# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# 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_pk-choome_auto_1
_database_code_depnum_ccdc_archive 'CCDC 2221369'
loop_
_audit_author_name
_audit_author_address
'KAKOLI MAJI'
;INDIAN INSTITUTE OF SCIENCE EDUCATION AND RESEARCH KOLKATA
India
;
_audit_update_record             
;
2022-11-22 deposited with the CCDC.	2023-09-07 downloaded from the CCDC.
;
_audit_creation_date             2022-11-22
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H28 O3'
_chemical_formula_sum            'C31 H28 O3'
_chemical_formula_weight         448.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O'
_chemical_oxdiff_usercomment     100K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.2216(2)
_cell_length_b                   15.1257(3)
_cell_length_c                   14.4955(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.837(2)
_cell_angle_gamma                90
_cell_volume                     2328.61(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15677
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.0700
_cell_measurement_theta_min      2.9080
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.939
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16598
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.135
_diffrn_reflns_theta_min         4.351
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00  34.00   0.50    0.20    --  -41.21  12.00-120.00  116
  2  ω    -24.00  34.00   0.50    0.20    --  -41.21  12.00 -60.00  116
  3  ω    -24.00  34.00   0.50    0.20    --  -41.21  12.00   0.00  116
  4  ω    -31.00  29.00   0.50    0.20    --  -41.21  25.00  60.00  120
  5  ω    -43.00  25.00   0.50    0.20    --  -41.21  38.00 120.00  136
  6  ω    -24.00  34.00   0.50    0.20    --  -41.21  12.00-180.00  116
  7  ω     26.00 111.00   0.50    0.20    --   41.21  25.00-150.00  170
  8  ω     80.00 163.00   0.50    0.20    --   96.67  42.00 -30.00  166
  9  ω     70.00 165.00   0.50    0.20    --   96.67  77.00-180.00  190
 10  ω     41.00 100.00   0.50    0.20    --   41.21-138.00 -60.00  118
 11  ω     30.00 109.00   0.50    0.20    --   96.67-117.00 -90.00  158
 12  ω      3.00  78.00   0.50    0.20    --   41.21-101.00  42.00  150
 13  ω     24.00 107.00   0.50    0.20    --   96.67-101.00  42.00  166
 14  ω     27.00 127.00   0.50    0.20    --   96.67 -87.00  60.00  200
 15  ω     28.00 105.00   0.50    0.20    --   96.67 -77.00  60.00  154
 16  ω     29.00  68.00   0.50    0.20    --   96.67 -59.00  90.00   78
 17  ω     29.00  68.00   0.50    0.20    --   96.67 -59.00 120.00   78
 18  ω     29.00  83.00   0.50    0.20    --   96.67 -68.00 150.00  108
 19  ω     29.00  68.00   0.50    0.20    --   96.67 -59.00 -60.00   78
 20  ω     29.00  83.00   0.50    0.20    --   96.67 -68.00 -90.00  108
 21  ω     29.00  83.00   0.50    0.20    --   96.67 -68.00-120.00  108
 22  ω     30.00  57.00   0.50    0.20    --   96.67 -50.00-180.00   54
 23  ω     30.00  57.00   0.50    0.20    --   96.67 -50.00-120.00   54
 24  ω     30.00  57.00   0.50    0.20    --   96.67 -50.00 -60.00   54
 25  ω     30.00  57.00   0.50    0.20    --   96.67 -50.00 -30.00   54
 26  ω    -34.00  24.00   0.50    0.20    --   41.21 -12.00-120.00  116
 27  ω     30.00  57.00   0.50    0.20    --   96.67 -50.00   0.00   54
 28  ω     30.00  57.00   0.50    0.20    --   96.67 -50.00  30.00   54
 29  ω     30.00  57.00   0.50    0.20    --   96.67 -50.00  60.00   54
 30  ω    106.00 169.00   0.50    0.20    --   96.67 101.00 146.00  126
 31  ω     99.00 164.00   0.50    0.20    --   96.67 117.00  30.00  130
 32  ω     81.00 164.00   0.50    0.20    --   96.67 145.00 -60.00  166
 33  ω    -78.00  19.00   0.50    0.20    --  -41.21 101.00 146.00  194
 34  ω    -81.00 -10.00   0.50    0.20    --  -82.50 101.00 146.00  142
 35  ω    -47.00 -15.00   0.50    0.20    --  -82.50  42.00 -60.00   64
 36  ω    -47.00 -15.00   0.50    0.20    --  -82.50  42.00 -90.00   64
 37  ω   -109.00 -18.00   0.50    0.20    --  -41.21 -64.00 -90.00  182
 38  ω   -157.00 -83.00   0.50    0.20    --  -82.50 -96.00-180.00  148
 39  ω   -155.00 -84.00   0.50    0.20    --  -82.50-101.00  42.00  142
 40  ω   -149.00 -78.00   0.50    0.20    --  -82.50-117.00 120.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0993280000
_diffrn_orient_matrix_UB_12      -0.0072286000
_diffrn_orient_matrix_UB_13      0.0523400000
_diffrn_orient_matrix_UB_21      -0.0402460000
_diffrn_orient_matrix_UB_22      0.0962859000
_diffrn_orient_matrix_UB_23      -0.0279746000
_diffrn_orient_matrix_UB_31      -0.0977839000
_diffrn_orient_matrix_UB_32      -0.0322145000
_diffrn_orient_matrix_UB_33      -0.0953633000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3940
_reflns_number_total             4212
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0567
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1051P)²+0.8403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1626
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C11(H11), C14(H14), C26(H26), C23(H23), C20(H20), C13(H13),
 C10(H10), C5(H5), C19(H19), C6(H6), C8(H8), C16(H16), C25(H25), C7(H7),
 C17(H17), C31(H31)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
O2 O 0.05008(11) 0.77950(8) 0.55387(8) 0.0236(3) Uani 1 1 d . . . . .
O3 O 1.07343(11) 0.44350(8) 0.68750(9) 0.0257(3) Uani 1 1 d . . . . .
O1 O 0.70823(13) 0.47333(9) 1.09428(9) 0.0333(3) Uani 1 1 d . . . . .
C22 C 0.32541(15) 0.65343(11) 0.53888(11) 0.0190(3) Uani 1 1 d . . . . .
H22 H 0.347842 0.613204 0.496911 0.023 Uiso 1 1 calc R . . . .
C11 C 0.95127(15) 0.57344(11) 0.61349(11) 0.0204(4) Uani 1 1 d . . . . .
H11 H 1.017966 0.597209 0.594216 0.024 Uiso 1 1 calc R . . . .
C3 C 0.57879(14) 0.67784(11) 0.49502(11) 0.0176(3) Uani 1 1 d . . . . .
C14 C 0.75482(15) 0.50548(11) 0.66903(11) 0.0189(3) Uani 1 1 d . . . . .
H14 H 0.687752 0.481345 0.687567 0.023 Uiso 1 1 calc R . . . .
C24 C 0.16803(15) 0.74404(11) 0.57316(12) 0.0193(4) Uani 1 1 d . . . . .
C26 C 0.37942(16) 0.73833(11) 0.68575(11) 0.0211(4) Uani 1 1 d . . . . .
H26 H 0.439383 0.756695 0.745428 0.025 Uiso 1 1 calc R . . . .
C12 C 0.96713(14) 0.49389(10) 0.66377(11) 0.0187(3) Uani 1 1 d . . . . .
C21 C 0.41669(15) 0.67958(10) 0.62536(11) 0.0178(3) Uani 1 1 d . . . . .
C15 C 0.59919(15) 0.61653(10) 0.76048(11) 0.0181(3) Uani 1 1 d . . . . .
C23 C 0.20213(15) 0.68485(11) 0.51252(11) 0.0197(4) Uani 1 1 d . . . . .
H23 H 0.141596 0.665919 0.453367 0.024 Uiso 1 1 calc R . . . .
C1 C 0.54758(14) 0.64409(10) 0.65586(11) 0.0174(3) Uani 1 1 d . . . . .
C9 C 0.73784(14) 0.58681(11) 0.61987(11) 0.0172(3) Uani 1 1 d . . . . .
C4 C 0.57631(14) 0.77006(11) 0.48060(11) 0.0189(4) Uani 1 1 d . . . . .
C18 C 0.69767(15) 0.55948(11) 0.95423(11) 0.0202(4) Uani 1 1 d . . . . .
C20 C 0.52982(14) 0.56005(10) 0.80061(11) 0.0186(3) Uani 1 1 d . . . . .
H20 H 0.447846 0.541896 0.761967 0.022 Uiso 1 1 calc R . . . .
C13 C 0.86718(15) 0.45985(11) 0.69097(11) 0.0199(3) Uani 1 1 d . . . . .
H13 H 0.876745 0.405092 0.724687 0.024 Uiso 1 1 calc R . . . .
C2 C 0.61663(15) 0.63704(10) 0.59461(11) 0.0182(3) Uani 1 1 d . . . . .
C10 C 0.83734(15) 0.61809(11) 0.59153(11) 0.0200(4) Uani 1 1 d . . . . .
H10 H 0.826996 0.671859 0.555926 0.024 Uiso 1 1 calc R . . . .
C5 C 0.55252(15) 0.80205(11) 0.38564(12) 0.0215(4) Uani 1 1 d . . . . .
H5 H 0.552023 0.864099 0.375398 0.026 Uiso 1 1 calc R . . . .
C19 C 0.57910(15) 0.53036(11) 0.89575(11) 0.0197(4) Uani 1 1 d . . . . .
H19 H 0.532454 0.490294 0.921228 0.024 Uiso 1 1 calc R . . . .
C28 C 0.60470(15) 0.83557(11) 0.56372(12) 0.0213(4) Uani 1 1 d . . . . .
H28A H 0.556693 0.818716 0.607557 0.026 Uiso 1 1 calc R . . . .
H28B H 0.575533 0.894888 0.537011 0.026 Uiso 1 1 calc R . . . .
C6 C 0.52974(15) 0.74608(12) 0.30633(11) 0.0225(4) Uani 1 1 d . . . . .
H6 H 0.513388 0.769650 0.242685 0.027 Uiso 1 1 calc R . . . .
C8 C 0.55697(14) 0.62215(11) 0.41390(11) 0.0193(4) Uani 1 1 d . . . . .
H8 H 0.560095 0.559929 0.423290 0.023 Uiso 1 1 calc R . . . .
C16 C 0.71572(15) 0.64709(11) 0.82028(11) 0.0204(4) Uani 1 1 d . . . . .
H16 H 0.762474 0.687198 0.794947 0.025 Uiso 1 1 calc R . . . .
C25 C 0.25746(16) 0.77022(11) 0.66057(12) 0.0216(4) Uani 1 1 d . . . . .
H25 H 0.234629 0.809945 0.702790 0.026 Uiso 1 1 calc R . . . .
C7 C 0.53094(15) 0.65549(11) 0.32030(12) 0.0211(4) Uani 1 1 d . . . . .
H7 H 0.514074 0.616473 0.266234 0.025 Uiso 1 1 calc R . . . .
C17 C 0.76405(15) 0.61943(11) 0.91652(12) 0.0214(4) Uani 1 1 d . . . . .
H17 H 0.842881 0.641534 0.956904 0.026 Uiso 1 1 calc R . . . .
C31 C 0.75409(17) 0.52806(12) 1.05567(12) 0.0244(4) Uani 1 1 d . . . . .
H31 H 0.832469 0.552955 1.093207 0.029 Uiso 1 1 calc R . . . .
C30 C 1.17853(16) 0.47978(12) 0.66435(13) 0.0269(4) Uani 1 1 d . . . . .
H30A H 1.154334 0.490371 0.594001 0.040 Uiso 1 1 calc GR . . . .
H30B H 1.249035 0.438026 0.683935 0.040 Uiso 1 1 calc GR . . . .
H30C H 1.203967 0.535708 0.699295 0.040 Uiso 1 1 calc GR . . . .
C29 C 0.74462(16) 0.84067(12) 0.62311(12) 0.0245(4) Uani 1 1 d . . . . .
H29A H 0.793687 0.851765 0.579301 0.037 Uiso 1 1 calc GR . . . .
H29B H 0.771416 0.784632 0.657490 0.037 Uiso 1 1 calc GR . . . .
H29C H 0.758406 0.888867 0.670590 0.037 Uiso 1 1 calc GR . . . .
C27 C -0.03454(16) 0.76899(12) 0.45650(12) 0.0240(4) Uani 1 1 d . . . . .
H27A H 0.006489 0.789308 0.410029 0.036 Uiso 1 1 calc GR . . . .
H27B H -0.110735 0.804005 0.448379 0.036 Uiso 1 1 calc GR . . . .
H27C H -0.057235 0.706487 0.444501 0.036 Uiso 1 1 calc GR . . . .


_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
O2 C24 1.3708(19) . ?
O2 C27 1.433(2) . ?
O3 C12 1.3627(19) . ?
O3 C30 1.435(2) . ?
O1 C31 1.204(2) . ?
C22 C21 1.396(2) . ?
C22 C23 1.394(2) . ?
C11 C12 1.388(2) . ?
C11 C10 1.389(2) . ?
C3 C4 1.409(2) . ?
C3 C2 1.500(2) . ?
C3 C8 1.402(2) . ?
C14 C9 1.404(2) . ?
C14 C13 1.381(2) . ?
C24 C23 1.392(2) . ?
C24 C25 1.396(2) . ?
C26 C21 1.403(2) . ?
C26 C25 1.384(2) . ?
C12 C13 1.402(2) . ?
C21 C1 1.491(2) . ?
C15 C1 1.497(2) . ?
C15 C20 1.402(2) . ?
C15 C16 1.394(2) . ?
C1 C2 1.358(2) . ?
C9 C2 1.497(2) . ?
C9 C10 1.391(2) . ?
C4 C5 1.401(2) . ?
C4 C28 1.512(2) . ?
C18 C19 1.398(2) . ?
C18 C17 1.392(2) . ?
C18 C31 1.479(2) . ?
C20 C19 1.384(2) . ?
C5 C6 1.384(2) . ?
C28 C29 1.529(2) . ?
C6 C7 1.385(2) . ?
C8 C7 1.387(2) . ?
C16 C17 1.388(2) . ?

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
C24 O2 C27 116.53(12) . . ?
C12 O3 C30 116.45(13) . . ?
C23 C22 C21 121.67(15) . . ?
C12 C11 C10 119.62(15) . . ?
C4 C3 C2 122.41(14) . . ?
C8 C3 C4 118.71(14) . . ?
C8 C3 C2 118.59(14) . . ?
C13 C14 C9 121.27(15) . . ?
O2 C24 C23 124.54(14) . . ?
O2 C24 C25 115.98(14) . . ?
C23 C24 C25 119.48(15) . . ?
C25 C26 C21 121.66(15) . . ?
O3 C12 C11 124.80(14) . . ?
O3 C12 C13 115.99(14) . . ?
C11 C12 C13 119.18(14) . . ?
C22 C21 C26 117.38(14) . . ?
C22 C21 C1 122.10(14) . . ?
C26 C21 C1 120.46(14) . . ?
C20 C15 C1 120.31(14) . . ?
C16 C15 C1 121.06(14) . . ?
C16 C15 C20 118.62(14) . . ?
C24 C23 C22 119.79(15) . . ?
C21 C1 C15 114.99(13) . . ?
C2 C1 C21 123.37(14) . . ?
C2 C1 C15 121.64(14) . . ?
C14 C9 C2 122.20(14) . . ?
C10 C9 C14 117.24(14) . . ?
C10 C9 C2 120.52(14) . . ?
C3 C4 C28 122.78(14) . . ?
C5 C4 C3 118.42(15) . . ?
C5 C4 C28 118.73(14) . . ?
C19 C18 C31 121.31(15) . . ?
C17 C18 C19 119.48(15) . . ?
C17 C18 C31 119.21(15) . . ?
C19 C20 C15 120.93(15) . . ?
C14 C13 C12 120.37(15) . . ?
C1 C2 C3 123.57(14) . . ?
C1 C2 C9 123.04(14) . . ?
C9 C2 C3 113.38(13) . . ?
C11 C10 C9 122.28(15) . . ?
C6 C5 C4 122.05(15) . . ?
C20 C19 C18 119.85(15) . . ?
C4 C28 C29 113.29(13) . . ?
C5 C6 C7 119.57(15) . . ?
C7 C8 C3 121.77(15) . . ?
C17 C16 C15 120.58(15) . . ?
C26 C25 C24 120.02(15) . . ?
C6 C7 C8 119.46(15) . . ?
C16 C17 C18 120.39(15) . . ?
O1 C31 C18 124.97(16) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.442
_oxdiff_exptl_absorpt_empirical_full_min 0.646
####################################################################### 
# 
# 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_pka730_pd_auto_1
_database_code_depnum_ccdc_archive 'CCDC 2265650'
loop_
_audit_author_name
_audit_author_address
'KAKOLI MAJI'
;INDIAN INSTITUTE OF SCIENCE EDUCATION AND RESEARCH KOLKATA
India
;
_audit_update_record             
;
2023-05-26 deposited with the CCDC.	2023-09-07 downloaded from the CCDC.
;
_audit_creation_date             2023-05-26
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 Cl2 N2 Pd'
_chemical_formula_sum            'C30 H22 Cl2 N2 Pd'
_chemical_formula_weight         587.79
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Pd Cl'
_chemical_oxdiff_usercomment     100K
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'
Pd Pd -0.9988 1.0072 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.6299(2)
_cell_length_b                   8.9441(2)
_cell_length_c                   10.0875(2)
_cell_angle_alpha                97.816(2)
_cell_angle_beta                 106.126(2)
_cell_angle_gamma                102.556(2)
_cell_volume                     631.18(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6289
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      26.5100
_cell_measurement_theta_min      2.1400
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.909
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10383
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.990
_diffrn_reflns_theta_min         2.149
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  76.00   0.50    0.70    --   12.13  57.00-120.00  164
  2  ω    -13.00  62.00   0.50    0.70    --   12.13  77.00-180.00  150
  3  ω    -10.00  44.00   0.50    0.70    --   12.13  54.00-176.00  108
  4  ω    -15.00  11.00   0.50    0.70    --   12.13 -38.00 -30.00   52
  5  ω    -52.00  18.00   0.50    0.70    --   12.13 -38.00 -60.00  140
  6  ω    -46.00 -20.00   0.50    0.70    --   12.13 -38.00 -30.00   52
  7  ω    -45.00 -12.00   0.50    0.70    --   12.13 -54.00  39.00   66
  8  ω    -23.00  19.00   0.50    0.70    --   12.13 -38.00  60.00   84
  9  ω    -29.00   5.00   0.50    0.70    --   12.13 -19.00  90.00   68
 10  ω    -61.00 -36.00   0.50    0.70    --   12.13 -19.00  90.00   50
 11  ω    -62.00 -17.00   0.50    0.70    --   12.13 -19.00  60.00   90
 12  ω    -45.00 -10.00   0.50    0.70    --   12.13 -19.00 -30.00   70
 13  ω    -15.00  11.00   0.50    0.70    --  -12.09 -57.00   0.00   52
 14  ω    -80.00 -13.00   0.50    0.70    --  -12.09 -54.00  39.00  134
 15  ω    -75.00 -30.00   0.50    0.70    --  -12.09 -57.00   0.00   90
 16  ω     -6.00  49.00   0.50    0.70    --  -12.09  54.00-176.00  110
 17  ω    -21.00  23.00   0.50    0.70    --  -12.09 -99.00  30.00   88
 18  ω     -8.00  18.00   0.50    0.70    --  -12.09 -99.00 -90.00   52
 19  ω    -20.00   9.00   0.50    0.70    --  -12.09 -99.00-150.00   58
 20  ω    -20.00  18.00   0.50    0.70    --  -12.09 -99.00 -30.00   76
 21  ω    -15.00  21.00   0.50    0.70    --  -12.09 -99.00 120.00   72
 22  ω     16.00  48.00   0.50    0.70    --   12.13-125.00  60.00   64
 23  ω     13.00  43.00   0.50    0.70    --   12.13-125.00   0.00   60
 24  ω     13.00  61.00   0.50    0.70    --   12.13-125.00 -60.00   96
 25  ω    -20.00  19.00   0.50    0.70    --   12.13 -99.00 -90.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0908406000
_diffrn_orient_matrix_UB_12      -0.0533004000
_diffrn_orient_matrix_UB_13      -0.0182692000
_diffrn_orient_matrix_UB_21      -0.0261398000
_diffrn_orient_matrix_UB_22      0.0523484000
_diffrn_orient_matrix_UB_23      0.0455487000
_diffrn_orient_matrix_UB_31      -0.0339796000
_diffrn_orient_matrix_UB_32      0.0363668000
_diffrn_orient_matrix_UB_33      -0.0565228000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2456
_reflns_number_total             2627
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2627
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0402
_refine_ls_restrained_S_all      1.072
_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)+(0.0291P)²+0.7477P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0883
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C11(H11), C12(H12), C13(H13), C14(H14), C3(H3), C1(H1), C15(H15),
 C5(H5), C2(H2), C4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Pd1 Pd 0.500000 0.000000 0.500000 0.02181(12) Uani 1 2 d S T P . .
Cl1 Cl 0.56008(14) 0.12088(10) 0.72938(9) 0.0359(2) Uani 1 1 d . . . . .
N1 N 0.5409(4) 0.2055(3) 0.4478(3) 0.0264(6) Uani 1 1 d . . . . .
C10 C 0.7951(4) 0.5907(4) 0.4869(4) 0.0246(7) Uani 1 1 d . . . . .
C9 C 0.5800(5) 0.3206(4) 0.4134(4) 0.0261(7) Uani 1 1 d . . . . .
C6 C 0.3919(5) 0.3846(4) 0.1338(3) 0.0259(7) Uani 1 1 d . . . . .
C7 C 0.5446(5) 0.4956(4) 0.2517(4) 0.0293(8) Uani 1 1 d . . . . .
H7 H 0.582559 0.598688 0.236671 0.035 Uiso 1 1 calc R . . . .
C8 C 0.6377(5) 0.4717(4) 0.3773(4) 0.0275(7) Uani 1 1 d . . . . .
C11 C 0.8538(5) 0.5686(4) 0.6247(4) 0.0300(8) Uani 1 1 d . . . . .
H11 H 0.791519 0.476784 0.648255 0.036 Uiso 1 1 calc R . . . .
C12 C 1.0017(5) 0.6788(5) 0.7274(4) 0.0374(9) Uani 1 1 d . . . . .
H12 H 1.037621 0.663925 0.821646 0.045 Uiso 1 1 calc R . . . .
C13 C 1.0969(5) 0.8097(4) 0.6942(4) 0.0354(9) Uani 1 1 d . . . . .
H13 H 1.200058 0.884289 0.764800 0.043 Uiso 1 1 calc R . . . .
C14 C 1.0424(5) 0.8320(4) 0.5587(4) 0.0326(8) Uani 1 1 d . . . . .
H14 H 1.108920 0.922513 0.535949 0.039 Uiso 1 1 calc R . . . .
C3 C 0.0911(6) 0.1874(5) -0.0897(4) 0.0406(10) Uani 1 1 d . . . . .
H3 H -0.013460 0.119310 -0.164115 0.049 Uiso 1 1 calc R . . . .
C1 C 0.3652(6) 0.2226(4) 0.1084(4) 0.0354(9) Uani 1 1 d . . . . .
H1 H 0.450923 0.178361 0.167777 0.042 Uiso 1 1 calc R . . . .
C15 C 0.8934(5) 0.7261(4) 0.4554(4) 0.0314(8) Uani 1 1 d . . . . .
H15 H 0.856623 0.744386 0.362289 0.038 Uiso 1 1 calc R . . . .
C5 C 0.2707(5) 0.4485(4) 0.0415(4) 0.0319(8) Uani 1 1 d . . . . .
H5 H 0.291387 0.558866 0.053745 0.038 Uiso 1 1 calc R . . . .
C2 C 0.2167(6) 0.1275(5) -0.0013(4) 0.0420(10) Uani 1 1 d . . . . .
H2 H 0.199848 0.017412 -0.016698 0.050 Uiso 1 1 calc R . . . .
C4 C 0.1180(5) 0.3482(5) -0.0697(4) 0.0400(9) Uani 1 1 d . . . . .
H4 H 0.032612 0.390557 -0.131464 0.048 Uiso 1 1 calc R . . . .


_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
Pd1 Cl1 2.2908(9) 2_656 ?
Pd1 Cl1 2.2908(9) . ?
Pd1 N1 1.964(3) . ?
Pd1 N1 1.964(3) 2_656 ?
N1 C9 1.136(4) . ?
C10 C8 1.478(4) . ?
C10 C11 1.393(5) . ?
C10 C15 1.404(4) . ?
C9 C8 1.455(4) . ?
C6 C7 1.471(5) . ?
C6 C1 1.396(5) . ?
C6 C5 1.395(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.340(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.381(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.372(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.370(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.372(5) . ?
C3 H3 0.9500 . ?
C3 C2 1.371(6) . ?
C3 C4 1.386(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.364(5) . ?
C15 H15 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.402(5) . ?
C2 H2 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
Cl1 Pd1 Cl1 180.00(4) 2_656 . ?
N1 Pd1 Cl1 89.74(8) . . ?
N1 Pd1 Cl1 89.74(8) 2_656 2_656 ?
N1 Pd1 Cl1 90.26(8) . 2_656 ?
N1 Pd1 Cl1 90.26(8) 2_656 . ?
N1 Pd1 N1 180.0 . 2_656 ?
C9 N1 Pd1 172.7(3) . . ?
C11 C10 C8 120.3(3) . . ?
C11 C10 C15 118.0(3) . . ?
C15 C10 C8 121.6(3) . . ?
N1 C9 C8 176.7(4) . . ?
C1 C6 C7 124.1(3) . . ?
C5 C6 C7 116.7(3) . . ?
C5 C6 C1 119.2(3) . . ?
C6 C7 H7 115.5 . . ?
C8 C7 C6 129.0(3) . . ?
C8 C7 H7 115.5 . . ?
C9 C8 C10 116.1(3) . . ?
C7 C8 C10 124.6(3) . . ?
C7 C8 C9 119.2(3) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.5(4) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(3) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.2(3) . . ?
C15 C14 H14 119.4 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.4(3) . . ?
C4 C3 H3 120.3 . . ?
C6 C1 H1 119.8 . . ?
C2 C1 C6 120.3(4) . . ?
C2 C1 H1 119.8 . . ?
C10 C15 H15 119.9 . . ?
C14 C15 C10 120.1(3) . . ?
C14 C15 H15 119.9 . . ?
C6 C5 H5 120.4 . . ?
C6 C5 C4 119.3(3) . . ?
C4 C5 H5 120.4 . . ?
C3 C2 H2 119.3 . . ?
C1 C2 C3 121.4(4) . . ?
C1 C2 H2 119.3 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.307
_oxdiff_exptl_absorpt_empirical_full_min 0.742
####################################################################### 
# 
# 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_pka_538a_auto_1
_database_code_depnum_ccdc_archive 'CCDC 2232806'
loop_
_audit_author_name
_audit_author_address
'KAKOLI MAJI'
;INDIAN INSTITUTE OF SCIENCE EDUCATION AND RESEARCH KOLKATA
India
;
_audit_update_record             
;
2022-12-26 deposited with the CCDC.	2023-09-07 downloaded from the CCDC.
;
_audit_creation_date             2022-12-26
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H28 O3'
_chemical_formula_sum            'C31 H28 O3'
_chemical_formula_weight         448.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O'
_chemical_oxdiff_usercomment     100K
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'
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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.9595(4)
_cell_length_b                   15.8984(5)
_cell_length_c                   14.7337(5)
_cell_angle_alpha                90
_cell_angle_beta                 111.118(4)
_cell_angle_gamma                90
_cell_volume                     2394.77(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19629
_cell_measurement_temperature    113(18)
_cell_measurement_theta_max      26.8870
_cell_measurement_theta_min      1.9500
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.962
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29857
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.067
_diffrn_reflns_theta_min         1.959
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      113(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00  18.00   0.50   10.50    --  -12.09 -84.00-143.00  122
  2  ω    -42.00  22.00   0.50   10.50    --  -12.09  84.00 -23.00  128
  3  ω    -38.00  58.00   0.50   10.50    --  -12.09  71.00-132.00  192
  4  ω    -38.00  58.00   0.50   10.50    --  -12.09  68.00  99.00  192
  5  ω    -23.00  23.00   0.50   10.50    --  -12.09 -99.00 120.00   92
  6  ω    -23.00  23.00   0.50   10.50    --  -12.09 -99.00  60.00   92
  7  ω    -23.00  23.00   0.50   10.50    --  -12.09 -99.00 -30.00   92
  8  ω    -23.00  23.00   0.50   10.50    --  -12.09 -99.00 -60.00   92
  9  ω    -23.00  23.00   0.50   10.50    --  -12.09 -99.00-150.00   92
 10  ω     12.00  62.00   0.50   10.50    --   12.13-125.00 120.00  100
 11  ω     12.00  62.00   0.50   10.50    --   12.13-125.00-120.00  100
 12  ω    -62.00   5.00   0.50   10.50    --   12.13 -19.00 -90.00  134
 13  ω    -86.00 -49.00   0.50   10.50    --  -12.09 -19.00 -60.00   74
 14  ω    -15.00  86.00   0.50   10.50    --   12.13  19.00 -90.00  202
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0116373000
_diffrn_orient_matrix_UB_12      0.0329321000
_diffrn_orient_matrix_UB_13      -0.0345252000
_diffrn_orient_matrix_UB_21      -0.0669063000
_diffrn_orient_matrix_UB_22      -0.0116404000
_diffrn_orient_matrix_UB_23      -0.0202606000
_diffrn_orient_matrix_UB_31      -0.0142493000
_diffrn_orient_matrix_UB_32      0.0277735000
_diffrn_orient_matrix_UB_33      0.0325657000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4102
_reflns_number_total             5010
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5010
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0428
_refine_ls_restrained_S_all      1.047
_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)+(0.0537P)²+0.9666P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1177
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C10(H10), C13(H13), C4(H4), C11(H11), C5(H5), C14(H14), C22(H22),
 C26(H26), C7(H7), C16(H16), C8(H8), C18(H18), C17(H17), C25(H25), C27(H27)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C29(H29A,H29B,
 H29C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 -0.08211(10) 0.57135(7) 0.32306(7) 0.0279(2) Uani 1 1 d . . . . .
O2 O 0.95344(10) 0.22885(7) 0.43137(7) 0.0300(2) Uani 1 1 d . . . . .
O3 O 0.30077(11) 0.48118(8) -0.12206(8) 0.0382(3) Uani 1 1 d . . . . .
C12 C 0.02141(13) 0.51847(9) 0.33572(9) 0.0222(3) Uani 1 1 d . . . . .
C2 C 0.44397(14) 0.36800(9) 0.33138(10) 0.0227(3) Uani 1 1 d . . . . .
C23 C 0.80279(14) 0.31834(9) 0.47716(10) 0.0245(3) Uani 1 1 d . . . . .
H23 H 0.867824 0.332439 0.538062 0.029 Uiso 1 1 calc R . . . .
C21 C 0.57838(14) 0.33114(9) 0.36247(10) 0.0227(3) Uani 1 1 d . . . . .
C15 C 0.41580(13) 0.33422(9) 0.48895(10) 0.0239(3) Uani 1 1 d . . . . .
C3 C 0.38779(14) 0.39197(9) 0.22565(10) 0.0229(3) Uani 1 1 d . . . . .
C24 C 0.83276(14) 0.26455(9) 0.41352(10) 0.0242(3) Uani 1 1 d . . . . .
C9 C 0.24894(14) 0.42296(9) 0.36437(10) 0.0219(3) Uani 1 1 d . . . . .
C10 C 0.23088(13) 0.50228(9) 0.31904(10) 0.0227(3) Uani 1 1 d . . . . .
H10 H 0.296535 0.523888 0.297413 0.027 Uiso 1 1 calc R . . . .
C13 C 0.03437(14) 0.43883(9) 0.37746(10) 0.0239(3) Uani 1 1 d . . . . .
H13 H -0.033626 0.416085 0.395684 0.029 Uiso 1 1 calc R . . . .
C1 C 0.37408(14) 0.37500(9) 0.39019(10) 0.0229(3) Uani 1 1 d . . . . .
C4 C 0.45405(14) 0.44742(9) 0.18556(10) 0.0234(3) Uani 1 1 d . . . . .
H4 H 0.533650 0.472442 0.226323 0.028 Uiso 1 1 calc R . . . .
C11 C 0.11969(14) 0.54945(9) 0.30532(10) 0.0236(3) Uani 1 1 d . . . . .
H11 H 0.110087 0.603088 0.275121 0.028 Uiso 1 1 calc R . . . .
C5 C 0.40476(14) 0.46618(9) 0.08712(10) 0.0249(3) Uani 1 1 d . . . . .
H5 H 0.448718 0.505602 0.061249 0.030 Uiso 1 1 calc R . . . .
C14 C 0.14810(14) 0.39290(9) 0.39220(10) 0.0242(3) Uani 1 1 d . . . . .
H14 H 0.157313 0.339216 0.422261 0.029 Uiso 1 1 calc R . . . .
C22 C 0.67709(14) 0.35138(9) 0.45117(10) 0.0239(3) Uani 1 1 d . . . . .
H22 H 0.657804 0.388564 0.494666 0.029 Uiso 1 1 calc R . . . .
C26 C 0.61193(14) 0.27711(9) 0.29975(10) 0.0258(3) Uani 1 1 d . . . . .
H26 H 0.547207 0.262640 0.238851 0.031 Uiso 1 1 calc R . . . .
C7 C 0.22470(14) 0.37117(9) 0.06480(10) 0.0266(3) Uani 1 1 d . . . . .
H7 H 0.147043 0.344446 0.023440 0.032 Uiso 1 1 calc R . . . .
C16 C 0.45839(14) 0.38506(9) 0.57246(10) 0.0262(3) Uani 1 1 d . . . . .
H16 H 0.464039 0.444252 0.566087 0.031 Uiso 1 1 calc R . . . .
C8 C 0.27214(14) 0.35424(9) 0.16385(10) 0.0260(3) Uani 1 1 d . . . . .
H8 H 0.225806 0.316739 0.189993 0.031 Uiso 1 1 calc R . . . .
C6 C 0.29030(14) 0.42712(9) 0.02573(10) 0.0247(3) Uani 1 1 d . . . . .
C20 C 0.40267(14) 0.24686(9) 0.49782(11) 0.0265(3) Uani 1 1 d . . . . .
C19 C 0.43559(14) 0.21111(9) 0.59193(11) 0.0283(3) Uani 1 1 d . . . . .
C18 C 0.48014(15) 0.26313(10) 0.67307(11) 0.0292(3) Uani 1 1 d . . . . .
H18 H 0.502803 0.239072 0.736027 0.035 Uiso 1 1 calc R . . . .
C17 C 0.49236(14) 0.34937(10) 0.66439(11) 0.0283(3) Uani 1 1 d . . . . .
H17 H 0.523681 0.383732 0.720851 0.034 Uiso 1 1 calc R . . . .
C25 C 0.73669(15) 0.24436(9) 0.32419(10) 0.0272(3) Uani 1 1 d . . . . .
H25 H 0.756851 0.208200 0.280203 0.033 Uiso 1 1 calc R . . . .
C27 C 0.24250(15) 0.44103(10) -0.08039(11) 0.0288(3) Uani 1 1 d . . . . .
H27 H 0.160756 0.416978 -0.118636 0.035 Uiso 1 1 calc R . . . .
C28 C -0.18708(15) 0.53872(11) 0.34913(11) 0.0317(3) Uani 1 1 d . . . . .
H28A H -0.221941 0.487704 0.311357 0.048 Uiso 1 1 calc GR . . . .
H28B H -0.256578 0.580962 0.335143 0.048 Uiso 1 1 calc GR . . . .
H28C H -0.154434 0.525216 0.418696 0.048 Uiso 1 1 calc GR . . . .
C30 C 0.34991(17) 0.19138(10) 0.40951(11) 0.0332(4) Uani 1 1 d . . . . .
H30A H 0.317298 0.226388 0.350922 0.050 Uiso 1 1 calc GR . . . .
H30B H 0.278307 0.156945 0.414302 0.050 Uiso 1 1 calc GR . . . .
H30C H 0.419768 0.154651 0.405773 0.050 Uiso 1 1 calc GR . . . .
C31 C 1.04462(15) 0.23124(11) 0.52933(11) 0.0323(4) Uani 1 1 d . . . . .
H31A H 1.123912 0.200354 0.533672 0.049 Uiso 1 1 calc GR . . . .
H31B H 1.005262 0.205200 0.572530 0.049 Uiso 1 1 calc GR . . . .
H31C H 1.067186 0.289820 0.548948 0.049 Uiso 1 1 calc GR . . . .
C29 C 0.41943(18) 0.11808(10) 0.60429(13) 0.0404(4) Uani 1 1 d . . . . .
H29A H 0.326562 0.103214 0.575623 0.061 Uiso 1 1 calc GR . . . .
H29B H 0.452730 0.104056 0.673721 0.061 Uiso 1 1 calc GR . . . .
H29C H 0.468501 0.086528 0.571551 0.061 Uiso 1 1 calc GR . . . .


_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 C12 1.3698(17) . ?
O1 C28 1.4348(18) . ?
O2 C24 1.3747(17) . ?
O2 C31 1.4297(18) . ?
O3 C27 1.2143(19) . ?
C12 C13 1.392(2) . ?
C12 C11 1.397(2) . ?
C2 C21 1.496(2) . ?
C2 C3 1.5033(19) . ?
C2 C1 1.352(2) . ?
C23 C24 1.393(2) . ?
C23 C22 1.393(2) . ?
C21 C22 1.401(2) . ?
C21 C26 1.404(2) . ?
C15 C1 1.5058(19) . ?
C15 C16 1.404(2) . ?
C15 C20 1.407(2) . ?
C3 C4 1.401(2) . ?
C3 C8 1.401(2) . ?
C24 C25 1.395(2) . ?
C9 C10 1.4073(19) . ?
C9 C1 1.4937(19) . ?
C9 C14 1.394(2) . ?
C10 C11 1.382(2) . ?
C13 C14 1.393(2) . ?
C4 C5 1.3856(19) . ?
C5 C6 1.400(2) . ?
C26 C25 1.384(2) . ?
C7 C8 1.388(2) . ?
C7 C6 1.392(2) . ?
C16 C17 1.390(2) . ?
C6 C27 1.476(2) . ?
C20 C19 1.420(2) . ?
C20 C30 1.504(2) . ?
C19 C18 1.390(2) . ?
C19 C29 1.508(2) . ?
C18 C17 1.388(2) . ?

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
C12 O1 C28 116.51(11) . . ?
C24 O2 C31 117.16(11) . . ?
O1 C12 C13 124.47(13) . . ?
O1 C12 C11 115.88(12) . . ?
C13 C12 C11 119.64(13) . . ?
C21 C2 C3 114.03(11) . . ?
C1 C2 C21 123.98(13) . . ?
C1 C2 C3 121.88(13) . . ?
C22 C23 C24 119.74(13) . . ?
C22 C21 C2 122.68(13) . . ?
C22 C21 C26 117.20(13) . . ?
C26 C21 C2 120.04(12) . . ?
C16 C15 C1 119.23(13) . . ?
C16 C15 C20 119.97(13) . . ?
C20 C15 C1 120.60(13) . . ?
C4 C3 C2 121.03(13) . . ?
C4 C3 C8 118.71(13) . . ?
C8 C3 C2 120.11(13) . . ?
O2 C24 C23 124.65(13) . . ?
O2 C24 C25 115.64(13) . . ?
C23 C24 C25 119.71(13) . . ?
C10 C9 C1 122.52(12) . . ?
C14 C9 C10 117.12(13) . . ?
C14 C9 C1 120.16(12) . . ?
C11 C10 C9 121.43(13) . . ?
C12 C13 C14 119.28(13) . . ?
C2 C1 C15 122.61(13) . . ?
C2 C1 C9 123.99(13) . . ?
C9 C1 C15 113.40(11) . . ?
C5 C4 C3 120.73(13) . . ?
C10 C11 C12 120.19(13) . . ?
C4 C5 C6 120.10(13) . . ?
C13 C14 C9 122.28(13) . . ?
C23 C22 C21 121.65(13) . . ?
C25 C26 C21 121.82(13) . . ?
C8 C7 C6 120.35(13) . . ?
C17 C16 C15 120.45(14) . . ?
C7 C8 C3 120.58(13) . . ?
C5 C6 C27 120.77(13) . . ?
C7 C6 C5 119.49(13) . . ?
C7 C6 C27 119.66(13) . . ?
C15 C20 C19 119.17(13) . . ?
C15 C20 C30 121.24(13) . . ?
C19 C20 C30 119.55(13) . . ?
C20 C19 C29 120.72(14) . . ?
C18 C19 C20 119.27(14) . . ?
C18 C19 C29 119.99(14) . . ?
C17 C18 C19 121.63(14) . . ?
C18 C17 C16 119.48(14) . . ?
C26 C25 C24 119.87(13) . . ?
O3 C27 C6 124.32(14) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.340
_oxdiff_exptl_absorpt_empirical_full_min 0.715
