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_7129174
_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_formula_moiety         'C104.25 H93.5 Cu4 N9.75 O44 S4, C2 H3 N'
_chemical_formula_sum            'C106.25 H96.5 Cu4 N10.75 O44 S4'
_chemical_formula_weight         2610.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
;
2021-08-04 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.244(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2290(4)
_cell_length_b                   24.2010(5)
_cell_length_c                   19.7403(5)
_cell_measurement_reflns_used    15199
_cell_measurement_temperature    123.00(13)
_cell_measurement_theta_max      71.4180
_cell_measurement_theta_min      3.6530
_cell_volume                     6779.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00 121.00   0.50    6.50    --   47.64  33.00  39.00  172
  2  \w     95.00 167.00   0.50   26.50    --  107.75  33.00  39.00  144
  3  \w     97.00 122.00   0.50   26.50    --  107.75 125.00 -60.00   50
  4  \w    145.00 172.00   0.50   26.50    --  107.75 125.00 -60.00   54
  5  \w     95.00 125.00   0.50   26.50    --  107.75   0.00-150.00   60
  6  \w    132.00 159.00   0.50   26.50    --  107.75   0.00-150.00   54
  7  \w     68.00 121.00   0.50   26.50    --  107.75 -15.00-150.00  106
  8  \w     39.00  64.00   0.50   26.50    --  107.75 -33.00-118.00   50
  9  \w     33.00  58.00   0.50   26.50    --  107.75 -30.00 -90.00   50
 10  \w     40.00  75.00   0.50   26.50    --  107.75 -45.00 -60.00   70
 11  \w     38.00  75.00   0.50   26.50    --  107.75 -45.00  30.00   74
 12  \w     94.00 121.00   0.50   26.50    --  107.75 -61.00  60.00   54
 13  \w     84.00 124.00   0.50   26.50    --  107.75 -61.00  30.00   80
 14  \w     55.00  82.00   0.50   26.50    --  107.75 -15.00  60.00   54
 15  \w     45.00  72.00   0.50   26.50    --  107.75 -61.00  60.00   54
 16  \w     49.00  76.00   0.50   26.50    --  107.75 -61.00  30.00   54
 17  \w     34.00  66.00   0.50   26.50    --  107.75 -30.00  60.00   64
 18  \w     36.00  66.00   0.50   26.50    --  107.75 -30.00  90.00   60
 19  \w     42.00  71.00   0.50   26.50    --  107.75 -45.00  60.00   58
 20  \w     33.00  65.00   0.50   26.50    --  107.75 -30.00 120.00   64
 21  \w     34.00  64.00   0.50   26.50    --  107.75 -30.00 150.00   60
 22  \w     35.00 106.00   0.50   26.50    --  107.75 -94.00 150.00  142
 23  \w     39.00  84.00   0.50   26.50    --  107.75 -94.00  60.00   90
 24  \w     34.00  66.00   0.50   26.50    --  107.75 -30.00  30.00   64
 25  \w     35.00  87.00   0.50    6.50    --   47.64-125.00 120.00  104
 26  \w    -26.00  62.00   0.50    6.50    --   47.64 -33.00-118.00  176
 27  \w     34.00  65.00   0.50   26.50    --  107.75 -15.00-150.00   62
 28  \w     34.00  59.00   0.50   26.50    --  107.75 -30.00-150.00   50
 29  \w     41.00  89.00   0.50   26.50    --  107.75   0.00-150.00   96
 30  \w     35.00  94.00   0.50   26.50    --  107.75 -94.00-180.00  118
 31  \w    -61.00  26.00   0.50    6.50    --  -47.64  33.00  39.00  174
 32  \w    -69.00 -12.00   0.50   26.50    --  -86.25  33.00  39.00  114
 33  \w    -77.00 -25.00   0.50    6.50    --  -47.64 125.00   0.00  104
 34  \w   -121.00 -34.00   0.50    6.50    --  -47.64 -33.00-118.00  174
 35  \w   -120.00 -77.00   0.50    6.50    --  -47.64-125.00 -60.00   86
 36  \w   -120.00 -92.00   0.50    6.50    --  -47.64-125.00  60.00   56
 37  \w   -160.00 -98.00   0.50   26.50    --  -86.25 -33.00-118.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0628200000
_diffrn_orient_matrix_UB_12      -0.0208563000
_diffrn_orient_matrix_UB_13      0.0617693000
_diffrn_orient_matrix_UB_21      0.0884803000
_diffrn_orient_matrix_UB_22      0.0172544000
_diffrn_orient_matrix_UB_23      -0.0352208000
_diffrn_orient_matrix_UB_31      -0.0036996000
_diffrn_orient_matrix_UB_32      0.0575624000
_diffrn_orient_matrix_UB_33      0.0328270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73068
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.689
_diffrn_reflns_theta_min         3.611
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             2682
_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          0.05
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.295
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         14158
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.1138
_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          0.3277
_refine_ls_wR_factor_ref         0.3567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8769
_reflns_number_total             14158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05610g2.cif
_cod_data_source_block           sw3_67_2
_cod_original_formula_sum        'C106.25 H96.50 Cu4 N10.75 O44 S4'
_cod_database_code               7129174
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu2 C50 H100 N4 O20 S2'
_diffrn_oxdiff_digest_frames
;
01c608e5a77a0925456fa5a5fef28fc53000026ca5b
;
_diffrn_oxdiff_digest_hkl
;
01fccf5fff21343e1c5a9ffe36792a96546d95
;
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
2. Restrained distances
 N6C-C55C
 1.5 with sigma of 0.02
 C53A-C54A
 1.5 with sigma of 0.02
 N6C-C56C
 1.5 with sigma of 0.02
 N6B-C55B
 1.5 with sigma of 0.02
 C53C-N6C
 1.3 with sigma of 0.02
 C55A-N6A
 1.5 with sigma of 0.02
 N6A-C53A
 1.3 with sigma of 0.02
 C56A-N6A
 1.5 with sigma of 0.02
 C53A-O22
 1.3 with sigma of 0.02
 C54C-C53C
 1.5 with sigma of 0.02
 N6B-C56B
 1.5 with sigma of 0.02
 N6B-C53B
 1.3 with sigma of 0.02
 C54B-C53B
 1.5 with sigma of 0.02
 N5-C52
 1.5 with sigma of 0.02
 N5-C51 = N5-C52
 1.45 with sigma of 0.02
 C49B-O21
 1.5 with sigma of 0.02
 C53B-C55B
 2.5 with sigma of 0.04
 C55B-O22
 2.8 with sigma of 0.04
 C55B-C56B
 2.5 with sigma of 0.04
 C56C-C53C
 2.5 with sigma of 0.04
 C55C-O22
 2.8 with sigma of 0.04
 C55C-C53C
 2.5 with sigma of 0.04
 C55C-C56C
 2.6 with sigma of 0.04
 C55A-C53A
 2.5 with sigma of 0.04
 C55A-C56A
 2.5 with sigma of 0.04
 C56A-C53A
 2.5 with sigma of 0.04
 C56A-C54A
 2.7 with sigma of 0.04
 C54C-C56C
 2.7 with sigma of 0.04
 C54B-C56B
 2.7 with sigma of 0.04
 C53B-C56B
 2.5 with sigma of 0.04
 C52-C50
 2.7 with sigma of 0.04
 C51-C52
 2.5 with sigma of 0.04
 N5-C50
 2.2 with sigma of 0.04
3. Restrained planarity
 O21, N5, C50, C51, C52
 with sigma of 0.1
4. Others
 Sof(S2A)=Sof(O15A)=Sof(O16A)=1-FVAR(1)
 Sof(S2B)=Sof(O15B)=Sof(O16B)=FVAR(1)
 Fixed Sof: N5(0.375) N6C(0.125) C50(0.375) H50A(0.375) H50B(0.375)
 H50C(0.375) C51(0.375) H51A(0.375) H51B(0.375) H51C(0.375) C52(0.375)
 H52A(0.375) H52B(0.375) H52C(0.375) C53C(0.125) C54C(0.125) C55C(0.125)
 C56C(0.125) N6A(0.25) C49B(0.625) C53A(0.25) C54A(0.25) C55A(0.25) H55A(0.25)
 H55B(0.25) H55C(0.25) C56A(0.25) H56A(0.25) H56B(0.25) H56C(0.25) N6B(0.125)
 C53B(0.125) C54B(0.125) C55B(0.125) C56B(0.125) N7(0.5) C57(0.5) C58(0.5)
 H58A(0.5) H58B(0.5) H58C(0.5) C49A(0.375)
 Fixed Uiso: N6A(0.12) C53A(0.2) C54A(0.12)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C14(H14), C15(H15), C18(H18), C33(H33), C34(H34),
 C36(H36), C38(H38), C39(H39), C42(H42)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C55A(H55A,H55B,H55C), C56A(H56A,H56B,H56C), C58(H58A,H58B,H58C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89904
_shelx_fab_checksum              75915
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.646
_oxdiff_exptl_absorpt_empirical_full_min 0.314