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_1572094
_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
'C108 H108 Cu2 N4 O18, 0.5(C6 H8 N2), 2[C3H7NO], 6[H2O], 4[H2O]'
_chemical_formula_sum            'C117 H146 Cu2 N7 O30'
_chemical_formula_weight         2257.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 92.088(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.8584(7)
_cell_length_b                   41.6812(12)
_cell_length_c                   13.7257(5)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      73.94
_cell_measurement_theta_min      3.72
_cell_volume                     13068.7(7)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (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 III'
_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 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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            66435
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         2.205
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_type              'Incoatec I\ms DIAMOND'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1185 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.8826.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       block
_exptl_crystal_F_000             4780
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00075(10)
_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   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         11944
_refine_ls_number_restraints     328
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0992
_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^)+(0.1200P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2673
_refine_ls_wR_factor_ref         0.2841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8638
_reflns_number_total             11944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           cu_230701lu_lgpz299151_2_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               1572094
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.875
_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. Restrained distances
 N3-C52 = N4-C57
 1.15 with sigma of 0.01
 C60-C59
 1.5 with sigma of 0.01
 O6-C58 = O7-C58
 1.25 with sigma of 0.01
 C56-C57 = C56-C55 = C54-C55 = C54-C53 = C52-C53
 1.5 with sigma of 0.01
 O9-C59 = O8-C59
 1.25 with sigma of 0.01
 O6-O7
 2.2 with sigma of 0.01
 C52-C54
 2.5 with sigma of 0.01
 N3-C53
 2.9 with sigma of 0.01
 C56-N4
 2.9 with sigma of 0.01
 C53-C55
 2.5 with sigma of 0.01
 C54-C56
 2.5 with sigma of 0.01
 C55-C57
 2.5 with sigma of 0.01
 O8-O9
 2.2 with sigma of 0.01
 C57-C55
 2.5 with sigma of 0.01
 O9-C60 \\sim O8-C60
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O6 \\sim O7 \\sim C58: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O7 \\sim C58 \\sim O7A \\sim C58A \\sim O6 \\sim O6A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C59 \\sim O9 \\sim O8 \\sim C60: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N3 \\sim C57 \\sim C56 \\sim N4 \\sim C55 \\sim C54 \\sim C53 \\sim C52: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Cu1A \\sim Cu1: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O8 \\sim C59 \\sim O9 \\sim C60 \\sim O8A \\sim C59A \\sim O9A \\sim C60A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C58) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(O9) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{O7A, C58A, O6A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{O7, C58, O6}
{O8A, C59A, O9A, C60A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{O8, C59, O9, C60}
5. Others
 Sof(Cu1A)=Sof(O10)=Sof(H10A)=Sof(H10B)=1-FVAR(1)
 Sof(Cu1)=Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(1)
 Sof(O7A)=Sof(C58A)=Sof(H58A)=Sof(O6A)=1-FVAR(2)
 Sof(O7)=Sof(C58)=Sof(H58)=Sof(O6)=FVAR(2)
 Sof(O8A)=Sof(C59A)=Sof(O9A)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(3)
 Sof(O8)=Sof(C59)=Sof(O9)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(3)
 Fixed Sof: C57(0.25) C52(0.25) C56(0.25) H56A(0.25) H56B(0.25) C53(0.25)
 H53A(0.25) H53B(0.25) C55(0.25) H55A(0.25) H55B(0.25) C54(0.25) H54A(0.25)
 H54B(0.25) N4(0.25) N3(0.25)
 Fixed Y: C52(0.82585) O6A(0.494769)
6.a Riding coordinates:
 O5(H5A,H5B), O10(H10A,H10B)
6.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C29(H29A,H29B), C40(H40A,H40B), C38(H38A,H38B), C49(H49A,
 H49B), C36(H36A,H36B), C47(H47A,H47B), C56(H56A,H56B), C53(H53A,H53B),
 C55(H55A,H55B), C54(H54A,H54B)
6.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C43(H43), C14(H14), C32(H32), C46(H46), C35(H35), C8(H8), C19(H19),
 C23(H23), C10(H10), C11(H11), C7(H7), C20(H20), C22(H22), C2(H2), C4(H4),
 C5(H5), C58(H58), C1(H1), C27(H27), C28(H28), C25(H25), C24(H24), C58A(H58A)
6.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C39(H39A,H39B,H39C), C60(H60A,H60B,H60C), C48(H48A,H48B,
 H48C), C37(H37A,H37B,H37C), C60A(H60D,H60E,H60F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 744 electrons were 
found in a volume of 3528\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
2[C3H7NO], 6[H2O], 4[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              68457
_shelx_hkl_checksum              66412
_shelx_fab_checksum              12994
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU