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_1564492
_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 H258 Co8 N72, 2.3(B F4), 1.1(C10 H9 N O2), 2.7(C H3 O), 9.7(N O3), 0.7[BF4], 3.3[NO3], 25.3[CH3OH]'
_chemical_formula_sum            'C375 H379.9 B3 Co8 F12 N86.1 O69.2'
_chemical_formula_weight         7932.00
_chemical_name_systematic        H?MAC?NO3
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-25
_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                 95.7000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.7342(4)
_cell_length_b                   29.9459(4)
_cell_length_c                   40.2590(7)
_cell_measurement_reflns_used    69559
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.6620
_cell_measurement_theta_min      1.6360
_cell_volume                     39269.0(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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 3.0.1-g63768655c-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.7.38-g6919f305-dials-3.0 (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 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 0.998
_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    0.40   0.00   0.00   0.00    --   900
  2  \w   -145.00  25.00   0.20    0.40    --   30.00   0.00   0.00  850
  3  \w   -145.00  25.00   0.20    0.40    --   30.00   0.00 120.00  850
  4  \w   -145.00  25.00   0.20    0.40    --   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      0.0072809000
_diffrn_orient_matrix_UB_12      0.0159994000
_diffrn_orient_matrix_UB_13      0.0113829000
_diffrn_orient_matrix_UB_21      0.0153700000
_diffrn_orient_matrix_UB_22      -0.0143263000
_diffrn_orient_matrix_UB_23      0.0061980000
_diffrn_orient_matrix_UB_31      0.0125622000
_diffrn_orient_matrix_UB_32      0.0082700000
_diffrn_orient_matrix_UB_33      -0.0113005000
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            343424
_diffrn_reflns_point_group_measured_fraction_full 0.998
_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         1.646
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             16501
_exptl_crystal_preparation
'Crystal was soaked in methanolic mother liquor (from the solvothermal crystals growth). A saturated methanolic solution of tetra-butyl ammonium nitrate 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          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.006
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2410
_refine_ls_number_reflns         62520
_refine_ls_number_restraints     7876
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0943
_refine_ls_shift/su_max          0.003
_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          0.3056
_refine_ls_wR_factor_ref         0.3364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                35876
_reflns_number_total             62520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04272f2.cif
_cod_data_source_block           dmwms-2v1-255_mac_no3_rf
_cod_original_formula_sum        'C375 H379.90 B3 Co8 F12 N86.10 O69.20'
_cod_database_code               1564492
_smtbx_masks_special_details
;
A solvent mask was calculated and 2284 electrons were 
found in a volume of 9232\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.7[BF4], 3.3[NO3], 25.3[CH3OH] per Formula Unit 
which account for 2346 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 N16 O48'
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.955
_reflns_odcompleteness_completeness 99.88
_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
 N11X-O12X = N11X-O13X = N11X-O14X
 1.2459 with sigma of 0.02
 O12X-O13X = O13X-O14X = O14X-O12X
 2.1579 with sigma of 0.02
 N11Y-O12Y = N11Y-O13Y = N11Y-O14Y
 1.2459 with sigma of 0.02
 N21X-O22X = N21X-O23X = N21X-O24X
 1.2459 with sigma of 0.02
 N31X-O32X = N31X-O33X = N31X-O34X
 1.2459 with sigma of 0.02
 N31Y-O32Y = N31Y-O33Y = N31Y-O34Y
 1.2459 with sigma of 0.02
 N41X-O42X = N41X-O43X = N41X-O44X
 1.2459 with sigma of 0.02
 N61X-O62X = N61X-O63X = N61X-O64X
 1.2459 with sigma of 0.02
 O11G-C12G
 1.378 with sigma of 0.02
 C12G-C13G
 1.44 with sigma of 0.02
 C13G-C14G
 1.347 with sigma of 0.02
 C14G-C15G
 1.449 with sigma of 0.02
 C15G-C16G
 1.402 with sigma of 0.02
 C16G-O11G
 1.38 with sigma of 0.02
 C16G-C17G
 1.384 with sigma of 0.02
 C17G-C18G
 1.394 with sigma of 0.02
 C18G-C19G
 1.395 with sigma of 0.02
 C19G-C20G
 1.383 with sigma of 0.02
 C20G-C15G
 1.395 with sigma of 0.02
 O21G-C12G
 1.211 with sigma of 0.02
 C22G-C14G
 1.501 with sigma of 0.02
 N23G-C18G
 1.377 with sigma of 0.02
 O12Y-O13Y = O13Y-O14Y = O14Y-O12Y
 2.1579 with sigma of 0.04
 O22X-O23X = O23X-O24X = O24X-O22X
 2.1579 with sigma of 0.04
 O32X-O33X = O33X-O34X = O34X-O32X
 2.1579 with sigma of 0.04
 O32Y-O33Y = O33Y-O34Y = O34Y-O32Y
 2.1579 with sigma of 0.04
 O42X-O43X = O43X-O44X = O44X-O42X
 2.1579 with sigma of 0.04
 O62X-O63X = O63X-O64X = O64X-O62X
 2.1579 with sigma of 0.04
 O21G-C13G
 2.36 with sigma of 0.04
 O11G-O21G
 2.33 with sigma of 0.04
 F12Z-B11Z \\sim F13Z-B11Z \\sim F14Z-B11Z \\sim F15Z-B11Z \\sim F18Z-B16Z
\\sim F19Z-B16Z \\sim F17Z-
 B16Z
 with sigma of 0.02
3. Restrained planarity
 N11X, O12X, O13X, O14X
 with sigma of 0.1
 N11Y, O12Y, O13Y, O14Y
 with sigma of 0.1
 N21X, O22X, O23X, O24X
 with sigma of 0.1
 N31X, O32X, O33X, O34X
 with sigma of 0.1
 N31Y, O32Y, O33Y, O34Y
 with sigma of 0.05
 N41X, O42X, O43X, O44X
 with sigma of 0.1
 N61X, O62X, O63X, O64X
 with sigma of 0.1
 N23G, C17G, C18G, C19G
 with sigma of 0.1
 C22G, C13G, C14G, C15G
 with sigma of 0.1
 O11G, C12G, C13G, C14G, C15G, C16G
 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 C50A \\sim C51A \\sim C52A \\sim C53A \\sim
C54A \\sim C55A \\sim C56A \\sim C57A \\sim C58A \\sim C59A \\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 C50B \\sim C51B \\sim C52B \\sim C53B \\sim C54B \\sim
C55B \\sim C56B \\sim C57B \\sim C58B \\sim C59B \\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 C50C \\sim C51C \\sim C52C \\sim C53C \\sim C54C \\sim C55C \\sim
C56C \\sim C57C \\sim C58C \\sim C59C \\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
C50D \\sim C51D \\sim C52D \\sim C53D \\sim C54D \\sim C55D \\sim C56D \\sim
C57D \\sim C58D \\sim C59D \\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 C50E \\sim
C51E \\sim C52E \\sim C53E \\sim C54E \\sim C55E \\sim C56E \\sim C57E \\sim
C58E \\sim C59E \\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 C50F \\sim C51F \\sim
C52F \\sim C53F \\sim C54F \\sim C55F \\sim C56F \\sim C57F \\sim C58F \\sim
C59F \\sim B16Z \\sim F19Z \\sim F18Z \\sim F17Z \\sim B11Z \\sim F12Z \\sim
F14Z \\sim F13Z \\sim F15Z \\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 \\sim O11S \\sim C12S \\sim O13S \\sim C14S \\sim N11X \\sim
O12X \\sim O13X \\sim O14X \\sim N11Y \\sim O12Y \\sim O13Y \\sim O14Y \\sim
N21X \\sim O22X \\sim O23X \\sim O24X \\sim N31X \\sim O32X \\sim O33X \\sim
O34X \\sim N31Y \\sim O32Y \\sim O33Y \\sim O34Y \\sim N41X \\sim O42X \\sim
O43X \\sim O44X \\sim N51X \\sim O52X \\sim O53X \\sim O54X \\sim N51Y \\sim
O52Y \\sim O53Y \\sim O54Y \\sim N61X \\sim O62X \\sim O63X \\sim O64X: within
2.5A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2.5A
N51Y \\sim O52Y \\sim O53Y \\sim O54Y \\sim N51X \\sim O52X \\sim O53X \\sim
O54X: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
Uanis(N51X) = Uanis(O52Y)
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, C50A, C51A,
 C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A, N11B, C12B, C13B, C14B, C15B,
 C16B, N21B, N22B, C23B, C24B, C25B, C26B, N31B, C32B, C33B, C34B, C35B, C36B,
 N41B, N42B, C43B, C44B, C45B, C46B, C50B, C51B, C52B, C53B, C54B, C55B, C56B,
 C57B, C58B, C59B, N11C, C12C, C13C, C14C, C15C, C16C, N21C, N22C, C23C, C24C,
 C25C, C26C, N31C, C32C, C33C, C34C, C35C, C36C, N41C, N42C, C43C, C44C, C45C,
 C46C, C50C, C51C, C52C, C53C, C54C, C55C, C56C, C57C, C58C, C59C, N11D, C12D,
 C13D, C14D, C15D, C16D, N21D, N22D, C23D, C24D, C25D, C26D, N31D, C32D, C33D,
 C34D, C35D, C36D, N41D, N42D, C43D, C44D, C45D, C46D, C50D, C51D, C52D, C53D,
 C54D, C55D, C56D, C57D, C58D, C59D, N11E, C12E, C13E, C14E, C15E, C16E, N21E,
 N22E, C23E, C24E, C25E, C26E, N31E, C32E, C33E, C34E, C35E, C36E, N41E, N42E,
 C43E, C44E, C45E, C46E, C50E, C51E, C52E, C53E, C54E, C55E, C56E, C57E, C58E,
 C59E, N11F, C12F, C13F, C14F, C15F, C16F, N21F, N22F, C23F, C24F, C25F, C26F,
 N31F, C32F, C33F, C34F, C35F, C36F, N41F, N42F, C43F, C44F, C45F, C46F, C50F,
 C51F, C52F, C53F, C54F, C55F, C56F, C57F, C58F, C59F, B16Z, F19Z, F18Z, F17Z,
 B11Z, F12Z, F14Z, F13Z, F15Z, O11G, C12G, C13G, C14G, C15G, C16G, C17G, C18G,
 C19G, C20G, O21G, C22G, N23G, O11S, C12S, O13S, C14S, N11X, O12X, O13X, O14X,
 N11Y, O12Y, O13Y, O14Y, N21X, O22X, O23X, O24X, N31X, O32X, O33X, O34X, N31Y,
 O32Y, O33Y, O34Y, N41X, O42X, O43X, O44X, N51X, O52X, O53X, O54X, N51Y, O52Y,
 O53Y, O54Y, N61X, O62X, O63X, O64X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N51Y, O52Y, O53Y, O54Y, N51X, O52X, O53X, O54X
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
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}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21B, N22B, C23B, C24B, C25B}
{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}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50B, C51B, C52B, C53B, C54B, C55B, C56B, C57B, C58B, C59B}
{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}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50C, C51C, C52C, C53C, C54C, C55C, C56C, C57C, C58C, C59C}
{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}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50D, C51D, C52D, C53D, C54D, C55D, C56D, C57D, C58D, C59D}
{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}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50E, C51E, C52E, C53E, C54E, C55E, C56E, C57E, C58E, C59E}
{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}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50F, C51F, C52F, C53F, C54F, C55F, C56F, C57F, C58F, C59F}
7. Others
 Fixed Sof: B16Z(0.5) F18Z(0.5) B11Z(0.65) F12Z(0.65) F14Z(0.65) F13Z(0.65)
 F15Z(0.65) O11G(0.55) C12G(0.55) C13G(0.55) H13G(0.55) C14G(0.55) C15G(0.55)
 C16G(0.55) C17G(0.55) H17G(0.55) C18G(0.55) C19G(0.55) H19G(0.55) C20G(0.55)
 H20G(0.55) O21G(0.55) C22G(0.55) H22A(0.55) H22B(0.55) H22C(0.55) N23G(0.55)
 H23G(0.55) H23H(0.55) O13S(0.35) C14S(0.35) H14G(0.35) H14H(0.35) H14I(0.35)
 N11X(0.5) O12X(0.5) O13X(0.5) O14X(0.5) N11Y(0.35) O12Y(0.35) O13Y(0.35)
 O14Y(0.35) N21X(0.75) O22X(0.75) O23X(0.75) O24X(0.75) N31X(0.5) O32X(0.5)
 O33X(0.5) O34X(0.5) N31Y(0.5) O32Y(0.5) O33Y(0.5) O34Y(0.5) N41X(0.75)
 O42X(0.75) O43X(0.75) O44X(0.75) N51X(0.2) O52X(0.2) O53X(0.2) O54X(0.2)
 N51Y(0.3) O52Y(0.3) O53Y(0.3) O54Y(0.3)
8.a Free rotating group:
 N51X(O52X,O53X,O54X), N51Y(O52Y,O53Y,O54Y)
8.b Rotating group:
 N23G(H23G,H23H)
8.c 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.d 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),
 C51A(H51A), C52A(H52A), C53A(H53A), C58A(H58A), C13B(H13B), C14B(H14B),
 C15B(H15B), C16B(H16B), C23B(H23B), C24B(H24B), C33B(H33B), C34B(H34B),
 C35B(H35B), C36B(H36B), C43B(H43B), C44B(H44B), C51B(H51B), C53B(H53B),
 C56B(H56B), C57B(H57B), C58B(H58B), C13C(H13C), C14C(H14C), C15C(H15C),
 C16C(H16C), C23C(H23C), C24C(H24C), C33C(H33C), C34C(H34C), C35C(H35C),
 C36C(H36C), C43C(H43C), C44C(H44C), C51C(H51C), C52C(H52C), C53C(H53C),
 C56C(H56C), C57C(H57C), C58C(H58C), C13D(H13D), C14D(H14D), C15D(H15D),
 C16D(H16D), C23D(H23D), C24D(H24D), C33D(H33D), C34D(H34D), C35D(H35D),
 C36D(H36D), C43D(H43D), C44D(H44D), C51D(H51D), C52D(H52D), C53D(H53D),
 C56D(H56D), C57D(H57D), C58D(H58D), C13E(H13E), C14E(H14E), C15E(H15E),
 C16E(H16E), C23E(H23E), C24E(H24E), C33E(H33E), C34E(H34E), C35E(H35E),
 C36E(H36E), C43E(H43E), C44E(H44E), C51E(H51E), C52E(H52E), C53E(H53E),
 C56E(H56E), C57E(H57E), C58E(H58E), C13F(H13F), C14F(H14F), C15F(H15F),
 C16F(H16F), C23F(H23F), C24F(H24F), C33F(H33F), C34F(H34F), C35F(H35F),
 C36F(H36F), C43F(H43F), C44F(H44F), C51F(H51F), C52F(H52F), C53F(H53F),
 C56F(H56F), C57F(H57F), C58F(H58F), C13G(H13G), C17G(H17G), C19G(H19G),
 C20G(H20G)
8.e Idealised Me refined with riding coordinates:
 C22G(H22A,H22B,H22C), C12S(H12A,H12B,H12C), C14S(H14G,H14H,H14I)
;
_shelx_res_checksum              3974
_shelx_hkl_checksum              40625
_shelx_fab_checksum              37161
_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 1.401
_oxdiff_exptl_absorpt_empirical_full_min 0.767