An investigation into catalysed xanthene-based dye oxidation by a family of coordination cages.
Williams, James R.; Ward, Michael D.; Nanoscale 17 (2025) 17285–17293; doi:10.1039/d5nr02293b

data_1575067
_publ_section_title
;
 An investigation into catalysed xanthene-based dye oxidation by a family
 of coordination cages.
;
_journal_issue                   29
_journal_name_full               Nanoscale
_journal_page_first              17285
_journal_page_last               17293
_journal_paper_doi               10.1039/d5nr02293b
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety
'2(C168 H132 N36 Ni4), 0.15(Cl), 1.7(C20 H6 Br4 O5), 10.35(B F4), [+ solvents]'
_chemical_formula_sum
'C401 H398.2 B10.45 Br6.8 Cl0.15 F41.8 N72 Ni8 O40'
_chemical_formula_weight         8791.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-29 deposited with the CCDC.	2025-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                104.597(2)
_cell_angle_beta                 98.324(2)
_cell_angle_gamma                94.218(2)
_cell_formula_units_Z            2
_cell_length_a                   21.8986(4)
_cell_length_b                   22.3981(4)
_cell_length_c                   43.4906(8)
_cell_measurement_reflns_used    33079
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.8040
_cell_measurement_theta_min      2.5610
_cell_volume                     20290.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.124a 64-bit (release 23-05-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.887
_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    -82.00  -3.00   0.50    0.90    --  -48.96 112.00 -74.00  158
  2  \w     25.00  96.00   0.50    0.90    --   49.46-112.00-167.00  142
  3  \w    -83.00 -11.00   0.50    0.90    --  -82.51 112.00 -74.00  144
  4  \w   -153.00 -81.00   0.50    0.90    --  -82.51-112.00-167.00  144
  5  \w   -153.00 -81.00   0.50    0.90    --  -82.51-112.00-167.00  144
  6  \w    -83.00 -11.00   0.50    0.90    --  -82.51 112.00 -74.00  144
  7  \w     28.00 108.00   0.50    0.90    --   99.24-112.00-167.00  160
  8  \w    103.00 178.00   0.50    0.90    --  109.47 112.00 -74.00  150
  9  \w   -160.00 -66.00   0.50    0.90    --  -82.51 -45.00  60.00  188
 10  \w    -51.00  -4.00   0.50    0.90    --  -82.51  45.00 150.00   94
 11  \w     34.00 111.00   0.50    0.90    --   99.24-125.00 -60.00  154
 12  \w     21.00  51.00   0.50    0.90    --   99.24 -45.00-180.00   60
 13  \w     31.00 106.00   0.50    0.90    --   99.24 -77.00  30.00  150
 14  \w     34.00 111.00   0.50    0.90    --   99.24-125.00  60.00  154
 15  \w    103.00 170.00   0.50    0.90    --   99.24 112.00 -74.00  134
 16  \w     27.00 172.00   0.50    0.90    --   99.24   0.00 -60.00  290
 17  \w     39.00 108.00   0.50    0.90    --  109.47-112.00-167.00  138
 18  \w     23.00 118.00   0.50    0.90    --   49.46  77.00 150.00  190
 19  \w     23.00 118.00   0.50    0.90    --   49.46  77.00 -30.00  190
 20  \w    -35.00  -3.00   0.50    0.90    --  -82.51  30.00 -30.00   64
 21  \w   -157.00 -62.00   0.50    0.90    --  -82.51 -61.00 120.00  190
 22  \w   -151.00 -56.00   0.50    0.90    --  -82.51 -77.00-180.00  190
 23  \w   -151.00 -56.00   0.50    0.90    --  -82.51 -77.00-150.00  190
 24  \w   -151.00 -56.00   0.50    0.90    --  -82.51 -77.00 -90.00  190
 25  \w   -151.00 -56.00   0.50    0.90    --  -82.51 -77.00 -30.00  190
 26  \w   -151.00 -56.00   0.50    0.90    --  -82.51 -77.00  30.00  190
 27  \w     79.00 174.00   0.50    0.90    --   99.24  61.00  60.00  190
 28  \w     21.00  51.00   0.50    0.90    --   99.24 -45.00  60.00   60
 29  \w     93.00 178.00   0.50    0.90    --  109.47  45.00   0.00  170
 30  \w     35.00  71.00   0.50    0.90    --  109.47 -61.00 -30.00   72
 31  \w     35.00  71.00   0.50    0.90    --  109.47 -61.00-150.00   72
 32  \w     23.00 118.00   0.50    0.90    --   49.46  77.00  60.00  190
 33  \w     23.00 118.00   0.50    0.90    --   49.46  77.00-120.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0485988000
_diffrn_orient_matrix_UB_12      0.0324624000
_diffrn_orient_matrix_UB_13      0.0184678000
_diffrn_orient_matrix_UB_21      0.0337335000
_diffrn_orient_matrix_UB_22      -0.0108265000
_diffrn_orient_matrix_UB_23      0.0314241000
_diffrn_orient_matrix_UB_31      0.0402850000
_diffrn_orient_matrix_UB_32      0.0628353000
_diffrn_orient_matrix_UB_33      0.0071308000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1465
_diffrn_reflns_av_unetI/netI     0.1141
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            372612
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.696
_diffrn_reflns_theta_min         2.551
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.986
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             9042
_exptl_crystal_recrystallization_method
'Crystals were prepared solvothermally in a teflon lined pressure reactor. Ligand A and Ni(BF4)2.6H20 were combined in a 3:2 ratio in a saturated solution of eosin Y in methanol and heated to 120 C for 3 hours with gradual cooling of 0.1 deg/min to room temperature, which yielded a mixture of trapazoidal and bar shaped crystals. The bar shaped crystals were used.'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.145
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4837
_refine_ls_number_reflns         78392
_refine_ls_number_restraints     1206
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1691
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1322P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2214
_refine_ls_wR_factor_ref         0.2636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                35919
_reflns_number_total             78392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr02293b2.cif
_cod_data_source_block           nicube_depey_1
_cod_depositor_comments
'Adding full bibliography for 1575067--1575070.cif.'
_cod_original_cell_volume        20290.2(7)
_cod_original_formula_sum
'C401 H398.20 B10.45 Br6.80 Cl0.15 F41.80 N72 Ni8 O40'
_cod_database_code               1575067
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.681
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 B41X-F44X = B41X-F42X = B41X-F45X = B41X-F43X
 1.42 with sigma of 0.02
 B61X-F62X = B61X-F64X = B61X-F65X = B61X-F63X
 1.42 with sigma of 0.02
 B61Z-F65Z = B61Z-F62Z = B61Z-F63Z = B61Z-F64Z
 1.42 with sigma of 0.02
 B51X-F53X = B51X-F54X = B51X-F55X = B51X-F52X
 1.42 with sigma of 0.02
 B61Y-F64Y = B61Y-F65Y = B61Y-F62Y = B61Y-F63Y
 1.42 with sigma of 0.02
 B66Y-F67Y = B66Y-F68Y = B66Y-F70Y = B66Y-F69Y
 1.42 with sigma of 0.02
 B66X-F68X = B66X-F67X = B66X-F70X = B66X-F69X
 1.42 with sigma of 0.02
 B36X-F40X = B36X-F37X = B36X-F39X = B36X-F38X
 1.42 with sigma of 0.02
 B46X-F47X = B46X-F48X = B46X-F50X = B46X-F49X
 1.42 with sigma of 0.02
 B31X-F35X = B31X-F32X = B31X-F34X = B31X-F33X
 1.42 with sigma of 0.02
 B26X-F28X = B26X-F30X = B26X-F29X = B26X-F27X
 1.42 with sigma of 0.02
 B21X-F24X = B21X-F23X = B21X-F22X = B21X-F25X
 1.42 with sigma of 0.02
 B16X-F18X = B16X-F20X = B16X-F19X = B16X-F17X
 1.42 with sigma of 0.02
 B11X-F14X = B11X-F12X = B11X-F15X = B11X-F13X
 1.42 with sigma of 0.02
 B56Y-F57Y = B56Y-F59Y = B56Y-F60Y = B56Y-F58Y
 1.42 with sigma of 0.02
 B61X-F62X \\sim B61X-F64X \\sim B61X-F65X \\sim B61X-F63X
 with sigma of 0.02
 B61Z-F65Z \\sim B61Z-F62Z \\sim B61Z-F63Z \\sim B61Z-F64Z
 with sigma of 0.02
 F65Z-F62Z \\sim F62Z-F63Z \\sim F63Z-F64Z \\sim F64Z-F65Z \\sim F62Z-F64Z
\\sim F65Z-F63Z
 with sigma of 0.04
 F62X-F64X \\sim F64X-F65X \\sim F65X-F63X \\sim F63X-F62X \\sim F64X-F63X
\\sim F62X-F65X
 with sigma of 0.04
 B61Y-F64Y \\sim B61Y-F65Y \\sim B61Y-F62Y \\sim B61Y-F63Y
 with sigma of 0.02
 F64Y-F65Y \\sim F65Y-F62Y \\sim F62Y-F63Y \\sim F63Y-F64Y \\sim F65Y-F63Y
\\sim F64Y-F62Y
 with sigma of 0.04
 B51X-F53X \\sim B51X-F54X \\sim B51X-F55X \\sim B51X-F52X
 with sigma of 0.02
 B41X-F44X \\sim B41X-F42X \\sim B41X-F45X \\sim B41X-F43X
 with sigma of 0.02
 F53X-F54X \\sim F54X-F55X \\sim F55X-F52X \\sim F52X-F53X \\sim F54X-F52X
\\sim F53X-F55X
 with sigma of 0.04
 F44X-F42X \\sim F42X-F45X \\sim F45X-F43X \\sim F43X-F44X \\sim F42X-F43X
\\sim F44X-F45X
 with sigma of 0.04
 B66X-F68X \\sim B66X-F67X \\sim B66X-F70X \\sim B66X-F69X
 with sigma of 0.02
 B66Y-F67Y \\sim B66Y-F68Y \\sim B66Y-F70Y \\sim B66Y-F69Y
 with sigma of 0.02
 F67Y-F68Y \\sim F68Y-F70Y \\sim F70Y-F69Y \\sim F69Y-F67Y \\sim F68Y-F69Y
\\sim F67Y-F70Y
 with sigma of 0.04
 F68X-F67X \\sim F67X-F70X \\sim F70X-F69X \\sim F69X-F68X \\sim F67X-F69X
\\sim F68X-F70X
 with sigma of 0.04
 B36X-F40X \\sim B36X-F37X \\sim B36X-F39X \\sim B36X-F38X
 with sigma of 0.02
 F40X-F37X \\sim F37X-F39X \\sim F39X-F38X \\sim F38X-F40X \\sim F37X-F38X
\\sim F40X-F39X
 with sigma of 0.04
 B46X-F47X \\sim B46X-F48X \\sim B46X-F50X \\sim B46X-F49X
 with sigma of 0.02
 F47X-F48X \\sim F48X-F50X \\sim F50X-F49X \\sim F49X-F47X \\sim F48X-F49X
\\sim F47X-F50X
 with sigma of 0.04
 B31X-F35X \\sim B31X-F32X \\sim B31X-F34X \\sim B31X-F33X
 with sigma of 0.02
 F35X-F32X \\sim F32X-F34X \\sim F34X-F33X \\sim F33X-F35X \\sim F32X-F33X
\\sim F35X-F34X
 with sigma of 0.04
 B26X-F28X \\sim B26X-F30X \\sim B26X-F29X \\sim B26X-F27X
 with sigma of 0.02
 F28X-F30X \\sim F30X-F29X \\sim F29X-F27X \\sim F27X-F28X \\sim F30X-F27X
\\sim F28X-F29X
 with sigma of 0.04
 B21X-F24X \\sim B21X-F23X \\sim B21X-F22X \\sim B21X-F25X
 with sigma of 0.02
 F24X-F23X \\sim F23X-F22X \\sim F22X-F25X \\sim F25X-F24X \\sim F23X-F25X
\\sim F24X-F22X
 with sigma of 0.04
 B16X-F18X \\sim B16X-F20X \\sim B16X-F19X \\sim B16X-F17X
 with sigma of 0.02
 F18X-F20X \\sim F20X-F19X \\sim F19X-F17X \\sim F17X-F18X \\sim F20X-F17X
\\sim F18X-F19X
 with sigma of 0.04
 B11X-F14X \\sim B11X-F12X \\sim B11X-F15X \\sim B11X-F13X
 with sigma of 0.02
 F14X-F12X \\sim F12X-F15X \\sim F15X-F13X \\sim F13X-F14X \\sim F12X-F13X
\\sim F14X-F15X
 with sigma of 0.04
 B56Y-F57Y \\sim B56Y-F59Y \\sim B56Y-F60Y \\sim B56Y-F58Y
 with sigma of 0.02
 F57Y-F59Y \\sim F59Y-F60Y \\sim F60Y-F58Y \\sim F58Y-F57Y \\sim F59Y-F58Y
\\sim F57Y-F60Y
 with sigma of 0.04
3. Restrained planarity
 N31K, C32K, C33K, C34K, C35K, C36K
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
B61Z \\sim F62Z \\sim F63Z \\sim F64Z \\sim F65Z: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B61X \\sim F62X \\sim F63X \\sim F64X \\sim F65X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B41X \\sim F42X \\sim F43X \\sim F44X \\sim F45X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B61Y \\sim F62Y \\sim F63Y \\sim F64Y \\sim F65Y: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B51X \\sim F52X \\sim F53X \\sim F54X \\sim F55X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B66X \\sim F67X \\sim F68X \\sim F69X \\sim F70X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B66Y \\sim F67Y \\sim F68Y \\sim F69Y \\sim F70Y: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B36X \\sim F37X \\sim F38X \\sim F39X \\sim F40X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B46X \\sim F47X \\sim F48X \\sim F49X \\sim F50X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B31X \\sim F32X \\sim F33X \\sim F34X \\sim F35X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B26X \\sim F27X \\sim F28X \\sim F29X \\sim F30X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B21X \\sim F22X \\sim F23X \\sim F24X \\sim F25X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B16X \\sim F17X \\sim F18X \\sim F19X \\sim F20X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B11X \\sim F12X \\sim F13X \\sim F14X \\sim F15X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
B56Y \\sim F57Y \\sim F58Y \\sim F59Y \\sim F60Y: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(F65Y) = Uanis(B61Y) = Uanis(F64Y) = Uanis(F63Y) = Uanis(F62Y)
Uanis(F68X) = Uanis(B66X) = Uanis(F67X) = Uanis(F70X) = Uanis(F69X)
Uanis(F54X) = Uanis(F53X) = Uanis(F55X)
Uanis(N31K) = Uanis(C36K) = Uanis(C35K) = Uanis(C34K) = Uanis(C33K) =
Uanis(C32K)
Uanis(F14X) = Uanis(B11X) = Uanis(F12X) = Uanis(F13X) = Uanis(F15X)
5. Rigid body (RIGU) restrains
 B61X, F62X, F63X, F64X, F65X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B61Z, F62Z, F63Z, F64Z, F65Z
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B61Y, F62Y, F63Y, F64Y, F65Y
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B51X, F52X, F53X, F54X, F55X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B41X, F42X, F43X, F44X, F45X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B66X, F67X, F68X, F69X, F70X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B66Y, F67Y, F68Y, F69Y, F70Y
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B36X, F37X, F38X, F39X, F40X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B46X, F47X, F48X, F49X, F50X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B31X, F32X, F33X, F34X, F35X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B26X, F27X, F28X, F29X, F30X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B21X, F22X, F23X, F24X, F25X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B16X, F17X, F18X, F19X, F20X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B11X, F12X, F13X, F14X, F15X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B56Y, F57Y, F58Y, F59Y, F60Y
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl3(0.15) Br1M(0.7) Br2M(0.7) Br3M(0.7) Br4M(0.7) C11M(0.7)
 C12M(0.7) C13M(0.7) O14M(0.7) C15M(0.7) C16M(0.7) C17M(0.7) C18M(0.7)
 C19M(0.7) H19M(0.7) C20M(0.7) C21M(0.7) C22M(0.7) C23M(0.7) H23M(0.7)
 C24M(0.7) O25M(0.7) O28M(0.7) C31M(0.7) C32M(0.7) C33M(0.7) H33M(0.7)
 C34M(0.7) H34M(0.7) C35M(0.7) H35M(0.7) C36M(0.7) H36M(0.7) C37M(0.7)
 O38M(0.7) O39M(0.7) B11X(0.75) F12X(0.75) F13X(0.75) F14X(0.75) F15X(0.75)
 B16X(0.9) F17X(0.9) F18X(0.9) F19X(0.9) F20X(0.9) B21X(0.9) F22X(0.9)
 F23X(0.9) F24X(0.9) F25X(0.9) B26X(0.9) F27X(0.9) F28X(0.9) F29X(0.9)
 F30X(0.9) B41X(0.9) F42X(0.9) F43X(0.9) F44X(0.9) F45X(0.9) B46X(0.9)
 F47X(0.9) F48X(0.9) F49X(0.9) F50X(0.9) B51X(0.6) F52X(0.6) F53X(0.6)
 F54X(0.6) F55X(0.6) B61X(0.25) F62X(0.25) F63X(0.25) F64X(0.25) F65X(0.25)
 B66X(0.5) F67X(0.5) F68X(0.5) F69X(0.5) F70X(0.5) B56Y(0.75) F57Y(0.75)
 F58Y(0.75) F59Y(0.75) F60Y(0.75) B61Y(0.35) F62Y(0.35) F63Y(0.35) F64Y(0.35)
 F65Y(0.35) B66Y(0.4) F67Y(0.4) F68Y(0.4) F69Y(0.4) F70Y(0.4) B61Z(0.25)
 F62Z(0.25) F63Z(0.25) F64Z(0.25) F65Z(0.25)
7.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), C26H(H26O,H26P), C46H(H46O,H46P), C26I(H26Q,H26R), C46I(H46Q,H46R),
 C26J(H26S,H26T), C46J(H46S,H46T), C26K(H26U,H26V), C46K(H46U,H46V), C26L(H26W,
 H26X), C46L(H46W,H46X)
7.b Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A), C23A(H23A), C24A(H24A),
 C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C43A(H43A), C44A(H44A),
 C52A(H52A), C53A(H53A), C54A(H54A), C62A(H62A), C63A(H63A), C64A(H64A),
 C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C23B(H23B), C24B(H24B),
 C32B(H32B), C33B(H33B), C34B(H34B), C35B(H35B), C43B(H43B), C44B(H44B),
 C52B(H52B), C53B(H53B), C54B(H54B), C62B(H62B), C63B(H63B), C64B(H64B),
 C12C(H12C), C13C(H13C), C14C(H14C), C15C(H15C), C23C(H23C), C24C(H24C),
 C32C(H32C), C33C(H33C), C34C(H34C), C35C(H35C), C43C(H43C), C44C(H44C),
 C52C(H52C), C53C(H53C), C54C(H54C), C62C(H62C), C63C(H63C), C64C(H64C),
 C12D(H12D), C13D(H13D), C14D(H14D), C15D(H15D), C23D(H23D), C24D(H24D),
 C32D(H32D), C33D(H33D), C34D(H34D), C35D(H35D), C43D(H43D), C44D(H44D),
 C52D(H52D), C53D(H53D), C54D(H54D), C62D(H62D), C63D(H63D), C64D(H64D),
 C12E(H12E), C13E(H13E), C14E(H14E), C15E(H15E), C23E(H23E), C24E(H24E),
 C32E(H32E), C33E(H33E), C34E(H34E), C35E(H35E), C43E(H43E), C44E(H44E),
 C52E(H52E), C53E(H53E), C54E(H54E), C62E(H62E), C63E(H63E), C64E(H64E),
 C12F(H12F), C13F(H13F), C14F(H14F), C15F(H15F), C23F(H23F), C24F(H24F),
 C32F(H32F), C33F(H33F), C34F(H34F), C35F(H35F), C43F(H43F), C44F(H44F),
 C52F(H52F), C53F(H53F), C54F(H54F), C62F(H62F), C63F(H63F), C64F(H64F),
 C12G(H12G), C13G(H13G), C14G(H14G), C15G(H15G), C23G(H23G), C24G(H24G),
 C32G(H32G), C33G(H33G), C34G(H34G), C35G(H35G), C43G(H43G), C44G(H44G),
 C52G(H52G), C53G(H53G), C54G(H54G), C62G(H62G), C63G(H63G), C64G(H64G),
 C12H(H12H), C13H(H13H), C14H(H14H), C15H(H15H), C23H(H23H), C24H(H24H),
 C32H(H32H), C33H(H33H), C34H(H34H), C35H(H35H), C43H(H43H), C44H(H44H),
 C52H(H52H), C53H(H53H), C54H(H54H), C62H(H62H), C63H(H63H), C64H(H64H),
 C12I(H12I), C13I(H13I), C14I(H14I), C15I(H15I), C23I(H23I), C24I(H24I),
 C32I(H32I), C33I(H33I), C34I(H34I), C35I(H35I), C43I(H43I), C44I(H44I),
 C52I(H52I), C53I(H53I), C54I(H54I), C62I(H62I), C64I(H64I), C12J(H12J),
 C13J(H13J), C14J(H14J), C15J(H15J), C23J(H23J), C24J(H24J), C32J(H32J),
 C33J(H33J), C34J(H34J), C35J(H35J), C43J(H43J), C44J(H44J), C52J(H52J),
 C53J(H53J), C54J(H54J), C62J(H62J), C63J(H63J), C64J(H64J), C12K(H12K),
 C13K(H13K), C14K(H14K), C15K(H15K), C23K(H23K), C24K(H24K), C32K(H32K),
 C33K(H33K), C34K(H34K), C35K(H35K), C43K(H43K), C44K(H44K), C52K(H52K),
 C53K(H53K), C54K(H54K), C62K(H62K), C63K(H63K), C64K(H64K), C12L(H12L),
 C13L(H13L), C14L(H14L), C15L(H15L), C23L(H23L), C24L(H24L), C32L(H32L),
 C33L(H33L), C34L(H34L), C35L(H35L), C43L(H43L), C44L(H44L), C52L(H52L),
 C53L(H53L), C54L(H54L), C62L(H62L), C63L(H63L), C64L(H64L), C19M(H19M),
 C23M(H23M), C33M(H33M), C34M(H34M), C35M(H35M), C36M(H36M), C19N(H19N),
 C23N(H23N), C33N(H33N), C34N(H34N), C35N(H35N), C36N(H36N)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1138 electrons were 
found in a volume of 4639\%A^3^ in 5 voids per unit cell. 
This is consistent with the presence of 
31 MeOH, 0.5 H2O and 0.1 BF4 per formula unit 
which account for 1134 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31626
_shelx_fab_checksum              94415
_olex2_exptl_crystal_mounting_method 'Flombin oil on a nylon loop.'
_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 1.210
_oxdiff_exptl_absorpt_empirical_full_min 0.779