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_4130137
_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         'C31 H29 F5 N3 O Re'
_chemical_formula_sum            'C31 H29 F5 N3 O Re'
_chemical_formula_weight         740.77
_chemical_name_common            FLP2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   24.5115(7)
_cell_length_b                   24.6966(9)
_cell_length_c                   18.6378(6)
_cell_measurement_reflns_used    491
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      24.3059
_cell_measurement_theta_min      2.2021
_cell_volume                     11282.4(6)
_computing_cell_refinement       'APEX2 v2014.9-0 (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      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0616
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            71001
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.17
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.371
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5824
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.817
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    88
_refine_ls_number_parameters     752
_refine_ls_number_reflns         13979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+4.2507P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                11071
_reflns_number_total             13979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00705_si_002.cif
_cod_data_source_block           rds325
_cod_database_code               4130137
_shelx_res_checksum              63913
_shelx_hkl_checksum              74942