Frustrated Lewis Pair vs Metal–Carbon σ-Bond Insertion Chemistry at an o-Phenylene-Bridged Cp2Zr+/PPh2 System
Jian, Zhongbao; Daniliuc, Constantin G.; Kehr, Gerald; Erker, Gerhard; Organometallics 36 (2017) 424–; doi:10.1021/acs.organomet.6b00828

data_4086914
_publ_section_title
;
 Frustrated Lewis Pair vs Metal--Carbon \s-Bond Insertion Chemistry at an
 o-Phenylene-Bridged Cp2Zr+/PPh2 System
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              424
_journal_paper_doi               10.1021/acs.organomet.6b00828
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C55 H27.5 B Br0.5 Cl F20 P Zr'
_chemical_formula_weight         1276.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 114.612(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7855(10)
_cell_length_b                   16.5114(7)
_cell_length_c                   16.8379(9)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    105.(2)
_cell_measurement_theta_max      25.3461
_cell_measurement_theta_min      2.2644
_cell_volume                     5001.0(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection
;
APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)

;
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      105.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            132234
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.741
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         9142
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+13.3205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                7385
_reflns_number_total             9142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00828_si_002.cif
_cod_data_source_block           erk8410
_cod_depositor_comments
'Adding full bibliography for 4086908--4086918.cif.'
_cod_original_formula_sum        'C55 H27.50 B Br0.50 Cl F20 P Zr'
_cod_database_code               4086914
_shelx_res_checksum              23507
_shelx_hkl_checksum              42792