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_4107105
_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_moiety         'C35 H54 Cl2 O P Zr, C24 B F20, C H2 Cl2'
_chemical_formula_sum            'C60 H56 B Cl4 F20 O P Zr'
_chemical_formula_weight         1447.85
_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                64.470(1)
_cell_angle_beta                 85.548(1)
_cell_angle_gamma                85.835(1)
_cell_formula_units_Z            2
_cell_length_a                   10.7053(2)
_cell_length_b                   16.7854(3)
_cell_length_c                   18.9334(4)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.29
_cell_volume                     3057.84(11)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       '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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53024
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The disordered solvent is probably n-hexane, but a suitable model could
not be obtained.
;
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         14080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0348P)^2^+1.9033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                12747
_reflns_number_total             14080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207936p_si_010.cif
_cod_data_source_block           amc233asqueeze
_cod_original_cell_volume        3057.84(10)
_cod_database_code               4107105