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_1564359
_publ_section_title
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 Trimacrocyclic hexasubstituted benzene linked by labile octahedral
 [X(CHCl3)6]-- clusters
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03713G
_journal_year                    2021
_chemical_formula_moiety
'1(Cl), 6(C H0.969 Cl3), 2(C66 H70.574 O18), 2(C1 H5.5 N3)'
_chemical_formula_sum            'C140 H157.96 Cl19 N6 O36'
_chemical_formula_weight         3174.22
_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   mixed
_audit_creation_date             2021-03-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
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_audit_update_record
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2021-03-06 deposited with the CCDC.	2021-08-11 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.694(3)
_cell_length_b                   21.694(3)
_cell_length_c                   27.480(4)
_cell_measurement_reflns_used    1594
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      22.15
_cell_measurement_theta_min      2.29
_cell_volume                     11200(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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            24200
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.058
_diffrn_reflns_theta_min         2.291
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6000
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1367 before and 0.0540 after correction.
The Ratio of minimum to maximum transmission is 0.8043.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       bulk
_exptl_crystal_F_000             4953
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.359
_exptl_crystal_size_min          0.311
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7306
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.1054
_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^)+(0.0630P)^2^+138.2162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2633
_refine_ls_wR_factor_ref         0.2670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6412
_reflns_number_total             7306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03713g2.cif
_cod_data_source_block           1-GuaCl
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1564359
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.812
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All C(H,H,H,H)
  groups, All N(H,H) groups
2. Restrained distances
 O1A-C1A \\sim O1A-C1
 with sigma of 0.02
 O00D-C21 \\sim O6A-C21
 with sigma of 0.02
 O1A-C1 \\sim O1-C1
 with sigma of 0.02
 O1A-C2 \\sim O1-C2
 with sigma of 0.02
 O1A-C1A \\sim O1-C1A
 with sigma of 0.02
 Cl3-C24 \\sim Cl4-C24 \\sim Cl2-C24
 with sigma of 0.02
 Cl4-C24 \\sim Cl5-C24
 with sigma of 0.02
 Cl3-C24 \\sim Cl6-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl5) \\sim Ueq, Uanis(Cl6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Sof(C1)=Sof(H1A)=Sof(H1B)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=FVAR(1)
 Sof(H2BC)=Sof(H2BD)=Sof(O1)=1-FVAR(2)
 Sof(H2AA)=Sof(H2AB)=Sof(O1A)=FVAR(2)
 Sof(H22)=Sof(O6A)=1-FVAR(3)
 Sof(H22A)=Sof(H22B)=Sof(O00D)=FVAR(3)
 Sof(H24A)=Sof(Cl6)=1-FVAR(4)
 Sof(Cl3)=FVAR(4)
 Sof(Cl5)=1-FVAR(5)
 Sof(H24)=Sof(Cl4)=FVAR(5)
 Fixed Sof: H1C(0.91667) H1D(0.91667)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C24(H24A)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD), C3(H3A,H3B), C10(H10A,H10B), C13(H13A,H13B),
 C20(H20A,H20B), C22(H22A,H22B), C1A(H1AA,H1AB), C1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C15(H15), C16(H16), C17(H17), C18(H18),
 C22(H22)
5.d X=CH2 refined with riding coordinates:
 N1(H1C,H1D)
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_shelx_res_checksum              56526
_olex2_submission_special_instructions 'No special instructions were received'