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_4122681
_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         'C20 H16 N5 Pt, F6 Sb'
_chemical_formula_sum            'C20 H16 F6 N5 Pt Sb'
_chemical_formula_weight         757.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.9813(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.82761(9)
_cell_length_b                   7.52718(6)
_cell_length_c                   24.4124(2)
_cell_measurement_reflns_used    10418
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.2745
_cell_measurement_theta_min      3.6269
_cell_volume                     2168.16(3)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15882
_diffrn_reflns_theta_full        72.42
_diffrn_reflns_theta_max         72.42
_diffrn_reflns_theta_min         3.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.427
_exptl_absorpt_correction_T_max  0.556
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
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    2.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.000232(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4255
_refine_ls_number_restraints     902
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+4.2399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                3858
_reflns_number_total             4255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5055143_si_002.cif
_cod_data_source_block           '[Pt(8)Me](SbF6)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4122679--4122681.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4122681