Bis(4,4'-bipyridinium) bis(μ~5~-hydrogen phosphate)pentakis(μ~2~-oxido)decaoxidopentamolybdate dihydrate
Wu-Hua Chen; Yong Xiang; Zhan-Feng Chen; Qiu-Mu Wu; Qing-Xin Zeng; Acta Crystallographica Section E 63 (2007) m2245–m2246; doi:10.1107/S1600536807033119

data_2214860
_publ_section_title
;
 Bis(4,4'-bipyridinium) bis(\m~5~-hydrogen
 phosphate)pentakis(\m~2~-oxido)decaoxidopentamolybdate dihydrate
;
_journal_coeditor_code           SI2017
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2245
_journal_page_last               m2246
_journal_paper_doi               10.1107/S1600536807033119
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C10 H10 N2)2 [Mo5 O15 (H P O4)2], 2H2 O'
_chemical_formula_moiety         '2(C10 H10 N2 2+), H2 Mo5 O23 P2 4-, 2(H2 O)'
_chemical_formula_sum            'C20 H26 Mo5 N4 O25 P2'
_chemical_formula_weight         1264.09
_chemical_name_systematic
;
 bis(4,4'-bipyridinium) bis(\m~5~-hydrogen
phosphate)pentakis(\m~2~-oxido)decaoxidopentamolybdate dihydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.823(2)
_cell_length_b                   18.307(4)
_cell_length_c                   31.517(6)
_cell_measurement_reflns_used    58657
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.10
_cell_volume                     6822(2)
_computing_cell_refinement       Rapid-Auto
_computing_data_collection       'Rapid-Auto (Rigaku, 2004)'
_computing_data_reduction        Rapid-Auto
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER'
_diffrn_measurement_method       '\w oscillation'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            58657
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  0
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_T_max  0.8880
_exptl_absorpt_correction_T_min  0.7880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4912
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.532
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         7810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0204
_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^)+(0.0232P)^2^+8.9692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0517
_reflns_number_gt                6885
_reflns_number_total             7810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            si2017.cif
_cod_data_source_block           I
_cod_original_cell_volume        6821(2)
_cod_database_code               2214860
_cod_database_fobs_code          2214860