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_1566924
_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, 5(C7 H8), C5 H12'
_chemical_formula_sum            'C145 H148 O12'
_chemical_formula_weight         2082.63
_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             2021-04-01
_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                82.321(2)
_cell_angle_beta                 87.364(2)
_cell_angle_gamma                74.141(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1660(6)
_cell_length_b                   18.6824(10)
_cell_length_c                   23.8099(13)
_cell_measurement_reflns_used    9144
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.19
_cell_volume                     6006.9(5)
_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 0.996
_diffrn_measurement_device_type  'zju Bruker D8 Venture Ims3.0'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            125272
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.447
_diffrn_reflns_theta_min         2.112
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1061 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.8697.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       block
_exptl_crystal_F_000             2228
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1420
_refine_ls_number_reflns         24666
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1432P)^2^+3.0635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18000
_reflns_number_total             24666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01782b2.cif
_cod_data_source_block           mo_210331_fang_699_0m
_cod_database_code               1566924
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.971
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111 \\sim C112: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
3. Others
 Sof(H14H)=Sof(H14I)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(H14J)=Sof(H14K)=Sof(C145)=Sof(H14L)=Sof(H14M)=Sof(H14N)=FVAR(1)
4.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),
 C142(H14D,H14E), C143(H14F,H14G), C144(H14J,H14K), C144(H14H,H14I)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C16(H16),
 C19(H19), C25(H25), C28(H28), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39),
  C41(H41), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49), C53(H53),
 C56(H56), C62(H62), C65(H65), C70(H70), C71(H71), C73(H73), C74(H74), C76(H76),
  C77(H77), C79(H79), C80(H80), C84(H84), C87(H87), C93(H93), C96(H96),
 C101(H101), C102(H102), C104(H104), C105(H105), C106(H106), C107(H107),
 C108(H108), C109(H109), C110(H110), C113(H113), C114(H114), C115(H115),
 C116(H116), C117(H117), C120(H120), C121(H121), C122(H122), C123(H123),
 C124(H124), C127(H127), C128(H128), C129(H129), C130(H130), C131(H131),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138)
4.c Fitted hexagon refined as free rotating group:
 C106(C107,C108,C109,C110,C111), C120(C121,C122,C123,C124,C125)
4.d 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), C119(H11D,H11E,H11F), C126(H12A,
 H12B,H12C), C133(H13C,H13D,H13E), C140(H14O,H14P,H14Q), C141(H14A,H14B,H14C),
 C1A(H1AA,H1AB,H1AC), C145(H14L,H14M,H14N)
;
_shelx_res_checksum              6874
_olex2_submission_special_instructions 'No special instructions were received'