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_1572096
_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
'C118 H120 Cu4 N4 O24, 2(C3 H7 N O), 6[H2O], 4[H2O]'
_chemical_formula_sum            'C124 H154 Cu4 N6 O36'
_chemical_formula_weight         2558.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 91.5770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.2976(8)
_cell_length_b                   30.0377(8)
_cell_length_c                   15.6700(4)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      79.11
_cell_measurement_theta_min      3.53
_cell_volume                     14255.4(6)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_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 III'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_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  0.0504
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            102073
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.725
_diffrn_reflns_theta_min         2.071
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_type              'Incoatec I\ms DIAMOND'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0885 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.8684.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       block
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         15264
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1010P)^2^+24.0805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.1893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12770
_reflns_number_total             15264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           cu_230701lu_lgpz299151_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_database_code               1572096
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.853
_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
2. Restrained distances
 C36A-C37A = C37-C36
 1.5 with sigma of 0.01
 C48-C47 = C47A-C48A
 1.5 with sigma of 0.01
 C35A-C34A = C35-C34
 1.5 with sigma of 0.01
 O9-C36 \\sim O9-C36A
 with sigma of 0.02
 O12-C47 \\sim O12-C47A
 with sigma of 0.02
 O10-C34 \\sim O0-C34A
 with sigma of 0.02
 O0-C29 \\sim O10-C29
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C61 \\sim N3 \\sim C62 \\sim C60 \\sim O13: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C36A \\sim C36 \\sim C37A \\sim C37: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O0 \\sim C34A \\sim C35A \\sim O10 \\sim C34 \\sim C35: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O0) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1)
 Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(2)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(2)
 Sof(O0)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 1-FVAR(3)
 Sof(O10)=Sof(C34)=Sof(H34C)=Sof(H34D)=Sof(C35)=Sof(H35D)=Sof(H35E)=Sof(H35F)=
 FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C38(H38A,H38B), C45(H45A,H45B), C33(H33A,H33B), C34A(H34A,
 H34B), C36(H36A,H36B), C47(H47A,H47B), C47A(H47C,H47D), C36A(H36C,H36D),
 C34(H34C,H34D)
5.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C9(H9), C10(H10), C22(H22), C18(H18), C19(H19), C58(H58), C59(H59),
 C16(H16), C40(H40), C15(H15), C57(H57), C56(H56), C51(H51), C28(H28), C12(H12),
  C43(H43), C50(H50), C13(H13), C31(H31), C53(H53), C54(H54), C62(H62)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C46(H46A,H46B,H46C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C),
 C2(H2A,H2B,H2C), C61(H61A,H61B,H61C), C60(H60A,H60B,H60C), C48(H48A,H48B,H48C),
  C48A(H48D,H48E,H48F), C37(H37A,H37B,H37C), C37A(H37D,H37E,H37F), C35A(H35A,
 H35B,H35C), C35(H35D,H35E,H35F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 374 electrons were 
found in a volume of 3766\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
6[H2O], 4[H2O] per formula unit 
which account for 400 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32285
_shelx_hkl_checksum              84083
_shelx_fab_checksum              53997
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU