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zou_jiyong

金虫 (小有名气)

应助: 11 (小学生)
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帖子: 191
在线: 1465.9小时
虫号: 946356
注册: 2010-01-21
性别: GG
专业: 配位化学

[交流] 【请教】cif问题已有7人参与

我是个菜鸟，自己瞎整的，哪位大虾帮忙看看该CIF文件是否正确
data_p100617d

_audit_creation_method          SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common          ?
_chemical_melting_point          ?
_chemical_formula_moiety       ?
_chemical_formula_sum
'C4 H4.67 Cu0.67 N4 O4'
_chemical_formula_weight       215.14

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'
'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'
'H'  'H' 0.0000 0.0000
'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, -y, -z'

_cell_length_a                   6.7683(7)
_cell_length_b                   8.8573(10)
_cell_length_c                   9.9815(10)
_cell_angle_alpha                68.473(10)
_cell_angle_beta                75.425(9)
_cell_angle_gamma                88.442(9)
_cell_volume                   537.31(10)
_cell_formula_units_Z          3
_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    1.995
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             324
_exptl_absorpt_coefficient_mu    2.072
_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          3984
_diffrn_reflns_av_R_equivalents 0.0275
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min       2.48
_diffrn_reflns_theta_max       28.87
_reflns_number_total             2435
_reflns_number_gt                2092
_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^)+(0.0503P)^2^+0.2121P] 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       2435
_refine_ls_number_parameters    187
_refine_ls_number_restraints    4
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt          0.0380
_refine_ls_wR_factor_ref       0.0987
_refine_ls_wR_factor_gt          0.0961
_refine_ls_goodness_of_fit_ref 1.101
_refine_ls_restrained_S_all    1.102
_refine_ls_shift/su_max          12.534
_refine_ls_shift/su_mean       0.072

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
Cu0A Cu 0.65314(5) 1.06587(4) 0.78351(4) 0.01098(13) Uani 1 1 d D . .
O O 0.1308(3) 0.3810(2) 1.1002(2) 0.0118(4) Uani 1 1 d . . .
O0AA O 0.2925(3) 0.4606(2) 0.8614(2) 0.0130(4) Uani 1 1 d . . .
H0A H 0.3546 0.5435 0.7954 0.020 Uiso 1 1 calc R . .
O1AA O 0.5153(3) 0.7070(3) 0.6572(2) 0.0172(5) Uani 1 1 d . . .
O2AA O 0.6520(3) 0.9372(3) 0.6514(2) 0.0170(5) Uani 1 1 d . . .
O3AA O 0.3020(4) 0.1618(3) 0.6835(3) 0.0348(6) Uani 1 1 d . . .
O4AA O 0.9448(4) 0.9572(3) 0.8259(4) 0.0535(10) Uani 1 1 d D . .
N N 0.9392(4) 1.3985(3) 0.3747(3) 0.0145(5) Uani 1 1 d . . .
N0AA N 0.3633(4) 0.8150(3) 1.0788(3) 0.0113(5) Uani 1 1 d . . .
N1AA N 0.2656(4) 0.6728(3) 1.1128(3) 0.0112(5) Uani 1 1 d . . .
N2AA N 0.4689(4) 0.8746(3) 0.9346(3) 0.0106(5) Uani 1 1 d . . .
N3AA N 0.8136(4) 1.5022(3) 0.4234(3) 0.0139(5) Uani 1 1 d . . .
N4AA N 0.7786(4) 1.2538(3) 0.6021(2) 0.0107(5) Uani 1 1 d . . .
C C 0.7202(5) 1.4089(4) 0.5602(3) 0.0131(6) Uani 1 1 d . . .
H H 0.6226 1.4455 0.6232 0.016 Uiso 1 1 calc R . .
C0AA C 0.9170(4) 1.2533(4) 0.4808(3) 0.0143(6) Uani 1 1 d . . .
H0AA H 0.9870 1.1641 0.4724 0.017 Uiso 1 1 calc R . .
C2BA C 0.3098(4) 0.6400(3) 0.9876(3) 0.0089(5) Uani 1 1 d . . .
C3BA C 0.5420(4) 0.8057(3) 0.7156(3) 0.0120(6) Uani 1 1 d . . .
C4AA C 0.4371(4) 0.7680(3) 0.8750(3) 0.0089(5) Uani 1 1 d . . .
C4BA C 0.2362(4) 0.4840(3) 0.9874(3) 0.0093(6) Uani 1 1 d . . .
H3AA H 0.256(9) 0.278(8) 0.679(6) 0.089(19) Uiso 1 1 d . . .
H3AB H 0.253(4) 0.159(4) 0.798(3) 0.000(7) Uiso 1 1 d . . .
H4AA H 0.944(4) 0.857(2) 0.864(3) 0.000 Uiso 1 1 d D . .
H4AB H 1.053(3) 1.010(3) 0.789(3) 0.000 Uiso 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
Cu0A 0.0150(2) 0.00763(19) 0.00745(19) -0.00265(14) 0.00230(13) -0.00449(13)
O 0.0125(10) 0.0088(10) 0.0116(10) -0.0027(8) 0.0001(8) -0.0026(8)
O0AA 0.0154(11) 0.0092(10) 0.0134(10) -0.0052(8) 0.0001(8) -0.0032(8)
O1AA 0.0238(12) 0.0141(11) 0.0128(10) -0.0084(9) 0.0026(9) -0.0063(9)
O2AA 0.0223(12) 0.0115(10) 0.0131(10) -0.0064(8) 0.0064(8) -0.0079(9)
O3AA 0.0347(15) 0.0257(14) 0.0385(16) -0.0072(12) -0.0073(12) 0.0029(12)
O4AA 0.0172(14) 0.0105(13) 0.121(3) -0.0102(16) -0.0203(17) 0.0008(11)
N 0.0134(12) 0.0164(13) 0.0106(12) -0.0034(10) 0.0001(9) -0.0024(10)
N0AA 0.0144(12) 0.0098(12) 0.0067(11) -0.0014(9) 0.0004(9) -0.0035(9)
N1AA 0.0122(12) 0.0089(12) 0.0105(12) -0.0024(9) -0.0010(9) -0.0033(9)
N2AA 0.0129(12) 0.0082(11) 0.0087(11) -0.0018(9) -0.0008(9) -0.0014(9)
N3AA 0.0174(13) 0.0118(12) 0.0111(12) -0.0024(10) -0.0037(10) -0.0009(10)
N4AA 0.0139(12) 0.0105(12) 0.0063(11) -0.0039(9) 0.0012(9) -0.0024(9)
C 0.0169(15) 0.0116(14) 0.0116(14) -0.0054(11) -0.0034(11) -0.0015(11)
C0AA 0.0120(14) 0.0151(15) 0.0139(14) -0.0047(12) -0.0009(11) 0.0001(11)
C2BA 0.0090(13) 0.0071(13) 0.0096(13) -0.0019(10) -0.0027(10) 0.0016(10)
C3BA 0.0126(14) 0.0109(14) 0.0105(14) -0.0036(11) 0.0002(11) -0.0004(11)
C4AA 0.0084(13) 0.0085(13) 0.0102(13) -0.0041(11) -0.0023(10) 0.0019(10)
C4BA 0.0057(13) 0.0102(13) 0.0124(13) -0.0039(11) -0.0037(10) 0.0018(10)

_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
Cu0A N4AA 1.965(2) . ?
Cu0A N2AA 1.999(2) . ?
Cu0A N0AA 1.999(2) 2_677 ?
Cu0A O2AA 2.036(2) . ?
Cu0A O4AA 2.241(3) . ?
O C4BA 1.219(3) . ?
O0AA C4BA 1.309(3) . ?
O1AA C3BA 1.255(4) . ?
O2AA C3BA 1.257(3) . ?
N C0AA 1.314(4) . ?
N N3AA 1.371(4) . ?
N0AA N1AA 1.326(3) . ?
N0AA N2AA 1.343(3) . ?
N0AA Cu0A 1.999(2) 2_677 ?
N1AA C2BA 1.344(4) . ?
N2AA C4AA 1.334(4) . ?
N3AA C 1.309(4) . ?
N4AA C0AA 1.333(4) . ?
N4AA C 1.361(4) . ?
C2BA C4AA 1.386(4) . ?
C2BA C4BA 1.483(4) . ?
C3BA C4AA 1.483(4) . ?

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
N4AA Cu0A N2AA 163.65(10) . . ?
N4AA Cu0A N0AA 94.75(10) . 2_677 ?
N2AA Cu0A N0AA 95.04(10) . 2_677 ?
N4AA Cu0A O2AA 88.11(9) . . ?
N2AA Cu0A O2AA 81.65(9) . . ?
N0AA Cu0A O2AA 176.32(9) 2_677 . ?
N4AA Cu0A O4AA 96.99(11) . . ?
N2AA Cu0A O4AA 95.52(10) . . ?
N0AA Cu0A O4AA 93.14(12) 2_677 . ?
O2AA Cu0A O4AA 88.79(12) . . ?
C3BA O2AA Cu0A 114.28(18) . . ?
C0AA N N3AA 110.4(2) . . ?
N1AA N0AA N2AA 110.7(2) . . ?
N1AA N0AA Cu0A 125.68(18) . 2_677 ?
N2AA N0AA Cu0A 123.57(19) . 2_677 ?
N0AA N1AA C2BA 106.7(2) . . ?
C4AA N2AA N0AA 107.4(2) . . ?
C4AA N2AA Cu0A 111.22(19) . . ?
N0AA N2AA Cu0A 141.3(2) . . ?
C N3AA N 102.6(2) . . ?
C0AA N4AA C 103.5(2) . . ?
C0AA N4AA Cu0A 127.7(2) . . ?
C N4AA Cu0A 127.95(19) . . ?
N3AA C N4AA 114.0(3) . . ?
N C0AA N4AA 109.5(3) . . ?
N1AA C2BA C4AA 108.2(2) . . ?
N1AA C2BA C4BA 121.4(2) . . ?
C4AA C2BA C4BA 130.4(3) . . ?
O1AA C3BA O2AA 126.0(3) . . ?
O1AA C3BA C4AA 118.8(3) . . ?
O2AA C3BA C4AA 115.3(3) . . ?
N2AA C4AA C2BA 107.0(2) . . ?
N2AA C4AA C3BA 117.6(3) . . ?
C2BA C4AA C3BA 135.4(3) . . ?
O C4BA O0AA 121.5(3) . . ?
O C4BA C2BA 121.4(3) . . ?
O0AA C4BA C2BA 117.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.860
_diffrn_reflns_theta_full             28.87
_diffrn_measured_fraction_theta_full 0.860
_refine_diff_density_max 1.197
_refine_diff_density_min -0.542
_refine_diff_density_rms 0.112

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