Forced topochemistry of a solid-state Diels–Alder reaction by encapsulation in epoxy glue
Lau, T. A.; Khorasani, S.; Fernandes, M. A.; CrystEngComm 25 (2023) 3988–3997; doi:10.1039/D3CE00388D

data_7246825
_publ_section_title
;
 Forced topochemistry of a solid-state Diels--Alder reaction by
 encapsulation in epoxy glue
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              3988
_journal_page_last               3997
_journal_paper_doi               10.1039/D3CE00388D
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
;        
0.364(C16 H14 N2 O4 S2), 0.364(C14 H9 Br), 0.636(C30 H23 Br N2 O4 S2)
;
_chemical_formula_sum            'C30 H23 Br N2 O4 S2'
_chemical_formula_weight         619.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-19 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                63.453(4)
_cell_angle_beta                 78.220(4)
_cell_angle_gamma                61.190(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5260(10)
_cell_length_b                   11.8060(11)
_cell_length_c                   12.2903(11)
_cell_measurement_reflns_used    7220
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      24.663
_cell_measurement_theta_min      2.264
_cell_volume                     1310.8(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      173.0
_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  0.0681
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            40827
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.852
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.769
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1053 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.8710.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       rod
_exptl_crystal_F_000             632
_exptl_crystal_recrystallization_method 'Thermal solid-state reaction at 20degC'
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         4609
_refine_ls_number_restraints     1122
_refine_ls_restrained_S_all      1.734
_refine_ls_R_factor_all          0.1635
_refine_ls_R_factor_gt           0.1331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4123
_refine_ls_wR_factor_ref         0.4426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3246
_reflns_number_total             4609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00388d2.cif
_cod_data_source_block           22talb35_90c_dc49b_fzgrt_103d4h_0f
_cod_depositor_comments
'Adding full bibliography for 7246822--7246827.cif.'
_cod_database_code               7246825
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.729
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1R-Br1R \\sim C8R-Br2R \\sim C1P-Br1P
 with sigma of 0.005
 C8R-Br2R \\sim C1R-Br1R
 with sigma of 0.003
 C17R-C16R \\sim C25P-C24P \\sim C25R-C24R
 with sigma of 0.005
3. Restrained planarity
 S1R, O1R, O2R, N1R, C15R, C16R, C17R, C18R
 with sigma of 0.05
 S1P, S2P, O3P, O4P, N2P, C23P, C24P, C25P, C26P
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
Br1R \\sim Br2R \\sim C1R \\sim C2R \\sim C3R \\sim C4R \\sim C5R \\sim C6R
\\sim C7R \\sim C8R \\sim C9R \\sim C10R \\sim C11R \\sim C12R \\sim C13R \\sim
C14R: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
S1R \\sim O1R \\sim O2R \\sim N1R \\sim C15R \\sim C16R \\sim C17R \\sim C18R
\\sim C19R \\sim C20R \\sim C21R \\sim C22R: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Br1P \\sim S1P \\sim S2P \\sim O1P \\sim O2P \\sim N1P \\sim C15P \\sim C16P
\\sim C17P \\sim C18P \\sim C19P \\sim C20P \\sim C21P \\sim C22P \\sim C1P
\\sim C2P \\sim C3P \\sim C4P \\sim C5P \\sim C6P \\sim C7P \\sim C8P \\sim C9P
\\sim C10P \\sim C11P \\sim C12P \\sim C13P \\sim C14P \\sim O3P \\sim O4P
\\sim N2P \\sim C23P \\sim C24P \\sim C25P \\sim C26P \\sim C27P \\sim C28P
\\sim C29P \\sim C30P: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(Br1P) \\sim Ueq, Uanis(S1P) \\sim Ueq, Uanis(S2P) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2P) = Uanis(O2R)
Uanis(O1P) = Uanis(O1R)
5. Rigid body (RIGU) restrains
 Br1R, Br2R, C1R, C2R, C3R, C4R, C5R, C6R, C7R, C8R, C9R, C10R, C11R, C12R,
 C13R, C14R
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S1R, O1R, O2R, N1R, C15R, C16R, C17R, C18R, C19R, C20R, C21R, C22R
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Br1P, S1P, S2P, O1P, O2P, N1P, C15P, C16P, C17P, C18P, C19P, C20P, C21P, C22P,
  C1P, C2P, C3P, C4P, C5P, C6P, C7P, C8P, C9P, C10P, C11P, C12P, C13P, C14P,
 O3P, O4P, N2P, C23P, C24P, C25P, C26P, C27P, C28P, C29P, C30P
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Same fragment restrains
{C19R, C20R, C21R, C22R} sigma for 1-2: 0.005, 1-3: 0.04
as in
{C27P, C28P, C29P, C30P}
{O1R, O2R, N1R, C15R, C16R, C17R, C18R} sigma for 1-2: 0.005, 1-3: 0.04
as in
{O3P, O4P, N2P, C23P, C24P, C25P, C26P}
{O1R, O2R, N1R, C15R, C16R, C17R, C18R, C19R, C20R, C21R, C22R} sigma for 1-2:
0.005, 1-3: 0.04
as in
{O1P, O2P, N1P, C15P, C16P, C17P, C18P, C19P, C20P, C21P, C22P}
7. Others
 1*[Sof(C1R)+Sof(C2R)+Sof(C3R)+Sof(H3R)+Sof(C4R)+Sof(H4R)+Sof(C5R)+Sof(H5R)+
 Sof(C6R)+Sof(H6R)+Sof(C7R)+Sof(C8R)+Sof(C9R)+Sof(C10R)+Sof(H10R)+Sof(C11R)+
 Sof(H11R)+Sof(C12R)+Sof(H12R)+Sof(C13R)+Sof(H13R)+Sof(C14R)]+1*[Sof(Br1P)+
 Sof(S1P)+Sof(S2P)+Sof(O1P)+Sof(O2P)+Sof(N1P)+Sof(C15P)+Sof(C16P)+Sof(C17P)+
 Sof(C18P)+Sof(C19P)+Sof(H19P)+Sof(C20P)+Sof(H20A)+Sof(H20B)+Sof(C21P)+
 Sof(H21A)+Sof(H21B)+Sof(C22P)+Sof(H22A)+Sof(H22B)+Sof(C1P)+Sof(C2P)+Sof(C3P)+
 Sof(H3P)+Sof(C4P)+Sof(H4P)+Sof(C5P)+Sof(H5P)+Sof(C6P)+Sof(H6P)+Sof(C7P)+
 Sof(C8P)+Sof(H8P)+Sof(C9P)+Sof(C10P)+Sof(H10P)+Sof(C11P)+Sof(H11P)+Sof(C12P)+
 Sof(H12P)+Sof(C13P)+Sof(H13P)+Sof(C14P)+Sof(O3P)+Sof(O4P)+Sof(N2P)+Sof(C23P)+
 Sof(C24P)+Sof(C25P)+Sof(C26P)+Sof(C27P)+Sof(H27P)+Sof(C28P)+Sof(H28C)+
 Sof(H28D)+Sof(C29P)+Sof(H29C)+Sof(H29D)+Sof(C30P)+Sof(H30C)+Sof(H30D)+Sof(O1R)+
 Sof(O2R)+Sof(N1R)+Sof(C15R)+Sof(C16R)+Sof(C17R)+Sof(C18R)+Sof(C19R)+Sof(H19R)+
 Sof(C20R)+Sof(H20C)+Sof(H20D)+Sof(C21R)+Sof(H21C)+Sof(H21D)+Sof(C22R)+
 Sof(H22C)+Sof(H22D)+Sof(S1R)]+1*[Sof(Br1Q)+Sof(C1Q)+Sof(S2Q)+Sof(S3Q)+Sof(O3Q)+
 Sof(O4Q)+Sof(O5Q)+Sof(O6Q)+Sof(N2Q)+Sof(N3Q)+Sof(C2Q)+Sof(C3Q)+Sof(H3Q)+
 Sof(C4Q)+Sof(H4Q)+Sof(C5Q)+Sof(H5Q)+Sof(C6Q)+Sof(H6Q)+Sof(C7Q)+Sof(C8Q)+
 Sof(H8Q)+Sof(C9Q)+Sof(C10Q)+Sof(H10Q)+Sof(C11Q)+Sof(H11Q)+Sof(C12Q)+Sof(H12Q)+
 Sof(C13Q)+Sof(H13Q)+Sof(C14Q)+Sof(C23Q)+Sof(C24Q)+Sof(C25Q)+Sof(C26Q)+
 Sof(C27Q)+Sof(H27Q)+Sof(C28Q)+Sof(H28A)+Sof(H28B)+Sof(C29Q)+Sof(H29A)+
 Sof(H29B)+Sof(C30Q)+Sof(H30A)+Sof(H30B)+Sof(C31Q)+Sof(C32Q)+Sof(C33Q)+
 Sof(C34Q)+Sof(C35Q)+Sof(H35Q)+Sof(C36Q)+Sof(H36A)+Sof(H36B)+Sof(C37Q)+
 Sof(H37A)+Sof(H37B)+Sof(C38Q)+Sof(H38A)+Sof(H38B)+Sof(S2R)+Sof(O3R)+Sof(O4R)+
 Sof(N2R)+Sof(C23R)+Sof(C24R)+Sof(C25R)+Sof(C26R)+Sof(C27R)+Sof(H27R)+Sof(C28R)+
 Sof(H28E)+Sof(H28F)+Sof(C29R)+Sof(H29E)+Sof(H29F)+Sof(C30R)+Sof(H30E)+
 Sof(H30F)]=1 with esd of 0.0001
 1*[Sof(Br1P)+Sof(S1P)+Sof(S2P)+Sof(O1P)+Sof(O2P)+Sof(N1P)+Sof(C15P)+Sof(C16P)+
 Sof(C17P)+Sof(C18P)+Sof(C19P)+Sof(H19P)+Sof(C20P)+Sof(H20A)+Sof(H20B)+
 Sof(C21P)+Sof(H21A)+Sof(H21B)+Sof(C22P)+Sof(H22A)+Sof(H22B)+Sof(C1P)+Sof(C2P)+
 Sof(C3P)+Sof(H3P)+Sof(C4P)+Sof(H4P)+Sof(C5P)+Sof(H5P)+Sof(C6P)+Sof(H6P)+
 Sof(C7P)+Sof(C8P)+Sof(H8P)+Sof(C9P)+Sof(C10P)+Sof(H10P)+Sof(C11P)+Sof(H11P)+
 Sof(C12P)+Sof(H12P)+Sof(C13P)+Sof(H13P)+Sof(C14P)+Sof(O3P)+Sof(O4P)+Sof(N2P)+
 Sof(C23P)+Sof(C24P)+Sof(C25P)+Sof(C26P)+Sof(C27P)+Sof(H27P)+Sof(C28P)+
 Sof(H28C)+Sof(H28D)+Sof(C29P)+Sof(H29C)+Sof(H29D)+Sof(C30P)+Sof(H30C)+
 Sof(H30D)+Sof(O1R)+Sof(O2R)+Sof(N1R)+Sof(C15R)+Sof(C16R)+Sof(C17R)+Sof(C18R)+
 Sof(C19R)+Sof(H19R)+Sof(C20R)+Sof(H20C)+Sof(H20D)+Sof(C21R)+Sof(H21C)+
 Sof(H21D)+Sof(C22R)+Sof(H22C)+Sof(H22D)+Sof(S1R)]+1*[Sof(Br1Q)+Sof(C1Q)+
 Sof(S2Q)+Sof(S3Q)+Sof(O3Q)+Sof(O4Q)+Sof(O5Q)+Sof(O6Q)+Sof(N2Q)+Sof(N3Q)+
 Sof(C2Q)+Sof(C3Q)+Sof(H3Q)+Sof(C4Q)+Sof(H4Q)+Sof(C5Q)+Sof(H5Q)+Sof(C6Q)+
 Sof(H6Q)+Sof(C7Q)+Sof(C8Q)+Sof(H8Q)+Sof(C9Q)+Sof(C10Q)+Sof(H10Q)+Sof(C11Q)+
 Sof(H11Q)+Sof(C12Q)+Sof(H12Q)+Sof(C13Q)+Sof(H13Q)+Sof(C14Q)+Sof(C23Q)+
 Sof(C24Q)+Sof(C25Q)+Sof(C26Q)+Sof(C27Q)+Sof(H27Q)+Sof(C28Q)+Sof(H28A)+
 Sof(H28B)+Sof(C29Q)+Sof(H29A)+Sof(H29B)+Sof(C30Q)+Sof(H30A)+Sof(H30B)+
 Sof(C31Q)+Sof(C32Q)+Sof(C33Q)+Sof(C34Q)+Sof(C35Q)+Sof(H35Q)+Sof(C36Q)+
 Sof(H36A)+Sof(H36B)+Sof(C37Q)+Sof(H37A)+Sof(H37B)+Sof(C38Q)+Sof(H38A)+
 Sof(H38B)+Sof(S2R)+Sof(O3R)+Sof(O4R)+Sof(N2R)+Sof(C23R)+Sof(C24R)+Sof(C25R)+
 Sof(C26R)+Sof(C27R)+Sof(H27R)+Sof(C28R)+Sof(H28E)+Sof(H28F)+Sof(C29R)+
 Sof(H29E)+Sof(H29F)+Sof(C30R)+Sof(H30E)+Sof(H30F)]+1*[Sof(Br1R)+Sof(H8R)]+1*
 [Sof(Br2R)+Sof(H1R)]=1 with esd of 0.0001
 Sof(C1R)=Sof(C2R)=Sof(C3R)=Sof(H3R)=Sof(C4R)=Sof(H4R)=Sof(C5R)=Sof(H5R)=
 Sof(C6R)=Sof(H6R)=Sof(C7R)=Sof(C8R)=Sof(C9R)=Sof(C10R)=Sof(H10R)=Sof(C11R)=
 Sof(H11R)=Sof(C12R)=Sof(H12R)=Sof(C13R)=Sof(H13R)=Sof(C14R)=FVAR(1)
 Sof(O1R)=Sof(O2R)=Sof(N1R)=Sof(C15R)=Sof(C16R)=Sof(C17R)=Sof(C18R)=Sof(C19R)=
 Sof(H19R)=Sof(C20R)=Sof(H20C)=Sof(H20D)=Sof(C21R)=Sof(H21C)=Sof(H21D)=
 Sof(C22R)=Sof(H22C)=Sof(H22D)=Sof(S1R)=1-FVAR(2)
 Sof(S1P)=Sof(S2P)=Sof(O1P)=Sof(O2P)=Sof(N1P)=Sof(C15P)=Sof(C16P)=Sof(C17P)=
 Sof(C18P)=Sof(C19P)=Sof(H19P)=Sof(C20P)=Sof(H20A)=Sof(H20B)=Sof(C21P)=
 Sof(H21A)=Sof(H21B)=Sof(C22P)=Sof(H22A)=Sof(H22B)=Sof(O3P)=Sof(O4P)=Sof(N2P)=
 Sof(C23P)=Sof(C24P)=Sof(C25P)=Sof(C26P)=Sof(C27P)=Sof(H27P)=Sof(C28P)=
 Sof(H28C)=Sof(H28D)=Sof(C29P)=Sof(H29C)=Sof(H29D)=Sof(C30P)=Sof(H30C)=
 Sof(H30D)=0.5*FVAR(3)
 Sof(Br1P)=Sof(C1P)=Sof(C2P)=Sof(C3P)=Sof(H3P)=Sof(C4P)=Sof(H4P)=Sof(C5P)=
 Sof(H5P)=Sof(C6P)=Sof(H6P)=Sof(C7P)=Sof(C8P)=Sof(H8P)=Sof(C9P)=Sof(C10P)=
 Sof(H10P)=Sof(C11P)=Sof(H11P)=Sof(C12P)=Sof(H12P)=Sof(C13P)=Sof(H13P)=
 Sof(C14P)=FVAR(2)
 Sof(S2R)=Sof(O3R)=Sof(O4R)=Sof(N2R)=Sof(C23R)=Sof(C24R)=Sof(C25R)=Sof(C26R)=
 Sof(C27R)=Sof(H27R)=Sof(C28R)=Sof(H28E)=Sof(H28F)=Sof(C29R)=Sof(H29E)=
 Sof(H29F)=Sof(C30R)=Sof(H30E)=Sof(H30F)=1-FVAR(3)
 Sof(S2Q)=Sof(S3Q)=Sof(O3Q)=Sof(O4Q)=Sof(O5Q)=Sof(O6Q)=Sof(N2Q)=Sof(N3Q)=
 Sof(C23Q)=Sof(C24Q)=Sof(C25Q)=Sof(C26Q)=Sof(C27Q)=Sof(H27Q)=Sof(C28Q)=
 Sof(H28A)=Sof(H28B)=Sof(C29Q)=Sof(H29A)=Sof(H29B)=Sof(C30Q)=Sof(H30A)=
 Sof(H30B)=Sof(C31Q)=Sof(C32Q)=Sof(C33Q)=Sof(C34Q)=Sof(C35Q)=Sof(H35Q)=
 Sof(C36Q)=Sof(H36A)=Sof(H36B)=Sof(C37Q)=Sof(H37A)=Sof(H37B)=Sof(C38Q)=
 Sof(H38A)=Sof(H38B)=0.5*FVAR(4)
 Sof(Br1Q)=Sof(C1Q)=Sof(C2Q)=Sof(C3Q)=Sof(H3Q)=Sof(C4Q)=Sof(H4Q)=Sof(C5Q)=
 Sof(H5Q)=Sof(C6Q)=Sof(H6Q)=Sof(C7Q)=Sof(C8Q)=Sof(H8Q)=Sof(C9Q)=Sof(C10Q)=
 Sof(H10Q)=Sof(C11Q)=Sof(H11Q)=Sof(C12Q)=Sof(H12Q)=Sof(C13Q)=Sof(H13Q)=
 Sof(C14Q)=FVAR(3)
 Sof(Br1R)=Sof(H8R)=FVAR(4)
 Sof(Br2R)=Sof(H1R)=FVAR(5)
 Uiso(C1Q)=Uiso(S2Q)=Uiso(S3Q)=Uiso(O3Q)=Uiso(O4Q)=Uiso(O5Q)=Uiso(O6Q)=
 Uiso(N2Q)=Uiso(N3Q)=Uiso(C2Q)=Uiso(C3Q)=Uiso(C4Q)=Uiso(C5Q)=Uiso(C6Q)=
 Uiso(C7Q)=Uiso(C8Q)=Uiso(C9Q)=Uiso(C10Q)=Uiso(C11Q)=Uiso(C12Q)=Uiso(C13Q)=
 Uiso(C14Q)=Uiso(C23Q)=Uiso(C24Q)=Uiso(C25Q)=Uiso(C26Q)=Uiso(C27Q)=Uiso(C28Q)=
 Uiso(C29Q)=Uiso(C30Q)=Uiso(C31Q)=Uiso(C32Q)=Uiso(C33Q)=Uiso(C34Q)=Uiso(C35Q)=
 Uiso(C36Q)=Uiso(C37Q)=Uiso(C38Q)=FVAR(6)
8.a Free rotating group:
 C1Q(S2Q,S3Q,O3Q,O4Q,O5Q,O6Q,N2Q,N3Q,C2Q,C3Q,C4Q,C5Q,C6Q,C7Q,C8Q,C9Q,C10Q,C11Q,
 C12Q,C13Q,C14Q,C23Q,C24Q,C25Q,C26Q,C27Q,C28Q,C29Q,C30Q,C31Q,C32Q,C33Q,C34Q,
 C35Q,C36Q,C37Q,C38Q)
8.b Ternary CH refined with riding coordinates:
 C8Q(H8Q), C27Q(H27Q), C35Q(H35Q), C19P(H19P), C8P(H8P), C27P(H27P),
 C19R(H19R), C27R(H27R)
8.c Secondary CH2 refined with riding coordinates:
 C28Q(H28A,H28B), C29Q(H29A,H29B), C30Q(H30A,H30B), C36Q(H36A,H36B), C37Q(H37A,
 H37B), C38Q(H38A,H38B), C20P(H20A,H20B), C21P(H21A,H21B), C22P(H22A,H22B),
 C28P(H28C,H28D), C29P(H29C,H29D), C30P(H30C,H30D), C20R(H20C,H20D), C21R(H21C,
 H21D), C22R(H22C,H22D), C28R(H28E,H28F), C29R(H29E,H29F), C30R(H30E,H30F)
8.d Aromatic/amide H refined with riding coordinates:
 C3Q(H3Q), C4Q(H4Q), C5Q(H5Q), C6Q(H6Q), C10Q(H10Q), C11Q(H11Q), C12Q(H12Q),
 C13Q(H13Q), C3P(H3P), C4P(H4P), C5P(H5P), C6P(H6P), C10P(H10P), C11P(H11P),
 C12P(H12P), C13P(H13P), C1R(H1R), C3R(H3R), C4R(H4R), C5R(H5R), C6R(H6R),
 C8R(H8R), C10R(H10R), C11R(H11R), C12R(H12R), C13R(H13R)
8.e Fitted hexagon refined as free rotating group:
 C9P(C10P,C11P,C12P,C13P,C14P)
;
_shelx_res_checksum              16809
_olex2_submission_special_instructions 'No special instructions were received'