Stable, Well-Defined Nickel(0) Catalysts for Catalytic C-C and C-N Bond Formation.
Nett, Alex J.; Cañellas, Santiago; Higuchi, Yuki; Robo, Michael T.; Kochkodan, Jeanne M.; Haynes, 2nd, M Taylor; Kampf, Jeff W.; Montgomery, John; ACS catalysis 8 (2018) 6606–6611; doi:10.1021/acscatal.8b02187

data_4515670
_publ_section_title
;
 Stable, Well-Defined Nickel(0) Catalysts for Catalytic C-C and C-N Bond
 Formation.
;
_journal_issue                   7
_journal_name_full               'ACS catalysis'
_journal_page_first              6606
_journal_page_last               6611
_journal_paper_doi               10.1021/acscatal.8b02187
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C45 H64 N2 Ni O8, 0.5(C5 H12) [+ solvent]'
_chemical_formula_sum            'C47.5 H70 N2 Ni O8'
_chemical_formula_weight         855.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                64.8392(12)
_cell_angle_beta                 80.3426(11)
_cell_angle_gamma                86.1838(11)
_cell_formula_units_Z            8
_cell_length_a                   11.54858(16)
_cell_length_b                   30.1957(4)
_cell_length_c                   32.8403(4)
_cell_measurement_reflns_used    44464
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      69.0580
_cell_measurement_theta_min      2.9430
_cell_volume                     10218.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            157862
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.764
_diffrn_reflns_theta_min         2.632
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       needle
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2232
_refine_ls_number_reflns         36992
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+4.0643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30671
_reflns_number_total             36992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02187_si_002.cif
_cod_data_source_block           ajn3257_sq
_cod_original_formula_sum        'C47.50 H70 N2 Ni O8'
_cod_database_code               4515670
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              46621
_shelx_hkl_checksum              87806
_shelx_fab_checksum              51459