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_1572095
_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         '4(I), C102 H104 Cu2 N4 O12, 4[C3H7NO], 2[H2O]'
_chemical_formula_sum            'C114 H136 Cu2 I4 N8 O18'
_chemical_formula_weight         2540.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           48
_space_group_name_Hall           '-P 2ab 2bc'
_space_group_name_H-M_alt        'P n n n :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            4
_cell_length_a                   13.7025(3)
_cell_length_b                   22.6702(5)
_cell_length_c                   41.6085(10)
_cell_measurement_reflns_used    6346
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      62.25
_cell_measurement_theta_min      3.40
_cell_volume                     12925.2(5)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1172
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            88773
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.544
_diffrn_reflns_theta_min         2.219
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms DIAMOND'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.385
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.2906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1442 before and 0.0777 after correction.
The Ratio of minimum to maximum transmission is 0.3859.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             5160
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         11909
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.1716
_refine_ls_R_factor_gt           0.1319
_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^)+(0.0700P)^2^+60.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3146
_refine_ls_wR_factor_ref         0.3384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7024
_reflns_number_total             11909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           cu_231121lu_lgpz184505_1_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_sg_symbol_H-M      'P n n n'
_cod_database_code               1572095
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.519
_shelx_estimated_absorpt_t_min   0.433
_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,H) groups
2. Restrained distances
 C2A-C3 = C1A-C2A = N1-C1A = N1-C5A = C4A-C5A = C4A-C3
 1.39 with sigma of 0.01
 Cu1-O6B \\sim Cu1-O6 \\sim Cu1-O6A \\sim Cu1-O5A \\sim Cu1-O5
 with sigma of 0.02
3. Restrained planarity
 N1, C1A, C2A, C3, C4A, C5A
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C1A \\sim C2 \\sim C2A \\sim C3 \\sim C4 \\sim C4A \\sim C5
\\sim C5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O5 \\sim O5A \\sim O6 \\sim O6A \\sim O6B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N2 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O6B) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(I1) \\sim Ueq, Uanis(I2) \\sim Ueq, Uanis(I3) \\sim Ueq, Uanis(I4) \\sim
Ueq, Uanis(I5) \\sim Ueq, Uanis(I6) \\sim Ueq, Uanis(I7) \\sim Ueq, Uanis(I8)
\\sim Ueq, Uanis(I9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 1*[Sof(O6)+Sof(H6A)+Sof(H6B)]+1*[Sof(O6B)+Sof(H6BA)+Sof(H6BB)]+1*[Sof(O6A)+
 Sof(H6AA)+Sof(H6AB)]=1 with esd of 0
 1*[Sof(I1)+Sof(O5)+Sof(H5A)+Sof(H5B)+Sof(O5A)+Sof(H5AA)+Sof(H5AB)]+1*
 [Sof(I7)]+1*[Sof(I6)]+1*[Sof(I5)]=1 with esd of 0
 1*[Sof(I8)]+1*[Sof(I4)]+1*[Sof(I2)]+1*[Sof(I3)]+1*[Sof(I9)]=1 with esd of 0
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AC)=1-
 FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=FVAR(1)
 Sof(O6)=Sof(H6A)=Sof(H6B)=FVAR(2)
 Sof(O6B)=Sof(H6BA)=Sof(H6BB)=FVAR(3)
 Sof(O6A)=Sof(H6AA)=Sof(H6AB)=FVAR(4)
 Sof(O5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(5)
 Sof(I1)=Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(5)
6.a Riding coordinates:
 O5(H5A,H5B), O5A(H5AA,H5AB), O6(H6A,H6B), O6A(H6AA,H6AB), O6B(H6BA,H6BB)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C36(H36A,
 H36B), C38(H38A,H38B), C40(H40A,H40B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C2(H2), C2A(H2A), C4(H4), C4A(H4A), C5(H5), C5A(H5AC),
 C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C16(H16), C20(H20), C23(H23),
 C32(H32), C35(H35), C42(H42), C43(H43), C45(H45), C46(H46), C50(H50), C51(H51),
  C47(H47), C48(H48)
6.d Fitted hexagon refined as free rotating group:
 C49(C50,C51,N2,C47,C48)
6.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 710 electrons were 
found in a volume of 2406\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[C3H7NO], 2[H2O] per formula unit 
which account for 720 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28425
_shelx_hkl_checksum              4869
_shelx_fab_checksum              68369
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU