Tetrapyridinium μ-oxido-di-μ-sulfato-bis[chloridodioxidomolybdate(VI)]
Fernandes, José A.; Gomes, Ana C.; Figueiredo, Sónia; Gago, Sandra; Lopes, André D.; Pillinger, Martyn; Ribeiro-Claro, Paulo J. A.; Gonçalves, Isabel S.; Almeida Paz, Filipe A.; Acta Crystallographica Section E 66 (2010) m1005–m1006; doi:10.1107/S1600536810028254

data_2227102
_publ_section_title
;
 Tetrapyridinium
 \m-oxido-di-\m-sulfato-bis[chloridodioxidomolybdate(VI)]
;
_journal_coeditor_code           TK2692
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1005
_journal_page_last               m1006
_journal_paper_doi               10.1107/S1600536810028254
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C5 H6 N)4 [Mo2 Cl2 O5 (S O4)2]'
_chemical_formula_moiety         '4(C5 H6 N +), Cl2 Mo2 O13 S2 4-'
_chemical_formula_sum            'C20 H24 Cl2 Mo2 N4 O13 S2'
_chemical_formula_weight         855.33
_chemical_name_systematic
;
Tetrapyridinium \m-oxido-di-\m-sulfato-bis[chloridodioxidomolybdate(VI)]
;
_space_group_IT_number           14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.07(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   10.517(4)
_cell_length_b                   49.281(15)
_cell_length_c                   17.557(6)
_cell_measurement_reflns_used    1387
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.79
_cell_measurement_theta_min      3.93
_cell_volume                     9064(5)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEXII'
_diffrn_measurement_method       '\w/\f scans'
_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  0.2547
_diffrn_reflns_av_sigmaI/netI    0.2881
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49290
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  0.9880
_exptl_absorpt_correction_T_min  0.9645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1998)
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             5112
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.075
_refine_diff_density_min         -1.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         16283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.2563
_refine_ls_R_factor_gt           0.0979
_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^)+(0.1162P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2046
_refine_ls_wR_factor_ref         0.2860
_reflns_number_gt                6037
_reflns_number_total             16283
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2692.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2227102
_cod_database_fobs_code          2227102