A Comparative Reactivity Survey of Some Prominent Bisphosphine Nickel(II) Precatalysts in C‒N Cross-Coupling
Clark, Jillian S. K.; Lavoie, Christopher M.; MacQueen, Preston M.; Ferguson, Michael J.; Stradiotto, Mark; Organometallics 35 (2016) 3248–; doi:10.1021/acs.organomet.6b00650

data_4086710
_publ_section_title
;
 A Comparative Reactivity Survey of Some Prominent Bisphosphine Nickel(II)
 Precatalysts in C--N Cross-Coupling
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3248
_journal_paper_doi               10.1021/acs.organomet.6b00650
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C43 H63 Cl Fe Ni P2'
_chemical_formula_sum            'C43 H63 Cl Fe Ni P2'
_chemical_formula_weight         791.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.5628(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0219(4)
_cell_length_b                   12.0236(5)
_cell_length_c                   16.5337(6)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.41
_cell_volume                     1991.56(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19085
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.292
_diffrn_reflns_theta_min         2.033
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.9507
_exptl_absorpt_correction_T_min  0.8209
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
; 
 Flack x determined using 3715 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9745
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                8738
_reflns_number_total             9745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00650_si_002.cif
_cod_data_source_block           dal1572
_cod_database_code               4086710
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.928
_shelx_res_checksum              64709
_shelx_hkl_checksum              35115