A one-dimensional iodido-bridged Pt^II^/Pt^IV^ mixed-valence complex cation with a hydrogen sulfate counter-anion
Matsushita, Nobuyuki; Acta Crystallographica Section E 74 (2018) 1821–1825; doi:10.1107/S2056989018016158

data_2242759
_publ_section_title
;
 A one-dimensional iodido-bridged Pt^II^/Pt^IV^ mixed-valence complex
 cation with a hydrogen sulfate counter-anion
;
_journal_coeditor_code           WM5469
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1821
_journal_page_last               1825
_journal_paper_doi               10.1107/S2056989018016158
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'[Pt (C2 H8 N2)2] [Pt I2 (C2 H8 N2)2] (H S O4)4, 2H2 O'
_chemical_formula_moiety
;
C4 H16 N4 Pt 2+, C4 H16 I2 N4 Pt 2+, 4(H O4 S 1-), 2(H2 O)
;
_chemical_formula_sum            'C8 H40 I2 N8 O18 Pt2 S4'
_chemical_formula_weight         1308.70
_chemical_name_systematic
'<i>catena</i>-Poly[[[bis(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')platinum(II)]-\m-iodido-[bis(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')platinum(IV)]-\m-iodido] tetra(hydrogen sulfate) dihydrate]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.3180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   7.2964(2)
_cell_length_b                   5.9451(2)
_cell_length_c                   18.2253(7)
_cell_measurement_reflns_used    14539
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.06
_cell_measurement_theta_min      3.05
_cell_volume                     789.93(5)
_computing_cell_refinement
;
<i>RAPID-AUTO</i> (Rigaku, 2015)
;
_computing_data_collection
;
<i>RAPID-AUTO</i> (Rigaku, 2015)
;
_computing_data_reduction
;
<i>RAPID-AUTO</i> (Rigaku, 2015)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg, 2018)
;
_computing_publication_material
;
SHELXL-2014/7 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16218
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.031
_diffrn_reflns_theta_min         3.052
_diffrn_source                   'X-ray sealed tube'
_exptl_absorpt_coefficient_mu    11.146
_exptl_absorpt_correction_T_max  0.0200
_exptl_absorpt_correction_T_min  0.0095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Rigaku, 1995)
;
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    2.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         2.118
_refine_diff_density_min         -1.685
_refine_ls_extinction_coef       0.0149(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2014/7 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+0.4688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0455
_reflns_number_gt                2541
_reflns_number_total             2733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5469sup1.cif
_cod_data_source_block           I
_cod_database_code               2242759
_shelx_hkl_checksum              64028
_shelx_res_checksum              45345
_cod_database_fobs_code 2242759