Porous Materials Formed by Four Self-construction Processes
Liu, Qiuhua; Shen, Xiaorong; Dai, Ye; Zhang, Mengchen; Zhou, Zaichun; Organic & Biomolecular Chemistry  (2022) –; doi:10.1039/D2OB01530G

data_7158915
_publ_section_title
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 Porous Materials Formed by Four Self-construction Processes
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_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/D2OB01530G
_journal_year                    2022
_chemical_compound_source        THF/chloroform
_chemical_formula_moiety         'C70 H40 O20, 2(C4 H8 O)'
_chemical_formula_sum            'C78 H56 O22'
_chemical_formula_weight         1345.22
_chemical_name_common            cyclomer-1
_chemical_name_systematic        1-pentamer
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2020-07-02
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2022-08-22 deposited with the CCDC.	2022-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                93.479(4)
_cell_angle_beta                 93.467(4)
_cell_angle_gamma                92.039(4)
_cell_formula_units_Z            1
_cell_length_a                   9.672(2)
_cell_length_b                   11.175(3)
_cell_length_c                   15.326(3)
_cell_measurement_reflns_used    2597
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.33
_cell_volume                     1649.1(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9996
_diffrn_reflns_point_group_measured_fraction_full 0.592
_diffrn_reflns_point_group_measured_fraction_max 0.546
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.610
_diffrn_reflns_theta_min         2.329
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0642 before and 0.0332 after correction.
The Ratio of minimum to maximum transmission is 0.9096.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 884 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.9(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         8363
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.3547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.167
_reflns_Friedel_fraction_full    0.192
_reflns_Friedel_fraction_max     0.157
_reflns_number_gt                6279
_reflns_number_total             8363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob01530g2.cif
_cod_data_source_block           ww
_cod_database_code               7158915
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.989
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C65A) \\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(C66A) \\sim Ueq,
Uanis(C68A) \\sim Ueq, Uanis(C67A) \\sim Ueq, Uanis(C69A) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(C66) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62A)
\\sim Ueq, Uanis(C60A) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C58) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(C59A) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63A)
\\sim Ueq, Uanis(C58A) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C54A) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C51A) \\sim Ueq, Uanis(C55A)
\\sim Ueq, Uanis(C56A) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq,
Uanis(C51) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(O17A) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O18A) \\sim Ueq, Uanis(C57A) \\sim Ueq,
Uanis(C57) \\sim Ueq, Uanis(O16A) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(O16)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C65) \\sim Ueq, Uanis(C65A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Fixed Sof: H52(0.5) H52A(0.5) H53(0.5) H53A(0.5) O16(0.5) O17(0.5) O18(0.5)
 C51(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5) C56(0.5) C57(0.5) C58(0.5)
 C59(0.5) H59(0.5) C60(0.5) H60(0.5) C62(0.5) H62(0.5) C63(0.5) H63(0.5)
 C65(0.5) C66(0.5) H66(0.5) C67(0.5) H67(0.5) C68(0.5) H68(0.5) C69(0.5)
 H69(0.5) C70(0.5) O16A(0.5) O17A(0.5) O18A(0.5) C51A(0.5) C54A(0.5) H54A(0.5)
 C55A(0.5) H55A(0.5) C56A(0.5) C57A(0.5) C58A(0.5) C59A(0.5) H59A(0.5)
 C60A(0.5) H60A(0.5) C62A(0.5) H62A(0.5) C63A(0.5) H63A(0.5) C65A(0.5)
 C66A(0.5) H66A(0.5) C67A(0.5) H67A(0.5) C68A(0.5) H68A(0.5) C69A(0.5)
 H69A(0.5) C70A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27),
  C31(H31), C32(H32), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40),
 C41(H41), C45(H45), C46(H46), C48(H48), C49(H49), C52(H52), C52(H52A),
 C53(H53), C53(H53A), C54(H54), C55(H55), C59(H59), C60(H60), C62(H62),
 C63(H63), C66(H66), C67(H67), C68(H68), C69(H69), C54A(H54A), C55A(H55A),
 C59A(H59A), C60A(H60A), C62A(H62A), C63A(H63A), C66A(H66A), C67A(H67A),
 C68A(H68A), C69A(H69A)
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_shelx_res_checksum              63373
_olex2_submission_special_instructions 'No special instructions were received'