Identifying the Imperative Role of Metal‒Olefin Interactions in Catalytic C‒O Reductive Elimination from Nickel(II)
Lohrey, Trevor D.; Cusumano, Alexander Q.; Goddard, William A.; Stoltz, Brian M.; ACS Catalysis 11 (2021) 10208–10222; doi:10.1021/acscatal.1c02790

data_4518998
_publ_section_title
;
 Identifying the Imperative Role of Metal--Olefin Interactions in
 Catalytic C--O Reductive Elimination from Nickel(II)
;
_journal_issue                   16
_journal_name_full               'ACS Catalysis'
_journal_page_first              10208
_journal_page_last               10222
_journal_paper_doi               10.1021/acscatal.1c02790
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C36 H52 I2 N2 Ni2 O3, 3.5(C4 H8 O)'
_chemical_formula_sum            'C50 H80 I2 N2 Ni2 O6.5'
_chemical_formula_weight         1184.38
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                73.188(4)
_cell_angle_beta                 86.253(4)
_cell_angle_gamma                70.648(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7775(13)
_cell_length_b                   14.7475(15)
_cell_length_c                   15.2774(16)
_cell_measurement_reflns_used    9512
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.15
_cell_volume                     2598.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            110737
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.398
_diffrn_reflns_theta_min         1.871
_exptl_absorpt_coefficient_mu    1.961
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       lath
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.433
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         9509
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0260P)^2^+31.7558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8758
_reflns_number_total             9509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c02790_si_002.cif
_cod_data_source_block           5THF_2078292
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C50 H80 I2 N2 Ni2 O6.50'
_cod_database_code               4518998
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              31398
_shelx_hkl_checksum              62665