Tris[3,3'-(<i>p</i>-phenylenedimethylene)diimidazol-1-ium] bis(phosphatododecamolybdate)
Yuan, Ji-Hong; Wang, Cheng; Yu, Ming-Juan; Li, Jing; Acta Crystallographica Section E 64 (2008) m831–; doi:10.1107/S1600536808014463

data_2218370
_publ_section_title
;
 Tris[3,3'-(<i>p</i>-phenylenedimethylene)diimidazol-1-ium]
 bis(phosphatododecamolybdate)
;
_journal_coeditor_code           CS2077
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m831
_journal_paper_doi               10.1107/S1600536808014463
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C14 H16 N4)3 [P Mo12 O40]2'
_chemical_formula_moiety         '3(C14 H16 N4 2+), 2(Mo12 O40 P 3-)'
_chemical_formula_sum            'C42 H48 Mo24 N12 O80 P2'
_chemical_formula_weight         4365.42
_chemical_name_systematic
;
bis(phosphatododecamolybdate)
;
_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                73.3820(10)
_cell_angle_beta                 87.2970(10)
_cell_angle_gamma                67.5570(10)
_cell_formula_units_Z            1
_cell_length_a                   11.8790(4)
_cell_length_b                   12.5030(4)
_cell_length_c                   18.4180(6)
_cell_measurement_reflns_used    8978
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      1.84
_cell_volume                     2416.76(14)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15040
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  0.536
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2062
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.812
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         11046
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+0.7857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                9555
_reflns_number_total             11046
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cs2077.cif
_cod_data_source_block           I
_cod_database_code               2218370
_cod_database_fobs_code          2218370