# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AJ1534
_database_code_depnum_ccdc_archive 'CCDC 2097818'
loop_
_audit_author_name
_audit_author_address
'Anukul Jana'
;Tata Institute of Fundamental Research Hyderabad
India
;
_audit_update_record             
;
2021-07-20 deposited with the CCDC.	2022-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H30 N2, 2(C F3 O3 S)'
_chemical_formula_sum            'C32 H30 F6 N2 O6 S2'
_chemical_formula_weight         716.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0759(2)
_cell_length_b                   12.3329(2)
_cell_length_c                   15.6196(3)
_cell_angle_alpha                107.554(2)
_cell_angle_beta                 102.974(2)
_cell_angle_gamma                90.901(2)
_cell_volume                     1617.80(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18260
_cell_measurement_theta_min      3.0110
_cell_measurement_theta_max      29.0640

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_F_000             740
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.246
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34455
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.810
_diffrn_reflns_theta_max         28.966
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7573
_reflns_number_gt                6590
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0370P)²+0.6707P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7573
_refine_ls_number_parameters     435
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0850
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.58586(11) 0.36866(9) 0.94172(7) 0.0111(2) Uani 1 1 d . . . . .
C1 C 0.54194(13) 0.27069(10) 0.94623(8) 0.0115(2) Uani 1 1 d . . . . .
C2 C 0.48600(13) 0.46308(10) 0.94910(8) 0.0121(2) Uani 1 1 d . . . . .
H2A H 0.378396 0.431660 0.925451 0.015 Uiso 1 1 calc R U . . .
H2B H 0.507744 0.510257 0.911381 0.015 Uiso 1 1 calc R U . . .
C3 C 0.73684(13) 0.39944(11) 0.93092(9) 0.0154(2) Uani 1 1 d . . . . .
H3A H 0.807864 0.345792 0.947332 0.023 Uiso 1 1 calc R U . . .
H3B H 0.773525 0.477081 0.971716 0.023 Uiso 1 1 calc R U . . .
H3C H 0.729446 0.395888 0.866553 0.023 Uiso 1 1 calc R U . . .
C4 C 0.38855(13) 0.25649(10) 0.96341(8) 0.0119(2) Uani 1 1 d . . . . .
C5 C 0.26296(14) 0.22228(10) 0.88785(8) 0.0148(2) Uani 1 1 d . . . . .
H5 H 0.275961 0.203085 0.826516 0.018 Uiso 1 1 calc R U . . .
C6 C 0.11889(14) 0.21671(11) 0.90359(9) 0.0165(3) Uani 1 1 d . . . . .
H6 H 0.032680 0.193865 0.852674 0.020 Uiso 1 1 calc R U . . .
C7 C 0.09984(14) 0.24427(11) 0.99320(9) 0.0156(2) Uani 1 1 d . . . . .
H7 H 0.000861 0.240098 1.003374 0.019 Uiso 1 1 calc R U . . .
C8 C 0.22543(14) 0.27796(11) 1.06803(9) 0.0148(2) Uani 1 1 d . . . . .
H8 H 0.212038 0.297005 1.129267 0.018 Uiso 1 1 calc R U . . .
C9 C 0.37049(14) 0.28389(10) 1.05355(8) 0.0136(2) Uani 1 1 d . . . . .
H9 H 0.456513 0.306393 1.104596 0.016 Uiso 1 1 calc R U . . .
C10 C 0.63527(13) 0.17261(10) 0.93347(8) 0.0126(2) Uani 1 1 d . . . . .
C11 C 0.65430(15) 0.11118(11) 0.99656(9) 0.0188(3) Uani 1 1 d . . . . .
H11 H 0.607190 0.132169 1.047007 0.023 Uiso 1 1 calc R U . . .
C12 C 0.74236(16) 0.01941(12) 0.98507(10) 0.0230(3) Uani 1 1 d . . . . .
H12 H 0.758275 -0.020915 1.028993 0.028 Uiso 1 1 calc R U . . .
C13 C 0.80748(15) -0.01400(11) 0.90979(10) 0.0201(3) Uani 1 1 d . . . . .
H13 H 0.868532 -0.076472 0.902633 0.024 Uiso 1 1 calc R U . . .
C14 C 0.78318(14) 0.04407(11) 0.84507(9) 0.0170(3) Uani 1 1 d . . . . .
H14 H 0.824750 0.019532 0.792444 0.020 Uiso 1 1 calc R U . . .
C15 C 0.69860(14) 0.13767(11) 0.85684(9) 0.0148(2) Uani 1 1 d . . . . .
H15 H 0.683655 0.178016 0.812939 0.018 Uiso 1 1 calc R U . . .
N2 N 0.84623(11) 0.59512(9) 0.52764(7) 0.0124(2) Uani 1 1 d . . . . .
C16 C 0.83930(13) 0.69694(11) 0.58274(8) 0.0129(2) Uani 1 1 d . . . . .
C17 C 0.98446(13) 0.55907(10) 0.49554(8) 0.0136(2) Uani 1 1 d . . . . .
H17A H 1.072098 0.614812 0.533217 0.016 Uiso 1 1 calc R U . . .
H17B H 0.970299 0.556445 0.430202 0.016 Uiso 1 1 calc R U . . .
C18 C 0.71176(14) 0.51079(11) 0.48281(9) 0.0170(3) Uani 1 1 d . . . . .
H18A H 0.714728 0.453765 0.515201 0.026 Uiso 1 1 calc R U . . .
H18B H 0.712633 0.472857 0.418053 0.026 Uiso 1 1 calc R U . . .
H18C H 0.619052 0.550021 0.485559 0.026 Uiso 1 1 calc R U . . .
C19 C 0.95853(13) 0.79071(10) 0.60287(9) 0.0142(2) Uani 1 1 d . . . . .
C20 C 1.01958(14) 0.85732(11) 0.69437(9) 0.0179(3) Uani 1 1 d . . . . .
H20 H 0.989537 0.839692 0.743469 0.021 Uiso 1 1 calc R U . . .
C21 C 1.12478(15) 0.94974(12) 0.71317(10) 0.0239(3) Uani 1 1 d . . . . .
H21 H 1.168607 0.994093 0.775467 0.029 Uiso 1 1 calc R U . . .
C22 C 1.16615(15) 0.97763(12) 0.64163(11) 0.0261(3) Uani 1 1 d . . . . .
H22 H 1.236563 1.041737 0.654859 0.031 Uiso 1 1 calc R U . . .
C23 C 1.10449(16) 0.91169(12) 0.55080(11) 0.0242(3) Uani 1 1 d . . . . .
H23 H 1.133377 0.930688 0.501922 0.029 Uiso 1 1 calc R U . . .
C24 C 1.00086(15) 0.81810(11) 0.53054(9) 0.0189(3) Uani 1 1 d . . . . .
H24 H 0.959083 0.773088 0.468166 0.023 Uiso 1 1 calc R U . . .
C25 C 0.70837(13) 0.72433(11) 0.62447(8) 0.0151(2) Uani 1 1 d . . . . .
C26 C 0.64902(14) 0.65050(11) 0.66357(8) 0.0170(3) Uani 1 1 d . . . . .
H26 H 0.693332 0.581331 0.663985 0.020 Uiso 1 1 calc R U . . .
C27 C 0.52489(15) 0.67879(12) 0.70182(9) 0.0205(3) Uani 1 1 d . . . . .
H27 H 0.484507 0.629078 0.728644 0.025 Uiso 1 1 calc R U . . .
C28 C 0.46028(15) 0.77960(13) 0.70073(9) 0.0241(3) Uani 1 1 d . . . . .
H28 H 0.374048 0.797865 0.725541 0.029 Uiso 1 1 calc R U . . .
C29 C 0.52054(15) 0.85395(13) 0.66370(10) 0.0235(3) Uani 1 1 d . . . . .
H29 H 0.476413 0.923381 0.664041 0.028 Uiso 1 1 calc R U . . .
C30 C 0.64520(14) 0.82724(11) 0.62611(9) 0.0185(3) Uani 1 1 d . . . . .
H30 H 0.687395 0.878782 0.601584 0.022 Uiso 1 1 calc R U . . .
C31 C 0.95957(15) 0.52162(12) 0.22047(10) 0.0219(3) Uani 1 1 d . . . . .
F1 F 0.87919(11) 0.60767(7) 0.25081(7) 0.0364(2) Uani 1 1 d . . . . .
F2 F 1.09282(10) 0.53931(9) 0.28225(7) 0.0407(3) Uani 1 1 d . . . . .
F3 F 0.98671(11) 0.52804(9) 0.14143(7) 0.0384(2) Uani 1 1 d . . . . .
S1 S 0.86172(3) 0.38363(3) 0.20440(2) 0.01341(8) Uani 1 1 d . . . . .
O1 O 0.84588(11) 0.39248(8) 0.29593(6) 0.0206(2) Uani 1 1 d . . . . .
O2 O 0.96414(11) 0.30299(9) 0.17049(7) 0.0262(2) Uani 1 1 d . . . . .
O3 O 0.72186(11) 0.38183(9) 0.13823(7) 0.0243(2) Uani 1 1 d . . . . .
C32 C 0.60700(16) 0.22927(13) 0.61721(10) 0.0231(3) Uani 1 1 d . . . . .
F4 F 0.64379(11) 0.28226(9) 0.56073(6) 0.0361(2) Uani 1 1 d . . . . .
F5 F 0.56093(12) 0.12135(8) 0.56687(7) 0.0391(2) Uani 1 1 d . . . . .
F6 F 0.73561(9) 0.22868(9) 0.67938(6) 0.0334(2) Uani 1 1 d . . . . .
S2 S 0.46193(4) 0.29954(3) 0.67307(2) 0.01996(8) Uani 1 1 d . . . . .
O4 O 0.44137(12) 0.23170(11) 0.73081(7) 0.0311(3) Uani 1 1 d . . . . .
O5 O 0.53367(13) 0.41290(10) 0.72268(8) 0.0383(3) Uani 1 1 d . . . . .
O6 O 0.33527(12) 0.29044(10) 0.59641(7) 0.0300(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.2934(16) . ?
N1 C3 1.4752(15) . ?
N1 C2 1.4798(15) . ?
C1 C10 1.4775(17) . ?
C1 C4 1.4931(16) . ?
C2 C2 1.536(2) 2_667 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C9 1.3934(17) . ?
C4 C5 1.3967(17) . ?
C5 C6 1.3880(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.3886(18) . ?
C6 H6 0.9500 . ?
C7 C8 1.3899(18) . ?
C7 H7 0.9500 . ?
C8 C9 1.3894(17) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.3974(18) . ?
C10 C15 1.3979(17) . ?
C11 C12 1.3865(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.3874(19) . ?
C13 H13 0.9500 . ?
C14 C15 1.3852(18) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
N2 C16 1.3024(16) . ?
N2 C17 1.4794(15) . ?
N2 C18 1.4827(15) . ?
C16 C25 1.4761(17) . ?
C16 C19 1.4818(17) . ?
C17 C17 1.530(2) 2_766 ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.3950(18) . ?
C19 C24 1.3997(18) . ?
C20 C21 1.3910(19) . ?
C20 H20 0.9500 . ?
C21 C22 1.387(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3888(19) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.3964(19) . ?
C25 C26 1.3999(19) . ?
C26 C27 1.3917(18) . ?
C26 H26 0.9500 . ?
C27 C28 1.386(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.386(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.3881(19) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 F1 1.3265(17) . ?
C31 F2 1.3349(16) . ?
C31 F3 1.3364(16) . ?
C31 S1 1.8282(14) . ?
S1 O2 1.4373(10) . ?
S1 O1 1.4405(9) . ?
S1 O3 1.4409(9) . ?
C32 F5 1.3297(17) . ?
C32 F4 1.3380(16) . ?
C32 F6 1.3420(16) . ?
C32 S2 1.8280(15) . ?
S2 O6 1.4369(10) . ?
S2 O5 1.4389(12) . ?
S2 O4 1.4401(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C3 125.01(10) . . ?
C1 N1 C2 121.70(10) . . ?
C3 N1 C2 113.29(9) . . ?
N1 C1 C10 122.98(11) . . ?
N1 C1 C4 117.96(11) . . ?
C10 C1 C4 119.05(10) . . ?
N1 C2 C2 109.23(12) . 2_667 ?
N1 C2 H2A 109.8 . . ?
C2 C2 H2A 109.8 2_667 . ?
N1 C2 H2B 109.8 . . ?
C2 C2 H2B 109.8 2_667 . ?
H2A C2 H2B 108.3 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C9 C4 C5 120.79(11) . . ?
C9 C4 C1 120.33(11) . . ?
C5 C4 C1 118.76(11) . . ?
C6 C5 C4 119.09(11) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 120.49(12) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C8 120.07(11) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 120.21(11) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C4 119.34(11) . . ?
C8 C9 H9 120.3 . . ?
C4 C9 H9 120.3 . . ?
C11 C10 C15 119.83(12) . . ?
C11 C10 C1 119.41(11) . . ?
C15 C10 C1 120.69(11) . . ?
C12 C11 C10 119.59(12) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 120.47(13) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 119.86(12) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C15 C14 C13 120.31(12) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C10 119.85(12) . . ?
C14 C15 H15 120.1 . . ?
C10 C15 H15 120.1 . . ?
C16 N2 C17 122.60(10) . . ?
C16 N2 C18 122.86(10) . . ?
C17 N2 C18 114.14(9) . . ?
N2 C16 C25 120.92(11) . . ?
N2 C16 C19 121.58(11) . . ?
C25 C16 C19 117.45(11) . . ?
N2 C17 C17 109.44(12) . 2_766 ?
N2 C17 H17A 109.8 . . ?
C17 C17 H17A 109.8 2_766 . ?
N2 C17 H17B 109.8 . . ?
C17 C17 H17B 109.8 2_766 . ?
H17A C17 H17B 108.2 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C24 120.14(12) . . ?
C20 C19 C16 119.32(11) . . ?
C24 C19 C16 120.34(11) . . ?
C21 C20 C19 119.51(13) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C22 C21 C20 120.48(13) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 119.81(13) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.64(14) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C19 119.39(13) . . ?
C23 C24 H24 120.3 . . ?
C19 C24 H24 120.3 . . ?
C30 C25 C26 119.87(12) . . ?
C30 C25 C16 118.77(12) . . ?
C26 C25 C16 121.34(12) . . ?
C27 C26 C25 119.77(13) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C28 C27 C26 119.90(13) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C29 C28 C27 120.49(12) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C30 120.17(14) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C29 C30 C25 119.76(13) . . ?
C29 C30 H30 120.1 . . ?
C25 C30 H30 120.1 . . ?
F1 C31 F2 107.13(12) . . ?
F1 C31 F3 107.35(12) . . ?
F2 C31 F3 107.57(11) . . ?
F1 C31 S1 111.91(9) . . ?
F2 C31 S1 111.13(10) . . ?
F3 C31 S1 111.51(10) . . ?
O2 S1 O1 114.92(6) . . ?
O2 S1 O3 115.11(6) . . ?
O1 S1 O3 115.02(6) . . ?
O2 S1 C31 103.43(6) . . ?
O1 S1 C31 103.16(6) . . ?
O3 S1 C31 102.73(6) . . ?
F5 C32 F4 107.25(11) . . ?
F5 C32 F6 107.36(12) . . ?
F4 C32 F6 106.79(11) . . ?
F5 C32 S2 111.87(10) . . ?
F4 C32 S2 111.63(10) . . ?
F6 C32 S2 111.66(9) . . ?
O6 S2 O5 115.82(7) . . ?
O6 S2 O4 115.05(7) . . ?
O5 S2 O4 114.64(7) . . ?
O6 S2 C32 103.18(6) . . ?
O5 S2 C32 102.77(7) . . ?
O4 S2 C32 102.74(7) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2B O3 0.99 2.59 3.1000(15) 112.1 2_666 yes
C3 H3C O5 0.98 2.60 3.4132(18) 140.6 . yes
C17 H17A O1 0.99 2.63 3.1436(15) 112.1 2_766 yes
C17 H17B O1 0.99 2.46 3.1334(15) 124.6 . yes
C18 H18A F4 0.98 2.54 3.4867(16) 161.7 . yes
C18 H18B O1 0.98 2.45 3.3487(16) 151.8 . yes

_refine_diff_density_max         0.390
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.050

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AJ1670R
_database_code_depnum_ccdc_archive 'CCDC 2097821'
loop_
_audit_author_name
_audit_author_address
'Anukul Jana'
;Tata Institute of Fundamental Research Hyderabad
India
;
_audit_update_record             
;
2021-07-20 deposited with the CCDC.	2022-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H22 N2'
_chemical_formula_sum            'C18 H22 N2'
_chemical_formula_weight         266.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.0877(12)
_cell_length_b                   5.7417(4)
_cell_length_c                   18.1222(14)
_cell_angle_alpha                90
_cell_angle_beta                 108.833(8)
_cell_angle_gamma                90
_cell_volume                     1584.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5745
_cell_measurement_theta_min      3.0870
_cell_measurement_theta_max      27.6220

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_F_000             576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.066
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.26035
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14432
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.080
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3213
_reflns_number_gt                2528
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0755P)²+0.1727P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3213
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1623
_refine_ls_wR_factor_gt          0.1521
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.20844(9) 0.7116(2) 0.65026(8) 0.0468(3) Uani 1 1 d . . . . .
C2 C 0.05366(10) 0.7220(3) 0.58124(10) 0.0654(5) Uani 1 1 d . . . . .
H2A H 0.009273 0.705373 0.530491 0.078 Uiso 1 1 calc R U . . .
H2B H 0.049561 0.878543 0.599926 0.078 Uiso 1 1 calc R U . . .
C3 C 0.03698(10) 0.5492(3) 0.63656(11) 0.0662(5) Uani 1 1 d . . . . .
H3A H -0.022183 0.569070 0.638431 0.079 Uiso 1 1 calc R U . . .
H3B H 0.042028 0.392516 0.618436 0.079 Uiso 1 1 calc R U . . .
C4 C 0.18991(9) 0.5517(2) 0.71207(8) 0.0468(4) Uani 1 1 d . . . . .
C5 C 0.15470(13) 0.8515(4) 0.51792(10) 0.0770(5) Uani 1 1 d . . . . .
H5A H 0.110375 0.829741 0.468176 0.115 Uiso 1 1 calc R U . . .
H5B H 0.211587 0.825071 0.512971 0.115 Uiso 1 1 calc R U . . .
H5C H 0.151594 1.007690 0.535712 0.115 Uiso 1 1 calc R U . . .
C6 C 0.08249(12) 0.4161(3) 0.76850(13) 0.0773(5) Uani 1 1 d . . . . .
H6A H 0.022284 0.429401 0.766405 0.116 Uiso 1 1 calc R U . . .
H6B H 0.120209 0.449427 0.820418 0.116 Uiso 1 1 calc R U . . .
H6C H 0.093464 0.260631 0.754442 0.116 Uiso 1 1 calc R U . . .
C7 C 0.29813(9) 0.6523(2) 0.64490(8) 0.0460(3) Uani 1 1 d . . . . .
C8 C 0.31152(10) 0.4476(3) 0.60997(9) 0.0572(4) Uani 1 1 d . . . . .
H8 H 0.264398 0.348322 0.587743 0.069 Uiso 1 1 calc R U . . .
C9 C 0.39425(12) 0.3887(3) 0.60766(10) 0.0663(5) Uani 1 1 d . . . . .
H9 H 0.402101 0.251084 0.583633 0.080 Uiso 1 1 calc R U . . .
C10 C 0.46520(11) 0.5338(3) 0.64100(10) 0.0671(5) Uani 1 1 d . . . . .
H10 H 0.520884 0.493763 0.640116 0.081 Uiso 1 1 calc R U . . .
C11 C 0.45235(11) 0.7366(3) 0.67517(10) 0.0657(5) Uani 1 1 d . . . . .
H11 H 0.499481 0.836062 0.697181 0.079 Uiso 1 1 calc R U . . .
C12 C 0.36979(10) 0.7952(3) 0.67731(8) 0.0546(4) Uani 1 1 d . . . . .
H12 H 0.362329 0.933599 0.701067 0.066 Uiso 1 1 calc R U . . .
C13 C 0.25502(9) 0.5999(2) 0.79169(8) 0.0469(3) Uani 1 1 d . . . . .
C14 C 0.32047(10) 0.4442(3) 0.82793(9) 0.0596(4) Uani 1 1 d . . . . .
H14 H 0.326124 0.307171 0.802618 0.071 Uiso 1 1 calc R U . . .
C15 C 0.37800(12) 0.4899(4) 0.90178(10) 0.0767(5) Uani 1 1 d . . . . .
H15 H 0.421930 0.383094 0.925573 0.092 Uiso 1 1 calc R U . . .
C16 C 0.37105(13) 0.6889(4) 0.93988(10) 0.0758(5) Uani 1 1 d . . . . .
H16 H 0.409587 0.717391 0.989697 0.091 Uiso 1 1 calc R U . . .
C17 C 0.30690(13) 0.8473(3) 0.90445(10) 0.0721(5) Uani 1 1 d . . . . .
H17 H 0.302191 0.984560 0.930045 0.087 Uiso 1 1 calc R U . . .
C18 C 0.24953(11) 0.8036(3) 0.83120(9) 0.0609(4) Uani 1 1 d . . . . .
H18 H 0.206248 0.912301 0.807635 0.073 Uiso 1 1 calc R U . . .
N1 N 0.14033(8) 0.6872(2) 0.57396(7) 0.0572(4) Uani 1 1 d . . . . .
N2 N 0.09994(8) 0.5811(2) 0.71421(8) 0.0562(4) Uani 1 1 d . . . . .
H4 H 0.1964(9) 0.392(3) 0.6965(9) 0.052(4) Uiso 1 1 d . . . . .
H1 H 0.2092(9) 0.880(3) 0.6683(9) 0.052(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.4677(18) . ?
C1 C7 1.5159(19) . ?
C1 C4 1.550(2) . ?
C1 H1 1.018(16) . ?
C2 N1 1.456(2) . ?
C2 C3 1.495(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.456(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N2 1.4700(18) . ?
C4 C13 1.510(2) . ?
C4 H4 0.974(16) . ?
C5 N1 1.458(2) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N2 1.457(2) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C12 1.382(2) . ?
C7 C8 1.384(2) . ?
C8 C9 1.387(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.385(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.365(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.383(2) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.376(2) . ?
C13 C18 1.389(2) . ?
C14 C15 1.384(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.358(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.370(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.373(2) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C7 110.78(11) . . ?
N1 C1 C4 111.42(11) . . ?
C7 C1 C4 108.83(11) . . ?
N1 C1 H1 108.7(8) . . ?
C7 C1 H1 108.6(8) . . ?
C4 C1 H1 108.3(8) . . ?
N1 C2 C3 110.73(13) . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C2 110.19(13) . . ?
N2 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
N2 C4 C13 109.82(11) . . ?
N2 C4 C1 111.84(11) . . ?
C13 C4 C1 110.26(11) . . ?
N2 C4 H4 108.3(9) . . ?
C13 C4 H4 110.1(9) . . ?
C1 C4 H4 106.5(9) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 117.82(13) . . ?
C12 C7 C1 121.35(12) . . ?
C8 C7 C1 120.77(13) . . ?
C7 C8 C9 120.90(15) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C10 C9 C8 120.25(15) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 119.14(15) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 120.50(16) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C7 C12 C11 121.39(15) . . ?
C7 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C14 C13 C18 117.86(14) . . ?
C14 C13 C4 121.68(13) . . ?
C18 C13 C4 120.46(13) . . ?
C13 C14 C15 120.54(16) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C16 C15 C14 120.79(17) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 119.57(16) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C16 C17 C18 120.09(17) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C13 121.16(16) . . ?
C17 C18 H18 119.4 . . ?
C13 C18 H18 119.4 . . ?
C2 N1 C5 110.25(13) . . ?
C2 N1 C1 110.31(11) . . ?
C5 N1 C1 110.89(13) . . ?
C3 N2 C6 110.20(14) . . ?
C3 N2 C4 110.11(11) . . ?
C6 N2 C4 110.44(12) . . ?

_refine_diff_density_max         0.167
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.046

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AJ1650
_database_code_depnum_ccdc_archive 'CCDC 2097823'
loop_
_audit_author_name
_audit_author_address
'Anukul Jana'
;Tata Institute of Fundamental Research Hyderabad
India
;
_audit_update_record             
;
2021-07-20 deposited with the CCDC.	2022-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H30 N2, 2(F6 Sb)'
_chemical_formula_sum            'C30 H30 F12 N2 Sb2'
_chemical_formula_weight         890.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3302(2)
_cell_length_b                   15.9677(3)
_cell_length_c                   16.8928(3)
_cell_angle_alpha                86.189(2)
_cell_angle_beta                 83.167(2)
_cell_angle_gamma                84.182(2)
_cell_volume                     2482.20(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16840
_cell_measurement_theta_min      2.8960
_cell_measurement_theta_max      28.1480

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_F_000             1302
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    1.724
_shelx_estimated_absorpt_T_min   0.682
_shelx_estimated_absorpt_T_max   0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.60504
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40157
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.568
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10104
_reflns_number_gt                8240
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0648P)²+1.9098P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10104
_refine_ls_number_parameters     625
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1347
_refine_ls_wR_factor_gt          0.1277
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.1840(3) 0.30460(19) 0.89602(19) 0.0421(7) Uani 1 1 d . . . . .
N2 N 0.5185(3) 0.38136(19) 0.77902(18) 0.0415(7) Uani 1 1 d . . . . .
C1 C 0.1614(4) 0.2394(2) 0.9445(2) 0.0398(8) Uani 1 1 d . . . . .
C2 C 0.3273(4) 0.3388(3) 0.8811(2) 0.0451(9) Uani 1 1 d . . . . .
H2A H 0.398951 0.300429 0.905502 0.054 Uiso 1 1 calc R U . . .
H2B H 0.322042 0.392590 0.905210 0.054 Uiso 1 1 calc R U . . .
C3 C 0.3731(4) 0.3502(3) 0.7920(2) 0.0451(9) Uani 1 1 d . . . . .
H3A H 0.375669 0.296786 0.767319 0.054 Uiso 1 1 calc R U . . .
H3B H 0.303753 0.390182 0.767639 0.054 Uiso 1 1 calc R U . . .
C4 C 0.5470(4) 0.4480(2) 0.7335(2) 0.0407(8) Uani 1 1 d . . . . .
C5 C 0.0687(5) 0.3541(3) 0.8557(3) 0.0626(12) Uani 1 1 d . . . . .
H5A H 0.071600 0.336200 0.802297 0.094 Uiso 1 1 calc R U . . .
H5B H 0.083370 0.412821 0.853810 0.094 Uiso 1 1 calc R U . . .
H5C H -0.024021 0.345308 0.884647 0.094 Uiso 1 1 calc R U . . .
C6 C 0.6317(5) 0.3271(3) 0.8172(3) 0.0565(11) Uani 1 1 d . . . . .
H6A H 0.725413 0.337586 0.790571 0.085 Uiso 1 1 calc R U . . .
H6B H 0.616584 0.268944 0.813439 0.085 Uiso 1 1 calc R U . . .
H6C H 0.626543 0.339410 0.872365 0.085 Uiso 1 1 calc R U . . .
C7 C 0.0313(4) 0.1941(2) 0.9459(2) 0.0441(8) Uani 1 1 d . . . . .
C8 C -0.0235(5) 0.1785(3) 0.8759(3) 0.0547(10) Uani 1 1 d . . . . .
H8 H 0.022766 0.196357 0.826814 0.066 Uiso 1 1 calc R U . . .
C9 C -0.1462(5) 0.1364(3) 0.8792(3) 0.0664(12) Uani 1 1 d . . . . .
H9 H -0.183653 0.127050 0.832266 0.080 Uiso 1 1 calc R U . . .
C10 C -0.2136(6) 0.1084(4) 0.9516(4) 0.0820(16) Uani 1 1 d . . . . .
H10 H -0.297439 0.081083 0.953388 0.098 Uiso 1 1 calc R U . . .
C11 C -0.1580(6) 0.1202(4) 1.0214(4) 0.0793(16) Uani 1 1 d . . . . .
H11 H -0.201821 0.098969 1.069893 0.095 Uiso 1 1 calc R U . . .
C12 C -0.0353(5) 0.1644(3) 1.0193(3) 0.0598(11) Uani 1 1 d . . . . .
H12 H 0.001479 0.173899 1.066399 0.072 Uiso 1 1 calc R U . . .
C13 C 0.2665(4) 0.2110(2) 1.0025(2) 0.0402(8) Uani 1 1 d . . . . .
C14 C 0.3080(5) 0.2687(3) 1.0509(2) 0.0506(9) Uani 1 1 d . . . . .
H14 H 0.271224 0.324960 1.046307 0.061 Uiso 1 1 calc R U . . .
C15 C 0.4037(5) 0.2431(3) 1.1061(3) 0.0627(12) Uani 1 1 d . . . . .
H15 H 0.431002 0.281836 1.138891 0.075 Uiso 1 1 calc R U . . .
C16 C 0.4585(5) 0.1597(4) 1.1123(3) 0.0679(14) Uani 1 1 d . . . . .
H16 H 0.525029 0.142407 1.148319 0.082 Uiso 1 1 calc R U . . .
C17 C 0.4152(5) 0.1020(3) 1.0654(3) 0.0615(12) Uani 1 1 d . . . . .
H17 H 0.451661 0.045709 1.070488 0.074 Uiso 1 1 calc R U . . .
C18 C 0.3177(4) 0.1268(3) 1.0103(2) 0.0502(9) Uani 1 1 d . . . . .
H18 H 0.287258 0.087550 0.979281 0.060 Uiso 1 1 calc R U . . .
C19 C 0.4475(4) 0.4842(3) 0.6761(2) 0.0469(9) Uani 1 1 d . . . . .
C20 C 0.4008(6) 0.4327(3) 0.6231(3) 0.0672(13) Uani 1 1 d . . . . .
H20 H 0.429000 0.375137 0.625524 0.081 Uiso 1 1 calc R U . . .
C21 C 0.3130(7) 0.4667(5) 0.5671(3) 0.095(2) Uani 1 1 d . . . . .
H21 H 0.279302 0.431854 0.532808 0.114 Uiso 1 1 calc R U . . .
C22 C 0.2752(6) 0.5512(5) 0.5617(4) 0.099(2) Uani 1 1 d . . . . .
H22 H 0.216830 0.573866 0.523109 0.118 Uiso 1 1 calc R U . . .
C23 C 0.3223(6) 0.6035(4) 0.6126(4) 0.0847(18) Uani 1 1 d . . . . .
H23 H 0.295490 0.661199 0.608072 0.102 Uiso 1 1 calc R U . . .
C24 C 0.4098(5) 0.5710(3) 0.6709(3) 0.0639(12) Uani 1 1 d . . . . .
H24 H 0.442206 0.606241 0.705280 0.077 Uiso 1 1 calc R U . . .
C25 C 0.6823(4) 0.4881(2) 0.7348(2) 0.0429(8) Uani 1 1 d . . . . .
C26 C 0.7575(5) 0.5145(3) 0.6628(3) 0.0584(11) Uani 1 1 d . . . . .
H26 H 0.722292 0.506509 0.614861 0.070 Uiso 1 1 calc R U . . .
C27 C 0.8834(6) 0.5522(4) 0.6624(3) 0.0767(15) Uani 1 1 d . . . . .
H27 H 0.935045 0.567990 0.614106 0.092 Uiso 1 1 calc R U . . .
C28 C 0.9332(5) 0.5666(3) 0.7329(4) 0.0742(14) Uani 1 1 d . . . . .
H28 H 1.018559 0.592261 0.732135 0.089 Uiso 1 1 calc R U . . .
C29 C 0.8575(5) 0.5434(3) 0.8050(3) 0.0625(12) Uani 1 1 d . . . . .
H29 H 0.890593 0.554591 0.852657 0.075 Uiso 1 1 calc R U . . .
C30 C 0.7325(5) 0.5036(3) 0.8060(3) 0.0519(10) Uani 1 1 d . . . . .
H30 H 0.682077 0.487142 0.854426 0.062 Uiso 1 1 calc R U . . .
N3 N 0.1876(4) 0.9758(2) 0.5291(2) 0.0510(8) Uani 1 1 d . . . . .
C31 C 0.2145(4) 0.9156(2) 0.5818(2) 0.0445(8) Uani 1 1 d . . . . .
C32 C 0.0407(5) 1.0217(3) 0.5270(3) 0.0561(10) Uani 1 1 d . . . . .
H32A H 0.049276 1.079640 0.507450 0.067 Uiso 1 1 calc R U . . .
H32B H -0.010843 1.021821 0.580369 0.067 Uiso 1 1 calc R U . . .
C33 C 0.2953(6) 1.0066(4) 0.4667(3) 0.0792(16) Uani 1 1 d . . . . .
H33A H 0.389784 0.980206 0.475247 0.119 Uiso 1 1 calc R U . . .
H33B H 0.294668 1.066573 0.468469 0.119 Uiso 1 1 calc R U . . .
H33C H 0.272218 0.993106 0.415413 0.119 Uiso 1 1 calc R U . . .
C34 C 0.3542(4) 0.8628(2) 0.5799(2) 0.0438(8) Uani 1 1 d . . . . .
C35 C 0.4217(4) 0.8277(3) 0.5103(3) 0.0535(10) Uani 1 1 d . . . . .
H35 H 0.380318 0.838134 0.462733 0.064 Uiso 1 1 calc R U . . .
C36 C 0.5504(5) 0.7771(3) 0.5122(3) 0.0639(12) Uani 1 1 d . . . . .
H36 H 0.595229 0.753262 0.465792 0.077 Uiso 1 1 calc R U . . .
C37 C 0.6127(5) 0.7617(3) 0.5813(3) 0.0712(14) Uani 1 1 d . . . . .
H37 H 0.701617 0.729584 0.581311 0.085 Uiso 1 1 calc R U . . .
C38 C 0.5443(6) 0.7938(4) 0.6512(3) 0.0721(14) Uani 1 1 d . . . . .
H38 H 0.585342 0.781784 0.698703 0.087 Uiso 1 1 calc R U . . .
C39 C 0.4146(5) 0.8437(3) 0.6505(3) 0.0592(11) Uani 1 1 d . . . . .
H39 H 0.367622 0.864669 0.697791 0.071 Uiso 1 1 calc R U . . .
C40 C 0.1035(4) 0.8978(3) 0.6505(2) 0.0475(9) Uani 1 1 d . . . . .
C41 C 0.0594(6) 0.9563(3) 0.7074(3) 0.0680(13) Uani 1 1 d . . . . .
H41 H 0.096792 1.008455 0.703127 0.082 Uiso 1 1 calc R U . . .
C42 C -0.0415(7) 0.9358(5) 0.7707(3) 0.0910(19) Uani 1 1 d . . . . .
H42 H -0.069184 0.973785 0.810352 0.109 Uiso 1 1 calc R U . . .
C43 C -0.1006(7) 0.8617(5) 0.7757(4) 0.096(2) Uani 1 1 d . . . . .
H43 H -0.171105 0.850109 0.817648 0.116 Uiso 1 1 calc R U . . .
C44 C -0.0574(6) 0.8031(4) 0.7196(4) 0.0876(18) Uani 1 1 d . . . . .
H44 H -0.097087 0.751654 0.724099 0.105 Uiso 1 1 calc R U . . .
C45 C 0.0450(5) 0.8210(3) 0.6566(3) 0.0658(12) Uani 1 1 d . . . . .
H45 H 0.074672 0.781675 0.618402 0.079 Uiso 1 1 calc R U . . .
Sb1 Sb 0.24287(3) 0.60205(2) 0.92308(2) 0.05618(11) Uani 1 1 d . . . . .
F1 F 0.2133(6) 0.5084(3) 0.9928(2) 0.1200(15) Uani 1 1 d . . . . .
F2 F 0.4338(4) 0.5615(3) 0.9004(3) 0.1332(17) Uani 1 1 d . . . . .
F3 F 0.2727(5) 0.6941(2) 0.8527(2) 0.1102(13) Uani 1 1 d . . . . .
F4 F 0.0460(4) 0.6401(3) 0.9414(3) 0.1115(14) Uani 1 1 d . . . . .
F5 F 0.2012(4) 0.5396(2) 0.8404(2) 0.0904(10) Uani 1 1 d . . . . .
F6 F 0.2809(5) 0.6622(3) 1.0057(2) 0.1199(15) Uani 1 1 d . . . . .
Sb2 Sb 0.43999(3) 0.08636(2) 0.74555(2) 0.05196(11) Uani 1 1 d . . . . .
F7 F 0.3496(5) 0.0008(2) 0.8063(2) 0.0993(11) Uani 1 1 d . . . . .
F8 F 0.6071(5) 0.0147(3) 0.7293(3) 0.1396(19) Uani 1 1 d . . . . .
F9 F 0.3790(4) 0.0523(2) 0.6537(2) 0.0929(10) Uani 1 1 d . . . . .
F10 F 0.5278(5) 0.1739(3) 0.6865(2) 0.1065(13) Uani 1 1 d . . . . .
F11 F 0.2743(4) 0.1577(2) 0.7645(3) 0.1118(14) Uani 1 1 d . . . . .
F12 F 0.5015(5) 0.1230(3) 0.8369(2) 0.1244(16) Uani 1 1 d . . . . .
Sb3 Sb 0.96158(4) 0.26445(2) 0.60281(2) 0.06661(13) Uani 1 1 d . . . . .
F13 F 0.9212(8) 0.1789(4) 0.6772(4) 0.187(3) Uani 1 1 d . . . . .
F14 F 1.1325(5) 0.2017(4) 0.5741(4) 0.154(2) Uani 1 1 d . . . . .
F15 F 0.8776(5) 0.2090(4) 0.5331(4) 0.156(2) Uani 1 1 d . . . . .
F16 F 1.0050(6) 0.3507(4) 0.5300(4) 0.178(3) Uani 1 1 d . . . . .
F17 F 0.7743(6) 0.3222(3) 0.6245(4) 0.154(2) Uani 1 1 d . . . . .
F18 F 1.0307(14) 0.3162(4) 0.6770(5) 0.301(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.300(5) . ?
N1 C5 1.475(5) . ?
N1 C2 1.482(5) . ?
N2 C4 1.301(5) . ?
N2 C6 1.478(5) . ?
N2 C3 1.479(5) . ?
C1 C7 1.472(5) . ?
C1 C13 1.485(5) . ?
C2 C3 1.519(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C19 1.473(5) . ?
C4 C25 1.476(6) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.388(6) . ?
C7 C12 1.396(6) . ?
C8 C9 1.379(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.377(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.374(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.400(7) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.383(5) . ?
C13 C14 1.384(6) . ?
C14 C15 1.381(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.380(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.374(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.389(6) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.389(6) . ?
C19 C24 1.396(6) . ?
C20 C21 1.374(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.359(10) . ?
C21 H21 0.9300 . ?
C22 C23 1.375(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.394(7) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C30 1.386(6) . ?
C25 C26 1.393(6) . ?
C26 C27 1.373(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.370(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.381(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.382(6) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
N3 C31 1.293(5) . ?
N3 C33 1.463(6) . ?
N3 C32 1.490(5) . ?
C31 C34 1.476(5) . ?
C31 C40 1.493(5) . ?
C32 C32 1.498(9) 2_576 ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C39 1.382(6) . ?
C34 C35 1.391(6) . ?
C35 C36 1.380(6) . ?
C35 H35 0.9300 . ?
C36 C37 1.362(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.377(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.382(6) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.383(6) . ?
C40 C45 1.384(6) . ?
C41 C42 1.383(8) . ?
C41 H41 0.9300 . ?
C42 C43 1.349(9) . ?
C42 H42 0.9300 . ?
C43 C44 1.373(9) . ?
C43 H43 0.9300 . ?
C44 C45 1.378(7) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
Sb1 F6 1.834(3) . ?
Sb1 F2 1.837(4) . ?
Sb1 F3 1.851(4) . ?
Sb1 F1 1.863(4) . ?
Sb1 F5 1.868(3) . ?
Sb1 F4 1.871(4) . ?
Sb2 F11 1.834(3) . ?
Sb2 F8 1.842(4) . ?
Sb2 F9 1.847(3) . ?
Sb2 F12 1.857(4) . ?
Sb2 F10 1.863(3) . ?
Sb2 F7 1.864(3) . ?
Sb3 F18 1.763(5) . ?
Sb3 F15 1.812(4) . ?
Sb3 F14 1.827(4) . ?
Sb3 F16 1.828(4) . ?
Sb3 F13 1.830(5) . ?
Sb3 F17 1.898(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C5 123.4(3) . . ?
C1 N1 C2 122.2(3) . . ?
C5 N1 C2 114.4(3) . . ?
C4 N2 C6 122.5(3) . . ?
C4 N2 C3 123.0(3) . . ?
C6 N2 C3 114.4(3) . . ?
N1 C1 C7 121.9(3) . . ?
N1 C1 C13 119.5(3) . . ?
C7 C1 C13 118.5(3) . . ?
N1 C2 C3 110.5(3) . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C2 109.2(3) . . ?
N2 C3 H3A 109.8 . . ?
C2 C3 H3A 109.8 . . ?
N2 C3 H3B 109.8 . . ?
C2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
N2 C4 C19 120.9(3) . . ?
N2 C4 C25 121.6(3) . . ?
C19 C4 C25 117.4(3) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C12 119.7(4) . . ?
C8 C7 C1 121.5(3) . . ?
C12 C7 C1 118.8(4) . . ?
C9 C8 C7 120.1(4) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 120.2(5) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 120.6(5) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 119.9(5) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C7 C12 C11 119.4(5) . . ?
C7 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C18 C13 C14 120.3(4) . . ?
C18 C13 C1 120.1(4) . . ?
C14 C13 C1 119.6(3) . . ?
C15 C14 C13 120.3(4) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 119.5(5) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C17 C16 C15 120.3(4) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.7(4) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C13 C18 C17 118.9(4) . . ?
C13 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C20 C19 C24 120.2(4) . . ?
C20 C19 C4 119.8(4) . . ?
C24 C19 C4 119.7(4) . . ?
C21 C20 C19 120.1(6) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 120.1(6) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.7(5) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C22 C23 C24 120.7(6) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C19 118.1(5) . . ?
C23 C24 H24 121.0 . . ?
C19 C24 H24 121.0 . . ?
C30 C25 C26 119.4(4) . . ?
C30 C25 C4 121.6(3) . . ?
C26 C25 C4 119.0(4) . . ?
C27 C26 C25 120.1(5) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C28 C27 C26 120.2(5) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 120.5(5) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C28 C29 C30 119.7(5) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C29 C30 C25 120.0(4) . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
C31 N3 C33 124.6(4) . . ?
C31 N3 C32 122.2(4) . . ?
C33 N3 C32 113.2(3) . . ?
N3 C31 C34 123.3(4) . . ?
N3 C31 C40 120.4(3) . . ?
C34 C31 C40 116.3(3) . . ?
N3 C32 C32 108.7(4) . 2_576 ?
N3 C32 H32A 109.9 . . ?
C32 C32 H32A 109.9 2_576 . ?
N3 C32 H32B 109.9 . . ?
C32 C32 H32B 109.9 2_576 . ?
H32A C32 H32B 108.3 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C39 C34 C35 119.2(4) . . ?
C39 C34 C31 118.7(3) . . ?
C35 C34 C31 122.0(4) . . ?
C36 C35 C34 119.6(4) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C37 C36 C35 120.8(4) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C36 C37 C38 120.1(4) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C37 C38 C39 119.8(5) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
C38 C39 C34 120.4(4) . . ?
C38 C39 H39 119.8 . . ?
C34 C39 H39 119.8 . . ?
C41 C40 C45 120.1(4) . . ?
C41 C40 C31 121.1(4) . . ?
C45 C40 C31 118.7(4) . . ?
C40 C41 C42 118.7(5) . . ?
C40 C41 H41 120.7 . . ?
C42 C41 H41 120.7 . . ?
C43 C42 C41 121.1(5) . . ?
C43 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C42 C43 C44 120.6(5) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C43 C44 C45 119.7(6) . . ?
C43 C44 H44 120.2 . . ?
C45 C44 H44 120.2 . . ?
C44 C45 C40 119.8(5) . . ?
C44 C45 H45 120.1 . . ?
C40 C45 H45 120.1 . . ?
F6 Sb1 F2 93.1(2) . . ?
F6 Sb1 F3 90.2(2) . . ?
F2 Sb1 F3 90.1(2) . . ?
F6 Sb1 F1 90.5(2) . . ?
F2 Sb1 F1 89.6(2) . . ?
F3 Sb1 F1 179.21(17) . . ?
F6 Sb1 F5 178.77(18) . . ?
F2 Sb1 F5 87.6(2) . . ?
F3 Sb1 F5 90.78(18) . . ?
F1 Sb1 F5 88.49(19) . . ?
F6 Sb1 F4 90.2(2) . . ?
F2 Sb1 F4 176.79(19) . . ?
F3 Sb1 F4 89.8(2) . . ?
F1 Sb1 F4 90.4(2) . . ?
F5 Sb1 F4 89.14(18) . . ?
F11 Sb2 F8 178.5(2) . . ?
F11 Sb2 F9 91.4(2) . . ?
F8 Sb2 F9 90.0(2) . . ?
F11 Sb2 F12 88.1(2) . . ?
F8 Sb2 F12 90.5(3) . . ?
F9 Sb2 F12 178.74(18) . . ?
F11 Sb2 F10 89.1(2) . . ?
F8 Sb2 F10 91.4(2) . . ?
F9 Sb2 F10 89.91(17) . . ?
F12 Sb2 F10 88.94(18) . . ?
F11 Sb2 F7 89.66(18) . . ?
F8 Sb2 F7 89.8(2) . . ?
F9 Sb2 F7 90.93(17) . . ?
F12 Sb2 F7 90.21(18) . . ?
F10 Sb2 F7 178.55(18) . . ?
F18 Sb3 F15 174.9(4) . . ?
F18 Sb3 F14 94.4(4) . . ?
F15 Sb3 F14 88.7(2) . . ?
F18 Sb3 F16 90.1(4) . . ?
F15 Sb3 F16 93.7(3) . . ?
F14 Sb3 F16 93.0(3) . . ?
F18 Sb3 F13 88.6(4) . . ?
F15 Sb3 F13 87.6(3) . . ?
F14 Sb3 F13 86.6(3) . . ?
F16 Sb3 F13 178.6(3) . . ?
F18 Sb3 F17 92.2(4) . . ?
F15 Sb3 F17 84.6(3) . . ?
F14 Sb3 F17 173.3(3) . . ?
F16 Sb3 F17 87.8(3) . . ?
F13 Sb3 F17 92.8(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2B F1 0.97 2.50 3.414(6) 156.2 . yes
C3 H3A F11 0.97 2.51 3.372(6) 148.7 . yes
C5 H5A F18 0.96 2.24 3.184(8) 166.3 1_455 yes
C5 H5B F5 0.96 2.39 3.307(6) 160.9 . yes
C6 H6C F6 0.96 2.32 3.213(6) 153.7 2_667 yes
C32 H32A F14 0.97 2.55 3.256(8) 130.1 1_465 yes
C32 H32A F15 0.97 2.51 3.218(7) 129.7 1_465 yes
C33 H33C F8 0.96 2.57 3.358(8) 139.2 2_666 yes

_refine_diff_density_max         1.172
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.102

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AJ1505
_database_code_depnum_ccdc_archive 'CCDC 2097820'
loop_
_audit_author_name
_audit_author_address
'Anukul Jana'
;Tata Institute of Fundamental Research Hyderabad
India
;
_audit_update_record             
;
2021-07-20 deposited with the CCDC.	2022-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H30 N2'
_chemical_formula_sum            'C30 H30 N2'
_chemical_formula_weight         418.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8709(2)
_cell_length_b                   15.6676(3)
_cell_length_c                   16.3721(4)
_cell_angle_alpha                87.090(2)
_cell_angle_beta                 88.058(2)
_cell_angle_gamma                86.128(2)
_cell_volume                     2266.31(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13082
_cell_measurement_theta_min      2.5730
_cell_measurement_theta_max      29.0000

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.071
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94966
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33503
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.570
_diffrn_reflns_theta_max         28.989
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10375
_reflns_number_gt                8497
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0461P)²+0.5489P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10375
_refine_ls_number_parameters     581
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1024
_refine_ls_wR_factor_gt          0.0977
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.62266(11) 0.76686(6) 0.21686(6) 0.0160(2) Uani 1 1 d . . . . .
N2 N 0.41095(10) 0.72581(6) 0.34968(6) 0.01423(19) Uani 1 1 d . . . . .
C1 C 0.53419(12) 0.68913(7) 0.21294(7) 0.0140(2) Uani 1 1 d . . . . .
C2 C 0.54146(14) 0.83420(7) 0.26296(7) 0.0184(2) Uani 1 1 d . . . . .
H2A H 0.450454 0.855786 0.232986 0.022 Uiso 1 1 calc R U . . .
H2B H 0.607084 0.882464 0.266467 0.022 Uiso 1 1 calc R U . . .
C3 C 0.49396(13) 0.80371(7) 0.34847(7) 0.0169(2) Uani 1 1 d . . . . .
H3A H 0.585061 0.792442 0.381650 0.020 Uiso 1 1 calc R U . . .
H3B H 0.429403 0.849679 0.373995 0.020 Uiso 1 1 calc R U . . .
C4 C 0.49658(12) 0.65446(7) 0.30698(6) 0.0126(2) Uani 1 1 d . . . . .
C5 C 0.67262(14) 0.80526(8) 0.13764(7) 0.0218(3) Uani 1 1 d . . . . .
H5A H 0.585426 0.833847 0.109973 0.033 Uiso 1 1 calc R U . . .
H5B H 0.718989 0.760325 0.103607 0.033 Uiso 1 1 calc R U . . .
H5C H 0.746777 0.847220 0.146482 0.033 Uiso 1 1 calc R U . . .
C6 C 0.36135(13) 0.70585(7) 0.43443(7) 0.0178(2) Uani 1 1 d . . . . .
H6A H 0.449406 0.699442 0.469325 0.027 Uiso 1 1 calc R U . . .
H6B H 0.309835 0.652335 0.437209 0.027 Uiso 1 1 calc R U . . .
H6C H 0.291666 0.752433 0.453409 0.027 Uiso 1 1 calc R U . . .
C7 C 0.39205(13) 0.71620(7) 0.16126(7) 0.0164(2) Uani 1 1 d . . . . .
C8 C 0.25757(13) 0.75488(7) 0.19354(7) 0.0187(2) Uani 1 1 d . . . . .
H8 H 0.245477 0.758750 0.251140 0.022 Uiso 1 1 calc R U . . .
C9 C 0.14118(15) 0.78779(8) 0.14390(8) 0.0251(3) Uani 1 1 d . . . . .
H9 H 0.050014 0.811622 0.168067 0.030 Uiso 1 1 calc R U . . .
C10 C 0.15705(16) 0.78612(9) 0.05979(9) 0.0316(3) Uani 1 1 d . . . . .
H10 H 0.077936 0.808964 0.025813 0.038 Uiso 1 1 calc R U . . .
C11 C 0.29043(17) 0.75051(9) 0.02591(8) 0.0317(3) Uani 1 1 d . . . . .
H11 H 0.303416 0.749672 -0.031885 0.038 Uiso 1 1 calc R U . . .
C12 C 0.40557(15) 0.71597(8) 0.07551(7) 0.0226(3) Uani 1 1 d . . . . .
H12 H 0.495755 0.691582 0.050778 0.027 Uiso 1 1 calc R U . . .
C13 C 0.39608(12) 0.57813(7) 0.30260(6) 0.0135(2) Uani 1 1 d . . . . .
C14 C 0.23823(13) 0.58806(7) 0.30529(7) 0.0166(2) Uani 1 1 d . . . . .
H14 H 0.189957 0.643367 0.311941 0.020 Uiso 1 1 calc R U . . .
C15 C 0.15015(13) 0.51853(8) 0.29844(7) 0.0198(2) Uani 1 1 d . . . . .
H15 H 0.043054 0.526989 0.300147 0.024 Uiso 1 1 calc R U . . .
C16 C 0.21784(14) 0.43721(8) 0.28914(7) 0.0203(2) Uani 1 1 d . . . . .
H16 H 0.157872 0.389988 0.283483 0.024 Uiso 1 1 calc R U . . .
C17 C 0.37410(13) 0.42556(7) 0.28820(7) 0.0181(2) Uani 1 1 d . . . . .
H17 H 0.421645 0.369823 0.283183 0.022 Uiso 1 1 calc R U . . .
C18 C 0.46137(12) 0.49499(7) 0.29456(7) 0.0144(2) Uani 1 1 d . . . . .
H18 H 0.568368 0.485871 0.293433 0.017 Uiso 1 1 calc R U . . .
C19 C 0.63760(12) 0.62716(7) 0.35954(7) 0.0134(2) Uani 1 1 d . . . . .
C20 C 0.62095(13) 0.56772(7) 0.42603(7) 0.0159(2) Uani 1 1 d . . . . .
H20 H 0.530485 0.538523 0.431949 0.019 Uiso 1 1 calc R U . . .
C21 C 0.73233(13) 0.55021(7) 0.48339(7) 0.0184(2) Uani 1 1 d . . . . .
H21 H 0.716806 0.509728 0.527547 0.022 Uiso 1 1 calc R U . . .
C22 C 0.86583(13) 0.59147(7) 0.47652(7) 0.0191(2) Uani 1 1 d . . . . .
H22 H 0.943007 0.579047 0.515017 0.023 Uiso 1 1 calc R U . . .
C23 C 0.88423(13) 0.65117(7) 0.41235(7) 0.0178(2) Uani 1 1 d . . . . .
H23 H 0.974896 0.680243 0.407138 0.021 Uiso 1 1 calc R U . . .
C24 C 0.77217(13) 0.66944(7) 0.35521(7) 0.0158(2) Uani 1 1 d . . . . .
H24 H 0.787328 0.711478 0.312369 0.019 Uiso 1 1 calc R U . . .
C25 C 0.63237(13) 0.61760(7) 0.17085(7) 0.0159(2) Uani 1 1 d . . . . .
C26 C 0.78977(14) 0.61381(8) 0.17062(7) 0.0205(3) Uani 1 1 d . . . . .
H26 H 0.839091 0.656961 0.196027 0.025 Uiso 1 1 calc R U . . .
C27 C 0.87618(15) 0.54791(9) 0.13381(8) 0.0282(3) Uani 1 1 d . . . . .
H27 H 0.983339 0.546329 0.134862 0.034 Uiso 1 1 calc R U . . .
C28 C 0.80697(17) 0.48476(8) 0.09574(8) 0.0297(3) Uani 1 1 d . . . . .
H28 H 0.865923 0.439831 0.070679 0.036 Uiso 1 1 calc R U . . .
C29 C 0.65079(16) 0.48790(8) 0.09464(8) 0.0261(3) Uani 1 1 d . . . . .
H29 H 0.602261 0.445245 0.068058 0.031 Uiso 1 1 calc R U . . .
C30 C 0.56455(15) 0.55293(7) 0.13212(7) 0.0198(2) Uani 1 1 d . . . . .
H30 H 0.457423 0.553625 0.131504 0.024 Uiso 1 1 calc R U . . .
N3 N 0.22332(10) 0.04169(6) 0.16715(6) 0.01440(19) Uani 1 1 d . . . . .
N4 N -0.09535(10) 0.09297(6) 0.17596(6) 0.0163(2) Uani 1 1 d . . . . .
C31 C 0.17282(12) 0.11633(7) 0.21750(6) 0.0121(2) Uani 1 1 d . . . . .
C32 C 0.12500(13) 0.03122(7) 0.09880(7) 0.0176(2) Uani 1 1 d . . . . .
H32A H 0.162222 -0.020113 0.069401 0.021 Uiso 1 1 calc R U . . .
H32B H 0.129462 0.081603 0.059990 0.021 Uiso 1 1 calc R U . . .
C33 C -0.03652(13) 0.02181(8) 0.12731(7) 0.0194(2) Uani 1 1 d . . . . .
H33A H -0.100047 0.018803 0.079108 0.023 Uiso 1 1 calc R U . . .
H33B H -0.042796 -0.032502 0.160521 0.023 Uiso 1 1 calc R U . . .
C34 C -0.00271(12) 0.10558(7) 0.24884(6) 0.0128(2) Uani 1 1 d . . . . .
C35 C 0.37849(13) 0.04280(8) 0.13347(7) 0.0195(2) Uani 1 1 d . . . . .
H35A H 0.409047 -0.012920 0.111349 0.029 Uiso 1 1 calc R U . . .
H35B H 0.446665 0.054412 0.176854 0.029 Uiso 1 1 calc R U . . .
H35C H 0.383464 0.087664 0.089700 0.029 Uiso 1 1 calc R U . . .
C36 C -0.25525(13) 0.08049(8) 0.19568(8) 0.0230(3) Uani 1 1 d . . . . .
H36A H -0.313064 0.087881 0.145569 0.035 Uiso 1 1 calc R U . . .
H36B H -0.294304 0.122656 0.234652 0.035 Uiso 1 1 calc R U . . .
H36C H -0.265147 0.022604 0.219989 0.035 Uiso 1 1 calc R U . . .
C37 C -0.06382(12) 0.19025(7) 0.28664(7) 0.0146(2) Uani 1 1 d . . . . .
C38 C -0.14852(13) 0.25400(8) 0.24219(7) 0.0193(2) Uani 1 1 d . . . . .
H38 H -0.170696 0.245164 0.187009 0.023 Uiso 1 1 calc R U . . .
C39 C -0.20105(14) 0.32997(8) 0.27675(8) 0.0250(3) Uani 1 1 d . . . . .
H39 H -0.257921 0.372254 0.244928 0.030 Uiso 1 1 calc R U . . .
C40 C -0.17135(15) 0.34466(8) 0.35709(8) 0.0261(3) Uani 1 1 d . . . . .
H40 H -0.206565 0.396776 0.380649 0.031 Uiso 1 1 calc R U . . .
C41 C -0.08912(14) 0.28171(8) 0.40249(8) 0.0222(3) Uani 1 1 d . . . . .
H41 H -0.068409 0.290652 0.457849 0.027 Uiso 1 1 calc R U . . .
C42 C -0.03676(13) 0.20586(7) 0.36803(7) 0.0174(2) Uani 1 1 d . . . . .
H42 H 0.018773 0.163511 0.400446 0.021 Uiso 1 1 calc R U . . .
C43 C -0.02154(12) 0.02817(7) 0.31148(7) 0.0144(2) Uani 1 1 d . . . . .
C44 C -0.13614(13) 0.03228(8) 0.37244(7) 0.0187(2) Uani 1 1 d . . . . .
H44 H -0.196227 0.084338 0.377792 0.022 Uiso 1 1 calc R U . . .
C45 C -0.16479(14) -0.03743(8) 0.42538(7) 0.0214(3) Uani 1 1 d . . . . .
H45 H -0.241163 -0.031655 0.467197 0.026 Uiso 1 1 calc R U . . .
C46 C -0.08301(14) -0.11506(8) 0.41765(7) 0.0219(3) Uani 1 1 d . . . . .
H46 H -0.102190 -0.162721 0.453807 0.026 Uiso 1 1 calc R U . . .
C47 C 0.02751(14) -0.12186(7) 0.35602(7) 0.0211(3) Uani 1 1 d . . . . .
H47 H 0.083354 -0.175082 0.349326 0.025 Uiso 1 1 calc R U . . .
C48 C 0.05784(13) -0.05185(7) 0.30382(7) 0.0172(2) Uani 1 1 d . . . . .
H48 H 0.134038 -0.058302 0.261995 0.021 Uiso 1 1 calc R U . . .
C49 C 0.27149(12) 0.11477(7) 0.29385(6) 0.0129(2) Uani 1 1 d . . . . .
C50 C 0.28538(12) 0.18955(7) 0.33545(7) 0.0155(2) Uani 1 1 d . . . . .
H50 H 0.229650 0.240687 0.317804 0.019 Uiso 1 1 calc R U . . .
C51 C 0.37859(13) 0.19105(8) 0.40193(7) 0.0196(2) Uani 1 1 d . . . . .
H51 H 0.384511 0.242491 0.429641 0.024 Uiso 1 1 calc R U . . .
C52 C 0.46277(13) 0.11750(8) 0.42772(7) 0.0204(3) Uani 1 1 d . . . . .
H52 H 0.528630 0.118435 0.472187 0.024 Uiso 1 1 calc R U . . .
C53 C 0.44968(13) 0.04260(8) 0.38786(7) 0.0194(2) Uani 1 1 d . . . . .
H53 H 0.506144 -0.008261 0.405566 0.023 Uiso 1 1 calc R U . . .
C54 C 0.35476(12) 0.04112(7) 0.32220(7) 0.0161(2) Uani 1 1 d . . . . .
H54 H 0.346421 -0.011080 0.296108 0.019 Uiso 1 1 calc R U . . .
C55 C 0.19815(12) 0.19968(7) 0.16439(7) 0.0137(2) Uani 1 1 d . . . . .
C56 C 0.09597(13) 0.23472(7) 0.10670(7) 0.0165(2) Uani 1 1 d . . . . .
H56 H 0.002241 0.209633 0.102175 0.020 Uiso 1 1 calc R U . . .
C57 C 0.12801(14) 0.30545(8) 0.05568(7) 0.0210(3) Uani 1 1 d . . . . .
H57 H 0.055823 0.328061 0.017386 0.025 Uiso 1 1 calc R U . . .
C58 C 0.26370(15) 0.34307(8) 0.06019(8) 0.0245(3) Uani 1 1 d . . . . .
H58 H 0.283919 0.392685 0.026910 0.029 Uiso 1 1 calc R U . . .
C59 C 0.36973(15) 0.30701(8) 0.11420(8) 0.0240(3) Uani 1 1 d . . . . .
H59 H 0.464933 0.330967 0.116704 0.029 Uiso 1 1 calc R U . . .
C60 C 0.33808(13) 0.23629(7) 0.16459(7) 0.0186(2) Uani 1 1 d . . . . .
H60 H 0.413331 0.211919 0.200298 0.022 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.4639(14) . ?
N1 C5 1.4692(15) . ?
N1 C1 1.4980(14) . ?
N2 C6 1.4662(14) . ?
N2 C3 1.4663(14) . ?
N2 C4 1.4981(13) . ?
C1 C25 1.5477(15) . ?
C1 C7 1.5650(15) . ?
C1 C4 1.6375(15) . ?
C2 C3 1.5116(16) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C13 1.5451(15) . ?
C4 C19 1.5658(15) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.4007(16) . ?
C7 C12 1.4052(16) . ?
C8 C9 1.3910(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.3900(18) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.3979(16) . ?
C13 C18 1.3999(15) . ?
C14 C15 1.3940(16) . ?
C14 H14 0.9500 . ?
C15 C16 1.3845(17) . ?
C15 H15 0.9500 . ?
C16 C17 1.3856(17) . ?
C16 H16 0.9500 . ?
C17 C18 1.3871(16) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.4018(15) . ?
C19 C20 1.4068(16) . ?
C20 C21 1.3905(16) . ?
C20 H20 0.9500 . ?
C21 C22 1.3856(17) . ?
C21 H21 0.9500 . ?
C22 C23 1.3838(17) . ?
C22 H22 0.9500 . ?
C23 C24 1.3938(16) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.3934(17) . ?
C25 C30 1.4014(16) . ?
C26 C27 1.3934(17) . ?
C26 H26 0.9500 . ?
C27 C28 1.384(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.384(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.3879(17) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
N3 C32 1.4642(14) . ?
N3 C35 1.4663(14) . ?
N3 C31 1.4999(14) . ?
N4 C33 1.4607(15) . ?
N4 C36 1.4678(15) . ?
N4 C34 1.5001(14) . ?
C31 C49 1.5482(15) . ?
C31 C55 1.5568(15) . ?
C31 C34 1.6397(15) . ?
C32 C33 1.5063(16) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C37 1.5492(15) . ?
C34 C43 1.5621(15) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.3977(16) . ?
C37 C42 1.3985(16) . ?
C38 C39 1.3892(17) . ?
C38 H38 0.9500 . ?
C39 C40 1.3838(19) . ?
C39 H39 0.9500 . ?
C40 C41 1.3865(18) . ?
C40 H40 0.9500 . ?
C41 C42 1.3864(17) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.4010(16) . ?
C43 C48 1.4051(16) . ?
C44 C45 1.3911(17) . ?
C44 H44 0.9500 . ?
C45 C46 1.3826(17) . ?
C45 H45 0.9500 . ?
C46 C47 1.3858(18) . ?
C46 H46 0.9500 . ?
C47 C48 1.3910(16) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C54 1.3951(16) . ?
C49 C50 1.3993(15) . ?
C50 C51 1.3911(16) . ?
C50 H50 0.9500 . ?
C51 C52 1.3856(17) . ?
C51 H51 0.9500 . ?
C52 C53 1.3848(17) . ?
C52 H52 0.9500 . ?
C53 C54 1.3899(16) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.3975(16) . ?
C55 C60 1.4023(16) . ?
C56 C57 1.3926(16) . ?
C56 H56 0.9500 . ?
C57 C58 1.3813(18) . ?
C57 H57 0.9500 . ?
C58 C59 1.3855(19) . ?
C58 H58 0.9500 . ?
C59 C60 1.3859(17) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C5 108.00(9) . . ?
C2 N1 C1 112.34(9) . . ?
C5 N1 C1 115.68(9) . . ?
C6 N2 C3 107.99(9) . . ?
C6 N2 C4 115.89(9) . . ?
C3 N2 C4 112.60(8) . . ?
N1 C1 C25 109.56(9) . . ?
N1 C1 C7 106.98(8) . . ?
C25 C1 C7 110.10(9) . . ?
N1 C1 C4 107.73(8) . . ?
C25 C1 C4 107.57(8) . . ?
C7 C1 C4 114.81(9) . . ?
N1 C2 C3 112.90(9) . . ?
N1 C2 H2A 109.0 . . ?
C3 C2 H2A 109.0 . . ?
N1 C2 H2B 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N2 C3 C2 112.76(9) . . ?
N2 C3 H3A 109.0 . . ?
C2 C3 H3A 109.0 . . ?
N2 C3 H3B 109.0 . . ?
C2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N2 C4 C13 109.74(8) . . ?
N2 C4 C19 106.58(8) . . ?
C13 C4 C19 109.82(8) . . ?
N2 C4 C1 107.71(8) . . ?
C13 C4 C1 107.46(8) . . ?
C19 C4 C1 115.45(9) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C12 116.12(10) . . ?
C8 C7 C1 123.98(10) . . ?
C12 C7 C1 118.98(10) . . ?
C9 C8 C7 122.06(11) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C10 C9 C8 120.55(12) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 118.75(12) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C10 C11 C12 120.75(12) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C7 121.73(12) . . ?
C11 C12 H12 119.1 . . ?
C7 C12 H12 119.1 . . ?
C14 C13 C18 116.95(10) . . ?
C14 C13 C4 122.54(10) . . ?
C18 C13 C4 120.51(10) . . ?
C15 C14 C13 121.40(10) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C16 C15 C14 120.39(11) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 119.19(10) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C16 C17 C18 120.24(10) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C13 121.80(10) . . ?
C17 C18 H18 119.1 . . ?
C13 C18 H18 119.1 . . ?
C24 C19 C20 116.10(10) . . ?
C24 C19 C4 124.17(10) . . ?
C20 C19 C4 118.57(10) . . ?
C21 C20 C19 122.28(10) . . ?
C21 C20 H20 118.9 . . ?
C19 C20 H20 118.9 . . ?
C22 C21 C20 120.39(11) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 118.51(11) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C22 C23 C24 121.21(11) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C23 C24 C19 121.48(10) . . ?
C23 C24 H24 119.3 . . ?
C19 C24 H24 119.3 . . ?
C26 C25 C30 117.39(11) . . ?
C26 C25 C1 122.09(10) . . ?
C30 C25 C1 120.51(10) . . ?
C25 C26 C27 121.24(12) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C28 C27 C26 120.46(13) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C29 C28 C27 119.15(12) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C28 C29 C30 120.46(12) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C25 121.30(12) . . ?
C29 C30 H30 119.3 . . ?
C25 C30 H30 119.3 . . ?
C32 N3 C35 107.20(9) . . ?
C32 N3 C31 113.29(8) . . ?
C35 N3 C31 114.95(8) . . ?
C33 N4 C36 107.53(9) . . ?
C33 N4 C34 113.49(8) . . ?
C36 N4 C34 114.29(9) . . ?
N3 C31 C49 109.06(8) . . ?
N3 C31 C55 107.71(8) . . ?
C49 C31 C55 108.83(8) . . ?
N3 C31 C34 108.44(8) . . ?
C49 C31 C34 108.06(8) . . ?
C55 C31 C34 114.65(8) . . ?
N3 C32 C33 111.86(9) . . ?
N3 C32 H32A 109.2 . . ?
C33 C32 H32A 109.2 . . ?
N3 C32 H32B 109.2 . . ?
C33 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
N4 C33 C32 112.05(9) . . ?
N4 C33 H33A 109.2 . . ?
C32 C33 H33A 109.2 . . ?
N4 C33 H33B 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
N4 C34 C37 107.61(8) . . ?
N4 C34 C43 108.30(8) . . ?
C37 C34 C43 110.46(9) . . ?
N4 C34 C31 108.60(8) . . ?
C37 C34 C31 108.17(8) . . ?
C43 C34 C31 113.53(8) . . ?
N3 C35 H35A 109.5 . . ?
N3 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N3 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N4 C36 H36A 109.5 . . ?
N4 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N4 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C42 116.86(10) . . ?
C38 C37 C34 122.34(10) . . ?
C42 C37 C34 120.80(10) . . ?
C39 C38 C37 121.59(11) . . ?
C39 C38 H38 119.2 . . ?
C37 C38 H38 119.2 . . ?
C40 C39 C38 120.64(12) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C39 C40 C41 118.61(11) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 H40 120.7 . . ?
C42 C41 C40 120.76(12) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C41 C42 C37 121.52(11) . . ?
C41 C42 H42 119.2 . . ?
C37 C42 H42 119.2 . . ?
C44 C43 C48 116.17(10) . . ?
C44 C43 C34 120.14(10) . . ?
C48 C43 C34 123.10(10) . . ?
C45 C44 C43 122.11(11) . . ?
C45 C44 H44 118.9 . . ?
C43 C44 H44 118.9 . . ?
C46 C45 C44 120.55(11) . . ?
C46 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?
C45 C46 C47 118.59(11) . . ?
C45 C46 H46 120.7 . . ?
C47 C46 H46 120.7 . . ?
C46 C47 C48 120.93(11) . . ?
C46 C47 H47 119.5 . . ?
C48 C47 H47 119.5 . . ?
C47 C48 C43 121.58(11) . . ?
C47 C48 H48 119.2 . . ?
C43 C48 H48 119.2 . . ?
C54 C49 C50 117.10(10) . . ?
C54 C49 C31 122.38(10) . . ?
C50 C49 C31 120.47(9) . . ?
C51 C50 C49 121.80(10) . . ?
C51 C50 H50 119.1 . . ?
C49 C50 H50 119.1 . . ?
C52 C51 C50 119.97(11) . . ?
C52 C51 H51 120.0 . . ?
C50 C51 H51 120.0 . . ?
C53 C52 C51 119.15(11) . . ?
C53 C52 H52 120.4 . . ?
C51 C52 H52 120.4 . . ?
C52 C53 C54 120.65(11) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 H53 119.7 . . ?
C53 C54 C49 121.30(11) . . ?
C53 C54 H54 119.3 . . ?
C49 C54 H54 119.3 . . ?
C56 C55 C60 116.35(10) . . ?
C56 C55 C31 123.34(10) . . ?
C60 C55 C31 119.70(10) . . ?
C57 C56 C55 121.69(11) . . ?
C57 C56 H56 119.2 . . ?
C55 C56 H56 119.2 . . ?
C58 C57 C56 120.66(11) . . ?
C58 C57 H57 119.7 . . ?
C56 C57 H57 119.7 . . ?
C57 C58 C59 118.69(11) . . ?
C57 C58 H58 120.7 . . ?
C59 C58 H58 120.7 . . ?
C58 C59 C60 120.56(11) . . ?
C58 C59 H59 119.7 . . ?
C60 C59 H59 119.7 . . ?
C59 C60 C55 121.88(11) . . ?
C59 C60 H60 119.1 . . ?
C55 C60 H60 119.1 . . ?

_refine_diff_density_max         0.312
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.042

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AJ2019
_database_code_depnum_ccdc_archive 'CCDC 2117405'
loop_
_audit_author_name
_audit_author_address
'Anukul Jana'
;Tata Institute of Fundamental Research Hyderabad
India
;
_audit_update_record             
;
2021-10-23 deposited with the CCDC.	2022-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H30 N2 O2'
_chemical_formula_sum            'C30 H30 N2 O2'
_chemical_formula_weight         450.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'I a'
_space_group_name_Hall           'I -2ya'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z'
'x+1/2, y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'

_cell_length_a                   17.0368(6)
_cell_length_b                   17.3714(5)
_cell_length_c                   17.3317(7)
_cell_angle_alpha                90
_cell_angle_beta                 104.214(4)
_cell_angle_gamma                90
_cell_volume                     4972.3(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    12193
_cell_measurement_theta_min      2.8320
_cell_measurement_theta_max      26.5440

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_F_000             1920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.217
_exptl_absorpt_coefficient_mu    0.075
_shelx_estimated_absorpt_T_min   0.980
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58719
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36487
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.703
_diffrn_reflns_theta_max         28.929
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.749
_diffrn_reflns_point_group_measured_fraction_full 0.885
_reflns_number_total             9847
_reflns_number_gt                7692
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_max     0.589
_reflns_Friedel_fraction_full    0.772

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXT-2016 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0547P)²+0.1283P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2798 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9847
_refine_ls_number_parameters     618
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1054
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.46255(9) 0.42443(8) 0.45359(10) 0.0437(4) Uani 1 1 d . . . . .
O2 O 0.52037(9) 0.37008(9) 0.50091(10) 0.0449(4) Uani 1 1 d . . . . .
N1 N 0.53339(11) 0.51830(11) 0.54980(12) 0.0448(5) Uani 1 1 d . . . . .
N2 N 0.61233(11) 0.41929(11) 0.42556(13) 0.0457(5) Uani 1 1 d . . . . .
C1 C 0.45676(13) 0.48948(12) 0.50633(15) 0.0405(5) Uani 1 1 d . . . . .
C2 C 0.59105(13) 0.54014(13) 0.50379(17) 0.0492(6) Uani 1 1 d . . . . .
H2A H 0.624783 0.581812 0.532419 0.059 Uiso 1 1 calc R U . . .
H2B H 0.560241 0.561424 0.452989 0.059 Uiso 1 1 calc R U . . .
C3 C 0.64760(14) 0.47803(14) 0.48546(17) 0.0503(6) Uani 1 1 d . . . . .
H3A H 0.691296 0.503855 0.467829 0.060 Uiso 1 1 calc R U . . .
H3B H 0.672395 0.451375 0.535322 0.060 Uiso 1 1 calc R U . . .
C4 C 0.57984(13) 0.35243(13) 0.45415(14) 0.0417(5) Uani 1 1 d . . . . .
C5 C 0.40278(13) 0.46798(13) 0.56187(15) 0.0427(5) Uani 1 1 d . . . . .
C6 C 0.38667(16) 0.52276(15) 0.61464(17) 0.0560(7) Uani 1 1 d . . . . .
H6 H 0.411247 0.571487 0.617698 0.067 Uiso 1 1 calc R U . . .
C7 C 0.33520(19) 0.50625(18) 0.66229(18) 0.0646(7) Uani 1 1 d . . . . .
H7 H 0.325654 0.543276 0.698470 0.078 Uiso 1 1 calc R U . . .
C8 C 0.29760(17) 0.43568(18) 0.65718(18) 0.0646(8) Uani 1 1 d . . . . .
H8 H 0.262246 0.424527 0.689657 0.078 Uiso 1 1 calc R U . . .
C9 C 0.31183(17) 0.38190(16) 0.60476(19) 0.0626(7) Uani 1 1 d . . . . .
H9 H 0.285675 0.333900 0.600879 0.075 Uiso 1 1 calc R U . . .
C10 C 0.36441(14) 0.39749(14) 0.55733(16) 0.0501(6) Uani 1 1 d . . . . .
H10 H 0.374094 0.359870 0.521793 0.060 Uiso 1 1 calc R U . . .
C11 C 0.40917(13) 0.54776(13) 0.44613(14) 0.0430(5) Uani 1 1 d . . . . .
C12 C 0.42409(15) 0.62643(14) 0.45592(18) 0.0524(6) Uani 1 1 d . . . . .
H12 H 0.464848 0.644333 0.499101 0.063 Uiso 1 1 calc R U . . .
C13 C 0.37903(17) 0.67839(16) 0.4022(2) 0.0633(7) Uani 1 1 d . . . . .
H13 H 0.390456 0.731261 0.408819 0.076 Uiso 1 1 calc R U . . .
C14 C 0.31864(18) 0.65436(19) 0.34013(19) 0.0668(8) Uani 1 1 d . . . . .
H14 H 0.288700 0.690190 0.303958 0.080 Uiso 1 1 calc R U . . .
C15 C 0.30179(18) 0.5768(2) 0.33082(18) 0.0692(8) Uani 1 1 d . . . . .
H15 H 0.259633 0.559813 0.288424 0.083 Uiso 1 1 calc R U . . .
C16 C 0.34650(16) 0.52348(17) 0.38347(17) 0.0565(6) Uani 1 1 d . . . . .
H16 H 0.334286 0.470770 0.376664 0.068 Uiso 1 1 calc R U . . .
C17 C 0.54344(13) 0.29627(13) 0.38746(15) 0.0436(5) Uani 1 1 d . . . . .
C18 C 0.46738(15) 0.26337(14) 0.37989(17) 0.0518(6) Uani 1 1 d . . . . .
H18 H 0.435307 0.279074 0.414107 0.062 Uiso 1 1 calc R U . . .
C19 C 0.43834(19) 0.20785(15) 0.32266(19) 0.0646(8) Uani 1 1 d . . . . .
H19 H 0.386890 0.186172 0.318391 0.077 Uiso 1 1 calc R U . . .
C20 C 0.4844(2) 0.18424(15) 0.27200(18) 0.0658(8) Uani 1 1 d . . . . .
H20 H 0.464820 0.146171 0.233552 0.079 Uiso 1 1 calc R U . . .
C21 C 0.55963(19) 0.21678(17) 0.27795(18) 0.0644(8) Uani 1 1 d . . . . .
H21 H 0.590848 0.201479 0.242800 0.077 Uiso 1 1 calc R U . . .
C22 C 0.58921(16) 0.27179(15) 0.33540(17) 0.0549(6) Uani 1 1 d . . . . .
H22 H 0.640829 0.292983 0.339461 0.066 Uiso 1 1 calc R U . . .
C23 C 0.64432(14) 0.30815(13) 0.51590(15) 0.0441(5) Uani 1 1 d . . . . .
C24 C 0.62210(18) 0.25889(15) 0.57012(18) 0.0576(7) Uani 1 1 d . . . . .
H24 H 0.567551 0.255454 0.572045 0.069 Uiso 1 1 calc R U . . .
C25 C 0.6802(2) 0.21480(18) 0.6214(2) 0.0722(8) Uani 1 1 d . . . . .
H25 H 0.664806 0.181553 0.657863 0.087 Uiso 1 1 calc R U . . .
C26 C 0.7602(2) 0.2194(2) 0.6193(2) 0.0761(9) Uani 1 1 d . . . . .
H26 H 0.799401 0.189511 0.654243 0.091 Uiso 1 1 calc R U . . .
C27 C 0.78257(18) 0.26822(19) 0.5654(2) 0.0704(8) Uani 1 1 d . . . . .
H27 H 0.837237 0.271607 0.563914 0.084 Uiso 1 1 calc R U . . .
C28 C 0.72538(16) 0.31185(16) 0.51413(18) 0.0588(7) Uani 1 1 d . . . . .
H28 H 0.741235 0.344537 0.477458 0.071 Uiso 1 1 calc R U . . .
C29 C 0.57165(16) 0.48659(16) 0.62789(17) 0.0570(7) Uani 1 1 d . . . . .
H29A H 0.532294 0.484039 0.659856 0.086 Uiso 1 1 calc R U . . .
H29B H 0.616374 0.519367 0.654077 0.086 Uiso 1 1 calc R U . . .
H29C H 0.591721 0.435290 0.621676 0.086 Uiso 1 1 calc R U . . .
O3 O 0.52012(9) 0.86828(9) 0.49578(10) 0.0471(4) Uani 1 1 d . . . . .
O4 O 0.48267(9) 0.91910(9) 0.54416(11) 0.0471(4) Uani 1 1 d . . . . .
N3 N 0.64629(12) 0.91757(12) 0.57653(15) 0.0544(5) Uani 1 1 d . . . . .
N4 N 0.50414(12) 1.01947(11) 0.45382(13) 0.0493(5) Uani 1 1 d . . . . .
C30 C 0.57359(16) 0.45179(16) 0.34818(18) 0.0569(6) Uani 1 1 d . . . . .
H30A H 0.559249 0.410690 0.309381 0.085 Uiso 1 1 calc R U . . .
H30B H 0.610634 0.487026 0.331849 0.085 Uiso 1 1 calc R U . . .
H30C H 0.525060 0.479309 0.351738 0.085 Uiso 1 1 calc R U . . .
C31 C 0.60098(13) 0.85055(13) 0.54580(16) 0.0471(6) Uani 1 1 d . . . . .
C32 C 0.65067(15) 0.97781(15) 0.5179(2) 0.0600(7) Uani 1 1 d . . . . .
H32A H 0.649851 0.952385 0.467207 0.072 Uiso 1 1 calc R U . . .
H32B H 0.703234 1.003522 0.535468 0.072 Uiso 1 1 calc R U . . .
C33 C 0.58530(15) 1.03969(14) 0.5019(2) 0.0568(7) Uani 1 1 d . . . . .
H33A H 0.579387 1.058481 0.553499 0.068 Uiso 1 1 calc R U . . .
H33B H 0.605188 1.082863 0.475639 0.068 Uiso 1 1 calc R U . . .
C34 C 0.44936(13) 0.98643(12) 0.49537(15) 0.0434(5) Uani 1 1 d . . . . .
C35 C 0.59434(15) 0.79413(14) 0.61161(15) 0.0486(6) Uani 1 1 d . . . . .
C36 C 0.52062(17) 0.77027(15) 0.62322(18) 0.0593(7) Uani 1 1 d . . . . .
H36 H 0.472422 0.791057 0.591639 0.071 Uiso 1 1 calc R U . . .
C37 C 0.5170(2) 0.71581(17) 0.6812(2) 0.0723(8) Uani 1 1 d . . . . .
H37 H 0.466644 0.700575 0.689050 0.087 Uiso 1 1 calc R U . . .
C38 C 0.5873(3) 0.68423(18) 0.7270(2) 0.0791(10) Uani 1 1 d . . . . .
H38 H 0.584977 0.646545 0.765254 0.095 Uiso 1 1 calc R U . . .
C39 C 0.6610(2) 0.70807(19) 0.71644(19) 0.0749(9) Uani 1 1 d . . . . .
H39 H 0.709002 0.687559 0.748603 0.090 Uiso 1 1 calc R U . . .
C40 C 0.66474(18) 0.76170(17) 0.65919(18) 0.0635(7) Uani 1 1 d . . . . .
H40 H 0.715437 0.776784 0.651955 0.076 Uiso 1 1 calc R U . . .
C41 C 0.63949(15) 0.80618(13) 0.48749(16) 0.0481(6) Uani 1 1 d . . . . .
C42 C 0.59522(18) 0.75207(15) 0.43657(18) 0.0579(7) Uani 1 1 d . . . . .
H42 H 0.539480 0.746662 0.432672 0.069 Uiso 1 1 calc R U . . .
C43 C 0.6325(2) 0.70574(16) 0.3912(2) 0.0698(8) Uani 1 1 d . . . . .
H43 H 0.602010 0.668708 0.357044 0.084 Uiso 1 1 calc R U . . .
C44 C 0.7137(2) 0.71340(18) 0.3957(2) 0.0738(9) Uani 1 1 d . . . . .
H44 H 0.738663 0.681593 0.364898 0.089 Uiso 1 1 calc R U . . .
C45 C 0.75855(19) 0.76791(19) 0.4456(2) 0.0700(8) Uani 1 1 d . . . . .
H45 H 0.814045 0.773725 0.448496 0.084 Uiso 1 1 calc R U . . .
C46 C 0.72181(16) 0.81365(17) 0.49113(19) 0.0617(7) Uani 1 1 d . . . . .
H46 H 0.752641 0.850547 0.525236 0.074 Uiso 1 1 calc R U . . .
C47 C 0.43231(13) 1.03979(13) 0.55982(15) 0.0454(5) Uani 1 1 d . . . . .
C48 C 0.44118(15) 1.11917(14) 0.55608(18) 0.0547(6) Uani 1 1 d . . . . .
H48 H 0.459264 1.140975 0.513903 0.066 Uiso 1 1 calc R U . . .
C49 C 0.42360(17) 1.16628(17) 0.6139(2) 0.0669(8) Uani 1 1 d . . . . .
H49 H 0.430770 1.219762 0.611047 0.080 Uiso 1 1 calc R U . . .
C50 C 0.39612(19) 1.1364(2) 0.6749(2) 0.0746(9) Uani 1 1 d . . . . .
H50 H 0.384553 1.168905 0.714043 0.090 Uiso 1 1 calc R U . . .
C51 C 0.3853(2) 1.0576(2) 0.6785(2) 0.0727(8) Uani 1 1 d . . . . .
H51 H 0.366086 1.036471 0.720318 0.087 Uiso 1 1 calc R U . . .
C52 C 0.40271(17) 1.00998(16) 0.62129(19) 0.0597(7) Uani 1 1 d . . . . .
H52 H 0.394383 0.956661 0.623973 0.072 Uiso 1 1 calc R U . . .
C53 C 0.36832(14) 0.96611(13) 0.43907(15) 0.0447(5) Uani 1 1 d . . . . .
C54 C 0.32171(16) 1.02364(15) 0.39407(17) 0.0551(6) Uani 1 1 d . . . . .
H54 H 0.341739 1.074240 0.396613 0.066 Uiso 1 1 calc R U . . .
C55 C 0.24623(17) 1.00716(18) 0.34566(18) 0.0612(7) Uani 1 1 d . . . . .
H55 H 0.215668 1.046687 0.315389 0.073 Uiso 1 1 calc R U . . .
C56 C 0.21557(17) 0.93464(19) 0.3412(2) 0.0695(8) Uani 1 1 d . . . . .
H56 H 0.165068 0.923336 0.306679 0.083 Uiso 1 1 calc R U . . .
C57 C 0.2599(2) 0.87791(18) 0.3882(3) 0.0843(11) Uani 1 1 d . . . . .
H57 H 0.238297 0.828057 0.387582 0.101 Uiso 1 1 calc R U . . .
C58 C 0.33534(17) 0.89368(15) 0.4358(2) 0.0674(8) Uani 1 1 d . . . . .
H58 H 0.364983 0.854097 0.466870 0.081 Uiso 1 1 calc R U . . .
C59 C 0.64484(19) 0.94688(18) 0.6550(2) 0.0709(8) Uani 1 1 d . . . . .
H59A H 0.591624 0.967664 0.653372 0.106 Uiso 1 1 calc R U . . .
H59B H 0.685132 0.987134 0.670224 0.106 Uiso 1 1 calc R U . . .
H59C H 0.656808 0.905353 0.693480 0.106 Uiso 1 1 calc R U . . .
C60 C 0.50347(18) 0.99216(16) 0.37420(19) 0.0616(7) Uani 1 1 d . . . . .
H60A H 0.524886 0.940203 0.377410 0.092 Uiso 1 1 calc R U . . .
H60B H 0.536716 1.025732 0.350650 0.092 Uiso 1 1 calc R U . . .
H60C H 0.448376 0.992369 0.341514 0.092 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 O2 1.462(2) . ?
O1 C1 1.472(3) . ?
O2 C4 1.477(3) . ?
N1 C1 1.428(3) . ?
N1 C29 1.458(4) . ?
N1 C2 1.459(3) . ?
N2 C4 1.427(3) . ?
N2 C30 1.455(4) . ?
N2 C3 1.474(3) . ?
C1 C5 1.532(3) . ?
C1 C11 1.535(3) . ?
C2 C3 1.531(3) . ?
C4 C17 1.523(3) . ?
C4 C23 1.538(3) . ?
C5 C10 1.381(3) . ?
C5 C6 1.393(4) . ?
C6 C7 1.374(4) . ?
C7 C8 1.376(4) . ?
C8 C9 1.366(4) . ?
C9 C10 1.383(4) . ?
C11 C16 1.388(4) . ?
C11 C12 1.393(3) . ?
C12 C13 1.386(4) . ?
C13 C14 1.359(4) . ?
C14 C15 1.379(5) . ?
C15 C16 1.389(4) . ?
C17 C18 1.393(3) . ?
C17 C22 1.396(4) . ?
C18 C19 1.385(4) . ?
C19 C20 1.376(4) . ?
C20 C21 1.381(4) . ?
C21 C22 1.383(4) . ?
C23 C28 1.390(3) . ?
C23 C24 1.390(4) . ?
C24 C25 1.388(4) . ?
C25 C26 1.374(5) . ?
C26 C27 1.383(5) . ?
C27 C28 1.375(4) . ?
O3 O4 1.467(2) . ?
O3 C31 1.469(3) . ?
O4 C34 1.473(3) . ?
N3 C31 1.426(3) . ?
N3 C59 1.457(4) . ?
N3 C32 1.473(4) . ?
N4 C34 1.431(3) . ?
N4 C60 1.457(4) . ?
N4 C33 1.471(3) . ?
C31 C35 1.529(4) . ?
C31 C41 1.540(3) . ?
C32 C33 1.524(4) . ?
C34 C53 1.524(3) . ?
C34 C47 1.533(3) . ?
C35 C36 1.384(4) . ?
C35 C40 1.396(4) . ?
C36 C37 1.392(4) . ?
C37 C38 1.378(5) . ?
C38 C39 1.375(5) . ?
C39 C40 1.374(5) . ?
C41 C42 1.380(4) . ?
C41 C46 1.394(4) . ?
C42 C43 1.384(4) . ?
C43 C44 1.372(5) . ?
C44 C45 1.380(5) . ?
C45 C46 1.374(4) . ?
C47 C52 1.386(4) . ?
C47 C48 1.390(4) . ?
C48 C49 1.383(4) . ?
C49 C50 1.359(5) . ?
C50 C51 1.385(5) . ?
C51 C52 1.379(4) . ?
C53 C58 1.373(3) . ?
C53 C54 1.390(4) . ?
C54 C55 1.382(4) . ?
C55 C56 1.359(4) . ?
C56 C57 1.379(5) . ?
C57 C58 1.374(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 O1 C1 106.63(15) . . ?
O1 O2 C4 106.55(15) . . ?
C1 N1 C29 119.97(19) . . ?
C1 N1 C2 116.98(19) . . ?
C29 N1 C2 113.45(19) . . ?
C4 N2 C30 120.6(2) . . ?
C4 N2 C3 116.41(19) . . ?
C30 N2 C3 113.2(2) . . ?
N1 C1 O1 113.87(17) . . ?
N1 C1 C5 111.5(2) . . ?
O1 C1 C5 110.19(17) . . ?
N1 C1 C11 112.91(18) . . ?
O1 C1 C11 100.90(18) . . ?
C5 C1 C11 106.83(17) . . ?
N1 C2 C3 118.2(2) . . ?
N2 C3 C2 117.74(19) . . ?
N2 C4 O2 113.48(17) . . ?
N2 C4 C17 112.2(2) . . ?
O2 C4 C17 110.07(17) . . ?
N2 C4 C23 112.15(18) . . ?
O2 C4 C23 101.02(17) . . ?
C17 C4 C23 107.20(18) . . ?
C10 C5 C6 118.4(2) . . ?
C10 C5 C1 122.0(2) . . ?
C6 C5 C1 119.4(2) . . ?
C7 C6 C5 120.6(2) . . ?
C6 C7 C8 120.2(3) . . ?
C9 C8 C7 119.8(2) . . ?
C8 C9 C10 120.5(2) . . ?
C5 C10 C9 120.4(2) . . ?
C16 C11 C12 118.4(2) . . ?
C16 C11 C1 120.5(2) . . ?
C12 C11 C1 121.0(2) . . ?
C13 C12 C11 120.2(3) . . ?
C14 C13 C12 121.2(3) . . ?
C13 C14 C15 119.2(3) . . ?
C14 C15 C16 120.7(3) . . ?
C11 C16 C15 120.2(3) . . ?
C18 C17 C22 118.0(2) . . ?
C18 C17 C4 122.0(2) . . ?
C22 C17 C4 119.8(2) . . ?
C19 C18 C17 120.9(3) . . ?
C20 C19 C18 120.3(3) . . ?
C19 C20 C21 119.6(3) . . ?
C20 C21 C22 120.3(3) . . ?
C21 C22 C17 120.9(3) . . ?
C28 C23 C24 118.7(2) . . ?
C28 C23 C4 120.3(2) . . ?
C24 C23 C4 120.8(2) . . ?
C25 C24 C23 120.2(3) . . ?
C26 C25 C24 120.5(3) . . ?
C25 C26 C27 119.5(3) . . ?
C28 C27 C26 120.4(3) . . ?
C27 C28 C23 120.7(3) . . ?
O4 O3 C31 105.38(16) . . ?
O3 O4 C34 108.06(16) . . ?
C31 N3 C59 120.1(2) . . ?
C31 N3 C32 115.9(2) . . ?
C59 N3 C32 114.3(2) . . ?
C34 N4 C60 119.5(2) . . ?
C34 N4 C33 116.7(2) . . ?
C60 N4 C33 113.7(2) . . ?
N3 C31 O3 113.11(18) . . ?
N3 C31 C35 112.2(2) . . ?
O3 C31 C35 110.14(18) . . ?
N3 C31 C41 112.02(19) . . ?
O3 C31 C41 101.9(2) . . ?
C35 C31 C41 106.87(18) . . ?
N3 C32 C33 117.9(2) . . ?
N4 C33 C32 118.5(2) . . ?
N4 C34 O4 113.60(17) . . ?
N4 C34 C53 111.8(2) . . ?
O4 C34 C53 110.15(17) . . ?
N4 C34 C47 112.81(18) . . ?
O4 C34 C47 100.19(18) . . ?
C53 C34 C47 107.62(17) . . ?
C36 C35 C40 118.2(3) . . ?
C36 C35 C31 122.5(2) . . ?
C40 C35 C31 119.3(2) . . ?
C35 C36 C37 120.7(3) . . ?
C38 C37 C36 120.0(3) . . ?
C39 C38 C37 119.7(3) . . ?
C40 C39 C38 120.4(3) . . ?
C39 C40 C35 120.9(3) . . ?
C42 C41 C46 118.6(2) . . ?
C42 C41 C31 120.4(2) . . ?
C46 C41 C31 120.6(2) . . ?
C41 C42 C43 120.3(3) . . ?
C44 C43 C42 120.5(3) . . ?
C43 C44 C45 119.8(3) . . ?
C46 C45 C44 119.8(3) . . ?
C45 C46 C41 121.0(3) . . ?
C52 C47 C48 118.1(2) . . ?
C52 C47 C34 120.3(2) . . ?
C48 C47 C34 121.6(2) . . ?
C49 C48 C47 120.5(3) . . ?
C50 C49 C48 121.0(3) . . ?
C49 C50 C51 119.2(3) . . ?
C52 C51 C50 120.4(3) . . ?
C51 C52 C47 120.8(3) . . ?
C58 C53 C54 117.7(2) . . ?
C58 C53 C34 122.4(2) . . ?
C54 C53 C34 119.7(2) . . ?
C55 C54 C53 120.6(2) . . ?
C56 C55 C54 120.9(3) . . ?
C55 C56 C57 118.8(3) . . ?
C58 C57 C56 120.5(3) . . ?
C53 C58 C57 121.3(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 O1 O2 C4 -129.03(16) . . . . ?
C29 N1 C1 O1 -90.1(3) . . . . ?
C2 N1 C1 O1 53.9(3) . . . . ?
C29 N1 C1 C5 35.3(3) . . . . ?
C2 N1 C1 C5 179.34(18) . . . . ?
C29 N1 C1 C11 155.6(2) . . . . ?
C2 N1 C1 C11 -60.4(2) . . . . ?
O2 O1 C1 N1 47.8(2) . . . . ?
O2 O1 C1 C5 -78.26(19) . . . . ?
O2 O1 C1 C11 169.09(14) . . . . ?
C1 N1 C2 C3 -87.8(3) . . . . ?
C29 N1 C2 C3 58.5(3) . . . . ?
C4 N2 C3 C2 -88.3(3) . . . . ?
C30 N2 C3 C2 57.9(3) . . . . ?
N1 C2 C3 N2 73.0(3) . . . . ?
C30 N2 C4 O2 -90.4(3) . . . . ?
C3 N2 C4 O2 53.3(3) . . . . ?
C30 N2 C4 C17 35.2(3) . . . . ?
C3 N2 C4 C17 178.83(18) . . . . ?
C30 N2 C4 C23 155.9(2) . . . . ?
C3 N2 C4 C23 -60.4(2) . . . . ?
O1 O2 C4 N2 49.7(2) . . . . ?
O1 O2 C4 C17 -77.00(19) . . . . ?
O1 O2 C4 C23 169.93(15) . . . . ?
N1 C1 C5 C10 -129.8(2) . . . . ?
O1 C1 C5 C10 -2.4(3) . . . . ?
C11 C1 C5 C10 106.4(2) . . . . ?
N1 C1 C5 C6 55.1(3) . . . . ?
O1 C1 C5 C6 -177.5(2) . . . . ?
C11 C1 C5 C6 -68.7(3) . . . . ?
C10 C5 C6 C7 1.4(4) . . . . ?
C1 C5 C6 C7 176.7(3) . . . . ?
C5 C6 C7 C8 -1.3(5) . . . . ?
C6 C7 C8 C9 0.2(5) . . . . ?
C7 C8 C9 C10 0.7(5) . . . . ?
C6 C5 C10 C9 -0.5(4) . . . . ?
C1 C5 C10 C9 -175.7(2) . . . . ?
C8 C9 C10 C5 -0.5(4) . . . . ?
N1 C1 C11 C16 160.8(2) . . . . ?
O1 C1 C11 C16 38.8(3) . . . . ?
C5 C1 C11 C16 -76.4(3) . . . . ?
N1 C1 C11 C12 -23.5(3) . . . . ?
O1 C1 C11 C12 -145.5(2) . . . . ?
C5 C1 C11 C12 99.4(2) . . . . ?
C16 C11 C12 C13 -2.4(4) . . . . ?
C1 C11 C12 C13 -178.2(2) . . . . ?
C11 C12 C13 C14 1.3(4) . . . . ?
C12 C13 C14 C15 0.3(4) . . . . ?
C13 C14 C15 C16 -0.8(4) . . . . ?
C12 C11 C16 C15 1.9(4) . . . . ?
C1 C11 C16 C15 177.7(2) . . . . ?
C14 C15 C16 C11 -0.3(4) . . . . ?
N2 C4 C17 C18 -132.7(2) . . . . ?
O2 C4 C17 C18 -5.3(3) . . . . ?
C23 C4 C17 C18 103.8(2) . . . . ?
N2 C4 C17 C22 52.3(3) . . . . ?
O2 C4 C17 C22 179.7(2) . . . . ?
C23 C4 C17 C22 -71.2(3) . . . . ?
C22 C17 C18 C19 0.3(4) . . . . ?
C4 C17 C18 C19 -174.8(2) . . . . ?
C17 C18 C19 C20 -0.1(4) . . . . ?
C18 C19 C20 C21 -0.6(4) . . . . ?
C19 C20 C21 C22 1.2(4) . . . . ?
C20 C21 C22 C17 -1.0(4) . . . . ?
C18 C17 C22 C21 0.3(4) . . . . ?
C4 C17 C22 C21 175.4(2) . . . . ?
N2 C4 C23 C28 -27.7(3) . . . . ?
O2 C4 C23 C28 -148.9(2) . . . . ?
C17 C4 C23 C28 95.9(3) . . . . ?
N2 C4 C23 C24 157.6(2) . . . . ?
O2 C4 C23 C24 36.5(3) . . . . ?
C17 C4 C23 C24 -78.8(3) . . . . ?
C28 C23 C24 C25 0.3(4) . . . . ?
C4 C23 C24 C25 175.0(3) . . . . ?
C23 C24 C25 C26 0.1(5) . . . . ?
C24 C25 C26 C27 -0.2(5) . . . . ?
C25 C26 C27 C28 -0.2(5) . . . . ?
C26 C27 C28 C23 0.5(5) . . . . ?
C24 C23 C28 C27 -0.6(4) . . . . ?
C4 C23 C28 C27 -175.4(3) . . . . ?
C31 O3 O4 C34 130.59(17) . . . . ?
C59 N3 C31 O3 93.8(3) . . . . ?
C32 N3 C31 O3 -50.3(3) . . . . ?
C59 N3 C31 C35 -31.6(3) . . . . ?
C32 N3 C31 C35 -175.62(19) . . . . ?
C59 N3 C31 C41 -151.7(2) . . . . ?
C32 N3 C31 C41 64.2(3) . . . . ?
O4 O3 C31 N3 -52.7(2) . . . . ?
O4 O3 C31 C35 73.70(19) . . . . ?
O4 O3 C31 C41 -173.14(15) . . . . ?
C31 N3 C32 C33 90.0(3) . . . . ?
C59 N3 C32 C33 -56.2(3) . . . . ?
C34 N4 C33 C32 86.3(3) . . . . ?
C60 N4 C33 C32 -59.0(3) . . . . ?
N3 C32 C33 N4 -74.9(4) . . . . ?
C60 N4 C34 O4 90.1(3) . . . . ?
C33 N4 C34 O4 -53.1(3) . . . . ?
C60 N4 C34 C53 -35.3(3) . . . . ?
C33 N4 C34 C53 -178.52(18) . . . . ?
C60 N4 C34 C47 -156.8(2) . . . . ?
C33 N4 C34 C47 60.0(3) . . . . ?
O3 O4 C34 N4 -46.6(2) . . . . ?
O3 O4 C34 C53 79.72(19) . . . . ?
O3 O4 C34 C47 -167.11(15) . . . . ?
N3 C31 C35 C36 122.1(3) . . . . ?
O3 C31 C35 C36 -4.8(3) . . . . ?
C41 C31 C35 C36 -114.8(3) . . . . ?
N3 C31 C35 C40 -61.7(3) . . . . ?
O3 C31 C35 C40 171.4(2) . . . . ?
C41 C31 C35 C40 61.5(3) . . . . ?
C40 C35 C36 C37 0.4(4) . . . . ?
C31 C35 C36 C37 176.7(2) . . . . ?
C35 C36 C37 C38 -0.9(5) . . . . ?
C36 C37 C38 C39 1.5(5) . . . . ?
C37 C38 C39 C40 -1.7(5) . . . . ?
C38 C39 C40 C35 1.2(4) . . . . ?
C36 C35 C40 C39 -0.5(4) . . . . ?
C31 C35 C40 C39 -176.9(3) . . . . ?
N3 C31 C41 C42 -163.4(2) . . . . ?
O3 C31 C41 C42 -42.2(3) . . . . ?
C35 C31 C41 C42 73.4(3) . . . . ?
N3 C31 C41 C46 23.7(3) . . . . ?
O3 C31 C41 C46 144.9(2) . . . . ?
C35 C31 C41 C46 -99.5(3) . . . . ?
C46 C41 C42 C43 0.9(4) . . . . ?
C31 C41 C42 C43 -172.1(2) . . . . ?
C41 C42 C43 C44 -0.6(4) . . . . ?
C42 C43 C44 C45 -0.2(5) . . . . ?
C43 C44 C45 C46 0.7(5) . . . . ?
C44 C45 C46 C41 -0.3(5) . . . . ?
C42 C41 C46 C45 -0.5(4) . . . . ?
C31 C41 C46 C45 172.5(3) . . . . ?
N4 C34 C47 C52 -159.6(2) . . . . ?
O4 C34 C47 C52 -38.5(3) . . . . ?
C53 C34 C47 C52 76.6(3) . . . . ?
N4 C34 C47 C48 24.3(3) . . . . ?
O4 C34 C47 C48 145.4(2) . . . . ?
C53 C34 C47 C48 -99.4(2) . . . . ?
C52 C47 C48 C49 2.3(4) . . . . ?
C34 C47 C48 C49 178.5(2) . . . . ?
C47 C48 C49 C50 -1.1(4) . . . . ?
C48 C49 C50 C51 -0.3(5) . . . . ?
C49 C50 C51 C52 0.3(5) . . . . ?
C50 C51 C52 C47 1.0(5) . . . . ?
C48 C47 C52 C51 -2.2(4) . . . . ?
C34 C47 C52 C51 -178.5(3) . . . . ?
N4 C34 C53 C58 125.8(3) . . . . ?
O4 C34 C53 C58 -1.5(3) . . . . ?
C47 C34 C53 C58 -109.8(3) . . . . ?
N4 C34 C53 C54 -60.2(3) . . . . ?
O4 C34 C53 C54 172.5(2) . . . . ?
C47 C34 C53 C54 64.2(3) . . . . ?
C58 C53 C54 C55 -2.4(4) . . . . ?
C34 C53 C54 C55 -176.7(2) . . . . ?
C53 C54 C55 C56 0.4(4) . . . . ?
C54 C55 C56 C57 2.4(5) . . . . ?
C55 C56 C57 C58 -3.0(6) . . . . ?
C54 C53 C58 C57 1.8(5) . . . . ?
C34 C53 C58 C57 175.9(3) . . . . ?
C56 C57 C58 C53 0.9(6) . . . . ?

_refine_diff_density_max         0.124
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.033

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AJ1544
_database_code_depnum_ccdc_archive 'CCDC 2097819'
loop_
_audit_author_name
_audit_author_address
'Anukul Jana'
;Tata Institute of Fundamental Research Hyderabad
India
;
_audit_update_record             
;
2021-07-20 deposited with the CCDC.	2022-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H22 N2, 2(C F3 O3 S)'
_chemical_formula_sum            'C20 H22 F6 N2 O6 S2'
_chemical_formula_weight         564.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.4612(17)
_cell_length_b                   24.723(7)
_cell_length_c                   7.2683(18)
_cell_angle_alpha                90
_cell_angle_beta                 94.82(2)
_cell_angle_gamma                90
_cell_volume                     1156.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3234
_cell_measurement_theta_min      3.1770
_cell_measurement_theta_max      29.0720

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_F_000             580
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.320
_shelx_estimated_absorpt_T_min   0.927
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.51479
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9389
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.931
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2354
_reflns_number_gt                1906
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+0.9859P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2354
_refine_ls_number_parameters     168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1122
_refine_ls_wR_factor_gt          0.1080
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
H1 H 0.681(4) 0.3938(9) 0.506(4) 0.014(6) Uiso 1 1 d . . . . .
C1 C 0.5568(4) 0.38910(9) 0.5714(3) 0.0160(5) Uani 1 1 d . . . . .
C2 C 0.5733(3) 0.48612(9) 0.5736(3) 0.0157(5) Uani 1 1 d . . . . .
H2A H 0.709315 0.479484 0.524345 0.019 Uiso 1 1 calc R U . . .
H2B H 0.596019 0.509836 0.683152 0.019 Uiso 1 1 calc R U . . .
C3 C 0.3067(4) 0.43882(9) 0.7433(3) 0.0197(5) Uani 1 1 d . . . . .
H3A H 0.175584 0.437514 0.665209 0.030 Uiso 1 1 calc R U . . .
H3B H 0.316164 0.473170 0.810841 0.030 Uiso 1 1 calc R U . . .
H3C H 0.311769 0.408741 0.831411 0.030 Uiso 1 1 calc R U . . .
C4 C 0.4955(4) 0.33389(9) 0.6026(3) 0.0165(5) Uani 1 1 d . . . . .
C5 C 0.2981(4) 0.31650(10) 0.6488(3) 0.0194(5) Uani 1 1 d . . . . .
H5 H 0.191488 0.342114 0.664836 0.023 Uiso 1 1 calc R U . . .
C6 C 0.2615(4) 0.26187(10) 0.6703(3) 0.0224(6) Uani 1 1 d . . . . .
H6 H 0.128261 0.250058 0.699732 0.027 Uiso 1 1 calc R U . . .
C7 C 0.4162(4) 0.22409(9) 0.6497(3) 0.0231(6) Uani 1 1 d . . . . .
H7 H 0.389365 0.186755 0.667429 0.028 Uiso 1 1 calc R U . . .
C8 C 0.6103(4) 0.24061(10) 0.6033(3) 0.0225(6) Uani 1 1 d . . . . .
H8 H 0.716304 0.214670 0.589418 0.027 Uiso 1 1 calc R U . . .
C9 C 0.6489(4) 0.29500(9) 0.5772(3) 0.0197(5) Uani 1 1 d . . . . .
H9 H 0.780501 0.306142 0.541661 0.024 Uiso 1 1 calc R U . . .
N1 N 0.4820(3) 0.43438(7) 0.6269(3) 0.0151(4) Uani 1 1 d . . . . .
C10 C 0.8621(4) 0.40781(10) 0.0228(3) 0.0199(5) Uani 1 1 d . . . . .
F1 F 0.8819(2) 0.45526(6) -0.0605(2) 0.0333(4) Uani 1 1 d . . . . .
F2 F 0.6626(2) 0.40216(7) 0.0554(2) 0.0340(4) Uani 1 1 d . . . . .
F3 F 0.9047(2) 0.36946(6) -0.0983(2) 0.0310(4) Uani 1 1 d . . . . .
S1 S 1.03056(9) 0.40196(2) 0.23667(8) 0.01578(18) Uani 1 1 d . . . . .
O1 O 0.9616(3) 0.44551(7) 0.3486(3) 0.0290(5) Uani 1 1 d . . . . .
O2 O 0.9816(3) 0.34864(7) 0.2999(3) 0.0279(4) Uani 1 1 d . . . . .
O3 O 1.2364(2) 0.40844(6) 0.1776(2) 0.0203(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.297(3) . ?
C1 C4 1.444(3) . ?
C1 H1 0.97(3) . ?
C2 N1 1.474(3) . ?
C2 C2 1.530(4) 3_666 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.474(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C9 1.404(3) . ?
C4 C5 1.413(3) . ?
C5 C6 1.382(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 F1 1.331(3) . ?
C10 F2 1.337(3) . ?
C10 F3 1.338(3) . ?
C10 S1 1.827(3) . ?
S1 O2 1.4400(18) . ?
S1 O3 1.4402(18) . ?
S1 O1 1.4423(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C4 130.7(2) . . ?
N1 C1 H1 113.1(14) . . ?
C4 C1 H1 116.0(14) . . ?
N1 C2 C2 109.6(2) . 3_666 ?
N1 C2 H2A 109.8 . . ?
C2 C2 H2A 109.8 3_666 . ?
N1 C2 H2B 109.8 . . ?
C2 C2 H2B 109.8 3_666 . ?
H2A C2 H2B 108.2 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C9 C4 C5 119.0(2) . . ?
C9 C4 C1 114.9(2) . . ?
C5 C4 C1 126.1(2) . . ?
C6 C5 C4 119.4(2) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C7 121.0(2) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C8 120.2(2) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 119.8(2) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C4 120.7(2) . . ?
C8 C9 H9 119.7 . . ?
C4 C9 H9 119.7 . . ?
C1 N1 C2 120.0(2) . . ?
C1 N1 C3 124.6(2) . . ?
C2 N1 C3 115.47(18) . . ?
F1 C10 F2 107.67(19) . . ?
F1 C10 F3 107.0(2) . . ?
F2 C10 F3 107.29(19) . . ?
F1 C10 S1 112.57(16) . . ?
F2 C10 S1 110.78(17) . . ?
F3 C10 S1 111.28(16) . . ?
O2 S1 O3 115.46(11) . . ?
O2 S1 O1 114.63(12) . . ?
O3 S1 O1 114.97(10) . . ?
O2 S1 C10 102.28(11) . . ?
O3 S1 C10 103.68(11) . . ?
O1 S1 C10 103.33(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2A O1 0.99 2.31 3.266(3) 161.5 . yes
C2 H2B O3 0.99 2.47 3.347(3) 147.6 3_766 yes
C3 H3A O1 0.98 2.59 3.487(3) 152.0 1_455 yes
C3 H3C O3 0.98 2.60 3.313(3) 129.4 1_456 yes

_refine_diff_density_max         0.509
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.074

