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_2019019
_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)3 [P Mo12 O40]2'
_chemical_formula_moiety         '3(C10 H16 N4 2+), 2(P Mo12 O40 3-)'
_chemical_formula_sum            'C30 H48 Mo24 N12 O80 P2'
_chemical_formula_weight         4221.30
_chemical_name_systematic
;
Tris[1,1'-(butane-1,4-diyl)bis(1<i>H</i>-imidazol-3-ium)]
bis[tetracosa-\m~2~-oxido-dodecaoxido-\m~12~-phosphato-dodecamolybdenum(VI)]
;
_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                74.134(2)
_cell_angle_beta                 71.0440(10)
_cell_angle_gamma                71.8720(10)
_cell_formula_units_Z            1
_cell_length_a                   11.8380(10)
_cell_length_b                   12.1071(11)
_cell_length_c                   17.8029(18)
_cell_measurement_reflns_used    7806
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.80
_cell_volume                     2250.9(4)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11740
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.378
_exptl_absorpt_correction_T_max  0.7288
_exptl_absorpt_correction_T_min  0.5515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1990
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.711
_refine_diff_density_min         -1.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         7806
_refine_ls_number_restraints     380
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0358P)^2^+12.8740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                5770
_reflns_number_total             7806
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yf3031.cif
_cod_data_source_block           I
_cod_database_code               2019019
_cod_database_fobs_code          2019019