Synthesis and crystal structure of a new hybrid organic–inorganic material containing neutral molecules, cations and heptamolybdate anions
Sarr, Bougar; Mbaye, Abdou; Diallo, Wally; Diop, Cheikh Abdoul Khadir; Sidibe, Mamadou; Michaud, Francois; Acta Crystallographica Section E 75 (2019) 1001–1004; doi:10.1107/S2056989019008454

data_2242992
_publ_section_title
;
 Synthesis and crystal structure of a new hybrid organic--inorganic
 material containing neutral molecules, cations and heptamolybdate anions
;
_journal_coeditor_code           HB7831
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1001
_journal_page_last               1004
_journal_paper_doi               10.1107/S2056989019008454
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '(C4 H7 N2)6 [Mo7 O24], 2C4 H6 N2, 2H2 O'
_chemical_formula_moiety
'6(C4 H7 N2 +), Mo7 O24 6-, 2(C4 H6 N2), 2(H2 O)'
_chemical_formula_sum            'C32 H58 Mo7 N16 O26'
_chemical_formula_weight         1754.52
_chemical_name_systematic
;
Hexakis(2-methyl-1<i>H</i>-imidazol-3-ium) heptamolybdate
2-methyl-1<i>H</i>-imidazole disolvate dihydrate
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.6530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5325(2)
_cell_length_b                   17.5842(2)
_cell_length_c                   19.8873(2)
_cell_measurement_reflns_used    38522
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      37.413
_cell_measurement_theta_min      3.543
_cell_volume                     5781.08(11)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1992)
;
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            104921
_diffrn_reflns_theta_full        36.32
_diffrn_reflns_theta_max         36.32
_diffrn_reflns_theta_min         3.32
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_T_max  0.7558
_exptl_absorpt_correction_T_min  0.4761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'fragment of prism'
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.828
_refine_diff_density_min         -2.872
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         27993
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+11.2859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.104
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                21593
_reflns_number_total             27993
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7831sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2242992
_cod_database_fobs_code          2242992