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_1572098
_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
'C68.192 H64.788 Cl0.404 Cu N2 O11.192, 2.5(C3 H7 N O)'
_chemical_formula_sum            'C75.69 H82.28 Cl0.41 Cu I0 N4.5 O13.69'
_chemical_formula_weight         1351.96
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-06-20
_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                81.365(2)
_cell_angle_beta                 71.316(2)
_cell_angle_gamma                86.856(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2377(3)
_cell_length_b                   14.9966(3)
_cell_length_c                   20.4324(4)
_cell_measurement_reflns_used    30921
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      73.6390
_cell_measurement_theta_min      3.4730
_cell_volume                     3798.83(15)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            102440
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.766
_diffrn_reflns_theta_min         2.980
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.54877
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             1427
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         15301
_refine_ls_number_restraints     1234
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0779
_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^)+(0.1661P)^2^+2.5047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.2497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12653
_reflns_number_total             15301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           zlp-1
_cod_depositor_comments
'Adding full bibliography for 1572083--1572100.cif.'
_cod_original_cell_volume        3798.83(14)
_cod_original_formula_sum        'C75.69 H82.28 Cl0.41 Cu I0 N4.50 O13.69'
_cod_database_code               1572098
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H1 of C1, H1 of C1, H17 of C17, H7 of C7, H19 of C19,
  H25 of C25, H31 of C31, H26 of C26, H10 of C10, H34 of C34, H11 of C11, H14
  of C14, H8 of C8, H49 of C49, H1S of C1S, H40 of C40, H5 of C5, H61 of C61,
  H20 of C20, H58 of C58, H22 of C22, H4 of C4, H28 of C28, H43 of C43, H27 of
  C27, H52 of C52, H2S of C2S, H23 of C23, H1 of C1, H1 of C1, H1 of C1
 At 1.5 times of:
  All C(H,H,H) groups, H1 of C1
2. Restrained distances
 C1_3-C2_3
 C1_4-C2_4
 with sigma of 0.02
 C1_3-O1_3 \\sim C1_3-O2_3
 C1_4-O1_4 \\sim C1_4-O2_4
 with sigma of 0.02
 O1_3-O2_3
 O1_4-O2_4
 with sigma of 0.04
 O1_3-C2_3 \\sim C2_3-O2_3
 O1_4-C2_4 \\sim C2_4-O2_4
 with sigma of 0.04
 N1_1-C2_1 \\sim N1_1-C3_1
 N1_2-C2_2 \\sim N1_2-C3_2
 N1_5-C2_5 \\sim N1_5-C3_5
 N1_6-C2_6 \\sim N1_6-C3_6
 N1_7-C2_7 \\sim N1_7-C3_7
 N1_8-C2_8 \\sim N1_8-C3_8
 with sigma of 0.02
 N1_1-C1_1
 N1_2-C1_2
 N1_5-C1_5
 N1_6-C1_6
 N1_7-C1_7
 N1_8-C1_8
 with sigma of 0.02
 C1_1-O1_1
 C1_2-O1_2
 C1_5-O1_5
 C1_6-O1_6
 C1_7-O1_7
 C1_8-O1_8
 with sigma of 0.02
 C2_1-C3_1
 C2_2-C3_2
 C2_5-C3_5
 C2_6-C3_6
 C2_7-C3_7
 C2_8-C3_8
 with sigma of 0.04
 C1_1-C3_1
 C1_2-C3_2
 C1_5-C3_5
 C1_6-C3_6
 C1_7-C3_7
 C1_8-C3_8
 with sigma of 0.04
 C1_1-C2_1
 C1_2-C2_2
 C1_5-C2_5
 C1_6-C2_6
 C1_7-C2_7
 C1_8-C2_8
 with sigma of 0.04
3. Restrained planarity
 O1_3, O2_3, C1_3, C2_3
 O1_4, O2_4, C1_4, C2_4
 with sigma of 0.1
 C1_1, O1_1, N1_1, C2_1, C3_1
 C1_2, O1_2, N1_2, C2_2, C3_2
 C1_5, O1_5, N1_5, C2_5, C3_5
 C1_6, O1_6, N1_6, C2_6, C3_6
 C1_7, O1_7, N1_7, C2_7, C3_7
 C1_8, O1_8, N1_8, C2_8, C3_8
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 O1_3, O2_3, C1_3, C2_3
 O1_4, O2_4, C1_4, C2_4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_1, O1_1, N1_1, C2_1, C3_1
 C1_2, O1_2, N1_2, C2_2, C3_2
 C1_5, O1_5, N1_5, C2_5, C3_5
 C1_6, O1_6, N1_6, C2_6, C3_6
 C1_7, O1_7, N1_7, C2_7, C3_7
 C1_8, O1_8, N1_8, C2_8, C3_8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O1_4, O2_4, C1_4, C2_4}
as
{O1_3, O2_3, C1_3, C2_3} sigma for 1-2: 0.02 1-3: 0.04
{C1_2, O1_2, N1_2, C2_2, C3_2}
{C1_5, O1_5, N1_5, C2_5, C3_5}
{C1_6, O1_6, N1_6, C2_6, C3_6}
{C1_7, O1_7, N1_7, C2_7, C3_7}
{C1_8, O1_8, N1_8, C2_8, C3_8}
as
{C1_1, O1_1, N1_1, C2_1, C3_1} sigma for 1-2: 0.02 1-3: 0.04
7. Others
 Sof(C1)=Sof(H1)=Sof(O1)=Sof(N1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(O1)=Sof(N1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
 Sof(Cl1S)=1-FVAR(2)
 Sof(O1)=Sof(O2)=Sof(C1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(2)
 Sof(C1)=Sof(H1)=Sof(O1)=Sof(N1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=0.5*(1-FVAR(4))
 Sof(C1)=Sof(H1)=Sof(O1)=Sof(N1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=0.5*FVAR(4)
 Fixed Sof: C1(0.5) H1(0.5) O1(0.5) N1(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C1(0.5) H1(0.5) O1(0.5) N1(0.5) C2(0.5)
 H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
 Fixed Y: C2(0.22784)
 Fixed Z: C2(0.808041)
8.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C65(H65A,H65B), C38(H38A,H38B), C56(H56A,H56B), C47(H47A,H47B)
8.b Me refined with riding coordinates:
 C37(H37A,H37B,H37C), C55(H55A,H55B,H55C), C46(H46A,H46B,H46C), C64(H64A,H64B,
 H64C), C36(H36A,H36B,H36C), C63(H63A,H63B,H63C), C45(H45A,H45B,H45C), C54(H54A,
 H54B,H54C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C),
  C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2(H2A,
 H2B,H2C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C),
 C3(H3A,H3B,H3C)
8.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C7(H7), C8(H8), C14(H14), C19(H19), C34(H34), C25(H25), C11(H11),
 C31(H31), C26(H26), C10(H10), C20(H20), C61(H61), C4(H4), C2S(H2S), C58(H58),
 C5(H5), C52(H52), C40(H40), C1S(H1S), C43(H43), C23(H23), C27(H27), C22(H22),
 C49(H49), C28(H28), C1(H1), C1(H1), C1(H1), C1(H1), C1(H1), C1(H1)
;
_shelx_res_checksum              67157
_shelx_hkl_checksum              97949
_olex2_submission_special_instructions 'No special instructions were received'