Disentangling contributions to guest binding inside a coordination cage host: analysis of a set of isomeric guests with differing polarities
Mozaceanu, Cristina; Solea, Atena B.; Taylor, Christopher; Sudittapong, Burin; Ward, Michael D.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02623F

data_7711278
_publ_section_title
;
 Disentangling contributions to guest binding inside a coordination cage
 host: analysis of a set of isomeric guests with differing polarities
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02623F
_journal_year                    2022
_chemical_formula_moiety
'C336 H264 Co8 N72, 2(C8 H4 N2), 12.5(B F4), 0.5(Cl), 3[BF4], 33[CH3OH]'
_chemical_formula_sum            'C385 H404 B15.5 Cl0.5 Co8 F62 N76 O33'
_chemical_formula_weight         8458.54
_chemical_name_systematic        DMWMS_2v2_340_B20
_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             2021-04-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-08-04 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.20586(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.92731(7)
_cell_length_b                   30.26746(6)
_cell_length_c                   39.97143(8)
_cell_measurement_reflns_used    139837
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.811
_cell_measurement_theta_min      0.977
_cell_volume                     39603.12(14)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 3.1.2-gc563cd297-release'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 3.1.2-gc563cd297-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.7.90-g7281562a-dials-3.1 (Winter, G., 2010)
;
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            338129
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         29.947
_diffrn_reflns_theta_min         0.985
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.1.003: AIMLESS, version 0.7.4 : 13/12/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_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    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             17480
_exptl_crystal_preparation
'Crystal was soaked in methanolic mother liquor (from the solvothermal crystals growth). A solution of 1,2-dicyanobenzene 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
'Solvothermal cooling from MeOH, followed by soaking of crystals in solution of guest'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2538
_refine_ls_number_reflns         62969
_refine_ls_number_restraints     9242
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1176P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                45752
_reflns_number_total             62969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02623f2.cif
_cod_data_source_block           dmwms-2v2-340_b20
_cod_original_cell_volume        39603.12(10)
_cod_original_formula_sum        'C385 H404 B15.50 Cl0.50 Co8 F62 N76 O33'
_cod_database_code               7711278
_smtbx_masks_special_details
;
A solvent mask was calculated and 2848 electrons were 
found in a volume of 9930\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[BF4], 33[CH3OH] per Formula Unit 
which account for 2868 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N22H-C16H \\sim N22H-C12H
 with sigma of 0.06
 C21H-C16H \\sim C21H-C12H
 with sigma of 0.04
3. Restrained planarity
 N22H, C21H, C11H, C16H, C12H
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
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 C11G \\sim C12G \\sim C13G \\sim C14G \\sim C15G \\sim C16G \\sim
C21G \\sim N22G \\sim C31G \\sim N32G \\sim C11H \\sim C12H \\sim C13H \\sim
C14H \\sim C15H \\sim C16H \\sim C21H \\sim N22H \\sim C31H \\sim N32H \\sim
B10X \\sim F11X \\sim F12X \\sim F13X \\sim F14X \\sim B15X \\sim F16X \\sim
F17X \\sim F18X \\sim F19X \\sim B20X \\sim F21X \\sim F22X \\sim F23X \\sim
F24X \\sim B25X \\sim F26X \\sim F27X \\sim F28X \\sim F29X \\sim B25Y \\sim
F26Y \\sim F27Y \\sim F28Y \\sim F29Y \\sim B30X \\sim F31X \\sim F32X \\sim
F33X \\sim F34X \\sim B30Y \\sim F31Y \\sim F32Y \\sim F33Y \\sim F34Y \\sim
B35X \\sim F36X \\sim F37X \\sim F38X \\sim F39X \\sim Cl3X \\sim B40X \\sim
F41X \\sim F42X \\sim F43X \\sim F44X \\sim B40Y \\sim F41Y \\sim F42Y \\sim
F43Y \\sim F44Y \\sim B95X \\sim F96X \\sim F97X \\sim F98X: within 2.5A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2.5A
Uanis(Cl3X) = Uanis(B35X)
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, C11G, C12G, C13G, C14G,
 C15G, C16G, C21G, N22G, C31G, N32G, C11H, C12H, C13H, C14H, C15H, C16H, C21H,
 N22H, C31H, N32H, B10X, F11X, F12X, F13X, F14X, B15X, F16X, F17X, F18X, F19X,
 B20X, F21X, F22X, F23X, F24X, B25X, F26X, F27X, F28X, F29X, B25Y, F26Y, F27Y,
 F28Y, F29Y, B30X, F31X, F32X, F33X, F34X, B30Y, F31Y, F32Y, F33Y, F34Y, B35X,
 F36X, F37X, F38X, F39X, Cl3X, B40X, F41X, F42X, F43X, F44X, B40Y, F41Y, F42Y,
 F43Y, F44Y, B95X, F96X, F97X, F98X
 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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41A, N42A, C43A, C44A, C45A, C46A}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11B, C12B, C13B, C14B, C15B, C16B}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21B, N22B, C23B, C24B, C25B, C26B}
{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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41B, N42B, C43B, C44B, C45B, C46B}
{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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21C, N22C, C23C, C24C, C25C, C26C}
{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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41C, N42C, C43C, C44C, C45C, C46C}
{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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21D, N22D, C23D, C24D, C25D, C26D}
{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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41D, N42D, C43D, C44D, C45D, C46D}
{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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21E, N22E, C23E, C24E, C25E, C26E}
{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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41E, N42E, C43E, C44E, C45E, C46E}
{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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21F, N22F, C23F, C24F, C25F, C26F}
{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, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41F, N42F, C43F, C44F, C45F, C46F}
{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}
{C11G, C12G, C13G, C14G, C15G, C16G, C21G, N22G, C31G, N32G} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C11H, C12H, C13H, C14H, C15H, C16H, C21H, N22H, C31H, N32H}
{B10X, F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B15X, F16X, F17X, F18X, F19X}
{B10X, F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B20X, F21X, F22X, F23X, F24X}
{B10X, F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B25X, F26X, F27X, F28X, F29X}
{B10X, F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B25Y, F26Y, F27Y, F28Y, F29Y}
{B10X, F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B30X, F31X, F32X, F33X, F34X}
{B10X, F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B30Y, F31Y, F32Y, F33Y, F34Y}
{B10X, F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B35X, F36X, F37X, F38X, F39X}
{B10X, F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B40X, F41X, F42X, F43X, F44X}
{B10X, F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B40Y, F41Y, F42Y, F43Y, F44Y}
{B10X, F11X, F12X, F13X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B95X, F96X, F97X, F98X}
7. Others
 Fixed Sof: C11G(0.88154) C12G(0.88154) C13G(0.88154) H13G(0.88154)
 C14G(0.88154) H14G(0.88154) C15G(0.88154) H15G(0.88154) C16G(0.88154)
 H16G(0.88154) C21G(0.88154) N22G(0.88154) C31G(0.88154) N32G(0.88154)
 C11H(0.11846) C12H(0.11846) C13H(0.11846) H13H(0.11846) C14H(0.11846)
 H14H(0.11846) C15H(0.11846) H15H(0.11846) C16H(0.11846) H16H(0.11846)
 C21H(0.11846) N22H(0.11846) C31H(0.11846) N32H(0.11846) B15X(0.75) F16X(0.75)
 F17X(0.75) F18X(0.75) F19X(0.75) B20X(0.5) F21X(0.5) F22X(0.5) F23X(0.5)
 F24X(0.5) B25X(0.85613) F26X(0.85613) F27X(0.85613) F28X(0.85613)
 F29X(0.85613) B25Y(0.14387) F26Y(0.14387) F27Y(0.14387) F28Y(0.14387)
 F29Y(0.14387) B30X(0.83484) F31X(0.83484) F32X(0.83484) F33X(0.83484)
 F34X(0.83484) B30Y(0.16516) F31Y(0.16516) F32Y(0.16516) F33Y(0.16516)
 F34Y(0.16516) B35X(0.75) F36X(0.75) F37X(0.75) F38X(0.75) F39X(0.75)
 Cl3X(0.25) B40X(0.5) F41X(0.5) F42X(0.5) F43X(0.5) F44X(0.5) B40Y(0.25)
 F41Y(0.25) F42Y(0.25) F43Y(0.25) F44Y(0.25) B95X(0.5) F96X(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),
 C12E(H12E), C13E(H13E), C14E(H14E), C15E(H15E), 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), C14G(H14G), C15G(H15G), C16G(H16G), C13H(H13H), C14H(H14H),
 C15H(H15H), C16H(H16H)
;
_shelx_res_checksum              59974
_shelx_hkl_checksum              60021
_shelx_fab_checksum              40153
_olex2_submission_special_instructions 'No special instructions were received'