Bis(3,5-dimethylpyrazolium) bis(hydroxonium) β-octamolybdate(VI) ethanol disolvate
Deng, Zhao-Peng; Gao, Shan; Huo, Li-Hua; Zhao, Hui; Acta Crystallographica Section E 61 (2005) m2553–m2555; doi:10.1107/S1600536805035968

data_2207542
_publ_section_title
;
 Bis(3,5-dimethylpyrazolium) bis(hydroxonium) \b-octamolybdate(VI)
 ethanol disolvate
;
_journal_coeditor_code           HB6295
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2553
_journal_page_last               m2555
_journal_paper_doi               10.1107/S1600536805035968
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C5 H9 N2)2 (H3 O)2 [Mo8 O26] , 2C2 H6 O'
_chemical_formula_moiety         '2C5 H9 N2 + , 2H3 O + , Mo8 O26 4- , 2C2 H6 O'
_chemical_formula_sum            'C14 H36 Mo8 N4 O30'
_chemical_formula_weight         1507.99
_chemical_name_systematic
;
Bis(3,5-dimethylpyrazolium) bis(hydroxonium) \b-octamolybdate(VI)
diethanol solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                93.72(3)
_cell_angle_beta                 97.55(3)
_cell_angle_gamma                111.96(3)
_cell_formula_units_Z            1
_cell_length_a                   8.9910(18)
_cell_length_b                   10.475(2)
_cell_length_c                   11.441(2)
_cell_measurement_reflns_used    9165
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.06
_cell_volume                     983.0(4)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_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  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9637
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.567
_exptl_absorpt_correction_T_max  0.635
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    2.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.638
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4427
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0242P)^2^+1.8158P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                3936
_reflns_number_total             4427
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6295.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap and geom' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_database_code               2207542
_cod_database_fobs_code          2207542