Cagearenes: synthesis, characterization, and application for programmed vapor release
Fang, Shuai; Wang, Mengbin; Wu, Yating; Guo, Qing-Hui; Li, Errui; Li, Hao; Huang, Feihe; Chemical Science  (2022) –; doi:10.1039/D2SC01782B

data_1566923
_publ_section_title
;
 Cagearenes: synthesis, characterization, and application for programmed
 vapor release
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01782B
_journal_year                    2022
_chemical_formula_moiety         'C105 H96 O12, 3(C6 H6)'
_chemical_formula_sum            'C123 H114 O12'
_chemical_formula_weight         1784.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-18 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.813(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7782(7)
_cell_length_b                   18.2534(4)
_cell_length_c                   27.4389(10)
_cell_measurement_reflns_used    5031
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      36.41
_cell_measurement_theta_min      2.70
_cell_volume                     11419.5(6)
_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      192.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1285
_diffrn_reflns_av_unetI/netI     0.1191
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            64386
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.097
_diffrn_reflns_theta_min         2.698
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1220 before and 0.0731 after correction. The Ratio of minimum to maximum transmission is 0.8069. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       block
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10921
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.2533
_refine_ls_R_factor_gt           0.1120
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3053
_refine_ls_wR_factor_ref         0.3993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3357
_reflns_number_total             10921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01782b2.cif
_cod_data_source_block           210722fs
_cod_database_code               1566923
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C61-C60 = C62-C61
 1.39 with sigma of 0.02
 C62_$1-C62
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C60 \\sim C61 \\sim C62: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C57 \\sim C58 \\sim C59 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H49A(0.5) H49B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C27(H27A,H27B), C42(H42A,H42B), C49(H49A,H49B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15),
 C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C29(H29), C32(H32), C37(H37),
  C38(H38), C40(H40), C41(H41), C45(H45), C48(H48), C54(H54), C55(H55),
 C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62)
5.c Fitted hexagon refined as free rotating group:
 C54(C55,C56,C57,C58,C59)
5.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              94789
_shelx_fab_checksum              35147
_olex2_submission_special_instructions 'No special instructions were received'