Metal−Ligand Cooperativity in O2Activation: Observation of a “Pt−O−O−C” Peroxo Intermediate§
Scheuermann, Margaret L.; Fekl, Ulrich; Kaminsky, Werner; Goldberg, Karen I.; Organometallics 29 (2010) 4749–; doi:10.1021/om1003946

data_4066319
_publ_section_title
;
 Metal&#x2212;Ligand Cooperativity in O2Activation: Observation of a
 &#x201C;Pt&#x2212;O&#x2212;O&#x2212;C&#x201D; Peroxo Intermediate&#x00A7;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4749
_journal_paper_doi               10.1021/om1003946
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         '2(C38 H60 N2 Pt), C7 H8'
_chemical_formula_sum            'C83 H128 N4 Pt2'
_chemical_formula_weight         1572.07
_chemical_name_common            mls_3_161_1
_chemical_name_systematic
;
 mls_3_161_1
;
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-04-09T09:45:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                89.109(5)
_cell_angle_beta                 78.762(5)
_cell_angle_gamma                76.840(5)
_cell_formula_units_Z            1
_cell_length_a                   9.264(5)
_cell_length_b                   11.244(5)
_cell_length_c                   19.100(5)
_cell_measurement_reflns_used    148
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1899.3(14)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            122416
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         37.37
_diffrn_reflns_theta_min         1.86
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.723
_exptl_absorpt_correction_T_max  0.8965
_exptl_absorpt_correction_T_min  0.4947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.86
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         19150
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.04
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.7740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                16406
_reflns_number_total             19150
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om1003946_si_001.cif
_cod_data_source_block           mls_3_161_1_0m
_cod_database_code               4066319