Steric Control of Sorting Regimes in Self-Assembled Cages
Walker, Samuel Edward; Boer, Stephanie A.; Malcomson, Thomas; Paterson, Martin J.; Tuck, Kellie; Turner, David Roger; Chemical Communications  (2021) –; doi:10.1039/D1CC05610G

data_7129173
_publ_section_title
;
 Steric Control of Sorting Regimes in Self-Assembled Cages
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05610G
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety
'C90 H61 Cu4 N8 O44 S4, 2(C2 H3 N), C3 H4 N O, 0.667(C H3 O)'
_chemical_formula_sum            'C97.67 H73 Cu4 N11 O45.67 S4'
_chemical_formula_weight         2513.76
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.438(3)
_cell_length_b                   17.438(3)
_cell_length_c                   41.986(8)
_cell_measurement_reflns_used    7337
_cell_measurement_temperature    373.15
_cell_measurement_theta_max      'Value not reported by XDS'
_cell_measurement_theta_min      'Value not reported by XDS'
_cell_volume                     12767(4)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      373.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.710915
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            225176
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.249
_diffrn_reflns_theta_max         32.271
_diffrn_reflns_theta_min         1.265
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  'Value not reported by XDS'
_exptl_absorpt_correction_T_min  'Value not reported by XDS'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5125
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol, Acetonitrile'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details
;
 Flack x determined using 4100 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         21123
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0967
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2479
_refine_ls_wR_factor_ref         0.2879
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                12000
_reflns_number_total             21123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05610g2.cif
_cod_data_source_block           sw3_167a_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' 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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7129173
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O22-H22
 0.85 with sigma of 0.01
 C46A-O23A
 1.5 with sigma of 0.02
 C46B-O23B
 1.5 with sigma of 0.02
 C15-C18
 1.45 with sigma of 0.002
 Cu2-H22
 2.825701 with sigma of 0.02
 C45-H22
 1.890256 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O23B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 1.7A
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 1.7A
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: H36(0.5) N6A(0.5) C49A(0.5) C50A(0.5) H50A(0.5) H50B(0.5)
 H50C(0.5) N6B(0.5) C49B(0.5) C50B(0.5) H50D(0.5) H50E(0.5) H50F(0.5) O23A(0.5)
 H23A(0.5) C46A(0.5) N5(0.5) C47(0.5) H46A(0.5) H47B(0.5) H47A(0.5) C48(0.5)
 O23B(0.33333) C46B(0.33333) H46B(0.33333) H46C(0.33333) H46D(0.33333)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C20(H20), C24(H24), C42(H42)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C14(H14), C17(H17), C30(H30), C31(H31), C33(H33),
 C35(H35), C36(H36), C39(H39)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C50A(H50A,H50B,H50C), C50B(H50D,H50E,H50F),
 C47(H46A,H47B,H47A), C46B(H46B,H46C,H46D)
5.d Idealised tetrahedral OH refined as rotating group:
 O23A(H23A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58607
_shelx_fab_checksum              5769
_olex2_submission_special_instructions 'No special instructions were received'