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_1564355
_publ_section_title
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 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         'C66 H72 O18'
_chemical_formula_sum            'C66 H72 O18'
_chemical_formula_weight         1153.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                98.113(10)
_cell_angle_beta                 91.340(9)
_cell_angle_gamma                108.395(10)
_cell_formula_units_Z            4
_cell_length_a                   16.250(8)
_cell_length_b                   18.296(7)
_cell_length_c                   25.707(12)
_cell_measurement_reflns_used    459
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      15.81
_cell_measurement_theta_min      2.24
_cell_volume                     7161(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.990
_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  0.0949
_diffrn_reflns_av_unetI/netI     0.1453
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            78130
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.370
_diffrn_reflns_theta_min         2.141
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.1942
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1946 before and 0.0977 after correction.
The Ratio of minimum to maximum transmission is 0.2604.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.139
_refine_diff_density_max         1.403
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1513
_refine_ls_number_reflns         35530
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1685
_refine_ls_R_factor_gt           0.1093
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1789P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3100
_refine_ls_wR_factor_ref         0.3558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17730
_reflns_number_total             35530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03713g2.cif
_cod_data_source_block           receptor-1
_cod_depositor_comments
;

2022-03-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C132 H144 O36'
_cod_original_formula_weight         2306.46
_cod_original_formula_moiety         '2(C66 H72 O18)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        7161(5)
_cod_database_code               1564355
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.967
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95)
\\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(O26) \\sim Ueq,
Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(C99)
\\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(O28) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C126) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq,
Uanis(C129) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 O26, O27, C92, C93, C94, C95, C96, C97, C98, C99, C100
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C21(H21A,H21B), C24(H24A,H24B), C31(H31A,H31B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C43(H43A,H43B), C46(H46A,H46B), C53(H53A,H53B), C54(H54A,H54B),
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C65(H65A,H65B),
  C68(H68A,H68B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,
 H78B), C79(H79A,H79B), C80(H80A,H80B), C87(H87A,H87B), C90(H90A,H90B),
 C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10C,H10D), C101(H10E,
 H10F), C102(H10G,H10H), C109(H10I,H10J), C112(H11C,H11D), C119(H11E,H11F),
 C120(H12C,H12D), C121(H12E,H12F), C122(H12G,H12H), C123(H12I,H12J), C124(H12K,
 H12L), C131(H13C,H13D)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C18(H18), C19(H19),
 C26(H26), C27(H27), C28(H28), C29(H29), C38(H38), C39(H39), C40(H40), C41(H41),
  C48(H48), C49(H49), C50(H50), C51(H51), C60(H60), C61(H61), C62(H62),
 C63(H63), C70(H70), C71(H71), C72(H72), C73(H73), C82(H82), C83(H83), C84(H84),
  C85(H85), C92(H92), C93(H93), C94(H94), C95(H95), C104(H104), C105(H105),
 C106(H106), C107(H107), C114(H114), C115(H115), C116(H116), C117(H117),
 C126(H126), C127(H127), C128(H128), C129(H129)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7568
_shelx_fab_checksum              69463
_olex2_submission_special_instructions 'No special instructions were received'