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_1572100
_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 H108 Cu2 N4 O16, C3 H7 N O, 3[H2O], 3[C3H7NO], 3[H2O]'
_chemical_formula_sum            'C122 H148 Cu2 N8 O26'
_chemical_formula_weight         2269.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 91.860(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7491(7)
_cell_length_b                   41.664(2)
_cell_length_c                   22.7927(13)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      52.53
_cell_measurement_theta_min      3.24
_cell_volume                     13049.7(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE 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  0.0899
_diffrn_reflns_av_unetI/netI     0.1157
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            87570
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.907
_diffrn_reflns_theta_min         1.923
_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    2.117
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.5953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1414 before and 0.0919 after correction.
The Ratio of minimum to maximum transmission is 0.7918.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             4808
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1530
_refine_ls_number_reflns         23828
_refine_ls_number_restraints     1597
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1896
_refine_ls_R_factor_gt           0.1124
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2949
_refine_ls_wR_factor_ref         0.3365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10929
_reflns_number_total             23828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           230717lu_lgpz149553_4_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        13049.9(12)
_cod_database_code               1572100
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.756
_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
 C1F-C1B
 1.5 with sigma of 0.02
 C111-C112
 1.5 with sigma of 0.02
 O15-C113 = O16-C113
 1.3 with sigma of 0.01
 C114-C113
 1.5 with sigma of 0.02
 C109-O13
 1.25 with sigma of 0.02
 C1H-O24A
 1.25 with sigma of 0.02
 C115-O18 = C115-O17
 1.25 with sigma of 0.02
 C1H-C1D
 1.5 with sigma of 0.02
 C109-C110
 1.5 with sigma of 0.02
 C1G-O23A
 1.25 with sigma of 0.02
 C1G-C1C
 1.5 with sigma of 0.02
 N5-C106 = N5-C107 = N6-C104 = N6-C105
 1.5 with sigma of 0.01
 O1-C33 = N6-C103 = N5-C108
 1.45 with sigma of 0.01
 O9-C108 = O10-C103
 1.2 with sigma of 0.01
 C109-O14
 1.24 with sigma of 0.02
 C1G-O21A
 1.24 with sigma of 0.02
 C111-O11 = C111-O12
 1.25 with sigma of 0.02
 C1H-O25A
 1.24 with sigma of 0.02
 C1F-O19A = C1F-O18A
 1.25 with sigma of 0.02
 O17-C116
 2.5 with sigma of 0.02
 O21A-C1G = O23A-C1G = O12-C111 = O11-C111 = O24A-C1H = O25A-C1H = O17-C115 =
 O18-C115 = O18A-C1F = O19A-C1F
 1.25 with sigma of 0.01
 C106-C107
 2.5 with sigma of 0.01
 O23A-O21A = O11-O12 = O24A-O25A = O17-O18 = O18A-O19A
 2.2 with sigma of 0.01
 O19A-C1B \\sim C1B-O18A
 with sigma of 0.04
 O11-C112 \\sim C112-O12
 with sigma of 0.04
 C115-O18 \\sim C115-O17
 with sigma of 0.02
 Cu2-O16 \\sim Cu2-O15A
 with sigma of 0.02
 C113-O16 \\sim C1E-O15A
 with sigma of 0.02
 O15-O16 \\sim O11A-O15A
 with sigma of 0.04
 C1F-O19A \\sim C1F-O18A
 with sigma of 0.02
 O15-C114 \\sim O11A-C1A
 with sigma of 0.04
 O18-C116 \\sim C116-O17
 with sigma of 0.04
 C1H-O24A \\sim C1H-O25A
 with sigma of 0.02
 Cu2-O18 \\sim Cu2A-O18
 with sigma of 0.02
 O25A-C1D \\sim C1D-O24A
 with sigma of 0.04
 C111-O11 \\sim C111-O12
 with sigma of 0.02
 C109-O14 \\sim C109-O13
 with sigma of 0.02
 C110-O14 \\sim O13-C110
 with sigma of 0.04
 O21A-C1C \\sim C1C-O23A
 with sigma of 0.04
 C1G-O23A \\sim C1G-O21A
 with sigma of 0.02
 Cu1-O23A \\sim Cu1A-O23A
 with sigma of 0.02
 Cu2-N3 \\sim Cu2A-N3
 with sigma of 0.02
 Cu2-O15 \\sim Cu2A-O15
 with sigma of 0.02
 Cu2-C1F \\sim Cu2A-C1F
 with sigma of 0.02
 Cu2-O19A \\sim Cu2A-O19A
 with sigma of 0.02
 Cu2-O18A \\sim Cu2A-O18A
 with sigma of 0.02
 Cu2-O15 \\sim Cu2-O11A
 with sigma of 0.02
 O15-C113 \\sim O11A-C1E
 with sigma of 0.02
 O15-Cu2A \\sim O11A-Cu2A
 with sigma of 0.02
 Cu2-C113 \\sim Cu2-C1E
 with sigma of 0.04
 C113-Cu2A \\sim C1E-Cu2A
 with sigma of 0.04
 Cu1-N2 \\sim Cu1A-N2
 with sigma of 0.02
 Cu1-O14 \\sim Cu1A-O14
 with sigma of 0.02
 Cu1-O12 \\sim Cu1A-O12
 with sigma of 0.02
 Cu1-C111 \\sim Cu1A-C111
 with sigma of 0.02
 Cu1-O21A \\sim Cu1A-O21A
 with sigma of 0.02
 Cu1-O24A \\sim Cu1A-O24A
 with sigma of 0.02
 Cu1-C1G \\sim Cu1A-C1G
 with sigma of 0.02
 N2-C96 \\sim N2-C96A
 with sigma of 0.02
 N2-C101 \\sim N2-C117
 with sigma of 0.02
 C82-C95 \\sim C82-C95A
 with sigma of 0.02
 C82-C102 \\sim C82-C1I
 with sigma of 0.02
 C95-C96 \\sim C95A-C96A
 with sigma of 0.02
 C101-C102 \\sim C117-C1I
 with sigma of 0.02
 N2-C95 \\sim N2-C95A
 with sigma of 0.04
 N2-C102 \\sim N2-C1I
 with sigma of 0.04
 C82-C96 \\sim C82-C96A
 with sigma of 0.04
 C82-C101 \\sim C82-C117
 with sigma of 0.04
 N4-C99 \\sim N4-C99A
 with sigma of 0.02
 N4-C100 \\sim N4-C118
 with sigma of 0.02
 C76-C97 \\sim C76-C97A
 with sigma of 0.02
 C76-C98 \\sim C76-C98A
 with sigma of 0.02
 C97-C100 \\sim C97A-C118
 with sigma of 0.02
 C98-C99 \\sim C98A-C99A
 with sigma of 0.02
 N4-C97 \\sim N4-C97A
 with sigma of 0.04
 N4-C98 \\sim N4-C98A
 with sigma of 0.04
 C76-C99 \\sim C76-C99A
 with sigma of 0.04
 C76-C100 \\sim C76-C118
 with sigma of 0.04
3. Restrained planarity
 O18A, O19A, C1B, C1F
 with sigma of 0.1
 O11, O12, C111, C112
 with sigma of 0.1
 O15, O16, C113, C114
 with sigma of 0.1
 O17, O18, C115, C116
 with sigma of 0.1
 O24A, O25A, C1D, C1H
 with sigma of 0.1
 O13, O14, C109, C110
 with sigma of 0.1
 O21A, O23A, C1C, C1G
 with sigma of 0.1
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
O18A \\sim O19A \\sim C1B \\sim C1F: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O11 \\sim O12 \\sim C111 \\sim C112: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O17 \\sim O18 \\sim C115 \\sim C116: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O24A \\sim O25A \\sim C1D \\sim C1H: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O13 \\sim O14 \\sim C109 \\sim C110: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O21A \\sim O23A \\sim C1C \\sim C1G: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 O18A, O19A, C1B, C1F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11, O12, C111, C112
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, O18, C115, C116
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O24A, O25A, C1D, C1H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, O14, C109, C110
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21A, O23A, C1C, C1G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Cu1A)=Sof(Cu2A)=Sof(O11A)=Sof(O15A)=Sof(O18A)=Sof(O19A)=Sof(O21A)=
 Sof(O23A)=Sof(O24A)=Sof(O25A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1B)=
 Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C1D)=
 Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=Sof(C1E)=Sof(C1F)=Sof(C1G)=Sof(C1H)=Sof(C1I)=
 Sof(H1I)=Sof(C95A)=Sof(H95A)=Sof(C96A)=Sof(H96A)=Sof(C97A)=Sof(H97A)=Sof(C98A)=
 Sof(H98A)=Sof(C99A)=Sof(H99A)=Sof(C117)=Sof(H117)=Sof(C118)=Sof(H118)=1-FVAR(1)
 Sof(Cu1)=Sof(Cu2)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=
 Sof(O17)=Sof(O18)=Sof(C95)=Sof(H95)=Sof(C96)=Sof(H96)=Sof(C97)=Sof(H97)=
 Sof(C98)=Sof(H98)=Sof(C99)=Sof(H99)=Sof(C100)=Sof(H100)=Sof(C101)=Sof(H101)=
 Sof(C102)=Sof(H102)=Sof(C109)=Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C111)=Sof(C112)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C113)=Sof(C114)=
 Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C115)=Sof(C116)=Sof(H11J)=Sof(H11K)=
 Sof(H11L)=FVAR(1)
 Fixed Sof: O9(0.5) N5(0.5) C106(0.5) H10C(0.5) H10D(0.5) H10E(0.5) C107(0.5)
 H10F(0.5) H10G(0.5) H10H(0.5) C108(0.5) H108(0.5) O10(0.5) N6(0.5) C103(0.5)
 H103(0.5) C104(0.5) H10I(0.5) H10J(0.5) H10K(0.5) C105(0.5) H10L(0.5)
 H10M(0.5) H10N(0.5)
7.a Everything fixed:
 H11D, H11E, H11F
7.b Riding coordinates:
 C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,H1DC)
7.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C25(H25A,H25B), C36(H36A,H36B),
 C48(H48A,H48B), C59(H59A,H59B), C67(H67A,H67B), C69(H69A,H69B), C71(H71A,H71B),
  C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C77(H77A,H77B)
7.d Aromatic/amide H refined with riding coordinates:
 C1I(H1I), C5(H5), C7(H7), C8(H8), C21(H21), C23(H23), C29(H29), C30(H30),
 C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C47(H47), C49(H49),
  C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58),
 C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C68(H68), C79(H79), C85(H85),
  C86(H86), C87(H87), C88(H88), C90(H90), C91(H91), C94(H94), C95(H95),
 C95A(H95A), C96(H96), C96A(H96A), C97(H97), C97A(H97A), C98(H98), C98A(H98A),
 C99(H99), C99A(H99A), C100(H100), C101(H101), C102(H102), C117(H117),
 C118(H118), C108(H108), C103(H103)
7.e Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C89(H89A,H89B,H89C), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C110(H11A,H11B,H11C), C114(H11G,H11H,H11I),
 C116(H11J,H11K,H11L), C106(H10C,H10D,H10E), C107(H10F,H10G,H10H), C104(H10I,
 H10J,H10K), C105(H10L,H10M,H10N)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 724 electrons were 
found in a volume of 3382\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
3[H2O], 3[C3H7NO], 3[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              87857
_shelx_hkl_checksum              11640
_shelx_fab_checksum              82877
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU