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_7041393
_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         'C14 H39 N Ni P4, 2(B F4)'
_chemical_formula_sum            'C14 H39 B2 F8 N Ni P4'
_chemical_formula_weight         577.67
_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                 121.948(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1498(3)
_cell_length_b                   16.0585(6)
_cell_length_c                   19.1814(7)
_cell_measurement_reflns_used    6997
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      73.8190
_cell_measurement_theta_min      3.8370
_cell_volume                     2652.83(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      108.2(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9120
_diffrn_measured_fraction_theta_max 0.8816
_diffrn_measurement_details
;
  1 omega -124.00  -79.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4802  -99.0000   30.0000 45

  2 omega  -32.00   71.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       41.4802  -57.0000  150.0000 103

  3 omega   24.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -94.0000    0.0000 85

  4 omega   31.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000  -90.0000 38

  5 omega   31.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000 -150.0000 38

  6 omega   34.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000    0.0000 43

  7 omega   31.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000 -120.0000 38

  8 omega   75.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000   30.0000 83

  9 omega -115.00  -12.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4802  -57.0000 -150.0000 103

 10 omega -115.00  -12.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4802  -57.0000   90.0000 103

 11 omega   75.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000  -90.0000 83

 12 omega   81.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   45.0000 -180.0000 77

 13 omega   75.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000  -30.0000 83

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1134761000
_diffrn_orient_matrix_UB_12      -0.0635838000
_diffrn_orient_matrix_UB_13      0.0040453000
_diffrn_orient_matrix_UB_21      -0.0998410000
_diffrn_orient_matrix_UB_22      -0.0716581000
_diffrn_orient_matrix_UB_23      -0.0099569000
_diffrn_orient_matrix_UB_31      0.0147711000
_diffrn_orient_matrix_UB_32      0.0048612000
_diffrn_orient_matrix_UB_33      -0.0939989000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14353
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         74.2490
_diffrn_reflns_theta_min         3.8670
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.891
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+5.0530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                4300
_reflns_number_total             4798
_reflns_threshold_expression     >2sigma(I)
_publcif_datablock.id            {043af71d-75df-4730-93a2-8b5d46d01bf4}
_cod_data_source_file            c6dt04048a2.cif
_cod_data_source_block           upa159
_cod_depositor_comments
'Adding full bibliography for 7041386--7041393.cif.'
_cod_original_cell_volume        2652.83(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7041393