Nickel-Catalyzed Cyclopolymerization of Hexyl- and Phenylsilanes
Tanabe, Makoto; Takahashi, Atsushi; Fukuta, Tomoko; Osakada, Kohtaro; Organometallics 32 (2013) 1037–; doi:10.1021/om301052f

data_4080074
_publ_section_title
;
 Nickel-Catalyzed Cyclopolymerization of Hexyl- and Phenylsilanes
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1037
_journal_paper_doi               10.1021/om301052f
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C54 H48 P2 Pd Si4'
_chemical_formula_sum            'C54 H48 P2 Pd Si4'
_chemical_formula_weight         977.66
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      86
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.447(3)
_cell_length_b                   14.447(3)
_cell_length_c                   22.606(5)
_cell_measurement_reflns_used    12286
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.28
_cell_volume                     4718.2(17)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38324
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.590
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5402
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0480P)^2^+3.5649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                4422
_reflns_number_total             5402
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om301052f_si_002.cif
_cod_data_source_block           '__complex1'
_cod_original_cell_volume        4718.2(15)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4080074