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_1572097
_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_absolute_configuration ad
_chemical_formula_moiety
'C181 H161 Co4 N8 O26.5, C186 H163 Co4 N8 O28, C2 H3 O2, C H O2, 1[C3H7NO], 2[H2O], 5[C3H7NO], 1[C3H7NO], 2[H2O], 5[C3H7NO], 1[], 0.5[], 1[C3H7NO], 1[H2O], 1[], 0.5[]'
_chemical_formula_sum            'C409 H429 Co8 N29 O76.5'
_chemical_formula_weight         7446.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 90.150(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.5576(19)
_cell_length_b                   40.892(4)
_cell_length_c                   24.167(2)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      50.944
_cell_measurement_theta_min      2.608
_cell_volume                     18339(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  (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.1246
_diffrn_reflns_av_unetI/netI     0.2317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            84763
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        42.120
_diffrn_reflns_theta_max         42.120
_diffrn_reflns_theta_min         0.940
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19931339999999997
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.69
_exptl_absorpt_coefficient_mu    2.383
_exptl_absorpt_correction_T_max  0.7501
_exptl_absorpt_correction_T_min  0.5246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1101 before and 0.0727 after correction.
The Ratio of minimum to maximum transmission is 0.6994.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             7828
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3865
_refine_ls_number_reflns         35136
_refine_ls_number_restraints     7263
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.2205
_refine_ls_R_factor_gt           0.1129
_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^)+(0.0800P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2609
_refine_ls_wR_factor_ref         0.3069
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                18874
_reflns_number_total             35136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03022b2.cif
_cod_data_source_block           p21_sq_sq
_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_original_formula_sum        'C409 H429 Co8 N29 O76.50'
_cod_database_code               1572097
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.763
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.27(2)
 0.368(12) 0.094(12) 0.273(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H61 of C61, H58 of C58, H60 of C60, H69 of C69, H78 of
  C78, H81 of C81, H62 of C62, H55 of C55, H65 of C65, H51 of C51, H66 of C66,
  H57 of C57, H63 of C63, H72 of C72, H52 of C52, H54 of C54, H12 of C12, H13
  of C13, H14 of C14, H3 of C3, H6 of C6, H8 of C8, H9 of C9, H17 of C17, H11
  of C11, H19 of C19, H20 of C20, H16 of C16, H22 of C22, H23 of C23, H47 of
  C47, H27 of C27, H25 of C25, H24 of C24, H35 of C35, H40 of C40, H32 of C32,
  H46 of C46, H43 of C43, H50 of C50, H49 of C49, H28 of C28, H3 of C3, H17 of
  C17, H16 of C16, H20 of C20, H25 of C25, H27 of C27, H22 of C22, H28 of C28,
  H19 of C19, H8 of C8, H14 of C14, H12 of C12, H23 of C23, H13 of C13, H6 of
  C6, H9 of C9, H11 of C11, H24 of C24, H55 of C55, H57 of C57, H58 of C58, H60
  of C60, H46 of C46, H62 of C62, H63 of C63, H32 of C32, H61 of C61, H47 of
  C47, H49 of C49, H65 of C65, H43 of C43, H40 of C40, H52 of C52, H35 of C35,
  H50 of C50, H51 of C51, H54 of C54, H72 of C72, H3 of C3, H8 of C8, H9 of C9,
  H12 of C12, H13 of C13, H11 of C11, H6 of C6, H69 of C69, H66 of C66, H78 of
  C78, H81 of C81, H25 of C25, H20 of C20, H22 of C22, H28 of C28, H17 of C17,
  H32 of C32, H35 of C35, H19 of C19, H23 of C23, H27 of C27, H24 of C24, H16
  of C16, H14 of C14, H72 of C72, H58 of C58, H54 of C54, H62 of C62, H60 of
  C60, H46 of C46, H40 of C40, H52 of C52, H57 of C57, H61 of C61, H65 of C65,
  H66 of C66, H63 of C63, H47 of C47, H50 of C50, H49 of C49, H51 of C51, H69
  of C69, H55 of C55, H43 of C43, H24 of C24, H9 of C9, H13 of C13, H3 of C3,
  H14 of C14, H22 of C22, H8 of C8, H17 of C17, H12 of C12, H11 of C11, H81 of
  C81, H16 of C16, H19 of C19, H78 of C78, H6 of C6, H23 of C23, H20 of C20,
  H25 of C25, H43 of C43, H47 of C47, H28 of C28, H49 of C49, H32 of C32, H50
  of C50, H27 of C27, H35 of C35, H51 of C51, H46 of C46, H52 of C52, H54 of
  C54, H55 of C55, H40 of C40, H81 of C81, H60 of C60, H72 of C72, H66 of C66,
  H62 of C62, H61 of C61, H63 of C63, H65 of C65, H69 of C69, H57 of C57, H78
  of C78, {H2A,H2B,H2C} of C2, H1 of C1, {H2A,H2B,H2C} of C2, {H2A,H2B,H2C} of
  C2, All O(H,H) groups
 At 1.5 times of:
  {H74A,H74B,H74C} of C74, {H83A,H83B,H83C} of C83, {H75A,H75B,H75C} of C75,
  {H36A,H36B,H36C} of C36, {H37A,H37B,H37C} of C37, {H84A,H84B,H84C} of C84,
  {H36A,H36B,H36C} of C36, {H37A,H37B,H37C} of C37, {H75A,H75B,H75C} of C75,
  {H74A,H74B,H74C} of C74, {H84A,H84B,H84C} of C84, {H83A,H83B,H83C} of C83,
  {H37A,H37B,H37C} of C37, {H36A,H36B,H36C} of C36, {H74A,H74B,H74C} of C74,
  {H75A,H75B,H75C} of C75, {H84A,H84B,H84C} of C84, {H83A,H83B,H83C} of C83,
  {H37A,H37B,H37C} of C37, {H36A,H36B,H36C} of C36, {H84A,H84B,H84C} of C84,
  {H75A,H75B,H75C} of C75, {H83A,H83B,H83C} of C83, {H74A,H74B,H74C} of C74,
  {H2A,H2B,H2C} of C2, {H2A,H2B,H2C} of C2, {H2A,H2B,H2C} of C2, {H2A,H2B,H2C}
  of C2, {H2A,H2B,H2C} of C2, {H2A,H2B,H2C} of C2, {H2A,H2B,H2C} of C2, {H2A,
  H2B,H2C} of C2, {H2A,H2B,H2C} of C2, {H2A,H2B,H2C} of C2, {H2A,H2B,H2C} of C2,
   H1 of C1
3. Restrained distances
 C4_1-C7_1 = C1_1-C18_1 = C10_1-C15_1 = C21_1-C26_1
 C4_2-C7_2 = C1_2-C18_2 = C10_2-C15_2 = C21_2-C26_2
 C4_3-C7_3 = C1_3-C18_3 = C10_3-C15_3 = C21_3-C26_3
 C4_4-C7_4 = C1_4-C18_4 = C10_4-C15_4 = C21_4-C26_4
 1.54 with sigma of 0.01
 C80_1-C85_1 = C2_1-C85_1
 C80_2-C85_2 = C2_2-C85_2
 C80_3-C85_3 = C2_3-C85_3
 C80_4-C85_4 = C2_4-C85_4
 1.5 with sigma of 0.01
 C79_1-O6_1 = O6_1-C83_1 = C82_1-O5_1 = O5_1-C84_1 = C70_1-O4_1 = O4_1-C75_1 =
 C73_1-O3_1 = C74_1-O3_1
 C79_2-O6_2 = O6_2-C83_2 = C82_2-O5_2 = O5_2-C84_2 = C70_2-O4_2 = O4_2-C75_2 =
 C73_2-O3_2 = C74_2-O3_2
 C79_3-O6_3 = O6_3-C83_3 = C82_3-O5_3 = O5_3-C84_3 = C70_3-O4_3 = O4_3-C75_3 =
 C73_3-O3_3 = C74_3-O3_3
 C79_4-O6_4 = O6_4-C83_4 = C82_4-O5_4 = O5_4-C84_4 = C70_4-O4_4 = O4_4-C75_4 =
 C73_4-O3_4 = C74_4-O3_4
 1.43 with sigma of 0.01
 O2_1-C34_1 = O2_1-C37_1 = O1_1-C31_1 = O1_1-C36_1
 O2_2-C34_2 = O2_2-C37_2 = O1_2-C31_2 = O1_2-C36_2
 O2_3-C34_3 = O2_3-C37_3 = O1_3-C31_3 = O1_3-C36_3
 O2_4-C34_4 = O2_4-C37_4 = O1_4-C31_4 = O1_4-C36_4
 1.43 with sigma of 0.01
 H2B-H3B_$1
 2.1 with sigma of 0.01
 C1_5-C2_5
 C1_6-C2_6
 C1_7-C2_7
 C1_8-C2_8
 C1_9-C2_9
 C1_10-C2_10
 C1_12-C2_12
 C1_13-C2_13
 C1_14-C2_14
 C1_15-C2_15
 C1_18-C2_18
 C1_19-C2_19
 C1_20-C2_20
 C1_21-C2_21
 with sigma of 0.02
 C1_5-O1_5 \\sim C1_5-O2_5
 C1_6-O1_6 \\sim C1_6-O2_6
 C1_7-O1_7 \\sim C1_7-O2_7
 C1_8-O1_8 \\sim C1_8-O2_8
 C1_9-O1_9 \\sim C1_9-O2_9
 C1_10-O1_10 \\sim C1_10-O2_10
 C1_11-O1_11 \\sim C1_11-O2_11
 C1_12-O1_12 \\sim C1_12-O2_12
 C1_13-O1_13 \\sim C1_13-O2_13
 C1_14-O1_14 \\sim C1_14-O2_14
 C1_15-O1_15 \\sim C1_15-O2_15
 C1_18-O1_18 \\sim C1_18-O2_18
 C1_19-O1_19 \\sim C1_19-O2_19
 C1_20-O1_20 \\sim C1_20-O2_20
 C1_21-O1_21 \\sim C1_21-O2_21
 C1_22-O1_22 \\sim C1_22-O2_22
 with sigma of 0.02
 O1_5-O2_5
 O1_6-O2_6
 O1_7-O2_7
 O1_8-O2_8
 O1_9-O2_9
 O1_10-O2_10
 O1_11-O2_11
 O1_12-O2_12
 O1_13-O2_13
 O1_14-O2_14
 O1_15-O2_15
 O1_18-O2_18
 O1_19-O2_19
 O1_20-O2_20
 O1_21-O2_21
 O1_22-O2_22
 with sigma of 0.04
 O1_5-C2_5 \\sim C2_5-O2_5
 O1_6-C2_6 \\sim C2_6-O2_6
 O1_7-C2_7 \\sim C2_7-O2_7
 O1_8-C2_8 \\sim C2_8-O2_8
 O1_9-C2_9 \\sim C2_9-O2_9
 O1_10-C2_10 \\sim C2_10-O2_10
 O1_11-O2_11
 O1_12-C2_12 \\sim C2_12-O2_12
 O1_13-C2_13 \\sim C2_13-O2_13
 O1_14-C2_14 \\sim C2_14-O2_14
 O1_15-C2_15 \\sim C2_15-O2_15
 O1_18-C2_18 \\sim C2_18-O2_18
 O1_19-C2_19 \\sim C2_19-O2_19
 O1_20-C2_20 \\sim C2_20-O2_20
 O1_21-C2_21 \\sim C2_21-O2_21
 O1_22-O2_22
 with sigma of 0.04
 C21_1-C25_1 \\sim C21_1-C27_1 \\sim C26_1-C22_1 \\sim C26_1-C20_1
 C21_2-C25_2 \\sim C21_2-C27_2 \\sim C26_2-C22_2 \\sim C26_2-C20_2
 C21_3-C25_3 \\sim C21_3-C27_3 \\sim C26_3-C22_3 \\sim C26_3-C20_3
 C21_4-C25_4 \\sim C21_4-C27_4 \\sim C26_4-C22_4 \\sim C26_4-C20_4
 with sigma of 0.01
 C44_1-C61_1 \\sim C44_1-C57_1 \\sim C56_1-C39_1 \\sim C56_1-C43_1 \\sim
C59_1-C63_1 \\sim C59_1-
 C65_1 \\sim C64_1-C58_1 \\sim C64_1-C60_1
 C44_2-C61_2 \\sim C44_2-C57_2 \\sim C56_2-C39_2 \\sim C56_2-C43_2 \\sim
C59_2-C63_2 \\sim C59_2-
 C65_2 \\sim C64_2-C58_2 \\sim C64_2-C60_2
 C44_3-C61_3 \\sim C44_3-C57_3 \\sim C56_3-C39_3 \\sim C56_3-C43_3 \\sim
C59_3-C63_3 \\sim C59_3-
 C65_3 \\sim C64_3-C58_3 \\sim C64_3-C60_3
 C44_4-C61_4 \\sim C44_4-C57_4 \\sim C56_4-C39_4 \\sim C56_4-C43_4 \\sim
C59_4-C63_4 \\sim C59_4-
 C65_4 \\sim C64_4-C58_4 \\sim C64_4-C60_4
 with sigma of 0.01
 C41_1-C46_1 \\sim C41_1-C50_1 \\sim C45_1-C40_1 \\sim C45_1-C42_1
 C41_2-C46_2 \\sim C41_2-C50_2 \\sim C45_2-C40_2 \\sim C45_2-C42_2
 C41_3-C46_3 \\sim C41_3-C50_3 \\sim C45_3-C40_3 \\sim C45_3-C42_3
 C41_4-C46_4 \\sim C41_4-C50_4 \\sim C45_4-C40_4 \\sim C45_4-C42_4
 with sigma of 0.02
 O3_1-C72_1 \\sim O3_1-C68_1 \\sim O4_1-C71_1 \\sim O4_1-C69_1
 O3_2-C72_2 \\sim O3_2-C68_2 \\sim O4_2-C71_2 \\sim O4_2-C69_2
 O3_3-C72_3 \\sim O3_3-C68_3 \\sim O4_3-C71_3 \\sim O4_3-C69_3
 O3_4-C72_4 \\sim O3_4-C68_4 \\sim O4_4-C71_4 \\sim O4_4-C69_4
 with sigma of 0.01
 C82_1-C84_1 \\sim C79_1-C83_1
 C82_2-C84_2 \\sim C79_2-C83_2
 C82_3-C84_3 \\sim C79_3-C83_3
 C82_4-C84_4 \\sim C79_4-C83_4
 with sigma of 0.01
 C5_1-C29_1 \\sim C29_1-C30_1
 C5_2-C29_2 \\sim C29_2-C30_2
 C5_3-C29_3 \\sim C29_3-C30_3
 C5_4-C29_4 \\sim C29_4-C30_4
 with sigma of 0.01
 C29_1-C35_1 \\sim C29_1-C31_1
 C29_2-C35_2 \\sim C29_2-C31_2
 C29_3-C35_3 \\sim C29_3-C31_3
 C29_4-C35_4 \\sim C29_4-C31_4
 with sigma of 0.01
4. Restrained planarity
 O1_5, O2_5, C1_5, C2_5
 O1_6, O2_6, C1_6, C2_6
 O1_7, O2_7, C1_7, C2_7
 O1_8, O2_8, C1_8, C2_8
 O1_9, O2_9, C1_9, C2_9
 O1_10, O2_10, C1_10, C2_10
 O1_12, O2_12, C1_12, C2_12
 O1_13, O2_13, C1_13, C2_13
 O1_14, O2_14, C1_14, C2_14
 O1_15, O2_15, C1_15, C2_15
 O1_18, O2_18, C1_18, C2_18
 O1_19, O2_19, C1_19, C2_19
 O1_20, O2_20, C1_20, C2_20
 O1_21, O2_21, C1_21, C2_21
 with sigma of 0.1
 C48_1, C51_1, C52_1, C53_1, C54_1, C55_1, N3_1
 C48_2, C51_2, C52_2, C53_2, C54_2, C55_2, N3_2
 C48_3, C51_3, C52_3, C53_3, C54_3, C55_3, N3_3
 C48_4, C51_4, C52_4, C53_4, C54_4, C55_4, N3_4
 with sigma of 0.01
 C45_1, C46_1, C47_1, C48_1, C49_1, C50_1, C53_1
 C45_2, C46_2, C47_2, C48_2, C49_2, C50_2, C53_2
 C45_3, C46_3, C47_3, C48_3, C49_3, C50_3, C53_3
 C45_4, C46_4, C47_4, C48_4, C49_4, C50_4, C53_4
 with sigma of 0.01
5. 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
Uanis(C64_4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C4_3) \\sim Ueq, Uanis(C64_3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C54_2) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of
0.014
Uanis(C8_3) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(C47_3) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of
0.014
Uanis(C13_4) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of
0.014
Uanis(C58_4) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of
0.014
Uanis(C21_3) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of
0.014
6. Rigid body (RIGU) restrains
 O1_5, O2_5, C1_5, C2_5
 O1_6, O2_6, C1_6, C2_6
 O1_7, O2_7, C1_7, C2_7
 O1_8, O2_8, C1_8, C2_8
 O1_9, O2_9, C1_9, C2_9
 O1_10, O2_10, C1_10, C2_10
 O1_12, O2_12, C1_12, C2_12
 O1_13, O2_13, C1_13, C2_13
 O1_14, O2_14, C1_14, C2_14
 O1_15, O2_15, C1_15, C2_15
 O1_18, O2_18, C1_18, C2_18
 O1_19, O2_19, C1_19, C2_19
 O1_20, O2_20, C1_20, C2_20
 O1_21, O2_21, C1_21, C2_21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{O1_6, O2_6, C1_6, C2_6}
{O1_7, O2_7, C1_7, C2_7}
{O1_8, O2_8, C1_8, C2_8}
{O1_9, O2_9, C1_9, C2_9}
{O1_10, O2_10, C1_10, C2_10}
{O1_12, O2_12, C1_12, C2_12}
{O1_13, O2_13, C1_13, C2_13}
{O1_14, O2_14, C1_14, C2_14}
{O1_15, O2_15, C1_15, C2_15}
{O1_18, O2_18, C1_18, C2_18}
{O1_19, O2_19, C1_19, C2_19}
{O1_20, O2_20, C1_20, C2_20}
{O1_21, O2_21, C1_21, C2_21}
as
{O1_5, O2_5, C1_5, C2_5} sigma for 1-2: 0.02 1-3: 0.04
{C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, C9_2, C10_2, C11_2, C12_2,
C13_2, C14_2, C15_2, C16_2, C17_2, N1_2, C18_2, C19_2, C20_2, C21_2, C22_2,
C23_2, C24_2, C25_2, C26_2, C27_2, C28_2, N2_2, O1_2, O2_2, O3_2, O4_2, O5_2,
O6_2, C29_2, C30_2, C31_2, C32_2, C33_2, C34_2, C35_2, C36_2, C37_2, C38_2,
C39_2, C40_2, C41_2, C42_2, C43_2, C44_2, C45_2, C46_2, C47_2, C48_2, C49_2,
C50_2, C51_2, C52_2, C53_2, C54_2, C55_2, N3_2, C56_2, C57_2, C58_2, C59_2,
C60_2, C61_2, C62_2, C63_2, C64_2, C65_2, C66_2, N4_2, C67_2, C68_2, C69_2,
C70_2, C71_2, C72_2, C73_2, C74_2, C75_2, C76_2, C77_2, C78_2, C79_2, C80_2,
C81_2, C82_2, C83_2, C84_2, C85_2}
{C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3, C9_3, C10_3, C11_3, C12_3,
C13_3, C14_3, C15_3, C16_3, C17_3, N1_3, C18_3, C19_3, C20_3, C21_3, C22_3,
C23_3, C24_3, C25_3, C26_3, C27_3, C28_3, N2_3, O1_3, O2_3, O3_3, O4_3, O5_3,
O6_3, C29_3, C30_3, C31_3, C32_3, C33_3, C34_3, C35_3, C36_3, C37_3, C38_3,
C39_3, C40_3, C41_3, C42_3, C43_3, C44_3, C45_3, C46_3, C47_3, C48_3, C49_3,
C50_3, C51_3, C52_3, C53_3, C54_3, C55_3, N3_3, C56_3, C57_3, C58_3, C59_3,
C60_3, C61_3, C62_3, C63_3, C64_3, C65_3, C66_3, N4_3, C67_3, C68_3, C69_3,
C70_3, C71_3, C72_3, C73_3, C74_3, C75_3, C76_3, C77_3, C78_3, C79_3, C80_3,
C81_3, C82_3, C83_3, C84_3, C85_3}
{C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4, C8_4, C9_4, C10_4, C11_4, C12_4,
C13_4, C14_4, C15_4, C16_4, C17_4, N1_4, C18_4, C19_4, C20_4, C21_4, C22_4,
C23_4, C24_4, C25_4, C26_4, C27_4, C28_4, N2_4, O1_4, O2_4, O3_4, O4_4, O5_4,
O6_4, C29_4, C30_4, C31_4, C32_4, C33_4, C34_4, C35_4, C36_4, C37_4, C38_4,
C39_4, C40_4, C41_4, C42_4, C43_4, C44_4, C45_4, C46_4, C47_4, C48_4, C49_4,
C50_4, C51_4, C52_4, C53_4, C54_4, C55_4, N3_4, C56_4, C57_4, C58_4, C59_4,
C60_4, C61_4, C62_4, C63_4, C64_4, C65_4, C66_4, N4_4, C67_4, C68_4, C69_4,
C70_4, C71_4, C72_4, C73_4, C74_4, C75_4, C76_4, C77_4, C78_4, C79_4, C80_4,
C81_4, C82_4, C83_4, C84_4, C85_4}
as
{C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, C9_1, C10_1, C11_1, C12_1,
C13_1, C14_1, C15_1, C16_1, C17_1, N1_1, C18_1, C19_1, C20_1, C21_1, C22_1,
C23_1, C24_1, C25_1, C26_1, C27_1, C28_1, N2_1, O1_1, O2_1, O3_1, O4_1, O5_1,
O6_1, C29_1, C30_1, C31_1, C32_1, C33_1, C34_1, C35_1, C36_1, C37_1, C38_1,
C39_1, C40_1, C41_1, C42_1, C43_1, C44_1, C45_1, C46_1, C47_1, C48_1, C49_1,
C50_1, C51_1, C52_1, C53_1, C54_1, C55_1, N3_1, C56_1, C57_1, C58_1, C59_1,
C60_1, C61_1, C62_1, C63_1, C64_1, C65_1, C66_1, N4_1, C67_1, C68_1, C69_1,
C70_1, C71_1, C72_1, C73_1, C74_1, C75_1, C76_1, C77_1, C78_1, C79_1, C80_1,
C81_1, C82_1, C83_1, C84_1, C85_1} sigma for 1-2: 0.01 1-3: 0.04
8. Others
 Fixed Sof: O3(0.5) H3A(0.5) H3B(0.5)
9.a Riding coordinates:
 O3(H3A,H3B), C16(H16), C46(H46)
9.b Secondary CH2 refined with riding coordinates:
 O1(H1A,H1B), C29(H29A,H29B), C38(H38A,H38B), C67(H67A,H67B), C76(H76A,H76B),
 C85(H85A,H85B), C29(H29A,H29B), C38(H38A,H38B), C67(H67A,H67B), C76(H76A,H76B),
  C85(H85A,H85B), C29(H29A,H29B), C38(H38A,H38B), C67(H67A,H67B), C76(H76A,
 H76B), C85(H85A,H85B), C29(H29A,H29B), C38(H38A,H38B), C67(H67A,H67B),
 C76(H76A,H76B), C85(H85A,H85B)
9.c Me refined with riding coordinates:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C74(H74A,H74B,
 H74C), C75(H75A,H75B,H75C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C),
 C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,
 H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C),
 C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C)
9.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C27(H27), C28(H28), C32(H32), C35(H35), C40(H40), C43(H43), C46(H46),
 C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C57(H57),
  C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66),
 C69(H69), C72(H72), C78(H78), C81(H81), C3(H3), C6(H6), C8(H8), C9(H9),
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20),
  C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C32(H32),
 C35(H35), C40(H40), C43(H43), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51),
  C52(H52), C54(H54), C55(H55), C57(H57), C58(H58), C60(H60), C61(H61),
 C62(H62), C63(H63), C65(H65), C66(H66), C69(H69), C72(H72), C78(H78), C81(H81),
  C3(H3), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C27(H27), C28(H28), C32(H32), C35(H35), C40(H40), C43(H43), C46(H46),
 C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C57(H57),
  C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66),
 C69(H69), C72(H72), C78(H78), C81(H81), C3(H3), C6(H6), C8(H8), C9(H9),
 C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C32(H32), C35(H35),
 C40(H40), C43(H43), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54),
  C55(H55), C57(H57), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65),
 C66(H66), C69(H69), C72(H72), C78(H78), C81(H81), C1(H1), C1(H1)
9.e Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C7(C8,C9,C10,C11,C12), C13(C14,C15,C16,C17,N1), C18(C19,
 C20,C21,C22,C23), C24(C25,C26,C27,C28,N2), C30(C31,C32,C33,C34,C35), C39(C40,
 C41,C42,C43,C44), C45(C46,C47,C48,C49,C50), C51(C52,C53,C54,C55,N3), C56(C57,
 C58,C59,C60,C61), C62(C63,C64,C65,C66,N4), C68(C69,C70,C71,C72,C73), C77(C78,
 C79,C80,C81,C82), C13(C14,C15,C16,C17,N1), C30(C31,C32,C33,C34,C35), C13(C14,
 C15,C16,C17,N1), C24(C25,C26,C27,C28,N2), C51(C52,C53,C54,C55,N3)
9.f X=CH2 refined with riding coordinates:
 O2(H2A,H2B)
;
_shelx_res_checksum              92559
_shelx_hkl_checksum              70142
_shelx_fab_checksum              78661
_platon_squeeze_special_details
;
A solvent mask was calculated and 1103 electrons were 
found in a volume of 3667\%A^3^ in 9 voids per unit cell. 
This is consistent with the presence of 
1[C3H7NO], 2[H2O], 5[C3H7NO], 1[C3H7NO], 2[H2O], 5[C3H7NO], 1[C3H7NO], 1[H2O],per formula unit 
which account for 1140 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU