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_1572091
_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
'C67.764 H64.146 Co N2 O10.764, C3 H7 N O, 0.618(C2 H3 O2), 3[C3H7NO], 4[H2O]'
_chemical_formula_sum            'C81 H102 Co N6 O20'
_chemical_formula_weight         1538.61
_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             2024-06-18
_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                94.792(2)
_cell_angle_beta                 106.615(3)
_cell_angle_gamma                92.619(3)
_cell_formula_units_Z            2
_cell_length_a                   13.9662(6)
_cell_length_b                   14.9970(6)
_cell_length_c                   20.3479(8)
_cell_measurement_reflns_used    5890
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      54.34
_cell_measurement_theta_min      2.58
_cell_volume                     4058.9(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0806
_diffrn_reflns_av_unetI/netI     0.1150
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43239
_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         53.905
_diffrn_reflns_theta_min         2.880
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19931339999999997
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0979 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.8546.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             1634
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00118(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         14819
_refine_ls_number_restraints     2324
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.2276
_refine_ls_R_factor_gt           0.1242
_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^)+(0.0800P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2793
_refine_ls_wR_factor_ref         0.3242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5389
_reflns_number_total             14819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           221005_wqangz_209277_l_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_database_code               1572091
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.825
_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
 O10-C91 = O11-C91
 1.25 with sigma of 0.005
 C92-C91
 1.53 with sigma of 0.005
 C96-C95
 1.53 with sigma of 0.005
 O15-C95 = O14-C95
 1.25 with sigma of 0.005
 C97-C98
 1.53 with sigma of 0.005
 C94-C93
 1.53 with sigma of 0.005
 O12-C93 = O13-C93
 1.25 with sigma of 0.005
 O17-C97 = O16-C97
 1.25 with sigma of 0.005
 O15-O14
 2.2 with sigma of 0.005
 O12-O13
 2.2 with sigma of 0.005
 O11-O10
 2.2 with sigma of 0.005
 O17-O16
 2.2 with sigma of 0.005
 C78-C2 \\sim C11-C2
 with sigma of 0.02
 O14-C96 \\sim O15-C96
 with sigma of 0.02
 C75-C70 \\sim C58-C14
 with sigma of 0.02
 O17-C98 \\sim O16-C98
 with sigma of 0.02
 C85-C7 \\sim C45-C7
 with sigma of 0.02
 O12-C94 \\sim O13-C94
 with sigma of 0.02
 C87-C82 \\sim C64-C48
 with sigma of 0.02
 O11-C92 \\sim O10-C92
 with sigma of 0.02
3. Restrained planarity
 O14, C95, O15, C96
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim
O8 \\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim
O16 \\sim O17 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O14 \\sim O15 \\sim C95 \\sim C96 \\sim C97 \\sim O16 \\sim C98 \\sim O17 \\sim
O12 \\sim C93 \\sim O13 \\sim C94 \\sim C91 \\sim O10 \\sim O11 \\sim C92:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
Co2 \\sim Co1: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C53 \\sim N1 \\sim C42 \\sim C56 \\sim O9: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
Uanis(C91) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C92)
\\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq,
Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(O16)
\\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O12) \\sim Ueq,
Uanis(C93) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O12) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Co1) \\sim Ueq, Uanis(Co2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. 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
6. Others
 Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(H13)=Sof(C14)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(C59)=Sof(H59)=Sof(C60)=
 Sof(H60)=Sof(N2)=Sof(C61)=Sof(H61)=1-FVAR(1)
 Sof(C69)=Sof(H69)=Sof(C70)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72)=Sof(N4)=
 Sof(C73)=Sof(H73)=Sof(C74)=Sof(H74)=Sof(C75)=Sof(C76)=Sof(H76)=Sof(C77)=
 Sof(H77)=Sof(C78)=Sof(C79)=Sof(H79)=FVAR(1)
 Sof(Co1)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=
 Sof(C48)=Sof(C49)=Sof(H49)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(C65)=Sof(H65)=
 Sof(C66)=Sof(H66)=Sof(N3)=Sof(C67)=Sof(H67)=Sof(C91)=Sof(O10)=Sof(O11)=
 Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(H92C)=Sof(O14)=Sof(O15)=Sof(C95)=Sof(C96)=
 Sof(H96A)=Sof(H96B)=Sof(H96C)=1-FVAR(2)
 Sof(C80)=Sof(H80)=Sof(C81)=Sof(H81)=Sof(C82)=Sof(C83)=Sof(H83)=Sof(C84)=
 Sof(H84)=Sof(C85)=Sof(C86)=Sof(H86)=Sof(C87)=Sof(C88)=Sof(H88)=Sof(C89)=
 Sof(H89)=Sof(N5)=Sof(C90)=Sof(H90)=Sof(Co2)=Sof(O12)=Sof(C93)=Sof(O13)=
 Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=Sof(C97)=Sof(O16)=Sof(C98)=Sof(H98A)=
 Sof(H98B)=Sof(H98C)=Sof(O17)=FVAR(2)
 Fixed X: O14(0.81609)
 Fixed Y: C91(0.873429)
7.a Riding coordinates:
 C68(H68A,H68B,H68C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C98(H98A,H98B,
 H98C)
7.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C37(H37A,H37B), C43(H43A,H43B), C50(H50A,H50B)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C9(H9), C10(H10), C12(H12), C13(H13), C20(H20), C22(H22),
 C23(H23), C26(H26), C33(H33), C35(H35), C39(H39), C42(H42), C44(H44), C46(H46),
  C47(H47), C49(H49), C52(H52), C57(H57), C59(H59), C60(H60), C61(H61),
 C63(H63), C65(H65), C66(H66), C67(H67), C69(H69), C71(H71), C72(H72), C73(H73),
  C74(H74), C76(H76), C77(H77), C79(H79), C80(H80), C81(H81), C83(H83),
 C84(H84), C86(H86), C88(H88), C89(H89), C90(H90)
7.d Fitted hexagon refined as free rotating group:
 C9(C10,C11,C12,C13,C14), C44(C45,C46,C47,C48,C49), C57(C58,C59,C60,N2,C61),
 C63(C64,C65,C66,N3,C67), C69(C70,C71,C72,N4,C73), C74(C75,C76,C77,C78,C79),
 C80(C81,C82,C83,C84,C85), C86(C87,C88,C89,N5,C90)
7.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C51(H51A,H51B,
 H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C62(H62A,H62B,H62C), C92(H92A,H92B,H92C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 328 electrons were 
found in a volume of 1046\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[C3H7NO], 4[H2O] per formula unit 
which account for 320 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97909
_shelx_hkl_checksum              34885
_shelx_fab_checksum              52324
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU