Frustrated Lewis Pairs beyond the Main Group: Cationic Zirconocene-Phosphinoaryloxide Complexes and Their Application in Catalytic Dehydrogenation of Amine Boranes
Andy M. Chapman; Mairi F. Haddow; Duncan F. Wass; Journal of the American Chemical Society 133 (2011) 8826–8829; doi:10.1021/ja201989c

data_4106247
_publ_section_title
;
 Frustrated Lewis Pairs beyond the Main Group: Cationic
 Zirconocene-Phosphinoaryloxide Complexes and Their Application in
 Catalytic Dehydrogenation of Amine Boranes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8826
_journal_page_last               8829
_journal_paper_doi               10.1021/ja201989c
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C61 H64 B2 F20 N O P Zr'
_chemical_formula_weight         1350.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                102.193(5)
_cell_angle_beta                 98.131(5)
_cell_angle_gamma                93.585(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7432(18)
_cell_length_b                   15.051(3)
_cell_length_c                   18.839(3)
_cell_measurement_reflns_used    9471
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      66.28
_cell_measurement_theta_min      3.43
_cell_volume                     2934.1(9)
_computing_cell_refinement       'Bruker APEX II'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker Microstar kappa CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33721
_diffrn_reflns_theta_full        66.51
_diffrn_reflns_theta_max         66.51
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    2.742
_exptl_absorpt_correction_T_max  0.2188
_exptl_absorpt_correction_T_min  0.0867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         9448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+1.7460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                9304
_reflns_number_total             9448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201989c_si_004.cif
_cod_data_source_block           amc233menbh3_0m
_cod_original_cell_volume        2934.0(8)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4106247