From Bis(silylene) and Bis(germylene) Pincer-Type Nickel(II) Complexes to Isolable Intermediates of the Nickel-Catalyzed Sonogashira Cross-Coupling Reaction
Daniel Gallego; Andreas Brück; Elisabeth Irran; Florian Meier; Martin Kaupp; Matthias Driess; John F. Hartwig; Journal of the American Chemical Society 135 (2013) 15617–15626; doi:10.1021/ja408137t

data_4120936
_publ_section_title
;
 From Bis(silylene) and Bis(germylene) Pincer-Type Nickel(II) Complexes to
 Isolable Intermediates of the Nickel-Catalyzed Sonogashira Cross-Coupling
 Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15617
_journal_page_last               15626
_journal_paper_doi               10.1021/ja408137t
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C30 H55 Br N4 Ni O2 P2, C H2 Cl2'
_chemical_formula_sum            'C31 H57 Br Cl2 N4 Ni O2 P2'
_chemical_formula_weight         789.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_cell_angle_alpha                96.481(7)
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_cell_formula_units_Z            2
_cell_length_a                   11.8490(12)
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_cell_measurement_reflns_used    2323
_cell_measurement_temperature    150(2)
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_cell_volume                     1906.5(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_sigmaI/netI    0.1206
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13828
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_T_max  0.6403
_exptl_absorpt_correction_T_min  0.5095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6697
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                4360
_reflns_number_total             6697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408137t_si_002.cif
_cod_data_source_block           br10
_cod_database_code               4120936