Oxygen Insertion into Metal Carbon Bonds: Formation of Methylperoxo Pd(II) and Pt(II) Complexes via Photogenerated Dinuclear Intermediates.
Petersen, Allan R.; Taylor, Russell A.; Vicente-Hernández, Inmaculada; Mallender, Philip R.; Olley, Harriet; White, Andrew J. P.; Britovsek, George J. P.; Journal of the American Chemical Society 136 (2014) 14089–14099; doi:10.1021/ja5055143

data_4122680
_publ_section_title
;
 Oxygen Insertion into Metal Carbon Bonds: Formation of Methylperoxo
 Pd(II) and Pt(II) Complexes via Photogenerated Dinuclear Intermediates.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14089
_journal_page_last               14099
_journal_paper_doi               10.1021/ja5055143
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C24 H18 N3 Pt, F6 Sb, 0.9(C3 H6 O)'
_chemical_formula_sum            'C26.7 H23.4 F6 N3 O0.9 Pt Sb'
_chemical_formula_weight         831.52
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL
_cell_angle_alpha                91.8823(15)
_cell_angle_beta                 100.5989(14)
_cell_angle_gamma                104.1322(17)
_cell_formula_units_Z            4
_cell_length_a                   8.92385(16)
_cell_length_b                   14.6411(3)
_cell_length_c                   21.3047(3)
_cell_measurement_reflns_used    20078
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.6386
_cell_measurement_theta_min      3.1498
_cell_volume                     2644.42(9)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32651
_diffrn_reflns_point_group_measured_fraction_full 0.670
_diffrn_reflns_point_group_measured_fraction_max 0.551
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.724
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.374
_exptl_absorpt_correction_T_max  0.522
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1579
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.309(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1533
_refine_ls_number_reflns         21515
_refine_ls_number_restraints     1972
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.247
_reflns_Friedel_fraction_full    0.341
_reflns_Friedel_fraction_max     0.219
_reflns_number_gt                18042
_reflns_number_total             21515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5055143_si_002.cif
_cod_data_source_block           '[Pt(7)Me](SbF6)'
_cod_depositor_comments
'Adding full bibliography for 4122679--4122681.cif.'
_cod_original_cell_volume        2644.43(9)
_cod_original_formula_sum        'C26.70 H23.40 F6 N3 O0.90 Pt Sb'
_cod_database_code               4122680
_shelxl_version_number           2013-4