Tripyridinium <i>cis</i>-tetrachloridodioxidomolybdate(VI) chloride
Fernandes, José A.; Gomes, Ana C.; Figueiredo, Sónia; Gago, Sandra; Ribeiro-Claro, Paulo J. A.; Gonçalves, Isabel S.; Almeida Paz, Filipe A.; Acta Crystallographica Section E 66 (2010) m862–m863; doi:10.1107/S1600536810023950

data_2226677
_publ_section_title
;
 Tripyridinium <i>cis</i>-tetrachloridodioxidomolybdate(VI) chloride
;
_journal_coeditor_code           SJ5018
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m862
_journal_page_last               m863
_journal_paper_doi               10.1107/S1600536810023950
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C5 H6 N)3 [Mo Cl4 O2] Cl'
_chemical_formula_moiety         '3(C5 H6 N +), Cl4 Mo O2 2-, Cl -'
_chemical_formula_sum            'C15 H18 Cl5 Mo N3 O2'
_chemical_formula_weight         545.51
_chemical_name_systematic
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Tripyridinium <i>cis</i>-tetrachloridodioxidomolybdate(VI) chloride
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.3972(2)
_cell_length_b                   11.3972(2)
_cell_length_c                   29.4265(9)
_cell_measurement_reflns_used    6207
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.08
_cell_measurement_theta_min      5.49
_cell_volume                     3310.29(13)
_computing_cell_refinement       'APEX2 and SAINT-Plus (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            33230
_diffrn_reflns_theta_full        36.31
_diffrn_reflns_theta_max         36.31
_diffrn_reflns_theta_min         5.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_T_max  0.8882
_exptl_absorpt_correction_T_min  0.8111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1998)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.684
_refine_ls_abs_structure_details 'Flack (1983), 4490 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         10395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+0.1830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                8105
_reflns_number_total             10395
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5018.cif
_cod_data_source_block           I
_cod_original_cell_volume        3310.28(13)
_cod_database_code               2226677
_cod_database_fobs_code          2226677