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_4120940
_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_sum            'C44 H65 Br Ge2 N4 O2'
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_audit_creation_method
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_cell_angle_alpha                105.524(4)
_cell_angle_beta                 99.379(3)
_cell_angle_gamma                97.497(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5224(5)
_cell_length_b                   13.4646(6)
_cell_length_c                   17.1624(6)
_cell_measurement_reflns_used    5774
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.4556
_cell_measurement_theta_min      3.3505
_cell_volume                     2272.45(18)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15890
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_T_max  0.7610
_exptl_absorpt_correction_T_min  0.4302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.0630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                6598
_reflns_number_total             7973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408137t_si_007.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        2272.45(17)
_cod_database_code               4120940