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_1572093
_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         'C114 H114 Cu3 N4 O20, 4[C3H7NO], 3[H2O]'
_chemical_formula_sum            'C126 H148 Cu3 N8 O27'
_chemical_formula_weight         2397.14
_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   mixed
_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                69.195(4)
_cell_angle_beta                 81.270(4)
_cell_angle_gamma                83.209(3)
_cell_formula_units_Z            2
_cell_length_a                   16.692(2)
_cell_length_b                   19.198(3)
_cell_length_c                   20.104(3)
_cell_measurement_reflns_used    6369
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      25.21
_cell_measurement_theta_min      2.18
_cell_volume                     5938.1(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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22942
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        20.000
_diffrn_reflns_theta_max         20.000
_diffrn_reflns_theta_min         2.159
_diffrn_source                   TXS
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_type              'Rotaing Anode'
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0890 before and 0.0559 after correction.
The Ratio of minimum to maximum transmission is 0.6300.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             2526
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.274
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1283
_refine_ls_number_reflns         10964
_refine_ls_number_restraints     975
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_gt           0.1238
_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^)+(0.1200P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3054
_refine_ls_wR_factor_ref         0.3325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6754
_reflns_number_total             10964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           230813lu_lgpz099052_2_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_original_cell_volume        5938.0(14)
_cod_database_code               1572093
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.919
_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
 O6-C6 = O5-C6 = O4-C4 = O3-C4 = O2-C2 = O1-C2 = O7-C8 = O8-C8
 1.25 with sigma of 0.01
 C7-C8 = C1-C2 = C5-C6 = C3-C4
 1.5 with sigma of 0.01
 C47-C46 = C45-C44 = C56-C55 = C58-C57 = C96-C95 = C98-C97 = C109-C108 = C107-
 C106
 1.5 with sigma of 0.01
 O9-C114 = O10-C114
 1.25 with sigma of 0.01
 C111-C112
 1.5 with sigma of 0.01
 O12-C112 = O11-C112
 1.25 with sigma of 0.01
 C113-C114
 1.5 with sigma of 0.01
 C113-O9 \\sim C113-O10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
O12 \\sim O11 \\sim C112 \\sim C111: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
O9 \\sim C114 \\sim O10 \\sim C113: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Riding coordinates:
 C113(H11F,H11G,H11H)
4.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C44(H44A,H44B), C46(H46A,H46B), C48(H48A,H48B), C55(H55A,
 H55B), C57(H57A,H57B), C59(H59A,H59B), C88(H88A,H88B), C95(H95A,H95B),
 C97(H97A,H97B), C99(H99A,H99B), C106(H10A,H10B), C108(H10F,H10G), C110(H11A,
 H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19),
 C22(H22), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
  C35(H35), C36(H36), C39(H39), C42(H42), C50(H50), C53(H53), C61(H61),
 C64(H64), C67(H67), C68(H68), C70(H70), C71(H71), C72(H72), C73(H73), C75(H75),
  C76(H76), C78(H78), C79(H79), C81(H81), C82(H82), C83(H83), C84(H84),
 C86(H86), C87(H87), C91(H91), C94(H94), C102(H102), C105(H105)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C45(H45A,
 H45B,H45C), C47(H47A,H47B,H47C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C),
 C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), C107(H10C,H10D,H10E), C109(H10H,H10I,
 H10J), C111(H11C,H11D,H11E)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 386 electrons were 
found in a volume of 1550\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
4[C3H7NO], 3[H2O] per formula unit 
which account for 380 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63391
_shelx_hkl_checksum              57904
_shelx_fab_checksum              67540
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU