 0.0068(7) -0.0053(7)
C21 0.0133(7) 0.0681(13) 0.0314(9) 0.0087(9) 0.0061(7) 0.0053(8)
C22 0.0179(7) 0.0566(11) 0.0246(8) 0.0093(8) 0.0079(6) 0.0161(7)
C23 0.0175(7) 0.0387(9) 0.0190(7) 0.0073(6) 0.0069(6) 0.0104(6)
C24 0.0218(7) 0.0267(7) 0.0203(7) 0.0055(6) 0.0088(6) 0.0093(6)
C25 0.0393(10) 0.0372(9) 0.0319(9) 0.0085(7) 0.0142(8) 0.0238(8)
C26 0.0154(6) 0.0286(7) 0.0193(7) 0.0057(6) 0.0034(5) 0.0036(5)
C27 0.0241(8) 0.0383(9) 0.0208(8) 0.0020(7) -0.0019(6) 0.0145(7)
C28 0.0345(10) 0.0727(15) 0.0279(9) 0.0013(9) 0.0047(8) 0.0283(10)
C29 0.0575(16) 0.097(2) 0.0384(12) -0.0143(13) 0.0023(11) 0.0466(17)
C30 0.0693(18) 0.0666(17) 0.0483(14) -0.0219(13) -0.0155(13) 0.0445(16)
C31 0.0540(14) 0.0389(11) 0.0506(14) -0.0047(10) -0.0227(12) 0.0127(10)
C32 0.0334(9) 0.0352(9) 0.0324(10) 0.0035(8) -0.0077(8) 0.0090(8)
C33 0.0173(7) 0.0260(7) 0.0286(8) -0.0002(6) 0.0067(6) 0.0083(6)
C34 0.0203(7) 0.0324(8) 0.0290(8) -0.0027(7) 0.0067(6) 0.0101(6)
C35 0.0219(8) 0.0336(9) 0.0411(10) -0.0072(8) 0.0084(7) 0.0044(7)
C36 0.0374(10) 0.0302(9) 0.0539(12) -0.0004(8) 0.0203(9) 0.0019(8)
C37 0.0459(11) 0.0318(9) 0.0413(11) 0.0076(8) 0.0163(9) 0.0089(8)
C38 0.0298(8) 0.0287(8) 0.0305(9) 0.0014(7) 0.0065(7) 0.0092(7)
Cl1 0.077(2) 0.0349(9) 0.0771(19) -0.0159(11) 0.0531(17) -0.0093(10)
Cl2 0.0558(15) 0.080(2) 0.0684(13) 0.0231(12) 0.0234(11) -0.0044(10)
Cl3 0.0528(11) 0.0232(8) 0.172(3) 0.0034(12) 0.0216(15) 0.0087(6)
Cl1' 0.0417(13) 0.080(3) 0.0635(16) 0.0121(17) 0.0197(12) 0.0006(15)
Cl2' 0.0242(12) 0.073(2) 0.101(3) 0.054(2) 0.0031(13) 0.0041(10)
Cl3' 0.125(4) 0.058(2) 0.086(3) -0.0289(15) -0.034(2) 0.035(2)
C39 0.0399(11) 0.0378(10) 0.0523(13) 0.0079(9) 0.0119(10) 0.0055(8)

_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
S1 O1 1.4407(11) . ?
S1 O2 1.4443(13) . ?
S1 C33 1.7615(17) . ?
S1 C15 1.8150(15) . ?
S2 O4 1.4409(13) . ?
S2 O3 1.4412(12) . ?
S2 C27 1.7648(18) . ?
S2 C26 1.7794(15) . ?
O5 C9 1.221(2) . ?
O6 C24 1.223(2) . ?
N1 C9 1.371(2) . ?
N1 C2 1.402(2) . ?
N1 C1 1.453(2) . ?
N2 C14 1.4114(18) . ?
N2 C13 1.459(2) . ?
N2 C17 1.4642(19) . ?
N3 C24 1.3673(19) . ?
N3 C23 1.409(2) . ?
N3 C25 1.450(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.387(2) . ?
C2 C7 1.397(2) . ?
C3 C4 1.390(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.375(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.510(2) . ?
C8 C10 1.506(2) . ?
C8 C9 1.532(2) . ?
C8 H8 1.0000 . ?
C10 C14 1.342(2) . ?
C10 C11 1.510(2) . ?
C11 C12 1.529(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.520(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.511(2) . ?
C15 C16 1.5597(18) . ?
C15 H15 1.0000 . ?
C16 C26 1.526(2) . ?
C16 C17 1.554(2) . ?
C16 H16 1.0000 . ?
C17 C18 1.5089(19) . ?
C17 C24 1.550(2) . ?
C18 C19 1.377(2) . ?
C18 C23 1.393(2) . ?
C19 C20 1.408(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.394(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.388(2) . ?
C22 H22 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C32 1.384(3) . ?
C27 C28 1.401(3) . ?
C28 C29 1.387(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.375(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.388(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.400(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.385(3) . ?
C33 C34 1.398(2) . ?
C34 C35 1.386(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.377(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.392(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.389(3) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
Cl1 C39 1.738(4) . ?
Cl2 C39 1.755(4) . ?
Cl3 C39 1.754(4) . ?
Cl1' C39 1.761(5) . ?
Cl2' C39 1.756(4) . ?
Cl3' C39 1.720(5) . ?

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
O1 S1 O2 118.45(7) . . ?
O1 S1 C33 109.27(8) . . ?
O2 S1 C33 108.88(8) . . ?
O1 S1 C15 109.89(7) . . ?
O2 S1 C15 105.65(7) . . ?
C33 S1 C15 103.67(7) . . ?
O4 S2 O3 118.31(7) . . ?
O4 S2 C27 107.76(9) . . ?
O3 S2 C27 108.61(8) . . ?
O4 S2 C26 106.00(7) . . ?
O3 S2 C26 110.02(7) . . ?
C27 S2 C26 105.37(7) . . ?
C9 N1 C2 111.81(13) . . ?
C9 N1 C1 123.86(15) . . ?
C2 N1 C1 124.32(14) . . ?
C14 N2 C13 116.72(12) . . ?
C14 N2 C17 109.81(12) . . ?
C13 N2 C17 116.39(12) . . ?
C24 N3 C23 111.43(13) . . ?
C24 N3 C25 123.63(15) . . ?
C23 N3 C25 124.92(14) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C7 122.43(16) . . ?
C3 C2 N1 128.45(15) . . ?
C7 C2 N1 109.11(14) . . ?
C2 C3 C4 116.99(17) . . ?
C2 C3 H3 121.5 . . ?
C4 C3 H3 121.5 . . ?
C5 C4 C3 121.15(17) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 121.16(18) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 118.12(17) . . ?
C7 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C6 C7 C2 120.15(15) . . ?
C6 C7 C8 130.93(15) . . ?
C2 C7 C8 108.85(14) . . ?
C10 C8 C7 114.34(12) . . ?
C10 C8 C9 113.29(13) . . ?
C7 C8 C9 102.32(12) . . ?
C10 C8 H8 108.9 . . ?
C7 C8 H8 108.9 . . ?
C9 C8 H8 108.9 . . ?
O5 C9 N1 124.82(15) . . ?
O5 C9 C8 127.41(14) . . ?
N1 C9 C8 107.77(14) . . ?
C14 C10 C8 122.70(14) . . ?
C14 C10 C11 120.44(13) . . ?
C8 C10 C11 116.77(13) . . ?
C10 C11 C12 111.87(13) . . ?
C10 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C13 C12 C11 110.09(13) . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.2 . . ?
N2 C13 C12 108.94(13) . . ?
N2 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
N2 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C10 C14 N2 123.69(14) . . ?
C10 C14 C15 129.41(13) . . ?
N2 C14 C15 106.88(12) . . ?
C14 C15 C16 105.23(11) . . ?
C14 C15 S1 116.73(10) . . ?
C16 C15 S1 107.94(10) . . ?
C14 C15 H15 108.9 . . ?
C16 C15 H15 108.9 . . ?
S1 C15 H15 108.9 . . ?
C26 C16 C17 118.59(12) . . ?
C26 C16 C15 109.55(12) . . ?
C17 C16 C15 103.57(11) . . ?
C26 C16 H16 108.2 . . ?
C17 C16 H16 108.2 . . ?
C15 C16 H16 108.2 . . ?
N2 C17 C18 112.29(12) . . ?
N2 C17 C24 112.94(12) . . ?
C18 C17 C24 102.29(12) . . ?
N2 C17 C16 101.74(11) . . ?
C18 C17 C16 117.45(12) . . ?
C24 C17 C16 110.55(12) . . ?
C19 C18 C23 120.46(14) . . ?
C19 C18 C17 130.80(14) . . ?
C23 C18 C17 108.70(14) . . ?
C18 C19 C20 118.29(17) . . ?
C18 C19 H19 120.9 . . ?
C20 C19 H19 120.9 . . ?
C21 C20 C19 120.47(18) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 121.66(16) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C23 C22 C21 117.07(17) . . ?
C23 C22 H22 121.5 . . ?
C21 C22 H22 121.5 . . ?
C22 C23 C18 122.02(16) . . ?
C22 C23 N3 128.14(16) . . ?
C18 C23 N3 109.84(13) . . ?
O6 C24 N3 126.56(15) . . ?
O6 C24 C17 125.74(14) . . ?
N3 C24 C17 107.69(13) . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C16 C26 S2 117.29(10) . . ?
C16 C26 H26A 108.0 . . ?
S2 C26 H26A 108.0 . . ?
C16 C26 H26B 108.0 . . ?
S2 C26 H26B 108.0 . . ?
H26A C26 H26B 107.2 . . ?
C32 C27 C28 122.3(2) . . ?
C32 C27 S2 118.99(15) . . ?
C28 C27 S2 118.60(17) . . ?
C29 C28 C27 118.0(3) . . ?
C29 C28 H28 121.0 . . ?
C27 C28 H28 121.0 . . ?
C30 C29 C28 120.7(3) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 120.8(2) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 H30 119.6 . . ?
C30 C31 C32 120.0(3) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C27 C32 C31 118.2(2) . . ?
C27 C32 H32 120.9 . . ?
C31 C32 H32 120.9 . . ?
C38 C33 C34 121.73(17) . . ?
C38 C33 S1 119.26(13) . . ?
C34 C33 S1 118.97(14) . . ?
C35 C34 C33 118.90(18) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
C36 C35 C34 119.99(17) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C37 120.70(19) . . ?
C35 C36 H36 119.6 . . ?
C37 C36 H36 119.6 . . ?
C38 C37 C36 120.3(2) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C33 C38 C37 118.33(17) . . ?
C33 C38 H38 120.8 . . ?
C37 C38 H38 120.8 . . ?
Cl3' C39 Cl1 119.4(3) . . ?
Cl3' C39 Cl3 15.8(4) . . ?
Cl1 C39 Cl3 108.8(2) . . ?
Cl3' C39 Cl2 107.8(4) . . ?
Cl1 C39 Cl2 112.5(3) . . ?
Cl3 C39 Cl2 104.3(2) . . ?
Cl3' C39 Cl2' 116.2(5) . . ?
Cl1 C39 Cl2' 104.4(3) . . ?
Cl3 C39 Cl2' 111.4(3) . . ?
Cl2 C39 Cl2' 8.9(5) . . ?
Cl3' C39 Cl1' 110.8(3) . . ?
Cl1 C39 Cl1' 8.6(3) . . ?
Cl3 C39 Cl1' 100.4(3) . . ?
Cl2 C39 Cl1' 117.7(3) . . ?
Cl2' C39 Cl1' 110.2(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C2 C3 -179.21(16) . . . . ?
C1 N1 C2 C3 0.0(3) . . . . ?
C9 N1 C2 C7 0.33(18) . . . . ?
C1 N1 C2 C7 179.50(14) . . . . ?
C7 C2 C3 C4 -0.5(2) . . . . ?
N1 C2 C3 C4 179.00(16) . . . . ?
C2 C3 C4 C5 0.7(3) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
C4 C5 C6 C7 -0.7(3) . . . . ?
C5 C6 C7 C2 0.9(2) . . . . ?
C5 C6 C7 C8 -175.63(16) . . . . ?
C3 C2 C7 C6 -0.3(2) . . . . ?
N1 C2 C7 C6 -179.91(14) . . . . ?
C3 C2 C7 C8 176.93(14) . . . . ?
N1 C2 C7 C8 -2.65(17) . . . . ?
C6 C7 C8 C10 -56.6(2) . . . . ?
C2 C7 C8 C10 126.54(14) . . . . ?
C6 C7 C8 C9 -179.48(16) . . . . ?
C2 C7 C8 C9 3.66(16) . . . . ?
C2 N1 C9 O5 -177.78(15) . . . . ?
C1 N1 C9 O5 3.1(3) . . . . ?
C2 N1 C9 C8 2.08(17) . . . . ?
C1 N1 C9 C8 -177.09(14) . . . . ?
C10 C8 C9 O5 52.8(2) . . . . ?
C7 C8 C9 O5 176.42(16) . . . . ?
C10 C8 C9 N1 -127.03(14) . . . . ?
C7 C8 C9 N1 -3.43(16) . . . . ?
C7 C8 C10 C14 111.88(17) . . . . ?
C9 C8 C10 C14 -131.40(16) . . . . ?
C7 C8 C10 C11 -64.81(18) . . . . ?
C9 C8 C10 C11 51.91(18) . . . . ?
C14 C10 C11 C12 15.5(2) . . . . ?
C8 C10 C11 C12 -167.73(13) . . . . ?
C10 C11 C12 C13 -45.72(19) . . . . ?
C14 N2 C13 C12 -45.42(18) . . . . ?
C17 N2 C13 C12 -177.76(13) . . . . ?
C11 C12 C13 N2 60.66(18) . . . . ?
C8 C10 C14 N2 -175.64(13) . . . . ?
C11 C10 C14 N2 0.9(2) . . . . ?
C8 C10 C14 C15 2.6(2) . . . . ?
C11 C10 C14 C15 179.14(14) . . . . ?
C13 N2 C14 C10 15.0(2) . . . . ?
C17 N2 C14 C10 150.29(14) . . . . ?
C13 N2 C14 C15 -163.53(13) . . . . ?
C17 N2 C14 C15 -28.27(15) . . . . ?
C10 C14 C15 C16 -171.51(15) . . . . ?
N2 C14 C15 C16 6.93(15) . . . . ?
C10 C14 C15 S1 68.85(19) . . . . ?
N2 C14 C15 S1 -112.70(11) . . . . ?
O1 S1 C15 C14 -64.73(13) . . . . ?
O2 S1 C15 C14 166.42(11) . . . . ?
C33 S1 C15 C14 51.96(12) . . . . ?
O1 S1 C15 C16 177.10(10) . . . . ?
O2 S1 C15 C16 48.24(11) . . . . ?
C33 S1 C15 C16 -66.21(11) . . . . ?
C14 C15 C16 C26 142.22(12) . . . . ?
S1 C15 C16 C26 -92.47(12) . . . . ?
C14 C15 C16 C17 14.76(14) . . . . ?
S1 C15 C16 C17 140.08(10) . . . . ?
C14 N2 C17 C18 163.45(12) . . . . ?
C13 N2 C17 C18 -61.12(17) . . . . ?
C14 N2 C17 C24 -81.50(15) . . . . ?
C13 N2 C17 C24 53.93(17) . . . . ?
C14 N2 C17 C16 37.01(14) . . . . ?
C13 N2 C17 C16 172.44(12) . . . . ?
C26 C16 C17 N2 -151.70(12) . . . . ?
C15 C16 C17 N2 -30.13(14) . . . . ?
C26 C16 C17 C18 85.31(17) . . . . ?
C15 C16 C17 C18 -153.11(13) . . . . ?
C26 C16 C17 C24 -31.50(17) . . . . ?
C15 C16 C17 C24 90.08(13) . . . . ?
N2 C17 C18 C19 -54.8(2) . . . . ?
C24 C17 C18 C19 -176.13(17) . . . . ?
C16 C17 C18 C19 62.7(2) . . . . ?
N2 C17 C18 C23 123.10(14) . . . . ?
C24 C17 C18 C23 1.73(16) . . . . ?
C16 C17 C18 C23 -119.47(14) . . . . ?
C23 C18 C19 C20 1.1(3) . . . . ?
C17 C18 C19 C20 178.75(17) . . . . ?
C18 C19 C20 C21 -0.2(3) . . . . ?
C19 C20 C21 C22 -0.1(3) . . . . ?
C20 C21 C22 C23 -0.4(3) . . . . ?
C21 C22 C23 C18 1.3(3) . . . . ?
C21 C22 C23 N3 -177.84(16) . . . . ?
C19 C18 C23 C22 -1.7(3) . . . . ?
C17 C18 C23 C22 -179.82(15) . . . . ?
C19 C18 C23 N3 177.59(15) . . . . ?
C17 C18 C23 N3 -0.54(18) . . . . ?
C24 N3 C23 C22 178.11(16) . . . . ?
C25 N3 C23 C22 -0.3(3) . . . . ?
C24 N3 C23 C18 -1.12(19) . . . . ?
C25 N3 C23 C18 -179.54(15) . . . . ?
C23 N3 C24 O6 -178.88(16) . . . . ?
C25 N3 C24 O6 -0.4(3) . . . . ?
C23 N3 C24 C17 2.23(18) . . . . ?
C25 N3 C24 C17 -179.33(14) . . . . ?
N2 C17 C24 O6 57.8(2) . . . . ?
C18 C17 C24 O6 178.72(15) . . . . ?
C16 C17 C24 O6 -55.4(2) . . . . ?
N2 C17 C24 N3 -123.29(13) . . . . ?
C18 C17 C24 N3 -2.38(16) . . . . ?
C16 C17 C24 N3 123.46(13) . . . . ?
C17 C16 C26 S2 -82.00(15) . . . . ?
C15 C16 C26 S2 159.50(10) . . . . ?
O4 S2 C26 C16 -176.09(11) . . . . ?
O3 S2 C26 C16 54.88(13) . . . . ?
C27 S2 C26 C16 -62.01(14) . . . . ?
O4 S2 C27 C32 -147.14(14) . . . . ?
O3 S2 C27 C32 -17.84(16) . . . . ?
C26 S2 C27 C32 100.01(14) . . . . ?
O4 S2 C27 C28 29.70(16) . . . . ?
O3 S2 C27 C28 159.00(13) . . . . ?
C26 S2 C27 C28 -83.15(15) . . . . ?
C32 C27 C28 C29 0.4(3) . . . . ?
S2 C27 C28 C29 -176.31(16) . . . . ?
C27 C28 C29 C30 -0.6(3) . . . . ?
C28 C29 C30 C31 0.4(4) . . . . ?
C29 C30 C31 C32 -0.1(4) . . . . ?
C28 C27 C32 C31 -0.1(3) . . . . ?
S2 C27 C32 C31 176.66(14) . . . . ?
C30 C31 C32 C27 -0.1(3) . . . . ?
O1 S1 C33 C38 39.49(15) . . . . ?
O2 S1 C33 C38 170.25(13) . . . . ?
C15 S1 C33 C38 -77.63(14) . . . . ?
O1 S1 C33 C34 -142.98(12) . . . . ?
O2 S1 C33 C34 -12.22(15) . . . . ?
C15 S1 C33 C34 99.90(13) . . . . ?
C38 C33 C34 C35 0.5(2) . . . . ?
S1 C33 C34 C35 -177.00(12) . . . . ?
C33 C34 C35 C36 0.7(3) . . . . ?
C34 C35 C36 C37 -0.8(3) . . . . ?
C35 C36 C37 C38 -0.3(3) . . . . ?
C34 C33 C38 C37 -1.5(3) . . . . ?
S1 C33 C38 C37 175.98(14) . . . . ?
C36 C37 C38 C33 1.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full             27.54
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max 0.643
_refine_diff_density_min -0.482
_refine_diff_density_rms 0.060

B类错误.jpg

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