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_7129175
_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
'C98 H78.5 Cu4 N10.5 O44 S4, 6.667(C4 H9 N O), C H4 O, 3(H2O)'
_chemical_formula_sum            'C125.67 H148.5 Cu4 N17.17 O54.67 S4'
_chemical_formula_weight         3156.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_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
;
2021-08-04 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.549(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.2388(4)
_cell_length_b                   19.0842(2)
_cell_length_c                   28.2540(4)
_cell_measurement_reflns_used    56328
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.7370
_cell_measurement_theta_min      3.6080
_cell_volume                     15269.7(4)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_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 0.990
_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    -68.00  22.00   0.50    0.50    --  -47.64  84.00 127.00  180
  2  \w    -58.00  17.00   0.50    0.50    --  -47.64  38.00 120.00  150
  3  \w    -61.00  18.00   0.50    0.50    --  -47.64  38.00  60.00  158
  4  \w    -59.00 -15.00   0.50    2.00    --  -86.25  45.00 -30.00   88
  5  \w    -87.00 -62.00   0.50    2.00    --  -86.25  84.00 127.00   50
  6  \w   -128.00 -73.00   0.50    2.00    --  -86.25 -45.00 -60.00  110
  7  \w   -110.00 -84.00   0.50    2.00    --  -86.25 -45.00 -90.00   52
  8  \w   -120.00 -85.00   0.50    0.50    --  -47.64-125.00-180.00   70
  9  \w   -154.00-129.00   0.50    2.00    --  -86.25 -45.00 -90.00   50
 10  \w   -143.00-118.00   0.50    2.00    --  -86.25 -84.00   8.00   50
 11  \w   -106.00 -78.00   0.50    0.50    --  -47.64-125.00  60.00   56
 12  \w   -113.00 -73.00   0.50    0.50    --  -47.64-125.00  30.00   80
 13  \w   -119.00 -79.00   0.50    0.50    --  -47.64-125.00 150.00   80
 14  \w      1.00  26.00   0.50    0.50    --   47.64 -84.00   8.00   50
 15  \w     29.00  59.00   0.50    0.50    --   47.64 -84.00   8.00   60
 16  \w     58.00 129.00   0.50    2.00    --  107.75 -84.00   8.00  142
 17  \w     84.00 121.00   0.50    2.00    --  107.75 -61.00  60.00   74
 18  \w    144.00 169.00   0.50    2.00    --  107.75  15.00  60.00   50
 19  \w    134.00 176.00   0.50    2.00    --  107.75  61.00  60.00   84
 20  \w    128.00 176.00   0.50    2.00    --  107.75  61.00 -30.00   96
 21  \w    143.00 171.00   0.50    2.00    --  107.75  30.00 -90.00   56
 22  \w    117.00 175.00   0.50    2.00    --  107.75  15.00 -60.00  116
 23  \w    126.00 178.00   0.50    2.00    --  107.75  77.00  30.00  104
 24  \w    122.00 149.00   0.50    2.00    --  107.75  77.00  60.00   54
 25  \w    106.00 160.00   0.50    2.00    --  107.75  84.00 127.00  108
 26  \w    103.00 130.00   0.50    2.00    --  107.75  61.00  60.00   54
 27  \w     86.00 119.00   0.50    2.00    --  107.75  77.00  30.00   66
 28  \w     92.00 117.00   0.50    2.00    --  107.75  61.00 -30.00   50
 29  \w    103.00 141.00   0.50    2.00    --  107.75  30.00 -90.00   76
 30  \w     96.00 177.00   0.50    2.00    --  107.75  30.00-120.00  162
 31  \w    109.00 135.00   0.50    2.00    --  107.75 125.00-180.00   52
 32  \w     95.00 120.00   0.50    2.00    --  107.75  45.00 -90.00   50
 33  \w     97.00 138.00   0.50    2.00    --  107.75  15.00-120.00   82
 34  \w     43.00 105.00   0.50    2.00    --  107.75 -94.00-180.00  124
 35  \w     39.00  65.00   0.50    2.00    --  107.75 -30.00 -90.00   52
 36  \w     40.00  76.00   0.50    2.00    --  107.75 -45.00 -60.00   72
 37  \w     50.00 106.00   0.50    2.00    --  107.75 -94.00   0.00  112
 38  \w     49.00 104.00   0.50    2.00    --  107.75 -94.00 -60.00  110
 39  \w     38.00  75.00   0.50    2.00    --  107.75 -45.00  30.00   74
 40  \w     33.00  66.00   0.50    2.00    --  107.75 -30.00  90.00   66
 41  \w     40.00  73.00   0.50    2.00    --  107.75 -61.00  60.00   66
 42  \w     48.00  90.00   0.50    2.00    --  107.75 -94.00  90.00   84
 43  \w     34.00  66.00   0.50    2.00    --  107.75 -30.00  60.00   64
 44  \w     36.00  74.00   0.50    2.00    --  107.75 -45.00   0.00   76
 45  \w     33.00  58.00   0.50    2.00    --  107.75 -30.00   0.00   50
 46  \w    101.00 126.00   0.50    2.00    --  107.75  15.00  60.00   50
 47  \w     86.00 112.00   0.50    2.00    --  107.75  77.00  60.00   52
 48  \w     37.00  62.00   0.50    2.00    --  107.75 -45.00 150.00   50
 49  \w     35.00  96.00   0.50    2.00    --  107.75 -94.00 150.00  122
 50  \w     38.00  94.00   0.50    2.00    --  107.75-125.00  60.00  112
 51  \w     35.00  93.00   0.50    2.00    --  107.75 -94.00 120.00  116
 52  \w     39.00  65.00   0.50    2.00    --  107.75 -30.00-180.00   52
;
_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      0.0427556000
_diffrn_orient_matrix_UB_12      0.0264400000
_diffrn_orient_matrix_UB_13      0.0519127000
_diffrn_orient_matrix_UB_21      -0.0279438000
_diffrn_orient_matrix_UB_22      0.0660397000
_diffrn_orient_matrix_UB_23      -0.0010865000
_diffrn_orient_matrix_UB_31      -0.0187132000
_diffrn_orient_matrix_UB_32      -0.0381263000
_diffrn_orient_matrix_UB_33      0.0340265000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            115511
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.347
_diffrn_reflns_theta_min         3.562
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78580
_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            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             6560
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol, Acetonitrile'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         16053
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0698
_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^)+(0.1267P)^2^+57.9035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14726
_reflns_number_total             16053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05610g2.cif
_cod_data_source_block           sw3_80c
_cod_original_formula_sum        'C125.67 H148.50 Cu4 N17.17 O54.67 S4'
_cod_database_code               7129175
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu4 C100 H100 N8 O10 S4'
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.702
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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
2. Restrained distances
 C55B-N7 = N7-C56B
 1.46 with sigma of 0.02
 O23A-C53A
 1.25 with sigma of 0.02
 C53A-C54A
 1.5 with sigma of 0.02
 O22A-C49A
 1.25 with sigma of 0.02
 N6A-C51A
 1.45 with sigma of 0.002
 C52A-N6A
 1.45 with sigma of 0.002
 N6A-C49A
 1.45 with sigma of 0.002
 O26-C65
 1.5 with sigma of 0.02
 N8-C57
 1.3 with sigma of 0.02
 N8-C60 = N8-C59
 1.45 with sigma of 0.02
 O23B-N7
 2.2 with sigma of 0.04
 N7-C55B
 1.46 with sigma of 0.04
 N7-C56B
 1.46 with sigma of 0.04
 C56B-C55B
 2.46 with sigma of 0.04
 C54B-C56B
 2.88 with sigma of 0.04
 C53A-C56A
 2.4 with sigma of 0.04
 C53A-C55A
 2.4 with sigma of 0.04
 C56A-C55A
 2.46 with sigma of 0.04
 C52A-C49A
 2.4 with sigma of 0.001
 C52A-C51A
 2.4 with sigma of 0.001
 C51A-C49A
 2.4 with sigma of 0.001
 C59-C57
 2.4 with sigma of 0.04
 C62-C63
 2.8 with sigma of 0.04
 C60-C57
 2.5 with sigma of 0.04
 C60-C58
 2.8 with sigma of 0.02
3. Restrained planarity
 O22A, N6A, C49A, C50A, C51A, C52A
 with sigma of 0.001
4. Rigid bond restraints
 O23A, C56B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O23A \\sim C56B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
O5 \\sim S1 \\sim O6: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
Uanis(O22B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Others
 Fixed Sof: O22B(0.75) O23A(0.25) O23B(0.33333) O26(0.5) O27(0.5) O28(0.5)
 O29(0.5) N6A(0.25) N6B(0.75) N7(0.58333) C49A(0.25) C49B(0.75) C50A(0.25)
 H50C(0.25) H50B(0.25) H50A(0.25) C50B(0.75) H50F(0.75) H50D(0.75) H50E(0.75)
 C51A(0.25) H51C(0.25) H51A(0.25) H51B(0.25) C51B(0.75) H51D(0.75) H51E(0.75)
 H51F(0.75) C52A(0.25) H52A(0.25) H52C(0.25) H52B(0.25) C52B(0.75) H52D(0.75)
 H52E(0.75) H52F(0.75) C53A(0.25) C53B(0.33333) C54A(0.25) H54A(0.25)
 H54B(0.25) H54C(0.25) C54B(0.33333) H54D(0.33333) H54E(0.33333) H54F(0.33333)
 C55A(0.25) H55A(0.25) H55B(0.25) H55C(0.25) C55B(0.33333) H55D(0.33333)
 H55E(0.33333) H55F(0.33333) C56A(0.25) H56A(0.25) H56B(0.25) H56C(0.25)
 C56B(0.33333) H56D(0.33333) H56E(0.33333) H56F(0.33333) C65(0.5) H65A(0.5)
 H65B(0.5) H65C(0.5)
 Fixed Uiso: C51A(0.08) C52A(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C19(H19A,H19B)
7.b Me refined with riding coordinates:
 C52A(H52A,H52C,H52B), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C)
7.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C29(H29), C30(H30),
 C31(H31), C34(H34), C35(H35), C36(H36)
7.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C50A(H50C,H50B,H50A), C50B(H50F,H50D,H50E), C51A(H51C,H51A,H51B), C51B(H51D,
 H51E,H51F), C52B(H52D,H52E,H52F), C54A(H54A,H54B,H54C), C54B(H54D,H54E,H54F),
 C55A(H55A,H55B,H55C), C55B(H55D,H55E,H55F), C56A(H56A,H56B,H56C), C56B(H56D,
 H56E,H56F), C59(H59A,H59B,H59C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              22117
_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 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.745