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2014-06-04 09:30:11, 153 K
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2014-06-04 09:32:21, 153 K
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2014-06-04 09:33:03, 126.33 K
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2014-06-04 09:33:28, 304.14 K
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2014-06-04 09:34:15, 232.15 K
2014-06-04 09:34:44, 153 K
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ÊÇCuµÄһάÁ´£¬ÁòËá¸ùÇÅÁ¬µÄ¡£Ö»ÓÐphenÅäλ¡£ res: TITL wn I2/a CELL 0.71073 6.9815 13.8958 14.4131 90.000 99.620 90.000 ZERR 4 0.0007 0.0014 0.0013 0.000 0.004 0.000 LATT 2 SYMM 0.50000 - X , Y , - Z SFAC C H Cu N O S UNIT 48 0 4 8 24 4 OMIT -3 50 L.S. 20 ACTA BOND $H FMAP 2 PLAN 100 CONF WGHT 0.026600 1.346000 FVAR 0.075540 C1 1 0.406119 0.307876 0.180869 11.000000 0.039210 = 0.042830 0.031460 0.000530 -0.000110 -0.001770 AFIX 43 H1 2 0.432040 0.248351 0.209738 11.000000 -1.200000 AFIX 0 C2 1 0.452293 0.391265 0.234108 11.000000 0.044370 = 0.063310 0.032130 -0.012470 -0.000270 -0.006170 AFIX 43 H2 2 0.507755 0.386937 0.297287 11.000000 -1.200000 AFIX 0 C3 1 0.415495 0.478704 0.192812 11.000000 0.043400 = 0.045320 0.047310 -0.023220 0.009640 -0.011240 AFIX 43 H3 2 0.444834 0.534470 0.227997 11.000000 -1.200000 AFIX 0 C4 1 0.333104 0.485231 0.096944 11.000000 0.029050 = 0.030320 0.049030 -0.010770 0.013770 -0.005050 C5 1 0.291187 0.397881 0.048910 11.000000 0.022050 = 0.024790 0.034020 -0.002700 0.006670 -0.002090 C6 1 0.289810 0.573203 0.046063 11.000000 0.041390 = 0.022610 0.069400 -0.008750 0.022900 -0.004980 AFIX 43 H6 2 0.317051 0.631556 0.077063 11.000000 -1.200000 AFIX 0 Cu1 3 0.250000 0.200211 0.000000 10.500000 0.034050 = 0.018590 0.026990 0.000000 -0.000670 0.000000 N1 4 0.326379 0.310582 0.090331 11.000000 0.026260 = 0.027700 0.028040 -0.000130 0.001120 -0.000230 O1 5 -0.079680 0.198463 0.035693 11.000000 0.032340 = 0.031230 0.050360 -0.011310 0.002990 -0.008400 O2 5 -0.297068 0.076453 0.076754 11.000000 0.032680 = 0.029480 0.038870 0.006630 0.003770 0.004150 O3 5 0.158208 0.103258 -0.098477 11.000000 0.031720 = 0.023530 0.040250 -0.003690 0.004980 0.000180 S1 6 -0.250000 0.139648 0.000000 10.500000 0.024420 = 0.020380 0.035490 0.000000 0.000770 0.000000 H3A 2 0.041235 0.094199 -0.092414 11.000000 0.057060 H3B 2 0.205409 0.050881 -0.088613 11.000000 0.042980 HKLF 4 1 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 END HKLF 4 1 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 REM wn in I2/a REM R1= 0.0221 for 1141 Fo > 4sig(Fo) and 0.0243 for all 1221 data REM 109 parameters refined using 0 restraints cif: data_wn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H0 Cu N2 O6 S' _chemical_formula_weight 363.74 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' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 6.9815(7) _cell_length_b 13.8958(14) _cell_length_c 14.4131(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.620(4) _cell_angle_gamma 90.00 _cell_volume 1378.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 1.765 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3426 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1221 _reflns_number_gt 1141 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0266P)^2^+1.3460P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1221 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.000 _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 C1 C 0.4061(3) 0.30788(17) 0.18087(16) 0.0385(5) Uani 1 1 d . . . H1 H 0.4320 0.2484 0.2097 0.046 Uiso 1 1 calc R . . C2 C 0.4523(4) 0.3913(2) 0.23411(17) 0.0474(6) Uani 1 1 d . . . H2 H 0.5078 0.3869 0.2973 0.057 Uiso 1 1 calc R . . C3 C 0.4155(4) 0.47870(18) 0.19281(18) 0.0451(6) Uani 1 1 d . . . H3 H 0.4448 0.5345 0.2280 0.054 Uiso 1 1 calc R . . C4 C 0.3331(3) 0.48523(16) 0.09694(17) 0.0353(5) Uani 1 1 d . . . C5 C 0.2912(3) 0.39788(14) 0.04891(14) 0.0267(4) Uani 1 1 d . . . C6 C 0.2898(3) 0.57320(16) 0.04606(17) 0.0429(6) Uani 1 1 d . . . H6 H 0.3171 0.6316 0.0771 0.051 Uiso 1 1 calc R . . Cu1 Cu 0.2500 0.20021(2) 0.0000 0.02720(14) Uani 1 2 d S . . N1 N 0.3264(2) 0.31058(12) 0.09033(12) 0.0277(4) Uani 1 1 d . . . O1 O -0.0797(2) 0.19846(10) 0.03569(12) 0.0384(4) Uani 1 1 d . . . O2 O -0.2971(2) 0.07645(10) 0.07675(10) 0.0339(4) Uani 1 1 d . . . O3 O 0.1582(3) 0.10326(11) -0.09848(11) 0.0319(3) Uani 1 1 d . . . S1 S -0.2500 0.13965(5) 0.0000 0.02725(18) Uani 1 2 d S . . H3A H 0.041(4) 0.094(2) -0.0924(19) 0.057(9) Uiso 1 1 d . . . H3B H 0.205(4) 0.051(2) -0.0886(18) 0.043(8) Uiso 1 1 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 C1 0.0392(13) 0.0428(13) 0.0315(12) 0.0005(10) -0.0001(10) -0.0018(10) C2 0.0444(15) 0.0633(17) 0.0321(12) -0.0125(12) -0.0003(10) -0.0062(12) C3 0.0434(14) 0.0453(14) 0.0473(14) -0.0232(12) 0.0096(11) -0.0112(11) C4 0.0290(11) 0.0303(11) 0.0490(13) -0.0108(10) 0.0138(10) -0.0050(9) C5 0.0221(10) 0.0248(10) 0.0340(11) -0.0027(9) 0.0067(8) -0.0021(8) C6 0.0414(14) 0.0226(11) 0.0694(15) -0.0088(10) 0.0229(12) -0.0050(9) Cu1 0.0340(2) 0.0186(2) 0.0270(2) 0.000 -0.00067(15) 0.000 N1 0.0263(9) 0.0277(9) 0.0280(9) -0.0001(7) 0.0011(7) -0.0002(7) O1 0.0323(9) 0.0312(9) 0.0504(10) -0.0113(7) 0.0030(7) -0.0084(6) O2 0.0327(8) 0.0295(8) 0.0389(8) 0.0066(6) 0.0038(6) 0.0042(6) O3 0.0317(9) 0.0235(8) 0.0402(9) -0.0037(7) 0.0050(7) 0.0002(7) S1 0.0244(4) 0.0204(3) 0.0355(4) 0.000 0.0008(3) 0.000 _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 C1 N1 1.331(3) . ? C1 C2 1.397(3) . ? C1 H1 0.9300 . ? C2 C3 1.358(4) . ? C2 H2 0.9300 . ? C3 C4 1.408(4) . ? C3 H3 0.9300 . ? C4 C5 1.404(3) . ? C4 C6 1.432(3) . ? C5 N1 1.356(3) . ? C5 C5 1.431(4) 2 ? C6 C6 1.351(5) 2 ? C6 H6 0.9300 . ? Cu1 O3 1.9840(15) . ? Cu1 O3 1.9840(15) 2 ? Cu1 N1 2.0247(17) . ? Cu1 N1 2.0247(17) 2 ? O1 S1 1.4636(15) . ? O2 S1 1.4915(15) . ? O3 H3A 0.85(3) . ? O3 H3B 0.80(3) . ? S1 O1 1.4636(15) 2_455 ? S1 O2 1.4915(15) 2_455 ? 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 N1 C1 C2 122.4(2) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.5(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 120.3(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 116.5(2) . . ? C5 C4 C6 118.5(2) . . ? C3 C4 C6 125.1(2) . . ? N1 C5 C4 123.29(19) . . ? N1 C5 C5 116.56(11) . 2 ? C4 C5 C5 120.15(13) . 2 ? C6 C6 C4 121.36(13) 2 . ? C6 C6 H6 119.3 2 . ? C4 C6 H6 119.3 . . ? O3 Cu1 O3 94.46(10) . 2 ? O3 Cu1 N1 173.34(7) . . ? O3 Cu1 N1 92.03(7) 2 . ? O3 Cu1 N1 92.03(7) . 2 ? O3 Cu1 N1 173.34(7) 2 2 ? N1 Cu1 N1 81.52(9) . 2 ? C1 N1 C5 118.18(18) . . ? C1 N1 Cu1 129.13(15) . . ? C5 N1 Cu1 112.68(13) . . ? Cu1 O3 H3A 103.3(19) . . ? Cu1 O3 H3B 114.6(19) . . ? H3A O3 H3B 103(3) . . ? O1 S1 O1 112.11(13) . 2_455 ? O1 S1 O2 108.83(8) . 2_455 ? O1 S1 O2 109.56(9) 2_455 2_455 ? O1 S1 O2 109.56(9) . . ? O1 S1 O2 108.83(8) 2_455 . ? O2 S1 O2 107.86(12) 2_455 . ? 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 N1 C1 C2 C3 -0.1(4) . . . . ? C1 C2 C3 C4 -0.6(4) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? C2 C3 C4 C6 -179.4(2) . . . . ? C3 C4 C5 N1 -0.1(3) . . . . ? C6 C4 C5 N1 180.0(2) . . . . ? C3 C4 C5 C5 -179.5(2) . . . 2 ? C6 C4 C5 C5 0.6(4) . . . 2 ? C5 C4 C6 C6 0.1(4) . . . 2 ? C3 C4 C6 C6 -179.9(3) . . . 2 ? C2 C1 N1 C5 0.7(3) . . . . ? C2 C1 N1 Cu1 179.45(17) . . . . ? C4 C5 N1 C1 -0.6(3) . . . . ? C5 C5 N1 C1 178.8(2) 2 . . . ? C4 C5 N1 Cu1 -179.56(16) . . . . ? C5 C5 N1 Cu1 -0.1(3) 2 . . . ? O3 Cu1 N1 C1 166.7(5) . . . . ? O3 Cu1 N1 C1 -0.5(2) 2 . . . ? N1 Cu1 N1 C1 -178.8(2) 2 . . . ? O3 Cu1 N1 C5 -14.5(7) . . . . ? O3 Cu1 N1 C5 178.38(14) 2 . . . ? N1 Cu1 N1 C5 0.05(10) 2 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.219 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.052 |

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