Accurate construction of monolayer, bilayer, sandwich bilayer, four-layer, multi-layer and chiral bilayer 2D pillararene-type supramolecular networks.
Chen, Zhao-Nian; Zhang, Le-Ping; Wu, Huai-Li; Qi, Qiao-Yan; Yan, Meng; Tian, Jia; Yang, Guan-Yu; Li, Zhan-Ting; Yang, Bo; Chemical science 15 (2024) 13191–13200; doi:10.1039/d4sc03022b

data_1572083
_publ_section_title
;
 Accurate construction of monolayer, bilayer, sandwich bilayer,
 four-layer, multi-layer and chiral bilayer 2D pillararene-type
 supramolecular networks.
;
_journal_issue                   33
_journal_name_full               'Chemical science'
_journal_page_first              13191
_journal_page_last               13200
_journal_paper_doi               10.1039/d4sc03022b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C H2 Cl2), C85 H70 N4 O6, 2(C H4 O)'
_chemical_formula_sum            'C89 H82 Cl4 N4 O8'
_chemical_formula_weight         1477.38
_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             2024-06-18
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-25 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                94.9090(10)
_cell_angle_beta                 97.0560(10)
_cell_angle_gamma                91.9560(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9179(3)
_cell_length_b                   17.0625(4)
_cell_length_c                   17.3348(4)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      58.39
_cell_measurement_theta_min      3.00
_cell_volume                     3774.09(15)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE MetalJet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47111
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.903
_diffrn_reflns_theta_min         2.244
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1060 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.8682.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.112
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         13808
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0842
_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^)+(0.1371P)^2^+6.0051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2324
_refine_ls_wR_factor_ref         0.2696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8666
_reflns_number_total             13808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           230420zh_zhcz199461_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1572083--1572100.cif.
;
_cod_database_code               1572083
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.853
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O8-C89 \\sim O8-C89A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C89 \\sim C89A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C89A) \\sim Ueq, Uanis(C89) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H8B)=Sof(C89A)=Sof(H89A)=Sof(H89B)=Sof(H89C)=1-FVAR(1)
 Sof(H8A)=Sof(C89)=Sof(H89D)=Sof(H89E)=Sof(H89F)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C66(H66A,H66B), C57(H57A,H57B), C85(H85A,H85B), C76(H76A,
 H76B), C86(H86A,H86B), C87(H87A,H87B)
5.b Aromatic/amide H refined with riding coordinates:
 C72(H72), C42(H42), C69(H69), C19(H19), C14(H14), C45(H45), C20(H20),
 C59(H59), C17(H17), C23(H23), C62(H62), C81(H81), C51(H51), C50(H50), C22(H22),
  C10(H10), C35(H35), C36(H36), C48(H48), C4(H4), C11(H11), C7(H7), C47(H47),
 C78(H78), C2(H2), C39(H39), C8(H8), C38(H38), C25(H25), C5(H5), C1(H1),
 C27(H27), C30(H30), C28(H28), C53(H53), C55(H55), C24(H24), C29(H29), C32(H32),
  C56(H56), C33(H33), C52(H52)
5.c Tetrahedral OH refined with riding coordinates:
 O8(H8B), O8(H8A)
5.d Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C74(H74A,H74B,H74C), C65(H65A,H65B,H65C), C64(H64A,H64B,
 H64C), C75(H75A,H75B,H75C), C84(H84A,H84B,H84C), C88(H88A,H88B,H88C),
 C89A(H89A,H89B,H89C), C89(H89D,H89E,H89F)
5.e Idealised tetrahedral OH refined as rotating group:
 O7(H7A)
;
_shelx_res_checksum              43850
_shelx_hkl_checksum              74235
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU