Helical aromatic foldamers with tubular cavities capable of accommodating multiple halide ions.
Lee, Seungwon; Lee, Byeung Ju; Song, Geunmoo; Jeong, Kyu-Sung; Chemical communications (Cambridge, England) 60 (2024) 14081–14084; doi:10.1039/d4cc05474a

data_7133950
_publ_section_title
;
 Helical aromatic foldamers with tubular cavities capable of accommodating
 multiple halide ions.
;
_journal_issue                   95
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14081
_journal_page_last               14084
_journal_paper_doi               10.1039/d4cc05474a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '8(I), C258 H121 N22, H2 O'
_chemical_formula_sum            'C258 H123 I8 N22 O'
_chemical_formula_weight         4561.98
_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             2024-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-09 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                104.05(3)
_cell_angle_beta                 103.30(3)
_cell_angle_gamma                116.80(3)
_cell_formula_units_Z            2
_cell_length_a                   25.200(5)
_cell_length_b                   25.207(5)
_cell_length_c                   29.256(6)
_cell_measurement_reflns_used    179924
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.458
_cell_volume                     14803(9)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.800000
_diffrn_reflns_av_R_equivalents  0.2634
_diffrn_reflns_av_unetI/netI     0.5391
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            88769
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.111
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.024
_exptl_crystal_description       needle
_exptl_crystal_F_000             4514
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.694
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2030
_refine_ls_number_reflns         45583
_refine_ls_number_restraints     1838
_refine_ls_restrained_S_all      0.697
_refine_ls_R_factor_all          0.3728
_refine_ls_R_factor_gt           0.1292
_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^)+(0.1961P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3323
_refine_ls_wR_factor_ref         0.4456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5193
_reflns_number_total             45583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05474a2.cif
_cod_data_source_block           lsw15x_a
_cod_depositor_comments
'Adding full bibliography for 7133949--7133951.cif.'
_cod_original_cell_volume        14802(7)
_cod_database_code               7133950
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Restrained distances
 O1-H1B
 0.845 with sigma of 0.02
 C220-C183
 1.4 with sigma of 0.002
 C185-C221
 1.43 with sigma of 0.002
 C2-N3
 1.38 with sigma of 0.002
 C228-C226
 2.54 with sigma of 0.002
 C226-C227
 2.54 with sigma of 0.002
 C197-C142
 2.4 with sigma of 0.002
 H1A-O1
 0.845 with sigma of 0.02
 C225-C226
 1.55 with sigma of 0.002
 C197-C141
 1.43 with sigma of 0.002
 C210-C209
 1.1 with sigma of 0.002
 C164-C209
 1.42 with sigma of 0.002
 C81-C214
 1.45 with sigma of 0.002
 C210-C61
 1.42 with sigma of 0.002
 N63-C64
 1.38 with sigma of 0.002
 N46-C47
 1.38 with sigma of 0.002
 C82-N83
 1.38 with sigma of 0.002
 C97-C96
 1.45 with sigma of 0.002
 C62-N63
 1.38 with sigma of 0.002
 C53-C52
 1.45 with sigma of 0.002
 C76-N63
 2.29 with sigma of 0.002
 N83-C97
 2.29 with sigma of 0.002
 C77-N63
 2.29 with sigma of 0.002
 N46-C52
 2.29 with sigma of 0.002
 H1A-H1B
 1.35 with sigma of 0.008
 C48-C207
 1.43 with sigma of 0.002
 C245-C50
 1.55 with sigma of 0.002
 C257-C99
 1.55 with sigma of 0.002
 C99-C260
 2.54 with sigma of 0.002
 C259-C99
 2.54 with sigma of 0.002
 C258-C99
 2.54 with sigma of 0.002
 C264-C261
 1.55 with sigma of 0.002
 C88-C215
 1.45 with sigma of 0.002
 C261-C263
 1.55 with sigma of 0.002
 C263-C262
 2.45 with sigma of 0.002
 C264-C262
 2.45 with sigma of 0.002
 C264-C263
 2.45 with sigma of 0.002
 C65-N66
 1.38 with sigma of 0.002
 N66-C67
 1.38 with sigma of 0.002
 N66-C72
 2.29 with sigma of 0.002
 C73-N66
 2.29 with sigma of 0.002
 C275-C273
 1.55 with sigma of 0.002
 C80-C249
 2.55 with sigma of 0.002
 C70-C253
 1.55 with sigma of 0.002
 C249-C78
 2.55 with sigma of 0.002
 C262-C261
 1.55 with sigma of 0.002
 C30-C237
 1.55 with sigma of 0.002
 C79-C249
 1.55 with sigma of 0.002
 C274-C275
 2.45 with sigma of 0.002
 C251-C249
 1.55 with sigma of 0.002
 C275-C276
 2.45 with sigma of 0.002
 C237-C238
 1.55 with sigma of 0.002
 C252-C249
 1.55 with sigma of 0.002
 C254-C253
 1.55 with sigma of 0.002
 C249-C250
 1.55 with sigma of 0.002
 C253-C255
 1.55 with sigma of 0.002
 C237-C239
 1.55 with sigma of 0.002
 C253-C256
 1.55 with sigma of 0.002
 C237-C240
 1.55 with sigma of 0.002
 C17-C16
 1.45 with sigma of 0.002
 N3-C17
 2.29 with sigma of 0.002
 C1-C198
 1.43 with sigma of 0.002
 N3-C4
 1.38 with sigma of 0.002
 C5-N6
 1.38 with sigma of 0.002
 N6-C7
 1.38 with sigma of 0.002
 C24-N23
 1.38 with sigma of 0.002
 N23-C22
 1.38 with sigma of 0.002
 C25-N26
 1.38 with sigma of 0.002
 N26-C27
 1.38 with sigma of 0.002
 N43-C42
 1.38 with sigma of 0.002
 N43-C44
 1.38 with sigma of 0.002
 C45-N46
 1.38 with sigma of 0.002
 N83-C84
 1.38 with sigma of 0.002
 N86-C85
 1.38 with sigma of 0.002
 N86-C87
 1.38 with sigma of 0.002
 C102-N103
 1.38 with sigma of 0.002
 N103-C104
 1.38 with sigma of 0.002
 C105-N106
 1.38 with sigma of 0.002
 N106-C107
 1.38 with sigma of 0.002
 C122-N123
 1.38 with sigma of 0.002
 C124-N123
 1.38 with sigma of 0.002
 C125-N126
 1.38 with sigma of 0.002
 N126-C127
 1.38 with sigma of 0.002
 C13-C12
 1.45 with sigma of 0.002
 C32-C33
 1.45 with sigma of 0.002
 C36-C37
 1.45 with sigma of 0.002
 C57-C56
 1.45 with sigma of 0.002
 C77-C76
 1.45 with sigma of 0.002
 C73-C72
 1.45 with sigma of 0.002
 C93-C92
 1.45 with sigma of 0.002
 C117-C116
 1.45 with sigma of 0.002
 C113-C112
 1.45 with sigma of 0.002
 C137-C136
 1.45 with sigma of 0.002
 C133-C132
 1.45 with sigma of 0.002
 N6-C13
 2.29 with sigma of 0.002
 N6-C12
 2.29 with sigma of 0.002
 N3-C16
 2.29 with sigma of 0.002
 N26-C32
 2.29 with sigma of 0.002
 C53-N46
 2.29 with sigma of 0.002
 N83-C96
 2.29 with sigma of 0.002
 C133-N126
 2.29 with sigma of 0.002
 C132-N126
 2.29 with sigma of 0.002
 C136-N123
 2.29 with sigma of 0.002
 C137-N123
 2.29 with sigma of 0.002
 C28-C203
 1.43 with sigma of 0.002
 C155-C204
 1.43 with sigma of 0.002
 C206-C41
 1.43 with sigma of 0.002
 C208-C162
 1.43 with sigma of 0.002
 C216-C176
 1.43 with sigma of 0.002
 C178-C217
 1.43 with sigma of 0.002
 C218-C101
 1.43 with sigma of 0.002
 C108-C219
 1.43 with sigma of 0.002
 C222-C121
 1.43 with sigma of 0.002
 C190-C224
 1.43 with sigma of 0.002
 C223-C128
 1.43 with sigma of 0.002
 C8-C199
 1.43 with sigma of 0.002
 C200-C148
 1.43 with sigma of 0.002
 C150-C201
 1.43 with sigma of 0.002
 C202-C21
 1.43 with sigma of 0.002
 C241-C59
 1.55 with sigma of 0.002
 C19-C225
 1.55 with sigma of 0.002
 C10-C229
 1.55 with sigma of 0.002
 C265-C119
 1.55 with sigma of 0.002
 N86-C92
 2.29 with sigma of 0.002
 N106-C113
 2.29 with sigma of 0.002
 C112-N106
 2.29 with sigma of 0.002
 C224-C191
 2.45 with sigma of 0.002
 C273-C139
 1.55 with sigma of 0.002
 C276-C273
 1.55 with sigma of 0.002
 C273-C274
 1.55 with sigma of 0.002
 C277-C130
 1.55 with sigma of 0.002
 C257-C258
 1.55 with sigma of 0.002
 N173-C175
 1.47 with sigma of 0.002
 C229-C230
 1.55 with sigma of 0.002
 C231-C229
 1.55 with sigma of 0.002
 C232-C229
 1.55 with sigma of 0.002
 C225-C228
 1.55 with sigma of 0.002
 C277-C278
 1.55 with sigma of 0.002
 C257-C260
 1.55 with sigma of 0.002
 C241-C243
 1.55 with sigma of 0.002
 C241-C244
 1.55 with sigma of 0.002
 C245-C247
 1.55 with sigma of 0.002
 C245-C248
 1.55 with sigma of 0.002
 C245-C246
 1.55 with sigma of 0.002
 C231-C232
 2.46 with sigma of 0.002
 C231-C230
 2.46 with sigma of 0.002
 C230-C232
 2.46 with sigma of 0.002
 C244-C243
 2.46 with sigma of 0.002
 C242-C244
 2.46 with sigma of 0.002
 C243-C242
 2.46 with sigma of 0.002
 C277-C279
 1.55 with sigma of 0.002
 C277-C280
 1.55 with sigma of 0.002
 C278-C280
 2.45 with sigma of 0.002
 C278-C279
 2.45 with sigma of 0.002
 C280-C279
 2.45 with sigma of 0.002
 C277-C129
 2.55 with sigma of 0.002
 C277-C131
 2.55 with sigma of 0.002
 C265-C267
 1.55 with sigma of 0.002
 C265-C266
 1.55 with sigma of 0.002
 C265-C268
 1.55 with sigma of 0.002
 C118-C265
 2.55 with sigma of 0.002
 C265-C120
 2.55 with sigma of 0.002
 C267-C266
 2.45 with sigma of 0.002
 C267-C268
 2.45 with sigma of 0.002
 C266-C268
 2.45 with sigma of 0.002
 C254-C255
 2.45 with sigma of 0.002
 C254-C256
 2.45 with sigma of 0.002
 C255-C256
 2.45 with sigma of 0.002
 C239-C238
 2.45 with sigma of 0.002
 C238-C240
 2.45 with sigma of 0.002
 C239-C240
 2.45 with sigma of 0.002
 C110-C269
 1.55 with sigma of 0.002
 C270-C269
 1.55 with sigma of 0.002
 C272-C269
 1.55 with sigma of 0.002
 C271-C269
 1.55 with sigma of 0.002
 C272-C270
 2.54 with sigma of 0.002
 C270-C271
 2.54 with sigma of 0.002
 C271-C272
 2.54 with sigma of 0.002
 C228-C227
 2.54 with sigma of 0.002
 C225-C227
 1.55 with sigma of 0.002
 C225-C18
 2.55 with sigma of 0.002
 C225-C20
 2.55 with sigma of 0.002
 C234-C236
 2.45 with sigma of 0.002
 C235-C234
 2.45 with sigma of 0.002
 C235-C236
 2.45 with sigma of 0.002
 C250-C252
 2.45 with sigma of 0.002
 C251-C252
 2.45 with sigma of 0.002
 C251-C250
 2.45 with sigma of 0.002
 C274-C276
 2.45 with sigma of 0.002
 C257-C259
 1.55 with sigma of 0.002
 C261-C90
 1.54 with sigma of 0.002
 C91-C261
 2.55 with sigma of 0.002
 C89-C261
 2.55 with sigma of 0.002
 C259-C257
 1.55 with sigma of 0.002
 C241-C242
 1.55 with sigma of 0.002
 C39-C233
 1.55 with sigma of 0.002
 C233-C236
 1.55 with sigma of 0.002
 C233-C235
 1.55 with sigma of 0.002
 C233-C234
 1.55 with sigma of 0.002
 C236-C235
 2.45 with sigma of 0.002
 C236-C234
 2.45 with sigma of 0.002
 C234-C235
 2.45 with sigma of 0.002
 C38-C233
 2.55 with sigma of 0.002
 C40-C233
 2.55 with sigma of 0.002
 C154-N152
 1.47 with sigma of 0.002
 N43-C57
 2.29 with sigma of 0.002
 N43-C56
 2.29 with sigma of 0.002
 C212-C169
 1.45 with sigma of 0.002
 C171-C213
 1.45 with sigma of 0.002
 C70-C255
 2.51 with sigma of 0.002
 C70-C256
 2.51 with sigma of 0.002
 C70-C254
 2.51 with sigma of 0.002
 C253-C67
 4.33 with sigma of 0.002
 N192-C196
 1.45 with sigma of 0.002
 C196-C193
 2.4 with sigma of 0.002
 C144-C147
 2.4 with sigma of 0.002
 N143-C147
 1.46 with sigma of 0.002
2. Restrained planarity
 N86, C87, C92, C93, C85, N83, C84, C96, C95, C94, C97, C82
 with sigma of 0.01
3. Rigid bond restraints
 C188, C183, C220, C219
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C198, C197, C141, C142, N143, C144, C145, C146
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N159, C160, C155, C156, C157, C158
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C240, C238, C237, C239
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C18, C19, C20, C1, C17, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C279, C278, C277, C280
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C265, C267, C268, C266, C119, C118, C120
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C253, C254, C255, C256
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C249, C251, C252, C250
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C255, C253, C254, C256
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C233, C234, C235, C236
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C182, N180, C181, C176, C177, C178, C179
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C273, C275, C276, C274
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C232, C229, C231, C230
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C226, C225, C19, C18, C17, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C219 \\sim C220: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
N159 \\sim C160 \\sim C155 \\sim C156 \\sim C157 \\sim C158: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C237 \\sim C239 \\sim C240 \\sim C238: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
C253 \\sim C255 \\sim C254 \\sim C256: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
C233 \\sim C234 \\sim C235 \\sim C236: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
C177 \\sim C176 \\sim C181 \\sim C178 \\sim C179 \\sim N180 \\sim C182: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
C275 \\sim C274 \\sim C276 \\sim C273: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
C231 \\sim C230 \\sim C229 \\sim C232: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
H1A \\sim O1 \\sim H1B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
Uanis(C188) \\sim Ueq, Uanis(C183) \\sim Ueq, Uanis(C184) \\sim Ueq,
Uanis(C185) \\sim Ueq, Uanis(C186) \\sim Ueq, Uanis(N187) \\sim Ueq,
Uanis(C189) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C220) \\sim Ueq, Uanis(C219) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C210) \\sim Ueq, Uanis(C209) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C198) \\sim Ueq, Uanis(C197) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N63) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C81) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C100) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C99) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C82) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C97) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C98) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N143) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C141) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C142) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C146) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C145) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N166) \\sim Ueq, Uanis(C167) \\sim Ueq, Uanis(C162) \\sim Ueq,
Uanis(C164) \\sim Ueq, Uanis(C165) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C144) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C215) \\sim Ueq, Uanis(C216) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C211) \\sim Ueq, Uanis(C212) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C213) \\sim Ueq, Uanis(C214) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N66) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C273) \\sim Ueq, Uanis(C276) \\sim Ueq, Uanis(C274) \\sim Ueq,
Uanis(C275) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.0091 and sigma for terminal atoms of 0.00192
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N86) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N106) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N152) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N192) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C190) \\sim Ueq, Uanis(C195) \\sim Ueq, Uanis(C194) \\sim Ueq,
Uanis(C191) \\sim Ueq, Uanis(C193) \\sim Ueq, Uanis(C196) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C147) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C199) \\sim Ueq, Uanis(C200) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C153) \\sim Ueq, Uanis(C148) \\sim Ueq, Uanis(C149) \\sim Ueq,
Uanis(C150) \\sim Ueq, Uanis(C151) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C154) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N159) \\sim Ueq, Uanis(C160) \\sim Ueq, Uanis(C155) \\sim Ueq,
Uanis(C156) \\sim Ueq, Uanis(C157) \\sim Ueq, Uanis(C158) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C205) \\sim Ueq, Uanis(C206) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N126) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C208) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C80) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C75) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C64) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C72) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C163) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C174) \\sim Ueq, Uanis(C169) \\sim Ueq, Uanis(C170) \\sim Ueq,
Uanis(C171) \\sim Ueq, Uanis(C172) \\sim Ueq, Uanis(N173) \\sim Ueq,
Uanis(C175) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C96) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C91) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C88)
\\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C92) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C177) \\sim Ueq, Uanis(C178) \\sim Ueq, Uanis(C179) \\sim Ueq,
Uanis(N180) \\sim Ueq, Uanis(C182) \\sim Ueq, Uanis(C181) \\sim Ueq,
Uanis(C176) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C217) \\sim Ueq, Uanis(C218) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C120) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C101) \\sim Ueq,
Uanis(C102) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C118) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C116) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C112) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C107) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C223) \\sim Ueq, Uanis(C224) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C222) \\sim Ueq, Uanis(C221) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C139) \\sim Ueq, Uanis(C138) \\sim Ueq, Uanis(C137) \\sim Ueq,
Uanis(C122) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C140) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C135) \\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C134) \\sim Ueq,
Uanis(C133) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C124) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C128) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C132) \\sim Ueq,
Uanis(C131) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C129) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C230) \\sim Ueq, Uanis(C229) \\sim Ueq, Uanis(C232) \\sim Ueq,
Uanis(C231) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N46) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C207) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N83) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C168) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(I4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(I1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(I3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(I2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Ueq(O1): fixed at 0.25 with sigma of 0.1
5.a Aromatic/amide H refined with riding coordinates:
 N83(H83), C118(H118), C120(H120), N103(H103), N3(H3), C170(H170), C172(H172),
 C174(H174), N106(H106), C98(H98), C100(H100), N46(H46), N123(H123), N6(H6),
 C34(H34), C35(H35), C71(H71), C69(H69), N63(H63), C163(H163), C165(H165),
 C167(H167), C138(H138), C140(H140), N86(H86), C109(H109), C111(H111), C14(H14),
  C15(H15), C54(H54), C55(H55), C179(H179), C181(H181), C177(H177), C38(H38),
 C40(H40), C149(H149), C151(H151), C153(H153), C78(H78), C80(H80), C9(H9),
 C11(H11), C134(H134), C135(H135), C51(H51), C49(H49), C74(H74), C75(H75),
 C186(H186), C184(H184), C188(H188), C146(H146), C145(H145), C144(H144),
 C142(H142), N66(H66), C94(H94), C95(H95), C156(H156), C160(H160), C158(H158),
 C89(H89), C91(H91), N26(H26), N23(H23), C114(H114), C115(H115), C31(H31),
 C29(H29), N43(H43), C129(H129), C131(H131), C193(H193), C194(H194), C195(H195),
  C191(H191), N126(H126), C58(H58), C60(H60), C20(H20), C18(H18)
5.b Fitted hexagon refined as free rotating group:
 C102(C117,C118,C119,C120,C101), C170(C171,C172,N173,C174,C169), C81(C82,C97,
 C98,C99,C100), C25(C33,C34,C35,C36,C24), C67(C72,C71,C70,C69,C68), C162(C163,
 C164,C165,N166,C167), C121(C122,C137,C138,C139,C140), C107(C108,C109,C110,C111,
 C112), C5(C13,C14,C15,C16,C4), C44(C45,C53,C54,C55,C56), C178(C179,N180,C181,
 C176,C177), C38(C39,C40,C21,C22,C37), C149(C150,C151,N152,C153,C148), C62(C77,
 C78,C79,C80,C61), C8(C9,C10,C11,C12,C7), C124(C125,C133,C134,C135,C136),
 C47(C52,C51,C50,C49,C48), C64(C65,C73,C74,C75,C76), N187(C186,C185,C184,C183,
 C188), C141(C146,C145,C144,N143,C142), C96(C84,C85,C93,C94,C95), C157(C156,
 C155,C160,N159,C158), C88(C89,C90,C91,C92,C87), C104(C105,C113,C114,C115,C116),
  C31(C32,C27,C28,C29,C30), C127(C128,C129,C130,C131,C132), N192(C193,C194,C195,
 C190,C191), C41(C42,C57,C58,C59,C60), C19(C20,C1,C2,C17,C18)
5.c Idealised Me refined as rotating group:
 C196(H19A,H19B,H19C), C147(H14A,H14B,H14C), C175(H17A,H17B,H17C), C189(H18A,
 H18B,H18C), C154(H15A,H15B,H15C), C275(H27A,H27B,H27C), C168(H16A,H16B,H16C),
 C274(H27D,H27E,H27F), C182(H18D,H18E,H18F), C232(H23A,H23B,H23C), C231(H23D,
 H23E,H23F), C276(H27G,H27H,H27I), C230(H23G,H23H,H23I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86038
_shelx_hkl_checksum              71083
_shelx_fab_checksum              59971
_olex2_submission_special_instructions 'No special instructions were received'