Discrete Air-Stable Nickel(II)–Palladium(II) Complexes as Catalysts for Suzuki–Miyaura Reactions
Zhao, Tiankun; Ghosh, Pokhraj; Martinez, Zachary; Liu, Xufeng; Meng, Xianggao; Darensbourg, Marcetta Y.; Organometallics 36 (2017) 1822–; doi:10.1021/acs.organomet.7b00176

data_4089285
_publ_section_title
;
 Discrete Air-Stable Nickel(II)--Palladium(II) Complexes as Catalysts for
 Suzuki--Miyaura Reactions
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1822
_journal_paper_doi               10.1021/acs.organomet.7b00176
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         C36H43F12N3NiP4PdS2
_chemical_formula_sum            'C36 H43 F12 N3 Ni P4 Pd S2'
_chemical_formula_weight         1098.84
_chemical_melting_point          220
_chemical_name_common            C36H43F12N3NiP4PdS2
_chemical_name_systematic        C36H43F12N3NiP4PdS2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.491(8)
_cell_length_b                   11.413(3)
_cell_length_c                   13.660(4)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      2.44
_cell_volume                     4286(2)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51876
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.533
_diffrn_reflns_theta_min         1.784
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       Block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
; 
 Flack x determined using 5067 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.005(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         11336
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0313P)^2^+1.9149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                11069
_reflns_number_total             11336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00176_si_002.cif
_cod_data_source_block           a
_cod_database_code               4089285
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.890
_shelx_res_checksum              72065
_shelx_hkl_checksum              95194