Spontaneous Si-C bond cleavage in (Triphos(Si))-nickel complexes.
Petuker, Anette; Mebs, Stefan; Schuth, Nils; Gerschel, Philipp; Reback, Matthew L.; Mallick, Bert; van Gastel, Maurice; Haumann, Michael; Apfel, Ulf-Peter; Dalton transactions (Cambridge, England : 2003) 46 (2017) 907–917; doi:10.1039/c6dt04048a

data_7041387
_publ_section_title
;
 Spontaneous Si-C bond cleavage in (Triphos(Si))-nickel complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              907
_journal_page_last               917
_journal_paper_doi               10.1039/c6dt04048a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C53 H51 Ni P4 Si, B F4, C2 H3 N '
_chemical_formula_sum            'C55 H54 B F4 N Ni P4 Si'
_chemical_formula_weight         1026.48
_chemical_name_common            'Triphos(Si)Ni(CH2PPh2) BF4'
_chemical_name_systematic        'Triphos(Si)Ni(CH2PPh2) BF4'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-06-16 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.01(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.33010(10)
_cell_length_b                   20.6239(2)
_cell_length_c                   23.6859(2)
_cell_measurement_reflns_used    18275
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.0060
_cell_measurement_theta_min      4.2620
_cell_volume                     5046.21(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26336
_diffrn_reflns_theta_full        74.25
_diffrn_reflns_theta_max         74.25
_diffrn_reflns_theta_min         4.28
_exptl_absorpt_coefficient_mu    2.413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         9610
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+4.4625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                9272
_reflns_number_total             9610
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6dt04048a2.cif
_cod_data_source_block           ap104
_cod_depositor_comments
'Adding full bibliography for 7041386--7041393.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7041387
_publcif_datablock.id            {28239e12-f67a-482c-939e-7b890471db25}