Acetate-Bridged Platinum(III) Complexes Derived from Cisplatin
Justin J. Wilson; Stephen J. Lippard; Inorganic Chemistry 51 (2012) 9852–9864; doi:10.1021/ic301289j

data_4330370
_publ_contact_author_address
;77 Massachusetts Ave, 18-498
Cambridge, MA 02139
;
_publ_contact_author_email       lippard@mit.edu
_publ_contact_author_fax         (617)258-8150
_publ_contact_author_name        'Stephen J. Lippard'
_publ_contact_author_phone       (617)253-1892
_publ_section_title
;
 Acetate-Bridged Platinum(III) Complexes Derived from Cisplatin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9852
_journal_page_last               9864
_journal_paper_doi               10.1021/ic301289j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C24 H62 F6 N16 O28 Pt4'
_chemical_formula_weight         1917.26
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.367(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.401(4)
_cell_length_b                   13.8473(14)
_cell_length_c                   12.8506(13)
_cell_measurement_reflns_used    7534
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.16
_cell_volume                     6012.3(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            45478
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    9.384
_exptl_absorpt_correction_T_max  0.9120
_exptl_absorpt_correction_T_min  0.2829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_description       shard
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
 The disordered electron density resided about crystallographic 
 inversion center. We believe this electron density may correspond to
 two molecules of diethyl ether (84 e) per void. After drying crystalline
 samples under vacuum, elemental analyses is consistent with the presence
 of 4 DMF molecules per complex. Hence, we hypothesize that this density is
 due to ether, which is much more volatile than DMF
;
_refine_diff_density_max         4.849
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5366
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+22.5580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                3877
_reflns_number_total             5366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301289j_si_002_1.cif
_cod_data_source_block           '[4](NO3)4*4DMF'
_cod_database_code               4330370