Crystal structure of an organic–inorganic supramolecular salt based on a 4,4'-methylenebis(3,5-dimethyl-1<i>H</i>-pyrazol-2-ium) cation and a β-octamolybdate anion
Amarante, Tatiana R.; Gonçalves, Isabel S.; Almeida Paz, Filipe A.; Acta Crystallographica Section E 72 (2016) 124–127; doi:10.1107/S2056989015024524

data_2241452
_publ_section_title
;
 Crystal structure of an organic--inorganic supramolecular salt based on a
 4,4'-methylenebis(3,5-dimethyl-1<i>H</i>-pyrazol-2-ium) cation and a
 \b-octamolybdate anion
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              124
_journal_page_last               127
_journal_paper_doi               10.1107/S2056989015024524
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '(C11 H18 N4) [Mo8 O26]'
_chemical_formula_moiety         '2(C11 H18 N4 2+), Mo8 O26 4-'
_chemical_formula_sum            'C22 H36 Mo8 N8 O26'
_chemical_formula_weight         1596.11
_chemical_name_systematic
;
Bis[4,4'-methylenebis(3,5-dimethyl-1<i>H</i>-pyrazol-2-ium)] \b-octamolybdate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'SHELXL-2014/6, manual editing plus enCIFer'
_cell_angle_alpha                113.343(3)
_cell_angle_beta                 110.629(4)
_cell_angle_gamma                96.540(4)
_cell_formula_units_Z            1
_cell_length_a                   8.6394(10)
_cell_length_b                   12.0694(13)
_cell_length_c                   12.2249(14)
_cell_measurement_reflns_used    9149
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      2.53
_cell_volume                     1046.6(2)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w / \f scans'
_diffrn_radiation_monochromator  'Multi-layer X-ray mirror'
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            58761
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.128
_diffrn_reflns_theta_min         3.562
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.415
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.532
_exptl_crystal_description       Plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5605
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+0.8837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0449
_reflns_number_gt                4669
_reflns_number_total             5605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            gk2651sup1.cif
_cod_data_source_block           I
_cod_database_code               2241452
_cod_database_fobs_code          2241452
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.713
_shelx_hkl_checksum              7370
_shelx_res_checksum              44036
_shelxl_version_number           2014/6