Orthogonal binding and displacement of different guest types using a coordination cage host with cavity-based and surface-based binding sites
Ludden, Michael D.; Taylor, Christopher G. P.; Ward, Michael D.; Chemical Science  (2021) –; doi:10.1039/D1SC04272F

data_1564491
_publ_section_title
;
 Orthogonal binding and displacement of different guest types using a
 coordination cage host with cavity-based and surface-based binding sites
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04272F
_journal_year                    2021
_chemical_formula_moiety
'C336 H264 Co8 N72, 13.6(I), C H3 O, C10 H9 N O2, 2.4[I], 36[CH3OH]'
_chemical_formula_sum            'C347 H276 Co8 I13.6 N73 O3'
_chemical_formula_weight         7713.67
_chemical_name_systematic        H?MAC?I
_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             2021-05-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-01 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.9277(2)
_cell_length_b                   30.0730(2)
_cell_length_c                   40.7670(3)
_cell_measurement_reflns_used    93500
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.9900
_cell_measurement_theta_min      1.6260
_cell_volume                     40177.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'GDA - generic data acquisition software'
_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_temperature      100
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 180.00   0.20    0.20   0.00   0.00   0.00    --   900
  2  \w   -145.00  25.00   0.20    0.20    --   30.00   0.00   0.00  850
  3  \w   -145.00  25.00   0.20    0.20    --   30.00   0.00 120.00  850
  4  \w   -145.00  25.00   0.20    0.20    --   30.00   0.00 240.00  850
;
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0189324000
_diffrn_orient_matrix_UB_12      0.0098731000
_diffrn_orient_matrix_UB_13      -0.0023069000
_diffrn_orient_matrix_UB_21      0.0025707000
_diffrn_orient_matrix_UB_22      0.0082363000
_diffrn_orient_matrix_UB_23      0.0158300000
_diffrn_orient_matrix_UB_31      0.0087621000
_diffrn_orient_matrix_UB_32      0.0189602000
_diffrn_orient_matrix_UB_33      -0.0056890000
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            352450
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         29.947
_diffrn_reflns_theta_min         1.620
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71718
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             15319
_exptl_crystal_preparation
'Crystal was soaked in methanolic mother liquor (from the solvothermal crystals growth). A saturated methanolic solution of tetra-butyl ammonium iodide was added along with a saturated methanolic solution of 7-amino-4-methyl coumarin and left for around 24 hours. Crystals were transferred to Fomblin oil before a crystal was mounted on a MiteGen Microloop and flash frozen under liquid nitrogen for storage.'
_exptl_crystal_recrystallization_method
'slow cooling from solvothermal synthesis'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.672
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2152
_refine_ls_number_reflns         64020
_refine_ls_number_restraints     7039
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1166P)^2^+28.2886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2022
_refine_ls_wR_factor_ref         0.2289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                41185
_reflns_number_total             64020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04272f2.cif
_cod_data_source_block           dmwms-2v1-246_mac_i_rf2
_cod_original_formula_sum        'C347 H276 Co8 I13.60 N73 O3'
_cod_database_code               1564491
_smtbx_masks_special_details
;
A solvent mask was calculated and 3090 electrons were 
found in a volume of 11120 A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.42[I], 36[CH3OH] per Formula Unit 
which account for 3105 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C356 H280 N74 O4 Co8 I16 '
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.902
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O11G-C12G
 1.378 with sigma of 0.02
 O21G-C12G
 1.211 with sigma of 0.01
 C17G-C18G
 1.394 with sigma of 0.01
 N23G-C18G
 1.377 with sigma of 0.01
 C20G-C19G
 1.383 with sigma of 0.01
 O11G-C16G
 1.38 with sigma of 0.01
 C19G-C18G
 1.395 with sigma of 0.01
 C13G-C14G
 1.347 with sigma of 0.01
 C15G-C20G
 1.395 with sigma of 0.01
 C14G-C15G
 1.449 with sigma of 0.01
 C14G-C22G
 1.501 with sigma of 0.01
 C13G-C12G
 1.44 with sigma of 0.01
 C15G-C16G
 1.402 with sigma of 0.01
 C16G-C17G
 1.384 with sigma of 0.01
 O13S-C14S = C12S-O11S
 1.406 with sigma of 0.02
 O21G-C13G
 2.36 with sigma of 0.02
 O11G-O21G
 2.19 with sigma of 0.02
3. Restrained planarity
 N23G, C18G, C17G, C19G
 with sigma of 0.1
 C22G, C14G, C13G, C15G
 with sigma of 0.1
 C16G, C15G, C14G, C13G, C12G, O11G
 with sigma of 0.1
 C17G, C18G, C19G, C20G, C15G, C16G
 with sigma of 0.1
 O21G, C12G, C13G, O11G
 with sigma of 0.1
 C16G, O11G, C12G, O21G, C13G, C14G
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
I1 \\sim I5A \\sim I10 \\sim I2 \\sim I3A \\sim I3 \\sim I11 \\sim I4 \\sim I6A
\\sim I5 \\sim I6 \\sim I12 \\sim I7 \\sim I8: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim N21A \\sim
N22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim N31A \\sim C32A \\sim
C33A \\sim C34A \\sim C35A \\sim C36A \\sim N41A \\sim N42A \\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 N11B \\sim
C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim N21B \\sim N22B \\sim
C23B \\sim C24B \\sim C25B \\sim C26B \\sim N31B \\sim C32B \\sim C33B \\sim
C34B \\sim C35B \\sim C36B \\sim N41B \\sim N42B \\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 N11C \\sim C12C \\sim
C13C \\sim C14C \\sim C15C \\sim C16C \\sim N21C \\sim N22C \\sim C23C \\sim
C24C \\sim C25C \\sim C26C \\sim N31C \\sim C32C \\sim C33C \\sim C34C \\sim
C35C \\sim C36C \\sim N41C \\sim N42C \\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 N11D \\sim C12D \\sim C13D \\sim
C14D \\sim C15D \\sim C16D \\sim N21D \\sim N22D \\sim C23D \\sim C24D \\sim
C25D \\sim C26D \\sim N31D \\sim C32D \\sim C33D \\sim C34D \\sim C35D \\sim
C36D \\sim N41D \\sim N42D \\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 N11E \\sim C12E \\sim C13E \\sim C14E \\sim
C15E \\sim C16E \\sim N21E \\sim N22E \\sim C23E \\sim C24E \\sim C25E \\sim
C26E \\sim N31E \\sim C32E \\sim C33E \\sim C34E \\sim C35E \\sim C36E \\sim
N41E \\sim N42E \\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 N11F \\sim C12F \\sim C13F \\sim C14F \\sim C15F \\sim
C16F \\sim N21F \\sim N22F \\sim C23F \\sim C24F \\sim C25F \\sim C26F \\sim
N31F \\sim C32F \\sim C33F \\sim C34F \\sim C35F \\sim C36F \\sim N41F \\sim
N42F \\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 I1 \\sim I2 \\sim I3 \\sim I4 \\sim I5 \\sim I6 \\sim I7 \\sim I8
\\sim I5A \\sim I6A \\sim I3A \\sim I10 \\sim I12 \\sim I11 \\sim O11S \\sim
C12S \\sim O13S \\sim C14S \\sim O11G \\sim C12G \\sim C13G \\sim C14G \\sim
C15G \\sim C16G \\sim C17G \\sim C18G \\sim C19G \\sim C20G \\sim O21G \\sim
C22G \\sim N23G: within 2.5A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2.5A
Uanis(I1) \\sim Ueq, Uanis(I5A) \\sim Ueq, Uanis(I10) \\sim Ueq, Uanis(I2)
\\sim Ueq, Uanis(I3A) \\sim Ueq, Uanis(I3) \\sim Ueq, Uanis(I11) \\sim Ueq,
Uanis(I4) \\sim Ueq, Uanis(I6A) \\sim Ueq, Uanis(I5) \\sim Ueq, Uanis(I6) \\sim
Ueq, Uanis(I12) \\sim Ueq, Uanis(I7) \\sim Ueq, Uanis(I8) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 N11A, C12A, C13A, C14A, C15A, C16A, N21A, N22A, C23A, C24A, C25A, C26A, N31A,
 C32A, C33A, C34A, C35A, C36A, N41A, N42A, C43A, C44A, C45A, C46A, C51A, C52A,
 C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A, N11B, C12B, C13B, C14B, C15B,
 C16B, N21B, N22B, C23B, C24B, C25B, C26B, N31B, C32B, C33B, C34B, C35B, C36B,
 N41B, N42B, C43B, C44B, C45B, C46B, C51B, C52B, C53B, C54B, C55B, C56B, C61B,
 C62B, C63B, C64B, N11C, C12C, C13C, C14C, C15C, C16C, N21C, N22C, C23C, C24C,
 C25C, C26C, N31C, C32C, C33C, C34C, C35C, C36C, N41C, N42C, C43C, C44C, C45C,
 C46C, C51C, C52C, C53C, C54C, C55C, C56C, C61C, C62C, C63C, C64C, N11D, C12D,
 C13D, C14D, C15D, C16D, N21D, N22D, C23D, C24D, C25D, C26D, N31D, C32D, C33D,
 C34D, C35D, C36D, N41D, N42D, C43D, C44D, C45D, C46D, C51D, C52D, C53D, C54D,
 C55D, C56D, C61D, C62D, C63D, C64D, N11E, C12E, C13E, C14E, C15E, C16E, N21E,
 N22E, C23E, C24E, C25E, C26E, N31E, C32E, C33E, C34E, C35E, C36E, N41E, N42E,
 C43E, C44E, C45E, C46E, C51E, C52E, C53E, C54E, C55E, C56E, C61E, C62E, C63E,
 C64E, N11F, C12F, C13F, C14F, C15F, C16F, N21F, N22F, C23F, C24F, C25F, C26F,
 N31F, C32F, C33F, C34F, C35F, C36F, N41F, N42F, C43F, C44F, C45F, C46F, C51F,
 C52F, C53F, C54F, C55F, C56F, C61F, C62F, C63F, C64F, I1, I2, I3, I4, I5, I6,
 I7, I8, I5A, I6A, I3A, I10, I12, I11, O11S, C12S, O13S, C14S, O11G, C12G, C13G,
  C14G, C15G, C16G, C17G, C18G, C19G, C20G, O21G, C22G, N23G
 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} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31A, C32A, C33A, C34A, C35A, C36A}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41A, N42A, C43A, C44A, C45A}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11B, C12B, C13B, C14B, C15B, C16B}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31B, C32B, C33B, C34B, C35B, C36B}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{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
as in
{C51B, C52B, C53B, C54B, C55B, C56B, C61B, C62B, C63B, C64B}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11C, C12C, C13C, C14C, C15C, C16C}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21C, N22C, C23C, C24C, C25C}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31C, C32C, C33C, C34C, C35C, C36C}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{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
as in
{C51C, C52C, C53C, C54C, C55C, C56C, C61C, C62C, C63C, C64C}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11D, C12D, C13D, C14D, C15D, C16D}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21D, N22D, C23D, C24D, C25D}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31D, C32D, C33D, C34D, C35D, C36D}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{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
as in
{C51D, C52D, C53D, C54D, C55D, C56D, C61D, C62D, C63D, C64D}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11E, C12E, C13E, C14E, C15E, C16E}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21E, N22E, C23E, C24E, C25E}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31E, C32E, C33E, C34E, C35E, C36E}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{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
as in
{C51E, C52E, C53E, C54E, C55E, C56E, C61E, C62E, C63E, C64E}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11F, C12F, C13F, C14F, C15F, C16F}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21F, N22F, C23F, C24F, C25F}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31F, C32F, C33F, C34F, C35F, C36F}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{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
as in
{C51F, C52F, C53F, C54F, C55F, C56F, C61F, C62F, C63F, C64F}
7. Others
 Fixed Sof: I3(0.4) I4(0.83) I5(0.4) I6(0.5) I7(0.42) I8(0.55) I5A(0.25)
 I6A(0.25) I3A(0.35) I10(0.35) I12(0.25) I11(0.25) O11S(0.25) C12S(0.25)
 H12A(0.25) H12B(0.25) H12C(0.25) O13S(0.25) C14S(0.25) H14G(0.25) H14H(0.25)
 H14I(0.25) O11G(0.5) C12G(0.5) C13G(0.5) H13G(0.5) C14G(0.5) C15G(0.5)
 C16G(0.5) C17G(0.5) H17G(0.5) C18G(0.5) C19G(0.5) H19G(0.5) C20G(0.5)
 H20G(0.5) O21G(0.5) C22G(0.5) H22A(0.5) H22B(0.5) H22C(0.5) N23G(0.5)
 H23G(0.5) H23H(0.5)
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)
8.b 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), C54A(H54A), C61A(H61A), C62A(H62A), C63A(H63A),
 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), C54B(H54B), C61B(H61B), C62B(H62B), C63B(H63B),
 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), C54C(H54C), C61C(H61C), C62C(H62C), C63C(H63C),
 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), C54D(H54D), C61D(H61D), C62D(H62D), C63D(H63D),
 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), C54E(H54E), C61E(H61E), C62E(H62E), C63E(H63E),
 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), C54F(H54F), C61F(H61F), C62F(H62F), C63F(H63F),
 C13G(H13G), C17G(H17G), C19G(H19G), C20G(H20G)
8.c X=CH2 refined with riding coordinates:
 N23G(H23G,H23H)
8.d Idealised Me refined with riding coordinates:
 C12S(H12A,H12B,H12C), C14S(H14G,H14H,H14I), C22G(H22A,H22B,H22C)
;
_shelx_res_checksum              71080
_shelx_hkl_checksum              18958
_shelx_fab_checksum              59870
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.768