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_1572086
_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
'C146 H144 Cu4 N4 O32, C3 H7 N O, 2(H2 O), 5[C3H7NO], 6[H2O]'
_chemical_formula_sum            'C164 H202 Cu4 N10 O46'
_chemical_formula_weight         3303.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_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                 96.044(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1284(9)
_cell_length_b                   21.1102(19)
_cell_length_c                   35.055(3)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      50.14
_cell_measurement_theta_min      2.86
_cell_volume                     8925.3(13)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.1-1 (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 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  0.0530
_diffrn_reflns_av_unetI/netI     0.1150
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            54062
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.906
_diffrn_reflns_theta_min         2.129
_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    2.951
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0962 before and 0.0727 after correction.
The Ratio of minimum to maximum transmission is 0.8026.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.382(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1720
_refine_ls_number_reflns         29261
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0915P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1979
_reflns_Friedel_coverage         0.744
_reflns_Friedel_fraction_full    0.788
_reflns_Friedel_fraction_max     0.786
_reflns_number_gt                14552
_reflns_number_total             29261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           221226lu_lgpz235213_yb_3_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        8925.4(13)
_cod_database_code               1572086
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.700
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.61814
 0.38186
2. Restrained distances
 O11-C43
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C11 \\sim N1 \\sim C10 \\sim C13 \\sim C9 \\sim C12: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
N4 \\sim C145 \\sim C144 \\sim C142 \\sim C143 \\sim C141: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C148 \\sim N5 \\sim C146 \\sim C147 \\sim O34: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O9 \\sim C34: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4.a Riding coordinates:
 O33(H33D,H33E)
4.b Free rotating group:
 O35(H35C,H35D)
4.c Secondary CH2 refined with riding coordinates:
 C98(H98A,H98B), C107(H10A,H10B), C134(H13A,H13B), C125(H12A,H12B), C26(H26A,
 H26B), C61(H61A,H61B), C53(H53A,H53B), C116(H11A,H11B), C44(H44A,H44B),
 C35(H35A,H35B)
4.d Aromatic/amide H refined with riding coordinates:
 C56(H56), C94(H94), C81(H81), C82(H82), C84(H84), C85(H85), C128(H128),
 C104(H104), C139(H139), C110(H110), C97(H97), C88(H88), C90(H90), C71(H71),
 C72(H72), C69(H69), C70(H70), C113(H113), C101(H101), C22(H22), C15(H15),
 C91(H91), C29(H29), C87(H87), C16(H16), C63(H63), C10(H10), C9(H9), C13(H13),
 C12(H12), C136(H136), C32(H32), C140(H140), C64(H64), C59(H59), C122(H122),
 C67(H67), C143(H143), C142(H142), C145(H145), C144(H144), C50(H50), C18(H18),
 C19(H19), C137(H137), C119(H119), C66(H66), C131(H131), C47(H47), C38(H38),
 C41(H41), C146(H146), C25(H25)
4.e Fitted hexagon refined as free rotating group:
 N3(C81,C82,C83,C84,C85), N2(C71,C72,C68,C69,C70), C11(C10,C9,N1,C13,C12),
 N4(C143,C142,C141,C145,C144)
4.f Idealised Me refined as rotating group:
 C106(H10C,H10D,H10E), C60(H60A,H60B,H60C), C133(H13C,H13D,H13E), C132(H13F,
 H13G,H13H), C105(H10F,H10G,H10H), C123(H12C,H12D,H12E), C114(H11C,H11D,H11E),
 C79(H79A,H79B,H79C), C75(H75A,H75B,H75C), C124(H12F,H12G,H12H), C115(H11F,H11G,
 H11H), C51(H51A,H51B,H51C), C149(H14A,H14B,H14C), C34(H34A,H34B,H34C),
 C52(H52A,H52B,H52C), C73(H73A,H73B,H73C), C33(H33A,H33B,H33C), C148(H14D,H14E,
 H14F), C7(H7A,H7B,H7C), C147(H14G,H14H,H14I), C42(H42A,H42B,H42C), C1(H1A,H1B,
 H1C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C43(H43A,H43B,H43C), C77(H77A,H77B,
 H77C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 537 electrons were 
found in a volume of 3156\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5[C3H7NO], 6[H2O] per Asymmetric Unit 
which account for 520 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20086
_shelx_hkl_checksum              59064
_shelx_fab_checksum              10712
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU