Thermal decomposition of DMSO or DMF solvates: an advanced method for obtaining new hybrid bismuth(iii) halides
Dudko, Ekaterina M.; Buikin, Petr A.; Ilyukhin, Andey B.; Korlyukov, Alexander A.; Dorovatovskii, Pavel V.; Simonenko, Nikolai P.; Kotov, Vitalii Yu.; CrystEngComm 26 (2024) 3490–3500; doi:10.1039/D4CE00279B

data_7248701
_publ_section_title
;
 Thermal decomposition of DMSO or DMF solvates: an advanced method for
 obtaining new hybrid bismuth(iii) halides
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3490
_journal_page_last               3500
_journal_paper_doi               10.1039/D4CE00279B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '4(Bi I6), 6(C18 H18 N2), 4(C3 H7 N O)'
_chemical_formula_sum            'C120 H136 Bi4 I24 N16 O4'
_chemical_formula_weight         5747.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-04-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.399(2)
_cell_length_b                   21.812(2)
_cell_length_c                   32.531(3)
_cell_measurement_reflns_used    137650
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      26.311
_cell_measurement_theta_min      1.566
_cell_volume                     15894(3)
_computing_data_collection       'Bruker APEX3'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            216605
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.446
_exptl_absorpt_coefficient_mu    9.126
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_correction_T_min  0.379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.402
_exptl_crystal_description       irregular
_exptl_crystal_F_000             10416
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.579
_refine_diff_density_min         -5.851
_refine_diff_density_rms         0.355
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.503(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         31241
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0751
_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^)+1080.9854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                26987
_reflns_number_total             31241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00279b2.cif
_cod_data_source_block           kotov143
_cod_depositor_comments
'Adding full bibliography for 7248691--7248702.cif.'
_cod_database_code               7248701
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.200
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49742
 0.50258
2. Restrained distances
 O201-C201
 1.2 with sigma of 0.01
 O221-C221
 1.2 with sigma of 0.01
 N221-C222 = N221-C223
 1.45 with sigma of 0.01
 C221-C222
 2.6 with sigma of 0.02
 N221-C221
 1.35 with sigma of 0.01
 C221-C222 = C221-C223
 2.45 with sigma of 0.02
 O231-C231
 1.2 with sigma of 0.01
 N231-C232 = N231-C233
 1.45 with sigma of 0.01
 C231-C232
 2.6 with sigma of 0.02
 O221-N221
 2.26 with sigma of 0.02
 N231-C231
 1.35 with sigma of 0.01
 C231-C232 = C231-C233
 2.45 with sigma of 0.02
 O231-N231
 2.26 with sigma of 0.02
 N201-C202 = N201-C203
 1.45 with sigma of 0.01
 C201-C202
 2.6 with sigma of 0.02
 N201-C201
 1.35 with sigma of 0.01
 C201-C202 = C201-C203
 2.45 with sigma of 0.02
 O201-N201
 2.26 with sigma of 0.02
 O211-C211
 1.2 with sigma of 0.01
 N211-C212 = N211-C213
 1.45 with sigma of 0.01
 C211-C212
 2.6 with sigma of 0.02
 N211-C211
 1.35 with sigma of 0.01
 C211-C212 = C211-C213
 2.45 with sigma of 0.02
 O211-N211
 2.26 with sigma of 0.02
 C6-N1 = C6-C7 = C13-C10 = C13-N2 = C24-N3 = C24-C25 = C31-C28 = C31-N4
 1.54 with sigma of 0.01
 C42-N5 = C42-C43 = C49-C46 = C49-N6 = C60-N7 = C60-C61 = C67-C64 = C67-N8
 1.54 with sigma of 0.01
 C78-N9 = C78-C79 = C85-C82 = C85-N10 = C96-N11 = C96-C97 = C103-C100 = C103-N12
 1.54 with sigma of 0.01
 C6-C1 = C6-C5 = C6-C8 = C6-C12 = C13-C9 = C13-C11 = C13-C14 = C13-C18
 2.5 with sigma of 0.02
 C24-C19 = C24-C23 = C24-C26 = C24-C30 = C31-C27 = C31-C29 = C31-C32 = C31-C36
 2.5 with sigma of 0.02
 C42-C37 = C42-C41 = C42-C44 = C42-C48 = C49-C45 = C49-C47 = C49-C50 = C49-C54
 2.5 with sigma of 0.02
 C60-C55 = C60-C59 = C60-C62 = C60-C66 = C67-C63 = C67-C65 = C67-C68 = C67-C72
 2.5 with sigma of 0.02
 C78-C73 = C78-C79 = C78-C80 = C78-C84 = C85-C81 = C85-C83 = C85-C86 = C85-C90
 2.5 with sigma of 0.02
 C96-C91 = C96-C95 = C96-C98 = C96-C102 = C103-C99 = C103-C101 = C103-C104
 2.5 with sigma of 0.02
 C103-C108
 2.5 with sigma of 0.02
 O231-C231 \\sim O1-C111
 with sigma of 0.02
 N231-C231 \\sim N14-C111
 with sigma of 0.02
 N231-C232 \\sim N14-C1L
 with sigma of 0.02
 N231-C233 \\sim N14-C1K
 with sigma of 0.02
 O231-N231 \\sim O1-N14
 with sigma of 0.04
 C231-C232 \\sim C111-C1L
 with sigma of 0.04
 C231-C233 \\sim C111-C1K
 with sigma of 0.04
 C232-C233 \\sim C1L-C1K
 with sigma of 0.04
 O221-C221 \\sim O2-C110
 with sigma of 0.02
 N221-C221 \\sim N13-C110
 with sigma of 0.02
 N221-C222 \\sim N13-C1J
 with sigma of 0.02
 N221-C223 \\sim N13-C1I
 with sigma of 0.02
 O221-N221 \\sim O2-N13
 with sigma of 0.04
 C221-C222 \\sim C110-C1J
 with sigma of 0.04
 C221-C223 \\sim C110-C1I
 with sigma of 0.04
 C222-C223 \\sim C1J-C1I
 with sigma of 0.04
 N3-C19 \\sim N3A-C19A
 with sigma of 0.02
 N3-C23 \\sim N3A-C23A
 with sigma of 0.02
 N3-C24 \\sim N3A-C24A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 N4-C32 \\sim N4A-C32A
 with sigma of 0.02
 N4-C36 \\sim N4A-C36A
 with sigma of 0.02
 N4-C31 \\sim N4A-C31A
 with sigma of 0.02
 C32-C33 \\sim C32A-C33A
 with sigma of 0.02
 C33-C34 \\sim C33A-C34A
 with sigma of 0.02
 C34-C35 \\sim C34A-C35A
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C25-C26 \\sim C25A-C26A
 with sigma of 0.02
 C25-C30 \\sim C25A-C30A
 with sigma of 0.02
 C25-C24 \\sim C25A-C24A
 with sigma of 0.02
 C26-C27 \\sim C26A-C27A
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A
 with sigma of 0.02
 C28-C29 \\sim C28A-C29A
 with sigma of 0.02
 C28-C31 \\sim C28A-C31A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 N3-C20 \\sim N3A-C20A
 with sigma of 0.04
 N3-C22 \\sim N3A-C22A
 with sigma of 0.04
 N3-C25 \\sim N3A-C25A
 with sigma of 0.04
 C19-C21 \\sim C19A-C21A
 with sigma of 0.04
 C19-C23 \\sim C19A-C23A
 with sigma of 0.04
 C19-C24 \\sim C19A-C24A
 with sigma of 0.04
 C20-C22 \\sim C20A-C22A
 with sigma of 0.04
 C21-C23 \\sim C21A-C23A
 with sigma of 0.04
 C23-C24 \\sim C23A-C24A
 with sigma of 0.04
 N4-C33 \\sim N4A-C33A
 with sigma of 0.04
 N4-C35 \\sim N4A-C35A
 with sigma of 0.04
 N4-C28 \\sim N4A-C28A
 with sigma of 0.04
 C32-C34 \\sim C32A-C34A
 with sigma of 0.04
 C32-C36 \\sim C32A-C36A
 with sigma of 0.04
 C32-C31 \\sim C32A-C31A
 with sigma of 0.04
 C33-C35 \\sim C33A-C35A
 with sigma of 0.04
 C34-C36 \\sim C34A-C36A
 with sigma of 0.04
 C36-C31 \\sim C36A-C31A
 with sigma of 0.04
 C25-C27 \\sim C25A-C27A
 with sigma of 0.04
 C25-C29 \\sim C25A-C29A
 with sigma of 0.04
 C26-C28 \\sim C26A-C28A
 with sigma of 0.04
 C26-C30 \\sim C26A-C30A
 with sigma of 0.04
 C26-C24 \\sim C26A-C24A
 with sigma of 0.04
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 C27-C31 \\sim C27A-C31A
 with sigma of 0.04
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
 C29-C31 \\sim C29A-C31A
 with sigma of 0.04
 C30-C24 \\sim C30A-C24A
 with sigma of 0.04
 N12-C104 \\sim N12A-C1A
 with sigma of 0.02
 N12-C108 \\sim N12A-C1B
 with sigma of 0.02
 N12-C103 \\sim N12A-C1C
 with sigma of 0.02
 C104-C105 \\sim C1A-C1D
 with sigma of 0.02
 C105-C106 \\sim C1D-C1G
 with sigma of 0.02
 C106-C107 \\sim C1G-C1E
 with sigma of 0.02
 C107-C108 \\sim C1E-C1B
 with sigma of 0.02
 N11-C91 \\sim N11A-C91A
 with sigma of 0.02
 N11-C95 \\sim N11A-C95A
 with sigma of 0.02
 N11-C96 \\sim N11A-C96A
 with sigma of 0.02
 C91-C92 \\sim C91A-C92A
 with sigma of 0.02
 C92-C93 \\sim C92A-C93A
 with sigma of 0.02
 C93-C94 \\sim C93A-C94A
 with sigma of 0.02
 C94-C95 \\sim C94A-C95A
 with sigma of 0.02
 C97-C98 \\sim C97A-C98A
 with sigma of 0.02
 C97-C102 \\sim C97A-C109
 with sigma of 0.02
 C97-C96 \\sim C97A-C96A
 with sigma of 0.02
 C98-C99 \\sim C98A-C99A
 with sigma of 0.02
 C99-C100 \\sim C99A-C1F
 with sigma of 0.02
 C100-C101 \\sim C1F-C1H
 with sigma of 0.02
 C100-C103 \\sim C1F-C1C
 with sigma of 0.02
 C101-C102 \\sim C1H-C109
 with sigma of 0.02
 N12-C105 \\sim N12A-C1D
 with sigma of 0.04
 N12-C107 \\sim N12A-C1E
 with sigma of 0.04
 N12-C100 \\sim N12A-C1F
 with sigma of 0.04
 C104-C106 \\sim C1A-C1G
 with sigma of 0.04
 C104-C108 \\sim C1A-C1B
 with sigma of 0.04
 C104-C103 \\sim C1A-C1C
 with sigma of 0.04
 C105-C107 \\sim C1D-C1E
 with sigma of 0.04
 C106-C108 \\sim C1G-C1B
 with sigma of 0.04
 C108-C103 \\sim C1B-C1C
 with sigma of 0.04
 N11-C92 \\sim N11A-C92A
 with sigma of 0.04
 N11-C94 \\sim N11A-C94A
 with sigma of 0.04
 N11-C97 \\sim N11A-C97A
 with sigma of 0.04
 C91-C93 \\sim C91A-C93A
 with sigma of 0.04
 C91-C95 \\sim C91A-C95A
 with sigma of 0.04
 C91-C96 \\sim C91A-C96A
 with sigma of 0.04
 C92-C94 \\sim C92A-C94A
 with sigma of 0.04
 C93-C95 \\sim C93A-C95A
 with sigma of 0.04
 C95-C96 \\sim C95A-C96A
 with sigma of 0.04
 C97-C99 \\sim C97A-C99A
 with sigma of 0.04
 C97-C101 \\sim C97A-C1H
 with sigma of 0.04
 C98-C100 \\sim C98A-C1F
 with sigma of 0.04
 C98-C102 \\sim C98A-C109
 with sigma of 0.04
 C98-C96 \\sim C98A-C96A
 with sigma of 0.04
 C99-C101 \\sim C99A-C1H
 with sigma of 0.04
 C99-C103 \\sim C99A-C1C
 with sigma of 0.04
 C100-C102 \\sim C1F-C109
 with sigma of 0.04
 C101-C103 \\sim C1H-C1C
 with sigma of 0.04
 C102-C96 \\sim C109-C96A
 with sigma of 0.04
3. Restrained planarity
 O221, N221, C221, C222, C223
 with sigma of 0.001
 O231, N231, C231, C232, C233
 with sigma of 0.001
 O201, N201, C201, C202, C203
 with sigma of 0.001
 O211, N211, C211, C212, C213
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(I11A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(I11B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(I20B) \\sim Ueq, Uanis(I20A) \\sim Ueq, Uanis(I21B) \\sim Ueq,
Uanis(I21A) \\sim Ueq, Uanis(Bi4B) \\sim Ueq, Uanis(Bi4A) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(I12A) = Uanis(I12B)
Uanis(O231) = Uanis(N231) = Uanis(C231) = Uanis(C232) = Uanis(C233) =
Uanis(C1K) = Uanis(C111) = Uanis(O1) = Uanis(N14) = Uanis(C1L)
Uanis(I5A) = Uanis(I5B)
Uanis(I10A) = Uanis(I10B)
Uanis(I11A) = Uanis(I11B)
Uanis(I6B) = Uanis(I6A)
Uanis(I19A) = Uanis(I19B)
Uanis(C1I) = Uanis(O221) = Uanis(C221) = Uanis(N221) = Uanis(C222) =
Uanis(C223) = Uanis(N13) = Uanis(C110) = Uanis(C1J) = Uanis(O2)
Uanis(I16A) = Uanis(I16B)
Uanis(I24B) = Uanis(I24A)
Uanis(I23A) = Uanis(I23B)
Uanis(I22A) = Uanis(I22B)
Uanis(I18A) = Uanis(I18B)
Uanis(Bi4A) = Uanis(Bi4B)
Uanis(I21A) = Uanis(I21B)
Uanis(I17B) = Uanis(I17A)
Uanis(I20B) = Uanis(I20A)
Uanis(I15A) = Uanis(I15B)
Uanis(Bi3A) = Uanis(Bi3B)
Uanis(C54) = Uanis(C53) = Uanis(C52) = Uanis(C51) = Uanis(C50) = Uanis(N6)
Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48) = Uanis(C43) = Uanis(C44)
Uanis(C49) = Uanis(C42)
Uanis(N5) = Uanis(C41) = Uanis(C40) = Uanis(C39) = Uanis(C38) = Uanis(C37)
Uanis(C73) = Uanis(C74) = Uanis(C75) = Uanis(C76) = Uanis(C77) = Uanis(N9)
Uanis(C78) = Uanis(C85)
Uanis(C80) = Uanis(C81) = Uanis(C82) = Uanis(C83) = Uanis(C84) = Uanis(C79)
Uanis(N10) = Uanis(C90) = Uanis(C89) = Uanis(C88) = Uanis(C87) = Uanis(C86)
Uanis(N8) = Uanis(C72) = Uanis(C71) = Uanis(C70) = Uanis(C69) = Uanis(C68)
Uanis(C67) = Uanis(C60)
Uanis(C61) = Uanis(C66) = Uanis(C65) = Uanis(C64) = Uanis(C63) = Uanis(C62)
Uanis(N7) = Uanis(C55) = Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C59)
Uanis(N2) = Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(C15) = Uanis(C14)
Uanis(C13) = Uanis(C6)
Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C7) = Uanis(C8) = Uanis(C9)
Uanis(N1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C1)
Uanis(N4) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) =
Uanis(N4A) = Uanis(C32A) = Uanis(C36A) = Uanis(C33A) = Uanis(C35A) = Uanis(C34A)
Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30) =
Uanis(C25A) = Uanis(C26A) = Uanis(C30A) = Uanis(C27A) = Uanis(C29A) =
Uanis(C28A)
Uanis(N3) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23) =
Uanis(N3A) = Uanis(C19A) = Uanis(C23A) = Uanis(C20A) = Uanis(C22A) = Uanis(C21A)
Uanis(C24A) = Uanis(C24) = Uanis(C31A) = Uanis(C31)
Uanis(N11) = Uanis(C91) = Uanis(C92) = Uanis(C93) = Uanis(C94) = Uanis(C95) =
Uanis(N11A) = Uanis(C91A) = Uanis(C95A) = Uanis(C92A) = Uanis(C94A) =
Uanis(C93A)
Uanis(C97) = Uanis(C98) = Uanis(C99) = Uanis(C100) = Uanis(C101) = Uanis(C102)
= Uanis(C109) = Uanis(C1F) = Uanis(C99A) = Uanis(C1H) = Uanis(C98A) =
Uanis(C97A)
Uanis(N12) = Uanis(C104) = Uanis(C105) = Uanis(C106) = Uanis(C107) =
Uanis(C108) = Uanis(C103) = Uanis(N12A) = Uanis(C1A) = Uanis(C1B) = Uanis(C1C)
= Uanis(C1D) = Uanis(C1E) = Uanis(C1G)
Uanis(C100) = Uanis(C1F) = Uanis(C97A) = Uanis(C97)
Uanis(C96A) = Uanis(C96) = Uanis(C1C) = Uanis(C103)
Uanis(C212) = Uanis(N211) = Uanis(C211) = Uanis(O211) = Uanis(C213)
Uanis(C203) = Uanis(N201) = Uanis(C201) = Uanis(O201) = Uanis(C202)
5. Others
 Sof(I11B)=Sof(I12B)=Sof(I10A)=1-FVAR(1)
 Sof(I10B)=Sof(I12A)=Sof(I11A)=FVAR(1)
 Sof(I6B)=Sof(I5A)=1-FVAR(2)
 Sof(I5B)=Sof(I6A)=FVAR(2)
 Sof(Bi3B)=Sof(I15B)=Sof(I16A)=Sof(I18A)=Sof(I17A)=1-FVAR(3)
 Sof(I16B)=Sof(I17B)=Sof(I18B)=Sof(I15A)=Sof(Bi3A)=FVAR(3)
 Sof(I20B)=Sof(I24B)=Sof(I19A)=Sof(I23A)=Sof(I22A)=Sof(Bi4A)=Sof(I21A)=1-FVAR(4)
 Sof(Bi4B)=Sof(I19B)=Sof(I21B)=Sof(I22B)=Sof(I23B)=Sof(I24A)=Sof(I20A)=FVAR(4)
 Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(N3A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=
 Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(C25A)=Sof(C26A)=Sof(H26A)=
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(N4A)=Sof(C36A)=
 Sof(H36A)=Sof(C35A)=Sof(H35A)=Sof(C34A)=Sof(H34A)=Sof(C33A)=Sof(H33A)=
 Sof(C32A)=Sof(H32A)=1-FVAR(5)
 Sof(N3)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=
 Sof(H22)=Sof(C23)=Sof(H23)=Sof(N4)=Sof(C36)=Sof(H36)=Sof(C35)=Sof(H35)=
 Sof(C34)=Sof(H34)=Sof(C33)=Sof(H33)=Sof(C32)=Sof(H32)=Sof(C29)=Sof(H29)=
 Sof(C30)=Sof(H30)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C31)=Sof(H31A)=Sof(H31B)=FVAR(5)
 Sof(O2)=Sof(C110)=Sof(H110)=Sof(N13)=Sof(C1I)=Sof(H1IA)=Sof(H1IB)=Sof(H1IC)=
 Sof(C1J)=Sof(H1JA)=Sof(H1JB)=Sof(H1JC)=1-FVAR(6)
 Sof(O221)=Sof(N221)=Sof(C221)=Sof(H221)=Sof(C222)=Sof(H22B)=Sof(H22C)=
 Sof(H22D)=Sof(C223)=Sof(H22E)=Sof(H22F)=Sof(H22G)=FVAR(6)
 Sof(C111)=Sof(H111)=Sof(O1)=Sof(N14)=Sof(C1K)=Sof(H1KA)=Sof(H1KB)=Sof(H1KC)=
 Sof(C1L)=Sof(H1LA)=Sof(H1LB)=Sof(H1LC)=1-FVAR(7)
 Sof(O231)=Sof(N231)=Sof(C231)=Sof(H231)=Sof(C232)=Sof(H23B)=Sof(H23C)=
 Sof(H23D)=Sof(C233)=Sof(H23E)=Sof(H23F)=Sof(H23G)=FVAR(7)
 Fixed Sof: N12(0.5) C104(0.5) H104(0.5) C105(0.5) H105(0.5) C106(0.5)
 H106(0.5) C107(0.5) H107(0.5) C108(0.5) H108(0.5) C92(0.5) H92(0.5) C91(0.5)
 H91(0.5) N11(0.5) C95(0.5) H95(0.5) C94(0.5) H94(0.5) C93(0.5) H93(0.5)
 C102(0.5) H102(0.5) C97(0.5) C98(0.5) H98(0.5) C99(0.5) H99(0.5) C100(0.5)
 C101(0.5) H101(0.5) C96(0.5) H96A(0.5) H96B(0.5) C103(0.5) H10A(0.5) H10B(0.5)
 C109(0.5) H109(0.5) C97A(0.5) C98A(0.5) H98A(0.5) C99A(0.5) H99A(0.5) C1F(0.5)
 C1H(0.5) H1H(0.5) N12A(0.5) C1A(0.5) H1A(0.5) C1D(0.5) H1D(0.5) C1G(0.5)
 H1G(0.5) C1E(0.5) H1E(0.5) C1B(0.5) H1B(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5)
 C96A(0.5) H96C(0.5) H96D(0.5) C92A(0.5) H92A(0.5) C91A(0.5) H91A(0.5)
 N11A(0.5) C95A(0.5) H95A(0.5) C94A(0.5) H94A(0.5) C93A(0.5) H93A(0.5)
6.a Riding coordinates:
 C222(H22B,H22C,H22D), C223(H22E,H22F,H22G), C232(H23B,H23C,H23D), C233(H23E,
 H23F,H23G), C1I(H1IA,H1IB,H1IC), C1J(H1JA,H1JB,H1JC), C1K(H1KA,H1KB,H1KC),
 C1L(H1LA,H1LB,H1LC)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C24(H24A,H24B), C31(H31A,H31B), C42(H42A,H42B),
 C49(H49A,H49B), C60(H60A,H60B), C67(H67A,H67B), C78(H78A,H78B), C85(H85A,H85B),
  C96(H96A,H96B), C103(H10A,H10B), C24A(H24C,H24D), C31A(H31C,H31D), C1C(H1CA,
 H1CB), C96A(H96C,H96D)
6.c Me refined with riding coordinates:
 C202(H20B,H20C,H20D), C203(H20E,H20F,H20G), C212(H21B,H21C,H21D), C213(H21E,
 H21F,H21G)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C36(H36),
  C35(H35), C34(H34), C33(H33), C32(H32), C37(H37), C38(H38), C39(H39),
 C40(H40), C41(H41), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55),
  C56(H56), C57(H57), C58(H58), C59(H59), C68(H68), C69(H69), C70(H70),
 C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C86(H86),
  C87(H87), C88(H88), C89(H89), C90(H90), C104(H104), C105(H105), C106(H106),
 C107(H107), C108(H108), C8(H8), C9(H9), C11(H11), C12(H12), C29(H29), C30(H30),
  C26(H26), C27(H27), C44(H44), C45(H45), C47(H47), C48(H48), C62(H62),
 C63(H63), C65(H65), C66(H66), C80(H80), C81(H81), C83(H83), C84(H84), C92(H92),
  C91(H91), C95(H95), C94(H94), C93(H93), C102(H102), C98(H98), C99(H99),
 C101(H101), C201(H201), C211(H211), C221(H221), C231(H231), C19A(H19A),
 C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C29A(H29A), C30A(H30A),
 C26A(H26A), C27A(H27A), C36A(H36A), C35A(H35A), C34A(H34A), C33A(H33A),
 C32A(H32A), C109(H109), C98A(H98A), C99A(H99A), C1H(H1H), C1A(H1A), C1D(H1D),
 C1G(H1G), C1E(H1E), C1B(H1B), C92A(H92A), C91A(H91A), C95A(H95A), C94A(H94A),
 C93A(H93A), C110(H110), C111(H111)
6.e Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N2(C14,C15,C16,C17,C18), N3(C19,C20,C21,C22,C23), N4(C36,
 C35,C34,C33,C32), N5(C37,C38,C39,C40,C41), N6(C50,C51,C52,C53,C54), N7(C55,C56,
 C57,C58,C59), N8(C68,C69,C70,C71,C72), N9(C73,C74,C75,C76,C77), N10(C86,C87,
 C88,C89,C90), N12(C104,C105,C106,C107,C108), C7(C8,C9,C10,C11,C12), C29(C30,
 C25,C26,C27,C28), C43(C44,C45,C46,C47,C48), C61(C62,C63,C64,C65,C66), C79(C80,
 C81,C82,C83,C84), C92(C91,N11,C95,C94,C93), C102(C97,C98,C99,C100,C101),
 N3A(C19A,C20A,C21A,C22A,C23A), C29A(C30A,C25A,C26A,C27A,C28A), N4A(C36A,C35A,
 C34A,C33A,C32A), C109(C97A,C98A,C99A,C1F,C1H), N12A(C1A,C1D,C1G,C1E,C1B),
 C92A(C91A,N11A,C95A,C94A,C93A)
;
_shelx_res_checksum              51552
_olex2_submission_special_instructions 'No special instructions were received'