Intramolecular Frustrated Lewis Pair Mediated Approach to the C=O Bond Activation and Cleavage of Carbon Dioxide
Krempner, Clemens; Manankandayalage, Chamila; Katakam, Nandakumar; Unruh, Daniel K.; Aquino, Adelia; Chemical Communications  (2022) –; doi:10.1039/D2CC03413A

data_7130379
_publ_section_title
;
 Intramolecular Frustrated Lewis Pair Mediated Approach to the C=O Bond
 Activation and Cleavage of Carbon Dioxide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03413A
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_sum            'C38 H30 Al B F15 N3 O2'
_chemical_formula_weight         883.44
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-02-17T14:44:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7204(2)
_cell_length_b                   10.81340(10)
_cell_length_c                   18.6892(2)
_cell_measurement_reflns_used    50961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.324
_cell_measurement_theta_min      2.328
_cell_volume                     3783.28(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0456148
_diffrn_orient_matrix_UB_12      0.0767246
_diffrn_orient_matrix_UB_13      -0.0523059
_diffrn_orient_matrix_UB_21      0.0625335
_diffrn_orient_matrix_UB_22      -0.0023862
_diffrn_orient_matrix_UB_23      0.0535343
_diffrn_orient_matrix_UB_31      0.0280003
_diffrn_orient_matrix_UB_32      -0.1200714
_diffrn_orient_matrix_UB_33      -0.0344364
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66315
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.495
_diffrn_reflns_theta_min         4.722
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.511
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_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.40.70a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 3606 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         7871
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.7084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.9
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                7763
_reflns_number_total             7871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03413a2.cif
_cod_data_source_block           4
_cod_database_code               7130379
_shelx_estimated_absorpt_t_min   0.673
_shelx_estimated_absorpt_t_max   0.792
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              69796
_shelx_hkl_checksum              743