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_1559071
_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, 10.5(B F4), 9.25(O)'
_chemical_formula_sum            'C504 H472 B24 Cd12 F96 N120 O20'
_chemical_formula_weight         11962.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-04
_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                 147.82(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   89.68(3)
_cell_length_b                   24.7801(10)
_cell_length_c                   51.463(19)
_cell_measurement_reflns_used    16547
_cell_measurement_temperature    150.04(11)
_cell_measurement_theta_max      48.8880
_cell_measurement_theta_min      3.9080
_cell_volume                     60909(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      150.04(11)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     -7.00  37.00   1.00   30.00    --    0.00  37.00 -90.00   44
  2  \w    -11.00  26.00   1.00   30.00    --    0.00 -77.00 -30.00   37
  3  \w     47.00  72.00   1.00   30.00    --    0.00  37.00 -90.00   25
  4  \w    -74.00 -16.00   1.00   30.00    --    0.00 -77.00 -30.00   58
  5  \w     37.00 106.00   1.00  120.00    --   62.27-125.00 150.00   69
  6  \w     46.00 135.00   1.00  120.00    --   62.27  77.00  60.00   89
  7  \w     26.00 138.00   1.00  120.00    --   62.27  19.00  30.00  112
  8  \w     44.00  69.00   1.00  120.00    --   62.27 -99.00-150.00   25
  9  \w     -9.00  28.00   1.00  120.00    --   62.27 -37.00-150.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support
'mounted on a loop of keratinized protein fibre in Fomblin oil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0285570000
_diffrn_orient_matrix_UB_12      0.0140311000
_diffrn_orient_matrix_UB_13      0.0542844000
_diffrn_orient_matrix_UB_21      0.0121259000
_diffrn_orient_matrix_UB_22      0.0104048000
_diffrn_orient_matrix_UB_23      -0.0093954000
_diffrn_orient_matrix_UB_31      -0.0088244000
_diffrn_orient_matrix_UB_32      0.0596588000
_diffrn_orient_matrix_UB_33      -0.0111250000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -77
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            56697
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        42.095
_diffrn_reflns_theta_max         42.095
_diffrn_reflns_theta_min         3.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.067
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             24224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile, diisopropyl ether'
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.416
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.565
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2870
_refine_ls_number_reflns         20807
_refine_ls_number_restraints     11142
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.1632
_refine_ls_R_factor_gt           0.1287
_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          0.3762
_refine_ls_wR_factor_ref         0.4159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13213
_reflns_number_total             20807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04347h2.cif
_cod_data_source_block           AACC-C2c_sq
_cod_original_cell_volume        60909(87)
_cod_database_code               1559071
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Cd12C600H400O50N50B24F64
_chemical_oxdiff_usercomment     'WMDWA013_Cu same crystal'
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.463
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_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
 N11A-C16A
 1.34 with sigma of 0.01
 C16A-C15A
 1.38 with sigma of 0.01
 C15A-C14A
 1.38 with sigma of 0.01
 C14A-C13A
 1.38 with sigma of 0.01
 C13A-C12A
 1.39 with sigma of 0.01
 N11A-C12A
 1.35 with sigma of 0.01
 C25A-C12A
 1.45 with sigma of 0.01
 N21A-C25A
 1.34 with sigma of 0.01
 N22A-N21A
 1.35 with sigma of 0.01
 N22A-C23A
 1.34 with sigma of 0.01
 C24A-C23A
 1.37 with sigma of 0.01
 C25A-C24A
 1.39 with sigma of 0.01
 C71H-C26H \\sim C73H-C46H \\sim C75H-C66H \\sim C73G-C46G \\sim C75G-C66G
\\sim C71G-C26G
 with sigma of 0.001
 C54B-C46B \\sim C51B-C26B \\sim C51A-C26A \\sim C54A-C46A \\sim C54F-C46F
\\sim C51F-C26F \\sim C54E-
 C46E \\sim C51E-C26E \\sim C51C-C26C \\sim C54C-C46C \\sim C51D-C26D \\sim
C54D-C46D
 with sigma of 0.001
 N42C-C46C \\sim N22A-C26A \\sim N22B-C26B \\sim N42G-C46G \\sim N62G-C66G
\\sim N22G-C26G \\sim N42D-
 C46D \\sim N22E-C26E \\sim N42E-C46E \\sim N22F-C26F \\sim N42F-C46F \\sim
N22D-C26D \\sim N42H-C46H ~
 N62H-C66H \\sim N22H-C26H \\sim N22C-C26C \\sim N42B-C46B
 with sigma of 0.001
 N62G-C66G \\sim N22G-C26G \\sim N42G-C46G \\sim N22B-C26B \\sim N42A-C46A
\\sim N22A-C26A \\sim N42C-
 C46C \\sim N22C-C26C \\sim N42B-C46B \\sim N22H-C26H \\sim N42D-C46D \\sim
N42E-C46E \\sim N22F-C26F ~
 N22D-C26D \\sim N42F-C46F \\sim N42H-C46H \\sim N62H-C66H \\sim N22E-C26E
 with sigma of 0.001
 C54C-C46C \\sim C51C-C26C \\sim C51A-C26A \\sim C54A-C46A \\sim C54B-C46B
\\sim C51B-C26B \\sim C54D-
 C46D \\sim C51D-C26D \\sim C51F-C26F \\sim C54F-C46F \\sim C51E-C26E \\sim
C54E-C46E
 with sigma of 0.001
3. Restrained planarity
 N11C, C12C, C13C, C14C, C15C, C16C
 with sigma of 0.1
 N31C, C32C, C33C, C34C, C35C, C36C
 with sigma of 0.1
 N11D, C12D, C13D, C14D, C15D, C16D
 with sigma of 0.1
 N31D, C32D, C33D, C34D, C35D, C36D
 with sigma of 0.1
 N11E, C12E, C13E, C14E, C15E, C16E
 with sigma of 0.1
 N31E, C32E, C33E, C34E, C35E, C36E
 with sigma of 0.1
 N11F, C12F, C13F, C14F, C15F, C16F
 with sigma of 0.1
 N31F, C32F, C33F, C34F, C35F, C36F
 with sigma of 0.1
 N11G, C12G, C13G, C14G, C15G, C16G
 with sigma of 0.1
 N51G, C52G, C53G, C54G, C55G, C56G
 with sigma of 0.1
 N11H, C12H, C13H, C14H, C15H, C16H
 with sigma of 0.1
 N11B, C12B, C13B, C14B, C15B, C16B
 with sigma of 0.1
 N31G, C32G, C33G, C34G, C35G, C36G
 with sigma of 0.1
 N41A, N42A, C43A, C44A, C45A
 with sigma of 0.1
 N21B, N22B, C23B, C24B, C25B
 with sigma of 0.1
 N41B, N42B, C43B, C44B, C45B
 with sigma of 0.1
 N21C, N22C, C23C, C24C, C25C
 with sigma of 0.1
 N41C, N42C, C43C, C44C, C45C
 with sigma of 0.1
 N21D, N22D, C23D, C24D, C25D
 with sigma of 0.1
 N41D, N42D, C43D, C44D, C45D
 with sigma of 0.1
 N21E, N22E, C23E, C24E, C25E
 with sigma of 0.1
 N41E, N42E, C43E, C44E, C45E
 with sigma of 0.1
 N21F, N22F, C23F, C24F, C25F
 with sigma of 0.1
 N41F, N42F, C43F, C44F, C45F
 with sigma of 0.1
 N21G, N22G, C23G, C24G, C25G
 with sigma of 0.1
 N41G, N42G, C43G, C44G, C45G
 with sigma of 0.1
 N61G, N62G, C63G, C64G, C65G
 with sigma of 0.1
 N21H, N22H, C23H, C24H, C25H
 with sigma of 0.1
 N51H, C52H, C53H, C54H, C55H, C56H
 with sigma of 0.1
 N61H, N62H, C63H, C64H, C65H
 with sigma of 0.1
 N31H, C32H, C33H, C34H, C35H, C36H
 with sigma of 0.1
 N41H, N42H, C43H, C44H, C45H
 with sigma of 0.1
 N21A, N22A, C23A, C24A, C25A
 with sigma of 0.1
 N11A, C12A, C13A, C14A, C15A, C16A
 with sigma of 0.1
 C62A, C63A, C64A, C55A, C56A, C61A
 with sigma of 0.1
 C55D, C56D, C61D, C62D, C63D, C64D
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C12A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C23A \\sim C24A \\sim
C25A \\sim C26A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim
C43A \\sim C44A \\sim C45A \\sim C46A \\sim C51A \\sim C52A \\sim C53A \\sim
C54A \\sim C55A \\sim C56A \\sim C61A \\sim C62A \\sim C63A \\sim C64A \\sim
C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim C23B \\sim C24B \\sim
C25B \\sim C26B \\sim C32B \\sim C33B \\sim C34B \\sim C35B \\sim C36B \\sim
C43B \\sim C44B \\sim C45B \\sim C46B \\sim C51B \\sim C52B \\sim C53B \\sim
C54B \\sim C55B \\sim C56B \\sim C61B \\sim C62B \\sim C63B \\sim C64B \\sim
C12C \\sim C13C \\sim C14C \\sim C15C \\sim C16C \\sim C23C \\sim C24C \\sim
C25C \\sim C26C \\sim C32C \\sim C33C \\sim C34C \\sim C35C \\sim C36C \\sim
C43C \\sim C44C \\sim C45C \\sim C46C \\sim C51C \\sim C52C \\sim C53C \\sim
C54C \\sim C55C \\sim C56C \\sim C61C \\sim C62C \\sim C63C \\sim C64C \\sim
C12D \\sim C13D \\sim C14D \\sim C15D \\sim C16D \\sim C23D \\sim C24D \\sim
C25D \\sim C26D \\sim C32D \\sim C33D \\sim C34D \\sim C35D \\sim C36D \\sim
C43D \\sim C44D \\sim C45D \\sim C46D \\sim C51D \\sim C52D \\sim C53D \\sim
C54D \\sim C55D \\sim C56D \\sim C61D \\sim C62D \\sim C63D \\sim C64D \\sim
C12E \\sim C13E \\sim C14E \\sim C15E \\sim C16E \\sim C23E \\sim C24E \\sim
C25E \\sim C26E \\sim C32E \\sim C33E \\sim C34E \\sim C35E \\sim C36E \\sim
C43E \\sim C44E \\sim C45E \\sim C46E \\sim C51E \\sim C52E \\sim C53E \\sim
C54E \\sim C55E \\sim C56E \\sim C61E \\sim C62E \\sim C63E \\sim C64E \\sim
C12F \\sim C13F \\sim C14F \\sim C15F \\sim C16F \\sim C23F \\sim C24F \\sim
C25F \\sim C26F \\sim C32F \\sim C33F \\sim C34F \\sim C35F \\sim C36F \\sim
C43F \\sim C44F \\sim C45F \\sim C46F \\sim C51F \\sim C52F \\sim C53F \\sim
C54F \\sim C55F \\sim C56F \\sim C61F \\sim C62F \\sim C63F \\sim C64F \\sim
C12G \\sim C13G \\sim C14G \\sim C15G \\sim C16G \\sim C23G \\sim C24G \\sim
C25G \\sim C26G \\sim C32G \\sim C33G \\sim C34G \\sim C35G \\sim C36G \\sim
C43G \\sim C44G \\sim C45G \\sim C46G \\sim C52G \\sim C53G \\sim C54G \\sim
C55G \\sim C56G \\sim C63G \\sim C64G \\sim C65G \\sim C66G \\sim C71G \\sim
C72G \\sim C73G \\sim C74G \\sim C75G \\sim C76G \\sim C77G \\sim C78G \\sim
C79G \\sim C12H \\sim C13H \\sim C14H \\sim C15H \\sim C16H \\sim C23H \\sim
C24H \\sim C25H \\sim C26H \\sim C32H \\sim C33H \\sim C34H \\sim C35H \\sim
C36H \\sim C43H \\sim C44H \\sim C45H \\sim C46H \\sim C52H \\sim C53H \\sim
C54H \\sim C55H \\sim C56H \\sim C63H \\sim C64H \\sim C65H \\sim C66H \\sim
C71H \\sim C72H \\sim C73H \\sim C74H \\sim C75H \\sim C76H \\sim C77H \\sim
C78H \\sim C79H \\sim N11A \\sim N21A \\sim N22A \\sim N31A \\sim N41A \\sim
N42A \\sim N11B \\sim N21B \\sim N22B \\sim N31B \\sim N41B \\sim N42B \\sim
N11C \\sim N21C \\sim N22C \\sim N31C \\sim N41C \\sim N42C \\sim N11D \\sim
N21D \\sim N22D \\sim N31D \\sim N41D \\sim N42D \\sim N11E \\sim N21E \\sim
N22E \\sim N31E \\sim N41E \\sim N42E \\sim N11F \\sim N21F \\sim N22F \\sim
N31F \\sim N41F \\sim N42F \\sim N11G \\sim N21G \\sim N22G \\sim N31G \\sim
N41G \\sim N42G \\sim N51G \\sim N61G \\sim N62G \\sim N11H \\sim N21H \\sim
N22H \\sim N31H \\sim N41H \\sim N42H \\sim N51H \\sim N61H \\sim N62H \\sim
O1W \\sim O1X \\sim O2W \\sim O3W \\sim O4W \\sim O5W \\sim O6W \\sim B11 \\sim
B21 \\sim B31 \\sim B41 \\sim B51 \\sim B61 \\sim B71 \\sim B81 \\sim F12 \\sim
F13 \\sim F14 \\sim F15 \\sim F22 \\sim F23 \\sim F24 \\sim F25 \\sim F32 \\sim
F33 \\sim F34 \\sim F35 \\sim F42 \\sim F43 \\sim F44 \\sim F45 \\sim F52 \\sim
F53 \\sim F54 \\sim F55 \\sim F62 \\sim F63 \\sim F64 \\sim F65 \\sim F72 \\sim
F73 \\sim F75 \\sim F74 \\sim F82 \\sim F83 \\sim F84 \\sim F85: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C12A, C13A, C14A, C15A, C16A, C23A, C24A, C25A, C26A, C32A, C33A, C34A, C35A,
 C36A, C43A, C44A, C45A, C46A, C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A,
 C63A, C64A, C12B, C13B, C14B, C15B, C16B, C23B, C24B, C25B, C26B, C32B, C33B,
 C34B, C35B, C36B, C43B, C44B, C45B, C46B, C51B, C52B, C53B, C54B, C55B, C56B,
 C61B, C62B, C63B, C64B, C12C, C13C, C14C, C15C, C16C, C23C, C24C, C25C, C26C,
 C32C, C33C, C34C, C35C, C36C, C43C, C44C, C45C, C46C, C51C, C52C, C53C, C54C,
 C55C, C56C, C61C, C62C, C63C, C64C, C12D, C13D, C14D, C15D, C16D, C23D, C24D,
 C25D, C26D, C32D, C33D, C34D, C35D, C36D, C43D, C44D, C45D, C46D, C51D, C52D,
 C53D, C54D, C55D, C56D, C61D, C62D, C63D, C64D, C12E, C13E, C14E, C15E, C16E,
 C23E, C24E, C25E, C26E, C32E, C33E, C34E, C35E, C36E, C43E, C44E, C45E, C46E,
 C51E, C52E, C53E, C54E, C55E, C56E, C61E, C62E, C63E, C64E, C12F, C13F, C14F,
 C15F, C16F, C23F, C24F, C25F, C26F, C32F, C33F, C34F, C35F, C36F, C43F, C44F,
 C45F, C46F, C51F, C52F, C53F, C54F, C55F, C56F, C61F, C62F, C63F, C64F, C12G,
 C13G, C14G, C15G, C16G, C23G, C24G, C25G, C26G, C32G, C33G, C34G, C35G, C36G,
 C43G, C44G, C45G, C46G, C52G, C53G, C54G, C55G, C56G, C63G, C64G, C65G, C66G,
 C71G, C72G, C73G, C74G, C75G, C76G, C77G, C78G, C79G, C12H, C13H, C14H, C15H,
 C16H, C23H, C24H, C25H, C26H, C32H, C33H, C34H, C35H, C36H, C43H, C44H, C45H,
 C46H, C52H, C53H, C54H, C55H, C56H, C63H, C64H, C65H, C66H, C71H, C72H, C73H,
 C74H, C75H, C76H, C77H, C78H, C79H, N11A, N21A, N22A, N31A, N41A, N42A, N11B,
 N21B, N22B, N31B, N41B, N42B, N11C, N21C, N22C, N31C, N41C, N42C, N11D, N21D,
 N22D, N31D, N41D, N42D, N11E, N21E, N22E, N31E, N41E, N42E, N11F, N21F, N22F,
 N31F, N41F, N42F, N11G, N21G, N22G, N31G, N41G, N42G, N51G, N61G, N62G, N11H,
 N21H, N22H, N31H, N41H, N42H, N51H, N61H, N62H, O1W, O1X, O2W, O3W, O4W, O5W,
 O6W, B11, B21, B31, B41, B51, B61, B71, B81, F12, F13, F14, F15, F22, F23, F24,
  F25, F32, F33, F34, F35, F42, F43, F44, F45, F52, F53, F54, F55, F62, F63,
 F64, F65, F72, F73, F75, F74, F82, F83, F84, F85
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N31A, C32A, C33A, C34A, C35A, C36A, N41A, N42A, C43A, C44A, C45A}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N11B, C12B, C13B, C14B, C15B, C16B, N21B, N22B, C23B, C24B, C25B}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N31B, C32B, C33B, C34B, C35B, C36B, N41B, N42B, C43B, C44B, C45B}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
{C54A, C53A, C52A, C51A, C56A, C55A, C64A, C63A, C62A, C61A} sigma for 1-2:
0.02, 1-3: 0.04
as
{C51B, C52B, C53B, C54B, C55B, C56B, C61B, C62B, C63B, C64B}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N11C, C12C, C13C, C14C, C15C, C16C, N21C, N22C, C23C, C24C, C25C}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N31C, C32C, C33C, C34C, C35C, C36C, N41C, N42C, C43C, C44C, C45C}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
{C54A, C53A, C52A, C51A, C56A, C55A, C64A, C63A, C62A, C61A} sigma for 1-2:
0.02, 1-3: 0.04
as
{C51C, C52C, C53C, C54C, C55C, C56C, C61C, C62C, C63C, C64C}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N11D, C12D, C13D, C14D, C15D, C16D, N21D, N22D, C23D, C24D, C25D}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N31D, C32D, C33D, C34D, C35D, C36D, N41D, N42D, C43D, C44D, C45D}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
{C54A, C53A, C52A, C51A, C56A, C55A, C64A, C63A, C62A, C61A} sigma for 1-2:
0.02, 1-3: 0.04
as
{C51D, C52D, C53D, C54D, C55D, C56D, C61D, C62D, C63D, C64D}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N11E, C12E, C13E, C14E, C15E, C16E, N21E, N22E, C23E, C24E, C25E}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N31E, C32E, C33E, C34E, C35E, C36E, N41E, N42E, C43E, C44E, C45E}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
{C54A, C53A, C52A, C51A, C56A, C55A, C64A, C63A, C62A, C61A} sigma for 1-2:
0.02, 1-3: 0.04
as
{C51E, C52E, C53E, C54E, C55E, C56E, C61E, C62E, C63E, C64E}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N11F, C12F, C13F, C14F, C15F, C16F, N21F, N22F, C23F, C24F, C25F}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N31F, C32F, C33F, C34F, C35F, C36F, N41F, N42F, C43F, C44F, C45F}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
{C54A, C53A, C52A, C51A, C56A, C55A, C64A, C63A, C62A, C61A} sigma for 1-2:
0.02, 1-3: 0.04
as
{C51F, C52F, C53F, C54F, C55F, C56F, C61F, C62F, C63F, C64F}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N11G, C12G, C13G, C14G, C15G, C16G, N21G, N22G, C23G, C24G, C25G}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N31G, C32G, C33G, C34G, C35G, C36G, N41G, N42G, C43G, C44G, C45G}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N51G, C52G, C53G, C54G, C55G, C56G, N61G, N62G, C63G, C64G, C65G}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N11H, C12H, C13H, C14H, C15H, C16H, N21H, N22H, C23H, C24H, C25H}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N31H, C32H, C33H, C34H, C35H, C36H, N41H, N42H, C43H, C44H, C45H}
{N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A} sigma for
1-2: 0.02, 1-3: 0.04
as
{N51H, C52H, C53H, C54H, C55H, C56H, N61H, N62H, C63H, C64H, C65H}
{C71G, C72G, C73G, C74G, C75G, C76G, C77G, C78G, C79G} sigma for 1-2: 0.02,
1-3: 0.04
{C73G, C72G, C71G, C76G, C75G, C74G, C77G, C79G, C78G} sigma for 1-2: 0.02,
1-3: 0.04
{C75G, C76G, C71G, C72G, C73G, C74G, C79G, C77G, C78G} sigma for 1-2: 0.02,
1-3: 0.04
{C71G, C76G, C75G, C74G, C73G, C72G, C79G, C78G, C77G} sigma for 1-2: 0.02,
1-3: 0.04
{C73G, C74G, C75G, C76G, C71G, C72G, C78G, C79G, C77G} sigma for 1-2: 0.02,
1-3: 0.04
{C75G, C74G, C73G, C72G, C71G, C76G, C78G, C77G, C79G} sigma for 1-2: 0.02,
1-3: 0.04
as
{C71H, C72H, C73H, C74H, C75H, C76H, C77H, C78H, C79H}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F15, F14, F13, F12} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F14, F13, F12, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F13, F12, F15, F14} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F12, F15, F14, F13} sigma for 1-2: 0.02, 1-3: 0.04
as
{B21, F22, F23, F24, F25}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F15, F14, F13, F12} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F14, F13, F12, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F13, F12, F15, F14} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F12, F15, F14, F13} sigma for 1-2: 0.02, 1-3: 0.04
as
{B31, F32, F33, F34, F35}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F15, F14, F13, F12} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F14, F13, F12, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F13, F12, F15, F14} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F12, F15, F14, F13} sigma for 1-2: 0.02, 1-3: 0.04
as
{B41, F42, F43, F44, F45}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F15, F14, F13, F12} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F14, F13, F12, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F13, F12, F15, F14} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F12, F15, F14, F13} sigma for 1-2: 0.02, 1-3: 0.04
as
{B51, F52, F53, F54, F55}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F15, F14, F13, F12} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F14, F13, F12, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F13, F12, F15, F14} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F12, F15, F14, F13} sigma for 1-2: 0.02, 1-3: 0.04
as
{B61, F62, F63, F64, F65}
{B11, F13, F12, F15, F14} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F15, F14, F13, F12} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F14, F13, F12, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F12, F15, F14, F13} sigma for 1-2: 0.02, 1-3: 0.04
as
{B71, F72, F73, F75, F74}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F15, F14, F13, F12} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F14, F13, F12, F15} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F13, F12, F15, F14} sigma for 1-2: 0.02, 1-3: 0.04
{B11, F12, F15, F14, F13} sigma for 1-2: 0.02, 1-3: 0.04
as
{B81, F82, F83, F84, F85}
7. Others
 Sof(B61)=Sof(F62)=Sof(F63)=Sof(F64)=Sof(F65)=FVAR(1)
 Sof(B21)=Sof(F22)=Sof(F23)=Sof(F24)=Sof(F25)=FVAR(2)
 Sof(B51)=Sof(F52)=Sof(F53)=Sof(F54)=Sof(F55)=FVAR(3)
 Sof(B81)=Sof(F82)=Sof(F83)=Sof(F84)=Sof(F85)=1-FVAR(4)
 Sof(B11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=FVAR(4)
 Sof(B71)=Sof(F72)=Sof(F73)=Sof(F75)=Sof(F74)=FVAR(5)
 Sof(B41)=Sof(F42)=Sof(F43)=Sof(F44)=Sof(F45)=FVAR(6)
 Sof(B31)=Sof(F32)=Sof(F33)=Sof(F34)=Sof(F35)=FVAR(7)
 Sof(O1X)=1-FVAR(8)
 Sof(O1W)=FVAR(8)
 Fixed Uiso: B11(0.25) F12(0.25) F13(0.25) F14(0.25) F15(0.25) B31(0.25)
 F32(0.25) F33(0.25) F34(0.25) F35(0.25) B41(0.25) F42(0.25) F43(0.25)
 F44(0.25) F45(0.25) B71(0.25) F72(0.25) F73(0.25) F75(0.25) F74(0.25)
 B81(0.25) F82(0.25) F83(0.25) F84(0.25) F85(0.25) O1W(0.2) O1X(0.2) O2W(0.2)
 O3W(0.2) O4W(0.2) O5W(0.2) O6W(0.2)
8.a Secondary CH2 refined with riding coordinates:
 C26A(H26A,H26B), C46A(H46A,H46B), C26B(H26C,H26D), C46B(H46C,H46D), C26C(H26E,
 H26F), C46C(H46E,H46F), C26D(H26G,H26H), C46D(H46G,H46H), C26E(H26I,H26J),
 C46E(H46I,H46J), C26F(H26K,H26L), C46F(H46K,H46L), C26G(H26M,H26N), C46G(H46M,
 H46N), C66G(H66A,H66B), C26H(H26O,H26P), C46H(H46O,H46P), C66H(H66C,H66D)
8.b Me refined with riding coordinates:
 C77G(H77A,H77B,H77C), C78G(H78A,H78B,H78C), C79G(H79A,H79B,H79C), C77H(H77D,
 H77E,H77F), C78H(H78D,H78E,H78F), C79H(H79D,H79E,H79F)
8.c Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C23A(H23A), C24A(H24A),
 C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C43A(H43A), C44A(H44A),
 C52A(H52A), C53A(H53A), C61A(H61A), C62A(H62A), C63A(H63A), C64A(H64A),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C23B(H23B), C24B(H24B),
 C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B), C43B(H43B), C44B(H44B),
 C52B(H52B), C53B(H53B), C61B(H61B), C62B(H62B), C63B(H63B), C64B(H64B),
 C13C(H13C), C14C(H14C), C15C(H15C), C16C(H16C), C23C(H23C), C24C(H24C),
 C33C(H33C), C34C(H34C), C35C(H35C), C36C(H36C), C43C(H43C), C44C(H44C),
 C52C(H52C), C53C(H53C), C61C(H61C), C62C(H62C), C63C(H63C), C64C(H64C),
 C13D(H13D), C14D(H14D), C15D(H15D), C16D(H16D), C23D(H23D), C24D(H24D),
 C33D(H33D), C34D(H34D), C35D(H35D), C36D(H36D), C43D(H43D), C44D(H44D),
 C52D(H52D), C53D(H53D), C61D(H61D), C62D(H62D), C63D(H63D), C64D(H64D),
 C13E(H13E), C14E(H14E), C15E(H15E), C16E(H16E), C23E(H23E), C24E(H24E),
 C33E(H33E), C34E(H34E), C35E(H35E), C36E(H36E), C43E(H43E), C44E(H44E),
 C52E(H52E), C53E(H53E), C61E(H61E), C62E(H62E), C63E(H63E), C64E(H64E),
 C13F(H13F), C14F(H14F), C15F(H15F), C16F(H16F), C23F(H23F), C24F(H24F),
 C33F(H33F), C34F(H34F), C35F(H35F), C36F(H36F), C43F(H43F), C44F(H44F),
 C52F(H52F), C53F(H53F), C61F(H61F), C62F(H62F), C63F(H63F), C64F(H64F),
 C13G(H13G), C14G(H14G), C15G(H15G), C16G(H16G), C23G(H23G), C24G(H24G),
 C33G(H33G), C34G(H34G), C35G(H35G), C36G(H36G), C43G(H43G), C44G(H44G),
 C53G(H53G), C54G(H54G), C55G(H55G), C56G(H56G), C63G(H63G), C64G(H64G),
 C13H(H13H), C14H(H14H), C15H(H15H), C16H(H16H), C23H(H23H), C24H(H24H),
 C33H(H33H), C34H(H34H), C35H(H35H), C36H(H36H), C43H(H43H), C44H(H44H),
 C53H(H53H), C54H(H54H), C55H(H55H), C56H(H56H), C63H(H63H), C64H(H64H)
;
_shelx_res_checksum              31980
_shelx_fab_checksum              35277
_olex2_exptl_crystal_mounting_method
'mounted on a loop of keratinized protein fibre in Fomblin oil'
_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 1.390
_oxdiff_exptl_absorpt_empirical_full_min 0.768