Synthesis of Acetimino Complexes of Pt(II) and Pt(IV) and the First Heteronuclear μ-Acetimido Complexes
Vicente, José; Chicote, María-Teresa; Guerrero, Rita; Vicente-Hernández, Inmaculada; Jones, Peter G.; Bautista, Delia; Inorganic Chemistry 45 (2006) 5201–5209; doi:10.1021/ic060489i

data_4332538
_publ_section_title
;
 Synthesis of Acetimino Complexes of Pt(II) and Pt(IV) and the First
 Heteronuclear \m-Acetimido Complexes
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5201
_journal_page_last               5209
_journal_paper_doi               10.1021/ic060489i
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C27.5 H46 Cl2 N4 O9 Pt'
_chemical_formula_weight         842.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.420(2)
_cell_angle_beta                 81.402(2)
_cell_angle_gamma                80.928(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0737(7)
_cell_length_b                   12.5843(8)
_cell_length_c                   12.6521(8)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.34
_cell_volume                     1690.87(18)
_computing_cell_refinement       'Bruker SAINT'
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18512
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    4.361
_exptl_absorpt_correction_T_max  0.5803
_exptl_absorpt_correction_T_min  0.3545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.790
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment
'NH free with sadi, methyls of imine ligands rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6854
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0390
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+4.2910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                6477
_reflns_number_total             6854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060489isup1.cif
_cod_data_source_block           rh98s
_cod_original_formula_sum        'C27.50 H46 Cl2 N4 O9 Pt'
_cod_database_code               4332538