Bis{4,4'-[oxalylbis(azanediyl)]dipyridinium} octamolybdate
Qin, Jianbo; Dong, Jingren; Li, Jinghua; Gong, Yun; Acta Crystallographica Section E 66 (2010) m743–; doi:10.1107/S1600536810020714

data_2226691
_publ_section_title
;
 Bis{4,4'-[oxalylbis(azanediyl)]dipyridinium} octamolybdate
;
_journal_coeditor_code           SU2182
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m743
_journal_paper_doi               10.1107/S1600536810020714
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C12 H12 N4 O2)2 [Mo8 O26]'
_chemical_formula_moiety         '2(C12 H12 N4 O2 2+), Mo8 O26 4-'
_chemical_formula_sum            'C24 H24 Mo8 N8 O30'
_chemical_formula_weight         1672.03
_chemical_name_systematic
;
Bis{4,4'-[oxalylbis(azanediyl)]dipyridinium} octamolybdate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 101.553(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.633(2)
_cell_length_b                   11.552(2)
_cell_length_c                   17.240(4)
_cell_measurement_reflns_used    5569
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4797
_cell_measurement_theta_min      2.1355
_cell_volume                     2074.7(7)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Siemens CCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14669
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.451
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.401
_refine_diff_density_min         -2.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.395
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.395
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0540P)^2^+0.4946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                4215
_reflns_number_total             4534
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2182.cif
_cod_data_source_block           I
_cod_original_cell_volume        2074.7(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2226691
_cod_database_fobs_code          2226691