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_1566925
_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, C9 H12'
_chemical_formula_sum            'C114 H108 O12'
_chemical_formula_weight         1670.00
_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             2021-06-08
_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                112.073(13)
_cell_angle_beta                 103.948(14)
_cell_angle_gamma                93.107(10)
_cell_formula_units_Z            2
_cell_length_a                   13.898(4)
_cell_length_b                   19.031(6)
_cell_length_c                   24.191(8)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.35
_cell_volume                     5680(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_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      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            157316
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.166
_diffrn_reflns_theta_min         2.025
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1124 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.9682.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.977
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         25049
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0800P)^2^+1.9040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17618
_reflns_number_total             25049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01782b2.cif
_cod_data_source_block           mo_210601_fang_699_135_0m
_cod_database_code               1566925
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.979
_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
 C83-O9 \\sim C84-O9A
 with sigma of 0.02
 O9-C88 \\sim O9A-C88A
 with sigma of 0.02
 C83-O9A \\sim C84-O9
 with sigma of 0.02
 C86-O10 \\sim C87-O10A
 with sigma of 0.02
 O10-C89 \\sim O10-C89A
 with sigma of 0.02
 C86-O10A \\sim C87-O10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O9 \\sim C88 \\sim O9A \\sim C88A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
O10 \\sim C89 \\sim O10A \\sim C89A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
4. Others
 Sof(H83)=Sof(O9A)=Sof(C88A)=Sof(H88D)=Sof(H88E)=Sof(H88F)=1-FVAR(1)
 Sof(O9)=Sof(H84)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=FVAR(1)
 Sof(H86)=Sof(O10A)=Sof(C89A)=Sof(H89D)=Sof(H89E)=Sof(H89F)=1-FVAR(2)
 Sof(O10)=Sof(H87)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C22(H22A,H22B), C31(H31A,H31B), C50(H50A,H50B), C59(H59A,
 H59B), C68(H68A,H68B), C81(H81A,H81B), C90(H90A,H90B), C99(H99A,H99B)
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), C24(H24), C27(H27), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39),
  C41(H41), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49), C52(H52),
 C55(H55), C61(H61), C64(H64), C70(H70), C71(H71), C73(H73), C74(H74), C76(H76),
  C77(H77), C79(H79), C80(H80), C83(H83), C84(H84), C86(H86), C87(H87),
 C93(H93), C96(H96), C101(H101), C102(H102), C104(H104), C105(H105), C107(H107),
  C109(H109), C111(H111)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C97(H97A,H97B,H97C),
 C98(H98A,H98B,H98C), C112(H11A,H11B,H11C), C113(H11D,H11E,H11F), C114(H11G,
 H11H,H11I), C88A(H88D,H88E,H88F), C89A(H89D,H89E,H89F)
;
_shelx_res_checksum              21289
_shelx_fab_checksum              2258
_olex2_submission_special_instructions 'No special instructions were received'