The synthesis and application of <i>o</i>-carborane-based macrocyclic arenes.
Liu, Jiayi; Fu, Meigui; Yuan, Shuai; Lin, Caixia; Yuan, Yaofeng; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15316–15323; doi:10.1039/d4dt02001d

data_7716865
_publ_section_title
;
 The synthesis and application of <i>o</i>-carborane-based macrocyclic
 arenes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15316
_journal_page_last               15323
_journal_paper_doi               10.1039/d4dt02001d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '0.029(C86 H120 B20 O8)'
_chemical_formula_sum            'C H B Cl O'
_chemical_formula_weight         75.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-31 deposited with the CCDC.	2024-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            138
_cell_length_a                   35.4113(3)
_cell_length_b                   16.80310(10)
_cell_length_c                   17.1648(2)
_cell_measurement_reflns_used    28564
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.1870
_cell_measurement_theta_min      2.5400
_cell_volume                     9914.44(16)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48778
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.974
_diffrn_reflns_theta_min         2.927
_exptl_absorpt_coefficient_mu    9.292
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       block
_exptl_crystal_F_000             5106
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         10095
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+10.0973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.1756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8854
_reflns_number_total             10095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02001d2.cif
_cod_data_source_block           platon_sq
_cod_depositor_comments
'Adding full bibliography for 7716865--7716866.cif.'
_cod_original_cell_volume        9914.43(16)
_cod_database_code               7716865
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.402
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C44-C43
 1.54 with sigma of 0.02
 C42A-C41A = C43A-C42A = C44A-C43A
 1.5 with sigma of 0.01
 C42-C41 = C43-C42 = C44-C43
 1.5 with sigma of 0.01
 O3-C41 \\sim O3-C41A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 C44-C43 \\sim C44A-C43A
 with sigma of 0.02
 C42-C43 \\sim C42A-C43A
 with sigma of 0.02
 O3-C42 \\sim O3-C42A
 with sigma of 0.04
 C41-C43 \\sim C41A-C43A
 with sigma of 0.04
 C44-C42 \\sim C44A-C42A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C41A \\sim C42A \\sim C43A \\sim C44A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C42) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C41, C42, C43, C44, C41A, C42A, C43A, C44A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C43A)=
 Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C24(H24A,H24B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C41A(H41C,
 H41D), C42A(H42C,H42D), C43A(H43C,H43D)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C15(H15), C26(H26), C29(H29),
 C36(H36), C37(H37), C39(H39), C40(H40)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C34(H34A,H34B,H34C), C44(H44A,H44B,
 H44C), C44A(H44D,H44E,H44F)
6.d Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4A), B5(H5A), B6(H6), B7(H7A), B8(H8A), B9(H9),
 B10(H10)
;
_shelx_res_checksum              32732
_shelx_fab_checksum              78836
_olex2_submission_special_instructions 'No special instructions were received'