A cylinder-shaped macrocycle formed <i>via</i> Friedel-Crafts reaction.
Zhu, Dingsheng; Fang, Shuai; Tong, Lu; Lei, Ye; Wu, Guangcheng; Chudhary, Tayba; Li, Hao; Chemical communications (Cambridge, England) 57 (2021) 4440–4443; doi:10.1039/d1cc00498k

data_7128115
_publ_section_title
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 A cylinder-shaped macrocycle formed <i>via</i> Friedel-Crafts reaction.
;
_journal_issue                   36
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4440
_journal_page_last               4443
_journal_paper_doi               10.1039/d1cc00498k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C90 H72 O12'
_chemical_formula_sum            'C90 H72 O12'
_chemical_formula_weight         1345.47
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-09 deposited with the CCDC.	2021-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                83.19(2)
_cell_angle_beta                 70.854(15)
_cell_angle_gamma                69.918(19)
_cell_formula_units_Z            1
_cell_length_a                   11.934(8)
_cell_length_b                   12.680(8)
_cell_length_c                   15.587(11)
_cell_measurement_reflns_used    577
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      39.199
_cell_measurement_theta_min      3.227
_cell_volume                     2093(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      172.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1355
_diffrn_reflns_av_unetI/netI     0.1980
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24946
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.992
_diffrn_reflns_theta_min         3.229
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.9930
_exptl_absorpt_correction_T_min  0.9870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1401 before and 0.0792 after correction. The Ratio of minimum to maximum transmission is 0.5577. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.2391
_refine_ls_R_factor_gt           0.1412
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3542
_refine_ls_wR_factor_ref         0.4399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2701
_reflns_number_total             8284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00498k2.cif
_cod_data_source_block           mj21008_0m
_cod_depositor_comments          'Adding full bibliography for 7128115.cif.'
_cod_database_code               7128115
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C21(H21), C22(H22),
 C24(H24), C27(H27), C28(H28), C29(H29), C36(H36), C37(H37), C38(H38), C41(H41),
  C42(H42), C43(H43)
2.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              21279
_shelx_hkl_checksum              22362
_shelx_fab_checksum              56227
_olex2_submission_special_instructions 'No special instructions were received'