Redetermination of the crystal structure of 3,5-dimethylpyrazolium β-octamolybdate tetrahydrate
Amarante, Tatiana R.; Gonçalves, Isabel S.; Almeida Paz, Filipe A.; Acta Crystallographica Section E 71 (2015) m244–m245; doi:10.1107/S2056989015022823

data_2241397
_publ_section_title
;
 Redetermination of the crystal structure of 3,5-dimethylpyrazolium
 \b-octamolybdate tetrahydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m244
_journal_page_last               m245
_journal_paper_doi               10.1107/S2056989015022823
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C5 H9 N2)4 [Mo8 O26], 4H2 O'
_chemical_formula_moiety         '4(C5 H9 N2 +), Mo8 O26 4-, 4(H2 O)'
_chemical_formula_sum            'C20 H44 Mo8 N8 O30'
_chemical_formula_weight         1644.15
_chemical_name_systematic
;
Tetrakis(3,5-dimethylpyrazolium) \b-octamolybdate  tetrahydrate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                64.103(3)
_cell_angle_beta                 84.272(3)
_cell_angle_gamma                75.826(3)
_cell_formula_units_Z            1
_cell_length_a                   10.1105(9)
_cell_length_b                   10.7469(9)
_cell_length_c                   11.9839(10)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.64
_cell_volume                     1135.67(17)
_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, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0423
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25625
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.739
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.236
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.404
_exptl_crystal_description       Plate
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.535
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4141
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.001
_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^+2.2481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                3175
_reflns_number_total             4141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7547sup1.cif
_cod_data_source_block           I
_cod_database_code               2241397
_shelx_estimated_absorpt_t_min   0.663
_shelx_estimated_absorpt_t_max   0.978
_shelx_hkl_checksum              80242
_shelx_res_checksum              76921
_shelxl_version_number           2014/6
_cod_database_fobs_code 2241397