Photoswitching of Co(ii)-based coordination cages containing azobenzene backbones.
Tipping, Max B.; Pruñonosa Lara, Lidón; Solea, Atena B.; von Krbek, Larissa K. S.; Ward, Michael D.; Chemical science 15 (2024) 8488–8499; doi:10.1039/d4sc01575d

data_1571546
_publ_section_title
;
 Photoswitching of Co(ii)-based coordination cages containing azobenzene
 backbones.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              8488
_journal_page_last               8499
_journal_paper_doi               10.1039/d4sc01575d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'C180 H144.407 Co4 N48.107, 1.881(C H4 O), 6.668(B F4), B0.881 F4, [+ solvents]'
_chemical_formula_sum
'C191.88 H203.94 B7.94 Co4 F32.28 N48.11 O17.88'
_chemical_formula_weight         4405.01
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-16 deposited with the CCDC.	2024-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                93.3668(5)
_cell_angle_beta                 93.7613(5)
_cell_angle_gamma                94.7042(6)
_cell_formula_units_Z            2
_cell_length_a                   20.35957(13)
_cell_length_b                   21.05549(13)
_cell_length_c                   23.94804(13)
_cell_measurement_reflns_used    71741
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.319576310414686
_cell_measurement_theta_min      0.820877521877219
_cell_volume                     10188.21(11)
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 3.10.3-2-g650e29187-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 3.10.1 (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            203895
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.502
_diffrn_reflns_theta_max         22.502
_diffrn_reflns_theta_min         0.942
_entry.id                        xia2
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9723190591518912
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 8.0.001: AIMLESS, version 0.7.8 : 28/07/21
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             4546
_exptl_crystal_preparation       'solvothermal synthesis in MeOH'
_exptl_crystal_recrystallization_method solvothermal
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2943
_refine_ls_number_reflns         29237
_refine_ls_number_restraints     6264
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0638
_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^)+(0.1166P)^2^+7.3812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.1986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22728
_reflns_number_total             29237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01575d2.cif
_cod_data_source_block           shelxt_a
_cod_depositor_comments
'Adding full bibliography for 1571545--1571546.cif.'
_cod_original_cell_volume        10188.21(8)
_cod_database_code               1571546
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.962
_olex2_refinement_description
;
1. Restrained distances
 C12F-C13F
 1.54 with sigma of 0.02
 B25X-F27X \\sim B25X-F27Y
 with sigma of 0.02
 B25X-F29X \\sim B25X-F29Y
 with sigma of 0.02
 B25X-F26X \\sim B25X-F26Y
 with sigma of 0.02
 B25X-F28X \\sim B25X-F28Y
 with sigma of 0.02
 C23D-C27D \\sim C23H-C27D
 with sigma of 0.02
 C32D-H32D \\sim C32H-H32H
 with sigma of 0.02
 C27D-C32D \\sim C27H-C32H
 with sigma of 0.04
 C31D-N28D \\sim C31H-N28H
 with sigma of 0.04
 Co04-N1F \\sim Co04-N1G
 with sigma of 0.02
 C21D-C26D \\sim C21H-C26H
 with sigma of 0.02
 N1F-C6F \\sim N1G-C6G
 with sigma of 0.02
 C25D-C26D \\sim C25H-C26H
 with sigma of 0.02
 C21D-H22D \\sim C21H-H22H
 with sigma of 0.04
 C23D-H24D \\sim C23H-H24H
 with sigma of 0.04
 N1F-C2F \\sim N1G-C2G
 with sigma of 0.02
 Co04-N29D \\sim Co04-N29H
 with sigma of 0.02
 C6F-C5F \\sim C6G-C5G
 with sigma of 0.02
 C30D-C31D \\sim C30H-C31H
 with sigma of 0.02
 C6F-C7F \\sim C6G-C7F
 with sigma of 0.02
 C23D-N28D \\sim C23D-N28H
 with sigma of 0.04
 C5F-H5F \\sim C5G-H5G
 with sigma of 0.02
 C30D-H31D \\sim C30H-H31H
 with sigma of 0.04
 C5F-C4F \\sim C5G-C4G
 with sigma of 0.02
 N28D-C23H \\sim N28H-C23H
 with sigma of 0.04
 C22D-C24D \\sim C22H-C24H
 with sigma of 0.04
 C24D-C27D \\sim C24H-C27D
 with sigma of 0.04
 C3F-C2F \\sim C3G-C2G
 with sigma of 0.02
 C2F-H2F \\sim C2G-H2G
 with sigma of 0.02
 Co04-C6F \\sim Co04-C6G
 with sigma of 0.04
 Co04-C2F \\sim Co04-C2G
 with sigma of 0.04
 N20D-C21D \\sim N20D-C21H
 with sigma of 0.02
 N1F-C5F \\sim N1G-C5G
 with sigma of 0.04
 C22D-C23D \\sim C22H-C23H
 with sigma of 0.02
 N1F-C3F \\sim N1G-C3G
 with sigma of 0.04
 C24D-C25D \\sim C24H-C25H
 with sigma of 0.02
 N1F-H2F \\sim N1G-H2G
 with sigma of 0.04
 N20D-C22D \\sim N20D-C22H
 with sigma of 0.04
 N1F-C7F \\sim N1G-C7F
 with sigma of 0.04
 C21D-C25D \\sim C21H-C25H
 with sigma of 0.04
 C6F-H5F \\sim C6G-H5G
 with sigma of 0.04
 C22D-C27D \\sim C22H-C27D
 with sigma of 0.04
 C6F-C4F \\sim C6G-C4G
 with sigma of 0.04
 C24D-H25D \\sim C24H-H25H
 with sigma of 0.04
 C6F-C2F \\sim C6G-C2G
 with sigma of 0.04
 C27D-N28D \\sim C27H-N28H
 with sigma of 0.02
 C5F-C3F \\sim C5G-C3G
 with sigma of 0.04
 N29D-C30D \\sim N29H-C30H
 with sigma of 0.02
 C5F-C7F \\sim C5G-C7F
 with sigma of 0.04
 C31D-H31D \\sim C31H-H31H
 with sigma of 0.02
 H5F-C4F \\sim H5G-C4G
 with sigma of 0.04
 Co04-C30D \\sim Co04-C30H
 with sigma of 0.04
 C4F-C2F \\sim C4G-C2G
 with sigma of 0.04
 N29D-C32D \\sim N29H-C32H
 with sigma of 0.04
 C30D-N28D \\sim C30H-N28H
 with sigma of 0.04
 C3F-H2F \\sim C3G-H2G
 with sigma of 0.04
 H31D-C32D \\sim H31H-C32H
 with sigma of 0.04
 Co04-N8F \\sim Co04-N8G
 with sigma of 0.02
 C4F-C3F \\sim C4G-C3G
 with sigma of 0.02
 C6F-C7F \\sim C6F-C7G
 with sigma of 0.02
 N8F-C7F \\sim N8G-C7G
 with sigma of 0.02
 N9F-C10F \\sim N9G-C10G
 with sigma of 0.02
 N9F-C12F \\sim N9G-C12F
 with sigma of 0.02
 C10F-H10F \\sim C10G-H10G
 with sigma of 0.02
 C10F-C11F \\sim C10G-C11G
 with sigma of 0.02
 C11F-C7F \\sim C11G-C7G
 with sigma of 0.02
 C7F-C6G \\sim C7G-C6G
 with sigma of 0.02
 Co04-N9F \\sim Co04-N9G
 with sigma of 0.04
 Co04-C7F \\sim Co04-C7G
 with sigma of 0.04
 C6F-N8F \\sim C6F-N8G
 with sigma of 0.04
 C21D-C22D \\sim C21H-C22H
 with sigma of 0.02
 C6F-C11F \\sim C6F-C11G
 with sigma of 0.04
 C22D-H22D \\sim C22H-H22H
 with sigma of 0.02
 N8F-C10F \\sim N8G-C10G
 with sigma of 0.04
 C23D-C24D \\sim C23H-C24H
 with sigma of 0.02
 N8F-C11F \\sim N8G-C11G
 with sigma of 0.04
 C24D-H24D \\sim C24H-H24H
 with sigma of 0.02
 N8F-C12F \\sim N8G-C12F
 with sigma of 0.04
 C25D-H25D \\sim C25H-H25H
 with sigma of 0.02
 N8F-C6G \\sim N8G-C6G
 with sigma of 0.04
 N9F-H10F \\sim N9G-H10G
 with sigma of 0.04
 N20D-C26D \\sim N20D-C26H
 with sigma of 0.04
 N9F-C11F \\sim N9G-C11G
 with sigma of 0.04
 C21D-C23D \\sim C21H-C23H
 with sigma of 0.04
 N9F-C7F \\sim N9G-C7G
 with sigma of 0.04
 C22D-C26D \\sim C22H-C26H
 with sigma of 0.04
 C10F-C7F \\sim C10G-C7G
 with sigma of 0.04
 H22D-C23D \\sim H22H-C23H
 with sigma of 0.04
 C10F-C12F \\sim C10G-C12F
 with sigma of 0.04
 C23D-C25D \\sim C23H-C25H
 with sigma of 0.04
 H10F-C11F \\sim H10G-C11G
 with sigma of 0.04
 C24D-C26D \\sim C24H-C26H
 with sigma of 0.04
 C11F-C6G \\sim C11G-C6G
 with sigma of 0.04
 H24D-C25D \\sim H24H-C25H
 with sigma of 0.04
 H25D-C26D \\sim H25H-C26H
 with sigma of 0.04
 C23D-C27D \\sim C23D-C27H
 with sigma of 0.02
 C27D-C23H \\sim C27H-C23H
 with sigma of 0.02
 N29D-N28D \\sim N29H-N28H
 with sigma of 0.02
 C30D-C33D \\sim C30H-C33D
 with sigma of 0.02
 C31D-C32D \\sim C31H-C32H
 with sigma of 0.02
 C32D-N28D \\sim C32H-N28H
 with sigma of 0.02
 Co04-N28D \\sim Co04-N28H
 with sigma of 0.04
 C27D-N29D \\sim C27H-N29H
 with sigma of 0.04
 N29D-C31D \\sim N29H-C31H
 with sigma of 0.04
 N29D-C33D \\sim N29H-C33D
 with sigma of 0.04
 C30D-C32D \\sim C30H-C32H
 with sigma of 0.04
 C31D-H32D \\sim C31H-H32H
 with sigma of 0.04
 C31D-C33D \\sim C31H-C33D
 with sigma of 0.04
 H32D-N28D \\sim H32H-N28H
 with sigma of 0.04
 N8F-N9F \\sim N8G-N9G
 with sigma of 0.02
 H17F-C18F \\sim H17F-C18G
 with sigma of 0.04
 C16F-H16F \\sim C16G-H16F
 with sigma of 0.02
 C16F-C17F \\sim C16G-C17G
 with sigma of 0.02
 C17F-H17F \\sim C17G-H17F
 with sigma of 0.02
 C17F-C13F \\sim C17G-C13G
 with sigma of 0.04
 C17F-C18F \\sim C17G-C18G
 with sigma of 0.02
 C15F-N19F \\sim C15F-N19G
 with sigma of 0.02
 C18F-H18F \\sim C18G-H18F
 with sigma of 0.02
 C12F-C13F \\sim C12F-C13G
 with sigma of 0.02
 H16F-C17F \\sim H16F-C17G
 with sigma of 0.04
 H18F-C13F \\sim H18F-C13G
 with sigma of 0.04
 C13F-C14F \\sim C13G-C14G
 with sigma of 0.02
 C14F-N19F \\sim C14G-N19F
 with sigma of 0.04
 N20F-C21F \\sim N20G-C21F
 with sigma of 0.02
 C14F-H14F \\sim C14G-H14F
 with sigma of 0.02
 C17F-H18F \\sim C17G-H18F
 with sigma of 0.04
 C18F-C14F \\sim C18G-C14G
 with sigma of 0.04
 C12F-C18F \\sim C12F-C18G
 with sigma of 0.04
 C12F-C14F \\sim C12F-C14G
 with sigma of 0.04
 C15F-H16F \\sim C15G-H16F
 with sigma of 0.04
 C13F-H14F \\sim C13G-H14F
 with sigma of 0.04
 C15F-C17F \\sim C15G-C17G
 with sigma of 0.04
 C15F-C13F \\sim C15G-C13G
 with sigma of 0.04
 C15F-H14F \\sim C15G-H14F
 with sigma of 0.04
 C15F-C16F \\sim C15G-C16G
 with sigma of 0.02
 C15F-C14F \\sim C15G-C14G
 with sigma of 0.02
 N19F-N20F \\sim N19G-N20F
 with sigma of 0.02
 C15F-N19F \\sim C15G-N19F
 with sigma of 0.02
 C16F-H17F \\sim C16G-H17F
 with sigma of 0.04
 N19F-N20F \\sim N19F-N20G
 with sigma of 0.02
 C16F-C18F \\sim C16G-C18G
 with sigma of 0.04
 C16F-C14F \\sim C16G-C14G
 with sigma of 0.04
 C16F-N19F \\sim C16G-N19F
 with sigma of 0.04
 C18F-C13F \\sim C18G-C13G
 with sigma of 0.02
 C21F-N19G \\sim C21G-N19G
 with sigma of 0.02
 C23F-C24F \\sim C23G-C24G
 with sigma of 0.02
 C24F-C25F \\sim C24G-C25G
 with sigma of 0.02
 C25F-C26F \\sim C25G-C26G
 with sigma of 0.02
 C25F-N20G \\sim C25G-N20G
 with sigma of 0.04
 C26F-N20G \\sim C26G-N20G
 with sigma of 0.02
 C23F-C25F \\sim C23G-C25G
 with sigma of 0.04
 N20F-C26F \\sim N20F-C26G
 with sigma of 0.04
 C24F-C26F \\sim C24G-C26G
 with sigma of 0.04
 C21F-C23F \\sim C21G-C23G
 with sigma of 0.04
 C21F-C25F \\sim C21G-C25G
 with sigma of 0.04
 C26F-N19G \\sim C26G-N19G
 with sigma of 0.04
 C21F-C26F \\sim C21G-C26G
 with sigma of 0.02
 C21F-N20G \\sim C21G-N20G
 with sigma of 0.04
 N20F-C21F \\sim N20F-C21G
 with sigma of 0.02
 C22F-C23F \\sim C22G-C23F
 with sigma of 0.02
 C21F-C22F \\sim C21F-C22G
 with sigma of 0.02
 B40X-F44X \\sim B40X-F44Y
 with sigma of 0.02
 B40X-F42X \\sim B40X-F42Y
 with sigma of 0.02
 B40X-F41X \\sim B40X-F41Y
 with sigma of 0.02
 B40X-F43X \\sim B40X-F43Y
 with sigma of 0.02
 F31X-F32X \\sim F31Y-F32Y
 with sigma of 0.04
 F31X-F34X \\sim F31Y-F34Y
 with sigma of 0.04
 F32X-F34X \\sim F32Y-F34Y
 with sigma of 0.04
 F31X-F33X \\sim F31Y-F33Y
 with sigma of 0.04
 F32X-F33X \\sim F32Y-F33Y
 with sigma of 0.04
 F33X-F34X \\sim F33Y-F34Y
 with sigma of 0.04
 B30X-F31X \\sim B30Y-F31Y
 with sigma of 0.02
 B30X-F32X \\sim B30Y-F32Y
 with sigma of 0.02
 B30X-F33X \\sim B30Y-F33Y
 with sigma of 0.02
 B30X-F34X \\sim B30Y-F34Y
 with sigma of 0.02
 F37X-F38X \\sim F37Y-F38Y
 with sigma of 0.04
 F36X-F39X \\sim F36Y-F39Y
 with sigma of 0.04
 F38X-F39X \\sim F38Y-F39Y
 with sigma of 0.04
 F36X-F37X \\sim F36Y-F37Y
 with sigma of 0.04
 F36X-F38X \\sim F36Y-F38Y
 with sigma of 0.04
 F37X-F39X \\sim F37Y-F39Y
 with sigma of 0.04
2. Restrained planarity
 N28D, N29D, C30D, C31D, C32D
 with sigma of 0.1
3. Rigid bond restraints
 N19F, N20F
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim N8A \\sim
N9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim
C16A \\sim C17A \\sim C18A \\sim N19A \\sim N20A \\sim C21A \\sim C22A \\sim
C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim N28A \\sim N29A \\sim
C30A \\sim C31A \\sim C32A \\sim C33A \\sim N34A \\sim C35A \\sim C36A \\sim
C37A \\sim C38A \\sim N1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B
\\sim C7B \\sim N8B \\sim N9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B \\sim
C14B \\sim C15B \\sim C16B \\sim C17B \\sim C18B \\sim N19B \\sim N20B \\sim
C21B \\sim C22B \\sim C23B \\sim C24B \\sim C25B \\sim C26B \\sim C27B \\sim
N28B \\sim N29B \\sim C30B \\sim C31B \\sim C32B \\sim C33B \\sim N34B \\sim
C35B \\sim C36B \\sim C37B \\sim C38B \\sim N1C \\sim C2C \\sim C3C \\sim C4C
\\sim C5C \\sim C6C \\sim N8C \\sim C7C \\sim C11C \\sim C10C \\sim N9C \\sim
C12C \\sim C13C \\sim C14C \\sim C15C \\sim C16C \\sim C17C \\sim C18C \\sim
N19C \\sim N20C \\sim C21C \\sim C22C \\sim C23C \\sim C24C \\sim C25C \\sim
C26C \\sim C27C \\sim N28C \\sim N29C \\sim C30C \\sim C31C \\sim C32C \\sim
C33C \\sim N34C \\sim C35C \\sim C36C \\sim C37C \\sim C38C \\sim N1D \\sim C2D
\\sim C3D \\sim C4D \\sim C5D \\sim C6D \\sim C7D \\sim N8D \\sim N9D \\sim
C10D \\sim C11D \\sim C12D \\sim C13D \\sim C14D \\sim C15D \\sim C16D \\sim
C17D \\sim C18D \\sim N19D \\sim N20D \\sim C21D \\sim C22D \\sim C23D \\sim
C24D \\sim C25D \\sim C26D \\sim C27D \\sim N29D \\sim C30D \\sim C31D \\sim
C32D \\sim N28D \\sim C33D \\sim N34D \\sim C35D \\sim C36D \\sim C37D \\sim
C38D \\sim N1E \\sim C2E \\sim C3E \\sim C4E \\sim C5E \\sim C6E \\sim C7E
\\sim N8E \\sim N9E \\sim C10E \\sim C11E \\sim C12E \\sim C13E \\sim C14E
\\sim C15E \\sim C16E \\sim C17E \\sim C18E \\sim N19E \\sim N20E \\sim C21E
\\sim C22E \\sim C23E \\sim C24E \\sim C25E \\sim C26E \\sim C27E \\sim N28E
\\sim N29E \\sim C30E \\sim C31E \\sim C32E \\sim C33E \\sim N34E \\sim C35E
\\sim C36E \\sim C37E \\sim C38E \\sim N1F \\sim C6F \\sim C5F \\sim C4F \\sim
C3F \\sim C2F \\sim N8F \\sim N9F \\sim C10F \\sim C11F \\sim C7F \\sim C12F
\\sim C15F \\sim C16F \\sim C17F \\sim C18F \\sim C13F \\sim C14F \\sim N19F
\\sim N20F \\sim C21F \\sim C22F \\sim C23F \\sim C24F \\sim C25F \\sim C26F
\\sim C27F \\sim N28F \\sim N29F \\sim C30F \\sim C31F \\sim C32F \\sim C33F
\\sim N34F \\sim C35F \\sim C36F \\sim C37F \\sim C38F \\sim N1G \\sim C2G
\\sim C3G \\sim C4G \\sim C5G \\sim C6G \\sim C7G \\sim N8G \\sim N9G \\sim
C10G \\sim C11G \\sim C13G \\sim C14G \\sim C15G \\sim C16G \\sim C17G \\sim
C18G \\sim N19G \\sim N20G \\sim C21G \\sim C22G \\sim C23G \\sim C24G \\sim
C25G \\sim C26G \\sim C21H \\sim C22H \\sim C23H \\sim C24H \\sim C25H \\sim
C26H \\sim C27H \\sim N28H \\sim N29H \\sim C30H \\sim C31H \\sim C32H \\sim
O1S \\sim C2S \\sim O3S \\sim C4S \\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 F26Y \\sim F27Y \\sim F28Y \\sim F29Y \\sim B30X
\\sim F31X \\sim F32X \\sim F33X \\sim F34X \\sim B35X \\sim F36X \\sim F37X
\\sim F38X \\sim F39X \\sim F36Y \\sim F37Y \\sim F38Y \\sim F39Y \\sim B40X
\\sim F41X \\sim F42X \\sim F43X \\sim F44X \\sim F41Y \\sim F42Y \\sim F43Y
\\sim F44Y \\sim B45X \\sim F46X \\sim F47X \\sim F48X \\sim F49X \\sim B30Y
\\sim F31Y \\sim F32Y \\sim F33Y \\sim F34Y: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
H32H \\sim H31H \\sim N28H \\sim N29H \\sim C30H \\sim C31H \\sim C32H: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 N1A, C2A, C3A, C4A, C5A, C6A, C7A, N8A, N9A, C10A, C11A, C12A, C13A, C14A,
 C15A, C16A, C17A, C18A, N19A, N20A, C21A, C22A, C23A, C24A, C25A, C26A, C27A,
 N28A, N29A, C30A, C31A, C32A, C33A, N34A, C35A, C36A, C37A, C38A, N1B, C2B,
 C3B, C4B, C5B, C6B, C7B, N8B, N9B, C10B, C11B, C12B, C13B, C14B, C15B, C16B,
 C17B, C18B, N19B, N20B, C21B, C22B, C23B, C24B, C25B, C26B, C27B, N28B, N29B,
 C30B, C31B, C32B, C33B, N34B, C35B, C36B, C37B, C38B, N1C, C2C, C3C, C4C, C5C,
 C6C, N8C, C7C, C11C, C10C, N9C, C12C, C13C, C14C, C15C, C16C, C17C, C18C, N19C,
  N20C, C21C, C22C, C23C, C24C, C25C, C26C, C27C, N28C, N29C, C30C, C31C, C32C,
 C33C, N34C, C35C, C36C, C37C, C38C, N1D, C2D, C3D, C4D, C5D, C6D, C7D, N8D,
 N9D, C10D, C11D, C12D, C13D, C14D, C15D, C16D, C17D, C18D, N19D, N20D, C21D,
 C22D, C23D, C24D, C25D, C26D, C27D, N29D, C30D, C31D, C32D, N28D, C33D, N34D,
 C35D, C36D, C37D, C38D, N1E, C2E, C3E, C4E, C5E, C6E, C7E, N8E, N9E, C10E,
 C11E, C12E, C13E, C14E, C15E, C16E, C17E, C18E, N19E, N20E, C21E, C22E, C23E,
 C24E, C25E, C26E, C27E, N28E, N29E, C30E, C31E, C32E, C33E, N34E, C35E, C36E,
 C37E, C38E, N1F, C6F, C5F, C4F, C3F, C2F, N8F, N9F, C10F, C11F, C7F, C12F,
 C15F, C16F, C17F, C18F, C13F, C14F, N19F, N20F, C21F, C22F, C23F, C24F, C25F,
 C26F, C27F, N28F, N29F, C30F, C31F, C32F, C33F, N34F, C35F, C36F, C37F, C38F,
 N1G, C2G, C3G, C4G, C5G, C6G, C7G, N8G, N9G, C10G, C11G, C13G, C14G, C15G,
 C16G, C17G, C18G, N19G, N20G, C21G, C22G, C23G, C24G, C25G, C26G, C21H, C22H,
 C23H, C24H, C25H, C26H, C27H, N28H, N29H, C30H, C31H, C32H, O1S, C2S, O3S, C4S,
  B10X, F11X, F12X, F13X, F14X, B15X, F16X, F17X, F18X, F19X, B20X, F21X, F22X,
 F23X, F24X, B25X, F26X, F27X, F28X, F29X, F26Y, F27Y, F28Y, F29Y, B30X, F31X,
 F32X, F33X, F34X, B35X, F36X, F37X, F38X, F39X, F36Y, F37Y, F38Y, F39Y, B40X,
 F41X, F42X, F43X, F44X, F41Y, F42Y, F43Y, F44Y, B45X, F46X, F47X, F48X, F49X,
 B30Y, F31Y, F32Y, F33Y, F34Y
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{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}
{F11X, F12X, F13X, F14X} sigma for 1-2: 0.02, 1-3: 0.04
as in
{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
{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
{B45X, F46X, F47X, F48X, F49X}
7. Others
 Sof(B20X)=Sof(F21X)=Sof(F22X)=Sof(F23X)=Sof(F24X)=FVAR(1)
 Sof(O3S)=Sof(H3S)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=FVAR(2)
 Sof(F26Y)=Sof(F27Y)=Sof(F28Y)=Sof(F29Y)=1-FVAR(3)
 Sof(F26X)=Sof(F27X)=Sof(F28X)=Sof(F29X)=FVAR(3)
 Sof(N1G)=Sof(C2G)=Sof(H2G)=Sof(C3G)=Sof(H3G)=Sof(C4G)=Sof(H4G)=Sof(C5G)=
 Sof(H5G)=Sof(C6G)=1-FVAR(4)
 Sof(N1F)=Sof(C6F)=Sof(C5F)=Sof(H5F)=Sof(C4F)=Sof(H4F)=Sof(C3F)=Sof(H3F)=
 Sof(C2F)=Sof(H2F)=FVAR(4)
 Sof(C7G)=Sof(N8G)=Sof(N9G)=Sof(C10G)=Sof(H10G)=Sof(C11G)=Sof(H11G)=1-FVAR(5)
 Sof(N8F)=Sof(N9F)=Sof(C10F)=Sof(H10F)=Sof(C11F)=Sof(H11F)=Sof(C7F)=FVAR(5)
 Sof(C21H)=Sof(C22H)=Sof(H22H)=Sof(C23H)=Sof(C24H)=Sof(H24H)=Sof(C25H)=
 Sof(H25H)=Sof(C26H)=Sof(H26H)=1-FVAR(6)
 Sof(C21D)=Sof(C22D)=Sof(H22D)=Sof(C23D)=Sof(C24D)=Sof(H24D)=Sof(C25D)=
 Sof(H25D)=Sof(C26D)=Sof(H26D)=FVAR(6)
 Sof(C27H)=Sof(H27M)=Sof(H27N)=Sof(N28H)=Sof(N29H)=Sof(C30H)=Sof(C31H)=
 Sof(H31H)=Sof(C32H)=Sof(H32H)=1-FVAR(7)
 Sof(C27D)=Sof(H27G)=Sof(H27H)=Sof(N29D)=Sof(C30D)=Sof(C31D)=Sof(H31D)=
 Sof(C32D)=Sof(H32D)=Sof(N28D)=FVAR(7)
 Sof(C13G)=Sof(H13G)=Sof(C14G)=Sof(H14G)=Sof(C15G)=Sof(C16G)=Sof(H16G)=
 Sof(C17G)=Sof(H17G)=Sof(C18G)=Sof(H18G)=1-FVAR(8)
 Sof(C15F)=Sof(C16F)=Sof(H16F)=Sof(C17F)=Sof(H17F)=Sof(C18F)=Sof(H18F)=
 Sof(C13F)=Sof(C14F)=Sof(H14F)=FVAR(8)
 Sof(N19G)=1-FVAR(9)
 Sof(N19F)=Sof(N20F)=FVAR(9)
 Sof(C21G)=Sof(C22G)=Sof(H22G)=Sof(C23G)=Sof(C24G)=Sof(H24G)=Sof(C25G)=
 Sof(H25G)=Sof(C26G)=Sof(H26G)=1-FVAR(10)
 Sof(C21F)=Sof(C22F)=Sof(H22F)=Sof(C23F)=Sof(C24F)=Sof(H24F)=Sof(C25F)=
 Sof(H25F)=Sof(C26F)=Sof(H26F)=FVAR(10)
 Sof(F41Y)=Sof(F42Y)=Sof(F43Y)=Sof(F44Y)=1-FVAR(11)
 Sof(F41X)=Sof(F42X)=Sof(F43X)=Sof(F44X)=FVAR(11)
 Sof(B30Y)=Sof(F31Y)=Sof(F32Y)=Sof(F33Y)=Sof(F34Y)=1-FVAR(12)
 Sof(B30X)=Sof(F31X)=Sof(F32X)=Sof(F33X)=Sof(F34X)=FVAR(12)
 Sof(F36Y)=Sof(F37Y)=Sof(F38Y)=Sof(F39Y)=1-FVAR(13)
 Sof(F36X)=Sof(F37X)=Sof(F38X)=Sof(F39X)=FVAR(13)
8.a Secondary CH2 refined with riding coordinates:
 C12A(H12A,H12B), C27A(H27A,H27B), C12B(H12C,H12D), C27B(H27C,H27D), C12C(H12E,
 H12F), C27C(H27E,H27F), C12D(H12G,H12H), C27D(H27G,H27H), C12E(H12I,H12J),
 C27E(H27I,H27J), C12F(H12K,H12L), C27H(H27M,H27N)
8.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C10A(H10A), C11A(H11A), C14A(H14A),
 C16A(H16A), C17A(H17A), C18A(H18A), C22A(H22A), C23A(H23A), C24A(H24A),
 C26A(H26A), C31A(H31A), C32A(H32A), C35A(H35A), C36A(H36A), C37A(H37A),
 C38A(H38A), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C10B(H10B), C11B(H11B),
 C14B(H14B), C15B(H15B), C16B(H16B), C18B(H18B), C22B(H22B), C24B(H24B),
 C25B(H25B), C26B(H26B), C31B(H31B), C32B(H32B), C35B(H35B), C36B(H36B),
 C37B(H37B), C38B(H38B), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C), C11C(H11C),
 C10C(H10C), C14C(H14C), C16C(H16C), C17C(H17C), C18C(H18C), C22C(H22C),
 C24C(H24C), C25C(H25C), C26C(H26C), C31C(H31C), C32C(H32C), C35C(H35C),
 C36C(H36C), C37C(H37C), C38C(H38C), C3D(H3D), C4D(H4D), C5D(H5D), C6D(H6D),
 C10D(H10D), C11D(H11D), C14D(H14D), C16D(H16D), C17D(H17D), C18D(H18D),
 C22D(H22D), C24D(H24D), C25D(H25D), C26D(H26D), C31D(H31D), C32D(H32D),
 C35D(H35D), C36D(H36D), C37D(H37D), C38D(H38D), C2E(H2E), C3E(H3E), C4E(H4E),
 C5E(H5E), C10E(H10E), C11E(H11E), C14E(H14E), C16E(H16E), C17E(H17E),
 C18E(H18E), C22E(H22E), C24E(H24E), C25E(H25E), C26E(H26E), C31E(H31E),
 C32E(H32E), C35E(H35E), C36E(H36E), C37E(H37E), C38E(H38E), C5F(H5F), C4F(H4F),
  C3F(H3F), C2F(H2F), C10F(H10F), C11F(H11F), C16F(H16F), C17F(H17F),
 C18F(H18F), C14F(H14F), C22F(H22F), C24F(H24F), C25F(H25F), C26F(H26F),
 C31F(H31F), C32F(H32F), C35F(H35F), C36F(H36F), C37F(H37F), C38F(H38F),
 C3G(H3G), C4G(H4G), C5G(H5G), C10G(H10G), C11G(H11G), C13G(H13G), C14G(H14G),
 C16G(H16G), C17G(H17G), C18G(H18G), C22G(H22G), C24G(H24G), C25G(H25G),
 C26G(H26G), C22H(H22H), C24H(H24H), C25H(H25H), C26H(H26H), C31H(H31H),
 C32H(H32H)
8.c Fitted pentagon refined as free rotating group:
 N8C(C7C,C11C,C10C,N9C), N29D(C30D,C31D,C32D,N28D), N8F(N9F,C10F,C11F,C7F)
8.d Fitted hexagon refined as free rotating group:
 N1C(C2C,C3C,C4C,C5C,C6C), N1F(C6F,C5F,C4F,C3F,C2F), C15F(C16F,C17F,C18F,C13F,
 C14F)
8.e Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
8.f Idealised tetrahedral OH refined as rotating group:
 O1S(H1S), O3S(H3S)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 521 electrons were 
found in a volume of 1754\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
0.4[BF4], 8[CH4O], 4[H2O], 1[CH4O], 1[H2O], 1[CH4O], 1[H2O] per Formula Unit 
which account for 513 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80608
_shelx_fab_checksum              97678
_olex2_date_sample_data_collection 2022-08-08
_olex2_date_sample_submission    2022-08-01
_olex2_exptl_crystal_mounting_method
'Crystals were transferred to Fomblin oil before a crystal was mounted on a MiteGen Microloop and flash frozen under liquid nitrogen for storage.'
_olex2_submission_original_sample_id MT7_844
_olex2_submission_special_instructions 'No special instructions were received'