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

data_7710588
_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_absolute_configuration unk
_chemical_formula_moiety         '0.5(C52 H28 B4 F20 N4 O8), C0.5 Cl2'
_chemical_formula_sum            'C26.5 H14 B2 Cl2 F10 N2 O4'
_chemical_formula_weight         706.955
_space_group_crystal_system      tetragonal
_space_group_IT_number           118
_space_group_name_Hall           'P -4 -2n'
_space_group_name_H-M_alt        'P -4 n 2'
_symmetry_Int_Tables_number      118
_audit_creation_date             2021-10-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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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                   13.0676(7)
_cell_length_b                   13.0676(7)
_cell_length_c                   16.7235(12)
_cell_measurement_reflns_used    8857
_cell_measurement_temperature    149.76
_cell_measurement_theta_max      23.71
_cell_measurement_theta_min      2.44
_cell_volume                     2855.7(3)
_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  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.76
_diffrn_measured_fraction_theta_full 0.9902
_diffrn_measured_fraction_theta_max 0.9917
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.9902
_diffrn_reflns_Laue_measured_fraction_max 0.9917
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56062
_diffrn_reflns_point_group_measured_fraction_full 0.9919
_diffrn_reflns_point_group_measured_fraction_max 0.9933
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.98
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0794 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.9242.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       plate
_exptl_crystal_F_000             1414.353
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.4174
_refine_diff_density_min         -0.4469
_refine_diff_density_rms         0.1072
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.77(14)
_refine_ls_d_res_high            0.7691
_refine_ls_d_res_low             10.2969
_refine_ls_goodness_of_fit_ref   1.1476
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    12
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1476
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+1.1229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.995
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              12
_reflns_limit_k_min              -11
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                2350
_reflns_number_total             3267
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt01716d2.cif
_cod_data_source_block           pre_a
_cod_original_sg_symbol_Hall     ' P -4 -2n'
_cod_database_code               7710588
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Cl1(0.5) Cl0A(0.5) C1(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C00M(H00a,H00b), C00N(H00c,H00d)
3.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00J(H00J), C00L(H00L)
;
_olex2_submission_special_instructions 'No special instructions were received'