Investigation of the structure and phase transitions of the polymeric inorganic‒organic hybrids: [<i>M</i>(Im)~4~V~2~O~6~]~{∞~}; <i>M</i> = Mn, Co, Ni, Im = imidazole
Chainok, Kittipong; Haller, Kenneth J.; Rae, A. David; Willis, Anthony C.; Williams, Ian D.; Acta Crystallographica Section B 67 (2011) 41–52; doi:10.1107/S0108768110042941

data_2104900
_publ_section_title
;
 Investigation of the structure and phase transitions of the polymeric
 inorganic--organic hybrids: [<i>M</i>(Im)~4~V~2~O~6~]~{\\infty ~};
 <i>M</i> = Mn, Co, Ni, Im = imidazole
;
_journal_coeditor_code           GW5007
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              41
_journal_page_last               52
_journal_paper_doi               10.1107/S0108768110042941
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni(C3 H4 N2)4 V2 O6]'
_chemical_formula_moiety         'C12 H16 N8 Ni O6 V2'
_chemical_formula_structural     '[Ni(C3 H4 N2)4 V2 O6]'
_chemical_formula_sum            'C12 H16 N8 Ni O6 V2'
_chemical_formula_weight         528.904
_chemical_name_systematic
;
catena-tetrakis(imidazole)-tetrakis(\m~2~-oxo)-dioxo-nickel(ii)-di-vanadium
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.1205(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.1379(3)
_cell_length_b                   14.3657(2)
_cell_length_c                   16.3422(4)
_cell_measurement_reflns_used    69838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.55
_cell_volume                     3788.64(13)
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius KappaCCD'
_diffrn_measurement_method       '\f scan plus \w scans with \k offsets'
_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  0.055
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53813
_diffrn_reflns_reduction_process
;
Lorentz and polarization correction applied
;
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    2.000
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.30
_refine_diff_density_min         -2.32
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.6677
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         9089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0
_refine_ls_restrained_S_obs      0
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.2
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s(F)^2^ + (0.0004F)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                9089
_reflns_number_total             11073
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            gw5007.cif
_cod_data_source_block           Ni_100K
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2104900