A one-dimensional chloride-bridged PtII/PtIVmixed-valence complex with a 4-[(4-hydroxyphenyl)diazenyl]benzenesulfonate counter-ion
Matsushita, Nobuyuki; Taira, Ayako; Acta Crystallographica Section C Structural Chemistry 71 (2015) –; doi:10.1107/S2053229615019877

data_2020292
_publ_section_title
;
 A one-dimensional chloride-bridged PtII/PtIVmixed-valence complex with a
 4-[(4-hydroxyphenyl)diazenyl]benzenesulfonate counter-ion
;
_journal_coeditor_code           UK3120
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229615019877
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Pt2 Cl2 (C2 H8 N2)4] (C12 H9 N2 O4 S)4 , 2H2 O'
_chemical_formula_moiety
'C8 H32 Cl2 N8 Pt2 4+, 4(C12 H9 N2 O4 S -), 2(H2 O)'
_chemical_formula_sum            'C56 H72 Cl2 N16 O18 Pt2 S4'
_chemical_formula_weight         1846.62
_chemical_name_systematic
;<i>catena</i>-Poly[[[bis(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')platinum(II)]-\m-chlorido-[bis(ethylenediamine)platinum(IV)]-\m-chlorido]
tetrakis{4-[(4-hydroxyphenyl)diazenyl]benzenesulfonate} dihydrate]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 93.7245(7)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.0782(7)
_cell_length_b                   5.8922(3)
_cell_length_c                   15.8365(3)
_cell_measurement_reflns_used    19956
_cell_measurement_temperature    296
_cell_measurement_theta_max      32.05
_cell_measurement_theta_min      3.32
_cell_volume                     1683.35(11)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_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_source         'X-ray sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36062
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    4.436
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_description       platelet
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.670
_refine_ls_extinction_coef       0.00058(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         5847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0201P)^2^+1.4401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                4097
_reflns_number_total             5847
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            uk3120sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'C56 H72 Cl2 N16 O18 Pt2 S4 '
_cod_database_code               2020292
_cod_database_fobs_code          2020292