Direct C(sp3)-O Reductive Elimination of Olefin Oxides from PtIV-Oxetanes Prepared by Aerobic Oxidation of PtII Olefin Derivatives (Olefin = cis-Cyclooctene, Norbornene)
Julia R. Khusnutdinova; Laura L. Newman; Peter Y. Zavalij; Yiu-Fai Lam; Andrei N. Vedernikov; Journal of the American Chemical Society 130 (2008) 2174–2175; doi:10.1021/ja7107323

data_4107452
_publ_section_title
;
 Direct C(sp3)-O Reductive Elimination of Olefin Oxides from PtIV-Oxetanes
 Prepared by Aerobic Oxidation of PtII Olefin Derivatives (Olefin =
 cis-Cyclooctene, Norbornene)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2174
_journal_page_last               2175
_journal_paper_doi               10.1021/ja7107323
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H20 N2 O5 Pt S, C H4 O, 2(H2 O)'
_chemical_formula_sum            'C19 H28 N2 O8 Pt S'
_chemical_formula_weight         639.58
_chemical_name_common            Pt-complex
_chemical_name_systematic
;
Pt-complex
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 99.1130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4315(6)
_cell_length_b                   8.5602(6)
_cell_length_c                   15.7898(11)
_cell_measurement_reflns_used    8104
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      2.4
_cell_volume                     1125.25(14)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      366,366,366,366,366,366
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0243026
_diffrn_orient_matrix_UB_12      0.0224502
_diffrn_orient_matrix_UB_13      -0.0628706
_diffrn_orient_matrix_UB_21      -0.1171315
_diffrn_orient_matrix_UB_22      -0.0151950
_diffrn_orient_matrix_UB_23      0.0014554
_diffrn_orient_matrix_UB_31      -0.0108717
_diffrn_orient_matrix_UB_32      0.1136308
_diffrn_orient_matrix_UB_33      0.0126208
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19852
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.58
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.375
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_density_method    not-measure
_exptl_crystal_description       prism
_exptl_crystal_F_000             628
_exptl_crystal_id                'Vedern/Julia PtNB'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.022(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5143
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0154
_refine_ls_R_factor_gt           0.0144
_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^)+(0.0037P)^2^], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0344
_refine_ls_wR_factor_ref         0.0347
_reflns_Friedel_coverage         0.863
_reflns_number_gt                4974
_reflns_number_total             5143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7107323-file002.cif
_cod_data_source_block           1523
_cod_database_code               4107452
_diffrn_measurement_total_frames-ccd 2196
_diffrn_measurement_frame_width-ccd 0.5
_diffrn_detector_distance-ccd    5.000
_diffrn_measurement_frame_time-ccd 23
_diffrn_measurement_total_time-ccd 18.4
_diffrn_measurement_frame_size-ccd 512