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_1515439
_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         'C48 H38 N1 Ni1 P1'
_chemical_formula_sum            'C48 H38 N Ni P'
_chemical_formula_weight         718.47
_chemical_melting_point          483
_chemical_name_common
;Nickel bis(5-H-dibenzo(a,d)cyclohepten-5-yl)-amine
triphenylphosphane
;
_chemical_name_systematic
'Nickel bis(5-H-dibenzo[a,d]cyclohepten-5-yl)-amine triphenylphosphane'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.677(2)
_cell_angle_beta                 95.682(2)
_cell_angle_gamma                114.432(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4130(11)
_cell_length_b                   12.0679(11)
_cell_length_c                   14.4208(13)
_cell_measurement_reflns_used    5544
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.24
_cell_volume                     1758.7(3)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER Saint'
_computing_molecular_graphics    ORTEP3DIR
_computing_publication_material  SHELLXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'BRUKER APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18304
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.9054
_exptl_absorpt_correction_T_min  0.8576
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_recrystallization_method
'slow diffusion DME/iPrO : hexanes (1:1:3)'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          2.488
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+0.3227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                7229
_reflns_number_total             8645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00483a.txt
_cod_data_source_block           sadp-1
_cod_original_formula_sum        'C48 H38 N1 Ni1 P1'
_cod_database_code               1515439