Ring Expansion of Cyclic Triplatinum(0) Silylene Complexes Induced by Insertion of Alkyne into a Si‒Pt Bond
Tanaka, Kimiya; Kamono, Megumi; Tanabe, Makoto; Osakada, Kohtaro; Organometallics 34 (2015) 2985–; doi:10.1021/acs.organomet.5b00291

data_4085914
_publ_section_title
;
 Ring Expansion of Cyclic Triplatinum(0) Silylene Complexes Induced by
 Insertion of Alkyne into a Si--Pt Bond
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2985
_journal_paper_doi               10.1021/acs.organomet.5b00291
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C57 H63 F6 O8 P3 Pt3 Si3'
_chemical_formula_weight         1752.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 113.3360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.239(3)
_cell_length_b                   12.6686(14)
_cell_length_c                   22.217(3)
_cell_measurement_temperature    90
_cell_volume                     6264.2(13)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHELL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
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_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31638
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.037
_diffrn_reflns_theta_min         1.830
_exptl_absorpt_coefficient_mu    6.885
_exptl_absorpt_correction_T_max  0.546
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_description       prism
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.241
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.717
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         12310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.717
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.3561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9930
_reflns_number_total             12310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00291_si_001.cif
_cod_data_source_block           complex4
_cod_depositor_comments
'Adding full bibliography for 4085912--4085914.cif.'
_cod_original_cell_volume        6264.1(12)
_cod_database_code               4085914
_shelx_estimated_absorpt_t_min   0.546
_shelx_estimated_absorpt_t_max   0.546
_shelxl_version_number           2014/6
_shelx_hkl_checksum              88876