Dihydrogen cleavage by a dimetalloxycarbene-borane frustrated Lewis pair.
Paparo, Albert; Nguyen, Anh L. P.; Silvia, Jared S.; Spaniol, Thomas P.; Maron, Laurent; Cummins, Christopher C.; Okuda, Jun; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10692–10695; doi:10.1039/d1dt02273c

data_7707849
_publ_section_title
;
 Dihydrogen cleavage by a dimetalloxycarbene-borane frustrated Lewis pair.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10692
_journal_page_last               10695
_journal_paper_doi               10.1039/d1dt02273c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'2(C55 H55 B F15 N3 O2 Ti), 0.5(C8 H20 O2), 2(C4 H10 O)'
_chemical_formula_sum            'C122 H140 B2 F30 N6 O7 Ti2'
_chemical_formula_weight         2489.81
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_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   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-05-18 deposited with the CCDC.	2021-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                64.910(3)
_cell_angle_beta                 89.059(3)
_cell_angle_gamma                67.790(3)
_cell_formula_units_Z            1
_cell_length_a                   13.570(2)
_cell_length_b                   16.462(3)
_cell_length_c                   16.688(3)
_cell_measurement_reflns_used    5207
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.31
_cell_volume                     3079.3(9)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33876
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         1.951
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       plate
_exptl_crystal_F_000             1294
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether and benzene'
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.404
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         11182
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0972P)^2^+5.8481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.2020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8286
_reflns_number_total             11182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02273c2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7707848--7707849.cif.'
_cod_original_cell_volume        3079.4(10)
_cod_database_code               7707849
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2013-4
_shelx_res_checksum              33968
_shelx_hkl_checksum              29957