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_1572099
_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
'C110 H112 Cu2 N4 O18, 4.25(H2 O), 6[H2O], 3[H2O]'
_chemical_formula_sum            'C110 H138.5 Cu2 N4 O31.25'
_chemical_formula_weight         2143.82
_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                   13.8537(8)
_cell_length_b                   22.6927(15)
_cell_length_c                   41.561(3)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      43.21
_cell_measurement_theta_min      2.93
_cell_volume                     13065.9(15)
_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 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  0.0836
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            96701
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.898
_diffrn_reflns_theta_min         2.925
_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    2.111
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1391 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.7583.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       block
_exptl_crystal_F_000             4538
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         11951
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.2090
_refine_ls_R_factor_gt           0.1380
_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^)+(0.0700P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3019
_refine_ls_wR_factor_ref         0.3428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6242
_reflns_number_total             11951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           230917lu_lgpz145541_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        13066.0(14)
_cod_original_sg_symbol_H-M      'P n n n'
_cod_original_formula_sum        'C110 H138.50 Cu2 N4 O31.25'
_cod_database_code               1572099
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.742
_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
 O7-C55 = O8-C55
 1.25 with sigma of 0.005
 O5-C53 = O6-C53
 1.25 with sigma of 0.01
 C52-C53
 1.5 with sigma of 0.01
 C54-C55
 1.5 with sigma of 0.01
 O6-C53 = O6A-C53A = O5A-C53A = O5-C53
 1.25 with sigma of 0.01
 C53A-C52A = C53-C52
 1.5 with sigma of 0.01
 O5-O6
 2.2 with sigma of 0.01
 O7-O8
 2.2 with sigma of 0.01
 O6A-O5A = O5-O6
 2.2 with sigma of 0.01
 Cu1-O6 \\sim Cu1-O5
 with sigma of 0.002
 O8-C54 \\sim O7-C54
 with sigma of 0.02
 Cu1-O6 \\sim Cu1-O5 \\sim Cu1-O6A \\sim Cu1-O5A
 with sigma of 0.02
 Cu1-O9A \\sim Cu1-O9B
 with sigma of 0.02
 O6A-C52A \\sim O5A-C52A
 with sigma of 0.02
 Cu1-H9AA \\sim Cu1-H9AB
 with sigma of 0.02
 Cu1-H9BA \\sim Cu1-H9BB
 with sigma of 0.02
 O6-C52 \\sim O5-C52
 with sigma of 0.02
3. Restrained planarity
 O5, O6, C52, C53
 with sigma of 0.1
 O7, O8, C54, C55
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O5 \\sim O6 \\sim C52 \\sim C53: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
O8 \\sim C55 \\sim O7 \\sim C54: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
O6 \\sim O5 \\sim C52 \\sim C53 \\sim Cu1 \\sim O7 \\sim O8 \\sim C55 \\sim C54
\\sim O9B: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
within 2A
O9A \\sim O9B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O5 \\sim O6 \\sim C52 \\sim C53 \\sim O6A \\sim C52A \\sim C53A \\sim O5A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O16) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O9B)=Sof(H9BA)=Sof(H9BB)=1-FVAR(1)
 Sof(O9A)=Sof(H9AA)=Sof(H9AB)=FVAR(1)
 Sof(O6A)=Sof(C52A)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C53A)=Sof(O5A)=1-FVAR(2)
 Sof(O5)=Sof(O6)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=FVAR(2)
 Fixed Sof: O10(0.25) H10A(0.25) H10B(0.25) O11(0.25) H11A(0.25) H11B(0.25)
 O14(0.5) H14A(0.5) H14B(0.5) O15(0.25) H15A(0.25) H15B(0.25) O16(0.125)
 H16A(0.125) H16B(0.125) O17(0.25) H17A(0.25) H17B(0.25) O18(0.25) H18C(0.25)
 H18D(0.25) O12(0.25) H12A(0.25) H12B(0.25)
6.a Riding coordinates:
 O9B(H9BA,H9BB), C52(H52A,H52B,H52C), O10(H10A,H10B), O11(H11A,H11B), O14(H14A,
 H14B), O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O18(H18C,H18D),
 O12(H12A,H12B)
6.b Free rotating group:
 O9A(H9AA,H9AB)
6.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C34(H34A,
 H34B), C37(H37A,H37B), C39(H39A,H39B)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14),
 C17(H17), C21(H21), C24(H24), C31(H31), C35(H35), C42(H42), C43(H43), C45(H45),
  C46(H46), C47(H47), C48(H48), C50(H50), C51(H51)
6.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C54(H54A,H54B,H54C), C52A(H52D,H52E,H52F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 362 electrons were 
found in a volume of 2594\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
6[H2O], 3[H2O] per formula unit 
which account for 360 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36814
_shelx_hkl_checksum              72190
_shelx_fab_checksum              67979
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU