Trimacrocyclic hexasubstituted benzene linked by labile octahedral [X(CHCl3)6]‒ clusters
Lai, Zhenzhen; Li, Aimin; Peng, Sangshan; Sessler, Jonathan L.; He, Qing; Chemical Science  (2021) –; doi:10.1039/D1SC03713G

data_1564358
_publ_section_title
;
 Trimacrocyclic hexasubstituted benzene linked by labile octahedral
 [X(CHCl3)6]-- clusters
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03713G
_journal_year                    2021
_chemical_formula_moiety
'1(Br), 6(C H Cl3), 2(C66 H72 O18), 2(C1 H5.5 N3)'
_chemical_formula_sum            'C140 H161 Br Cl18 N6 O36'
_chemical_formula_weight         3221.75
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-03-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-03-06 deposited with the CCDC.	2021-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.8600(8)
_cell_length_b                   21.8600(8)
_cell_length_c                   27.7568(10)
_cell_measurement_reflns_used    2295
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8460
_cell_measurement_theta_min      3.9400
_cell_volume                     11486.8(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0697
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -26.00  85.00   1.00    2.00    --   35.42   0.00 -30.00  111
  2  \w     38.00 109.00   1.00    4.00    --  105.82 -94.00-150.00   71
  3  \w     43.00 121.00   1.00    4.00    --  105.82 -45.00-180.00   78
  4  \w     82.00 108.00   1.00    4.00    --  105.82  15.00 -90.00   26
  5  \w    124.00 172.00   1.00    4.00    --  105.82  15.00 -90.00   48
  6  \w     81.00 126.00   1.00    4.00    --  105.82  77.00 -60.00   45
  7  \w     24.00  61.00   1.00    2.00    --   35.42-125.00 -60.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0562700000
_diffrn_orient_matrix_UB_12      0.0214759000
_diffrn_orient_matrix_UB_13      -0.0091913000
_diffrn_orient_matrix_UB_21      -0.0281629000
_diffrn_orient_matrix_UB_22      -0.0225851000
_diffrn_orient_matrix_UB_23      0.0516497000
_diffrn_orient_matrix_UB_31      0.0516170000
_diffrn_orient_matrix_UB_32      0.0751032000
_diffrn_orient_matrix_UB_33      0.0181392000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8089
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.328
_diffrn_reflns_theta_min         2.825
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       cubic
_exptl_crystal_F_000             5016
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4902
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.1013
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1594P)^2^+43.9422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2969
_refine_ls_wR_factor_ref         0.3200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3566
_reflns_number_total             4902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03713g2.cif
_cod_data_source_block           1-GuaBr
_cod_original_cell_volume        11486.8(9)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1564358
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 O10 H50'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
2. Restrained distances
 O6-C22 \\sim O6-C22A
 with sigma of 0.02
3. Others
 Sof(H1BC)=Sof(H1BD)=Sof(C22A)=Sof(H22C)=Sof(H22D)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C22)=Sof(H22A)=Sof(H22B)=FVAR(1)
 Fixed Sof: H1A(0.91667) H1B(0.91667)
4.a Ternary CH refined with riding coordinates:
 C24(H24)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B),
 C13(H13A,H13B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C22A(H22C,H22D)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C15(H15), C16(H16), C17(H17), C18(H18)
4.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_shelx_res_checksum              95218
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.796
_oxdiff_exptl_absorpt_empirical_full_min 0.705