Anhydrous pentaguanidinium dihydrogen nonavanado(IV)platinate(IV)
Joo, Hea-Chung; Park, Ki-Min; Lee, Uk; Acta Crystallographica Section E 67 (2011) m1801–m1802; doi:10.1107/S1600536811049166

data_2233051
_publ_section_title
;
 Anhydrous pentaguanidinium dihydrogen nonavanado(IV)platinate(IV)
;
_journal_coeditor_code           ZL2427
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1801
_journal_page_last               m1802
_journal_paper_doi               10.1107/S1600536811049166
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C H6 N3)5 [H2 Pt V9 O28]'
_chemical_formula_moiety         '5(C H6 N3 +), H2 O28 Pt V9 5-'
_chemical_formula_sum            'C5 H32 N15 O28 Pt V9'
_chemical_formula_weight         1404.01
_chemical_name_systematic
;
pentaguanidinium dihydrogen nonavanado(IV)platinate(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 91.1430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8861(3)
_cell_length_b                   18.5137(5)
_cell_length_c                   15.2299(4)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.33
_cell_volume                     3632.66(16)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2009)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2009)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2009)'
_computing_molecular_graphics
'<i>ORTEP-3</i> (Farrugia, 1997) and <i>DIAMOND</i> (Brandenburg, 1998)'
_computing_publication_material  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      147(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35027
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.153
_exptl_absorpt_correction_T_max  0.3054
_exptl_absorpt_correction_T_min  0.1868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal prism'
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.021
_refine_diff_density_min         -0.749
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         9026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0349P)^2^+5.3131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                7369
_reflns_number_total             9026
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2427.cif
_cod_data_source_block           I
_cod_original_cell_volume        3632.67(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2233051
_cod_database_fobs_code          2233051