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_2104891
_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          '[Mn(C3 H4 N2)4 V2 O6]'
_chemical_formula_moiety         'C12 H16 Mn N8 O6 V2'
_chemical_formula_structural     '[Mn(C3 H4 N2)4 V2 O6]'
_chemical_formula_sum            'C12 H16 Mn N8 O6 V2'
_chemical_formula_weight         525.13
_chemical_name_systematic
;
catena-tetrakis(imidazole)-tetrakis(\m~2~-oxo)-dioxo-manganese(ii)-di-vanadium
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   23.0354(3)
_cell_length_b                   23.0354(3)
_cell_length_c                   29.6005(3)
_cell_measurement_reflns_used    65033
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.55
_cell_volume                     15706.9(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP (Burnett & Johnson, 1996) and Diamond V.3e (Brandenburg & Putz, 2006)'
_computing_publication_material  'RAELS06 (Rae, 2006)'
_computing_structure_refinement  'RAELS06 (Rae, 2006)'
_computing_structure_solution    'SIR97 (Altomare, et al.,  1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            106159
_diffrn_reflns_reduction_process
;
Lorentz and polarization correction applied
;
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    1.61
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            Orange-yellow
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             8416.0
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.980
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.4695
_refine_ls_goodness_of_fit_ref   1.4695
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         8019
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0316
_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         0.0458
_reflns_number_gt                8019
_reflns_number_total             11464
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            gw5007.cif
_cod_data_source_block           Mn_100K
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2104891