Frustrated Lewis Pairs beyond the Main Group: Synthesis, Reactivity, and Small Molecule Activation with Cationic Zirconocene-Phosphinoaryloxide Complexes
Andy M. Chapman; Mairi F. Haddow; Duncan F. Wass; Journal of the American Chemical Society 133 (2011) 18463–18478; doi:10.1021/ja207936p

data_4107106
_publ_section_title
;
 Frustrated Lewis Pairs beyond the Main Group: Synthesis, Reactivity, and
 Small Molecule Activation with Cationic Zirconocene-Phosphinoaryloxide
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18463
_journal_page_last               18478
_journal_paper_doi               10.1021/ja207936p
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C67 H64 B Cl F21 O P Zr'
_chemical_formula_weight         1452.63
_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                93.034(6)
_cell_angle_beta                 102.341(6)
_cell_angle_gamma                95.100(6)
_cell_formula_units_Z            2
_cell_length_a                   10.7652(12)
_cell_length_b                   16.9370(17)
_cell_length_c                   17.8214(19)
_cell_measurement_reflns_used    9083
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.33
_cell_measurement_theta_min      2.46
_cell_volume                     3153.1(6)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59739
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.604
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         14325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.1290
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0104P)^2^+65.2828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2918
_refine_ls_wR_factor_ref         0.2980
_reflns_number_gt                12652
_reflns_number_total             14325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207936p_si_011.cif
_cod_data_source_block           amc233iprcl_0m
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4107106