Lewis Acid Enhanced Ethene Dimerization and Alkene Isomerization—ESI-MS Identification of the Catalytically Active Pyridyldimethoxybenzimidazole Nickel(II) Hydride Species
Escobar, Manuel A.; Trofymchuk, Oleksandra S.; Rodriguez, Barbara E.; Lopez-Lira, Claudia; Tapia, Ricardo; Daniliuc, Constantin; Berke, Heinz; Nachtigall, Fabiane M.; Santos, Leonardo S.; Rojas, Rene S.; ACS Catalysis 5 (2015) 7338–; doi:10.1021/acscatal.5b02003

data_4516691
_publ_section_title
;
 Lewis Acid Enhanced Ethene Dimerization and Alkene Isomerization---ESI-MS
 Identification of the Catalytically Active Pyridyldimethoxybenzimidazole
 Nickel(II) Hydride Species
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              7338
_journal_paper_doi               10.1021/acscatal.5b02003
_journal_volume                  5
_journal_year                    2015
_chemical_formula_sum            'C50 H32 B F24 N3 Ni O2'
_chemical_formula_weight         1232.30
_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
_cell_angle_alpha                70.9510(10)
_cell_angle_beta                 80.7670(10)
_cell_angle_gamma                78.8870(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4773(5)
_cell_length_b                   13.0681(5)
_cell_length_c                   18.2775(8)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.3196
_cell_measurement_theta_min      2.2728
_cell_volume                     2528.57(18)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection
;
APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)
;
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43432
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.467
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         9271
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+3.0869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                7560
_reflns_number_total             9271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs5b02003_si_002.cif
_cod_data_source_block           I
_cod_database_code               4516691
_shelx_res_checksum              12293
_shelx_hkl_checksum              75869