Amino olefin nickel(i) and nickel(0) complexes as dehydrogenation catalysts for amine boranes
Vogt, Matthias; de Bruin, Bas; Berke, Heinz; Trincado, Mónica; Grützmacher, Hansjörg; Chemical Science 2 (2011) 723–; doi:10.1039/c0sc00483a

data_1515438
_publ_section_title
;
 Amino olefin nickel(i) and nickel(0) complexes as dehydrogenation
 catalysts for amine boranes
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              723
_journal_paper_doi               10.1039/c0sc00483a
_journal_volume                  2
_journal_year                    2011
_chemical_formula_moiety         'C32 H23 F3 N Ni O2 (O1 C4 H8)'
_chemical_formula_sum            'C36 H31 F3 N Ni O3'
_chemical_formula_weight         641.33
_chemical_melting_point          493
_chemical_name_common            '[Ni(trop2NH)(OOCCF3)] x [THF]'
_chemical_name_systematic
'Nickel bis(5-H-dibenzo[a,d]cyclohepten-5-yl)-amine trifluoroacetate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.992(3)
_cell_length_b                   11.424(2)
_cell_length_c                   18.291(4)
_cell_measurement_reflns_used    8349
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.29
_cell_volume                     2869.4(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP for Windows'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29172
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_correction_T_min  0.8669
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep green '
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1332
_exptl_crystal_recrystallization_method 'slow diffusion THF / n-hexane'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.078
_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     521
_refine_ls_number_reflns         7123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+1.2094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                6061
_reflns_number_total             7123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00483a.txt
_cod_data_source_block           sadp21n
_cod_original_cell_volume        2869.5(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1515438