[Ni(C~10~H~8~N~2~)~3~]~2~[V~4~O~12~].11H~2~O
Guo-Yu Yang; Da-Wei Gao; Ying Chen; Ji-Qing Xu; Qing-Xin Zeng; Hao-Ran Sun; Zhi-Wu Pei; Qiang Su; Yan Xing; Yong-Hua Ling; Heng-Qing Jia; Acta Crystallographica Section C 54 (1998) 616–618; doi:10.1107/S0108270197018751

data_2007290
_publ_section_title
;
 [Ni(C~10~H~8~N~2~)~3~]~2~[V~4~O~12~].11H~2~O
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              616
_journal_page_last               618
_journal_paper_doi               10.1107/S0108270197018751
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Ni(C10 H8 N2)3]2 [V4 O12], 11H2 O'
_chemical_formula_sum            'C60 H70 N12 Ni2 O23 V4'
_chemical_formula_weight         1648.46
_chemical_name_systematic        ' ?'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 105.7450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.880(2)
_cell_length_b                   13.9180(10)
_cell_length_c                   23.829(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.73
_cell_measurement_theta_min      4.715
_cell_volume                     6984.3(10)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'SHELXTL-Plus (Siemens, 1990)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w--2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7528
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.667
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   '\y scans (North et al., 1968)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.962
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_hydrogen_treatment
;
All H atoms except those of water were
  refined and assigned U~iso~ = 0.08\%A^2^
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         6153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_obs          .0376
_refine_ls_shift/esd_max         0.010
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0672P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1077
_refine_ls_wR_factor_obs         .1016
_reflns_number_observed          4659
_reflns_number_total             6153
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            ta1193.cif
_cod_data_source_block           YANG-27
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0672P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0672P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6984.30(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2007290