Transition-Metal Oxos as the Lewis Basic Component of Frustrated Lewis Pairs.
Lambic, Nikola S.; Sommer, Roger D.; Ison, Elon A.; Journal of the American Chemical Society 138 (2016) 4832–4842; doi:10.1021/jacs.6b00705

data_4130136
_publ_section_title
;
 Transition-Metal Oxos as the Lewis Basic Component of Frustrated Lewis
 Pairs.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4832
_journal_page_last               4842
_journal_paper_doi               10.1021/jacs.6b00705
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C49 H34 B F15 N3 O Re,0.398(C6 H6), 0.602(C5 H12)'
_chemical_formula_sum            'C54.4 H43.61 B F15 N3 O Re'
_chemical_formula_weight         1237.35
_chemical_name_common            119
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                69.605(3)
_cell_angle_beta                 74.537(3)
_cell_angle_gamma                72.549(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0773(7)
_cell_length_b                   13.7901(9)
_cell_length_c                   16.7455(9)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      26.2911
_cell_measurement_theta_min      2.3685
_cell_volume                     2452.4(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66459
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.579
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.877
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+1.3988P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0488
_reflns_number_gt                8685
_reflns_number_total             10040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00705_si_002.cif
_cod_data_source_block           119
_cod_original_formula_sum        'C54.40 H43.61 B F15 N3 O Re'
_cod_database_code               4130136
_shelx_res_checksum              29300
_shelx_hkl_checksum              90486