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_1572088
_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, H2 O'
_chemical_formula_sum            'C76 H81 Cu2 N3 O18'
_chemical_formula_weight         1451.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                97.3870(10)
_cell_angle_beta                 103.4240(10)
_cell_angle_gamma                98.4550(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3580(3)
_cell_length_b                   16.3529(4)
_cell_length_c                   17.9257(4)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      57.119
_cell_measurement_theta_min      3.254
_cell_volume                     3435.12(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54142
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.436
_diffrn_reflns_theta_min         1.277
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0726 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.7768.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.017
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         14051
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0918P)^2^+11.3221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10367
_reflns_number_total             14051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 1572083--1572100.cif.'
_cod_database_code               1572088
_shelx_shelxl_version_number     2018/3
_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, All O(H,H) groups
2. Shared sites
{C64, C64'}
{C63, C63'}
3. Restrained distances
 O17-C63'
 1.22 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C64 \\sim C62 \\sim C63 \\sim C64' \\sim C63' \\sim O16 \\sim O17:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C64) = Uanis(C64')
Uanis(C63) = Uanis(C63')
5. Others
 Sof(O17)=Sof(C64')=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C63')=Sof(H63')=1-FVAR(1)
 Sof(O16)=Sof(C64)=Sof(H64)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(1)
6.a Everything fixed:
 H64A, H64B, H64C, O18, H18A, H18B
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C61(H61A,H61B), C55(H55A,H55B), C46(H46A,H46B), C73(H73A,H73B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C17(H17), C59(H59), C53(H53), C9(H9), C10(H10), C42(H42), C16(H16),
 C39(H39), C57(H57), C15(H15), C21(H21), C66(H66), C18(H18), C29(H29), C27(H27),
  C30(H30), C24(H24), C13(H13), C28(H28), C34(H34), C50(H50), C33(H33),
 C35(H35), C36(H36), C70(H70), C64(H64), C63'(H63')
6.d Idealised Me refined as rotating group:
 C025(H02A,H02B,H02C), C6(H6A,H6B,H6C), C44(H44A,H44B,H44C), C49(H49A,H49B,
 H49C), C67(H67A,H67B,H67C), C3(H3A,H3B,H3C), C60(H60A,H60B,H60C), C68(H68A,
 H68B,H68C), C8(H8A,H8B,H8C), C45(H45A,H45B,H45C), C54(H54A,H54B,H54C),
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              1555
_shelx_hkl_checksum              34620
_olex2_submission_special_instructions 'No special instructions were received'