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_4106246
_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_moiety         'C34 H54 O P Zr, C24 B F20'
_chemical_formula_sum            'C58 H54 B F20 O P Zr'
_chemical_formula_weight         1280.01
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 97.928(2)
_cell_angle_gamma                109.720(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6311(3)
_cell_length_b                   14.6798(4)
_cell_length_c                   19.5986(6)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.16
_cell_volume                     2770.58(15)
_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 ShelXL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47710
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       plates
_exptl_crystal_F_000             1300
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_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.372
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         12686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+3.7423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                10353
_reflns_number_total             12686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201989c_si_003.cif
_cod_data_source_block           amc233h2p-1
_cod_original_cell_volume        2770.58(14)
_cod_database_code               4106246