Crystal structure of heptaguanidinium nonahydrogen bis[α-hexamolybdoplatinate(IV)] heptahydrate
Joo, Hea-Chung; Park, Ki-Min; Lee, Uk; Acta Crystallographica Section E 71 (2015) 268–271; doi:10.1107/S2056989015002601

data_2240422
_publ_section_title
;
 Crystal structure of heptaguanidinium nonahydrogen
 bis[\a-hexamolybdoplatinate(IV)] heptahydrate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              268
_journal_page_last               271
_journal_paper_doi               10.1107/S2056989015002601
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C H6 N3)7 H9 [Pt Mo6 O24]2, 7H2 O'
_chemical_formula_moiety         '7(C H6 N3 +), H9 Pt2 Mo12 O48 7-, 7(H2 O)'
_chemical_formula_structural     '(H9 Pt2 Mo12 O48), 7(H2 O), 7(C H6 N3+)'
_chemical_formula_sum            'C7 H65 Mo12 N21 O55 Pt2'
_chemical_formula_weight         2865.26
_chemical_name_systematic
;Heptaguanidinium nonahydrogen
bis[\a-hexamolybdoplatinate(IV)] heptahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 119.451(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.413(10)
_cell_length_b                   10.073(3)
_cell_length_c                   23.677(7)
_cell_measurement_reflns_used    9569
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.21
_cell_volume                     6524(4)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2009)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2009)'
_computing_data_reduction        <i>SAINT</i>
_computing_molecular_graphics
;ORTEP-3 for Windows (Farrugia, 2012), PLATON (Spek, 2009) and
 DIAMOND (Brandenburg,1998)
;
_computing_publication_material  <i>SHELXL97</i>
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'graphite multilayer'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            56606
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    6.617
_exptl_absorpt_correction_T_max  0.7290
_exptl_absorpt_correction_T_min  0.2407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' (SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5416
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.500
_refine_diff_density_min         -1.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7107
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0337P)^2^+47.9084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                6050
_reflns_number_total             7107
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2544sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        6524(3)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               2240422
_cod_database_fobs_code          2240422