Exploration of the polymorphic solid-state landscape of an amide-linked organic cage using computation and automation.
Shields, C. E.; Fellowes, T.; Slater, A. G.; Cooper, A. I.; Andrews, K. G.; Szczypiński, F T; Chemical communications (Cambridge, England) 60 (2024) 6023–6026; doi:10.1039/d4cc01407c

data_7132993
_publ_section_title
;
 Exploration of the polymorphic solid-state landscape of an amide-linked
 organic cage using computation and automation.
;
_journal_issue                   47
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6023
_journal_page_last               6026
_journal_paper_doi               10.1039/d4cc01407c
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C126 H112 N6 O10, 24[C2H6SO]'
_chemical_formula_sum            'C174 H256 N6 O34 S24'
_chemical_formula_weight         3745.27
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_Hall           'P 6c 2c'
_space_group_name_H-M_alt        'P 63 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-27 deposited with the CCDC.	2024-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   19.9064(2)
_cell_length_b                   19.9064(2)
_cell_length_c                   33.4510(5)
_cell_measurement_reflns_used    8374
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      18.05461910402454
_cell_measurement_theta_min      1.1770430987977856
_cell_volume                     11479.6(2)
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction
;
DIALS 3.17.0-2-gd57c1bda0-release (Winter, G. et al., 2018)
dials.scale (Beilsten-Edmands, J. et al., 2020)
XIA2 3.17.0 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61628
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        16.675
_diffrn_reflns_theta_max         16.675
_diffrn_reflns_theta_min         1.288
_diffrn_source_details           'Allan et al. (2017)'
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9981514936621928
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIALS 3.17.0-2-gd57c1bda0-release
Scaling & analysis of unmerged intensities, 
absorption correction using spherical harmonics
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_description       block
_exptl_crystal_F_000             3996
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 278 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2332
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.1987
_refine_ls_R_factor_gt           0.1451
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3485
_refine_ls_wR_factor_ref         0.3888
_reflns_Friedel_coverage         0.623
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                954
_reflns_number_total             2332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01407c3.cif
_cod_data_source_block           ka1_dmso_meoh_b
_cod_depositor_comments
'Adding full bibliography for 7132990--7132997.cif.'
_cod_original_cell_volume        11479.6(3)
_cod_database_code               7132993
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.997
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C12-C20
 1.54 with sigma of 0.01
 C15-C10 = C11-C10 = C12-C11 = C13-C12 = C14-C13 = C15-C14 = C3-C2 = C2-C1 =
 C6-C1 = C6-C5 = C5-C4 = C4-C3 = C22-C20 = C21-C20 = C10-C8
 1.39 with sigma of 0.01
 C22-C21
 2.32 with sigma of 0.04
 C14-C17 \\sim C14-C18 \\sim C14-C19 \\sim C17-C18 \\sim C17-C19 \\sim C18-C19
 with sigma of 0.02
 C16-C14 \\sim C16-C17 \\sim C16-C18 \\sim C16-C19
 with sigma of 0.01
3. Restrained planarity
 C12, C20, C21, C22
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(O26)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
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
 Fixed Sof: O26(0.6667) H26(0.333333)
7.a Ternary CH refined with riding coordinates:
 C23(H23)
7.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
7.c Aromatic/amide H refined with riding coordinates:
 N7(H7), C2(H2), C4(H4), C5(H5), C11(H11), C13(H13), C15(H15), C21(H21),
 C22(H22)
7.d Tetrahedral OH refined with riding coordinates:
 O26(H26)
;
_shelx_res_checksum              45183
_shelx_hkl_checksum              82097
_shelx_fab_checksum              26409
_olex2_submission_special_instructions 'No special instructions were received'