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_1572087
_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
'C73 H72 Cu2 N2 O16, C3 H7 N O, 3[C3H7NO], 1[H2O]'
_chemical_formula_sum            'C85 H102 Cu2 N6 O21'
_chemical_formula_weight         1670.80
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-21
_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                 104.018(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0846(19)
_cell_length_b                   21.322(4)
_cell_length_c                   19.015(3)
_cell_measurement_reflns_used    9657
_cell_measurement_temperature    292.00
_cell_measurement_theta_max      21.11
_cell_measurement_theta_min      2.21
_cell_volume                     4753.6(14)
_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      292.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_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 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0911
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66475
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        21.967
_diffrn_reflns_theta_max         21.967
_diffrn_reflns_theta_min         1.982
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms DIAMOND'
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1195 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.8337.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1088
_refine_ls_number_reflns         11585
_refine_ls_number_restraints     1966
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0696
_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^)+(0.1260P)^2^+1.1636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2079
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                8054
_reflns_number_total             11585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           zlp-4
_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        4753.7(14)
_cod_database_code               1572087
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.936
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(3)
 0.48(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
 O17-C69 = O16-C69
 1.25 with sigma of 0.01
 C74-C69
 1.5 with sigma of 0.01
 O9-C9
 1.25 with sigma of 0.01
 N3-C9
 1.35 with sigma of 0.01
 C73A-C68
 1.5 with sigma of 0.01
 O17-O16
 2.2 with sigma of 0.01
 O9-N3
 2.3 with sigma of 0.01
 C24A-C21 \\sim C24-C21
 with sigma of 0.02
 O6-C54B \\sim O6-C54A
 with sigma of 0.02
 O8-C45A \\sim O8-C45B
 with sigma of 0.02
 Cu1-O17 \\sim Cu2B-O16
 with sigma of 0.02
 C6-C3 \\sim C6-C3A
 with sigma of 0.02
 O2-C35A \\sim O2-C35B
 with sigma of 0.02
4. Restrained planarity
 O15A, C70A, C71A, O14A
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Cu2B \\sim Cu2A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C54B \\sim C54A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C45A \\sim C45B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C24 \\sim C28 \\sim C27 \\sim N2 \\sim C26 \\sim C25 \\sim C24A \\sim C28A
\\sim C27A \\sim N2A \\sim C26A \\sim C25A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C3 \\sim C2 \\sim C1 \\sim N1 \\sim C5 \\sim C4 \\sim C2A \\sim C1A \\sim N1A
\\sim C5A \\sim C4A \\sim C3A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C35A \\sim C35B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C9 \\sim N3 \\sim C64 \\sim C65 \\sim O9: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C73A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
O13 \\sim C67 \\sim C72 \\sim O13A \\sim C67A \\sim C72A \\sim O12 \\sim O12A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O15 \\sim O14 \\sim C70 \\sim C71 \\sim O15A \\sim O14A \\sim C70A \\sim C71A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O16 \\sim O17 \\sim C69 \\sim C74: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O10 \\sim C68 \\sim C73A \\sim O10A \\sim C68A \\sim C73B \\sim O11 \\sim O11A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C35B) \\sim Ueq, Uanis(C35A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{O13, O12, C67, C72} sigma for 1-2: 0.02, 1-3: 0.02
{O16, O17, C69, C74} sigma for 1-2: 0.02, 1-3: 0.02
as in
{O13A, O12A, C67A, C72A}
{O15A, O14A, C70A, C71A} sigma for 1-2: 0.02, 1-3: 0.02
{O17, O16, C69, C74} sigma for 1-2: 0.02, 1-3: 0.02
as in
{O15, O14, C70, C71}
{O11A, O10A, C68A, C73B} sigma for 1-2: 0.02, 1-3: 0.02
{O12, O13, C67, C72} sigma for 1-2: 0.02, 1-3: 0.02
as in
{O11, O10, C68, C73A}
8. Others
 Sof(C24A)=Sof(C28A)=Sof(H28A)=Sof(C27A)=Sof(H27A)=Sof(N2A)=Sof(C26A)=
 Sof(H26A)=Sof(C25A)=Sof(H25A)=1-FVAR(1)
 Sof(C24)=Sof(C28)=Sof(H28)=Sof(C27)=Sof(H27)=Sof(N2)=Sof(C26)=Sof(H26)=
 Sof(C25)=Sof(H25)=FVAR(1)
 Sof(C2A)=Sof(H2A)=Sof(C1A)=Sof(H1A)=Sof(N1A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=
 Sof(H4A)=Sof(C3A)=1-FVAR(2)
 Sof(C3)=Sof(C2)=Sof(H2)=Sof(C1)=Sof(H1)=Sof(N1)=Sof(C5)=Sof(H5)=Sof(C4)=
 Sof(H4)=FVAR(2)
 Sof(C45B)=Sof(H45A)=Sof(H45B)=Sof(H45C)=1-FVAR(3)
 Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=FVAR(3)
 Sof(C54B)=Sof(H54A)=Sof(H54B)=Sof(H54C)=1-FVAR(4)
 Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=FVAR(4)
 Sof(C35B)=Sof(H35A)=Sof(H35B)=Sof(H35C)=1-FVAR(5)
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=FVAR(5)
 Sof(O15A)=Sof(O14A)=Sof(C70A)=Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=1-FVAR(6)
 Sof(O15)=Sof(O14)=Sof(C70)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=FVAR(6)
 Sof(O13A)=Sof(O12A)=Sof(C67A)=Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=1-FVAR(7)
 Sof(O12)=Sof(O13)=Sof(C67)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=FVAR(7)
 Sof(O11A)=Sof(O10A)=Sof(C68A)=Sof(C73B)=Sof(H73D)=Sof(H73E)=Sof(H73F)=1-FVAR(8)
 Sof(O11)=Sof(O10)=Sof(C68)=Sof(C73A)=Sof(H73A)=Sof(H73B)=Sof(H73C)=FVAR(8)
 Sof(Cu2B)=1-FVAR(9)
 Sof(Cu2A)=FVAR(9)
 Fixed Y: Cu2A(0.31845)
 Fixed Z: C45B(0.712629)
9.a Riding coordinates:
 C71(H71A,H71B,H71C), C54A(H54D,H54E,H54F), C71A(H71D,H71E,H71F)
9.b Secondary CH2 refined with riding coordinates:
 C76(H76A,H76B), C63(H63A,H63B), C55(H55A,H55B), C37(H37A,H37B), C46(H46A,H46B)
9.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C60(H60), C7(H7), C11(H11), C10(H10), C8(H8), C14(H14), C57(H57),
 C30(H30), C33(H33), C39(H39), C48(H48), C2(H2), C1(H1), C5(H5), C4(H4),
 C51(H51), C19(H19), C23(H23), C22(H22), C20(H20), C28(H28), C27(H27), C26(H26),
  C25(H25), C42(H42), C9(H9), C28A(H28A), C27A(H27A), C26A(H26A), C25A(H25A),
 C2A(H2A), C1A(H1A), C5A(H5A), C4A(H4A)
9.d Fitted hexagon refined as free rotating group:
 C7(C6,C11,C10,C75,C8), C3(C2,C1,N1,C5,C4), C19(C18,C23,C22,C21,C20), C24(C28,
 C27,N2,C26,C25), C24A(C28A,C27A,N2A,C26A,C25A), C2A(C1A,N1A,C5A,C4A,C3A)
9.e Idealised Me refined as rotating group:
 C73A(H73A,H73B,H73C), C53(H53A,H53B,H53C), C45B(H45A,H45B,H45C), C64(H64A,
 H64B,H64C), C62(H62A,H62B,H62C), C36(H36A,H36B,H36C), C66(H66A,H66B,H66C),
 C65(H65A,H65B,H65C), C35B(H35A,H35B,H35C), C44(H44A,H44B,H44C), C54B(H54A,H54B,
 H54C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C45A(H45D,H45E,H45F),
 C35A(H35D,H35E,H35F), C72A(H72D,H72E,H72F), C73B(H73D,H73E,H73F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 254 electrons were 
found in a volume of 1690\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[C3H7NO], 1[H2O] per formula unit 
which account for 260 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              33818
_shelx_hkl_checksum              68805
_shelx_fab_checksum              4276
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU