A new hybrid Dawson-type molybdenum arsenate derivative: (H~2~bpy)~3~[As~2~Mo~18~O~62~] (bpy = 4,4'-bipyridine)
Yu, Hai-hui; Zhang, Xiao; Kong, Li; Xu, Ji-qing; Acta Crystallographica Section E 65 (2009) m1698–m1699; doi:10.1107/S1600536809050260

data_2224198
_publ_section_title
;
 A new hybrid Dawson-type molybdenum arsenate derivative:
 (H~2~bpy)~3~[As~2~Mo~18~O~62~] (bpy = 4,4'-bipyridine)
;
_journal_coeditor_code           FI2091
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1698
_journal_page_last               m1699
_journal_paper_doi               10.1107/S1600536809050260
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C10 H10 N2)3 [As2 Mo18 O62]'
_chemical_formula_moiety         '3(C10 H10 N2 2+), As2 Mo18 O62 6-'
_chemical_formula_sum            'C30 H30 As2 Mo18 N6 O62'
_chemical_formula_weight         3343.36
_chemical_name_systematic
;
Tris(4,4'-bipyridinium) diarsenooctadecamolybdate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.023(2)
_cell_angle_beta                 94.243(2)
_cell_angle_gamma                107.166(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2671(17)
_cell_length_b                   12.1365(19)
_cell_length_c                   13.871(2)
_cell_measurement_reflns_used    4839
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6352
_cell_measurement_theta_min      3.2328
_cell_volume                     1694.6(4)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'ORTEP-3 (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14379
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         2.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.304
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_correction_T_min  0.504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1569
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.418
_refine_diff_density_min         -1.788
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0669P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                4986
_reflns_number_total             6545
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fi2091.cif
_cod_data_source_block           I
_cod_database_code               2224198
_cod_database_fobs_code          2224198