Two polyoxometallate-based supramolecular compounds influenced by the ratio between the polyoxometallate anion and organic cation
Zhang, Qian; Liu, Jie; Lu, Jing; Gong, Shu-Wen; Acta Crystallographica Section C 69 (2013) 588–593; doi:10.1107/S0108270113011554

data_2019020
_publ_section_title
;
 Two polyoxometallate-based supramolecular compounds influenced by the
 ratio between the polyoxometallate anion and organic cation
;
_journal_coeditor_code           YF3031
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              588
_journal_page_last               593
_journal_paper_doi               10.1107/S0108270113011554
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'(C10 H16 N4) (C10 H15 N4) [P Mo12 O40] , 2H2 O'
_chemical_formula_moiety
'C10 H16 N4 2+, C10 H15 N4 +, P Mo12 O40 3-, 2(H2 O)'
_chemical_formula_sum            'C20 H34 Mo12 N8 O42 P'
_chemical_formula_weight         2240.80
_chemical_name_systematic
;
1,1'-(butane-1,4-diyl)bis(1<i>H</i>-imidazol-3-ium)
1-[4-(1<i>H</i>-imidazol-1-yl)butyl]-1<i>H</i>-imidazol-3-ium
tetracosa-\m~2~-oxido-dodecaoxido-\m~12~-phosphato-dodecamolybdenum(VI)
dihydrate
;
_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           SHELXL97
_cell_angle_alpha                102.1940(10)
_cell_angle_beta                 98.1840(10)
_cell_angle_gamma                115.998(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2350(12)
_cell_length_b                   11.7211(13)
_cell_length_c                   11.8459(13)
_cell_measurement_reflns_used    4586
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.83
_cell_volume                     1320.5(3)
_computing_cell_refinement       'SMART (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6912
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.891
_exptl_absorpt_correction_T_max  0.5955
_exptl_absorpt_correction_T_min  0.5687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1065
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.625
_refine_diff_density_min         -1.424
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     1285
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+18.6135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                3425
_reflns_number_total             4586
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yf3031.cif
_cod_data_source_block           II
_cod_original_cell_volume        1320.5(2)
_cod_database_code               2019020
_cod_database_fobs_code          2019020