New Hydrogen Bond-Supported 3-D Molecular Assembly from Polyoxovanadate and Tetramethylbiimidazole
Hitoshi Kumagai; Masashi Arishima; Susumu Kitagawa; Koichi Ymada; Satoshi Kawata; Sumio Kaizaki; Inorganic Chemistry 41 (2002) 1989–1992; doi:10.1021/ic010599j

data_4317758
_publ_section_title
;
 New Hydrogen Bond-Supported 3-D Molecular Assembly from Polyoxovanadate
 and Tetramethylbiimidazole
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1989
_journal_page_last               1992
_journal_paper_doi               10.1021/ic010599j
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C20 H42 N8 O32 V10 '
_chemical_formula_sum            'C20 H42 N8 O32 V10'
_chemical_formula_weight         1416.00
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Fri Feb 25 13:00:19 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 94.90(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.151(4)
_cell_length_b                   13.127(8)
_cell_length_c                   13.925(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      10.1
_cell_volume                     2213(2)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  SHELXL93
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.07329
_diffrn_orient_matrix_UB_12      -0.02729
_diffrn_orient_matrix_UB_13      -0.02630
_diffrn_orient_matrix_UB_21      -0.02102
_diffrn_orient_matrix_UB_22      -0.01099
_diffrn_orient_matrix_UB_23      0.06711
_diffrn_orient_matrix_UB_31      -0.03176
_diffrn_orient_matrix_UB_32      0.07027
_diffrn_orient_matrix_UB_33      0.00028
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.101
_diffrn_reflns_av_sigmaI/netI    0.211
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3653
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.05
_diffrn_standards_decay_%        -0.81
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    17.914
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.125
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1408.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.61
_refine_diff_density_rms         0.13
_refine_ls_extinction_coef       0.0001
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.995
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         0
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.2210
_refine_ls_R_factor_obs          0.0644
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1933
_reflns_number_observed          0
_reflns_number_total             0
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            ic010599j.cif
_cod_data_source_block           VO(bim)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not 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^) +
(0.0680P)^2^+0.0000P] 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^) +
(0.0680P)^2^+0.0000P] 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        2213(1)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C20 H42 N8 O32 V10 '
_cod_database_code               4317758