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_1572085
_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         'C102 H96 N4 O8, 1.5[H2O]'
_chemical_formula_sum            'C102 H99 N4 O9.5'
_chemical_formula_weight         1532.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 95.279(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3276(9)
_cell_length_b                   32.363(2)
_cell_length_c                   25.149(2)
_cell_measurement_reflns_used    6045
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      2.16
_cell_volume                     8370.0(11)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX5 V2023.9-2 (Bruker, 2023)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.1325
_diffrn_reflns_av_unetI/netI     0.1314
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            64178
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.488
_diffrn_reflns_theta_min         1.744
_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    0.078
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1416 before and 0.0707 after correction.
The Ratio of minimum to maximum transmission is 0.8473.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         15486
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1995
_refine_ls_R_factor_gt           0.0982
_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^)+(0.0401P)^2^+10.5836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7663
_reflns_number_total             15486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           231205lu_lgpz292798_7_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        8370.0(12)
_cod_original_formula_sum        'C102 H99 N4 O9.50'
_cod_database_code               1572085
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.988
_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 C(H,H,H,H,H,H) groups
2. Restrained distances
 C26-C25A \\sim C26-C25
 with sigma of 0.02
 O7-C25 \\sim O7-C25A
 with sigma of 0.02
3. Others
 Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C25A)=Sof(H25A)=Sof(H25B)=1-FVAR(1)
 Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C25)=Sof(H25C)=Sof(H25D)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C58(H58A,H58B), C40(H40A,H40B), C69(H69A,H69B), C29(H29A,
 H29B), C47(H47A,H47B), C38(H38A,H38B), C65(H65A,H65B), C56(H56A,H56B),
 C67(H67A,H67B), C36(H36A,H36B), C27(H27A,H27B), C54(H54A,H54B), C25A(H25A,
 H25B), C25(H25C,H25D)
4.b Aromatic/amide H refined with riding coordinates:
 C60(H60), C13(H13), C24(H24), C32(H32), C7(H7), C2(H2), C63(H63), C21(H21),
 C42(H42), C49(H49), C71(H71), C8(H8), C35(H35), C1(H1), C85(H85), C4(H4),
 C52(H52), C11(H11), C72(H72), C86(H86), C10(H10), C16(H16), C45(H45), C97(H97),
  C83(H83), C96(H96), C93(H93), C82(H82), C5(H5), C88(H88), C90(H90), C94(H94),
 C74(H74), C77(H77), C91(H91), C79(H79), C87(H87), C99(H99), C75(H75), C80(H80),
  C101(H101), C98(H98), C102(H102), C76(H76)
4.c Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C39(H39A,H39B,H39C), C57(H57A,H57B,
 H57C), C37(H37A,H37B,H37C), C26(H26D,H26E,H26F), C26(H26A,H26B,H26C), C55(H55A,
 H55B,H55C), C28(H28A,H28B,H28C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 68 electrons were 
found in a volume of 624\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
1.5[H2O] per formula unit 
which account for 60 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              41314
_shelx_hkl_checksum              57909
_shelx_fab_checksum              14120
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU