# Electronic Supplementary Material (ESI) for RSC Advances.
# 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. 
# 
#######################################################################

data_2d_komal_naveedzafar_qau_0ma_a_a
_database_code_depnum_ccdc_archive 'CCDC 2281737'
loop_
_audit_author_name
_audit_author_address
'Dr. Maqsood Ahmed'
;Materials Chemistry Laboratory, Institute of Chemistry, The Islamia University of Bahawalpur,
Pakistan
;
_audit_update_record             
;
2023-07-15 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_audit_creation_method           
;FinalCif V118 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_creation_date             2023-07-15
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.893(3)
 0.107(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3.a Free rotating group:
 O3(H3A,H3B)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C20(H20A,H20B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C6(H6), C12(H12), C18(H18), C7(H7), C3(H3), C10(H10), C4(H4A),
  C19(H19), C11(H11), C16(H16), C17(H17)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C21 H25 I2 N5 O3'
_chemical_formula_moiety         '2(I), C21 H23 N5 O2, H2 O'
_chemical_formula_weight         649.26
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                   15.8789(13)
_cell_length_b                   10.7830(9)
_cell_length_c                   15.3311(11)
_cell_angle_alpha                90
_cell_angle_beta                 110.401(2)
_cell_angle_gamma                90
_cell_volume                     2460.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9960
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      25.45
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    2.587
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.6050
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1173 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.8118.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.492
_shelx_estimated_absorpt_T_max   0.600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cobra Cryo device'
_diffrn_radiation_probe          X-ray
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 CPAD
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_detector_area_resol_mean 7.41
_diffrn_measurement_device       'Four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            4582
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_theta_min         2.332
_diffrn_reflns_theta_max         25.707
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             4582
_reflns_number_gt                3651
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 _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       ?
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_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)+(0.1577P)²+34.7324P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4582
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0880
_refine_ls_wR_factor_ref         0.2946
_refine_ls_wR_factor_gt          0.2703
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         3.480
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.893(3)
2 0.107(3)

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'
I I -0.4742 1.8119 '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'

_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_
_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
I1 I 0.55688(6) 0.46728(9) 0.80604(6) 0.0549(3) Uani 1 1 d . . . . .
I2 I -0.05738(8) 0.43444(13) 0.78428(10) 0.0796(4) Uani 1 1 d . . . . .
N2 N 0.5956(6) 0.7148(10) 0.6584(7) 0.047(2) Uani 1 1 d . . . . .
H2 H 0.555854 0.700066 0.683475 0.056 Uiso 1 1 calc R U . . .
N3 N 0.4253(6) 0.6475(9) 0.5786(7) 0.042(2) Uani 1 1 d . . . . .
N1 N 0.8398(7) 0.8348(10) 0.8418(8) 0.050(3) Uani 1 1 d . . . . .
O2 O 0.2034(6) 0.6052(12) 0.5721(7) 0.063(3) Uani 1 1 d . . . . .
N4 N 0.3326(7) 0.6102(10) 0.6978(8) 0.047(2) Uani 1 1 d . . . . .
H4 H 0.390150 0.612249 0.713921 0.056 Uiso 1 1 calc R U . . .
O1 O 0.6159(7) 0.7097(13) 0.5164(7) 0.071(3) Uani 1 1 d . . . . .
N5 N 0.2354(8) 0.5953(11) 0.9146(9) 0.057(3) Uani 1 1 d . . . . .
C14 C 0.2839(9) 0.6131(12) 0.6035(9) 0.047(3) Uani 1 1 d . . . . .
C9 C 0.4712(8) 0.6565(11) 0.5216(9) 0.046(3) Uani 1 1 d . . . . .
C6 C 0.6881(8) 0.7790(13) 0.8103(10) 0.051(3) Uani 1 1 d . . . . .
H6 H 0.639660 0.769631 0.830574 0.061 Uiso 1 1 calc R U . . .
C15 C 0.2976(8) 0.6043(12) 0.7688(9) 0.044(3) Uani 1 1 d . . . . .
C12 C 0.2981(9) 0.5927(13) 0.4483(10) 0.054(3) Uani 1 1 d . . . . .
H12 H 0.238239 0.568171 0.424864 0.065 Uiso 1 1 calc R U . . .
C5 C 0.6787(7) 0.7528(11) 0.7177(9) 0.043(3) Uani 1 1 d . . . . .
C18 C 0.3236(9) 0.5671(15) 0.9273(10) 0.060(4) Uani 1 1 d . . . . .
H18 H 0.362383 0.545072 0.986295 0.072 Uiso 1 1 calc R U . . .
C7 C 0.7691(8) 0.8185(13) 0.8699(9) 0.050(3) Uani 1 1 d . . . . .
H7 H 0.775856 0.834645 0.931507 0.060 Uiso 1 1 calc R U . . .
C2 C 0.9297(9) 0.8797(14) 0.9061(12) 0.064(4) Uani 1 1 d . . . . .
H2A H 0.954075 0.938615 0.873368 0.077 Uiso 1 1 calc R U . . .
H2B H 0.922006 0.922234 0.958586 0.077 Uiso 1 1 calc R U . . .
C13 C 0.3389(8) 0.6171(11) 0.5412(10) 0.048(3) Uani 1 1 d . . . . .
C8 C 0.5692(8) 0.6981(12) 0.5650(9) 0.048(3) Uani 1 1 d . . . . .
C3 C 0.8327(9) 0.8078(15) 0.7556(11) 0.062(4) Uani 1 1 d . . . . .
H3 H 0.882861 0.816802 0.738112 0.074 Uiso 1 1 calc R U . . .
C10 C 0.4354(9) 0.6337(13) 0.4268(9) 0.053(3) Uani 1 1 d . . . . .
H10 H 0.470666 0.637904 0.389525 0.064 Uiso 1 1 calc R U . . .
C4 C 0.7538(8) 0.7668(14) 0.6909(10) 0.054(3) Uani 1 1 d . . . . .
H4A H 0.750280 0.748661 0.630393 0.065 Uiso 1 1 calc R U . . .
C19 C 0.3542(9) 0.5708(14) 0.8577(9) 0.054(3) Uani 1 1 d . . . . .
H19 H 0.413852 0.550960 0.868034 0.065 Uiso 1 1 calc R U . . .
C11 C 0.3461(10) 0.6048(14) 0.3904(10) 0.059(4) Uani 1 1 d . . . . .
H11 H 0.318364 0.593472 0.326633 0.071 Uiso 1 1 calc R U . . .
C16 C 0.2093(9) 0.6357(14) 0.7555(10) 0.056(3) Uani 1 1 d . . . . .
H16 H 0.170552 0.661642 0.697611 0.067 Uiso 1 1 calc R U . . .
C17 C 0.1806(10) 0.6275(15) 0.8298(11) 0.060(3) Uani 1 1 d . . . . .
H17 H 0.120811 0.645061 0.820876 0.072 Uiso 1 1 calc R U . . .
C1 C 0.9928(10) 0.7782(19) 0.9401(15) 0.086(6) Uani 1 1 d . . . . .
H1A H 1.003613 0.739207 0.888697 0.129 Uiso 1 1 calc R U . . .
H1B H 0.968234 0.718552 0.971135 0.129 Uiso 1 1 calc R U . . .
H1C H 1.048399 0.809690 0.983022 0.129 Uiso 1 1 calc R U . . .
C20 C 0.2061(12) 0.5884(16) 0.9954(12) 0.068(4) Uani 1 1 d . . . . .
H20A H 0.153232 0.639758 0.984192 0.082 Uiso 1 1 calc R U . . .
H20B H 0.253231 0.620602 1.049791 0.082 Uiso 1 1 calc R U . . .
C21 C 0.1849(16) 0.4585(19) 1.0139(15) 0.092(6) Uani 1 1 d . . . . .
H21A H 0.222667 0.402229 0.995838 0.138 Uiso 1 1 calc R U . . .
H21B H 0.123023 0.440986 0.978732 0.138 Uiso 1 1 calc R U . . .
H21C H 0.195208 0.448750 1.079062 0.138 Uiso 1 1 calc R U . . .
O3 O 0.0868(19) 0.338(2) 0.3889(16) 0.135(7) Uani 1 1 d G . . . .
H3A H 0.106357 0.399846 0.424251 0.203 Uiso 1 1 d G U . . .
H3B H 0.036299 0.361217 0.350758 0.203 Uiso 1 1 d G U . . .


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
N2 H2 0.8600 . ?
N2 C5 1.378(15) . ?
N2 C8 1.357(16) . ?
N3 C9 1.323(17) . ?
N3 C13 1.331(15) . ?
N1 C7 1.346(17) . ?
N1 C2 1.504(16) . ?
N1 C3 1.320(19) . ?
O2 C14 1.201(16) . ?
N4 H4 0.8600 . ?
N4 C14 1.381(16) . ?
N4 C15 1.386(17) . ?
O1 C8 1.227(16) . ?
N5 C18 1.379(18) . ?
N5 C17 1.33(2) . ?
N5 C20 1.47(2) . ?
C14 C13 1.50(2) . ?
C9 C8 1.532(17) . ?
C9 C10 1.385(19) . ?
C6 H6 0.9300 . ?
C6 C5 1.403(19) . ?
C6 C7 1.361(18) . ?
C15 C19 1.394(17) . ?
C15 C16 1.386(18) . ?
C12 H12 0.9300 . ?
C12 C13 1.37(2) . ?
C12 C11 1.36(2) . ?
C5 C4 1.398(17) . ?
C18 H18 0.9300 . ?
C18 C19 1.32(2) . ?
C7 H7 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.45(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.37(2) . ?
C10 H10 0.9300 . ?
C10 C11 1.37(2) . ?
C4 H4A 0.9300 . ?
C19 H19 0.9300 . ?
C11 H11 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.37(2) . ?
C17 H17 0.9300 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.49(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
O3 H3A 0.8498 . ?
O3 H3B 0.8500 . ?

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 N2 H2 116.3 . . ?
C8 N2 H2 116.3 . . ?
C8 N2 C5 127.4(11) . . ?
C9 N3 C13 117.1(11) . . ?
C7 N1 C2 122.7(13) . . ?
C3 N1 C7 120.1(11) . . ?
C3 N1 C2 117.2(12) . . ?
C14 N4 H4 116.9 . . ?
C14 N4 C15 126.3(10) . . ?
C15 N4 H4 116.9 . . ?
C18 N5 C20 118.3(13) . . ?
C17 N5 C18 118.7(13) . . ?
C17 N5 C20 123.0(12) . . ?
O2 C14 N4 123.2(13) . . ?
O2 C14 C13 121.3(12) . . ?
N4 C14 C13 115.4(11) . . ?
N3 C9 C8 116.4(11) . . ?
N3 C9 C10 124.2(12) . . ?
C10 C9 C8 119.4(12) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
C7 C6 C5 118.9(12) . . ?
N4 C15 C19 118.9(11) . . ?
N4 C15 C16 122.4(12) . . ?
C16 C15 C19 118.7(13) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C11 C12 C13 119.3(12) . . ?
N2 C5 C6 117.8(11) . . ?
N2 C5 C4 123.8(12) . . ?
C4 C5 C6 118.4(11) . . ?
N5 C18 H18 119.3 . . ?
C19 C18 N5 121.4(13) . . ?
C19 C18 H18 119.3 . . ?
N1 C7 C6 121.7(13) . . ?
N1 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
N1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 N1 111.8(13) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
N3 C13 C14 118.2(12) . . ?
N3 C13 C12 122.6(13) . . ?
C12 C13 C14 119.2(11) . . ?
N2 C8 C9 112.9(11) . . ?
O1 C8 N2 126.8(12) . . ?
O1 C8 C9 120.3(12) . . ?
N1 C3 H3 118.9 . . ?
N1 C3 C4 122.2(13) . . ?
C4 C3 H3 118.9 . . ?
C9 C10 H10 121.4 . . ?
C11 C10 C9 117.2(13) . . ?
C11 C10 H10 121.4 . . ?
C5 C4 H4A 120.7 . . ?
C3 C4 C5 118.6(13) . . ?
C3 C4 H4A 120.7 . . ?
C15 C19 H19 119.8 . . ?
C18 C19 C15 120.4(13) . . ?
C18 C19 H19 119.8 . . ?
C12 C11 C10 119.5(13) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C15 C16 H16 120.8 . . ?
C17 C16 C15 118.4(13) . . ?
C17 C16 H16 120.8 . . ?
N5 C17 C16 122.3(13) . . ?
N5 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N5 C20 H20A 109.3 . . ?
N5 C20 H20B 109.3 . . ?
N5 C20 C21 111.6(15) . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 H20A 109.3 . . ?
C21 C20 H20B 109.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
H3A O3 H3B 104.5 . . ?

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
N2 C5 C4 C3 178.6(14) . . . . ?
N3 C9 C8 N2 2.6(16) . . . . ?
N3 C9 C8 O1 -179.4(13) . . . . ?
N3 C9 C10 C11 3(2) . . . . ?
N1 C3 C4 C5 0(2) . . . . ?
O2 C14 C13 N3 168.4(13) . . . . ?
O2 C14 C13 C12 -9.9(19) . . . . ?
N4 C14 C13 N3 -16.0(16) . . . . ?
N4 C14 C13 C12 165.7(12) . . . . ?
N4 C15 C19 C18 178.4(14) . . . . ?
N4 C15 C16 C17 -179.8(13) . . . . ?
N5 C18 C19 C15 0(2) . . . . ?
C14 N4 C15 C19 163.9(13) . . . . ?
C14 N4 C15 C16 -19(2) . . . . ?
C9 N3 C13 C14 -176.7(10) . . . . ?
C9 N3 C13 C12 1.6(18) . . . . ?
C9 C10 C11 C12 -4(2) . . . . ?
C6 C5 C4 C3 -1(2) . . . . ?
C15 N4 C14 O2 -3(2) . . . . ?
C15 N4 C14 C13 -178.9(12) . . . . ?
C15 C16 C17 N5 3(2) . . . . ?
C5 N2 C8 O1 3(2) . . . . ?
C5 N2 C8 C9 -179.4(11) . . . . ?
C5 C6 C7 N1 1(2) . . . . ?
C18 N5 C17 C16 -1(2) . . . . ?
C18 N5 C20 C21 -81(2) . . . . ?
C7 N1 C2 C1 99.9(18) . . . . ?
C7 N1 C3 C4 2(2) . . . . ?
C7 C6 C5 N2 -179.0(12) . . . . ?
C7 C6 C5 C4 1(2) . . . . ?
C2 N1 C7 C6 179.3(13) . . . . ?
C2 N1 C3 C4 -179.6(14) . . . . ?
C13 N3 C9 C8 176.9(10) . . . . ?
C13 N3 C9 C10 -1.5(18) . . . . ?
C13 C12 C11 C10 4(2) . . . . ?
C8 N2 C5 C6 172.1(13) . . . . ?
C8 N2 C5 C4 -8(2) . . . . ?
C8 C9 C10 C11 -175.8(12) . . . . ?
C3 N1 C7 C6 -3(2) . . . . ?
C3 N1 C2 C1 -78(2) . . . . ?
C10 C9 C8 N2 -178.9(11) . . . . ?
C10 C9 C8 O1 -1(2) . . . . ?
C19 C15 C16 C17 -3(2) . . . . ?
C11 C12 C13 N3 -3(2) . . . . ?
C11 C12 C13 C14 175.4(13) . . . . ?
C16 C15 C19 C18 1(2) . . . . ?
C17 N5 C18 C19 0(2) . . . . ?
C17 N5 C20 C21 99(2) . . . . ?
C20 N5 C18 C19 179.6(15) . . . . ?
C20 N5 C17 C16 178.8(15) . . . . ?

####################################################################### 
# 
# 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_4a_komal_navedzafar_qau_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2281739'
loop_
_audit_author_name
_audit_author_address
'Dr. Maqsood Ahmed'
;Materials Chemistry Laboratory, Institute of Chemistry, The Islamia University of Bahawalpur,
Pakistan
;
_audit_update_record             
;
2023-07-15 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_audit_creation_method           
;FinalCif V118 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_creation_date             2023-07-15
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C9(H9), C11(H11), C8(H8), C16(H16), C29(H29), C15(H15),
 C2(H2), C31(H31), C24(H24), C17(H17), C30(H30), C23(H23), C6(H6), C12(H12),
 C27(H27), C3(H3), C5(H5), C28(H28), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C15.50 H12.50 Cl N2.50 O Pd0.50'
_chemical_formula_moiety         '0.5(Cl), 0.5(C31 H25 Cl N5 O2 Pd)'
_chemical_formula_weight         338.43
_chemical_melting_point          ?
_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                   9.5070(4)
_cell_length_b                   11.2651(5)
_cell_length_c                   13.3444(5)
_cell_angle_alpha                86.5890(10)
_cell_angle_beta                 73.2160(10)
_cell_angle_gamma                76.0760(10)
_cell_volume                     1327.99(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0
_cell_measurement_reflns_used    1750
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      29.60
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5845
_exptl_absorpt_correction_T_max  0.6690
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1036 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.8737.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.785
_shelx_estimated_absorpt_T_max   0.864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      100.0
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cobra Cryo device'
_diffrn_radiation_probe          X-ray
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 CPAD
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_detector_area_resol_mean 7.41
_diffrn_measurement_device       'Four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            8475
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_theta_min         2.301
_diffrn_reflns_theta_max         29.653
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_measured_fraction_theta_max 0.661
_diffrn_measured_fraction_theta_full 0.855
_diffrn_reflns_Laue_measured_fraction_max 0.661
_diffrn_reflns_Laue_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.661
_diffrn_reflns_point_group_measured_fraction_full 0.855
_reflns_number_total             4965
_reflns_number_gt                3744
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_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)+4.7677P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4965
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1073
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.072
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'
Cl Cl 0.1484 0.1585 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_
_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
Cl2 Cl 0.38231(16) 0.33399(13) 0.45107(11) 0.0272(3) Uani 1 1 d . . . . .
O4 O 0.1642(4) 0.6936(3) 1.0107(3) 0.0195(8) Uani 1 1 d . . . . .
Cl1 Cl 0.74048(14) 0.42981(11) 0.77093(10) 0.0193(3) Uani 1 1 d . . . . .
N4 N 0.3993(4) 0.5894(4) 0.9065(3) 0.0137(8) Uani 1 1 d . . . . .
Pd1 Pd 0.61774(4) 0.61144(3) 0.86023(3) 0.01420(12) Uani 1 1 d . . . . .
O2 O 0.8617(4) 0.8396(3) 0.9194(3) 0.0252(9) Uani 1 1 d . . . . .
N2 N 0.8008(4) 0.6861(4) 0.8410(3) 0.0152(9) Uani 1 1 d . . . . .
N3 N 0.5266(5) 0.7434(4) 0.9625(3) 0.0160(9) Uani 1 1 d . . . . .
N1 N 1.1660(5) 0.6575(4) 0.5733(3) 0.0174(9) Uani 1 1 d . . . . .
N5 N 0.2146(4) 0.3610(4) 0.7738(3) 0.0148(9) Uani 1 1 d . . . . .
C21 C 0.2156(5) 0.4638(4) 0.9230(4) 0.0149(10) Uani 1 1 d . . . . .
H21 H 0.173288 0.482921 0.995486 0.018 Uiso 1 1 calc R U . . .
C14 C 0.6183(6) 0.8035(4) 0.9851(4) 0.0159(10) Uani 1 1 d . . . . .
C20 C 0.3374(6) 0.5113(4) 0.8648(4) 0.0150(10) Uani 1 1 d . . . . .
C22 C 0.1568(6) 0.3902(4) 0.8764(4) 0.0168(11) Uani 1 1 d . . . . .
H22 H 0.073897 0.359065 0.917129 0.020 Uiso 1 1 calc R U . . .
C19 C 0.3018(6) 0.6744(4) 0.9807(4) 0.0175(11) Uani 1 1 d . . . . .
C1 C 1.2400(6) 0.8042(5) 0.4378(4) 0.0184(11) Uani 1 1 d . . . . .
C18 C 0.3837(5) 0.7534(4) 1.0180(4) 0.0131(10) Uani 1 1 d . . . . .
C13 C 0.7756(5) 0.7782(4) 0.9128(4) 0.0153(10) Uani 1 1 d . . . . .
C9 C 1.0655(5) 0.6955(4) 0.7555(4) 0.0167(11) Uani 1 1 d . . . . .
H9 H 1.079235 0.716744 0.819320 0.020 Uiso 1 1 calc R U . . .
C11 C 0.9210(5) 0.6290(4) 0.6591(4) 0.0163(10) Uani 1 1 d . . . . .
H11 H 0.833442 0.604757 0.655678 0.020 Uiso 1 1 calc R U . . .
C8 C 1.1788(6) 0.6907(4) 0.6647(4) 0.0166(11) Uani 1 1 d . . . . .
H8 H 1.269412 0.711328 0.666087 0.020 Uiso 1 1 calc R U . . .
C10 C 0.9290(6) 0.6694(4) 0.7551(4) 0.0163(10) Uani 1 1 d . . . . .
C16 C 0.4166(6) 0.8970(5) 1.1297(4) 0.0204(11) Uani 1 1 d . . . . .
H16 H 0.378329 0.950268 1.188924 0.024 Uiso 1 1 calc R U . . .
C29 C 0.2982(6) -0.0980(5) 0.7928(4) 0.0245(12) Uani 1 1 d . . . . .
H29 H 0.331142 -0.182221 0.806859 0.029 Uiso 1 1 calc R U . . .
C7 C 1.2800(6) 0.6740(5) 0.4735(4) 0.0202(11) Uani 1 1 d . . . . .
H7A H 1.281484 0.616949 0.419430 0.024 Uiso 1 1 calc R U . . .
H7B H 1.381786 0.655898 0.484320 0.024 Uiso 1 1 calc R U . . .
C15 C 0.5646(6) 0.8827(5) 1.0703(4) 0.0178(11) Uani 1 1 d . . . . .
H15 H 0.628574 0.926315 1.087552 0.021 Uiso 1 1 calc R U . . .
C25 C 0.1473(6) 0.2807(5) 0.7254(4) 0.0211(12) Uani 1 1 d . . . . .
H25A H 0.176035 0.291213 0.648494 0.025 Uiso 1 1 calc R U . . .
H25B H 0.035767 0.305209 0.751801 0.025 Uiso 1 1 calc R U . . .
C2 C 1.2966(6) 0.8925(5) 0.4705(4) 0.0212(12) Uani 1 1 d . . . . .
H2 H 1.365905 0.869887 0.511211 0.025 Uiso 1 1 calc R U . . .
C26 C 0.2009(6) 0.1480(5) 0.7504(4) 0.0184(11) Uani 1 1 d . . . . .
C31 C 0.3353(6) 0.0782(5) 0.6874(4) 0.0191(11) Uani 1 1 d . . . . .
H31 H 0.393565 0.114739 0.629158 0.023 Uiso 1 1 calc R U . . .
C24 C 0.3977(5) 0.4757(4) 0.7591(4) 0.0160(10) Uani 1 1 d . . . . .
H24 H 0.483414 0.502680 0.717490 0.019 Uiso 1 1 calc R U . . .
C17 C 0.3224(6) 0.8338(5) 1.1033(4) 0.0196(11) Uani 1 1 d . . . . .
H17 H 0.219304 0.845326 1.142506 0.024 Uiso 1 1 calc R U . . .
C30 C 0.3853(6) -0.0445(5) 0.7087(4) 0.0259(13) Uani 1 1 d . . . . .
H30 H 0.478142 -0.091407 0.666080 0.031 Uiso 1 1 calc R U . . .
C23 C 0.3347(5) 0.4024(4) 0.7150(4) 0.0166(11) Uani 1 1 d . . . . .
H23 H 0.375646 0.380707 0.642935 0.020 Uiso 1 1 calc R U . . .
C6 C 1.1368(6) 0.8386(5) 0.3799(4) 0.0215(11) Uani 1 1 d . . . . .
H6 H 1.096949 0.778406 0.357676 0.026 Uiso 1 1 calc R U . . .
C12 C 1.0384(6) 0.6248(5) 0.5719(4) 0.0206(11) Uani 1 1 d . . . . .
H12 H 1.031162 0.598163 0.507751 0.025 Uiso 1 1 calc R U . . .
C27 C 0.1170(6) 0.0932(5) 0.8357(4) 0.0197(11) Uani 1 1 d . . . . .
H27 H 0.026404 0.140713 0.880365 0.024 Uiso 1 1 calc R U . . .
C3 C 1.2523(6) 1.0138(5) 0.4441(4) 0.0276(13) Uani 1 1 d . . . . .
H3 H 1.292675 1.074116 0.465403 0.033 Uiso 1 1 calc R U . . .
C5 C 1.0915(7) 0.9599(5) 0.3545(4) 0.0290(13) Uani 1 1 d . . . . .
H5 H 1.020781 0.982965 0.314934 0.035 Uiso 1 1 calc R U . . .
C28 C 0.1642(6) -0.0299(5) 0.8564(4) 0.0220(12) Uani 1 1 d . . . . .
H28 H 0.104989 -0.067123 0.913586 0.026 Uiso 1 1 calc R U . . .
C4 C 1.1489(7) 1.0469(5) 0.3863(4) 0.0297(14) Uani 1 1 d . . . . .
H4 H 1.117847 1.130208 0.368796 0.036 Uiso 1 1 calc R U . . .


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 C19 1.221(6) . ?
Cl1 Pd1 2.3035(12) . ?
N4 Pd1 2.060(4) . ?
N4 C20 1.387(6) . ?
N4 C19 1.383(6) . ?
Pd1 N2 2.055(4) . ?
Pd1 N3 1.939(4) . ?
O2 C13 1.215(6) . ?
N2 C13 1.385(6) . ?
N2 C10 1.394(6) . ?
N3 C14 1.331(6) . ?
N3 C18 1.327(6) . ?
N1 C8 1.344(6) . ?
N1 C7 1.489(6) . ?
N1 C12 1.354(6) . ?
N5 C22 1.349(6) . ?
N5 C25 1.494(6) . ?
N5 C23 1.354(6) . ?
C21 H21 0.9500 . ?
C21 C20 1.400(7) . ?
C21 C22 1.368(7) . ?
C14 C13 1.498(7) . ?
C14 C15 1.385(7) . ?
C20 C24 1.403(7) . ?
C22 H22 0.9500 . ?
C19 C18 1.502(7) . ?
C1 C7 1.509(7) . ?
C1 C2 1.384(7) . ?
C1 C6 1.389(7) . ?
C18 C17 1.394(7) . ?
C9 H9 0.9500 . ?
C9 C8 1.363(7) . ?
C9 C10 1.399(7) . ?
C11 H11 0.9500 . ?
C11 C10 1.414(7) . ?
C11 C12 1.354(7) . ?
C8 H8 0.9500 . ?
C16 H16 0.9500 . ?
C16 C15 1.376(7) . ?
C16 C17 1.397(7) . ?
C29 H29 0.9500 . ?
C29 C30 1.390(8) . ?
C29 C28 1.384(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C15 H15 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.509(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.386(7) . ?
C26 C31 1.391(7) . ?
C26 C27 1.394(7) . ?
C31 H31 0.9500 . ?
C31 C30 1.391(7) . ?
C24 H24 0.9500 . ?
C24 C23 1.374(7) . ?
C17 H17 0.9500 . ?
C30 H30 0.9500 . ?
C23 H23 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.384(8) . ?
C12 H12 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.389(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(8) . ?
C5 H5 0.9500 . ?
C5 C4 1.371(8) . ?
C28 H28 0.9500 . ?
C4 H4 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
C20 N4 Pd1 128.5(3) . . ?
C19 N4 Pd1 113.5(3) . . ?
C19 N4 C20 117.6(4) . . ?
N4 Pd1 Cl1 100.09(11) . . ?
N2 Pd1 Cl1 98.74(12) . . ?
N2 Pd1 N4 161.16(16) . . ?
N3 Pd1 Cl1 166.74(12) . . ?
N3 Pd1 N4 80.74(16) . . ?
N3 Pd1 N2 80.84(16) . . ?
C13 N2 Pd1 113.4(3) . . ?
C13 N2 C10 118.9(4) . . ?
C10 N2 Pd1 126.5(3) . . ?
C14 N3 Pd1 117.3(3) . . ?
C18 N3 Pd1 117.8(3) . . ?
C18 N3 C14 123.8(4) . . ?
C8 N1 C7 120.0(4) . . ?
C8 N1 C12 119.0(4) . . ?
C12 N1 C7 120.4(4) . . ?
C22 N5 C25 119.7(4) . . ?
C22 N5 C23 120.3(4) . . ?
C23 N5 C25 120.0(4) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C22 C21 C20 120.7(5) . . ?
N3 C14 C13 115.2(4) . . ?
N3 C14 C15 119.6(5) . . ?
C15 C14 C13 125.3(4) . . ?
N4 C20 C21 123.6(4) . . ?
N4 C20 C24 119.9(4) . . ?
C21 C20 C24 116.6(4) . . ?
N5 C22 C21 121.1(5) . . ?
N5 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
O4 C19 N4 127.3(5) . . ?
O4 C19 C18 120.7(4) . . ?
N4 C19 C18 111.9(4) . . ?
C2 C1 C7 119.6(5) . . ?
C2 C1 C6 119.5(5) . . ?
C6 C1 C7 120.7(5) . . ?
N3 C18 C19 115.1(4) . . ?
N3 C18 C17 119.2(4) . . ?
C17 C18 C19 125.8(5) . . ?
O2 C13 N2 128.0(5) . . ?
O2 C13 C14 119.7(4) . . ?
N2 C13 C14 112.2(4) . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.3(5) . . ?
C10 C9 H9 119.9 . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C12 C11 C10 119.9(5) . . ?
N1 C8 C9 121.8(5) . . ?
N1 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
N2 C10 C9 124.4(4) . . ?
N2 C10 C11 118.8(4) . . ?
C9 C10 C11 116.7(4) . . ?
C15 C16 H16 119.8 . . ?
C15 C16 C17 120.4(5) . . ?
C17 C16 H16 119.8 . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C28 C29 C30 120.7(5) . . ?
N1 C7 C1 109.1(4) . . ?
N1 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C1 C7 H7A 109.9 . . ?
C1 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C14 C15 H15 120.6 . . ?
C16 C15 C14 118.7(5) . . ?
C16 C15 H15 120.6 . . ?
N5 C25 H25A 109.4 . . ?
N5 C25 H25B 109.4 . . ?
N5 C25 C26 111.1(4) . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0(5) . . ?
C3 C2 H2 120.0 . . ?
C31 C26 C25 119.9(5) . . ?
C31 C26 C27 119.0(5) . . ?
C27 C26 C25 121.1(5) . . ?
C26 C31 H31 119.7 . . ?
C30 C31 C26 120.7(5) . . ?
C30 C31 H31 119.7 . . ?
C20 C24 H24 119.5 . . ?
C23 C24 C20 121.0(5) . . ?
C23 C24 H24 119.5 . . ?
C18 C17 C16 118.3(5) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C29 C30 C31 119.4(5) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
N5 C23 C24 120.3(5) . . ?
N5 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.4(5) . . ?
C5 C6 H6 119.8 . . ?
N1 C12 H12 119.0 . . ?
C11 C12 N1 122.1(5) . . ?
C11 C12 H12 119.0 . . ?
C26 C27 H27 119.6 . . ?
C28 C27 C26 120.8(5) . . ?
C28 C27 H27 119.6 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 119.9(5) . . ?
C4 C3 H3 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 C6 120.0(5) . . ?
C4 C5 H5 120.0 . . ?
C29 C28 C27 119.4(5) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 119.9 . . ?

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 C19 C18 N3 -164.7(4) . . . . ?
O4 C19 C18 C17 15.1(8) . . . . ?
N4 C20 C24 C23 -177.4(4) . . . . ?
N4 C19 C18 N3 10.9(6) . . . . ?
N4 C19 C18 C17 -169.3(5) . . . . ?
Pd1 N4 C20 C21 151.8(4) . . . . ?
Pd1 N4 C20 C24 -27.8(6) . . . . ?
Pd1 N4 C19 O4 168.9(4) . . . . ?
Pd1 N4 C19 C18 -6.4(5) . . . . ?
Pd1 N2 C13 O2 -178.8(4) . . . . ?
Pd1 N2 C13 C14 -1.8(5) . . . . ?
Pd1 N2 C10 C9 -163.2(4) . . . . ?
Pd1 N2 C10 C11 19.9(6) . . . . ?
Pd1 N3 C14 C13 11.9(5) . . . . ?
Pd1 N3 C14 C15 -168.3(4) . . . . ?
Pd1 N3 C18 C19 -10.6(5) . . . . ?
Pd1 N3 C18 C17 169.6(4) . . . . ?
N3 C14 C13 O2 171.1(5) . . . . ?
N3 C14 C13 N2 -6.2(6) . . . . ?
N3 C14 C15 C16 0.0(7) . . . . ?
N3 C18 C17 C16 -2.7(7) . . . . ?
N5 C25 C26 C31 -86.6(6) . . . . ?
N5 C25 C26 C27 94.0(6) . . . . ?
C21 C20 C24 C23 2.9(7) . . . . ?
C14 N3 C18 C19 -178.2(4) . . . . ?
C14 N3 C18 C17 2.0(7) . . . . ?
C20 N4 C19 O4 -4.1(8) . . . . ?
C20 N4 C19 C18 -179.4(4) . . . . ?
C20 C21 C22 N5 0.2(7) . . . . ?
C20 C24 C23 N5 -1.4(7) . . . . ?
C22 N5 C25 C26 -78.8(6) . . . . ?
C22 N5 C23 C24 -0.8(7) . . . . ?
C22 C21 C20 N4 178.0(4) . . . . ?
C22 C21 C20 C24 -2.3(7) . . . . ?
C19 N4 C20 C21 -36.4(7) . . . . ?
C19 N4 C20 C24 144.0(5) . . . . ?
C19 C18 C17 C16 177.5(5) . . . . ?
C1 C2 C3 C4 1.2(8) . . . . ?
C1 C6 C5 C4 0.1(8) . . . . ?
C18 N3 C14 C13 179.6(4) . . . . ?
C18 N3 C14 C15 -0.6(7) . . . . ?
C13 N2 C10 C9 30.1(7) . . . . ?
C13 N2 C10 C11 -146.8(5) . . . . ?
C13 C14 C15 C16 179.8(5) . . . . ?
C8 N1 C7 C1 -82.9(6) . . . . ?
C8 N1 C12 C11 2.6(8) . . . . ?
C8 C9 C10 N2 -171.9(5) . . . . ?
C8 C9 C10 C11 5.0(7) . . . . ?
C10 N2 C13 O2 -10.5(8) . . . . ?
C10 N2 C13 C14 166.6(4) . . . . ?
C10 C9 C8 N1 -2.1(8) . . . . ?
C10 C11 C12 N1 0.6(8) . . . . ?
C7 N1 C8 C9 169.4(5) . . . . ?
C7 N1 C12 C11 -168.6(5) . . . . ?
C7 C1 C2 C3 -175.6(5) . . . . ?
C7 C1 C6 C5 174.9(5) . . . . ?
C15 C14 C13 O2 -8.7(8) . . . . ?
C15 C14 C13 N2 174.0(5) . . . . ?
C15 C16 C17 C18 2.1(8) . . . . ?
C25 N5 C22 C21 -179.8(4) . . . . ?
C25 N5 C23 C24 -179.6(4) . . . . ?
C25 C26 C31 C30 -179.2(5) . . . . ?
C25 C26 C27 C28 177.8(5) . . . . ?
C2 C1 C7 N1 89.8(6) . . . . ?
C2 C1 C6 C5 0.5(8) . . . . ?
C2 C3 C4 C5 -0.6(8) . . . . ?
C26 C31 C30 C29 1.1(8) . . . . ?
C26 C27 C28 C29 1.7(8) . . . . ?
C31 C26 C27 C28 -1.7(7) . . . . ?
C17 C16 C15 C14 -0.8(8) . . . . ?
C30 C29 C28 C27 -0.3(8) . . . . ?
C23 N5 C22 C21 1.4(7) . . . . ?
C23 N5 C25 C26 100.1(5) . . . . ?
C6 C1 C7 N1 -84.6(6) . . . . ?
C6 C1 C2 C3 -1.1(8) . . . . ?
C6 C5 C4 C3 0.0(8) . . . . ?
C12 N1 C8 C9 -1.8(7) . . . . ?
C12 N1 C7 C1 88.2(6) . . . . ?
C12 C11 C10 N2 172.8(5) . . . . ?
C12 C11 C10 C9 -4.3(7) . . . . ?
C27 C26 C31 C30 0.2(8) . . . . ?
C28 C29 C30 C31 -1.1(8) . . . . ?


_vrf_PLAT029_4a_komal_navedzafar_qau_0ma_a 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.855 Why?  
RESPONSE: Probably due to triclinic space group and due to beamstop, many important reflections 
could not be measured due to which the compleleness has been compromised.
;
# 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_1B_Komal_NavedZafar_QAU_100K_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2281738'
loop_
_audit_author_name
_audit_author_address
'Dr. Maqsood Ahmed'
;Materials Chemistry Laboratory, Institute of Chemistry, The Islamia University of Bahawalpur,
Pakistan
;
_audit_update_record             
;
2023-07-15 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_audit_creation_method           
;FinalCif V118 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_creation_date             2023-07-15
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O3(H3a,H3b)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C25(H25a,H25b)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C5(H5), C6(H6), C3(H3), C31(H31), C27(H27), C2(H2a), C1(H1),
 C17(H17), C15(H15), C16(H16), C21(H21), C30(H30), C29(H29), C11(H11), C12(H12),
  C24(H24), C23(H23), C22(H22), C28(H28), C9(H9), C8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'
_refine_ls_d_res_high            0.7991
_refine_ls_d_res_low             9.0216
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C31 H29 Cl2 N5 O3'
_chemical_formula_moiety         '2(Cl), C31 H27 N5 O2, H2 O'
_chemical_formula_weight         590.513
_chemical_melting_point          ?
_space_group_crystal_system      triclinic
_symmetry_Int_Tables_number      2
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   9.2037(4)
_cell_length_b                   11.6728(5)
_cell_length_c                   14.0506(6)
_cell_angle_alpha                91.744(1)
_cell_angle_beta                 101.920(2)
_cell_angle_gamma                109.870(1)
_cell_volume                     1380.69(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    850
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      25.2
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_F_000             616.946
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5026
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1660 before and 0.0989 after correction.
The Ratio of minimum to maximum transmission is 0.6743.
The λ/2 correction factor is Not present.
;
_exptl_special_details           ?
_diffrn_ambient_temperature      100.00
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cobra Cryo device'
_diffrn_radiation_probe          X-ray
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 CPAD
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_detector_area_resol_mean 7.41
_diffrn_measurement_device       'Four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            39400
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_measured_fraction_theta_max 0.9961
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_reflns_Laue_measured_fraction_max 0.9961
_diffrn_reflns_Laue_measured_fraction_full 0.9968
_diffrn_reflns_point_group_measured_fraction_max 0.9961
_diffrn_reflns_point_group_measured_fraction_full 0.9968
_reflns_number_total             5655
_reflns_number_gt                4737
_reflns_threshold_expression     I>=2u(I)
_reflns_Friedel_coverage         0.0
_reflns_Friedel_fraction_max     ?
_reflns_Friedel_fraction_full    ?
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              -14
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              17
_reflns_special_details          ?
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_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)+(0.1565P)²+4.0463P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         5655
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_number_constraints    55
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0956
_refine_ls_wR_factor_ref         0.2773
_refine_ls_wR_factor_gt          0.2561
_refine_ls_goodness_of_fit_ref   1.0674
_refine_ls_restrained_S_all      1.0674
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0001
_refine_diff_density_max         2.8026
_refine_diff_density_min         -1.5084
_refine_diff_density_rms         0.1280
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55740 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_geom_special_details            ?

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_refinement_flags_posn
Cl1 Cl 0.74528(11) 0.54218(9) 0.19976(9) 0.0391(3) Uani 1.000000 .
Cl2 Cl 0.74265(17) 0.29930(12) 0.50120(9) 0.0535(4) Uani 1.000000 .
O1 O 0.1581(3) 0.3092(3) -0.0097(2) 0.0338(7) Uani 1.000000 .
O2 O 0.8189(4) 0.1366(3) 0.0689(2) 0.0388(7) Uani 1.000000 .
N2 N 0.3853(3) 0.4369(3) 0.0934(2) 0.0229(6) Uani 1.000000 .
H2 H 0.4870(3) 0.4504(3) 0.1157(2) 0.0275(8) Uiso 1.000000 R
N3 N 0.5328(3) 0.2800(3) 0.0462(2) 0.0217(6) Uani 1.000000 .
N4 N 0.8150(4) 0.2969(3) 0.1645(2) 0.0251(7) Uani 1.000000 .
H4 H 0.7654(4) 0.3490(3) 0.1668(2) 0.0301(8) Uiso 1.000000 R
N1 N 0.1973(4) 0.6665(3) 0.2162(2) 0.0267(7) Uani 1.000000 .
N5 N 1.1840(4) 0.3371(3) 0.4042(2) 0.0284(7) Uani 1.000000 .
O3 O 0.5481(5) 0.3931(4) 0.3410(3) 0.0550(9) Uani 1.000000 .
H3a H 0.608(6) 0.370(7) 0.387(4) 0.0824(14) Uiso 1.000000 G
H3b H 0.613(6) 0.435(6) 0.307(4) 0.0824(14) Uiso 1.000000 G
C20 C 0.9429(4) 0.3108(3) 0.2413(3) 0.0252(8) Uani 1.000000 .
C26 C 1.2596(4) 0.2209(4) 0.5376(3) 0.0288(8) Uani 1.000000 .
C4 C 0.2118(4) 0.8814(4) 0.2396(3) 0.0267(8) Uani 1.000000 .
C13 C 0.3012(4) 0.3421(3) 0.0217(3) 0.0247(7) Uani 1.000000 .
C5 C 0.3552(5) 0.9533(4) 0.3011(3) 0.0278(8) Uani 1.000000 .
H5 H 0.4018(5) 0.9208(4) 0.3553(3) 0.0334(9) Uiso 1.000000 R
C6 C 0.4306(5) 1.0731(4) 0.2833(3) 0.0312(8) Uani 1.000000 .
H6 H 0.5287(5) 1.1225(4) 0.3253(3) 0.0375(10) Uiso 1.000000 R
C3 C 0.1443(5) 0.9295(4) 0.1598(3) 0.0307(9) Uani 1.000000 .
H3 H 0.0465(5) 0.8803(4) 0.1172(3) 0.0369(10) Uiso 1.000000 R
C14 C 0.3950(4) 0.2725(3) -0.0132(3) 0.0241(7) Uani 1.000000 .
C10 C 0.3207(4) 0.5134(3) 0.1334(3) 0.0229(7) Uani 1.000000 .
C18 C 0.6067(4) 0.2087(3) 0.0181(3) 0.0246(7) Uani 1.000000 .
C19 C 0.7581(4) 0.2102(4) 0.0854(3) 0.0255(8) Uani 1.000000 .
C7 C 0.1321(5) 0.7517(4) 0.2591(3) 0.0315(9) Uani 1.000000 .
H7a H 0.0166(5) 0.7255(4) 0.2306(3) 0.0378(10) Uiso 1.000000 R
H7b H 0.1479(5) 0.7477(4) 0.3306(3) 0.0378(10) Uiso 1.000000 R
C31 C 1.3174(5) 0.1314(4) 0.5135(3) 0.0324(9) Uani 1.000000 .
H31 H 1.3920(5) 0.1484(4) 0.4734(3) 0.0389(11) Uiso 1.000000 R
C27 C 1.1535(5) 0.1954(4) 0.5978(3) 0.0388(10) Uani 1.000000 .
H27 H 1.1131(5) 0.2561(4) 0.6150(3) 0.0465(12) Uiso 1.000000 R
C2 C 0.2199(5) 1.0491(4) 0.1424(3) 0.0342(9) Uani 1.000000 .
H2a H 0.1735(5) 1.0819(4) 0.0882(3) 0.0411(11) Uiso 1.000000 R
C1 C 0.3617(5) 1.1204(4) 0.2035(3) 0.0329(9) Uani 1.000000 .
H1 H 0.4130(5) 1.2023(4) 0.1913(3) 0.0395(11) Uiso 1.000000 R
C17 C 0.5492(5) 0.1302(4) -0.0688(3) 0.0272(8) Uani 1.000000 .
H17 H 0.6044(5) 0.0796(4) -0.0851(3) 0.0326(9) Uiso 1.000000 R
C15 C 0.3300(5) 0.1990(4) -0.1019(3) 0.0314(9) Uani 1.000000 .
H15 H 0.2327(5) 0.1977(4) -0.1421(3) 0.0376(10) Uiso 1.000000 R
C16 C 0.4098(5) 0.1278(4) -0.1306(3) 0.0314(9) Uani 1.000000 .
H16 H 0.3697(5) 0.0781(4) -0.1917(3) 0.0377(10) Uiso 1.000000 R
C21 C 1.0535(5) 0.2532(4) 0.2402(3) 0.0352(9) Uani 1.000000 .
H21 H 1.0471(5) 0.2043(4) 0.1832(3) 0.0422(11) Uiso 1.000000 R
C30 C 1.2677(5) 0.0175(4) 0.5471(3) 0.0400(10) Uani 1.000000 .
H30 H 1.3070(5) -0.0435(4) 0.5292(3) 0.0480(12) Uiso 1.000000 R
C29 C 1.1604(5) -0.0079(5) 0.6069(3) 0.0420(11) Uani 1.000000 .
H29 H 1.1250(5) -0.0862(5) 0.6298(3) 0.0504(13) Uiso 1.000000 R
C25 C 1.3054(5) 0.3414(4) 0.4943(3) 0.0334(9) Uani 1.000000 .
H25a H 1.4099(5) 0.3590(4) 0.4779(3) 0.0401(11) Uiso 1.000000 R
H25b H 1.3150(5) 0.4082(4) 0.5430(3) 0.0401(11) Uiso 1.000000 R
C11 C 0.3235(5) 0.6468(4) 0.2669(3) 0.0351(9) Uani 1.000000 .
H11 H 0.3701(5) 0.6853(4) 0.3319(3) 0.0421(11) Uiso 1.000000 R
C12 C 0.3884(5) 0.5722(4) 0.2277(3) 0.0362(10) Uani 1.000000 .
H12 H 0.4799(5) 0.5608(4) 0.2651(3) 0.0434(12) Uiso 1.000000 R
C24 C 0.9655(6) 0.3873(4) 0.3242(3) 0.0409(11) Uani 1.000000 .
H24 H 0.8983(6) 0.4333(4) 0.3259(3) 0.0491(13) Uiso 1.000000 R
C23 C 1.0852(6) 0.3968(4) 0.4039(3) 0.0407(11) Uani 1.000000 .
H23 H 1.0975(6) 0.4483(4) 0.4609(3) 0.0489(13) Uiso 1.000000 R
C22 C 1.1710(5) 0.2682(5) 0.3225(3) 0.0376(10) Uani 1.000000 .
H22 H 1.2455(5) 0.2285(5) 0.3216(3) 0.0451(12) Uiso 1.000000 R
C28 C 1.1058(6) 0.0828(5) 0.6328(3) 0.0447(11) Uani 1.000000 .
H28 H 1.0347(6) 0.0672(5) 0.6752(3) 0.0536(13) Uiso 1.000000 R
C9 C 0.1950(6) 0.5415(5) 0.0800(4) 0.0461(12) Uani 1.000000 .
H9 H 0.1494(6) 0.5072(5) 0.0139(4) 0.0553(15) Uiso 1.000000 R
C8 C 0.1362(5) 0.6184(5) 0.1221(4) 0.0471(13) Uani 1.000000 .
H8 H 0.0512(5) 0.6380(5) 0.0844(4) 0.0565(15) Uiso 1.000000 R


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 C13 1.217(5) . ?
O2 C19 1.214(5) . ?
N2 H2 0.8800 . ?
N2 C13 1.366(5) . ?
N2 C10 1.392(5) . ?
N3 C14 1.339(5) . ?
N3 C18 1.337(5) . ?
N4 H4 0.8800 . ?
N4 C20 1.382(5) . ?
N4 C19 1.366(5) . ?
N1 C7 1.493(5) . ?
N1 C11 1.326(5) . ?
N1 C8 1.347(6) . ?
N5 C25 1.492(5) . ?
N5 C23 1.320(5) . ?
N5 C22 1.343(5) . ?
O3 H3a 0.8699 . ?
O3 H3b 0.8694 . ?
C20 C21 1.400(5) . ?
C20 C24 1.381(6) . ?
C26 C31 1.386(6) . ?
C26 C27 1.384(6) . ?
C26 C25 1.512(6) . ?
C4 C5 1.387(5) . ?
C4 C3 1.396(6) . ?
C4 C7 1.503(6) . ?
C13 C14 1.508(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(6) . ?
C6 H6 0.9500 . ?
C6 C1 1.396(6) . ?
C3 H3 0.9500 . ?
C3 C2 1.386(6) . ?
C14 C15 1.387(5) . ?
C10 C12 1.388(6) . ?
C10 C9 1.387(6) . ?
C18 C19 1.508(5) . ?
C18 C17 1.395(5) . ?
C7 H7a 0.9900 . ?
C7 H7b 0.9900 . ?
C31 H31 0.9500 . ?
C31 C30 1.383(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.379(7) . ?
C2 H2a 0.9500 . ?
C2 C1 1.373(6) . ?
C1 H1 0.9500 . ?
C17 H17 0.9500 . ?
C17 C16 1.384(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.383(6) . ?
C16 H16 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.371(6) . ?
C30 H30 0.9500 . ?
C30 C29 1.389(7) . ?
C29 H29 0.9500 . ?
C29 C28 1.385(7) . ?
C25 H25a 0.9900 . ?
C25 H25b 0.9900 . ?
C11 H11 0.9500 . ?
C11 C12 1.370(6) . ?
C12 H12 0.9500 . ?
C24 H24 0.9500 . ?
C24 C23 1.371(6) . ?
C23 H23 0.9500 . ?
C22 H22 0.9500 . ?
C28 H28 0.9500 . ?
C9 H9 0.9500 . ?
C9 C8 1.370(6) . ?
C8 H8 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
C13 N2 H2 117.85(19) . . ?
C10 N2 H2 117.85(19) . . ?
C10 N2 C13 124.3(3) . . ?
C18 N3 C14 116.8(3) . . ?
C20 N4 H4 116.8(2) . . ?
C19 N4 H4 116.76(19) . . ?
C19 N4 C20 126.5(3) . . ?
C11 N1 C7 120.7(3) . . ?
C8 N1 C7 119.4(3) . . ?
C8 N1 C11 119.7(3) . . ?
C23 N5 C25 121.4(3) . . ?
C22 N5 C25 119.6(3) . . ?
C22 N5 C23 119.0(3) . . ?
H3b O3 H3a 104.6 . . ?
C21 C20 N4 124.0(3) . . ?
C24 C20 N4 118.6(3) . . ?
C24 C20 C21 117.4(4) . . ?
C27 C26 C31 118.9(4) . . ?
C25 C26 C31 120.1(4) . . ?
C25 C26 C27 120.9(4) . . ?
C3 C4 C5 119.8(4) . . ?
C7 C4 C5 119.4(4) . . ?
C7 C4 C3 120.8(4) . . ?
N2 C13 O1 123.6(3) . . ?
C14 C13 O1 120.5(3) . . ?
C14 C13 N2 115.8(3) . . ?
H5 C5 C4 120.0(2) . . ?
C6 C5 C4 119.9(4) . . ?
C6 C5 H5 120.0(2) . . ?
H6 C6 C5 120.1(2) . . ?
C1 C6 C5 119.8(4) . . ?
C1 C6 H6 120.1(2) . . ?
H3 C3 C4 120.0(2) . . ?
C2 C3 C4 120.0(4) . . ?
C2 C3 H3 120.0(2) . . ?
C13 C14 N3 117.7(3) . . ?
C15 C14 N3 123.7(3) . . ?
C15 C14 C13 118.4(3) . . ?
C12 C10 N2 120.5(3) . . ?
C9 C10 N2 122.3(3) . . ?
C9 C10 C12 117.0(4) . . ?
C19 C18 N3 118.3(3) . . ?
C17 C18 N3 123.7(3) . . ?
C17 C18 C19 118.0(3) . . ?
N4 C19 O2 124.6(3) . . ?
C18 C19 O2 120.6(3) . . ?
C18 C19 N4 114.8(3) . . ?
C4 C7 N1 111.3(3) . . ?
H7a C7 N1 109.37(19) . . ?
H7a C7 C4 109.4(2) . . ?
H7b C7 N1 109.4(2) . . ?
H7b C7 C4 109.4(2) . . ?
H7b C7 H7a 108.0 . . ?
H31 C31 C26 119.6(3) . . ?
C30 C31 C26 120.7(4) . . ?
C30 C31 H31 119.6(3) . . ?
H27 C27 C26 119.8(3) . . ?
C28 C27 C26 120.5(4) . . ?
C28 C27 H27 119.8(3) . . ?
H2a C2 C3 119.9(2) . . ?
C1 C2 C3 120.2(4) . . ?
C1 C2 H2a 119.9(3) . . ?
C2 C1 C6 120.3(4) . . ?
H1 C1 C6 119.9(2) . . ?
H1 C1 C2 119.9(3) . . ?
H17 C17 C18 120.8(2) . . ?
C16 C17 C18 118.3(3) . . ?
C16 C17 H17 120.8(2) . . ?
H15 C15 C14 120.7(2) . . ?
C16 C15 C14 118.6(3) . . ?
C16 C15 H15 120.7(2) . . ?
C15 C16 C17 118.8(4) . . ?
H16 C16 C17 120.6(2) . . ?
H16 C16 C15 120.6(2) . . ?
H21 C21 C20 120.4(2) . . ?
C22 C21 C20 119.2(4) . . ?
C22 C21 H21 120.4(2) . . ?
H30 C30 C31 119.9(3) . . ?
C29 C30 C31 120.2(4) . . ?
C29 C30 H30 119.9(3) . . ?
H29 C29 C30 120.6(3) . . ?
C28 C29 C30 118.9(4) . . ?
C28 C29 H29 120.6(3) . . ?
C26 C25 N5 110.6(3) . . ?
H25a C25 N5 109.5(2) . . ?
H25a C25 C26 109.5(2) . . ?
H25b C25 N5 109.5(2) . . ?
H25b C25 C26 109.5(2) . . ?
H25b C25 H25a 108.1 . . ?
H11 C11 N1 119.2(2) . . ?
C12 C11 N1 121.6(4) . . ?
C12 C11 H11 119.2(2) . . ?
C11 C12 C10 120.2(4) . . ?
H12 C12 C10 119.9(2) . . ?
H12 C12 C11 119.9(2) . . ?
H24 C24 C20 120.1(2) . . ?
C23 C24 C20 119.9(4) . . ?
C23 C24 H24 120.1(3) . . ?
C24 C23 N5 122.4(4) . . ?
H23 C23 N5 118.8(2) . . ?
H23 C23 C24 118.8(3) . . ?
C21 C22 N5 122.0(4) . . ?
H22 C22 N5 119.0(2) . . ?
H22 C22 C21 119.0(2) . . ?
C29 C28 C27 120.8(4) . . ?
H28 C28 C27 119.6(3) . . ?
H28 C28 C29 119.6(3) . . ?
H9 C9 C10 119.8(2) . . ?
C8 C9 C10 120.4(4) . . ?
C8 C9 H9 119.8(3) . . ?
C9 C8 N1 120.8(4) . . ?
H8 C8 N1 119.6(2) . . ?
H8 C8 C9 119.6(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
O1 C13 N2 C10 -5.5(5) . . . . ?
O1 C13 C14 N3 -155.1(4) . . . . ?
O1 C13 C14 C15 21.3(5) . . . . ?
O2 C19 N4 C20 -4.4(5) . . . . ?
O2 C19 C18 N3 171.0(4) . . . . ?
O2 C19 C18 C17 -7.2(5) . . . . ?
N2 C13 C14 N3 21.0(4) . . . . ?
N2 C13 C14 C15 -162.6(3) . . . . ?
N2 C10 C12 C11 -179.6(4) . . . . ?
N2 C10 C9 C8 -179.3(5) . . . . ?
N3 C14 C15 C16 1.0(5) . . . . ?
N3 C18 C19 N4 -7.4(4) . . . . ?
N3 C18 C17 C16 1.5(4) . . . . ?
N4 C20 C21 C22 -176.5(4) . . . . ?
N4 C20 C24 C23 175.8(4) . . . . ?
N4 C19 C18 C17 174.3(3) . . . . ?
N1 C7 C4 C5 -83.8(4) . . . . ?
N1 C7 C4 C3 95.3(3) . . . . ?
N1 C11 C12 C10 -1.1(5) . . . . ?
N1 C8 C9 C10 -1.1(6) . . . . ?
N5 C25 C26 C31 94.0(4) . . . . ?
N5 C25 C26 C27 -82.7(4) . . . . ?
N5 C23 C24 C20 1.6(6) . . . . ?
N5 C22 C21 C20 -0.4(6) . . . . ?
C26 C31 C30 C29 -1.0(4) . . . . ?
C26 C27 C28 C29 -1.4(5) . . . . ?
C4 C5 C6 C1 -0.1(4) . . . . ?
C4 C3 C2 C1 0.3(4) . . . . ?
C13 C14 C15 C16 -175.1(4) . . . . ?
C5 C6 C1 C2 -0.1(5) . . . . ?
C6 C1 C2 C3 -0.0(4) . . . . ?
C14 C15 C16 C17 1.6(5) . . . . ?
C18 C17 C16 C15 -2.7(4) . . . . ?
C31 C30 C29 C28 -0.6(5) . . . . ?
C27 C28 C29 C30 1.8(5) . . . . ?


