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_1566922
_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         '3(C H Cl3), C105 H96 O12'
_chemical_formula_sum            'C108 H99 Cl9 O12'
_chemical_formula_weight         1907.92
_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             2021-04-07
_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                69.100(2)
_cell_angle_beta                 74.702(2)
_cell_angle_gamma                88.173(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9569(4)
_cell_length_b                   17.9039(5)
_cell_length_c                   22.5745(6)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.837
_cell_measurement_theta_min      2.826
_cell_volume                     5434.3(3)
_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 0.991
_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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            64089
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.987
_diffrn_reflns_theta_min         3.316
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.696
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1464 before and 0.0849 after correction. The Ratio of minimum to maximum transmission is 0.6775. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1174
_refine_ls_number_reflns         20496
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.1124
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2558
_refine_ls_wR_factor_ref         0.2719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14000
_reflns_number_total             20496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01782b2.cif
_cod_data_source_block           210407fs_0m
_cod_database_code               1566922
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.890
_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
 Cl4-C2 = Cl5-C2 = Cl6-C2 = Cl9-C3 = Cl7-C3 = Cl8-C3 = Cl2-C1 = Cl1-C1 = Cl3-C1
 1.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim Cl3 \\sim Cl1 \\sim Cl2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C3 \\sim Cl8 \\sim Cl9 \\sim Cl7: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C2 \\sim Cl6 \\sim Cl5 \\sim Cl4: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C25(H25A,H25B), C34(H34A,H34B), C43(H43A,H43B), C57(H57A,
 H57B), C66(H66A,H66B), C75(H75A,H75B), C93(H93A,H93B), C102(H10D,H10E)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C22(H22),
 C23(H23), C29(H29), C33(H33), C38(H38), C42(H42), C45(H45), C46(H46), C48(H48),
  C49(H49), C51(H51), C54(H54), C55(H55), C61(H61), C65(H65), C70(H70),
 C74(H74), C77(H77), C78(H78), C80(H80), C81(H81), C83(H83), C84(H84), C85(H85),
  C86(H86), C87(H87), C90(H90), C91(H91), C97(H97), C101(H101), C103(H103),
 C104(H104), C105(H105), C106(H106), C107(H107)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C37(H37A,H37B,
 H37C), C41(H41A,H41B,H41C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C69(H69A,
 H69B,H69C), C73(H73A,H73B,H73C), C96(H96A,H96B,H96C), C100(H10A,H10B,H10C),
 C108(H10F,H10G,H10H)
;
_shelx_res_checksum              73242
_shelx_fab_checksum              82286
_olex2_submission_special_instructions 'No special instructions were received'