Towards macrocyclic frustrated Lewis pairs
Yeung, Jason; Becker, Matthias; Stephan, Douglas W.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01716D

data_7710586
_publ_section_title
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 Towards macrocyclic frustrated Lewis pairs
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01716D
_journal_year                    2022
_chemical_formula_moiety
'C52 H22 B4 Br4 F20 N4 O8, 2(C H2 Cl2), C H Cl2'
_chemical_formula_sum            'C55 H27 B4 Br4 Cl6 F20 N4 O8'
_chemical_formula_weight         1827.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-08-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1341(4)
_cell_length_b                   27.7360(12)
_cell_length_c                   21.0109(9)
_cell_measurement_reflns_used    9181
_cell_measurement_temperature    149.25
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.94
_cell_volume                     6488.5(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69874
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.630
_diffrn_reflns_theta_min         2.196
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.843
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6052
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1026 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.8117.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       Shard
_exptl_crystal_F_000             3564
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.963
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+16.9570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5330
_reflns_number_total             7486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01716d2.cif
_cod_data_source_block           jky0125_a
_cod_database_code               7710586
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.784
_shelx_estimated_absorpt_t_min   0.659
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: C27(0.5) H27(0.5)
3.a Ternary CH refined with riding coordinates:
 C27(H27)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C6(H6A,H6B), C26(H26A,H26B)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C2(H2), C19(H19), C4(H4)
;
_shelx_res_checksum              33101
_shelx_hkl_checksum              73783
_olex2_submission_special_instructions 'No special instructions were received'