A Single Nickel Catalyst for the Acceptorless Dehydrogenation of Alcohols and Hydrogenation of Carbonyl Compounds
Chakraborty, Sumit; Piszel, Paige E.; Brennessel, William W.; Jones, William D.; Organometallics 34 (2015) 5203–; doi:10.1021/acs.organomet.5b00824

data_4086341
_publ_contact_author_address
;
 'Department of Chemistry, University of Rochester, Rochester,  New York 14627'
;
_publ_contact_author_email       jones@chem.rochester.edu
_publ_contact_author_name        'William D. Jones'
_publ_section_title
;
 A Single Nickel Catalyst for the Acceptorless Dehydrogenation of Alcohols
 and Hydrogenation of Carbonyl Compounds
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5203
_journal_paper_doi               10.1021/acs.organomet.5b00824
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C27 H29 B F6 N8 Ni O2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C27.5 H30 B Cl F6 N8 Ni O2'
_chemical_formula_weight         723.56
_chemical_name_common            jonsc19
_chemical_name_systematic
; 
 Tp'Ni(pyridinate)(pyridone)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                75.264(3)
_cell_angle_beta                 84.636(3)
_cell_angle_gamma                83.551(3)
_cell_formula_units_Z            4
_cell_length_a                   14.0566(17)
_cell_length_b                   14.3968(18)
_cell_length_c                   16.366(2)
_cell_measurement_reflns_used    3914
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.18
_cell_volume                     3175.5(7)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.1096
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50157
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         29.591
_diffrn_reflns_theta_min         1.461
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       needle
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         17769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0353P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10489
_reflns_number_total             17769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00824_si_002.cif
_cod_data_source_block           7
_cod_original_cell_volume        3175.4(7)
_cod_original_formula_sum        'C27.50 H30 B Cl F6 N8 Ni O2'
_cod_database_code               4086341
_shelx_estimated_absorpt_t_min   0.849
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              11130