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

data_7710587
_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         'C30 H28 B2 N2 O4'
_chemical_formula_sum            'C30 H28 B2 N2 O4'
_chemical_formula_weight         502.216
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2021-10-15
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                112.635(3)
_cell_angle_beta                 99.067(4)
_cell_angle_gamma                108.572(4)
_cell_formula_units_Z            1
_cell_length_a                   7.8349(13)
_cell_length_b                   9.0678(13)
_cell_length_c                   10.3304(16)
_cell_measurement_reflns_used    3708
_cell_measurement_temperature    149.49
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.68
_cell_volume                     608.31(17)
_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)'
_diffrn_ambient_temperature      149.49
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9929
_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  0.0323
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.9977
_diffrn_reflns_Laue_measured_fraction_max 0.9929
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11686
_diffrn_reflns_point_group_measured_fraction_full 0.9977
_diffrn_reflns_point_group_measured_fraction_max 0.9929
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.9478.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             264.124
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.2864
_refine_diff_density_min         -0.2895
_refine_diff_density_rms         0.0585
_refine_ls_d_res_high            0.7795
_refine_ls_d_res_low             6.7531
_refine_ls_goodness_of_fit_ref   1.0584
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0584
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0430P)^2^+0.2015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              10
_reflns_limit_k_min              -11
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2051
_reflns_number_total             2672
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt01716d2.cif
_cod_data_source_block           FINAL_a
_cod_database_code               7710587
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C008(H00a,H00b), C00A(H00c,H00d)
2.b Aromatic/amide H refined with riding coordinates:
 C007(H007), C009(H009), C00B(H00e), C00C(H00f), C00D(H00g), C00E(H00h),
 C00F(H00i), C00G(H00j), C00H(H00k), C00I(H00l)
;
_olex2_submission_special_instructions 'No special instructions were received'