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_1572092
_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], 4[H2O]'
_chemical_formula_sum            'C112 H122 Cu2 N6 O22'
_chemical_formula_weight         2031.23
_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                   19.800(3)
_cell_length_b                   21.138(4)
_cell_length_c                   13.471(3)
_cell_measurement_reflns_used    8241
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      21.90
_cell_measurement_theta_min      2.27
_cell_volume                     5638.0(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1009
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_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            69588
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.184
_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    0.445
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6669
_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 0.0824 after correction.
The Ratio of minimum to maximum transmission is 0.8947.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10335
_refine_ls_number_restraints     553
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0874
_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^)+(0.1976P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2423
_refine_ls_wR_factor_ref         0.2795
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6710
_reflns_number_total             10335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           mo_231210lu_lgpz046188_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        5638.1(17)
_cod_database_code               1572092
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.940
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(3)
 0.11(3)
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
 O2A-C53A = O1A-C53A = O1-C53 = O2-C53 = O3-C52 = O4-C52 = O3A-C52A = O4A-C52A
 1.25 with sigma of 0.01
 O4A-O3A = O4-O3 = O1-O2 = O2A-O1A
 2.2 with sigma of 0.01
 O6-C39 \\sim O6-C36 \\sim O5-C32 \\sim O5-C37 \\sim O7-C27 \\sim O7-C20 \\sim
O8-C23 \\sim O8-C25
 with sigma of 0.02
 Cu1-O4A \\sim Cu1-O3A \\sim Cu1-O3
 with sigma of 0.02
4. 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
Cu1 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim C52 \\sim C53 \\sim O1A \\sim O2A
\\sim C53A \\sim O3A \\sim O4A \\sim C52A: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C25 \\sim C26: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.014 within 2A
5. Others
 Sof(O1A)=Sof(O2A)=Sof(C53A)=Sof(H53A)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(C53)=Sof(H53)=FVAR(1)
 Sof(O3A)=Sof(O4A)=Sof(C52A)=Sof(H52A)=1-FVAR(2)
 Sof(O3)=Sof(O4)=Sof(C52)=Sof(H52)=FVAR(2)
6.a Riding coordinates:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C)
6.b 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.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C16(H16), C21(H21), C24(H24), C31(H31), C35(H35), C42(H42), C43(H43), C45(H45),
  C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53),
 C53A(H53A), C52A(H52A)
6.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 231 electrons were 
found in a volume of 1598\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C3H7NO], 4[H2O] per Asymmetric Unit 
which account for 240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8994
_shelx_hkl_checksum              27915
_shelx_fab_checksum              72276
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU