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_4086340
_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         'C25 H27 B F3 N7 Ni O, C H2 Cl2'
_chemical_formula_sum            'C26 H29 B Cl2 F3 N7 Ni O'
_chemical_formula_weight         652.98
_chemical_name_common            jonsc23
_chemical_name_systematic
; 
 Tp'Ni(4-CF3-quinolinate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.7160(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7931(10)
_cell_length_b                   13.2431(10)
_cell_length_c                   8.5001(6)
_cell_measurement_reflns_used    4011
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.90
_cell_volume                     1514.58(19)
_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      243(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            28267
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         29.597
_diffrn_reflns_theta_min         1.538
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
; 
 Flack x determined using 2103 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.039(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         8400
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1132P)^2^+0.1663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.970
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                5380
_reflns_number_total             8400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00824_si_002.cif
_cod_data_source_block           2c
_cod_database_code               4086340
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              49991