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_4086917
_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            'C65 H46 B F20 N2 P Zr'
_chemical_formula_weight         1368.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                76.795(2)
_cell_angle_beta                 76.520(3)
_cell_angle_gamma                86.720(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3724(11)
_cell_length_b                   16.2046(14)
_cell_length_c                   19.6938(19)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      26.2450
_cell_measurement_theta_min      2.2751
_cell_volume                     3435.9(6)
_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      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0640
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59383
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.25
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  0.98
_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            orange
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.081
_platon_squeeze_details
;
Two disordered solvent molecules (probably dichloromethane and pentane 
molecules) were found in the asymmetrical unit and could not be 
satisfactorily refined. The program SQUEEZE (A. L. Spek J. Appl. 
Cryst., 2003, 36, 7-13) was therefore used to remove mathematically 
the effect of the solvent. 
The quoted formula and derived parameters are not included the squeezed
solvent molecules.
;
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.899
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1237
_refine_ls_number_reflns         12096
_refine_ls_number_restraints     1339
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0971P)^2^+12.5718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1994
_refine_ls_wR_factor_ref         0.2122
_reflns_number_gt                9037
_reflns_number_total             12096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00828_si_002.cif
_cod_data_source_block           erk8303
_cod_depositor_comments
'Adding full bibliography for 4086908--4086918.cif.'
_cod_database_code               4086917
_shelx_res_checksum              84262
_shelx_hkl_checksum              88061