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_1564357
_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(I), 6(C H Cl3), 2(C67 H77.5 N3 O18)'
_chemical_formula_sum            'C140 H161 Cl18 I N6 O36'
_chemical_formula_weight         3268.74
_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                   21.738(3)
_cell_length_b                   21.738(3)
_cell_length_c                   27.712(5)
_cell_measurement_reflns_used    1003
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      20.35
_cell_measurement_theta_min      2.20
_cell_volume                     11341(3)
_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 0.998
_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  0.0473
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40495
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_min         2.205
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       bulk
_exptl_crystal_F_000             5070
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.332
_exptl_crystal_size_min          0.315
_refine_diff_density_max         1.205
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6249
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.1032
_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^)+(0.0968P)^2^+164.8354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2752
_refine_ls_wR_factor_ref         0.2797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5530
_reflns_number_total             6249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03713g2.cif
_cod_data_source_block           GuaI
_cod_original_cell_volume        11341(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1564357
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.820
_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
 O5A-C18 \\sim O5-C18
 with sigma of 0.02
 C20-C19A \\sim C20-C19
 with sigma of 0.02
 O5A-C19A \\sim O5-C19A
 with sigma of 0.02
 O5A-C19A \\sim O5A-C19
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl1 \\sim Cl3: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
4. Rigid body (RIGU) restrains
 Cl2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(H18C)=Sof(H18D)=Sof(O5)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(O5A)=FVAR(1)
 Sof(H20C)=Sof(H20D)=Sof(C19)=Sof(H19C)=Sof(H19D)=1-FVAR(2)
 Sof(H20A)=Sof(H20B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=FVAR(2)
 Fixed Sof: H1A(0.91667) H1B(0.91667)
6.a Ternary CH refined with riding coordinates:
 C23(H23)
6.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C17(H17A,H17B), C18(H18A,H18B), C18(H18C,H18D),
 C20(H20A,H20B), C20(H20C,H20D), C21(H21A,H21B), C22(H22A,H22B), C19A(H19A,
 H19B), C19(H19C,H19D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15)
6.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_shelx_res_checksum              7816
_olex2_submission_special_instructions 'No special instructions were received'