# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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. 
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data_mo_pd291121_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2190086'
loop_
_audit_author_name
_audit_author_address
'NABANITA ROY'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2023-04-13 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_audit_creation_date             2022-02-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        FmocF-AMN
_chemical_formula_moiety         'C24 H20 N O4, C10 H18 N'
_chemical_formula_sum            'C34 H36 N2 O4'
_chemical_formula_weight         536.65
_chemical_absolute_configuration Fmoc-L-Phenylalanine
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.381(5)
_cell_length_b                   6.665(2)
_cell_length_c                   15.732(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.009(9)
_cell_angle_gamma                90
_cell_volume                     1399.6(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    979
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.60
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.975
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.4689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1710 before and 0.0804 after correction.
The Ratio of minimum to maximum transmission is 0.6280.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             572
_exptl_crystal_preparation       'Nitromethane and ethanol mixture'
_exptl_crystal_recrystallization_method 'slow evaporation in beaker'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1267
_diffrn_reflns_av_unetI/netI     0.2489
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6685
_diffrn_reflns_point_group_measured_fraction_full 0.744
_diffrn_reflns_point_group_measured_fraction_max 0.744
_diffrn_reflns_theta_full        25.015
_diffrn_reflns_theta_max         25.015
_diffrn_reflns_theta_min         2.596
_diffrn_ambient_temperature      144.98
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.391
_reflns_Friedel_fraction_full    0.462
_reflns_Friedel_fraction_max     0.462
_reflns_number_gt                1258
_reflns_number_total             3671
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 
;
 Flack x determined using 249 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -2.2(10)
_refine_ls_extinction_coef       0.054(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         3671
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.2450
_refine_ls_R_factor_gt           0.1004
_refine_ls_restrained_S_all      0.957
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0884P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2717
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
2. Rigid bond restraints
 C30, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Ternary CH refined with riding coordinates:
 C16(H16), C30(H30), C13(H13), C27(H27), C32(H32)
3.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C29(H29A,H29B), C17(H17A,H17B), C26(H26A,H26B), C28(H28A,
 H28B), C33(H33A,H33B), C14(H14A,H14B), C34(H34A,H34B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C19(H19), C9(H9), C20(H20), C5(H5), C2(H2), C10(H10), C4(H4), C8(H8),
 C3(H3), C23(H23), C21(H21), C22(H22), C11(H11)
3.d Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
O4 O 0.5012(7) 0.2043(14) 0.8940(6) 0.074(3) Uani 1 1 d . . . . .
O3 O 0.5127(8) 0.5217(17) 0.8472(6) 0.086(3) Uani 1 1 d . . . . .
N1 N 0.4456(10) 0.4063(17) 0.6880(6) 0.072(3) Uani 1 1 d . . . . .
H1 H 0.482596 0.492008 0.661448 0.087 Uiso 1 1 calc R U . . .
O1 O 0.3274(8) 0.5822(19) 0.6210(7) 0.113(4) Uani 1 1 d . . . . .
N2 N 0.4358(8) 0.8216(19) 0.9394(6) 0.074(3) Uani 1 1 d . . . . .
H2A H 0.459163 0.702007 0.921200 0.089 Uiso 1 1 calc R U . . .
H2B H 0.453081 0.836462 0.996012 0.089 Uiso 1 1 calc R U . . .
H2C H 0.462942 0.923213 0.909988 0.089 Uiso 1 1 calc R U . . .
O2 O 0.2869(9) 0.309(2) 0.6978(8) 0.124(5) Uani 1 1 d . . . . .
C6 C 0.2275(12) 1.000(3) 0.4314(9) 0.073(4) Uani 1 1 d . . . . .
C15 C 0.3477(15) 0.419(3) 0.6735(11) 0.087(5) Uani 1 1 d . . . . .
C24 C 0.5042(10) 0.339(3) 0.8357(9) 0.073(4) Uani 1 1 d . . . . .
C19 C 0.6412(12) -0.091(3) 0.7846(8) 0.075(4) Uani 1 1 d . . . . .
H19 H 0.571967 -0.124149 0.779506 0.091 Uiso 1 1 calc R U . . .
C18 C 0.6738(14) 0.093(3) 0.7571(9) 0.075(4) Uani 1 1 d . . . . .
C25 C 0.3226(12) 0.827(3) 0.9244(8) 0.077(4) Uani 1 1 d . . . . .
C7 C 0.1320(12) 0.899(3) 0.4084(9) 0.077(5) Uani 1 1 d . . . . .
C9 C -0.0291(14) 0.815(4) 0.3394(10) 0.095(6) Uani 1 1 d . . . . .
H9 H -0.084199 0.847282 0.300411 0.114 Uiso 1 1 calc R U . . .
C20 C 0.7107(14) -0.226(3) 0.8197(9) 0.082(5) Uani 1 1 d . . . . .
H20 H 0.689111 -0.355392 0.836077 0.098 Uiso 1 1 calc R U . . .
C1 C 0.2784(12) 0.889(3) 0.4924(10) 0.083(5) Uani 1 1 d . . . . .
C31 C 0.2981(11) 0.851(3) 0.8314(8) 0.091(5) Uani 1 1 d . . . . .
H31A H 0.324373 0.735646 0.799965 0.110 Uiso 1 1 calc R U . . .
H31B H 0.328459 0.975460 0.810605 0.110 Uiso 1 1 calc R U . . .
C29 C 0.2862(13) 1.003(2) 0.9738(10) 0.084(5) Uani 1 1 d . . . . .
H29A H 0.315632 1.128562 0.953183 0.100 Uiso 1 1 calc R U . . .
H29B H 0.307449 0.987215 1.034977 0.100 Uiso 1 1 calc R U . . .
C17 C 0.6038(11) 0.239(2) 0.7126(9) 0.077(4) Uani 1 1 d . . . . .
H17A H 0.596580 0.200546 0.651702 0.092 Uiso 1 1 calc R U . . .
H17B H 0.636188 0.372363 0.715814 0.092 Uiso 1 1 calc R U . . .
C26 C 0.2824(12) 0.636(2) 0.9609(11) 0.087(5) Uani 1 1 d . . . . .
H26A H 0.300995 0.627655 1.022830 0.105 Uiso 1 1 calc R U . . .
H26B H 0.310085 0.517200 0.932805 0.105 Uiso 1 1 calc R U . . .
C16 C 0.4967(12) 0.263(2) 0.7438(8) 0.079(5) Uani 1 1 d . . . . .
H16 H 0.460701 0.131094 0.740257 0.095 Uiso 1 1 calc R U . . .
C30 C 0.1704(15) 1.013(3) 0.9618(11) 0.107(6) Uani 1 1 d . U . . .
H30 H 0.144364 1.130167 0.993239 0.128 Uiso 1 1 calc R U . . .
C5 C 0.2661(14) 1.175(3) 0.4007(9) 0.085(5) Uani 1 1 d . . . . .
H5 H 0.227780 1.256526 0.360995 0.102 Uiso 1 1 calc R U . . .
C2 C 0.3745(13) 0.950(3) 0.5243(10) 0.090(5) Uani 1 1 d . . . . .
H2 H 0.411815 0.870179 0.565423 0.108 Uiso 1 1 calc R U . . .
C10 C -0.0288(13) 0.648(3) 0.3858(11) 0.097(5) Uani 1 1 d . . . . .
H10 H -0.085133 0.560817 0.379042 0.117 Uiso 1 1 calc R U . . .
C4 C 0.3617(15) 1.228(2) 0.4292(10) 0.087(5) Uani 1 1 d . . . . .
H4 H 0.393274 1.338083 0.403408 0.104 Uiso 1 1 calc R U . . .
C8 C 0.0531(13) 0.942(3) 0.3495(9) 0.087(5) Uani 1 1 d . . . . .
H8 H 0.055393 1.059352 0.315579 0.104 Uiso 1 1 calc R U . . .
C3 C 0.4133(13) 1.124(3) 0.4954(11) 0.096(6) Uani 1 1 d . . . . .
H3 H 0.475063 1.174472 0.520195 0.115 Uiso 1 1 calc R U . . .
C12 C 0.1287(12) 0.722(3) 0.4545(10) 0.088(5) Uani 1 1 d . . . . .
C23 C 0.7750(15) 0.145(3) 0.7695(10) 0.098(6) Uani 1 1 d . . . . .
H23 H 0.797493 0.273682 0.753717 0.118 Uiso 1 1 calc R U . . .
C28 C 0.1268(14) 0.818(4) 0.9926(11) 0.120(6) Uani 1 1 d . U . . .
H28A H 0.144488 0.801712 1.054421 0.144 Uiso 1 1 calc R U . . .
H28B H 0.052907 0.821148 0.983458 0.144 Uiso 1 1 calc R U . . .
C13 C 0.2281(14) 0.683(3) 0.5068(13) 0.118(7) Uani 1 1 d . . . . .
H13 H 0.265427 0.581446 0.474601 0.142 Uiso 1 1 calc R U . . .
C21 C 0.8116(14) -0.177(4) 0.8314(10) 0.100(6) Uani 1 1 d . . . . .
H21 H 0.858329 -0.269522 0.857383 0.120 Uiso 1 1 calc R U . . .
C33 C 0.1446(14) 1.034(3) 0.8653(13) 0.126(7) Uani 1 1 d . . . . .
H33A H 0.071010 1.041871 0.853995 0.151 Uiso 1 1 calc R U . . .
H33B H 0.173859 1.160417 0.844781 0.151 Uiso 1 1 calc R U . . .
C27 C 0.1682(14) 0.644(3) 0.9442(12) 0.109(6) Uani 1 1 d . . . . .
H27 H 0.139006 0.516017 0.964856 0.131 Uiso 1 1 calc R U . . .
C22 C 0.8421(14) 0.004(4) 0.8053(12) 0.102(6) Uani 1 1 d . . . . .
H22 H 0.911398 0.036576 0.811589 0.122 Uiso 1 1 calc R U . . .
C11 C 0.0513(14) 0.593(3) 0.4445(9) 0.109(6) Uani 1 1 d . . . . .
H11 H 0.050625 0.471192 0.475615 0.130 Uiso 1 1 calc R U . . .
C32 C 0.1843(15) 0.860(5) 0.8177(10) 0.126(7) Uani 1 1 d . . . . .
H32 H 0.164147 0.873280 0.755503 0.151 Uiso 1 1 calc R U . . .
C14 C 0.2251(14) 0.611(4) 0.5886(13) 0.154(10) Uani 1 1 d . . . . .
H14A H 0.188041 0.482464 0.588570 0.185 Uiso 1 1 calc R U . . .
H14B H 0.191200 0.708481 0.624419 0.185 Uiso 1 1 calc R U . . .
C34 C 0.1429(15) 0.662(4) 0.8524(14) 0.143(9) Uani 1 1 d . . . . .
H34A H 0.069228 0.658522 0.841081 0.171 Uiso 1 1 calc R U . . .
H34B H 0.171521 0.547019 0.822442 0.171 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
O4 C24 1.285(18) . ?
O3 C24 1.24(2) . ?
N1 H1 0.8800 . ?
N1 C15 1.317(18) . ?
N1 C16 1.439(15) . ?
O1 C15 1.381(19) . ?
O1 C14 1.440(19) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N2 C25 1.516(15) . ?
O2 C15 1.18(2) . ?
C6 C7 1.47(2) . ?
C6 C1 1.355(19) . ?
C6 C5 1.38(2) . ?
C24 C16 1.530(18) . ?
C19 H19 0.9500 . ?
C19 C18 1.38(2) . ?
C19 C20 1.382(19) . ?
C18 C17 1.489(19) . ?
C18 C23 1.40(2) . ?
C25 C31 1.485(16) . ?
C25 C29 1.51(2) . ?
C25 C26 1.51(2) . ?
C7 C8 1.385(19) . ?
C7 C12 1.39(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.34(2) . ?
C9 C8 1.39(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.389(19) . ?
C1 C2 1.407(19) . ?
C1 C13 1.55(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.52(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.55(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C16 1.555(18) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.53(2) . ?
C16 H16 1.0000 . ?
C30 H30 1.0000 . ?
C30 C28 1.52(3) . ?
C30 C33 1.54(2) . ?
C5 H5 0.9500 . ?
C5 C4 1.372(19) . ?
C2 H2 0.9500 . ?
C2 C3 1.37(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.41(2) . ?
C4 H4 0.9500 . ?
C4 C3 1.39(2) . ?
C8 H8 0.9500 . ?
C3 H3 0.9500 . ?
C12 C13 1.54(2) . ?
C12 C11 1.35(2) . ?
C23 H23 0.9500 . ?
C23 C22 1.39(2) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C27 1.52(2) . ?
C13 H13 1.0000 . ?
C13 C14 1.38(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.35(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C32 1.50(3) . ?
C27 H27 1.0000 . ?
C27 C34 1.47(2) . ?
C22 H22 0.9500 . ?
C11 H11 0.9500 . ?
C32 H32 1.0000 . ?
C32 C34 1.55(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?

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
C15 N1 H1 117.5 . . ?
C15 N1 C16 125.0(14) . . ?
C16 N1 H1 117.5 . . ?
C15 O1 C14 117.3(15) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C25 N2 H2A 109.5 . . ?
C25 N2 H2B 109.5 . . ?
C25 N2 H2C 109.5 . . ?
C1 C6 C7 108.1(16) . . ?
C1 C6 C5 121.9(16) . . ?
C5 C6 C7 130.0(17) . . ?
N1 C15 O1 107.8(18) . . ?
O2 C15 N1 127.2(17) . . ?
O2 C15 O1 124.9(17) . . ?
O4 C24 C16 116.1(17) . . ?
O3 C24 O4 126.2(14) . . ?
O3 C24 C16 117.7(16) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
C20 C19 C18 119.0(15) . . ?
C19 C18 C17 121.5(16) . . ?
C19 C18 C23 119.9(17) . . ?
C23 C18 C17 118.6(18) . . ?
C31 C25 N2 107.8(12) . . ?
C31 C25 C29 111.6(15) . . ?
C31 C25 C26 113.9(14) . . ?
C29 C25 N2 107.0(12) . . ?
C29 C25 C26 108.8(12) . . ?
C26 C25 N2 107.4(13) . . ?
C8 C7 C6 132.9(17) . . ?
C8 C7 C12 118.3(16) . . ?
C12 C7 C6 108.7(14) . . ?
C10 C9 H9 120.8 . . ?
C10 C9 C8 118.3(17) . . ?
C8 C9 H9 120.8 . . ?
C19 C20 H20 119.3 . . ?
C19 C20 C21 121.4(17) . . ?
C21 C20 H20 119.3 . . ?
C6 C1 C2 119.9(16) . . ?
C6 C1 C13 112.6(15) . . ?
C2 C1 C13 126.6(16) . . ?
C25 C31 H31A 110.3 . . ?
C25 C31 H31B 110.3 . . ?
C25 C31 C32 107.0(13) . . ?
H31A C31 H31B 108.6 . . ?
C32 C31 H31A 110.3 . . ?
C32 C31 H31B 110.3 . . ?
C25 C29 H29A 109.9 . . ?
C25 C29 H29B 109.9 . . ?
C25 C29 C30 109.1(14) . . ?
H29A C29 H29B 108.3 . . ?
C30 C29 H29A 109.9 . . ?
C30 C29 H29B 109.9 . . ?
C18 C17 H17A 107.6 . . ?
C18 C17 H17B 107.6 . . ?
C18 C17 C16 118.8(12) . . ?
H17A C17 H17B 107.0 . . ?
C16 C17 H17A 107.6 . . ?
C16 C17 H17B 107.6 . . ?
C25 C26 H26A 110.4 . . ?
C25 C26 H26B 110.4 . . ?
C25 C26 C27 106.4(14) . . ?
H26A C26 H26B 108.6 . . ?
C27 C26 H26A 110.4 . . ?
C27 C26 H26B 110.4 . . ?
N1 C16 C24 110.7(13) . . ?
N1 C16 C17 106.5(11) . . ?
N1 C16 H16 110.1 . . ?
C24 C16 C17 109.3(11) . . ?
C24 C16 H16 110.1 . . ?
C17 C16 H16 110.1 . . ?
C29 C30 H30 110.8 . . ?
C28 C30 C29 109.1(15) . . ?
C28 C30 H30 110.8 . . ?
C28 C30 C33 109.3(16) . . ?
C33 C30 C29 106.1(15) . . ?
C33 C30 H30 110.8 . . ?
C6 C5 H5 121.1 . . ?
C4 C5 C6 117.9(16) . . ?
C4 C5 H5 121.1 . . ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 119.0(16) . . ?
C3 C2 H2 120.5 . . ?
C9 C10 H10 118.5 . . ?
C9 C10 C11 123.0(17) . . ?
C11 C10 H10 118.5 . . ?
C5 C4 H4 119.4 . . ?
C5 C4 C3 121.2(17) . . ?
C3 C4 H4 119.4 . . ?
C7 C8 C9 120.9(17) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C2 C3 C4 119.6(17) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C7 C12 C13 111.5(16) . . ?
C11 C12 C7 122.3(17) . . ?
C11 C12 C13 125.7(18) . . ?
C18 C23 H23 120.5 . . ?
C22 C23 C18 119.0(19) . . ?
C22 C23 H23 120.5 . . ?
C30 C28 H28A 109.8 . . ?
C30 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?
C27 C28 C30 109.5(14) . . ?
C27 C28 H28A 109.8 . . ?
C27 C28 H28B 109.8 . . ?
C1 C13 H13 106.7 . . ?
C12 C13 C1 98.0(15) . . ?
C12 C13 H13 106.7 . . ?
C14 C13 C1 119.1(19) . . ?
C14 C13 C12 118.7(17) . . ?
C14 C13 H13 106.7 . . ?
C20 C21 H21 120.5 . . ?
C22 C21 C20 118.9(18) . . ?
C22 C21 H21 120.5 . . ?
C30 C33 H33A 109.4 . . ?
C30 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C32 C33 C30 111.0(16) . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
C26 C27 H27 108.9 . . ?
C28 C27 C26 109.5(15) . . ?
C28 C27 H27 108.9 . . ?
C34 C27 C26 109.3(16) . . ?
C34 C27 C28 111.4(18) . . ?
C34 C27 H27 108.9 . . ?
C23 C22 H22 119.1 . . ?
C21 C22 C23 121.7(19) . . ?
C21 C22 H22 119.1 . . ?
C10 C11 H11 121.4 . . ?
C12 C11 C10 117.1(17) . . ?
C12 C11 H11 121.4 . . ?
C31 C32 H32 109.9 . . ?
C31 C32 C34 107.1(19) . . ?
C33 C32 C31 110.3(18) . . ?
C33 C32 H32 109.9 . . ?
C33 C32 C34 109.7(17) . . ?
C34 C32 H32 109.9 . . ?
O1 C14 H14A 110.4 . . ?
O1 C14 H14B 110.4 . . ?
C13 C14 O1 106.7(15) . . ?
C13 C14 H14A 110.4 . . ?
C13 C14 H14B 110.4 . . ?
H14A C14 H14B 108.6 . . ?
C27 C34 C32 110.8(16) . . ?
C27 C34 H34A 109.5 . . ?
C27 C34 H34B 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?

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
O4 C24 C16 N1 147.3(13) . . . . ?
O4 C24 C16 C17 -95.6(15) . . . . ?
O3 C24 C16 N1 -32.9(19) . . . . ?
O3 C24 C16 C17 84.2(16) . . . . ?
N2 C25 C31 C32 -178.8(16) . . . . ?
N2 C25 C29 C30 -179.1(12) . . . . ?
N2 C25 C26 C27 -179.4(12) . . . . ?
C6 C7 C8 C9 178.4(15) . . . . ?
C6 C7 C12 C13 -5.0(18) . . . . ?
C6 C7 C12 C11 -177.5(15) . . . . ?
C6 C1 C2 C3 3(2) . . . . ?
C6 C1 C13 C12 -10.9(19) . . . . ?
C6 C1 C13 C14 -140.1(18) . . . . ?
C6 C5 C4 C3 -8(2) . . . . ?
C15 N1 C16 C24 -85.3(17) . . . . ?
C15 N1 C16 C17 155.9(14) . . . . ?
C15 O1 C14 C13 -143.6(18) . . . . ?
C19 C18 C17 C16 39.2(19) . . . . ?
C19 C18 C23 C22 4(2) . . . . ?
C19 C20 C21 C22 -2(2) . . . . ?
C18 C19 C20 C21 3(2) . . . . ?
C18 C17 C16 N1 -178.1(12) . . . . ?
C18 C17 C16 C24 62.2(19) . . . . ?
C18 C23 C22 C21 -3(3) . . . . ?
C25 C31 C32 C33 60(2) . . . . ?
C25 C31 C32 C34 -59(2) . . . . ?
C25 C29 C30 C28 58.8(18) . . . . ?
C25 C29 C30 C33 -58.8(19) . . . . ?
C25 C26 C27 C28 -63.9(18) . . . . ?
C25 C26 C27 C34 58(2) . . . . ?
C7 C6 C1 C2 178.2(13) . . . . ?
C7 C6 C1 C13 8.8(19) . . . . ?
C7 C6 C5 C4 -175.3(14) . . . . ?
C7 C12 C13 C1 9.2(18) . . . . ?
C7 C12 C13 C14 139(2) . . . . ?
C7 C12 C11 C10 -1(3) . . . . ?
C9 C10 C11 C12 2(3) . . . . ?
C20 C19 C18 C17 175.1(12) . . . . ?
C20 C19 C18 C23 -4(2) . . . . ?
C20 C21 C22 C23 2(3) . . . . ?
C1 C6 C7 C8 -178.3(16) . . . . ?
C1 C6 C7 C12 -2.4(17) . . . . ?
C1 C6 C5 C4 5(2) . . . . ?
C1 C2 C3 C4 -6(2) . . . . ?
C1 C13 C14 O1 -63(2) . . . . ?
C31 C25 C29 C30 63.2(18) . . . . ?
C31 C25 C26 C27 -60.2(18) . . . . ?
C31 C32 C34 C27 63(2) . . . . ?
C29 C25 C31 C32 -62(2) . . . . ?
C29 C25 C26 C27 65.0(16) . . . . ?
C29 C30 C28 C27 -57.5(19) . . . . ?
C29 C30 C33 C32 59(2) . . . . ?
C17 C18 C23 C22 -175.3(14) . . . . ?
C26 C25 C31 C32 62(2) . . . . ?
C26 C25 C29 C30 -63.3(16) . . . . ?
C26 C27 C34 C32 -63(2) . . . . ?
C16 N1 C15 O1 176.3(11) . . . . ?
C16 N1 C15 O2 -6(3) . . . . ?
C30 C28 C27 C26 61.2(19) . . . . ?
C30 C28 C27 C34 -60(2) . . . . ?
C30 C33 C32 C31 -61(2) . . . . ?
C30 C33 C32 C34 56(2) . . . . ?
C5 C6 C7 C8 2(3) . . . . ?
C5 C6 C7 C12 177.6(15) . . . . ?
C5 C6 C1 C2 -2(2) . . . . ?
C5 C6 C1 C13 -171.2(15) . . . . ?
C5 C4 C3 C2 9(2) . . . . ?
C2 C1 C13 C12 -179.4(15) . . . . ?
C2 C1 C13 C14 51(3) . . . . ?
C10 C9 C8 C7 -2(2) . . . . ?
C8 C7 C12 C13 171.6(14) . . . . ?
C8 C7 C12 C11 -1(2) . . . . ?
C8 C9 C10 C11 0(3) . . . . ?
C12 C7 C8 C9 3(2) . . . . ?
C12 C13 C14 O1 178.1(16) . . . . ?
C23 C18 C17 C16 -141.9(14) . . . . ?
C28 C30 C33 C32 -58(2) . . . . ?
C28 C27 C34 C32 59(2) . . . . ?
C13 C1 C2 C3 170.3(16) . . . . ?
C13 C12 C11 C10 -172.7(16) . . . . ?
C33 C30 C28 C27 58(2) . . . . ?
C33 C32 C34 C27 -57(2) . . . . ?
C11 C12 C13 C1 -178.6(17) . . . . ?
C11 C12 C13 C14 -49(3) . . . . ?
C14 O1 C15 N1 172.9(15) . . . . ?
C14 O1 C15 O2 -5(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id PD291121
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT026_mo_pd291121_0m_a    
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        34% Check 
RESPONSE: The crystal was poorly diffracting at higher Bragg angles.
The situation did not improve even after recrystallisation and fresh
data collection.
;
_vrf_PLAT340_mo_pd291121_0m_a    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0267 Ang.  
RESPONSE: The crystal was poorly diffracting at higher Bragg angles.
The situation did not improve even after recrystallisation and fresh
data collection.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_mo_pd030322_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2190087'
loop_
_audit_author_name
_audit_author_address
'NABANITA ROY'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2023-04-13 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_audit_creation_date             2022-05-05
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        NbocF-MAF
_chemical_formula_moiety         'C7 H11 N2 O2 S, C14 H18 N O4'
_chemical_formula_sum            'C21 H29 N3 O6 S'
_chemical_formula_weight         451.53
_chemical_absolute_configuration Nboc-L-Phenylalanine
_chemical_melting_point          ?
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.809(4)
_cell_length_b                   6.008(2)
_cell_length_c                   17.143(6)
_cell_angle_alpha                90
_cell_angle_beta                 104.532(11)
_cell_angle_gamma                90
_cell_volume                     1077.6(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1300
_cell_measurement_temperature    197(2)
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      2.45
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1377 before and 0.0935 after correction.
The Ratio of minimum to maximum transmission is 0.7772.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             480
_exptl_crystal_preparation       
'Gel to crystal transformation in methyl salicylate medium'
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1240
_diffrn_reflns_av_unetI/netI     0.1573
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10667
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.369
_diffrn_reflns_theta_min         2.455
_diffrn_ambient_temperature      197.48
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    0.914
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                2268
_reflns_number_total             3761
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 
;
 Flack x determined using 618 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.17(15)
_refine_ls_extinction_coef       0.026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3761
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0622
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0354P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1421
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2D-N2
 1.017 with sigma of 0.02
 H2E-N2
 1.017 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C20(H20), C16(H16), C19(H19), C17(H17), C9(H9), C10(H10), C11(H11),
 C13(H13), C12(H12)
3.d Idealised Me refined as rotating group:
 N3(H3D,H3E,H3F), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
S1 S -0.24749(19) 0.1826(3) 0.35519(12) 0.0298(6) Uani 1 1 d . . . . .
O3 O 0.3958(5) 0.7841(8) 0.3982(3) 0.0282(13) Uani 1 1 d . . . . .
O2 O 0.5474(5) 1.0501(9) 0.1585(3) 0.0283(13) Uani 1 1 d . . . . .
O1 O 0.5873(5) 0.6991(9) 0.1214(3) 0.0295(12) Uani 1 1 d . . . . .
O4 O 0.4417(5) 0.5010(9) 0.3265(3) 0.0340(14) Uani 1 1 d . . . . .
O5 O -0.2917(5) 0.2764(9) 0.4203(3) 0.0367(15) Uani 1 1 d . . . . .
O6 O -0.2722(5) -0.0493(9) 0.3353(3) 0.0347(14) Uani 1 1 d . . . . .
N3 N 0.4164(5) 0.2196(11) 0.4460(3) 0.0277(16) Uani 1 1 d . . . . .
H3D H 0.415758 0.318826 0.405767 0.033 Uiso 1 1 calc R U . . .
H3E H 0.398013 0.081275 0.424541 0.033 Uiso 1 1 calc R U . . .
H3F H 0.495070 0.218484 0.481040 0.033 Uiso 1 1 calc R U . . .
N1 N 0.4625(6) 0.7432(10) 0.2036(3) 0.0275(16) Uani 1 1 d . . . . .
H1 H 0.448067 0.599740 0.195821 0.033 Uiso 1 1 calc R U . . .
C14 C 0.4164(6) 0.7011(15) 0.3347(4) 0.0244(17) Uani 1 1 d . . . . .
N2 N -0.3000(7) 0.3320(12) 0.2760(4) 0.0369(19) Uani 1 1 d D . . . .
C20 C 0.0003(7) 0.0426(14) 0.3769(4) 0.0269(19) Uani 1 1 d . . . . .
H20 H -0.034119 -0.093487 0.352570 0.032 Uiso 1 1 calc R U . . .
C15 C -0.0802(7) 0.2178(12) 0.3812(4) 0.0219(17) Uani 1 1 d . . . . .
C4 C 0.6869(7) 0.7634(13) 0.0806(4) 0.0266(19) Uani 1 1 d . . . . .
C16 C -0.0307(7) 0.4211(13) 0.4124(4) 0.0262(19) Uani 1 1 d . . . . .
H16 H -0.085516 0.543960 0.413558 0.031 Uiso 1 1 calc R U . . .
C5 C 0.5340(8) 0.8469(14) 0.1607(4) 0.028(2) Uani 1 1 d . . . . .
C19 C 0.1313(8) 0.0638(14) 0.4078(4) 0.0282(19) Uani 1 1 d . . . . .
H19 H 0.186132 -0.057818 0.404960 0.034 Uiso 1 1 calc R U . . .
C7 C 0.2690(7) 0.9309(13) 0.2256(4) 0.0279(19) Uani 1 1 d . . . . .
H7A H 0.236328 1.006219 0.267759 0.033 Uiso 1 1 calc R U . . .
H7B H 0.268037 1.040404 0.182281 0.033 Uiso 1 1 calc R U . . .
C18 C 0.1821(7) 0.2615(12) 0.4428(4) 0.0229(18) Uani 1 1 d . . . . .
C21 C 0.3196(7) 0.2847(14) 0.4891(4) 0.0277(19) Uani 1 1 d . . . . .
H21A H 0.334812 0.441960 0.506010 0.033 Uiso 1 1 calc R U . . .
H21B H 0.332938 0.193546 0.538584 0.033 Uiso 1 1 calc R U . . .
C17 C 0.1012(7) 0.4418(14) 0.4421(4) 0.0285(19) Uani 1 1 d . . . . .
H17 H 0.136479 0.581477 0.462161 0.034 Uiso 1 1 calc R U . . .
C6 C 0.4077(7) 0.8562(13) 0.2622(4) 0.0255(19) Uani 1 1 d . . . . .
H6 H 0.460313 0.991645 0.281444 0.031 Uiso 1 1 calc R U . . .
C8 C 0.1823(7) 0.7426(13) 0.1918(5) 0.028(2) Uani 1 1 d . . . . .
C2 C 0.7212(7) 0.5451(14) 0.0491(5) 0.040(2) Uani 1 1 d . . . . .
H2A H 0.750593 0.441473 0.094125 0.061 Uiso 1 1 calc R U . . .
H2B H 0.789483 0.568064 0.021645 0.061 Uiso 1 1 calc R U . . .
H2C H 0.645917 0.482981 0.011070 0.061 Uiso 1 1 calc R U . . .
C9 C 0.1303(8) 0.6063(13) 0.2406(5) 0.032(2) Uani 1 1 d . . . . .
H9 H 0.145072 0.640801 0.296266 0.038 Uiso 1 1 calc R U . . .
C1 C 0.6340(8) 0.9223(14) 0.0120(4) 0.037(2) Uani 1 1 d . . . . .
H1A H 0.556199 0.859206 -0.023223 0.055 Uiso 1 1 calc R U . . .
H1B H 0.697728 0.945790 -0.019057 0.055 Uiso 1 1 calc R U . . .
H1C H 0.613880 1.064837 0.033671 0.055 Uiso 1 1 calc R U . . .
C10 C 0.0578(8) 0.4223(15) 0.2107(5) 0.041(2) Uani 1 1 d . . . . .
H10 H 0.024107 0.331197 0.245676 0.049 Uiso 1 1 calc R U . . .
C11 C 0.0342(8) 0.3702(14) 0.1300(5) 0.036(2) Uani 1 1 d . . . . .
H11 H -0.013929 0.241614 0.109089 0.044 Uiso 1 1 calc R U . . .
C13 C 0.1548(7) 0.6926(16) 0.1098(4) 0.033(2) Uani 1 1 d . . . . .
H13 H 0.186580 0.785461 0.074368 0.039 Uiso 1 1 calc R U . . .
C3 C 0.8017(8) 0.8554(14) 0.1428(5) 0.036(2) Uani 1 1 d . . . . .
H3A H 0.781855 1.004930 0.159014 0.054 Uiso 1 1 calc R U . . .
H3B H 0.875536 0.862738 0.119410 0.054 Uiso 1 1 calc R U . . .
H3C H 0.821620 0.757642 0.190097 0.054 Uiso 1 1 calc R U . . .
C12 C 0.0818(8) 0.5089(16) 0.0801(5) 0.040(2) Uani 1 1 d . . . . .
H12 H 0.063865 0.476801 0.024071 0.048 Uiso 1 1 calc R U . . .
H2D H -0.345(9) 0.230(14) 0.233(4) 0.10(4) Uiso 1 1 d D . . . .
H2E H -0.319(13) 0.495(7) 0.271(8) 0.18(6) Uiso 1 1 d 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
S1 O5 1.436(5) . ?
S1 O6 1.443(6) . ?
S1 N2 1.607(7) . ?
S1 C15 1.763(7) . ?
O3 C14 1.267(8) . ?
O2 C5 1.231(9) . ?
O1 C4 1.475(8) . ?
O1 C5 1.330(9) . ?
O4 C14 1.249(10) . ?
N3 H3D 0.9100 . ?
N3 H3E 0.9100 . ?
N3 H3F 0.9100 . ?
N3 C21 1.477(9) . ?
N1 H1 0.8800 . ?
N1 C5 1.347(9) . ?
N1 C6 1.455(9) . ?
C14 C6 1.537(10) . ?
N2 H2D 0.99(3) . ?
N2 H2E 1.00(3) . ?
C20 H20 0.9500 . ?
C20 C15 1.380(10) . ?
C20 C19 1.388(10) . ?
C15 C16 1.386(10) . ?
C4 C2 1.499(11) . ?
C4 C1 1.511(10) . ?
C4 C3 1.523(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.394(10) . ?
C19 H19 0.9500 . ?
C19 C18 1.380(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C6 1.540(10) . ?
C7 C8 1.491(10) . ?
C18 C21 1.505(10) . ?
C18 C17 1.390(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C17 H17 0.9500 . ?
C6 H6 1.0000 . ?
C8 C9 1.386(10) . ?
C8 C13 1.395(10) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C9 H9 0.9500 . ?
C9 C10 1.378(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.377(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.384(11) . ?
C13 H13 0.9500 . ?
C13 C12 1.378(12) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C12 H12 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
O5 S1 O6 118.9(3) . . ?
O5 S1 N2 108.7(4) . . ?
O5 S1 C15 106.1(3) . . ?
O6 S1 N2 109.6(4) . . ?
O6 S1 C15 107.0(3) . . ?
N2 S1 C15 105.6(4) . . ?
C5 O1 C4 121.7(6) . . ?
H3D N3 H3E 109.5 . . ?
H3D N3 H3F 109.5 . . ?
H3E N3 H3F 109.5 . . ?
C21 N3 H3D 109.5 . . ?
C21 N3 H3E 109.5 . . ?
C21 N3 H3F 109.5 . . ?
C5 N1 H1 118.3 . . ?
C5 N1 C6 123.4(7) . . ?
C6 N1 H1 118.3 . . ?
O3 C14 C6 117.9(7) . . ?
O4 C14 O3 124.5(7) . . ?
O4 C14 C6 117.6(6) . . ?
S1 N2 H2D 107(6) . . ?
S1 N2 H2E 130(8) . . ?
H2D N2 H2E 119(10) . . ?
C15 C20 H20 119.8 . . ?
C15 C20 C19 120.4(8) . . ?
C19 C20 H20 119.8 . . ?
C20 C15 S1 121.0(6) . . ?
C20 C15 C16 120.3(7) . . ?
C16 C15 S1 118.4(6) . . ?
O1 C4 C2 102.5(6) . . ?
O1 C4 C1 110.9(6) . . ?
O1 C4 C3 109.0(6) . . ?
C2 C4 C1 110.6(6) . . ?
C2 C4 C3 109.7(7) . . ?
C1 C4 C3 113.5(7) . . ?
C15 C16 H16 120.7 . . ?
C15 C16 C17 118.7(7) . . ?
C17 C16 H16 120.7 . . ?
O2 C5 O1 125.3(8) . . ?
O2 C5 N1 124.3(8) . . ?
O1 C5 N1 110.4(7) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 C20 120.1(8) . . ?
C18 C19 H19 119.9 . . ?
H7A C7 H7B 107.8 . . ?
C6 C7 H7A 109.0 . . ?
C6 C7 H7B 109.0 . . ?
C8 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C8 C7 C6 113.0(6) . . ?
C19 C18 C21 122.8(7) . . ?
C19 C18 C17 119.1(7) . . ?
C17 C18 C21 117.9(7) . . ?
N3 C21 C18 116.2(6) . . ?
N3 C21 H21A 108.2 . . ?
N3 C21 H21B 108.2 . . ?
C18 C21 H21A 108.2 . . ?
C18 C21 H21B 108.2 . . ?
H21A C21 H21B 107.4 . . ?
C16 C17 H17 119.4 . . ?
C18 C17 C16 121.2(7) . . ?
C18 C17 H17 119.4 . . ?
N1 C6 C14 108.8(6) . . ?
N1 C6 C7 112.2(6) . . ?
N1 C6 H6 108.2 . . ?
C14 C6 C7 111.2(6) . . ?
C14 C6 H6 108.2 . . ?
C7 C6 H6 108.2 . . ?
C9 C8 C7 121.6(7) . . ?
C9 C8 C13 117.7(8) . . ?
C13 C8 C7 120.6(7) . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C8 C9 H9 119.1 . . ?
C10 C9 C8 121.9(8) . . ?
C10 C9 H9 119.1 . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.1(8) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.6 . . ?
C10 C11 C12 118.7(8) . . ?
C12 C11 H11 120.6 . . ?
C8 C13 H13 119.9 . . ?
C12 C13 C8 120.2(8) . . ?
C12 C13 H13 119.9 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C11 C12 H12 119.3 . . ?
C13 C12 C11 121.4(8) . . ?
C13 C12 H12 119.3 . . ?

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
S1 C15 C16 C17 172.4(5) . . . . ?
O3 C14 C6 N1 167.1(6) . . . . ?
O3 C14 C6 C7 -68.9(8) . . . . ?
O4 C14 C6 N1 -13.8(9) . . . . ?
O4 C14 C6 C7 110.2(7) . . . . ?
O5 S1 C15 C20 130.6(6) . . . . ?
O5 S1 C15 C16 -44.2(6) . . . . ?
O6 S1 C15 C20 2.6(7) . . . . ?
O6 S1 C15 C16 -172.1(6) . . . . ?
N2 S1 C15 C20 -114.1(6) . . . . ?
N2 S1 C15 C16 71.2(6) . . . . ?
C20 C15 C16 C17 -2.5(11) . . . . ?
C20 C19 C18 C21 170.0(6) . . . . ?
C20 C19 C18 C17 -3.9(11) . . . . ?
C15 C20 C19 C18 -0.4(10) . . . . ?
C15 C16 C17 C18 -1.9(11) . . . . ?
C4 O1 C5 O2 10.3(11) . . . . ?
C4 O1 C5 N1 -169.8(6) . . . . ?
C5 O1 C4 C2 177.4(6) . . . . ?
C5 O1 C4 C1 -64.5(8) . . . . ?
C5 O1 C4 C3 61.1(8) . . . . ?
C5 N1 C6 C14 -141.4(7) . . . . ?
C5 N1 C6 C7 95.1(8) . . . . ?
C19 C20 C15 S1 -171.1(5) . . . . ?
C19 C20 C15 C16 3.6(11) . . . . ?
C19 C18 C21 N3 55.3(10) . . . . ?
C19 C18 C17 C16 5.0(11) . . . . ?
C7 C8 C9 C10 -175.1(7) . . . . ?
C7 C8 C13 C12 175.4(7) . . . . ?
C21 C18 C17 C16 -169.1(6) . . . . ?
C17 C18 C21 N3 -130.8(7) . . . . ?
C6 N1 C5 O2 -9.6(12) . . . . ?
C6 N1 C5 O1 170.5(6) . . . . ?
C6 C7 C8 C9 81.0(9) . . . . ?
C6 C7 C8 C13 -96.4(8) . . . . ?
C8 C7 C6 N1 58.6(8) . . . . ?
C8 C7 C6 C14 -63.6(8) . . . . ?
C8 C9 C10 C11 -0.6(12) . . . . ?
C8 C13 C12 C11 0.0(12) . . . . ?
C9 C8 C13 C12 -2.1(11) . . . . ?
C9 C10 C11 C12 -1.6(12) . . . . ?
C10 C11 C12 C13 1.9(13) . . . . ?
C13 C8 C9 C10 2.4(12) . . . . ?

_olex2_submission_original_sample_id NR01064
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT340_mo_pd030322_0m_a    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01121 Ang.  
RESPONSE:The crystal was poorly diffracting at higher Bragg angles.
The situation did not improve even after recrystallisation and fresh
data collection.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_n101namn_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2190088'
loop_
_audit_author_name
_audit_author_address
'NABANITA ROY'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2023-04-13 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_audit_creation_date             2022-02-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        NbocF-AMN
_chemical_formula_moiety         'C14 H18 N O4, C10 H18 N'
_chemical_formula_sum            'C24 H36 N2 O4'
_chemical_formula_weight         416.55
_chemical_absolute_configuration NboC-L-Phenylalanine
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.423(14)
_cell_length_b                   6.446(7)
_cell_length_c                   13.679(15)
_cell_angle_alpha                90
_cell_angle_beta                 95.363(16)
_cell_angle_gamma                90
_cell_volume                     1178(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2297
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.78
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1869 before and 0.0770 after correction.
The Ratio of minimum to maximum transmission is 0.4940.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             452
_exptl_crystal_preparation       'DMSO soln'
_exptl_crystal_recrystallization_method 'slow evaporation in long test tube'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17464
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.853
_diffrn_reflns_theta_min         1.495
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                2180
_reflns_number_total             4396
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 
;
 Flack x determined using 693 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(10)
_refine_ls_extinction_coef       0.050(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4396
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0544
_refine_ls_restrained_S_all      0.901
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0742P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1584
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), C6(H6), C17(H17), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C7(H7A,H7B), C24(H24A,H24B), C22(H22A,H22B), C18(H18A,H18B),
 C23(H23A,H23B), C20(H20A,H20B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C9(H9), C10(H10), C13(H13), C11(H11), C12(H12)
2.d Idealised Me refined as rotating group:
 N2(H2D,H2E,H2F), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.7877(3) 0.2659(5) 0.1522(3) 0.0709(11) Uani 1 1 d . . . . .
O3 O 0.5587(3) 0.4014(5) 0.3406(3) 0.0707(10) Uani 1 1 d . . . . .
O4 O 0.5625(2) 0.7114(5) 0.4059(3) 0.0660(10) Uani 1 1 d . . . . .
N2 N 0.5922(3) 0.1026(5) 0.4859(3) 0.0573(11) Uani 1 1 d . . . . .
H2D H 0.583059 0.198929 0.439321 0.069 Uiso 1 1 calc R U . . .
H2E H 0.545837 0.116923 0.527956 0.069 Uiso 1 1 calc R U . . .
H2F H 0.587062 -0.022755 0.458699 0.069 Uiso 1 1 calc R U . . .
N1 N 0.6903(4) 0.4901(8) 0.2144(3) 0.0816(14) Uani 1 1 d . . . . .
H1 H 0.643150 0.428423 0.178597 0.098 Uiso 1 1 calc R U . . .
O2 O 0.8542(3) 0.5211(7) 0.2488(4) 0.1182(17) Uani 1 1 d . . . . .
C14 C 0.5877(4) 0.5816(7) 0.3462(4) 0.0561(13) Uani 1 1 d . . . . .
C5 C 0.7828(5) 0.4341(9) 0.2090(4) 0.0696(15) Uani 1 1 d . . . . .
C15 C 0.6936(3) 0.1275(6) 0.5393(4) 0.0529(12) Uani 1 1 d . . . . .
C16 C 0.6988(4) 0.3351(7) 0.5903(4) 0.0674(15) Uani 1 1 d . . . . .
H16A H 0.648839 0.342298 0.637048 0.081 Uiso 1 1 calc R U . . .
H16B H 0.685691 0.445496 0.542613 0.081 Uiso 1 1 calc R U . . .
C7 C 0.6346(5) 0.8555(8) 0.2279(4) 0.0813(18) Uani 1 1 d . . . . .
H7A H 0.682928 0.884793 0.181258 0.098 Uiso 1 1 calc R U . . .
H7B H 0.639537 0.966473 0.276010 0.098 Uiso 1 1 calc R U . . .
C8 C 0.5309(5) 0.8648(8) 0.1732(4) 0.0779(17) Uani 1 1 d . . . . .
C4 C 0.8846(4) 0.1723(10) 0.1360(5) 0.0848(18) Uani 1 1 d . . . . .
C24 C 0.7703(4) 0.1179(8) 0.4662(4) 0.0719(15) Uani 1 1 d . . . . .
H24A H 0.757983 0.227155 0.417779 0.086 Uiso 1 1 calc R U . . .
H24B H 0.765991 -0.014461 0.432284 0.086 Uiso 1 1 calc R U . . .
C22 C 0.7110(4) -0.0442(7) 0.6130(4) 0.0726(15) Uani 1 1 d . . . . .
H22A H 0.706328 -0.177552 0.579953 0.087 Uiso 1 1 calc R U . . .
H22B H 0.660723 -0.039376 0.659442 0.087 Uiso 1 1 calc R U . . .
C18 C 0.8806(5) 0.3500(9) 0.5710(5) 0.0862(19) Uani 1 1 d . . . . .
H18A H 0.869227 0.460288 0.522979 0.103 Uiso 1 1 calc R U . . .
H18B H 0.946737 0.368706 0.604965 0.103 Uiso 1 1 calc R U . . .
C21 C 0.8152(5) -0.0171(8) 0.6668(5) 0.0816(17) Uani 1 1 d . . . . .
H21 H 0.827439 -0.128501 0.715219 0.098 Uiso 1 1 calc R U . . .
C6 C 0.6656(4) 0.6560(7) 0.2804(4) 0.0695(15) Uani 1 1 d . . . . .
H6 H 0.726483 0.686302 0.323189 0.083 Uiso 1 1 calc R U . . .
C17 C 0.8031(5) 0.3602(8) 0.6432(5) 0.0793(17) Uani 1 1 d . . . . .
H17 H 0.807509 0.495147 0.676326 0.095 Uiso 1 1 calc R U . . .
C19 C 0.8748(4) 0.1442(10) 0.5203(5) 0.0815(17) Uani 1 1 d . . . . .
H19 H 0.925387 0.137225 0.473229 0.098 Uiso 1 1 calc R U . . .
C9 C 0.4650(6) 1.0147(10) 0.1948(5) 0.0917(19) Uani 1 1 d . . . . .
H9 H 0.483833 1.105525 0.246005 0.110 Uiso 1 1 calc R U . . .
C23 C 0.8215(5) 0.1903(9) 0.7190(4) 0.0877(18) Uani 1 1 d . . . . .
H23A H 0.771675 0.197311 0.765969 0.105 Uiso 1 1 calc R U . . .
H23B H 0.887070 0.207313 0.754339 0.105 Uiso 1 1 calc R U . . .
C20 C 0.8930(5) -0.0262(9) 0.5955(5) 0.093(2) Uani 1 1 d . . . . .
H20A H 0.890466 -0.159973 0.562859 0.112 Uiso 1 1 calc R U . . .
H20B H 0.958986 -0.009969 0.630147 0.112 Uiso 1 1 calc R U . . .
C10 C 0.3724(7) 1.0386(13) 0.1448(6) 0.115(2) Uani 1 1 d . . . . .
H10 H 0.330298 1.145644 0.160653 0.138 Uiso 1 1 calc R U . . .
C13 C 0.5019(6) 0.7319(11) 0.0985(5) 0.108(2) Uani 1 1 d . . . . .
H13 H 0.544701 0.627464 0.081125 0.129 Uiso 1 1 calc R U . . .
C2 C 0.9309(6) 0.0850(11) 0.2313(6) 0.115(2) Uani 1 1 d . . . . .
H2A H 0.939395 0.193817 0.279295 0.173 Uiso 1 1 calc R U . . .
H2B H 0.994931 0.025910 0.221694 0.173 Uiso 1 1 calc R U . . .
H2C H 0.888099 -0.020453 0.253891 0.173 Uiso 1 1 calc R U . . .
C3 C 0.8531(6) -0.0010(12) 0.0649(6) 0.126(3) Uani 1 1 d . . . . .
H3A H 0.814860 -0.101741 0.097029 0.189 Uiso 1 1 calc R U . . .
H3B H 0.911520 -0.066005 0.043182 0.189 Uiso 1 1 calc R U . . .
H3C H 0.813028 0.055121 0.009297 0.189 Uiso 1 1 calc R U . . .
C11 C 0.3434(7) 0.9034(15) 0.0718(6) 0.113(2) Uani 1 1 d . . . . .
H11 H 0.279996 0.913540 0.038326 0.136 Uiso 1 1 calc R U . . .
C1 C 0.9491(7) 0.3256(13) 0.0914(8) 0.172(5) Uani 1 1 d . . . . .
H1A H 0.915283 0.376747 0.031321 0.258 Uiso 1 1 calc R U . . .
H1B H 1.010714 0.260463 0.078012 0.258 Uiso 1 1 calc R U . . .
H1C H 0.963211 0.439010 0.136121 0.258 Uiso 1 1 calc R U . . .
C12 C 0.4068(8) 0.7548(14) 0.0484(6) 0.129(3) Uani 1 1 d . . . . .
H12 H 0.387014 0.664173 -0.002623 0.155 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 C5 1.339(7) . ?
O1 C4 1.469(6) . ?
O3 C14 1.225(5) . ?
O4 C14 1.238(6) . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N2 H2F 0.8900 . ?
N2 C15 1.492(6) . ?
N1 H1 0.8600 . ?
N1 C5 1.302(7) . ?
N1 C6 1.457(6) . ?
O2 C5 1.197(6) . ?
C14 C6 1.519(7) . ?
C15 C16 1.507(6) . ?
C15 C24 1.503(7) . ?
C15 C22 1.501(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.524(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.518(8) . ?
C7 C6 1.512(7) . ?
C8 C9 1.361(8) . ?
C8 C13 1.362(8) . ?
C4 C2 1.500(8) . ?
C4 C3 1.515(9) . ?
C4 C1 1.482(9) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C19 1.533(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C21 1.529(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C17 1.502(9) . ?
C18 C19 1.495(8) . ?
C21 H21 0.9800 . ?
C21 C23 1.515(8) . ?
C21 C20 1.496(9) . ?
C6 H6 0.9800 . ?
C17 H17 0.9800 . ?
C17 C23 1.512(8) . ?
C19 H19 0.9800 . ?
C19 C20 1.509(9) . ?
C9 H9 0.9300 . ?
C9 C10 1.371(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C10 H10 0.9300 . ?
C10 C11 1.355(10) . ?
C13 H13 0.9300 . ?
C13 C12 1.400(11) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C11 H11 0.9300 . ?
C11 C12 1.340(11) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C12 H12 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
C5 O1 C4 120.8(5) . . ?
H2D N2 H2E 109.5 . . ?
H2D N2 H2F 109.5 . . ?
H2E N2 H2F 109.5 . . ?
C15 N2 H2D 109.5 . . ?
C15 N2 H2E 109.5 . . ?
C15 N2 H2F 109.5 . . ?
C5 N1 H1 119.6 . . ?
C5 N1 C6 120.8(5) . . ?
C6 N1 H1 119.6 . . ?
O3 C14 O4 125.2(5) . . ?
O3 C14 C6 119.7(4) . . ?
O4 C14 C6 115.0(4) . . ?
N1 C5 O1 110.9(5) . . ?
O2 C5 O1 124.2(5) . . ?
O2 C5 N1 124.9(6) . . ?
N2 C15 C16 108.8(4) . . ?
N2 C15 C24 108.7(4) . . ?
N2 C15 C22 109.1(4) . . ?
C24 C15 C16 109.9(4) . . ?
C22 C15 C16 110.3(4) . . ?
C22 C15 C24 110.1(4) . . ?
C15 C16 H16A 110.0 . . ?
C15 C16 H16B 110.0 . . ?
C15 C16 C17 108.3(4) . . ?
H16A C16 H16B 108.4 . . ?
C17 C16 H16A 110.0 . . ?
C17 C16 H16B 110.0 . . ?
H7A C7 H7B 107.2 . . ?
C8 C7 H7A 107.9 . . ?
C8 C7 H7B 107.9 . . ?
C6 C7 H7A 107.9 . . ?
C6 C7 H7B 107.9 . . ?
C6 C7 C8 117.8(4) . . ?
C9 C8 C7 120.4(6) . . ?
C9 C8 C13 117.6(7) . . ?
C13 C8 C7 122.0(6) . . ?
O1 C4 C2 108.9(5) . . ?
O1 C4 C3 101.6(5) . . ?
O1 C4 C1 110.3(5) . . ?
C2 C4 C3 110.5(6) . . ?
C1 C4 C2 113.4(7) . . ?
C1 C4 C3 111.5(6) . . ?
C15 C24 H24A 109.9 . . ?
C15 C24 H24B 109.9 . . ?
C15 C24 C19 109.1(4) . . ?
H24A C24 H24B 108.3 . . ?
C19 C24 H24A 109.9 . . ?
C19 C24 H24B 109.9 . . ?
C15 C22 H22A 110.0 . . ?
C15 C22 H22B 110.0 . . ?
C15 C22 C21 108.5(4) . . ?
H22A C22 H22B 108.4 . . ?
C21 C22 H22A 110.0 . . ?
C21 C22 H22B 110.0 . . ?
H18A C18 H18B 108.2 . . ?
C17 C18 H18A 109.8 . . ?
C17 C18 H18B 109.8 . . ?
C19 C18 H18A 109.8 . . ?
C19 C18 H18B 109.8 . . ?
C19 C18 C17 109.5(5) . . ?
C22 C21 H21 109.2 . . ?
C23 C21 C22 109.6(5) . . ?
C23 C21 H21 109.2 . . ?
C20 C21 C22 110.2(5) . . ?
C20 C21 H21 109.2 . . ?
C20 C21 C23 109.3(5) . . ?
N1 C6 C14 110.1(4) . . ?
N1 C6 C7 113.5(5) . . ?
N1 C6 H6 106.9 . . ?
C14 C6 H6 106.9 . . ?
C7 C6 C14 112.1(4) . . ?
C7 C6 H6 106.9 . . ?
C16 C17 H17 109.1 . . ?
C18 C17 C16 110.2(5) . . ?
C18 C17 H17 109.1 . . ?
C18 C17 C23 109.9(5) . . ?
C23 C17 C16 109.5(5) . . ?
C23 C17 H17 109.1 . . ?
C24 C19 H19 109.6 . . ?
C18 C19 C24 109.2(5) . . ?
C18 C19 H19 109.6 . . ?
C18 C19 C20 109.4(5) . . ?
C20 C19 C24 109.4(5) . . ?
C20 C19 H19 109.6 . . ?
C8 C9 H9 118.3 . . ?
C8 C9 C10 123.3(7) . . ?
C10 C9 H9 118.3 . . ?
C21 C23 H23A 110.0 . . ?
C21 C23 H23B 110.0 . . ?
C17 C23 C21 108.5(5) . . ?
C17 C23 H23A 110.0 . . ?
C17 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
C21 C20 C19 109.7(5) . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
C19 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.7(8) . . ?
C11 C10 H10 120.7 . . ?
C8 C13 H13 120.5 . . ?
C8 C13 C12 119.0(7) . . ?
C12 C13 H13 120.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.4(8) . . ?
C12 C11 H11 120.3 . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C12 H12 119.0 . . ?
C11 C12 C13 122.0(8) . . ?
C11 C12 H12 119.0 . . ?

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
O3 C14 C6 N1 2.9(7) . . . . ?
O3 C14 C6 C7 130.2(5) . . . . ?
O4 C14 C6 N1 179.2(5) . . . . ?
O4 C14 C6 C7 -53.5(6) . . . . ?
N2 C15 C16 C17 -179.2(4) . . . . ?
N2 C15 C24 C19 179.8(4) . . . . ?
N2 C15 C22 C21 179.8(4) . . . . ?
C5 O1 C4 C2 66.2(6) . . . . ?
C5 O1 C4 C3 -177.1(5) . . . . ?
C5 O1 C4 C1 -58.8(8) . . . . ?
C5 N1 C6 C14 -126.8(5) . . . . ?
C5 N1 C6 C7 106.7(6) . . . . ?
C15 C16 C17 C18 59.9(6) . . . . ?
C15 C16 C17 C23 -61.1(6) . . . . ?
C15 C24 C19 C18 -60.3(6) . . . . ?
C15 C24 C19 C20 59.4(6) . . . . ?
C15 C22 C21 C23 60.3(6) . . . . ?
C15 C22 C21 C20 -60.1(6) . . . . ?
C16 C15 C24 C19 60.8(5) . . . . ?
C16 C15 C22 C21 -60.7(6) . . . . ?
C16 C17 C23 C21 61.2(6) . . . . ?
C7 C8 C9 C10 176.4(6) . . . . ?
C7 C8 C13 C12 -177.3(6) . . . . ?
C8 C7 C6 N1 74.9(6) . . . . ?
C8 C7 C6 C14 -50.6(6) . . . . ?
C8 C9 C10 C11 1.8(11) . . . . ?
C8 C13 C12 C11 -0.1(12) . . . . ?
C4 O1 C5 N1 -179.3(5) . . . . ?
C4 O1 C5 O2 1.1(8) . . . . ?
C24 C15 C16 C17 -60.3(5) . . . . ?
C24 C15 C22 C21 60.6(5) . . . . ?
C24 C19 C20 C21 -59.2(6) . . . . ?
C22 C15 C16 C17 61.2(6) . . . . ?
C22 C15 C24 C19 -60.8(5) . . . . ?
C22 C21 C23 C17 -60.7(6) . . . . ?
C22 C21 C20 C19 59.8(6) . . . . ?
C18 C17 C23 C21 -60.0(6) . . . . ?
C18 C19 C20 C21 60.4(6) . . . . ?
C6 N1 C5 O1 173.4(4) . . . . ?
C6 N1 C5 O2 -6.9(9) . . . . ?
C6 C7 C8 C9 123.5(6) . . . . ?
C6 C7 C8 C13 -59.6(7) . . . . ?
C17 C18 C19 C24 60.0(6) . . . . ?
C17 C18 C19 C20 -59.7(6) . . . . ?
C19 C18 C17 C16 -60.5(6) . . . . ?
C19 C18 C17 C23 60.2(6) . . . . ?
C9 C8 C13 C12 -0.3(9) . . . . ?
C9 C10 C11 C12 -2.1(12) . . . . ?
C23 C21 C20 C19 -60.7(6) . . . . ?
C20 C21 C23 C17 60.2(7) . . . . ?
C10 C11 C12 C13 1.4(13) . . . . ?
C13 C8 C9 C10 -0.6(9) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id N101NAMN
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_pd231221_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2190089'
loop_
_audit_author_name
_audit_author_address
'NABANITA ROY'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2023-04-13 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_audit_creation_date             2022-05-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        FmocF-MAF
_chemical_formula_moiety         'C7 H11 N2 O2 S, C24 H20 N O4'
_chemical_formula_sum            'C31 H31 N3 O6 S'
_chemical_formula_weight         573.65
_chemical_absolute_configuration Fmoc-L-Phenylalanine
_chemical_melting_point          ?
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   12.229(5)
_cell_length_b                   5.6301(17)
_cell_length_c                   20.557(6)
_cell_angle_alpha                90
_cell_angle_beta                 101.471(11)
_cell_angle_gamma                90
_cell_volume                     1387.1(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3284
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      30.70
_cell_measurement_theta_min      2.89
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.936
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.4857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1435 before and 0.0882 after correction.
The Ratio of minimum to maximum transmission is 0.6504.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             604
_exptl_crystal_preparation       'Ethanol and diethylether mixture'
_exptl_crystal_recrystallization_method 'slow evaporation in beaker'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_unetI/netI     0.1834
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19426
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.558
_diffrn_reflns_theta_min         2.368
_diffrn_ambient_temperature      259.84
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.723
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.728
_reflns_number_gt                4453
_reflns_number_total             9353
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 
;
 Flack x determined using 1205 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.19(10)
_refine_ls_extinction_coef       0.023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         9353
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1869
_refine_ls_R_factor_gt           0.0748
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0491P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1847
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C25(H25a,H25b), C17(H17a,H17b)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C27(H27), C28(H28), C30(H30), C1(H1a), C19(H19), C4(H4), C31(H31),
 C23(H23), C7(H7), C3(H3), C10(H10), C2(H2), C8(H8), C22(H22), C9(H9), C20(H20),
  C21(H21)
2.d Idealised Me refined as rotating group:
 N2(H2a,H2b,H2c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
S1 S 1.06145(12) 0.1615(2) 0.35136(6) 0.0336(3) Uani 1 1 d . . . . .
O1 O 0.6284(3) 0.1213(5) 0.27456(15) 0.0293(8) Uani 1 1 d . . . . .
O4 O 0.4642(3) 0.9671(6) 0.37409(16) 0.0319(9) Uani 1 1 d . . . . .
O3 O 0.5516(3) 0.6555(6) 0.42625(15) 0.0309(8) Uani 1 1 d . . . . .
O2 O 0.6751(3) 0.5123(6) 0.27107(17) 0.0325(9) Uani 1 1 d . . . . .
O6 O 1.1612(3) 0.0927(7) 0.39619(18) 0.0441(11) Uani 1 1 d . . . . .
N1 N 0.5201(4) 0.3918(7) 0.30769(19) 0.0282(10) Uani 1 1 d . . . . .
H1 H 0.490362 0.272985 0.323895 0.034 Uiso 1 1 calc R U . . .
O5 O 1.0544(4) 0.3889(7) 0.3197(2) 0.0472(11) Uani 1 1 d . . . . .
N2 N 0.5862(3) 0.2087(7) 0.47882(19) 0.0285(10) Uani 1 1 d . . . . .
H2A H 0.560049 0.109316 0.445693 0.034 Uiso 1 1 calc R U . . .
H2B H 0.590812 0.354208 0.462684 0.034 Uiso 1 1 calc R U . . .
H2C H 0.540269 0.210064 0.507414 0.034 Uiso 1 1 calc R U . . .
C24 C 0.4991(4) 0.7574(8) 0.3744(2) 0.0243(10) Uani 1 1 d . . . . .
N3 N 1.0413(5) -0.0352(12) 0.2940(3) 0.0440(13) Uani 1 1 d . . . . .
C5 C 0.8210(5) -0.0014(9) 0.1034(2) 0.0298(11) Uani 1 1 d . . . . .
C15 C 0.6128(5) 0.3570(8) 0.2831(2) 0.0261(11) Uani 1 1 d . . . . .
C26 C 0.7828(4) 0.1340(9) 0.4689(2) 0.0288(11) Uani 1 1 d . . . . .
C29 C 0.9520(4) 0.1500(10) 0.3959(2) 0.0278(10) Uani 1 1 d . . . . .
C6 C 0.7347(5) 0.1835(9) 0.0857(2) 0.0322(12) Uani 1 1 d . . . . .
C14 C 0.7262(4) 0.0510(8) 0.2492(2) 0.0266(11) Uani 1 1 d . . . . .
H14A H 0.765337 -0.074063 0.276943 0.032 Uiso 1 1 calc R U . . .
H14B H 0.776305 0.185432 0.251016 0.032 Uiso 1 1 calc R U . . .
C16 C 0.4689(4) 0.6241(8) 0.3077(2) 0.0266(10) Uani 1 1 d . . . . .
H16 H 0.493400 0.721216 0.273681 0.032 Uiso 1 1 calc R U . . .
C11 C 0.6573(4) 0.1596(9) 0.1270(2) 0.0279(10) Uani 1 1 d . . . . .
C12 C 0.7960(4) -0.1373(8) 0.1558(2) 0.0274(11) Uani 1 1 d . . . . .
C25 C 0.6975(4) 0.1300(10) 0.5130(2) 0.0317(11) Uani 1 1 d . . . . .
H25A H 0.692103 -0.030243 0.529317 0.038 Uiso 1 1 calc R U . . .
H25B H 0.723023 0.232111 0.550956 0.038 Uiso 1 1 calc R U . . .
C27 C 0.7914(5) 0.3264(9) 0.4278(2) 0.0311(12) Uani 1 1 d . . . . .
H27 H 0.741046 0.451476 0.425070 0.037 Uiso 1 1 calc R U . . .
C13 C 0.6931(4) -0.0378(9) 0.1773(2) 0.0260(10) Uani 1 1 d . . . . .
H13 H 0.634887 -0.159417 0.173602 0.031 Uiso 1 1 calc R U . . .
C17 C 0.3415(4) 0.6031(9) 0.2895(2) 0.0345(13) Uani 1 1 d . . . . .
H17A H 0.315783 0.516141 0.324390 0.041 Uiso 1 1 calc R U . . .
H17B H 0.309392 0.761090 0.287713 0.041 Uiso 1 1 calc R U . . .
C28 C 0.8752(5) 0.3330(9) 0.3904(2) 0.0307(12) Uani 1 1 d . . . . .
H28 H 0.879286 0.459920 0.362066 0.037 Uiso 1 1 calc R U . . .
C30 C 0.9435(5) -0.0461(9) 0.4362(2) 0.0344(13) Uani 1 1 d . . . . .
H30 H 0.994148 -0.170691 0.438980 0.041 Uiso 1 1 calc R U . . .
C1 C 0.8622(4) -0.3276(9) 0.1808(2) 0.0302(11) Uani 1 1 d . . . . .
H1A H 0.846463 -0.414917 0.216210 0.036 Uiso 1 1 calc R U . . .
C19 C 0.2444(5) 0.2636(10) 0.2230(3) 0.0367(13) Uani 1 1 d . . . . .
H19 H 0.237500 0.192701 0.262844 0.044 Uiso 1 1 calc R U . . .
C18 C 0.2994(4) 0.4805(9) 0.2244(2) 0.0292(11) Uani 1 1 d . . . . .
C4 C 0.9122(5) -0.0625(10) 0.0752(3) 0.0371(13) Uani 1 1 d . . . . .
H4 H 0.928982 0.025406 0.040122 0.044 Uiso 1 1 calc R U . . .
C31 C 0.8583(5) -0.0529(9) 0.4721(2) 0.0342(13) Uani 1 1 d . . . . .
H31 H 0.851659 -0.184032 0.498538 0.041 Uiso 1 1 calc R U . . .
C23 C 0.3105(5) 0.5803(10) 0.1638(3) 0.0386(14) Uani 1 1 d . . . . .
H23 H 0.347342 0.724306 0.162781 0.046 Uiso 1 1 calc R U . . .
C7 C 0.7221(5) 0.3609(10) 0.0378(3) 0.0392(14) Uani 1 1 d . . . . .
H7 H 0.774643 0.378084 0.011065 0.047 Uiso 1 1 calc R U . . .
C3 C 0.9768(5) -0.2555(10) 0.1001(3) 0.0396(14) Uani 1 1 d . . . . .
H3 H 1.037304 -0.297409 0.081415 0.047 Uiso 1 1 calc R U . . .
C10 C 0.5657(5) 0.3080(9) 0.1189(3) 0.0351(13) Uani 1 1 d . . . . .
H10 H 0.512654 0.290902 0.145359 0.042 Uiso 1 1 calc R U . . .
C2 C 0.9535(5) -0.3879(10) 0.1524(3) 0.0368(13) Uani 1 1 d . . . . .
H2 H 0.998272 -0.516724 0.168593 0.044 Uiso 1 1 calc R U . . .
C8 C 0.6318(5) 0.5109(10) 0.0302(3) 0.0419(15) Uani 1 1 d . . . . .
H8 H 0.622919 0.629757 -0.001862 0.050 Uiso 1 1 calc R U . . .
C22 C 0.2658(5) 0.4617(12) 0.1048(3) 0.0489(16) Uani 1 1 d . . . . .
H22 H 0.273778 0.527750 0.064526 0.059 Uiso 1 1 calc R U . . .
C9 C 0.5543(5) 0.4845(10) 0.0702(3) 0.0434(15) Uani 1 1 d . . . . .
H9 H 0.493194 0.586266 0.064550 0.052 Uiso 1 1 calc R U . . .
C20 C 0.2000(5) 0.1511(12) 0.1644(3) 0.0505(15) Uani 1 1 d . . . . .
H20 H 0.162668 0.007403 0.164978 0.061 Uiso 1 1 calc R U . . .
C21 C 0.2106(6) 0.2500(12) 0.1050(3) 0.0535(18) Uani 1 1 d . . . . .
H21 H 0.180495 0.174187 0.065317 0.064 Uiso 1 1 calc R U . . .
H3A H 1.057(6) -0.166(13) 0.306(3) 0.06(3) Uiso 1 1 d . . . . .
H3B H 0.984(6) -0.009(12) 0.259(3) 0.07(2) 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
S1 O6 1.429(4) . ?
S1 O5 1.431(4) . ?
S1 N3 1.600(5) . ?
S1 C29 1.766(5) . ?
O1 C15 1.357(6) . ?
O1 C14 1.451(6) . ?
O4 C24 1.255(5) . ?
O3 C24 1.266(5) . ?
O2 C15 1.217(6) . ?
N1 H1 0.8600 . ?
N1 C15 1.344(6) . ?
N1 C16 1.450(6) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C25 1.471(6) . ?
C24 C16 1.543(6) . ?
N3 H3A 0.79(7) . ?
N3 H3B 0.91(7) . ?
C5 C6 1.476(7) . ?
C5 C12 1.402(6) . ?
C5 C4 1.398(7) . ?
C26 C25 1.511(6) . ?
C26 C27 1.391(7) . ?
C26 C31 1.393(7) . ?
C29 C28 1.384(7) . ?
C29 C30 1.397(7) . ?
C6 C11 1.399(7) . ?
C6 C7 1.389(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.537(6) . ?
C16 H16 0.9800 . ?
C16 C17 1.533(7) . ?
C11 C13 1.522(7) . ?
C11 C10 1.381(7) . ?
C12 C13 1.522(7) . ?
C12 C1 1.379(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C27 H27 0.9300 . ?
C27 C28 1.397(7) . ?
C13 H13 0.9800 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.503(7) . ?
C28 H28 0.9300 . ?
C30 H30 0.9300 . ?
C30 C31 1.392(7) . ?
C1 H1A 0.9300 . ?
C1 C2 1.400(7) . ?
C19 H19 0.9300 . ?
C19 C18 1.392(8) . ?
C19 C20 1.374(8) . ?
C18 C23 1.398(7) . ?
C4 H4 0.9300 . ?
C4 C3 1.381(8) . ?
C31 H31 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.397(8) . ?
C7 H7 0.9300 . ?
C7 C8 1.374(8) . ?
C3 H3 0.9300 . ?
C3 C2 1.382(7) . ?
C10 H10 0.9300 . ?
C10 C9 1.399(7) . ?
C2 H2 0.9300 . ?
C8 H8 0.9300 . ?
C8 C9 1.381(8) . ?
C22 H22 0.9300 . ?
C22 C21 1.371(9) . ?
C9 H9 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.370(9) . ?
C21 H21 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
O6 S1 O5 120.2(3) . . ?
O6 S1 N3 105.9(3) . . ?
O6 S1 C29 107.1(2) . . ?
O5 S1 N3 107.3(3) . . ?
O5 S1 C29 106.6(3) . . ?
N3 S1 C29 109.5(3) . . ?
C15 O1 C14 117.4(4) . . ?
C15 N1 H1 119.1 . . ?
C15 N1 C16 121.9(4) . . ?
C16 N1 H1 119.1 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C25 N2 H2A 109.5 . . ?
C25 N2 H2B 109.5 . . ?
C25 N2 H2C 109.5 . . ?
O4 C24 O3 123.1(5) . . ?
O4 C24 C16 115.6(4) . . ?
O3 C24 C16 121.3(4) . . ?
S1 N3 H3A 115(5) . . ?
S1 N3 H3B 117(4) . . ?
H3A N3 H3B 121(7) . . ?
C12 C5 C6 108.7(4) . . ?
C4 C5 C6 131.4(5) . . ?
C4 C5 C12 119.9(5) . . ?
O2 C15 O1 124.5(5) . . ?
O2 C15 N1 125.5(4) . . ?
N1 C15 O1 110.0(4) . . ?
C27 C26 C25 121.4(5) . . ?
C27 C26 C31 119.1(5) . . ?
C31 C26 C25 119.4(5) . . ?
C28 C29 S1 120.2(4) . . ?
C28 C29 C30 120.4(5) . . ?
C30 C29 S1 119.3(4) . . ?
C11 C6 C5 108.6(4) . . ?
C7 C6 C5 130.9(5) . . ?
C7 C6 C11 120.5(5) . . ?
O1 C14 H14A 109.5 . . ?
O1 C14 H14B 109.5 . . ?
O1 C14 C13 110.9(4) . . ?
H14A C14 H14B 108.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
N1 C16 C24 114.3(4) . . ?
N1 C16 H16 108.0 . . ?
N1 C16 C17 110.4(4) . . ?
C24 C16 H16 108.0 . . ?
C17 C16 C24 107.8(4) . . ?
C17 C16 H16 108.0 . . ?
C6 C11 C13 110.2(4) . . ?
C10 C11 C6 119.9(5) . . ?
C10 C11 C13 129.9(4) . . ?
C5 C12 C13 110.0(4) . . ?
C1 C12 C5 120.6(5) . . ?
C1 C12 C13 129.4(4) . . ?
N2 C25 C26 113.2(4) . . ?
N2 C25 H25A 108.9 . . ?
N2 C25 H25B 108.9 . . ?
C26 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
H25A C25 H25B 107.8 . . ?
C26 C27 H27 119.8 . . ?
C26 C27 C28 120.5(5) . . ?
C28 C27 H27 119.8 . . ?
C14 C13 H13 110.5 . . ?
C11 C13 C14 113.6(4) . . ?
C11 C13 C12 102.4(4) . . ?
C11 C13 H13 110.5 . . ?
C12 C13 C14 109.0(4) . . ?
C12 C13 H13 110.5 . . ?
C16 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C18 C17 C16 113.8(4) . . ?
C18 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
C29 C28 C27 119.7(5) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C29 C30 H30 120.4 . . ?
C31 C30 C29 119.2(5) . . ?
C31 C30 H30 120.4 . . ?
C12 C1 H1A 120.3 . . ?
C12 C1 C2 119.3(5) . . ?
C2 C1 H1A 120.3 . . ?
C18 C19 H19 119.1 . . ?
C20 C19 H19 119.1 . . ?
C20 C19 C18 121.9(6) . . ?
C19 C18 C17 120.0(5) . . ?
C19 C18 C23 117.8(5) . . ?
C23 C18 C17 122.2(5) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 H4 120.6 . . ?
C26 C31 H31 119.6 . . ?
C30 C31 C26 120.9(5) . . ?
C30 C31 H31 119.6 . . ?
C18 C23 H23 120.3 . . ?
C22 C23 C18 119.4(5) . . ?
C22 C23 H23 120.3 . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.7(6) . . ?
C8 C7 H7 120.1 . . ?
C4 C3 H3 119.3 . . ?
C4 C3 C2 121.5(5) . . ?
C2 C3 H3 119.3 . . ?
C11 C10 H10 120.7 . . ?
C11 C10 C9 118.6(5) . . ?
C9 C10 H10 120.7 . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.9(5) . . ?
C3 C2 H2 120.1 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.8(5) . . ?
C9 C8 H8 120.1 . . ?
C23 C22 H22 119.3 . . ?
C21 C22 C23 121.3(6) . . ?
C21 C22 H22 119.3 . . ?
C10 C9 H9 119.3 . . ?
C8 C9 C10 121.4(6) . . ?
C8 C9 H9 119.3 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.2(6) . . ?
C21 C20 H20 119.9 . . ?
C22 C21 H21 120.3 . . ?
C20 C21 C22 119.4(6) . . ?
C20 C21 H21 120.3 . . ?

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
S1 C29 C28 C27 -177.6(4) . . . . ?
S1 C29 C30 C31 178.9(4) . . . . ?
O1 C14 C13 C11 73.4(5) . . . . ?
O1 C14 C13 C12 -173.2(4) . . . . ?
O4 C24 C16 N1 173.8(4) . . . . ?
O4 C24 C16 C17 -63.1(5) . . . . ?
O3 C24 C16 N1 -9.2(6) . . . . ?
O3 C24 C16 C17 114.0(5) . . . . ?
O6 S1 C29 C28 135.1(4) . . . . ?
O6 S1 C29 C30 -45.3(5) . . . . ?
N1 C16 C17 C18 -55.7(5) . . . . ?
O5 S1 C29 C28 5.3(5) . . . . ?
O5 S1 C29 C30 -175.1(4) . . . . ?
C24 C16 C17 C18 178.8(4) . . . . ?
N3 S1 C29 C28 -110.5(5) . . . . ?
N3 S1 C29 C30 69.1(5) . . . . ?
C5 C6 C11 C13 3.0(6) . . . . ?
C5 C6 C11 C10 -178.0(4) . . . . ?
C5 C6 C7 C8 178.8(5) . . . . ?
C5 C12 C13 C14 -116.3(4) . . . . ?
C5 C12 C13 C11 4.4(5) . . . . ?
C5 C12 C1 C2 -1.6(7) . . . . ?
C5 C4 C3 C2 -0.3(8) . . . . ?
C15 O1 C14 C13 -108.4(4) . . . . ?
C15 N1 C16 C24 -98.7(5) . . . . ?
C15 N1 C16 C17 139.5(4) . . . . ?
C26 C27 C28 C29 -1.8(7) . . . . ?
C29 C30 C31 C26 -0.8(8) . . . . ?
C6 C5 C12 C13 -2.8(5) . . . . ?
C6 C5 C12 C1 178.2(4) . . . . ?
C6 C5 C4 C3 -176.3(5) . . . . ?
C6 C11 C13 C14 112.9(5) . . . . ?
C6 C11 C13 C12 -4.5(5) . . . . ?
C6 C11 C10 C9 -1.7(7) . . . . ?
C6 C7 C8 C9 0.1(8) . . . . ?
C14 O1 C15 O2 -0.1(7) . . . . ?
C14 O1 C15 N1 -179.0(4) . . . . ?
C16 N1 C15 O1 -165.7(4) . . . . ?
C16 N1 C15 O2 15.4(8) . . . . ?
C16 C17 C18 C19 115.0(5) . . . . ?
C16 C17 C18 C23 -66.9(6) . . . . ?
C11 C6 C7 C8 -1.3(8) . . . . ?
C11 C10 C9 C8 0.5(8) . . . . ?
C12 C5 C6 C11 -0.1(6) . . . . ?
C12 C5 C6 C7 179.8(5) . . . . ?
C12 C5 C4 C3 -0.7(8) . . . . ?
C12 C1 C2 C3 0.6(8) . . . . ?
C25 C26 C27 C28 176.1(5) . . . . ?
C25 C26 C31 C30 -174.8(5) . . . . ?
C27 C26 C25 N2 45.1(7) . . . . ?
C27 C26 C31 C30 1.8(8) . . . . ?
C13 C11 C10 C9 177.1(5) . . . . ?
C13 C12 C1 C2 179.6(5) . . . . ?
C17 C18 C23 C22 -177.6(5) . . . . ?
C28 C29 C30 C31 -1.5(8) . . . . ?
C30 C29 C28 C27 2.8(8) . . . . ?
C1 C12 C13 C14 62.6(7) . . . . ?
C1 C12 C13 C11 -176.7(5) . . . . ?
C19 C18 C23 C22 0.6(8) . . . . ?
C19 C20 C21 C22 0.1(9) . . . . ?
C18 C19 C20 C21 1.0(9) . . . . ?
C18 C23 C22 C21 0.4(9) . . . . ?
C4 C5 C6 C11 175.9(5) . . . . ?
C4 C5 C6 C7 -4.3(9) . . . . ?
C4 C5 C12 C13 -179.3(5) . . . . ?
C4 C5 C12 C1 1.6(7) . . . . ?
C4 C3 C2 C1 0.3(8) . . . . ?
C31 C26 C25 N2 -138.4(5) . . . . ?
C31 C26 C27 C28 -0.4(7) . . . . ?
C23 C22 C21 C20 -0.8(9) . . . . ?
C7 C6 C11 C13 -176.9(4) . . . . ?
C7 C6 C11 C10 2.1(7) . . . . ?
C7 C8 C9 C10 0.3(8) . . . . ?
C10 C11 C13 C14 -66.0(7) . . . . ?
C10 C11 C13 C12 176.6(5) . . . . ?
C20 C19 C18 C17 176.9(5) . . . . ?
C20 C19 C18 C23 -1.3(8) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id pd231221
_olex2_submission_special_instructions 'No special instructions were received'
