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_1572089
_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_absolute_configuration ad
_chemical_formula_moiety         'C106 H100 Cu2 N4 O16, 2[C3H7NO]'
_chemical_formula_sum            'C112 H114 Cu2 N6 O18'
_chemical_formula_weight         1959.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.721(5)
_cell_length_b                   21.191(5)
_cell_length_c                   13.551(3)
_cell_measurement_reflns_used    8991
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      20.09
_cell_measurement_theta_min      2.44
_cell_volume                     5663(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1624
_diffrn_reflns_av_unetI/netI     0.1199
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            65274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         1.922
_diffrn_source                   TXS
_diffrn_source_current           1.6
_diffrn_source_power             0.08
_diffrn_source_type              'Rotaing Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1731 before and 0.0967 after correction.
The Ratio of minimum to maximum transmission is 0.6099.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         10366
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.0901
_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^)+(0.1810P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2368
_refine_ls_wR_factor_ref         0.2844
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5555
_reflns_number_total             10366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           a
_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               1572089
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.941
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.83(4)
 0.17(4)
2. 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
3. Restrained distances
 C41-C40
 1.5 with sigma of 0.01
 C42-C35
 1.5 with sigma of 0.01
 O1A-C1A = O2A-C1A = O1-C1 = O2-C1 = O4A-C2A = O3A-C2A = O3-C2 = O4-C2
 1.25 with sigma of 0.01
 C40-C33 = O6-C41
 2.4 with sigma of 0.01
 O1A-O2A = O1-O2 = O4A-O3A = O3-O4
 2.2 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O5 \\sim C38 \\sim C39 \\sim C36: within 2A with sigma of 0.007 and sigma for
terminal atoms of 0.015 within 2A
C40 \\sim C41: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
O1 \\sim O2 \\sim C1 \\sim O1A \\sim O2A \\sim C1A \\sim Cu1: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C41 \\sim C40 \\sim O6: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O3A \\sim C2A \\sim O4A \\sim O3 \\sim C2 \\sim O4: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C26 \\sim O7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Same fragment restrains
{O3A, O4A, C2A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3, O4, C2}
{O1A, O2A, C1A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O1, O2, C1}
6. Others
 Sof(O3A)=Sof(O4A)=Sof(C2A)=Sof(H2A)=1-FVAR(1)
 Sof(O3)=Sof(O4)=Sof(C2)=Sof(H2)=FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(C1A)=Sof(H1A)=1-FVAR(2)
 Sof(O1)=Sof(O2)=Sof(C1)=Sof(H1)=FVAR(2)
7.a Riding coordinates:
 C41(H41A,H41B,H41C)
7.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C38(H38A,
 H38B), C40(H40A,H40B), C42(H42A,H42B)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C2(H2), C2A(H2A), C3(H3), C4(H4), C6(H6), C7(H7), C9(H9),
 C10(H10), C12(H12), C13(H13), C16(H16), C19(H19), C22(H22), C25(H25), C34(H34),
  C37(H37), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50),
 C52(H52), C53(H53)
7.d Fitted hexagon refined as free rotating group:
 C34(C33,C32,C37,C36,C35)
7.e Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 171 electrons were 
found in a volume of 1599\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C3H7NO] per formula unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              183
_shelx_hkl_checksum              49012
_shelx_fab_checksum              89497
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU