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_1572090
_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
'C85 H72 Co N5 O10, C3 H7 N O, 1(N1 O3), 4[C3H7NO], 1[H2O]'
_chemical_formula_sum            'C100 H109 Co N11 O19'
_chemical_formula_weight         1827.91
_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                112.3290(10)
_cell_angle_beta                 103.5880(10)
_cell_angle_gamma                92.9400(10)
_cell_formula_units_Z            2
_cell_length_a                   13.9766(5)
_cell_length_b                   18.8234(8)
_cell_length_c                   24.3526(9)
_cell_measurement_reflns_used    8287
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.36
_cell_volume                     5689.8(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44378
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.379
_diffrn_reflns_theta_min         1.772
_diffrn_source                   TXS
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_type              'Rotaing Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6690
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0897 before and 0.0610 after correction.
The Ratio of minimum to maximum transmission is 0.8977.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       block
_exptl_crystal_F_000             1930
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1134
_refine_ls_number_reflns         20744
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1353
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1359P)^2^+1.7927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2301
_refine_ls_wR_factor_ref         0.2653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11900
_reflns_number_total             20744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           230106_wqangz_038351_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               1572090
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.973
_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
 N6-O13 = N6-O14
 1.25 with sigma of 0.02
 N6-O12
 1.24 with sigma of 0.02
 N6A-O13A = N6A-O12A
 1.25 with sigma of 0.02
 N6A-O14A
 1.24 with sigma of 0.02
 O9A-C59A \\sim O9-C59 \\sim O10A-C60A \\sim O10-C60
 with sigma of 0.02
 O13A-O14A \\sim O14A-O12A \\sim O12A-O13A
 with sigma of 0.04
 N6-O13 \\sim N6-O12 \\sim N6-O14
 with sigma of 0.02
 O13-O12 \\sim O12-O14 \\sim O14-O13
 with sigma of 0.04
 N6A-O13A \\sim N6A-O14A \\sim N6A-O12A
 with sigma of 0.02
 O3A-N5 \\sim O3B-N5
 with sigma of 0.02
3. Restrained planarity
 O12A, O13A, O14A, N6A
 with sigma of 0.1
 O12, O13, O14, N6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O9 \\sim O9A \\sim O10 \\sim O10A \\sim C59 \\sim C59A \\sim C60 \\sim C60A:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
O12A \\sim O13A \\sim N6A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O12 \\sim O13 \\sim O14 \\sim N6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O12 \\sim O13 \\sim O14 \\sim N6 \\sim O14A \\sim O12A \\sim O13A \\sim N6A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C45 \\sim C45A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O12A \\sim O14A \\sim N6A \\sim O13A \\sim N6B \\sim O13B \\sim O14B \\sim
O12B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
O3A \\sim O3B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O13A) \\sim Ueq, Uanis(N6A) \\sim Ueq, Uanis(O14A) \\sim Ueq, Uanis(O12A)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 O12, O13, O14, N6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12A, O13A, N6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O13B, O14B, O12B, N6B} sigma for 1-2: 0.02, 1-3: 0.02
as in
{O14A, O12A, O13A, N6A}
7. Others
 1*[Sof(O12)+Sof(O13)+Sof(O14)+Sof(N6)]+1*[Sof(O14A)+Sof(O12A)+Sof(O13A)+
 Sof(N6A)]+1*[Sof(O13B)+Sof(O14B)+Sof(O12B)+Sof(N6B)]=1 with esd of 0
 Sof(O9)=Sof(O10)=Sof(H54)=Sof(H57)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=1-FVAR(1)
 Sof(O9A)=Sof(O10A)=Sof(H55)=Sof(H58)=Sof(C59A)=Sof(H59D)=Sof(H59E)=Sof(H59F)=
 Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=FVAR(1)
 Sof(O12)=Sof(O13)=Sof(O14)=Sof(N6)=FVAR(2)
 Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(3)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(3)
 Sof(O14A)=Sof(O12A)=Sof(O13A)=Sof(N6A)=FVAR(4)
 Sof(O13B)=Sof(O14B)=Sof(O12B)=Sof(N6B)=FVAR(5)
 Sof(O3B)=1-FVAR(6)
 Sof(O3A)=FVAR(6)
8.a Riding coordinates:
 C59(H59A,H59B,H59C)
8.b Rotating group:
 O4(H4A,H4B)
8.c Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C38(H38A,H38B), C47(H47A,H47B), C52(H52A,H52B), C61(H61A,H61B)
8.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14),
 C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C31(H31), C34(H34), C40(H40), C43(H43), C49(H49), C54(H54),
 C55(H55), C57(H57), C58(H58), C62(H62), C65(H65), C66(H66), C68(H68), C69(H69),
  C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77), C79(H79),
 C80(H80), C82(H82), C83(H83), C84(H84), C85(H85), C88(H88)
8.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C45A(H45D,H45E,
 H45F), C46(H46A,H46B,H46C), C59A(H59D,H59E,H59F), C60(H60A,H60B,H60C),
 C60A(H60D,H60E,H60F), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 348 electrons were 
found in a volume of 2244\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
4[C3H7NO], 1[H2O] per formula unit 
which account for 340 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32810
_shelx_hkl_checksum              15127
_shelx_fab_checksum              76943
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU