Polynuclear Hydroxido-Bridged Complexes of Platinum(IV) with Terminal Nitrato Ligands.
Vasilchenko, Danila; Berdugin, Semen; Tkachev, Sergey; Baidina, Iraida; Romanenko, Galina; Gerasko, Olga; Korenev, Sergey; Inorganic chemistry 54 (2015) 4644–4651; doi:10.1021/ic502896s

data_4342812
_publ_section_title
;
 Polynuclear Hydroxido-Bridged Complexes of Platinum(IV) with Terminal
 Nitrato Ligands.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4644
_journal_page_last               4651
_journal_paper_doi               10.1021/ic502896s
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'H6 N10 O36 Pt4, C36 H36 N24 O12, 25(H2O)'
_chemical_formula_sum            'C36 H92 N34 O73 Pt4'
_chemical_formula_weight         2949.79
_chemical_properties_physical    moisture-sensitive
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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           SHELXL-97
_cell_angle_alpha                66.238(5)
_cell_angle_beta                 71.669(5)
_cell_angle_gamma                79.704(5)
_cell_formula_units_Z            1
_cell_length_a                   11.130(2)
_cell_length_b                   14.730(3)
_cell_length_c                   15.637(3)
_cell_measurement_reflns_used    8961
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      2.48
_cell_measurement_theta_min      28.36
_cell_volume                     2223.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker saint'
_computing_molecular_graphics    'local programs'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45421
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         29.878
_diffrn_reflns_theta_min         1.513
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.419
_exptl_absorpt_correction_T_max  0.7404
_exptl_absorpt_correction_T_min  0.5141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1442
_exptl_crystal_recrystallization_method 'nitric acid'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The unit cell contains 25  water molecules (248 electron count/cell) 
which have been treated as a diffuse contribution to the overall
scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.564
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         12523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                8363
_reflns_number_total             12523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502896s_si_004.cif
_cod_data_source_block           k_sq
_cod_depositor_comments
'Adding full bibliography for 4342811--4342813.cif.'
_cod_original_cell_volume        2223.3(7)
_cod_database_code               4342812
_shelx_estimated_absorpt_t_max   0.740
_shelx_estimated_absorpt_t_min   0.513