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_4089288
_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_absolute_configuration unk
_chemical_formula_moiety         'C36 H44 N2 Ni P2 Pd S2, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C40 H50 F12 N4 Ni P4 Pd S2'
_chemical_formula_weight         1167.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.662(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.476(3)
_cell_length_b                   25.940(6)
_cell_length_c                   15.729(3)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      2.55
_cell_volume                     4601.5(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.9143
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28325
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         1.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1279 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.6261.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.6858
_exptl_crystal_description       block
_exptl_crystal_F_000             2369.3689
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.6293
_refine_diff_density_min         -0.5514
_refine_diff_density_rms         0.0666
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.020(7)
_refine_ls_d_res_high            0.7212
_refine_ls_d_res_low             10.3428
_refine_ls_goodness_of_fit_ref   1.0230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     578
_refine_ls_number_reflns         11752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0230
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.0317
_refine_ls_shift/su_mean         0.0006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+1.7879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.884
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              35
_reflns_limit_k_min              -35
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                11310
_reflns_number_total             11752
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om7b00176_si_002.cif
_cod_data_source_block           PddpppNidach_0m
_cod_original_cell_volume        4601.6(17)
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_database_code               4089288
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C1(H1a,H1b), C13(H13a,H13b), C2(H2a,H2b), C3(H3a,H3b), C9(H9a,
 H9b), C5(H5a,H5b), C7(H7a,H7b), C11(H11a,H11b), C12(H12a,H12b), C6(H6a,H6b),
 C4(H4a,H4b)
2.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C19(H19), C31(H31), C27(H27), C29(H29), C15(H15), C16(H16),
 C25(H25), C21(H21), C17(H17), C30(H30), C28(H28), C18(H18), C22(H22), C23(H23),
  C34(H34), C35(H35), C37(H37), C36(H36), C24(H24)
2.c Idealised Me refined as rotating group:
 C39(H39a,H39b,H39c), C41(H41a,H41b,H41c)
;
_olex2_submission_special_instructions 'No special instructions were received'