Cerium-Oxo clusters for photocatalytic aerobic oxygenation of sulfides to sulfoxides
Lv, Xinjie; Zhao, Xiao-li; Zhao, Qixin; Zheng, Qi; Xuan, Weimin; Dalton Transactions  (2022) –; doi:10.1039/D2DT00856D

data_7710343
_publ_section_title
;
 Cerium-Oxo clusters for photocatalytic aerobic oxygenation of sulfides to
 sulfoxides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00856D
_journal_year                    2022
_chemical_formula_moiety
'C170 H110 Ce24 N4 O96 S30, 9[C5H5N], 13[C2H3N], 28[H2O]'
_chemical_formula_sum            'C241 H250 Ce24 N26 O124 S30'
_chemical_formula_weight         9819.33
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-22 deposited with the CCDC.	2022-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   40.8409(18)
_cell_length_b                   40.8409(18)
_cell_length_c                   51.871(4)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      23.20
_cell_measurement_theta_min      2.18
_cell_volume                     74928(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       HKL3000
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Shanghai Synchrotron Radiation Facility, beam line station 
BL17B, Bruker/ARINAX MD2 equipped with a MarCCD-300 detector
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67011
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            285392
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        23.244
_diffrn_reflns_theta_max         23.244
_diffrn_reflns_theta_min         0.940
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    2.988
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.4998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1391 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.6710.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       block
_exptl_crystal_F_000             42678
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.442
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2024
_refine_ls_number_reflns         28337
_refine_ls_number_restraints     6297
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0920
_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^)+(0.1440P)^2^+3335.3320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2542
_refine_ls_wR_factor_ref         0.2705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21266
_reflns_number_total             28337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00856d2.cif
_cod_data_source_block           r-3
_cod_original_cell_volume        74928(8)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7710343
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.697
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{S12A, C8C}
{C8A, S12C}
{S13A, C23C}
{C23A, S13C}
{S15A, C68C}
{C68A, S15C}
3. Restrained distances
 C3A-C3B
 1.3 with sigma of 0.02
 S9B-C61B = S9B-C64B = S14B-C29B = S14B-C26B = S7B-C59B = S7B-C56B = S15A-C66A
 = S12A-C6A = C3B-C4B = C3B-C2B = S3B-C39B = S3B-C36B = S13A-C21A = S8B-C34B =
 S8B-C31B = C53B-C54B = C53B-C52B = S5B-C49B = S5B-C46B
 1.73 with sigma of 0.02
 S11A-C4A = S11A-C1A = S3A-C39A = S3A-C36A = S12A-C9A = S12A-C6A = S4A-C44A =
 S4A-C41A = S5A-C49A = S5A-C46A = S13A-C21A = S2A-C16A = S2A-C19A = S14B-C26B =
 S14B-C29B = S8A-C34A = S8A-C31A = S7A-C59A = S7A-C56A = S6A-C51A = S6A-C54A =
 S9A-C64A = S9A-C61A = S10A-C74A = S10A-C71A = S15A-C66A = S1A-C14A = S1A-C11A
 1.73 with sigma of 0.02
 C52B-C51B = C46B-C47B = C47B-C48B = C48B-C49B = C41B-C42B = C36B-C37B = C37B-
 C38B = C38B-C39B = C7A-C6A = C7A-C8A = C1B-C2B = C11B-C12B = C67A-C68A = C66A-
 C67A = C63B-C64B = C62B-C63B = C61B-C62B = C72B-C71B = C27B-C28B = C28B-C29B =
 C26B-C27B = C58B-C59B = C56B-C57B = C57B-C58B = C33B-C34B = C32B-C33B = C31B-
 C32B = C21A-C22A = C16B-C17B
 1.43 with sigma of 0.02
 S15C-C69A = S13C-C24A
 1.6 with sigma of 0.02
 C71A-C72A = C72A-C73A = C73A-C74A = C66A-C67A = C13A-C14A = C12A-C13A = C12A-
 C11A = C61A-C62A = C62A-C63A = C63A-C64A = C18A-C19A = C17A-C18A = C17A-C16A =
 C8A-C9A = C7A-C8A = C7A-C6A = C38A-C39A = C37A-C38A = C36A-C37A = C3A-C4A =
 C2A-C3A = C1A-C2A = C58A-C59A = C57A-C58A = C56A-C57A = C28B-C29B = C27B-C28B =
  C26B-C27B = C33A-C34A = C32A-C33A = C31A-C32A = C53A-C54A = C52A-C53A = C51A-
 C52A = C48A-C49A = C47A-C48A = C46A-C47A = C43A-C44A = C42A-C43A = C42A-C41A
 1.43 with sigma of 0.02
 S12C-C9A = C9A-C8C
 1.63 with sigma of 0.02
 C74A-C75A = C74B-C75B = C64B-C65B = C64A-C65A = C29B-C30B = C59A-C60A = C59B-
 C60B = C35B-C34B = C35A-C34A = C54B-C55B = C54A-C55A = C49A-C50A = C49B-C50B =
 C44B-C45B = C44A-C45A = C39A-C40A = C39B-C40B = C19B-C20B = C19A-C20A = C9A-
 C10A = C14A-C15A = C14B-C15B = C69A-C70A = C24A-C25A = C4A-C5A = C4B-C5B
 1.5 with sigma of 0.02
 S6A-C54A = S6A-C51A
 1.7 with sigma of 0.02
 C54A-C55A = C54B-C55B
 1.5 with sigma of 0.02
 C51A-C52A = C52B-C51B = C52A-C53A = C53A-C54A
 1.42 with sigma of 0.02
 C53B-C54B = C53B-C52B = C52B-C51B
 1.43 with sigma of 0.02
 S6B-C54B = S6B-C51B
 1.72 with sigma of 0.02
 C52A-S6A
 2.5 with sigma of 0.02
 C53A-S6A
 2.6 with sigma of 0.02
 S11A-C1A
 1.6 with sigma of 0.02
 S3A-C38A
 2.7 with sigma of 0.02
 C40A-C39A
 1.5 with sigma of 0.02
 C37A-C39A
 2.4 with sigma of 0.02
 S3A-C39A = S3A-C36A
 1.7 with sigma of 0.02
 C39A-C38A = C37A-C38A = C36A-C37A = S3A-C36A
 1.4 with sigma of 0.02
 S1B-C14B = S1B-C11B
 1.7 with sigma of 0.02
 S3B-C39B = S3B-C36B
 1.7 with sigma of 0.02
 C38B-C39B = C37B-C38B = C36B-C37B
 1.4 with sigma of 0.02
 S11B-C4B = S11B-C1B
 1.7 with sigma of 0.02
 C39B-C40B
 1.51 with sigma of 0.02
 C38B-S3B
 2.7 with sigma of 0.02
 S3B-C37B
 2.7 with sigma of 0.02
 S1B-C13B
 2.57 with sigma of 0.02
 C2A-C4A
 2.3 with sigma of 0.02
 C3A-C4A
 1.5 with sigma of 0.02
 C1A-C2A
 1.5 with sigma of 0.02
 C13A-C14A = C11B-C12B = C12A-C11A = C12A-C13A
 1.51 with sigma of 0.02
 C4B-C5B = C4A-C5A
 1.5 with sigma of 0.02
 C1B-C2B = C3B-C2B = C3B-C4B
 1.43 with sigma of 0.02
 S1B-C12B
 2.57 with sigma of 0.02
 S1A-C14A = S1A-C11A
 1.7 with sigma of 0.02
 C17A-C18A = C16B-C17B = C17A-C16A = C18A-C19A
 1.42 with sigma of 0.02
 C13A-C14A = C12A-C13A = C12A-C11A = C11B-C12B
 1.4 with sigma of 0.02
 S2A-C19A = S2A-C16A
 1.7 with sigma of 0.02
 C19A-C20A = C19B-C20B
 1.51 with sigma of 0.02
 O41-C15B = O40-C15B = O40-C15A = O41-C15A
 1.25 with sigma of 0.02
 C15A-C13A
 2.4 with sigma of 0.02
 C15A-S1A
 2.7 with sigma of 0.02
 C14B-C15B = C14A-C15A
 1.51 with sigma of 0.02
 C43B-S4B
 2.58 with sigma of 0.02
 C43B-C41B
 2.56 with sigma of 0.02
 S4B-C44B = S4B-C41B
 1.7 with sigma of 0.02
 C44B-C43B = C42B-C43B
 1.43 with sigma of 0.02
 O40-C15A = O41-C15A = O31-C40A = O32-C40A = O33-C20A = O34-C20A = O8-C70A =
 O2-C75A = O1-C75A = O7-C70A = O4-C65A = O3-C65A = O12-C30B = O13-C30B = O18-
 C60A = O17-C60A = O15-C35A = O16-C35A = O21-C55A = O22-C55A
 1.26 with sigma of 0.02
 O18-C60A = O17-C60A = O40-C15A = O41-C15A = O28-C45A = O27-C45A
 1.26 with sigma of 0.02
 O41-C15A
 1.26 with sigma of 0.02
 O40-C15A = O41-C15A
 1.23 with sigma of 0.02
 O44-C5B = O43-C5B = O44-C5A = O43-C5A
 1.25 with sigma of 0.02
 S1A-C13A
 2.6 with sigma of 0.02
 C12A-S1A
 2.6 with sigma of 0.02
 C11A-C13A
 2.9 with sigma of 0.02
 O33-C20B = O34-C20B
 1.25 with sigma of 0.02
 C49B-C50B = C49A-C50A
 1.51 with sigma of 0.02
 C48B-C49B = C47B-C48B = C46B-C47B = C47A-C48A = C48A-C49A = C46A-C47A
 1.4 with sigma of 0.02
 S5B-C46B = S5A-C46A = S5B-C49B = S5A-C49A
 1.7 with sigma of 0.02
 O20-C50B = O20-C50A = O19-C50B = O19-C50A
 1.25 with sigma of 0.02
 S8B-C33B
 2.6 with sigma of 0.02
 C32A-C34A
 2.26 with sigma of 0.02
 O32-C40B = O31-C40B = O27-C45B = O28-C45B = O8-C70A = O7-C70A = O4-C65B = O3-
 C65B = O1-C75B = O2-C75B = O15-C35B = O16-C35B = O12-C30B = O13-C30B = O22-
 C55B = O21-C55B
 1.26 with sigma of 0.02
 O17-C60B = O18-C60B
 1.28 with sigma of 0.02
 C71A-C73A
 2.43 with sigma of 0.02
 S9A-C62A
 2.56 with sigma of 0.02
 S10A-C72A
 2.56 with sigma of 0.02
 C65A-S9A
 2.7 with sigma of 0.02
 C65A-C63A
 2.6 with sigma of 0.02
 S7A_$1-C61A
 2.4 with sigma of 0.02
 C14A-C15A
 1.5 with sigma of 0.02
 C74B-C73B = C72B-C73B = C72B-C71B
 1.43 with sigma of 0.02
 C73B-S10B
 2.68 with sigma of 0.02
 S10B-C74B = S10B-C71B
 1.7 with sigma of 0.02
 S2B-C19B = S2B-C16B
 1.7 with sigma of 0.02
 C18B-C19B = C18B-C17B = C16B-C17B
 1.43 with sigma of 0.02
 C14B-C13B = C12B-C13B = C11B-C12B
 1.43 with sigma of 0.02
 S10B-C72B
 2.6 with sigma of 0.02
 C29A-C30A
 1.5 with sigma of 0.02
 O12-C30A
 1.26 with sigma of 0.02
 C28A-C29A = C27A-C28A = C26A-C27A
 1.43 with sigma of 0.02
 C30A-O13
 1.26 with sigma of 0.02
 S14A-C29A = S14A-C26A
 1.7 with sigma of 0.02
 C26B-C29B
 2.5 with sigma of 0.02
 C26B-C28B
 2.4 with sigma of 0.02
 C26A-C28A
 2.4 with sigma of 0.02
 S4A-C42A
 2.61 with sigma of 0.02
 C51B-C53B \\sim C53B-S6B
 with sigma of 0.02
 S6B-C55B \\sim C55B-C53B
 with sigma of 0.02
 C53A-S6A \\sim S6A-C52A
 with sigma of 0.02
 C53A-C55A \\sim C55A-S6A
 with sigma of 0.02
 S11B-C5B \\sim C5B-C3B
 with sigma of 0.02
 S11A-C5A \\sim C5A-C3A
 with sigma of 0.02
 C38A-S3A \\sim S3A-C37A
 with sigma of 0.02
 C39A-C37A \\sim C38A-C36A
 with sigma of 0.02
 C39B-C37B \\sim C38B-C36B
 with sigma of 0.02
 S2B-C18B \\sim C18B-C16B
 with sigma of 0.02
 S2B-C20B \\sim C20B-C18B
 with sigma of 0.02
 C12A-S1A \\sim S1A-C13A
 with sigma of 0.02
 C12A-C14A \\sim C13A-C11A
 with sigma of 0.02
 C18A-S2A \\sim S2A-C17A
 with sigma of 0.02
4. Restrained planarity
 C54B, S6B, C51B, C53B, C52B, C55B
 with sigma of 0.1
 C3B, C2B, C1B, S11B, C4B
 with sigma of 0.01
 S6A, O22, C55A, C54A, C53A, C52A, C51A, O21
 with sigma of 0.1
 C5B, C4B, S11B, C3B, C2B, C1B
 with sigma of 0.1
 C13B, C14B, S1B, C11B, C12B, C15B
 with sigma of 0.1
 C3A, C4A, S11A, C1A, C2A
 with sigma of 0.01
 C5A, S11A, C4A, C3A, C2A, C1A
 with sigma of 0.1
 C39B, S3B, C36B, C37B, C38B, C40B
 with sigma of 0.1
 C39A, C37A, C36A, S3A, C40A, C38A
 with sigma of 0.1
 C19B, C18B, C17B, S2B, C16B, C20B
 with sigma of 0.1
 O27, O28, C44B, C45B, C43B, S4B, C41B, C42B
 with sigma of 0.1
 C15A, C14A, C13A, C12A, C11A, S1A
 with sigma of 0.1
 C20A, C19A, C18A, C17A, C16A, S2A
 with sigma of 0.1
 C50B, C49B, C48B, C47B, C46B, S5B
 with sigma of 0.1
 C48A, C47A, C46A, S5A, C49A, C50A
 with sigma of 0.1
 O17, C59B, C57B, C56B, S7B, C58B, C60B, O18
 with sigma of 0.1
 O1, O2, C75A, C74A, C72A, C71A, S10A, C73A
 with sigma of 0.1
 C64A, C62A, C61A, S9A, C63A, O3, C65A, O4
 with sigma of 0.1
 C71B, C73B, C72B, S10B, C74B, O1, O2, C75B
 with sigma of 0.1
 C30B, C29B, S14B, C26B, C28B, C27B
 with sigma of 0.1
 O1, C75A, C74A, C72A, C71A, C73A, O2, S10A
 with sigma of 0.1
 O27, O28, C45A, C44A, C41A, C42A, S4A, C43A
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C54A \\sim C53A \\sim C52A \\sim C51A \\sim S6A: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002 within 2A
C75A \\sim C74A \\sim C72A \\sim C71A: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Uanis(C33B) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C32B) \\sim Ueq,
Uanis(C32A) \\sim Ueq, Uanis(C31B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C35B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C30B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C58B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C58A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C18B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C50A) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(S15A) = Uanis(C68C)
Uanis(S12C) = Uanis(C8A)
Uanis(S15C) = Uanis(C68A)
Uanis(S12A) = Uanis(C8C)
Uanis(S15A) = Uanis(S15C)
Uanis(S13A) = Uanis(C23C)
Uanis(S13C) = Uanis(C23A)
Uanis(C23A) = Uanis(C23C)
Uanis(S13A) = Uanis(S13C)
Uanis(C8A) = Uanis(C8C)
Uanis(C52B) = Uanis(C51A)
Uanis(S10B) = Uanis(S10A)
Uanis(C71B) = Uanis(C71A) = Uanis(C74B) = Uanis(C74A)
Uanis(S2A) = Uanis(S2B)
Uanis(S11B) = Uanis(C4B) = Uanis(C3B) = Uanis(C2B) = Uanis(C1B)
Uanis(S11B) = Uanis(S11A)
Uanis(S3A) = Uanis(C36A) = Uanis(C39A) = Uanis(C38A) = Uanis(C37A)
Uanis(S3A) = Uanis(S3B)
Uanis(C1B) = Uanis(C1A)
Uanis(C2B) = Uanis(C2A)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C5A)=Sof(C3A)=Sof(H3A)=Sof(C2A)=Sof(H2A)=Sof(C1A)=Sof(H1A)=Sof(S11A)=
 Sof(C4A)=1-FVAR(1)
 Sof(C3B)=Sof(H3B)=Sof(C2B)=Sof(H2B)=Sof(C1B)=Sof(H1B)=Sof(S11B)=Sof(C4B)=
 Sof(C5B)=FVAR(1)
 Sof(S1A)=Sof(C15A)=Sof(C14A)=Sof(C13A)=Sof(H13A)=Sof(C11A)=Sof(H11A)=
 Sof(C12A)=Sof(H12A)=1-FVAR(2)
 Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(C15B)=Sof(S1B)=Sof(C11B)=Sof(H11B)=
 Sof(C12B)=Sof(H12B)=FVAR(2)
 Sof(S6A)=Sof(C55A)=Sof(C54A)=Sof(C53A)=Sof(H53A)=Sof(C52A)=Sof(H52A)=
 Sof(C51A)=Sof(H51A)=1-FVAR(3)
 Sof(C55B)=Sof(C54B)=Sof(S6B)=Sof(C51B)=Sof(H51B)=Sof(C52B)=Sof(H52B)=
 Sof(C53B)=Sof(H53B)=FVAR(3)
 Sof(C40A)=Sof(C39A)=Sof(C37A)=Sof(H37A)=Sof(C36A)=Sof(H36A)=Sof(S3A)=
 Sof(C38A)=Sof(H38A)=1-FVAR(4)
 Sof(C40B)=Sof(C39B)=Sof(S3B)=Sof(C36B)=Sof(H36B)=Sof(C37B)=Sof(H37B)=
 Sof(C38B)=Sof(H38B)=FVAR(4)
 Sof(S2A)=Sof(H6AA)=Sof(H7AA)=Sof(C20A)=Sof(C19A)=Sof(C18A)=Sof(H18A)=
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C8C)=Sof(H8C)=Sof(S12C)=1-FVAR(5)
 Sof(H6A)=Sof(H7A)=Sof(C20B)=Sof(C19B)=Sof(C18B)=Sof(H18B)=Sof(C17B)=Sof(H17B)=
 Sof(C16B)=Sof(H16B)=Sof(S2B)=Sof(S12A)=Sof(C8A)=Sof(H8A)=FVAR(5)
 Sof(S5A)=Sof(H22B)=Sof(H21B)=Sof(C50A)=Sof(C49A)=Sof(C48A)=Sof(H48A)=
 Sof(C47A)=Sof(H47A)=Sof(C46A)=Sof(H46A)=Sof(C23C)=Sof(H23C)=Sof(S13C)=1-FVAR(6)
 Sof(S13A)=Sof(C23A)=Sof(H23A)=Sof(H22A)=Sof(H21A)=Sof(C50B)=Sof(C49B)=
 Sof(S5B)=Sof(C46B)=Sof(H46B)=Sof(C47B)=Sof(H47B)=Sof(C48B)=Sof(H48B)=FVAR(6)
 Sof(H67B)=Sof(H66B)=Sof(C45A)=Sof(C44A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=
 Sof(H42A)=Sof(S4A)=Sof(C43A)=Sof(H43A)=Sof(C68C)=Sof(H68C)=Sof(S15C)=1-FVAR(7)
 Sof(S15A)=Sof(C68A)=Sof(H68A)=Sof(H67A)=Sof(H66A)=Sof(C44B)=Sof(C45B)=
 Sof(C43B)=Sof(H43B)=Sof(S4B)=Sof(C41B)=Sof(H41B)=Sof(C42B)=Sof(H42B)=FVAR(7)
 Sof(C75A)=Sof(C74A)=Sof(C72A)=Sof(H72A)=Sof(C71A)=Sof(H71A)=Sof(S10A)=
 Sof(C73A)=Sof(H73A)=1-FVAR(8)
 Sof(C71B)=Sof(H71B)=Sof(C73B)=Sof(H73B)=Sof(C72B)=Sof(H72B)=Sof(S10B)=
 Sof(C74B)=Sof(C75B)=FVAR(8)
 Sof(C65A)=Sof(C64A)=Sof(C62A)=Sof(H62A)=Sof(C61A)=Sof(H61A)=Sof(S9A)=
 Sof(C63A)=Sof(H63A)=1-FVAR(9)
 Sof(C65B)=Sof(C64B)=Sof(S9B)=Sof(C61B)=Sof(H61B)=Sof(C62B)=Sof(H62B)=
 Sof(C63B)=Sof(H63B)=FVAR(9)
 Sof(C34A)=Sof(C32A)=Sof(H32A)=Sof(C31A)=Sof(H31A)=Sof(C35A)=Sof(S8A)=
 Sof(C33A)=Sof(H33A)=1-FVAR(10)
 Sof(C35B)=Sof(C34B)=Sof(S8B)=Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=
 Sof(C33B)=Sof(H33B)=FVAR(10)
 Sof(C60A)=Sof(C59A)=Sof(C57A)=Sof(H57A)=Sof(C56A)=Sof(H56A)=Sof(S7A)=
 Sof(C58A)=Sof(H58A)=1-FVAR(11)
 Sof(C59B)=Sof(C57B)=Sof(H57B)=Sof(C56B)=Sof(H56B)=Sof(S7B)=Sof(C58B)=
 Sof(H58B)=Sof(C60B)=FVAR(11)
 Sof(C84A)=Sof(H84A)=Sof(C83A)=Sof(H83A)=Sof(C82A)=Sof(H82A)=Sof(C81A)=
 Sof(H81A)=Sof(N2A)=Sof(C85A)=Sof(H85A)=1-FVAR(12)
 Sof(C84B)=Sof(H84B)=Sof(C83B)=Sof(H83B)=Sof(C82B)=Sof(H82B)=Sof(C81B)=
 Sof(H81B)=Sof(N2B)=Sof(C85B)=Sof(H85B)=FVAR(12)
 Sof(C30A)=Sof(C29A)=Sof(C28A)=Sof(H28A)=Sof(C27A)=Sof(H27A)=Sof(C26A)=
 Sof(H26A)=Sof(S14A)=1-FVAR(13)
 Sof(S14B)=Sof(C30B)=Sof(C29B)=Sof(C28B)=Sof(H28B)=Sof(C27B)=Sof(H27B)=
 Sof(C26B)=Sof(H26B)=FVAR(13)
8.a Aromatic/amide H refined with riding coordinates:
 C84B(H84B), C83B(H83B), C82B(H82B), C81B(H81B), C85B(H85B), C80A(H80A),
 C79A(H79A), C78A(H78A), C77A(H77A), C76A(H76A), C3B(H3B), C2B(H2B), C1B(H1B),
 C3A(H3A), C2A(H2A), C1A(H1A), C6A(H6A), C6A(H6AA), C7A(H7A), C7A(H7AA),
 C13A(H13A), C11A(H11A), C12A(H12A), C68A(H68A), C67A(H67A), C67A(H67B),
 C66A(H66B), C66A(H66A), C62A(H62A), C61A(H61A), C72A(H72A), C71A(H71A),
 C18A(H18A), C16A(H16A), C53A(H53A), C52A(H52A), C51A(H51A), C57A(H57A),
 C56A(H56A), C28B(H28B), C27B(H27B), C26B(H26B), C23A(H23A), C22A(H22A),
 C22A(H22B), C21A(H21B), C21A(H21A), C41A(H41A), C42A(H42A), C48A(H48A),
 C47A(H47A), C46A(H46A), C32A(H32A), C31A(H31A), C37A(H37A), C36A(H36A),
 C17A(H17A), C13B(H13B), C11B(H11B), C12B(H12B), C51B(H51B), C52B(H52B),
 C53B(H53B), C38A(H38A), C36B(H36B), C37B(H37B), C38B(H38B), C18B(H18B),
 C17B(H17B), C16B(H16B), C46B(H46B), C47B(H47B), C48B(H48B), C43A(H43A),
 C43B(H43B), C41B(H41B), C42B(H42B), C8A(H8A), C63A(H63A), C33A(H33A),
 C58A(H58A), C73A(H73A), C71B(H71B), C73B(H73B), C72B(H72B), C61B(H61B),
 C62B(H62B), C63B(H63B), C31B(H31B), C32B(H32B), C33B(H33B), C57B(H57B),
 C56B(H56B), C58B(H58B), C84A(H84A), C83A(H83A), C82A(H82A), C81A(H81A),
 C85A(H85A), C28A(H28A), C27A(H27A), C26A(H26A), C8C(H8C), C23C(H23C),
 C68C(H68C)
8.b Fitted hexagon refined as free rotating group:
 C84B(C83B,C82B,C81B,N2B,C85B), C84A(C83A,C82A,C81A,N2A,C85A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 8437 electrons were 
found in a volume of 26443\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
81[C5H5N], 117[C2H3N], 252[H2O] per Unit Cell 
which account for 8496 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27916
_shelx_hkl_checksum              63529
_shelx_fab_checksum              63222
_olex2_submission_special_instructions 'No special instructions were received'