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_4130138
_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         '(C43 H29 B F15 N3 O Re), (C7 H8)'
_chemical_formula_sum            'C50 H37 B F15 N3 O Re'
_chemical_formula_weight         1131.77
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2377(3)
_cell_length_b                   16.2377(3)
_cell_length_c                   36.5045(7)
_cell_measurement_reflns_used    707
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      22.8246
_cell_measurement_theta_min      2.0586
_cell_volume                     9624.9(3)
_computing_cell_refinement       'APEX2 v2014.5-0 (Bruker AXS)'
_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)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            93856
_diffrn_reflns_theta_full        28.77
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.620
_exptl_absorpt_correction_T_max  0.50
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.401
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.304
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.086
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         12500
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0204P)^2^+11.5488P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0695
_reflns_number_gt                11803
_reflns_number_total             12500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00705_si_002.cif
_cod_data_source_block           rds301
_cod_original_cell_volume        9624.9(4)
_cod_database_code               4130138
_shelx_res_checksum              69650
_shelx_hkl_checksum              62113
_shelx_fab_checksum              30658