Reaction of alkyne with dinickel-diphenylsilyl complexes. Preparation of an emissive disilane via consecutive Si-C and Si-Si bond-making reactions
Makoto Tanabe; Ryouhei Yumoto; Kohtaro Osakada; Chem.Commun. 48 (2012) 2125–; doi:10.1039/c2cc16063c

data_7107347
_publ_section_title
;
 Reaction of alkyne with dinickel-diphenylsilyl complexes. Preparation of
 an emissive disilane via consecutive Si-C and Si-Si bond-making reactions
;
_journal_name_full               Chem.Commun.
_journal_page_first              2125
_journal_paper_doi               10.1039/c2cc16063c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C60 H88 Ni2 P2 Si2'
_chemical_formula_sum            'C60 H88 Ni2 P2 Si2'
_chemical_formula_weight         1044.87
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.961(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   10.2283(18)
_cell_length_b                   13.576(3)
_cell_length_c                   20.026(4)
_cell_measurement_reflns_used    6176
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     2779.2(10)
_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  0.1036
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22419
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1124.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.410
_refine_diff_density_min         -1.850
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     302
_refine_ls_number_reflns         6363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0700P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.2409
_reflns_number_gt                3470
_reflns_number_total             6363
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2cc16063c.txt
_cod_data_source_block           compound2
_cod_original_cell_volume        2779.2(9)
_cod_database_code               7107347