A family of diastereomeric dodecanuclear coordination cages based on inversion of chirality of individual triangular cyclic helicate faces
Argent, Stephen P.; Jackson, Fiona C.; Chan, Ho Man; Meyrick, Sam; Taylor, Christopher G. P.; Ronson, Tanya K.; Rourke, Jonathan P.; Ward, Michael D.; Chemical Science  (2020) –; doi:10.1039/D0SC04347H

data_1559070
_publ_section_title
;
 A family of diastereomeric dodecanuclear coordination cages based on
 inversion of chirality of individual triangular cyclic helicate faces
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC04347H
_journal_year                    2020
_chemical_formula_moiety         'C480 H396 Cd12 N108, 4(O)'
_chemical_formula_sum            'C640 H644 B24 Cd12 F96 N188 O4'
_chemical_formula_weight         14465.63
_space_group_crystal_system      cubic
_space_group_IT_number           196
_space_group_name_Hall           'F 2 2 3'
_space_group_name_H-M_alt        'F 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   geom
_audit_creation_date             2019-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-12 deposited with the CCDC.	2020-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   42.9589(6)
_cell_length_b                   42.9589(6)
_cell_length_c                   42.9589(6)
_cell_measurement_reflns_used    8566
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.5790
_cell_measurement_theta_min      4.1110
_cell_volume                     79279.2(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -87.00 -32.00   1.00   80.00    --    0.00 178.00   0.00   55
  2  \w     36.00 137.00   1.00  200.00    --   69.83-153.00-107.00  101
  3  \w     94.00 143.00   1.00  200.00    --   69.83 125.00-150.00   49
  4  \w    -76.00  33.00   1.00   80.00    --    0.00 -77.00-180.00  109
  5  \w    -33.00  76.00   1.00   80.00    --    0.00  77.00 -90.00  109
  6  \w     45.00  95.00   1.00  200.00    --   69.83  38.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0237288000
_diffrn_orient_matrix_UB_12      0.0001374000
_diffrn_orient_matrix_UB_13      -0.0269069000
_diffrn_orient_matrix_UB_21      0.0200904000
_diffrn_orient_matrix_UB_22      -0.0239146000
_diffrn_orient_matrix_UB_23      0.0176017000
_diffrn_orient_matrix_UB_31      -0.0178637000
_diffrn_orient_matrix_UB_32      -0.0267256000
_diffrn_orient_matrix_UB_33      -0.0158855000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22267
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        30.923
_diffrn_reflns_theta_max         30.923
_diffrn_reflns_theta_min         3.412
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.222
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.45b (Rigaku Oxford Diffraction, 2018) Analytical numeric absorption correction using a multifaceted crystal 			model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             29568
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile, diisopropyl ether'
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.083
_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   1.791
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         2076
_refine_ls_number_restraints     916
_refine_ls_restrained_S_all      1.651
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.1104
_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          0.2944
_refine_ls_wR_factor_ref         0.3288
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1801
_reflns_number_total             2076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04347h2.cif
_cod_data_source_block           AAAA-F23_sq
_cod_original_cell_volume        79279(3)
_cod_database_code               1559070
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Cd12C400H250N30O20B24F60
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.574
_reflns_odcompleteness_completeness 65.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.34
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.09(14)
 0.42(8) 0.42(8) 0.07(8)
2. 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
3. Restrained distances
 Cd1-N31B
 -2.3 with sigma of 0.02
 Cd1-N21A
 -2.3 with sigma of 0.02
 Cd1-N11A
 2.45 with sigma of 0.02
 C44B-C43B
 1.363 with sigma of 0.012
 C45B-C44B
 1.407 with sigma of 0.012
 C32B-C45B
 1.469 with sigma of 0.006
 C33B-C32B
 1.389 with sigma of 0.01
 C32B-N31B
 1.341 with sigma of 0.008
 C34B-C33B
 1.385 with sigma of 0.01
 C35B-C34B
 1.38 with sigma of 0.013
 C36B-C35B
 1.379 with sigma of 0.015
 C36B-N31B
 1.34 with sigma of 0.01
 C16B-N11B
 1.34 with sigma of 0.01
 C12B-N11B
 1.341 with sigma of 0.008
 N21B-N22B
 1.354 with sigma of 0.007
 C25B-N21B
 1.339 with sigma of 0.007
 C23B-N22B
 1.345 with sigma of 0.008
 C26B-N22B
 1.464 with sigma of 0.016
 C16B-C15B
 1.379 with sigma of 0.015
 C15B-C14B
 1.38 with sigma of 0.013
 C14B-C13B
 1.385 with sigma of 0.01
 C13B-C12B
 1.389 with sigma of 0.01
 C12B-C25B
 1.469 with sigma of 0.006
 C25B-C24B
 1.407 with sigma of 0.012
 C24B-C23B
 1.363 with sigma of 0.012
 C51B-C26B
 1.512 with sigma of 0.007
 C51B-C56B
 1.427 with sigma of 0.015
 C51B-C52B
 1.37 with sigma of 0.013
 C56B-C57B
 1.419 with sigma of 0.011
 C55B-C54B
 1.417 with sigma of 0.012
 C55B-C60B
 1.417 with sigma of 0.012
 C54B-C53B
 1.363 with sigma of 0.013
 C53B-C52B
 1.385 with sigma of 0.01
 C57B-C58B
 1.363 with sigma of 0.013
 C58B-C59B
 1.38 with sigma of 0.013
 C59B-C60B
 1.363 with sigma of 0.013
 C24A-C23A
 1.363 with sigma of 0.012
 C25A-C24A
 1.407 with sigma of 0.012
 C12A-C25A
 1.469 with sigma of 0.006
 C13A-C12A
 1.389 with sigma of 0.01
 C12A-N11A
 1.341 with sigma of 0.008
 C14A-C13A
 1.385 with sigma of 0.01
 C15A-C14A
 1.38 with sigma of 0.013
 C16A-C15A
 1.379 with sigma of 0.015
 C16A-N11A
 1.34 with sigma of 0.01
 C56B-C55B
 1.39 with sigma of 0.008
 C54B-C46B_$1
 1.512 with sigma of 0.007
 C31A-C32A
 1.402 with sigma of 0.008
 C31A-C32A_$2
 1.402 with sigma of 0.008
 C32A-C33A
 1.509 with sigma of 0.009
 C31A-C26A
 1.513 with sigma of 0.008
 H26C_$3-H33A
 -1.9 with sigma of 0.02
 C46B-N41B
 2.436 with sigma of 0.02
 C43B-N41B
 2.24 with sigma of 0.01
 C43B-C46B
 2.524 with sigma of 0.021
 C45B-N42B
 2.131 with sigma of 0.009
 C44B-N42B
 2.18 with sigma of 0.012
 C45B-C43B
 2.202 with sigma of 0.015
 C44B-N41B
 2.263 with sigma of 0.013
 C32B-N41B
 2.438 with sigma of 0.012
 C32B-C44B
 2.588 with sigma of 0.016
 C33B-C45B
 2.493 with sigma of 0.013
 C45B-N31B
 2.385 with sigma of 0.012
 C33B-N31B
 2.396 with sigma of 0.015
 C34B-C32B
 2.386 with sigma of 0.014
 C35B-C33B
 2.398 with sigma of 0.017
 C36B-C34B
 2.369 with sigma of 0.019
 C35B-N31B
 2.397 with sigma of 0.019
 C36B-C32B
 2.285 with sigma of 0.015
 C16B-C12B
 2.285 with sigma of 0.015
 C25B-N22B
 2.131 with sigma of 0.009
 C23B-N21B
 2.24 with sigma of 0.01
 C26B-N21B
 2.436 with sigma of 0.02
 C23B-C26B
 2.524 with sigma of 0.021
 C15B-N11B
 2.397 with sigma of 0.019
 C16B-C14B
 2.369 with sigma of 0.019
 C15B-C13B
 2.398 with sigma of 0.017
 C14B-C12B
 2.386 with sigma of 0.014
 C13B-N11B
 2.396 with sigma of 0.015
 C25B-N11B
 2.385 with sigma of 0.012
 C13B-C25B
 2.493 with sigma of 0.013
 C12B-N21B
 2.438 with sigma of 0.012
 C24B-N21B
 2.263 with sigma of 0.013
 C12B-C24B
 2.588 with sigma of 0.016
 C25B-C23B
 2.202 with sigma of 0.015
 C24B-N22B
 2.18 with sigma of 0.012
 C51B-N22B
 2.496 with sigma of 0.045
 C56B-C52B
 2.409 with sigma of 0.02
 C51B-C57B
 2.499 with sigma of 0.02
 C55B-C57B
 2.437 with sigma of 0.017
 C56B-C54B
 2.451 with sigma of 0.016
 C56B-C60B
 2.451 with sigma of 0.016
 C54B-C60B
 2.483 with sigma of 0.028
 C55B-C53B
 2.416 with sigma of 0.018
 C54B-C52B
 2.389 with sigma of 0.02
 C51B-C53B
 2.404 with sigma of 0.021
 C56B-C58B
 2.421 with sigma of 0.018
 C57B-C59B
 2.38 with sigma of 0.018
 C58B-C60B
 2.38 with sigma of 0.018
 C55B-C59B
 2.416 with sigma of 0.018
 C23A-N21A
 2.24 with sigma of 0.01
 C25A-N22A
 2.131 with sigma of 0.009
 C24A-N22A
 2.18 with sigma of 0.012
 C25A-C23A
 2.202 with sigma of 0.015
 C24A-N21A
 2.263 with sigma of 0.013
 C12A-N21A
 2.438 with sigma of 0.012
 C12A-C24A
 2.588 with sigma of 0.016
 C13A-C25A
 2.493 with sigma of 0.013
 C25A-N11A
 2.385 with sigma of 0.012
 C13A-N11A
 2.396 with sigma of 0.015
 C14A-C12A
 2.386 with sigma of 0.014
 C15A-C13A
 2.398 with sigma of 0.017
 C16A-C14A
 2.369 with sigma of 0.019
 C15A-N11A
 2.397 with sigma of 0.019
 C16A-C12A
 2.285 with sigma of 0.015
 C51B-C55B
 2.421 with sigma of 0.016
 C52B-C26B
 2.521 with sigma of 0.015
 C56B-C26B
 2.521 with sigma of 0.015
 C54B-N42B_$1
 2.496 with sigma of 0.045
 C54B-C46B_$1
 2.496 with sigma of 0.045
 C31A-N22A
 2.473 with sigma of 0.024
 C31A-C31A_$3
 2.428 with sigma of 0.016
 C31A-C33A
 2.527 with sigma of 0.017
 C26A-N21A
 2.436 with sigma of 0.02
 C23A-C26A
 2.524 with sigma of 0.021
 C26A-C32A \\sim C26A-C32A_$2
 with sigma of 0.02
 C26A-C33A \\sim C26A-C33A_$2
 with sigma of 0.02
4. Restrained planarity
 C32B, C45B, C33B, N31B
 with sigma of 0.1
 C45B, N41B, C44B, C32B
 with sigma of 0.1
 N42B, N41B, C46B, C43B
 with sigma of 0.1
 C44B, C45B, C32B, C33B
 with sigma of 0.1
 N42B, N41B, C45B, C44B
 with sigma of 0.1
 N41B, C45B, C44B, C43B
 with sigma of 0.1
 C45B, C44B, C43B, N42B
 with sigma of 0.1
 C44B, C43B, N42B, N41B
 with sigma of 0.1
 C43B, N42B, N41B, C45B
 with sigma of 0.1
 C32B, C33B, C34B, C35B
 with sigma of 0.1
 C33B, C34B, C35B, C36B
 with sigma of 0.1
 C34B, C35B, C36B, N31B
 with sigma of 0.1
 C35B, C36B, N31B, C32B
 with sigma of 0.1
 C36B, N31B, C32B, C33B
 with sigma of 0.1
 N31B, C32B, C33B, C34B
 with sigma of 0.1
 C51B, C26B, C56B, C52B
 with sigma of 0.1
 C56B, C51B, C55B, C57B
 with sigma of 0.1
 C55B, C56B, C54B, C60B
 with sigma of 0.1
 C12B, N11B, C13B, C25B
 with sigma of 0.1
 C25B, N21B, C12B, C24B
 with sigma of 0.1
 N22B, N21B, C23B, C26B
 with sigma of 0.1
 C13B, C12B, C25B, C24B
 with sigma of 0.1
 N21B, N22B, C23B, C24B
 with sigma of 0.1
 N22B, C23B, C24B, C25B
 with sigma of 0.1
 C23B, C24B, C25B, N21B
 with sigma of 0.1
 C24B, C25B, N21B, N22B
 with sigma of 0.1
 C25B, N21B, N22B, C23B
 with sigma of 0.1
 N11B, C16B, C15B, C14B
 with sigma of 0.1
 C16B, C15B, C14B, C13B
 with sigma of 0.1
 C15B, C14B, C13B, C12B
 with sigma of 0.1
 C14B, C13B, C12B, N11B
 with sigma of 0.1
 C13B, C12B, N11B, C16B
 with sigma of 0.1
 C12B, N11B, C16B, C15B
 with sigma of 0.1
 C51B, C56B, C55B, C54B
 with sigma of 0.1
 C56B, C55B, C54B, C53B
 with sigma of 0.1
 C55B, C54B, C53B, C52B
 with sigma of 0.1
 C54B, C53B, C52B, C51B
 with sigma of 0.1
 C53B, C52B, C51B, C56B
 with sigma of 0.1
 C52B, C51B, C56B, C55B
 with sigma of 0.1
 C56B, C55B, C60B, C59B
 with sigma of 0.1
 C55B, C60B, C59B, C58B
 with sigma of 0.1
 C60B, C59B, C58B, C57B
 with sigma of 0.1
 C59B, C58B, C57B, C56B
 with sigma of 0.1
 C58B, C57B, C56B, C55B
 with sigma of 0.1
 C57B, C56B, C55B, C60B
 with sigma of 0.1
 C12A, C25A, C13A, N11A
 with sigma of 0.1
 C25A, N21A, C24A, C12A
 with sigma of 0.1
 C24A, C25A, C12A, C13A
 with sigma of 0.1
 N22A, N21A, C25A, C24A
 with sigma of 0.1
 N21A, C25A, C24A, C23A
 with sigma of 0.1
 C25A, C24A, C23A, N22A
 with sigma of 0.1
 C24A, C23A, N22A, N21A
 with sigma of 0.1
 C23A, N22A, N21A, C25A
 with sigma of 0.1
 C12A, C13A, C14A, C15A
 with sigma of 0.1
 C13A, C14A, C15A, C16A
 with sigma of 0.1
 C14A, C15A, C16A, N11A
 with sigma of 0.1
 C15A, C16A, N11A, C12A
 with sigma of 0.1
 C16A, N11A, C12A, C13A
 with sigma of 0.1
 N11A, C12A, C13A, C14A
 with sigma of 0.1
 Cd1, N21A, C25A, C12A, N11A
 with sigma of 0.1
 Cd1, N31B, C32B, C45B, N41B
 with sigma of 0.1
 Cd1, N21B, C25B, C12B, N11B
 with sigma of 0.1
 C55B, C53B, C54B, C46B_$1
 with sigma of 0.1
 C46B_$1, N42B_$1, C43B_$1, N41B_$1
 with sigma of 0.1
 C31A, C32A, C31A_$3, C32A_$3, C31A_$2, C32A_$2
 with sigma of 0.1
 N22A, N21A, C26A, C23A
 with sigma of 0.1
 C26A, C31A, C32A, C32A_$2
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C16B \\sim C15B \\sim C14B \\sim C13B \\sim C12B \\sim C25B \\sim C24B \\sim
C23B \\sim C26B \\sim C51B \\sim C56B \\sim C55B \\sim C54B \\sim C53B \\sim
C52B \\sim C57B \\sim C58B \\sim C59B \\sim C60B \\sim C36B \\sim C35B \\sim
C34B \\sim C33B \\sim C32B \\sim C45B \\sim C44B \\sim C43B \\sim C46B \\sim
C16A \\sim C15A \\sim C14A \\sim C13A \\sim C12A \\sim C25A \\sim C24A \\sim
C23A \\sim C26A \\sim C31A \\sim C32A \\sim C33A \\sim N11B \\sim N21B \\sim
N22B \\sim N31B \\sim N41B \\sim N42B \\sim N11A \\sim N21A \\sim N22A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31A) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C33A) \\sim Ueq: with sigma
of 0.025 and sigma for terminal atoms of 0.05
6. Rigid body (RIGU) restrains
 C16B, C15B, C14B, C13B, C12B, C25B, C24B, C23B, C26B, C51B, C56B, C55B, C54B,
 C53B, C52B, C57B, C58B, C59B, C60B, C36B, C35B, C34B, C33B, C32B, C45B, C44B,
 C43B, C46B, C16A, C15A, C14A, C13A, C12A, C25A, C24A, C23A, C26A, C31A, C32A,
 C33A, N11B, N21B, N22B, N31B, N41B, N42B, N11A, N21A, N22A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Secondary CH2 refined with riding coordinates:
 C26B(H26A,H26B), C46B(H46A,H46B), C26A(H26C,H26D)
7.b Aromatic/amide H refined with riding coordinates:
 C16B(H16B), C15B(H15B), C14B(H14B), C13B(H13B), C24B(H24B), C23B(H23B),
 C53B(H53B), C52B(H52B), C57B(H57B), C58B(H58B), C59B(H59B), C60B(H60B),
 C36B(H36B), C35B(H35B), C34B(H34B), C33B(H33B), C44B(H44B), C43B(H43B),
 C16A(H16A), C15A(H15A), C14A(H14A), C13A(H13A), C24A(H24A), C23A(H23A)
7.c Idealised Me refined as rotating group:
 C33A(H33A,H33C,H33D)
;
_shelx_res_checksum              72064
_shelx_fab_checksum              9076
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_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 1.157
_oxdiff_exptl_absorpt_empirical_full_min 0.764