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

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

data_lk31212nd
_audit_block_doi                 10.5517/ccdc.csd.cc26sbq2
_database_code_depnum_ccdc_archive 'CCDC 2049184'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/adsc.202100491 2021
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi '
;Aix Marseille University
France
;
_audit_update_record             
;
2020-12-08 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2020-07-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H41 Cl N2 Pd'
_chemical_formula_sum            'C38 H41 Cl N2 Pd'
_chemical_formula_weight         667.58
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   16.3085(4)
_cell_length_b                   10.0558(2)
_cell_length_c                   23.0623(5)
_cell_angle_alpha                90
_cell_angle_beta                 110.063(2)
_cell_angle_gamma                90
_cell_volume                     3552.59(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25013
_cell_measurement_temperature    295
_cell_measurement_theta_max      28.4040
_cell_measurement_theta_min      3.7720
_shelx_estimated_absorpt_T_max   0.907
_shelx_estimated_absorpt_T_min   0.845
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40605
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.336
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  83.00   1.00   10.00    --    9.90  64.00 -79.00  103
  2  ω    -63.00  40.00   1.00   10.00    --    9.90 -64.00 144.00  103
  3  ω    -20.00  31.00   1.00   10.00    --   -9.59 -99.00  60.00   51
  4  ω    -84.00  15.00   1.00   10.00    --   -9.59 -38.00  30.00   99
  5  ω    -70.00  51.00   1.00   10.00    --    9.90 -19.00  90.00  121
  6  ω    -20.00  51.00   1.00   10.00    --    9.90 -99.00  30.00   71
  7  ω    -15.00  84.00   1.00   10.00    --    9.90  38.00-150.00   99
  8  ω    -15.00  84.00   1.00   10.00    --    9.90  38.00  90.00   99
  9  ω    -20.00  51.00   1.00   10.00    --    9.90 -99.00  90.00   71
 10  ω    -20.00   7.00   1.00   10.00    --    9.90 -99.00-120.00   27
 11  ω    -20.00  51.00   1.00   10.00    --    9.90 -99.00 -60.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0191894000
_diffrn_orient_matrix_UB_12      -0.0406312000
_diffrn_orient_matrix_UB_13      0.0170050000
_diffrn_orient_matrix_UB_21      -0.0104852000
_diffrn_orient_matrix_UB_22      0.0575158000
_diffrn_orient_matrix_UB_23      0.0138492000
_diffrn_orient_matrix_UB_31      -0.0408144000
_diffrn_orient_matrix_UB_32      0.0043483000
_diffrn_orient_matrix_UB_33      -0.0243066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                7033
_reflns_number_total             7195
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_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    ?
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.009(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7195
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0207
_refine_ls_restrained_S_all      1.049
_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)+(0.0301P)²+0.9691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0530
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.009(19)
 -0.009(19)
2. 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
3.a Riding coordinates:
 C36(H36A,H36B), C37(H37), C38(H38A,H38B)
3.b Ternary CH refined with riding coordinates:
 C14(H14)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C31(H31)
3.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.25625(2) 0.61284(2) 0.29414(2) 0.04216(7) Uani 1 1 d . . . . .
Cl1 Cl 0.37275(5) 0.74570(9) 0.28756(5) 0.0642(2) Uani 1 1 d . . . . .
N1 N 0.09881(13) 0.7961(2) 0.24188(10) 0.0354(4) Uani 1 1 d . . . . .
N2 N 0.18256(13) 0.8699(2) 0.32912(9) 0.0357(4) Uani 1 1 d . . . . .
C1 C 0.17418(19) 0.7680(3) 0.28854(13) 0.0353(6) Uani 1 1 d . . . . .
C2 C 0.11288(18) 0.9589(3) 0.30820(12) 0.0412(6) Uani 1 1 d . . . . .
C3 C 0.06022(17) 0.9124(3) 0.25363(12) 0.0413(6) Uani 1 1 d . . . . .
C4 C 0.1041(2) 1.0795(3) 0.34316(16) 0.0614(9) Uani 1 1 d . . . . .
H4A H 0.120237 1.058095 0.386199 0.092 Uiso 1 1 calc GR . . . .
H4B H 0.044685 1.109865 0.327962 0.092 Uiso 1 1 calc GR . . . .
H4C H 0.141701 1.148348 0.337845 0.092 Uiso 1 1 calc GR . . . .
C5 C -0.0227(2) 0.9694(4) 0.20899(14) 0.0587(8) Uani 1 1 d . . . . .
H5A H -0.011561 1.004622 0.173725 0.088 Uiso 1 1 calc GR . . . .
H5B H -0.043423 1.039163 0.228813 0.088 Uiso 1 1 calc GR . . . .
H5C H -0.066086 0.900707 0.195939 0.088 Uiso 1 1 calc GR . . . .
C6 C 0.05636(16) 0.7041(3) 0.19281(11) 0.0360(5) Uani 1 1 d . . . . .
C7 C 0.08405(15) 0.6919(2) 0.14190(11) 0.0331(5) Uani 1 1 d . . . . .
C8 C 0.03985(14) 0.6022(3) 0.09641(10) 0.0372(5) Uani 1 1 d . . . . .
H8 H 0.056452 0.593584 0.061836 0.045 Uiso 1 1 calc R . . . .
C9 C -0.02914(16) 0.5239(3) 0.10056(13) 0.0404(6) Uani 1 1 d . . . . .
C10 C -0.05277(18) 0.5371(3) 0.15196(14) 0.0481(7) Uani 1 1 d . . . . .
H10 H -0.097843 0.484864 0.155527 0.058 Uiso 1 1 calc R . . . .
C11 C -0.01123(15) 0.6264(4) 0.19882(12) 0.0461(6) Uani 1 1 d . . . . .
C12 C -0.0769(2) 0.4270(3) 0.05020(15) 0.0539(7) Uani 1 1 d . . . . .
H12A H -0.120808 0.473520 0.017874 0.081 Uiso 1 1 calc GR . . . .
H12B H -0.103898 0.359490 0.066947 0.081 Uiso 1 1 calc GR . . . .
H12C H -0.036184 0.386499 0.033787 0.081 Uiso 1 1 calc GR . . . .
C13 C -0.0375(2) 0.6327(5) 0.25573(15) 0.0665(10) Uani 1 1 d . . . . .
H13A H 0.010543 0.665269 0.289999 0.100 Uiso 1 1 calc GR . . . .
H13B H -0.053244 0.545304 0.265070 0.100 Uiso 1 1 calc GR . . . .
H13C H -0.086528 0.691329 0.248170 0.100 Uiso 1 1 calc GR . . . .
C14 C 0.16198(15) 0.7727(3) 0.13896(11) 0.0326(5) Uani 1 1 d . . . . .
H14 H 0.208065 0.760471 0.179129 0.039 Uiso 1 1 calc R . . . .
C15 C 0.20011(15) 0.7226(2) 0.09116(11) 0.0340(5) Uani 1 1 d . . . . .
C16 C 0.1724(2) 0.7667(3) 0.03080(13) 0.0474(6) Uani 1 1 d . . . . .
H16 H 0.128068 0.829640 0.017813 0.057 Uiso 1 1 calc R . . . .
C17 C 0.2100(2) 0.7182(3) -0.01098(14) 0.0561(8) Uani 1 1 d . . . . .
H17 H 0.190834 0.749614 -0.051355 0.067 Uiso 1 1 calc R . . . .
C18 C 0.27466(18) 0.6249(5) 0.00701(14) 0.0569(8) Uani 1 1 d . . . . .
H18 H 0.299059 0.591717 -0.021040 0.068 Uiso 1 1 calc R . . . .
C19 C 0.3030(2) 0.5812(4) 0.06641(16) 0.0643(10) Uani 1 1 d . . . . .
H19 H 0.347623 0.518619 0.079125 0.077 Uiso 1 1 calc R . . . .
C20 C 0.26588(17) 0.6290(4) 0.10832(13) 0.0520(8) Uani 1 1 d . . . . .
H20 H 0.285785 0.597372 0.148653 0.062 Uiso 1 1 calc R . . . .
C21 C 0.14401(16) 0.9208(3) 0.13299(12) 0.0350(5) Uani 1 1 d . . . . .
C22 C 0.2069(2) 1.0093(3) 0.16800(15) 0.0539(7) Uani 1 1 d . . . . .
H22 H 0.258900 0.977374 0.196010 0.065 Uiso 1 1 calc R . . . .
C23 C 0.1925(3) 1.1439(3) 0.1614(2) 0.0804(12) Uani 1 1 d . . . . .
H23 H 0.235177 1.201815 0.185341 0.096 Uiso 1 1 calc R . . . .
C24 C 0.1175(3) 1.1948(4) 0.1209(2) 0.0776(11) Uani 1 1 d . . . . .
H24 H 0.109065 1.286225 0.116812 0.093 Uiso 1 1 calc R . . . .
C25 C 0.0538(2) 1.1081(5) 0.08589(15) 0.0622(7) Uani 1 1 d . . . . .
H25 H 0.001776 1.141427 0.058355 0.075 Uiso 1 1 calc R . . . .
C26 C 0.06692(19) 0.9727(3) 0.09157(14) 0.0473(6) Uani 1 1 d . . . . .
H26 H 0.023918 0.915359 0.067518 0.057 Uiso 1 1 calc R . . . .
C27 C 0.24718(17) 0.8739(3) 0.39033(11) 0.0371(5) Uani 1 1 d . . . . .
C28 C 0.2354(2) 0.7930(3) 0.43566(13) 0.0477(7) Uani 1 1 d . . . . .
C29 C 0.2960(2) 0.7992(3) 0.49452(14) 0.0539(8) Uani 1 1 d . . . . .
H29 H 0.288681 0.745103 0.525103 0.065 Uiso 1 1 calc R . . . .
C30 C 0.3664(2) 0.8824(3) 0.50920(12) 0.0468(6) Uani 1 1 d . . . . .
C31 C 0.37509(19) 0.9662(3) 0.46351(13) 0.0454(6) Uani 1 1 d . . . . .
H31 H 0.421401 1.025982 0.473581 0.054 Uiso 1 1 calc R . . . .
C32 C 0.31614(17) 0.9629(3) 0.40303(12) 0.0377(5) Uani 1 1 d . . . . .
C33 C 0.1583(3) 0.7013(5) 0.42157(18) 0.0797(12) Uani 1 1 d . . . . .
H33A H 0.105612 0.750427 0.401811 0.120 Uiso 1 1 calc GR . . . .
H33B H 0.156399 0.663241 0.459269 0.120 Uiso 1 1 calc GR . . . .
H33C H 0.163604 0.631581 0.394630 0.120 Uiso 1 1 calc GR . . . .
C34 C 0.4339(2) 0.8849(4) 0.57394(14) 0.0649(9) Uani 1 1 d . . . . .
H34A H 0.406004 0.866112 0.603505 0.097 Uiso 1 1 calc GR . . . .
H34B H 0.460613 0.971208 0.582039 0.097 Uiso 1 1 calc GR . . . .
H34C H 0.477856 0.818966 0.577115 0.097 Uiso 1 1 calc GR . . . .
C35 C 0.3294(2) 1.0512(3) 0.35444(13) 0.0499(7) Uani 1 1 d . . . . .
H35A H 0.355160 1.000724 0.329799 0.075 Uiso 1 1 calc GR . . . .
H35B H 0.367356 1.123437 0.373894 0.075 Uiso 1 1 calc GR . . . .
H35C H 0.274081 1.085909 0.328587 0.075 Uiso 1 1 calc GR . . . .
C36 C 0.3187(3) 0.4205(4) 0.2924(2) 0.0806(13) Uani 1 1 d . . . . .
H36A H 0.306225 0.460627 0.254011 0.097 Uiso 1 1 d R . . . .
H36B H 0.374555 0.388747 0.313461 0.097 Uiso 1 1 d R . . . .
C37 C 0.2530(4) 0.4089(4) 0.3171(3) 0.0926(14) Uani 1 1 d . . . . .
H37 H 0.266214 0.368588 0.355548 0.111 Uiso 1 1 d R . . . .
C38 C 0.1679(3) 0.4520(4) 0.2869(3) 0.0790(14) Uani 1 1 d . . . . .
H38A H 0.153921 0.492467 0.248413 0.095 Uiso 1 1 d R . . . .
H38B H 0.125531 0.442467 0.305133 0.095 Uiso 1 1 d 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 2.3697(9) . ?
Pd1 C1 2.031(3) . ?
Pd1 C36 2.192(4) . ?
Pd1 H36A 2.0931 . ?
Pd1 C37 2.123(4) . ?
Pd1 C38 2.134(5) . ?
Pd1 H38A 2.0384 . ?
N1 C1 1.357(4) . ?
N1 C3 1.398(3) . ?
N1 C6 1.442(3) . ?
N2 C1 1.363(4) . ?
N2 C2 1.396(3) . ?
N2 C27 1.444(3) . ?
C2 C3 1.341(4) . ?
C2 C4 1.490(4) . ?
C3 C5 1.504(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.400(3) . ?
C6 C11 1.396(4) . ?
C7 C8 1.383(4) . ?
C7 C14 1.530(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.403(4) . ?
C9 C10 1.373(4) . ?
C9 C12 1.511(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.390(4) . ?
C11 C13 1.515(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14 0.9800 . ?
C14 C15 1.525(3) . ?
C14 C21 1.515(4) . ?
C15 C16 1.381(4) . ?
C15 C20 1.378(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.395(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.365(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.360(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.391(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.388(4) . ?
C21 C26 1.394(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.373(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.359(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.384(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.377(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.389(4) . ?
C27 C32 1.388(4) . ?
C28 C29 1.379(4) . ?
C28 C33 1.503(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.366(5) . ?
C30 C31 1.394(4) . ?
C30 C34 1.521(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.397(4) . ?
C32 C35 1.502(4) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9303 . ?
C36 H36B 0.9300 . ?
C36 C37 1.379(7) . ?
C37 H37 0.9301 . ?
C37 C38 1.391(7) . ?
C38 H38A 0.9301 . ?
C38 H38B 0.9298 . ?

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 H36A 86.7 . . ?
Cl1 Pd1 H38A 146.5 . . ?
C1 Pd1 Cl1 95.06(8) . . ?
C1 Pd1 C36 167.59(16) . . ?
C1 Pd1 H36A 151.9 . . ?
C1 Pd1 C37 133.29(17) . . ?
C1 Pd1 C38 99.50(12) . . ?
C1 Pd1 H38A 91.1 . . ?
C36 Pd1 Cl1 96.25(14) . . ?
C36 Pd1 H36A 24.9 . . ?
C36 Pd1 H38A 76.7 . . ?
H36A Pd1 H38A 73.2 . . ?
C37 Pd1 Cl1 130.52(15) . . ?
C37 Pd1 C36 37.24(18) . . ?
C37 Pd1 H36A 56.7 . . ?
C37 Pd1 C38 38.15(19) . . ?
C37 Pd1 H38A 58.0 . . ?
C38 Pd1 Cl1 163.08(14) . . ?
C38 Pd1 C36 68.6(2) . . ?
C38 Pd1 H36A 76.4 . . ?
C38 Pd1 H38A 25.6 . . ?
C1 N1 C3 111.4(2) . . ?
C1 N1 C6 123.4(2) . . ?
C3 N1 C6 124.2(2) . . ?
C1 N2 C2 111.5(2) . . ?
C1 N2 C27 124.0(2) . . ?
C2 N2 C27 123.7(2) . . ?
N1 C1 Pd1 127.5(2) . . ?
N1 C1 N2 103.8(2) . . ?
N2 C1 Pd1 128.7(2) . . ?
N2 C2 C4 123.6(2) . . ?
C3 C2 N2 106.5(2) . . ?
C3 C2 C4 129.9(3) . . ?
N1 C3 C5 123.0(2) . . ?
C2 C3 N1 106.7(2) . . ?
C2 C3 C5 130.2(3) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 120.5(2) . . ?
C11 C6 N1 117.6(2) . . ?
C11 C6 C7 121.8(2) . . ?
C6 C7 C14 120.2(2) . . ?
C8 C7 C6 117.3(2) . . ?
C8 C7 C14 122.5(2) . . ?
C7 C8 H8 118.8 . . ?
C7 C8 C9 122.4(2) . . ?
C9 C8 H8 118.8 . . ?
C8 C9 C12 121.5(3) . . ?
C10 C9 C8 118.2(2) . . ?
C10 C9 C12 120.2(3) . . ?
C9 C10 H10 119.1 . . ?
C9 C10 C11 121.9(2) . . ?
C11 C10 H10 119.1 . . ?
C6 C11 C13 122.0(3) . . ?
C10 C11 C6 118.4(2) . . ?
C10 C11 C13 119.5(3) . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C14 H14 105.7 . . ?
C15 C14 C7 114.0(2) . . ?
C15 C14 H14 105.7 . . ?
C21 C14 C7 112.9(2) . . ?
C21 C14 H14 105.7 . . ?
C21 C14 C15 111.9(2) . . ?
C16 C15 C14 123.3(2) . . ?
C20 C15 C14 119.2(2) . . ?
C20 C15 C16 117.5(2) . . ?
C15 C16 H16 119.5 . . ?
C15 C16 C17 121.0(3) . . ?
C17 C16 H16 119.5 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.5(3) . . ?
C18 C17 H17 119.8 . . ?
C17 C18 H18 120.4 . . ?
C19 C18 C17 119.2(3) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.6(3) . . ?
C20 C19 H19 119.7 . . ?
C15 C20 C19 121.2(3) . . ?
C15 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C22 C21 C14 119.8(2) . . ?
C22 C21 C26 118.1(3) . . ?
C26 C21 C14 122.1(2) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.3(3) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 119.1 . . ?
C24 C23 C22 121.8(3) . . ?
C24 C23 H23 119.1 . . ?
C23 C24 H24 120.6 . . ?
C23 C24 C25 118.9(3) . . ?
C25 C24 H24 120.6 . . ?
C24 C25 H25 119.8 . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C21 C26 H26 119.7 . . ?
C25 C26 C21 120.7(3) . . ?
C25 C26 H26 119.7 . . ?
C28 C27 N2 118.5(2) . . ?
C32 C27 N2 119.4(2) . . ?
C32 C27 C28 122.0(2) . . ?
C27 C28 C33 121.2(3) . . ?
C29 C28 C27 118.5(3) . . ?
C29 C28 C33 120.3(3) . . ?
C28 C29 H29 119.0 . . ?
C30 C29 C28 121.9(3) . . ?
C30 C29 H29 119.0 . . ?
C29 C30 C31 118.5(3) . . ?
C29 C30 C34 121.2(3) . . ?
C31 C30 C34 120.3(3) . . ?
C30 C31 H31 119.1 . . ?
C30 C31 C32 121.8(3) . . ?
C32 C31 H31 119.1 . . ?
C27 C32 C31 117.1(2) . . ?
C27 C32 C35 122.5(2) . . ?
C31 C32 C35 120.3(3) . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.5 . . ?
C28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
C30 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Pd1 C36 H36A 71.6 . . ?
Pd1 C36 H36B 132.2 . . ?
H36A C36 H36B 120.0 . . ?
C37 C36 Pd1 68.7(2) . . ?
C37 C36 H36A 118.9 . . ?
C37 C36 H36B 121.1 . . ?
Pd1 C37 H37 129.9 . . ?
C36 C37 Pd1 74.1(2) . . ?
C36 C37 H37 118.1 . . ?
C36 C37 C38 123.3(5) . . ?
C38 C37 Pd1 71.3(3) . . ?
C38 C37 H37 118.6 . . ?
Pd1 C38 H38A 71.4 . . ?
Pd1 C38 H38B 129.0 . . ?
C37 C38 Pd1 70.5(3) . . ?
C37 C38 H38A 119.4 . . ?
C37 C38 H38B 120.6 . . ?
H38A C38 H38B 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 C36 C37 C38 54.2(4) . . . . ?
N1 C6 C7 C8 -179.6(2) . . . . ?
N1 C6 C7 C14 2.2(4) . . . . ?
N1 C6 C11 C10 -179.9(3) . . . . ?
N1 C6 C11 C13 -2.6(5) . . . . ?
N2 C2 C3 N1 -0.3(3) . . . . ?
N2 C2 C3 C5 -177.6(3) . . . . ?
N2 C27 C28 C29 -178.4(3) . . . . ?
N2 C27 C28 C33 1.1(4) . . . . ?
N2 C27 C32 C31 177.7(2) . . . . ?
N2 C27 C32 C35 -3.5(4) . . . . ?
C1 N1 C3 C2 0.8(3) . . . . ?
C1 N1 C3 C5 178.3(3) . . . . ?
C1 N1 C6 C7 -82.2(3) . . . . ?
C1 N1 C6 C11 96.3(3) . . . . ?
C1 N2 C2 C3 -0.2(3) . . . . ?
C1 N2 C2 C4 179.5(3) . . . . ?
C1 N2 C27 C28 -74.2(3) . . . . ?
C1 N2 C27 C32 109.3(3) . . . . ?
C2 N2 C1 Pd1 178.9(2) . . . . ?
C2 N2 C1 N1 0.7(3) . . . . ?
C2 N2 C27 C28 95.1(3) . . . . ?
C2 N2 C27 C32 -81.4(3) . . . . ?
C3 N1 C1 Pd1 -179.1(2) . . . . ?
C3 N1 C1 N2 -0.9(3) . . . . ?
C3 N1 C6 C7 110.2(3) . . . . ?
C3 N1 C6 C11 -71.3(3) . . . . ?
C4 C2 C3 N1 179.9(3) . . . . ?
C4 C2 C3 C5 2.7(6) . . . . ?
C6 N1 C1 Pd1 11.9(4) . . . . ?
C6 N1 C1 N2 -169.9(2) . . . . ?
C6 N1 C3 C2 169.7(2) . . . . ?
C6 N1 C3 C5 -12.8(4) . . . . ?
C6 C7 C8 C9 -1.1(4) . . . . ?
C6 C7 C14 C15 164.0(2) . . . . ?
C6 C7 C14 C21 -66.8(3) . . . . ?
C7 C6 C11 C10 -1.4(4) . . . . ?
C7 C6 C11 C13 175.9(3) . . . . ?
C7 C8 C9 C10 -0.3(4) . . . . ?
C7 C8 C9 C12 179.7(3) . . . . ?
C7 C14 C15 C16 90.2(3) . . . . ?
C7 C14 C15 C20 -90.2(3) . . . . ?
C7 C14 C21 C22 136.6(3) . . . . ?
C7 C14 C21 C26 -45.7(3) . . . . ?
C8 C7 C14 C15 -14.2(3) . . . . ?
C8 C7 C14 C21 115.0(3) . . . . ?
C8 C9 C10 C11 0.9(4) . . . . ?
C9 C10 C11 C6 -0.1(5) . . . . ?
C9 C10 C11 C13 -177.4(3) . . . . ?
C11 C6 C7 C8 2.0(4) . . . . ?
C11 C6 C7 C14 -176.3(2) . . . . ?
C12 C9 C10 C11 -179.1(3) . . . . ?
C14 C7 C8 C9 177.1(2) . . . . ?
C14 C15 C16 C17 179.5(3) . . . . ?
C14 C15 C20 C19 -179.6(3) . . . . ?
C14 C21 C22 C23 177.8(4) . . . . ?
C14 C21 C26 C25 -178.0(3) . . . . ?
C15 C14 C21 C22 -93.2(3) . . . . ?
C15 C14 C21 C26 84.6(3) . . . . ?
C15 C16 C17 C18 0.5(5) . . . . ?
C16 C15 C20 C19 0.1(5) . . . . ?
C16 C17 C18 C19 -1.0(5) . . . . ?
C17 C18 C19 C20 0.9(6) . . . . ?
C18 C19 C20 C15 -0.5(6) . . . . ?
C20 C15 C16 C17 -0.1(4) . . . . ?
C21 C14 C15 C16 -39.5(3) . . . . ?
C21 C14 C15 C20 140.2(3) . . . . ?
C21 C22 C23 C24 -0.2(7) . . . . ?
C22 C21 C26 C25 -0.2(4) . . . . ?
C22 C23 C24 C25 0.6(7) . . . . ?
C23 C24 C25 C26 -0.8(6) . . . . ?
C24 C25 C26 C21 0.6(5) . . . . ?
C26 C21 C22 C23 0.0(5) . . . . ?
C27 N2 C1 Pd1 -10.7(4) . . . . ?
C27 N2 C1 N1 171.1(2) . . . . ?
C27 N2 C2 C3 -170.7(2) . . . . ?
C27 N2 C2 C4 9.1(4) . . . . ?
C27 C28 C29 C30 0.2(5) . . . . ?
C28 C27 C32 C31 1.4(4) . . . . ?
C28 C27 C32 C35 -179.8(3) . . . . ?
C28 C29 C30 C31 2.2(5) . . . . ?
C28 C29 C30 C34 -178.2(3) . . . . ?
C29 C30 C31 C32 -2.8(4) . . . . ?
C30 C31 C32 C27 1.1(4) . . . . ?
C30 C31 C32 C35 -177.7(3) . . . . ?
C32 C27 C28 C29 -2.0(4) . . . . ?
C32 C27 C28 C33 177.4(3) . . . . ?
C33 C28 C29 C30 -179.3(3) . . . . ?
C34 C30 C31 C32 177.5(3) . . . . ?
C36 C37 C38 Pd1 -55.4(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.043 0.500 180.1 38.5 ?
2 -0.004 0.256 0.201 21.7 0.0 ?
3 0.004 0.256 0.799 21.7 0.0 ?
4 0.500 0.457 0.500 180.1 38.5 ?
5 0.496 0.756 0.201 21.7 0.0 ?
6 0.504 0.756 0.799 21.7 0.0 ?

_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 1.271
_oxdiff_exptl_absorpt_empirical_full_min 0.678
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.009(19)
2 -0.009(19)

####################################################################### 
# 
# 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_lk4077diamaj
_database_code_depnum_ccdc_archive 'CCDC 2250208'
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi'
;Aix Marseille University CNRS
France
;
_audit_update_record             
;
2023-03-20 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2019-02-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H39 F2 N2, B F4'
_chemical_formula_sum            'C45 H38 B F6 N2'
_chemical_formula_weight         731.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c45 h33 b1 f6 n2'
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.4939(14)
_cell_length_b                   17.6838(6)
_cell_length_c                   16.9141(11)
_cell_angle_alpha                90
_cell_angle_beta                 118.570(10)
_cell_angle_gamma                90
_cell_volume                     4332.7(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1829
_cell_measurement_temperature    295
_cell_measurement_theta_max      66.8010
_cell_measurement_theta_min      3.8730
_shelx_estimated_absorpt_T_max   0.986
_shelx_estimated_absorpt_T_min   0.820
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.1139
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14465
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.234
_diffrn_reflns_theta_min         3.051
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     68.00 103.00   1.00    2.50    --    0.00 178.00   0.00   35
  2  ω     36.00  91.00   1.00    2.50    --    0.00  57.00 -90.00   55
  3  ω     58.00  90.00   1.00    2.50    --    0.00 178.00 -90.00   32
  4  ω    -15.00  20.00   1.00    2.50    --    0.00  57.00 -90.00   35
  5  ω   -151.00 -80.00   1.00    2.50    --  -53.50 -94.00  30.00   71
  6  ω   -133.00 -82.00   1.00    2.50    --  -53.50 -94.00 120.00   51
  7  ω   -134.00 -86.00   1.00    2.50    --  -53.50 -94.00 -30.00   48
  8  ω    107.00 149.00   1.00    2.50    --   53.50 125.00  30.00   42
  9  ω     94.00 149.00   1.00    2.50    --   53.50 125.00-180.00   55
 10  ω     97.00 124.00   1.00    2.50    --   53.50 125.00 -30.00   27
 11  ω     95.00 149.00   1.00    2.50    --   53.50 125.00  90.00   54
 12  ω     61.00 174.00   1.00   45.00    --  107.00  38.00 -30.00  113
 13  ω    142.00 176.00   1.00   45.00    --  107.00  38.00 150.00   34
 14  ω     61.00  86.00   1.00   45.00    --  107.00  38.00 150.00   25
 15  ω    148.00 175.00   1.00   45.00    --  107.00  77.00 120.00   27
 16  ω     73.00 100.00   1.00   45.00    --  107.00  77.00 120.00   27
 17  ω    109.00 137.00   1.00   45.00    --  107.00 111.00 -30.00   28
 18  ω     12.00 153.00   1.00   45.00    --  107.00 -50.00 120.00  141
 19  ω     12.00  82.00   1.00   45.00    --  107.00-111.00 120.00   70
 20  ω     51.00 139.00   1.00   45.00    --  107.00 -63.00-150.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0493606000
_diffrn_orient_matrix_UB_12      -0.0634116000
_diffrn_orient_matrix_UB_13      0.0229570000
_diffrn_orient_matrix_UB_21      -0.0854441000
_diffrn_orient_matrix_UB_22      0.0090932000
_diffrn_orient_matrix_UB_23      -0.0932881000
_diffrn_orient_matrix_UB_31      0.0399032000
_diffrn_orient_matrix_UB_32      -0.0589756000
_diffrn_orient_matrix_UB_33      -0.0390167000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3173
_reflns_number_total             7751
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         7751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1782
_refine_ls_R_factor_gt           0.0986
_refine_ls_restrained_S_all      1.034
_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)+(0.1498P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2795
_refine_ls_wR_factor_ref         0.3322
_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 Ternary CH refined with riding coordinates:
 C12(H12), C32(H32)
2.b Aromatic/amide H refined with riding coordinates:
 C4AA(H4AA), C8(H8), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), C30(H30),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C25(H25A,H25B,H25C), C45(H45A,H45B,H45C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
F1 F 0.5510(3) 0.3481(3) 0.5914(2) 0.1004(14) Uani 1 1 d . . . . .
F2 F 0.5511(3) 0.1166(3) 0.2677(3) 0.0909(12) Uani 1 1 d . . . . .
N1 N 0.5004(3) 0.2735(3) 0.4370(3) 0.0568(11) Uani 1 1 d . . . . .
N2 N 0.5945(3) 0.2026(2) 0.4150(3) 0.0553(11) Uani 1 1 d . . . . .
C2 C 0.5601(5) 0.1596(3) 0.4605(4) 0.0648(14) Uani 1 1 d . . . . .
C3 C 0.5033(4) 0.2025(4) 0.4768(4) 0.0655(14) Uani 1 1 d . . . . .
C4 C 0.5888(5) 0.0796(4) 0.4869(5) 0.0804(19) Uani 1 1 d . . . . .
H4A H 0.564437 0.048519 0.433973 0.121 Uiso 1 1 calc GR . . . .
H4B H 0.565520 0.062394 0.526015 0.121 Uiso 1 1 calc GR . . . .
H4C H 0.654974 0.076507 0.517695 0.121 Uiso 1 1 calc GR . . . .
C4AA C 0.5557(4) 0.2716(3) 0.4019(4) 0.0565(13) Uani 1 1 d . . . . .
H4AA H 0.566570 0.311562 0.372506 0.068 Uiso 1 1 calc R . . . .
C5 C 0.4490(6) 0.1870(5) 0.5255(5) 0.096(2) Uani 1 1 d . . . . .
H5A H 0.485943 0.199240 0.588087 0.144 Uiso 1 1 calc GR . . . .
H5B H 0.432461 0.134421 0.519557 0.144 Uiso 1 1 calc GR . . . .
H5C H 0.394089 0.217297 0.500021 0.144 Uiso 1 1 calc GR . . . .
C6 C 0.4482(4) 0.3390(3) 0.4375(4) 0.0591(13) Uani 1 1 d . . . . .
C7 C 0.4749(5) 0.3756(4) 0.5175(4) 0.0756(18) Uani 1 1 d . . . . .
C8 C 0.4315(5) 0.4381(4) 0.5273(4) 0.0801(19) Uani 1 1 d . . . . .
H8 H 0.452221 0.461781 0.582679 0.096 Uiso 1 1 calc R . . . .
C9 C 0.3562(5) 0.4640(4) 0.4516(5) 0.0734(17) Uani 1 1 d . . . . .
C10 C 0.3283(5) 0.4301(3) 0.3686(4) 0.0641(15) Uani 1 1 d . . . . .
H10 H 0.279101 0.451092 0.317909 0.077 Uiso 1 1 calc R . . . .
C11 C 0.3710(4) 0.3662(3) 0.3584(4) 0.0594(13) Uani 1 1 d . . . . .
C12 C 0.3421(5) 0.3281(3) 0.2682(4) 0.0670(15) Uani 1 1 d . . . . .
H12 H 0.395733 0.331385 0.258034 0.080 Uiso 1 1 calc R . . . .
C13 C 0.2631(5) 0.3693(3) 0.1883(4) 0.0687(15) Uani 1 1 d . . . . .
C14 C 0.2862(6) 0.4149(4) 0.1357(5) 0.091(2) Uani 1 1 d . . . . .
H14 H 0.347610 0.421618 0.150142 0.109 Uiso 1 1 calc R . . . .
C15 C 0.2161(8) 0.4504(5) 0.0611(6) 0.109(3) Uani 1 1 d . . . . .
H15 H 0.231289 0.480183 0.024707 0.131 Uiso 1 1 calc R . . . .
C16 C 0.1276(8) 0.4428(5) 0.0403(6) 0.113(3) Uani 1 1 d . . . . .
H16 H 0.081632 0.467308 -0.009791 0.136 Uiso 1 1 calc R . . . .
C17 C 0.1056(7) 0.3994(5) 0.0925(7) 0.110(3) Uani 1 1 d . . . . .
H17 H 0.044163 0.394729 0.078860 0.132 Uiso 1 1 calc R . . . .
C18 C 0.1738(5) 0.3613(4) 0.1668(5) 0.091(2) Uani 1 1 d . . . . .
H18 H 0.157477 0.330403 0.201419 0.109 Uiso 1 1 calc R . . . .
C19 C 0.3228(5) 0.2443(4) 0.2694(5) 0.0796(19) Uani 1 1 d . . . . .
C20 C 0.3561(7) 0.1942(4) 0.2299(7) 0.110(3) Uani 1 1 d . . . . .
H20 H 0.389544 0.212669 0.202726 0.132 Uiso 1 1 calc R . . . .
C21 C 0.3417(8) 0.1179(6) 0.2292(10) 0.140(5) Uani 1 1 d . . . . .
H21 H 0.362711 0.084738 0.200335 0.168 Uiso 1 1 calc R . . . .
C22 C 0.2960(8) 0.0927(5) 0.2719(10) 0.133(4) Uani 1 1 d . . . . .
H22 H 0.288509 0.040813 0.274353 0.159 Uiso 1 1 calc R . . . .
C23 C 0.2602(6) 0.1388(6) 0.3117(9) 0.137(4) Uani 1 1 d . . . . .
H23 H 0.227816 0.119086 0.339308 0.164 Uiso 1 1 calc R . . . .
C24 C 0.2739(6) 0.2192(5) 0.3098(7) 0.106(3) Uani 1 1 d . . . . .
H24 H 0.249914 0.252849 0.335581 0.128 Uiso 1 1 calc R . . . .
C25 C 0.3047(6) 0.5326(4) 0.4572(5) 0.095(2) Uani 1 1 d . . . . .
H25A H 0.318171 0.540124 0.518476 0.143 Uiso 1 1 calc GR . . . .
H25B H 0.239534 0.524894 0.420148 0.143 Uiso 1 1 calc GR . . . .
H25C H 0.323604 0.576264 0.436505 0.143 Uiso 1 1 calc GR . . . .
C26 C 0.6635(4) 0.1822(3) 0.3913(3) 0.0505(12) Uani 1 1 d . . . . .
C27 C 0.6402(4) 0.1381(3) 0.3153(4) 0.0659(15) Uani 1 1 d . . . . .
C28 C 0.7027(5) 0.1163(4) 0.2889(4) 0.0724(17) Uani 1 1 d . . . . .
H28 H 0.684780 0.086568 0.237858 0.087 Uiso 1 1 calc R . . . .
C29 C 0.7938(5) 0.1393(4) 0.3399(4) 0.0693(16) Uani 1 1 d . . . . .
C30 C 0.8177(5) 0.1844(3) 0.4151(4) 0.0648(15) Uani 1 1 d . . . . .
H30 H 0.878393 0.200799 0.448291 0.078 Uiso 1 1 calc R . . . .
C31 C 0.7545(4) 0.2053(3) 0.4419(3) 0.0520(12) Uani 1 1 d . . . . .
C32 C 0.7841(4) 0.2491(3) 0.5295(4) 0.0630(14) Uani 1 1 d . . . . .
H32 H 0.731779 0.281811 0.518597 0.076 Uiso 1 1 calc R . . . .
C33 C 0.8656(5) 0.3022(3) 0.5538(4) 0.0652(15) Uani 1 1 d . . . . .
C34 C 0.8540(6) 0.3631(4) 0.4993(5) 0.085(2) Uani 1 1 d . . . . .
H34 H 0.798465 0.369936 0.446781 0.102 Uiso 1 1 calc R . . . .
C35 C 0.9261(8) 0.4151(5) 0.5230(7) 0.108(3) Uani 1 1 d . . . . .
H35 H 0.917170 0.457542 0.487251 0.130 Uiso 1 1 calc R . . . .
C36 C 1.0087(8) 0.4042(7) 0.5973(8) 0.134(4) Uani 1 1 d . . . . .
H36 H 1.057368 0.437522 0.611375 0.161 Uiso 1 1 calc R . . . .
C37 C 1.0191(8) 0.3449(7) 0.6500(8) 0.145(5) Uani 1 1 d . . . . .
H37 H 1.075319 0.337794 0.701647 0.173 Uiso 1 1 calc R . . . .
C38 C 0.9489(6) 0.2939(5) 0.6300(6) 0.104(3) Uani 1 1 d . . . . .
H38 H 0.958162 0.253508 0.668560 0.125 Uiso 1 1 calc R . . . .
C39 C 0.7961(5) 0.1969(4) 0.6041(4) 0.0682(16) Uani 1 1 d . . . . .
C40 C 0.7585(6) 0.2145(5) 0.6589(5) 0.096(2) Uani 1 1 d . . . . .
H40 H 0.724887 0.259102 0.648126 0.115 Uiso 1 1 calc R . . . .
C41 C 0.7685(10) 0.1685(7) 0.7297(7) 0.135(5) Uani 1 1 d . . . . .
H41 H 0.743186 0.182045 0.766398 0.163 Uiso 1 1 calc R . . . .
C42 C 0.8165(9) 0.1031(7) 0.7435(6) 0.138(5) Uani 1 1 d . . . . .
H42 H 0.822287 0.071356 0.789750 0.165 Uiso 1 1 calc R . . . .
C43 C 0.8580(8) 0.0811(6) 0.6915(6) 0.124(4) Uani 1 1 d . . . . .
H43 H 0.891999 0.036721 0.703278 0.149 Uiso 1 1 calc R . . . .
C44 C 0.8453(6) 0.1300(4) 0.6200(5) 0.092(2) Uani 1 1 d . . . . .
H44 H 0.870505 0.116952 0.583052 0.110 Uiso 1 1 calc R . . . .
C45 C 0.8649(6) 0.1156(5) 0.3120(5) 0.093(2) Uani 1 1 d . . . . .
H45A H 0.889831 0.067186 0.337745 0.139 Uiso 1 1 calc GR . . . .
H45B H 0.913653 0.152339 0.333097 0.139 Uiso 1 1 calc GR . . . .
H45C H 0.836106 0.112394 0.247580 0.139 Uiso 1 1 calc GR . . . .
F3 F 0.5502(5) 0.4516(3) 0.1828(3) 0.135(2) Uani 1 1 d . . . . .
F4 F 0.6614(5) 0.4327(5) 0.3202(4) 0.158(3) Uani 1 1 d . . . . .
F5 F 0.5615(6) 0.3406(3) 0.2457(4) 0.169(3) Uani 1 1 d . . . . .
F6 F 0.5225(4) 0.4383(3) 0.3012(4) 0.127(2) Uani 1 1 d . . . . .
B51 B 0.5706(8) 0.4180(5) 0.2581(6) 0.084(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C7 1.369(8) . ?
F2 C27 1.348(7) . ?
N1 C3 1.415(7) . ?
N1 C4AA 1.306(7) . ?
N1 C6 1.446(7) . ?
N2 C2 1.382(7) . ?
N2 C4AA 1.346(7) . ?
N2 C26 1.422(6) . ?
C2 C3 1.332(9) . ?
C2 C4 1.491(8) . ?
C3 C5 1.504(8) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4AA H4AA 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.369(9) . ?
C6 C11 1.418(8) . ?
C7 C8 1.368(9) . ?
C8 H8 0.9300 . ?
C8 C9 1.368(10) . ?
C9 C10 1.386(9) . ?
C9 C25 1.509(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.387(8) . ?
C11 C12 1.521(8) . ?
C12 H12 0.9800 . ?
C12 C13 1.541(9) . ?
C12 C19 1.517(8) . ?
C13 C14 1.380(10) . ?
C13 C18 1.346(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.389(11) . ?
C15 H15 0.9300 . ?
C15 C16 1.336(13) . ?
C16 H16 0.9300 . ?
C16 C17 1.344(13) . ?
C17 H17 0.9300 . ?
C17 C18 1.395(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.372(11) . ?
C19 C24 1.358(12) . ?
C20 H20 0.9300 . ?
C20 C21 1.369(13) . ?
C21 H21 0.9300 . ?
C21 C22 1.344(16) . ?
C22 H22 0.9300 . ?
C22 C23 1.358(16) . ?
C23 H23 0.9300 . ?
C23 C24 1.442(12) . ?
C24 H24 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.392(8) . ?
C26 C31 1.386(8) . ?
C27 C28 1.360(9) . ?
C28 H28 0.9300 . ?
C28 C29 1.388(9) . ?
C29 C30 1.389(9) . ?
C29 C45 1.517(9) . ?
C30 H30 0.9300 . ?
C30 C31 1.372(7) . ?
C31 C32 1.531(7) . ?
C32 H32 0.9800 . ?
C32 C33 1.525(8) . ?
C32 C39 1.498(8) . ?
C33 C34 1.370(9) . ?
C33 C38 1.371(10) . ?
C34 H34 0.9300 . ?
C34 C35 1.402(11) . ?
C35 H35 0.9300 . ?
C35 C36 1.355(15) . ?
C36 H36 0.9300 . ?
C36 C37 1.333(15) . ?
C37 H37 0.9300 . ?
C37 C38 1.375(12) . ?
C38 H38 0.9300 . ?
C39 C40 1.375(9) . ?
C39 C44 1.386(10) . ?
C40 H40 0.9300 . ?
C40 C41 1.392(13) . ?
C41 H41 0.9300 . ?
C41 C42 1.357(17) . ?
C42 H42 0.9300 . ?
C42 C43 1.403(15) . ?
C43 H43 0.9300 . ?
C43 C44 1.419(11) . ?
C44 H44 0.9300 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
F3 B51 1.295(9) . ?
F4 B51 1.382(12) . ?
F5 B51 1.382(10) . ?
F6 B51 1.358(10) . ?

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
C3 N1 C6 126.4(4) . . ?
C4AA N1 C3 108.7(5) . . ?
C4AA N1 C6 124.8(5) . . ?
C2 N2 C26 128.0(5) . . ?
C4AA N2 C2 107.5(5) . . ?
C4AA N2 C26 124.4(4) . . ?
N2 C2 C4 122.1(6) . . ?
C3 C2 N2 108.6(5) . . ?
C3 C2 C4 129.2(6) . . ?
N1 C3 C5 121.9(6) . . ?
C2 C3 N1 105.9(5) . . ?
C2 C3 C5 132.2(6) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C4AA N2 109.3(5) . . ?
N1 C4AA H4AA 125.4 . . ?
N2 C4AA H4AA 125.4 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 118.3(6) . . ?
C7 C6 C11 119.4(6) . . ?
C11 C6 N1 122.3(5) . . ?
C6 C7 F1 117.1(6) . . ?
C8 C7 F1 118.7(6) . . ?
C8 C7 C6 124.2(7) . . ?
C7 C8 H8 121.6 . . ?
C9 C8 C7 116.8(6) . . ?
C9 C8 H8 121.6 . . ?
C8 C9 C10 121.1(6) . . ?
C8 C9 C25 119.8(6) . . ?
C10 C9 C25 119.1(7) . . ?
C9 C10 H10 118.8 . . ?
C9 C10 C11 122.4(6) . . ?
C11 C10 H10 118.8 . . ?
C6 C11 C12 120.4(5) . . ?
C10 C11 C6 116.1(5) . . ?
C10 C11 C12 123.5(6) . . ?
C11 C12 H12 105.9 . . ?
C11 C12 C13 113.5(5) . . ?
C13 C12 H12 105.9 . . ?
C19 C12 C11 112.7(5) . . ?
C19 C12 H12 105.9 . . ?
C19 C12 C13 112.3(6) . . ?
C14 C13 C12 117.6(7) . . ?
C18 C13 C12 123.0(7) . . ?
C18 C13 C14 119.4(7) . . ?
C13 C14 H14 120.5 . . ?
C13 C14 C15 119.0(9) . . ?
C15 C14 H14 120.5 . . ?
C14 C15 H15 119.2 . . ?
C16 C15 C14 121.5(9) . . ?
C16 C15 H15 119.2 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.2(9) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 119.5 . . ?
C16 C17 C18 120.9(10) . . ?
C18 C17 H17 119.5 . . ?
C13 C18 C17 119.9(9) . . ?
C13 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 C12 119.3(7) . . ?
C24 C19 C12 120.3(7) . . ?
C24 C19 C20 120.4(8) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 C19 122.2(11) . . ?
C21 C20 H20 118.9 . . ?
C20 C21 H21 121.3 . . ?
C22 C21 C20 117.5(11) . . ?
C22 C21 H21 121.3 . . ?
C21 C22 H22 118.1 . . ?
C21 C22 C23 123.7(10) . . ?
C23 C22 H22 118.1 . . ?
C22 C23 H23 120.9 . . ?
C22 C23 C24 118.1(11) . . ?
C24 C23 H23 120.9 . . ?
C19 C24 C23 118.0(11) . . ?
C19 C24 H24 121.0 . . ?
C23 C24 H24 121.0 . . ?
C9 C25 H25A 109.5 . . ?
C9 C25 H25B 109.5 . . ?
C9 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N2 119.8(5) . . ?
C31 C26 N2 121.8(4) . . ?
C31 C26 C27 118.4(5) . . ?
F2 C27 C26 116.8(5) . . ?
F2 C27 C28 120.3(5) . . ?
C28 C27 C26 122.9(6) . . ?
C27 C28 H28 120.7 . . ?
C27 C28 C29 118.6(6) . . ?
C29 C28 H28 120.7 . . ?
C28 C29 C30 119.1(6) . . ?
C28 C29 C45 119.6(6) . . ?
C30 C29 C45 121.3(7) . . ?
C29 C30 H30 119.0 . . ?
C31 C30 C29 122.0(6) . . ?
C31 C30 H30 119.0 . . ?
C26 C31 C32 119.8(4) . . ?
C30 C31 C26 119.0(5) . . ?
C30 C31 C32 121.0(5) . . ?
C31 C32 H32 105.8 . . ?
C33 C32 C31 113.9(4) . . ?
C33 C32 H32 105.8 . . ?
C39 C32 C31 110.8(5) . . ?
C39 C32 H32 105.8 . . ?
C39 C32 C33 114.1(5) . . ?
C34 C33 C32 118.8(6) . . ?
C34 C33 C38 118.0(7) . . ?
C38 C33 C32 123.1(6) . . ?
C33 C34 H34 120.1 . . ?
C33 C34 C35 119.8(8) . . ?
C35 C34 H34 120.1 . . ?
C34 C35 H35 119.6 . . ?
C36 C35 C34 120.7(9) . . ?
C36 C35 H35 119.6 . . ?
C35 C36 H36 120.6 . . ?
C37 C36 C35 118.9(10) . . ?
C37 C36 H36 120.6 . . ?
C36 C37 H37 119.1 . . ?
C36 C37 C38 121.9(11) . . ?
C38 C37 H37 119.1 . . ?
C33 C38 C37 120.6(9) . . ?
C33 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C40 C39 C32 120.5(7) . . ?
C40 C39 C44 118.3(7) . . ?
C44 C39 C32 121.2(6) . . ?
C39 C40 H40 118.6 . . ?
C39 C40 C41 122.8(10) . . ?
C41 C40 H40 118.6 . . ?
C40 C41 H41 121.1 . . ?
C42 C41 C40 117.8(9) . . ?
C42 C41 H41 121.1 . . ?
C41 C42 H42 118.4 . . ?
C41 C42 C43 123.2(9) . . ?
C43 C42 H42 118.4 . . ?
C42 C43 H43 121.7 . . ?
C42 C43 C44 116.7(10) . . ?
C44 C43 H43 121.7 . . ?
C39 C44 C43 121.3(8) . . ?
C39 C44 H44 119.4 . . ?
C43 C44 H44 119.4 . . ?
C29 C45 H45A 109.5 . . ?
C29 C45 H45B 109.5 . . ?
C29 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
F3 B51 F4 109.8(7) . . ?
F3 B51 F5 110.3(7) . . ?
F3 B51 F6 117.5(9) . . ?
F4 B51 F5 107.6(9) . . ?
F6 B51 F4 103.9(7) . . ?
F6 B51 F5 107.1(7) . . ?

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
F1 C7 C8 C9 179.6(7) . . . . ?
F2 C27 C28 C29 -179.8(6) . . . . ?
N1 C6 C7 F1 1.3(9) . . . . ?
N1 C6 C7 C8 -179.9(6) . . . . ?
N1 C6 C11 C10 -179.2(5) . . . . ?
N1 C6 C11 C12 -2.1(8) . . . . ?
N2 C2 C3 N1 2.1(7) . . . . ?
N2 C2 C3 C5 -178.0(7) . . . . ?
N2 C26 C27 F2 -0.1(7) . . . . ?
N2 C26 C27 C28 -179.7(5) . . . . ?
N2 C26 C31 C30 -179.5(5) . . . . ?
N2 C26 C31 C32 4.4(7) . . . . ?
C2 N2 C4AA N1 0.4(6) . . . . ?
C2 N2 C26 C27 81.0(7) . . . . ?
C2 N2 C26 C31 -99.1(7) . . . . ?
C3 N1 C4AA N2 0.8(7) . . . . ?
C3 N1 C6 C7 69.1(8) . . . . ?
C3 N1 C6 C11 -110.9(7) . . . . ?
C4 C2 C3 N1 179.9(6) . . . . ?
C4 C2 C3 C5 -0.2(13) . . . . ?
C4AA N1 C3 C2 -1.8(7) . . . . ?
C4AA N1 C3 C5 178.2(6) . . . . ?
C4AA N1 C6 C7 -108.3(7) . . . . ?
C4AA N1 C6 C11 71.7(8) . . . . ?
C4AA N2 C2 C3 -1.6(7) . . . . ?
C4AA N2 C2 C4 -179.6(6) . . . . ?
C4AA N2 C26 C27 -104.2(6) . . . . ?
C4AA N2 C26 C31 75.7(7) . . . . ?
C6 N1 C3 C2 -179.6(5) . . . . ?
C6 N1 C3 C5 0.5(10) . . . . ?
C6 N1 C4AA N2 178.6(5) . . . . ?
C6 C7 C8 C9 0.8(11) . . . . ?
C6 C11 C12 C13 -174.4(6) . . . . ?
C6 C11 C12 C19 56.5(8) . . . . ?
C7 C6 C11 C10 0.8(8) . . . . ?
C7 C6 C11 C12 177.9(6) . . . . ?
C7 C8 C9 C10 -2.8(11) . . . . ?
C7 C8 C9 C25 179.9(7) . . . . ?
C8 C9 C10 C11 3.9(10) . . . . ?
C9 C10 C11 C6 -2.8(9) . . . . ?
C9 C10 C11 C12 -179.8(6) . . . . ?
C10 C11 C12 C13 2.4(9) . . . . ?
C10 C11 C12 C19 -126.7(6) . . . . ?
C11 C6 C7 F1 -178.7(6) . . . . ?
C11 C6 C7 C8 0.1(10) . . . . ?
C11 C12 C13 C14 100.8(7) . . . . ?
C11 C12 C13 C18 -80.9(8) . . . . ?
C11 C12 C19 C20 -136.0(7) . . . . ?
C11 C12 C19 C24 43.4(10) . . . . ?
C12 C13 C14 C15 177.5(7) . . . . ?
C12 C13 C18 C17 -178.9(7) . . . . ?
C12 C19 C20 C21 179.5(9) . . . . ?
C12 C19 C24 C23 -177.9(8) . . . . ?
C13 C12 C19 C20 94.3(8) . . . . ?
C13 C12 C19 C24 -86.3(8) . . . . ?
C13 C14 C15 C16 1.5(14) . . . . ?
C14 C13 C18 C17 -0.6(11) . . . . ?
C14 C15 C16 C17 -0.4(15) . . . . ?
C15 C16 C17 C18 -1.2(15) . . . . ?
C16 C17 C18 C13 1.7(14) . . . . ?
C18 C13 C14 C15 -1.0(11) . . . . ?
C19 C12 C13 C14 -129.9(7) . . . . ?
C19 C12 C13 C18 48.4(9) . . . . ?
C19 C20 C21 C22 -2.4(18) . . . . ?
C20 C19 C24 C23 1.4(13) . . . . ?
C20 C21 C22 C23 3(2) . . . . ?
C21 C22 C23 C24 -1.5(19) . . . . ?
C22 C23 C24 C19 -0.8(15) . . . . ?
C24 C19 C20 C21 0.1(15) . . . . ?
C25 C9 C10 C11 -178.7(6) . . . . ?
C26 N2 C2 C3 173.8(5) . . . . ?
C26 N2 C2 C4 -4.2(9) . . . . ?
C26 N2 C4AA N1 -175.2(5) . . . . ?
C26 C27 C28 C29 -0.2(9) . . . . ?
C26 C31 C32 C33 -151.9(5) . . . . ?
C26 C31 C32 C39 77.9(7) . . . . ?
C27 C26 C31 C30 0.4(7) . . . . ?
C27 C26 C31 C32 -175.7(5) . . . . ?
C27 C28 C29 C30 -0.7(9) . . . . ?
C27 C28 C29 C45 179.9(6) . . . . ?
C28 C29 C30 C31 1.6(9) . . . . ?
C29 C30 C31 C26 -1.4(8) . . . . ?
C29 C30 C31 C32 174.6(5) . . . . ?
C30 C31 C32 C33 32.1(8) . . . . ?
C30 C31 C32 C39 -98.1(6) . . . . ?
C31 C26 C27 F2 180.0(5) . . . . ?
C31 C26 C27 C28 0.4(8) . . . . ?
C31 C32 C33 C34 66.1(7) . . . . ?
C31 C32 C33 C38 -117.0(7) . . . . ?
C31 C32 C39 C40 -132.9(6) . . . . ?
C31 C32 C39 C44 47.3(8) . . . . ?
C32 C33 C34 C35 176.3(6) . . . . ?
C32 C33 C38 C37 -177.9(9) . . . . ?
C32 C39 C40 C41 -179.2(8) . . . . ?
C32 C39 C44 C43 179.0(7) . . . . ?
C33 C32 C39 C40 97.0(7) . . . . ?
C33 C32 C39 C44 -82.8(8) . . . . ?
C33 C34 C35 C36 2.8(14) . . . . ?
C34 C33 C38 C37 -1.0(14) . . . . ?
C34 C35 C36 C37 -3.0(18) . . . . ?
C35 C36 C37 C38 1(2) . . . . ?
C36 C37 C38 C33 1(2) . . . . ?
C38 C33 C34 C35 -0.7(11) . . . . ?
C39 C32 C33 C34 -165.3(5) . . . . ?
C39 C32 C33 C38 11.5(9) . . . . ?
C39 C40 C41 C42 -1.0(15) . . . . ?
C40 C39 C44 C43 -0.8(12) . . . . ?
C40 C41 C42 C43 1.6(17) . . . . ?
C41 C42 C43 C44 -1.8(16) . . . . ?
C42 C43 C44 C39 1.4(13) . . . . ?
C44 C39 C40 C41 0.6(12) . . . . ?
C45 C29 C30 C31 -179.0(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.660 0.250 415.5 78.9 ?
2 0.000 -0.455 0.750 415.5 78.9 ?


_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 1.573
_oxdiff_exptl_absorpt_empirical_full_min 0.609
####################################################################### 
# 
# 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_lk4082diamaj
_database_code_depnum_ccdc_archive 'CCDC 2250209'
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi'
;Aix Marseille University CNRS
France
;
_audit_update_record             
;
2023-03-20 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2019-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'B F4, C47 H45 N2'
_chemical_formula_sum            'C47 H45 B F4 N2'
_chemical_formula_weight         724.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c45 h39 b1 f6 n2'
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   9.4507(3)
_cell_length_b                   27.0470(8)
_cell_length_c                   16.5020(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.028(3)
_cell_angle_gamma                90
_cell_volume                     4092.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4311
_cell_measurement_temperature    295
_cell_measurement_theta_max      69.9160
_cell_measurement_theta_min      4.2590
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.892
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27064
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.660
_diffrn_reflns_theta_min         3.208
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00  32.00   1.00    5.00    --  -41.82  77.00  60.00  103
  2  ω    -83.00 -18.00   1.00    5.00    --  -41.82 -38.00-120.00   65
  3  ω    -56.00  20.00   1.00    5.00    --  -41.82  38.00   0.00   76
  4  ω   -104.00 -16.00   1.00    5.00    --  -41.82 -57.00-180.00   88
  5  ω     39.00 107.00   1.00   30.00    --  100.78-125.00 -90.00   68
  6  ω     25.00 123.00   1.00   30.00    --  100.78 -77.00  90.00   98
  7  ω     28.00 114.00   1.00   30.00    --  100.78 -45.00 -90.00   86
  8  ω     94.00 162.00   1.00   30.00    --  100.78  45.00  90.00   68
  9  ω     25.00 129.00   1.00   30.00    --  100.78 -30.00  60.00  104
 10  ω     40.00 117.00   1.00   30.00    --  100.78-125.00  90.00   77
 11  ω    104.00 150.00   1.00   30.00    --  100.78 125.00  30.00   46
 12  ω    104.00 130.00   1.00   30.00    --  100.78 125.00-150.00   26
 13  ω     51.00 107.00   1.00   30.00    --  100.78 -94.00 -60.00   56
 14  ω     17.00 118.00   1.00   30.00    --  100.78   0.00  60.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0736985000
_diffrn_orient_matrix_UB_12      -0.0221969000
_diffrn_orient_matrix_UB_13      0.0858286000
_diffrn_orient_matrix_UB_21      0.0432850000
_diffrn_orient_matrix_UB_22      0.0522807000
_diffrn_orient_matrix_UB_23      0.0342169000
_diffrn_orient_matrix_UB_31      -0.1446044000
_diffrn_orient_matrix_UB_32      0.0043420000
_diffrn_orient_matrix_UB_33      0.0269157000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4936
_reflns_number_total             7721
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         7721
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0578
_refine_ls_restrained_S_all      1.025
_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)+(0.0663P)²+0.4004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1701
_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. Rigid body (RIGU) restrains
 F1, F2, F3, F4, B1, F8, F7, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: F1(0.8) F2(0.8) F3(0.8) F4(0.8) F5(0.2) F6(0.2) F7(0.2) F8(0.2)
4.a Ternary CH refined with riding coordinates:
 C14(H14), C35(H35)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C31(H31), C37(H37),
  C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
 C46(H46), C47(H47)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
F1 F 0.3002(5) 0.35622(17) 0.5780(5) 0.225(3) Uani 0.8 1 d . U P A 1
F2 F 0.3972(5) 0.3078(3) 0.6621(3) 0.197(2) Uani 0.8 1 d . U P A 1
F3 F 0.2780(7) 0.2806(3) 0.5362(5) 0.226(4) Uani 0.8 1 d . U P A 1
F4 F 0.4937(4) 0.3093(4) 0.5619(2) 0.193(3) Uani 0.8 1 d . U P A 1
F5 F 0.467(2) 0.3469(7) 0.5796(14) 0.163(7) Uani 0.2 1 d . U P A 2
F6 F 0.451(3) 0.2801(6) 0.613(3) 0.244(14) Uani 0.2 1 d . U P A 2
F7 F 0.2647(17) 0.2818(8) 0.5800(19) 0.210(14) Uani 0.2 1 d . U P A 2
F8 F 0.2919(13) 0.3355(6) 0.4962(9) 0.127(4) Uani 0.2 1 d . U P A 2
B1 B 0.3632(4) 0.31274(19) 0.5764(3) 0.0946(11) Uani 1 1 d . U . . .
N1 N 0.86086(19) 0.33862(6) 0.70376(11) 0.0493(4) Uani 1 1 d . . . . .
N2 N 0.81061(18) 0.27228(6) 0.76449(11) 0.0491(4) Uani 1 1 d . . . . .
C1 C 0.7546(2) 0.30731(7) 0.70969(14) 0.0497(5) Uani 1 1 d . . . . .
H1 H 0.657492 0.309641 0.680332 0.060 Uiso 1 1 calc R . . . .
C2 C 0.9593(2) 0.28135(8) 0.79545(14) 0.0527(5) Uani 1 1 d . . . . .
C3 C 0.9902(2) 0.32297(8) 0.75752(14) 0.0523(5) Uani 1 1 d . . . . .
C4 C 1.0553(3) 0.24897(11) 0.85855(18) 0.0770(7) Uani 1 1 d . . . . .
H4A H 1.033636 0.253728 0.911917 0.116 Uiso 1 1 calc GR . . . .
H4B H 1.155492 0.257281 0.862450 0.116 Uiso 1 1 calc GR . . . .
H4C H 1.038714 0.215025 0.841961 0.116 Uiso 1 1 calc GR . . . .
C5 C 1.1306(3) 0.35020(10) 0.76601(18) 0.0697(7) Uani 1 1 d . . . . .
H5A H 1.151102 0.353508 0.712071 0.105 Uiso 1 1 calc GR . . . .
H5B H 1.208034 0.332173 0.802445 0.105 Uiso 1 1 calc GR . . . .
H5C H 1.122821 0.382413 0.788975 0.105 Uiso 1 1 calc GR . . . .
C6 C 0.8380(2) 0.38310(8) 0.65372(14) 0.0536(5) Uani 1 1 d . . . . .
C7 C 0.8743(3) 0.38274(10) 0.57650(15) 0.0653(6) Uani 1 1 d . . . . .
C8 C 0.8503(3) 0.42608(12) 0.53046(17) 0.0806(8) Uani 1 1 d . . . . .
H8 H 0.875828 0.427033 0.479477 0.097 Uiso 1 1 calc R . . . .
C9 C 0.7903(4) 0.46797(11) 0.55660(18) 0.0805(8) Uani 1 1 d . . . . .
C10 C 0.7542(3) 0.46623(10) 0.63339(16) 0.0710(7) Uani 1 1 d . . . . .
H10 H 0.712779 0.493962 0.651748 0.085 Uiso 1 1 calc R . . . .
C11 C 0.7780(3) 0.42439(8) 0.68340(14) 0.0552(5) Uani 1 1 d . . . . .
C12 C 0.9342(4) 0.33746(13) 0.54419(19) 0.0894(9) Uani 1 1 d . . . . .
H12A H 1.024665 0.328323 0.581889 0.134 Uiso 1 1 calc GR . . . .
H12B H 0.950469 0.344266 0.490087 0.134 Uiso 1 1 calc GR . . . .
H12C H 0.865663 0.310803 0.539930 0.134 Uiso 1 1 calc GR . . . .
C13 C 0.7607(5) 0.51437(15) 0.5034(2) 0.1229(14) Uani 1 1 d . . . . .
H13A H 0.827053 0.515854 0.467697 0.184 Uiso 1 1 calc GR . . . .
H13B H 0.774097 0.542934 0.539016 0.184 Uiso 1 1 calc GR . . . .
H13C H 0.662298 0.513667 0.469969 0.184 Uiso 1 1 calc GR . . . .
C14 C 0.7463(3) 0.42435(8) 0.76977(14) 0.0553(5) Uani 1 1 d . . . . .
H14 H 0.719127 0.390340 0.779853 0.066 Uiso 1 1 calc R . . . .
C15 C 0.8829(3) 0.43586(8) 0.83753(14) 0.0564(5) Uani 1 1 d . . . . .
C16 C 0.9121(3) 0.40957(10) 0.91132(16) 0.0660(6) Uani 1 1 d . . . . .
H16 H 0.849051 0.384388 0.918250 0.079 Uiso 1 1 calc R . . . .
C17 C 1.0329(4) 0.41987(13) 0.97515(19) 0.0853(8) Uani 1 1 d . . . . .
H17 H 1.050496 0.401585 1.024315 0.102 Uiso 1 1 calc R . . . .
C18 C 1.1261(3) 0.45664(14) 0.9664(2) 0.0877(9) Uani 1 1 d . . . . .
H18 H 1.207234 0.463640 1.009422 0.105 Uiso 1 1 calc R . . . .
C19 C 1.0999(4) 0.48322(14) 0.8940(2) 0.0912(9) Uani 1 1 d . . . . .
H19 H 1.163385 0.508441 0.887950 0.109 Uiso 1 1 calc R . . . .
C20 C 0.9798(3) 0.47300(11) 0.82955(18) 0.0772(7) Uani 1 1 d . . . . .
H20 H 0.963753 0.491224 0.780372 0.093 Uiso 1 1 calc R . . . .
C21 C 0.6155(3) 0.45634(8) 0.77340(14) 0.0565(5) Uani 1 1 d . . . . .
C22 C 0.4777(3) 0.44080(11) 0.7318(2) 0.0761(7) Uani 1 1 d . . . . .
H22 H 0.466642 0.411375 0.701795 0.091 Uiso 1 1 calc R . . . .
C23 C 0.3555(3) 0.46875(13) 0.7345(2) 0.0894(9) Uani 1 1 d . . . . .
H23 H 0.263161 0.458066 0.706255 0.107 Uiso 1 1 calc R . . . .
C24 C 0.3714(4) 0.51236(12) 0.7791(2) 0.0880(9) Uani 1 1 d . . . . .
H24 H 0.289892 0.531177 0.780947 0.106 Uiso 1 1 calc R . . . .
C25 C 0.5067(4) 0.52779(11) 0.82054(19) 0.0825(8) Uani 1 1 d . . . . .
H25 H 0.517115 0.556974 0.851206 0.099 Uiso 1 1 calc R . . . .
C26 C 0.6288(3) 0.50045(9) 0.81739(16) 0.0673(6) Uani 1 1 d . . . . .
H26 H 0.720796 0.511752 0.845041 0.081 Uiso 1 1 calc R . . . .
C27 C 0.7289(2) 0.23237(8) 0.78984(13) 0.0498(5) Uani 1 1 d . . . . .
C28 C 0.6784(3) 0.23847(10) 0.86163(15) 0.0644(6) Uani 1 1 d . . . . .
C29 C 0.6072(3) 0.19916(11) 0.88741(16) 0.0707(7) Uani 1 1 d . . . . .
H29 H 0.572100 0.202723 0.935093 0.085 Uiso 1 1 calc R . . . .
C30 C 0.5861(3) 0.15461(10) 0.84491(15) 0.0608(6) Uani 1 1 d . . . . .
C31 C 0.6333(2) 0.15104(8) 0.77194(14) 0.0529(5) Uani 1 1 d . . . . .
H31 H 0.616623 0.121742 0.741613 0.063 Uiso 1 1 calc R . . . .
C32 C 0.7044(2) 0.18934(7) 0.74217(13) 0.0455(4) Uani 1 1 d . . . . .
C33 C 0.6990(4) 0.28637(13) 0.9096(2) 0.1037(12) Uani 1 1 d . . . . .
H33A H 0.801247 0.293363 0.928749 0.155 Uiso 1 1 calc GR . . . .
H33B H 0.656637 0.283616 0.956776 0.155 Uiso 1 1 calc GR . . . .
H33C H 0.652144 0.312671 0.873990 0.155 Uiso 1 1 calc GR . . . .
C34 C 0.5118(3) 0.11204(12) 0.87706(18) 0.0833(8) Uani 1 1 d . . . . .
H34A H 0.564684 0.103885 0.932798 0.125 Uiso 1 1 calc GR . . . .
H34B H 0.509605 0.083844 0.841431 0.125 Uiso 1 1 calc GR . . . .
H34C H 0.413889 0.121315 0.877385 0.125 Uiso 1 1 calc GR . . . .
C35 C 0.7541(2) 0.18483(7) 0.66127(13) 0.0470(5) Uani 1 1 d . . . . .
H35 H 0.748206 0.218240 0.637694 0.056 Uiso 1 1 calc R . . . .
C36 C 0.6512(2) 0.15303(8) 0.59606(13) 0.0471(5) Uani 1 1 d . . . . .
C37 C 0.6962(3) 0.11187(8) 0.55976(15) 0.0570(5) Uani 1 1 d . . . . .
H37 H 0.792012 0.101009 0.577864 0.068 Uiso 1 1 calc R . . . .
C38 C 0.6001(3) 0.08645(11) 0.49654(17) 0.0730(7) Uani 1 1 d . . . . .
H38 H 0.632050 0.058750 0.472711 0.088 Uiso 1 1 calc R . . . .
C39 C 0.4594(3) 0.10174(13) 0.46916(17) 0.0802(8) Uani 1 1 d . . . . .
H39 H 0.395786 0.084763 0.426398 0.096 Uiso 1 1 calc R . . . .
C40 C 0.4119(3) 0.14228(13) 0.50485(18) 0.0815(8) Uani 1 1 d . . . . .
H40 H 0.315577 0.152639 0.486548 0.098 Uiso 1 1 calc R . . . .
C41 C 0.5067(2) 0.16780(10) 0.56797(15) 0.0633(6) Uani 1 1 d . . . . .
H41 H 0.473349 0.195192 0.591943 0.076 Uiso 1 1 calc R . . . .
C42 C 0.9136(2) 0.16974(9) 0.67710(15) 0.0554(5) Uani 1 1 d . . . . .
C43 C 1.0058(3) 0.19638(11) 0.63878(18) 0.0719(7) Uani 1 1 d . . . . .
H43 H 0.969547 0.223112 0.604574 0.086 Uiso 1 1 calc R . . . .
C44 C 1.1520(3) 0.18308(16) 0.6516(2) 0.0944(10) Uani 1 1 d . . . . .
H44 H 1.213264 0.201303 0.626528 0.113 Uiso 1 1 calc R . . . .
C45 C 1.2052(3) 0.14385(17) 0.7002(3) 0.1044(12) Uani 1 1 d . . . . .
H45 H 1.302612 0.134959 0.707906 0.125 Uiso 1 1 calc R . . . .
C46 C 1.1163(3) 0.11718(15) 0.7379(3) 0.1003(11) Uani 1 1 d . . . . .
H46 H 1.153238 0.090079 0.771018 0.120 Uiso 1 1 calc R . . . .
C47 C 0.9709(3) 0.13049(11) 0.72703(19) 0.0748(7) Uani 1 1 d . . . . .
H47 H 0.911665 0.112574 0.753894 0.090 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
F1 B1 1.321(6) . ?
F2 B1 1.377(6) . ?
F3 B1 1.259(6) . ?
F4 B1 1.316(5) . ?
F5 B1 1.337(17) . ?
F6 F7 1.71(3) . ?
F6 B1 1.257(18) . ?
F7 B1 1.264(16) . ?
F8 B1 1.468(13) . ?
N1 C1 1.335(3) . ?
N1 C3 1.391(3) . ?
N1 C6 1.445(3) . ?
N2 C1 1.328(3) . ?
N2 C2 1.395(3) . ?
N2 C27 1.447(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.354(3) . ?
C2 C4 1.489(3) . ?
C3 C5 1.494(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.397(3) . ?
C6 C11 1.394(3) . ?
C7 C8 1.386(4) . ?
C7 C12 1.500(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.382(4) . ?
C9 C10 1.391(4) . ?
C9 C13 1.518(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.387(3) . ?
C11 C14 1.526(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14 0.9800 . ?
C14 C15 1.521(3) . ?
C14 C21 1.522(3) . ?
C15 C16 1.379(3) . ?
C15 C20 1.387(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.381(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.360(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.364(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.382(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(4) . ?
C21 C26 1.386(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.390(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.379(5) . ?
C24 H24 0.9300 . ?
C24 C25 1.361(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.382(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.390(3) . ?
C27 C32 1.392(3) . ?
C28 C29 1.380(4) . ?
C28 C33 1.506(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.384(4) . ?
C30 C31 1.385(3) . ?
C30 C34 1.510(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.388(3) . ?
C32 C35 1.524(3) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35 0.9800 . ?
C35 C36 1.528(3) . ?
C35 C42 1.522(3) . ?
C36 C37 1.379(3) . ?
C36 C41 1.391(3) . ?
C37 H37 0.9300 . ?
C37 C38 1.388(4) . ?
C38 H38 0.9300 . ?
C38 C39 1.360(4) . ?
C39 H39 0.9300 . ?
C39 C40 1.371(4) . ?
C40 H40 0.9300 . ?
C40 C41 1.383(4) . ?
C41 H41 0.9300 . ?
C42 C43 1.395(4) . ?
C42 C47 1.372(4) . ?
C43 H43 0.9300 . ?
C43 C44 1.393(4) . ?
C44 H44 0.9300 . ?
C44 C45 1.351(5) . ?
C45 H45 0.9300 . ?
C45 C46 1.367(6) . ?
C46 H46 0.9300 . ?
C46 C47 1.389(4) . ?
C47 H47 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
B1 F6 F7 47.5(9) . . ?
B1 F7 F6 47.2(10) . . ?
F1 B1 F2 93.4(5) . . ?
F3 B1 F1 113.1(5) . . ?
F3 B1 F2 115.7(6) . . ?
F3 B1 F4 111.3(6) . . ?
F4 B1 F1 120.9(6) . . ?
F4 B1 F2 100.6(4) . . ?
F5 B1 F8 85.2(12) . . ?
F6 B1 F5 94.4(15) . . ?
F6 B1 F7 85.3(16) . . ?
F6 B1 F8 146(2) . . ?
F7 B1 F5 174.7(19) . . ?
F7 B1 F8 97.9(12) . . ?
C1 N1 C3 108.70(18) . . ?
C1 N1 C6 123.98(18) . . ?
C3 N1 C6 127.16(18) . . ?
C1 N2 C2 108.91(17) . . ?
C1 N2 C27 125.21(18) . . ?
C2 N2 C27 125.85(18) . . ?
N1 C1 H1 125.7 . . ?
N2 C1 N1 108.62(18) . . ?
N2 C1 H1 125.7 . . ?
N2 C2 C4 122.8(2) . . ?
C3 C2 N2 106.72(19) . . ?
C3 C2 C4 130.5(2) . . ?
N1 C3 C5 122.2(2) . . ?
C2 C3 N1 107.05(18) . . ?
C2 C3 C5 130.7(2) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 118.7(2) . . ?
C11 C6 N1 118.88(19) . . ?
C11 C6 C7 122.5(2) . . ?
C6 C7 C12 121.8(2) . . ?
C8 C7 C6 116.8(2) . . ?
C8 C7 C12 121.4(2) . . ?
C7 C8 H8 118.4 . . ?
C9 C8 C7 123.2(2) . . ?
C9 C8 H8 118.4 . . ?
C8 C9 C10 117.8(3) . . ?
C8 C9 C13 122.0(3) . . ?
C10 C9 C13 120.2(3) . . ?
C9 C10 H10 119.0 . . ?
C11 C10 C9 122.0(3) . . ?
C11 C10 H10 119.0 . . ?
C6 C11 C14 121.09(19) . . ?
C10 C11 C6 117.8(2) . . ?
C10 C11 C14 121.1(2) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14 106.1 . . ?
C15 C14 C11 111.25(19) . . ?
C15 C14 H14 106.1 . . ?
C15 C14 C21 114.05(18) . . ?
C21 C14 C11 112.43(19) . . ?
C21 C14 H14 106.1 . . ?
C16 C15 C14 119.7(2) . . ?
C16 C15 C20 117.5(3) . . ?
C20 C15 C14 122.7(2) . . ?
C15 C16 H16 119.3 . . ?
C15 C16 C17 121.4(3) . . ?
C17 C16 H16 119.3 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.2(3) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 120.2 . . ?
C17 C18 C19 119.6(3) . . ?
C19 C18 H18 120.2 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.6(3) . . ?
C20 C19 H19 119.7 . . ?
C15 C20 H20 119.7 . . ?
C19 C20 C15 120.6(3) . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C14 119.0(2) . . ?
C22 C21 C26 118.5(2) . . ?
C26 C21 C14 122.6(2) . . ?
C21 C22 H22 119.7 . . ?
C21 C22 C23 120.6(3) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 120.1 . . ?
C24 C23 C22 119.9(3) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 H24 120.1 . . ?
C25 C24 C23 119.9(3) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 119.7 . . ?
C24 C25 C26 120.6(3) . . ?
C26 C25 H25 119.7 . . ?
C21 C26 H26 119.7 . . ?
C25 C26 C21 120.6(3) . . ?
C25 C26 H26 119.7 . . ?
C28 C27 N2 118.38(19) . . ?
C28 C27 C32 122.4(2) . . ?
C32 C27 N2 119.19(18) . . ?
C27 C28 C33 121.5(2) . . ?
C29 C28 C27 117.7(2) . . ?
C29 C28 C33 120.7(2) . . ?
C28 C29 H29 118.8 . . ?
C28 C29 C30 122.4(2) . . ?
C30 C29 H29 118.8 . . ?
C29 C30 C31 117.6(2) . . ?
C29 C30 C34 120.5(2) . . ?
C31 C30 C34 121.8(2) . . ?
C30 C31 H31 118.6 . . ?
C30 C31 C32 122.8(2) . . ?
C32 C31 H31 118.6 . . ?
C27 C32 C35 121.17(18) . . ?
C31 C32 C27 116.90(19) . . ?
C31 C32 C35 121.93(18) . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.5 . . ?
C28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
C30 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35 105.9 . . ?
C32 C35 C36 112.55(16) . . ?
C36 C35 H35 105.9 . . ?
C42 C35 C32 111.95(18) . . ?
C42 C35 H35 105.9 . . ?
C42 C35 C36 113.85(17) . . ?
C37 C36 C35 123.36(19) . . ?
C37 C36 C41 117.9(2) . . ?
C41 C36 C35 118.61(19) . . ?
C36 C37 H37 119.6 . . ?
C36 C37 C38 120.8(2) . . ?
C38 C37 H37 119.6 . . ?
C37 C38 H38 119.7 . . ?
C39 C38 C37 120.5(3) . . ?
C39 C38 H38 119.7 . . ?
C38 C39 H39 120.1 . . ?
C38 C39 C40 119.7(3) . . ?
C40 C39 H39 120.1 . . ?
C39 C40 H40 119.9 . . ?
C39 C40 C41 120.2(3) . . ?
C41 C40 H40 119.9 . . ?
C36 C41 H41 119.6 . . ?
C40 C41 C36 120.8(2) . . ?
C40 C41 H41 119.6 . . ?
C43 C42 C35 119.0(2) . . ?
C47 C42 C35 122.7(2) . . ?
C47 C42 C43 118.2(2) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 C42 120.2(3) . . ?
C44 C43 H43 119.9 . . ?
C43 C44 H44 119.8 . . ?
C45 C44 C43 120.3(3) . . ?
C45 C44 H44 119.8 . . ?
C44 C45 H45 119.9 . . ?
C44 C45 C46 120.2(3) . . ?
C46 C45 H45 119.9 . . ?
C45 C46 H46 119.9 . . ?
C45 C46 C47 120.1(4) . . ?
C47 C46 H46 119.9 . . ?
C42 C47 C46 120.8(3) . . ?
C42 C47 H47 119.6 . . ?
C46 C47 H47 119.6 . . ?

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
F6 F7 B1 F8 146(2) . . . . ?
F7 F6 B1 F5 174.7(19) . . . . ?
F7 F6 B1 F8 -97(3) . . . . ?
N1 C6 C7 C8 179.8(2) . . . . ?
N1 C6 C7 C12 0.7(4) . . . . ?
N1 C6 C11 C10 -178.6(2) . . . . ?
N1 C6 C11 C14 4.2(3) . . . . ?
N2 C2 C3 N1 -0.3(2) . . . . ?
N2 C2 C3 C5 179.9(2) . . . . ?
N2 C27 C28 C29 -176.8(2) . . . . ?
N2 C27 C28 C33 3.8(4) . . . . ?
N2 C27 C32 C31 176.17(19) . . . . ?
N2 C27 C32 C35 -3.7(3) . . . . ?
C1 N1 C3 C2 0.4(2) . . . . ?
C1 N1 C3 C5 -179.8(2) . . . . ?
C1 N1 C6 C7 -101.8(3) . . . . ?
C1 N1 C6 C11 76.9(3) . . . . ?
C1 N2 C2 C3 0.1(2) . . . . ?
C1 N2 C2 C4 179.9(2) . . . . ?
C1 N2 C27 C28 -94.7(3) . . . . ?
C1 N2 C27 C32 85.7(3) . . . . ?
C2 N2 C1 N1 0.1(2) . . . . ?
C2 N2 C27 C28 82.9(3) . . . . ?
C2 N2 C27 C32 -96.7(2) . . . . ?
C3 N1 C1 N2 -0.3(2) . . . . ?
C3 N1 C6 C7 83.3(3) . . . . ?
C3 N1 C6 C11 -98.0(3) . . . . ?
C4 C2 C3 N1 180.0(2) . . . . ?
C4 C2 C3 C5 0.2(4) . . . . ?
C6 N1 C1 N2 -176.02(18) . . . . ?
C6 N1 C3 C2 175.93(19) . . . . ?
C6 N1 C3 C5 -4.3(3) . . . . ?
C6 C7 C8 C9 -1.6(4) . . . . ?
C6 C11 C14 C15 82.1(3) . . . . ?
C6 C11 C14 C21 -148.6(2) . . . . ?
C7 C6 C11 C10 0.1(4) . . . . ?
C7 C6 C11 C14 -177.1(2) . . . . ?
C7 C8 C9 C10 0.7(5) . . . . ?
C7 C8 C9 C13 -177.9(3) . . . . ?
C8 C9 C10 C11 0.7(5) . . . . ?
C9 C10 C11 C6 -1.0(4) . . . . ?
C9 C10 C11 C14 176.2(3) . . . . ?
C10 C11 C14 C15 -95.0(3) . . . . ?
C10 C11 C14 C21 34.3(3) . . . . ?
C11 C6 C7 C8 1.2(4) . . . . ?
C11 C6 C7 C12 -177.9(3) . . . . ?
C11 C14 C15 C16 -138.2(2) . . . . ?
C11 C14 C15 C20 43.5(3) . . . . ?
C11 C14 C21 C22 70.2(3) . . . . ?
C11 C14 C21 C26 -110.3(2) . . . . ?
C12 C7 C8 C9 177.5(3) . . . . ?
C13 C9 C10 C11 179.3(3) . . . . ?
C14 C15 C16 C17 -178.2(2) . . . . ?
C14 C15 C20 C19 177.8(3) . . . . ?
C14 C21 C22 C23 179.3(2) . . . . ?
C14 C21 C26 C25 -178.5(2) . . . . ?
C15 C14 C21 C22 -161.9(2) . . . . ?
C15 C14 C21 C26 17.6(3) . . . . ?
C15 C16 C17 C18 0.2(4) . . . . ?
C16 C15 C20 C19 -0.6(4) . . . . ?
C16 C17 C18 C19 -0.2(5) . . . . ?
C17 C18 C19 C20 -0.2(5) . . . . ?
C18 C19 C20 C15 0.6(5) . . . . ?
C20 C15 C16 C17 0.2(4) . . . . ?
C21 C14 C15 C16 93.4(3) . . . . ?
C21 C14 C15 C20 -84.9(3) . . . . ?
C21 C22 C23 C24 -0.1(5) . . . . ?
C22 C21 C26 C25 1.0(4) . . . . ?
C22 C23 C24 C25 -0.1(5) . . . . ?
C23 C24 C25 C26 0.9(5) . . . . ?
C24 C25 C26 C21 -1.3(4) . . . . ?
C26 C21 C22 C23 -0.3(4) . . . . ?
C27 N2 C1 N1 178.07(18) . . . . ?
C27 N2 C2 C3 -177.81(19) . . . . ?
C27 N2 C2 C4 1.9(3) . . . . ?
C27 C28 C29 C30 0.5(4) . . . . ?
C27 C32 C35 C36 -146.65(19) . . . . ?
C27 C32 C35 C42 83.6(2) . . . . ?
C28 C27 C32 C31 -3.5(3) . . . . ?
C28 C27 C32 C35 176.7(2) . . . . ?
C28 C29 C30 C31 -3.0(4) . . . . ?
C28 C29 C30 C34 178.0(3) . . . . ?
C29 C30 C31 C32 2.3(4) . . . . ?
C30 C31 C32 C27 0.8(3) . . . . ?
C30 C31 C32 C35 -179.4(2) . . . . ?
C31 C32 C35 C36 33.5(3) . . . . ?
C31 C32 C35 C42 -96.3(2) . . . . ?
C32 C27 C28 C29 2.9(4) . . . . ?
C32 C27 C28 C33 -176.6(3) . . . . ?
C32 C35 C36 C37 -123.6(2) . . . . ?
C32 C35 C36 C41 60.4(3) . . . . ?
C32 C35 C42 C43 -131.1(2) . . . . ?
C32 C35 C42 C47 49.6(3) . . . . ?
C33 C28 C29 C30 179.9(3) . . . . ?
C34 C30 C31 C32 -178.6(2) . . . . ?
C35 C36 C37 C38 -175.3(2) . . . . ?
C35 C36 C41 C40 175.4(2) . . . . ?
C35 C42 C43 C44 -179.4(3) . . . . ?
C35 C42 C47 C46 178.2(3) . . . . ?
C36 C35 C42 C43 99.8(2) . . . . ?
C36 C35 C42 C47 -79.5(3) . . . . ?
C36 C37 C38 C39 0.0(4) . . . . ?
C37 C36 C41 C40 -0.8(4) . . . . ?
C37 C38 C39 C40 -0.6(4) . . . . ?
C38 C39 C40 C41 0.5(5) . . . . ?
C39 C40 C41 C36 0.2(4) . . . . ?
C41 C36 C37 C38 0.7(3) . . . . ?
C42 C35 C36 C37 5.2(3) . . . . ?
C42 C35 C36 C41 -170.9(2) . . . . ?
C42 C43 C44 C45 1.0(5) . . . . ?
C43 C42 C47 C46 -1.1(4) . . . . ?
C43 C44 C45 C46 -0.7(6) . . . . ?
C44 C45 C46 C47 -0.4(6) . . . . ?
C45 C46 C47 C42 1.3(5) . . . . ?
C47 C42 C43 C44 -0.1(4) . . . . ?


_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 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.710
####################################################################### 
# 
# 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_lk2087a
_database_code_depnum_ccdc_archive 'CCDC 2250211'
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi'
;Aix Marseille University CNRS
France
;
_audit_update_record             
;
2023-03-20 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2018-01-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H33 Cl N2 Pd, C0.5 H2 Cl'
_chemical_formula_sum            'C32.50 H35 Cl2 N2 Pd'
_chemical_formula_weight         630.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c32 h29 Cl1 n2 Pd1'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   9.35660(10)
_cell_length_b                   17.0040(2)
_cell_length_c                   18.8780(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.7570(10)
_cell_angle_gamma                90
_cell_volume                     2982.62(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    36465
_cell_measurement_temperature    293
_cell_measurement_theta_max      70.9780
_cell_measurement_theta_min      4.7280
_shelx_estimated_absorpt_T_max   0.875
_shelx_estimated_absorpt_T_min   0.342
_exptl_absorpt_coefficient_mu    6.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.18b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            76642
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.318
_diffrn_reflns_theta_min         3.509
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  57.00   1.00    2.00    --  -17.77  38.00 120.00   99
  2  ω    -94.00  15.00   1.00    2.00    --  -17.77 -77.00 120.00  109
  3  ω   -107.00 -35.00   1.00    2.00    --  -17.77-178.00-150.00   72
  4  ω    -92.00   7.00   1.00    2.00    --  -17.77 -38.00-180.00   99
  5  ω    -92.00   7.00   1.00    2.00    --  -17.77 -38.00  30.00   99
  6  ω    -92.00   7.00   1.00    2.00    --  -17.77 -38.00   0.00   99
  7  ω     57.00 107.00   1.00    2.00    --   17.77 178.00-150.00   50
  8  ω     17.00  69.00   1.00    2.00    --   17.77-117.00  88.00   52
  9  ω    -15.00  94.00   1.00    2.00    --   17.77  77.00  30.00  109
 10  ω     69.00 178.00   1.00   25.00    --  101.41  77.00   0.00  109
 11  ω     94.00 175.00   1.00   25.00    --  101.41 125.00 -90.00   81
 12  ω     72.00 174.00   1.00   25.00    --  101.41  61.00  30.00  102
 13  ω     69.00 178.00   1.00   25.00    --  101.41  77.00 -30.00  109
 14  ω     76.00 174.00   1.00   25.00    --  101.41  45.00  60.00   98
 15  ω     69.00 178.00   1.00   25.00    --  101.41  77.00  30.00  109
 16  ω     25.00 130.00   1.00   25.00    --  101.41 -30.00 -90.00  105
 17  ω     72.00 174.00   1.00   25.00    --  101.41  61.00   0.00  102
 18  ω     94.00 175.00   1.00   25.00    --  101.41 125.00-180.00   81
 19  ω     19.00 109.00   1.00   25.00    --  101.41 -94.00-150.00   90
 20  ω     76.00 174.00   1.00   25.00    --  101.41  45.00  90.00   98
 21  ω     25.00 134.00   1.00   25.00    --  101.41 -77.00 -90.00  109
 22  ω     49.00 178.00   1.00   25.00    --  101.41  15.00  90.00  129
 23  ω     73.00 178.00   1.00   25.00    --  101.41  30.00  90.00  105
 24  ω     20.00 154.00   1.00   25.00    --  101.41 -15.00 150.00  134
 25  ω    -92.00   7.00   1.00    2.00    --  -17.77 -38.00 -90.00   99
 26  ω    -94.00  15.00   1.00    2.00    --  -17.77 -77.00-180.00  109
 27  ω    -91.00  10.00   1.00    2.00    --  -17.77 -57.00-120.00  101
 28  ω    -42.00  57.00   1.00    2.00    --  -17.77  38.00  30.00   99
 29  ω    -98.00  23.00   1.00    2.00    --  -17.77 -19.00-120.00  121
 30  ω    -69.00   5.00   1.00    2.00    --  -17.77 117.00 175.00   74
 31  ω     57.00 107.00   1.00    2.00    --   17.77 178.00 -60.00   50
 32  ω     69.00 178.00   1.00   25.00    --  101.41  77.00-180.00  109
 33  ω     28.00 121.00   1.00   25.00    --  101.41-125.00 150.00   93
 34  ω     72.00 174.00   1.00   25.00    --  101.41  61.00 120.00  102
 35  ω     72.00 174.00   1.00   25.00    --  101.41  61.00 -60.00  102
 36  ω     72.00 174.00   1.00   25.00    --  101.41  61.00-120.00  102
 37  ω     69.00 178.00   1.00   25.00    --  101.41  77.00-150.00  109
 38  ω     72.00 174.00   1.00   25.00    --  101.41  61.00 150.00  102
 39  ω     72.00 174.00   1.00   25.00    --  101.41  61.00  90.00  102
 40  ω     76.00 174.00   1.00   25.00    --  101.41  45.00-180.00   98
 41  ω     72.00 174.00   1.00   25.00    --  101.41  61.00 -30.00  102
 42  ω     72.00 174.00   1.00   25.00    --  101.41  61.00-180.00  102
 43  ω     72.00 174.00   1.00   25.00    --  101.41  61.00 -90.00  102
 44  ω     72.00 174.00   1.00   25.00    --  101.41  61.00-150.00  102
 45  ω     76.00 174.00   1.00   25.00    --  101.41  45.00 -90.00   98
 46  ω    -92.00   7.00   1.00    2.00    --  -17.77 -38.00  90.00   99
 47  ω    -91.00  10.00   1.00    2.00    --  -17.77 -57.00  90.00  101
 48  ω    -94.00  15.00   1.00    2.00    --  -17.77 -77.00  90.00  109
 49  ω    -92.00   7.00   1.00    2.00    --  -17.77 -38.00-120.00   99
 50  ω      1.00  59.00   1.00    2.00    --   17.77 -99.00 -30.00   58
 51  ω      1.00  59.00   1.00    2.00    --   17.77 -99.00-180.00   58
 52  ω     55.00 105.00   1.00    2.00    --   17.77-178.00  30.00   50
 53  ω     69.00 106.00   1.00   25.00    --  101.41  77.00 120.00   37
 54  ω     69.00 178.00   1.00   25.00    --  101.41  77.00 -60.00  109
 55  ω     69.00 178.00   1.00   25.00    --  101.41  77.00  90.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0951255000
_diffrn_orient_matrix_UB_12      -0.0192907000
_diffrn_orient_matrix_UB_13      0.0589882000
_diffrn_orient_matrix_UB_21      -0.1171343000
_diffrn_orient_matrix_UB_22      -0.0325928000
_diffrn_orient_matrix_UB_23      -0.0565574000
_diffrn_orient_matrix_UB_31      0.0687406000
_diffrn_orient_matrix_UB_32      -0.0823058000
_diffrn_orient_matrix_UB_33      0.0085550000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5341
_reflns_number_total             5777
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_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         0.701
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5777
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0467
_refine_ls_restrained_S_all      1.059
_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)+(0.0877P)²+2.1579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1331
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-C34
 1.75 with sigma of 0.005
3. Rigid bond restraints
 Cl2, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim C34: within 1.8A with sigma of 0.001 and sigma for terminal atoms of
0.001
Uanis(C31) = Uanis(C32)
5. Rigid body (RIGU) restrains
 C24, C29, C25, C28, C26, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C31(0.75) H31(0.75) C32(0.25) H32(0.25) C34(0.5)
7.a Riding coordinates:
 C30(H30A,H30B), C30(H30C,H30D), C31(H31), C33(H33A,H33B), C33(H33C,H33D),
 C32(H32), C34(H34A,H34B)
7.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C17(H17), C16(H16), C15(H15), C14(H14),
 C13(H13), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29)
7.c Fitted hexagon refined as free rotating group:
 C24(C25,C26,C27,C28,C29)
7.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.48501(2) 0.43298(2) 0.30363(2) 0.04247(12) Uani 1 1 d . . . . .
Cl1 Cl 0.36684(10) 0.43290(5) 0.18490(5) 0.0557(2) Uani 1 1 d . . . . .
N1 N 0.7724(3) 0.50501(14) 0.26667(14) 0.0384(5) Uani 1 1 d . . . . .
N2 N 0.7545(3) 0.38340(14) 0.24123(13) 0.0378(5) Uani 1 1 d . . . . .
C2 C 0.8952(3) 0.48559(19) 0.23476(19) 0.0450(7) Uani 1 1 d . . . . .
C3 C 0.8839(3) 0.4084(2) 0.21823(19) 0.0446(7) Uani 1 1 d . . . . .
C4 C 1.0134(4) 0.5426(3) 0.2264(3) 0.0697(12) Uani 1 1 d . . . . .
H4A H 0.978647 0.582749 0.193014 0.105 Uiso 1 1 calc GR . . . .
H4B H 1.092377 0.515470 0.209148 0.105 Uiso 1 1 calc GR . . . .
H4C H 1.045202 0.566201 0.271734 0.105 Uiso 1 1 calc GR . . . .
C1 C 0.6850(3) 0.44174(16) 0.27051(16) 0.0350(6) Uani 1 1 d . . . . .
C5 C 0.9835(4) 0.3545(2) 0.1858(3) 0.0666(11) Uani 1 1 d . . . . .
H5A H 0.992667 0.306270 0.212374 0.100 Uiso 1 1 calc GR . . . .
H5B H 1.076230 0.378923 0.186883 0.100 Uiso 1 1 calc GR . . . .
H5C H 0.945761 0.343617 0.137310 0.100 Uiso 1 1 calc GR . . . .
C6 C 0.7479(3) 0.58171(18) 0.29532(17) 0.0404(6) Uani 1 1 d . . . . .
C7 C 0.7644(4) 0.5891(2) 0.3687(2) 0.0568(8) Uani 1 1 d . . . . .
H7 H 0.783837 0.545052 0.397403 0.068 Uiso 1 1 calc R . . . .
C8 C 0.7518(5) 0.6623(3) 0.3991(2) 0.0663(10) Uani 1 1 d . . . . .
H8 H 0.759799 0.667505 0.448428 0.080 Uiso 1 1 calc R . . . .
C9 C 0.7273(5) 0.7276(2) 0.3561(2) 0.0645(10) Uani 1 1 d . . . . .
H9 H 0.721007 0.777119 0.376441 0.077 Uiso 1 1 calc R . . . .
C10 C 0.7121(4) 0.7197(2) 0.2832(2) 0.0534(8) Uani 1 1 d . . . . .
H10 H 0.695648 0.764267 0.254917 0.064 Uiso 1 1 calc R . . . .
C11 C 0.7208(3) 0.64640(18) 0.25043(18) 0.0421(6) Uani 1 1 d . . . . .
C12 C 0.6989(4) 0.6407(2) 0.17194(19) 0.0501(7) Uani 1 1 d . . . . .
C17 C 0.6000(5) 0.5882(2) 0.1378(2) 0.0601(9) Uani 1 1 d . . . . .
H17 H 0.549731 0.554358 0.164662 0.072 Uiso 1 1 calc R . . . .
C16 C 0.5757(8) 0.5858(4) 0.0638(3) 0.0929(17) Uani 1 1 d . . . . .
H16 H 0.507851 0.551352 0.041140 0.112 Uiso 1 1 calc R . . . .
C15 C 0.6530(11) 0.6350(4) 0.0238(3) 0.122(3) Uani 1 1 d . . . . .
H15 H 0.638011 0.633283 -0.025726 0.147 Uiso 1 1 calc R . . . .
C14 C 0.7513(10) 0.6861(4) 0.0576(3) 0.114(2) Uani 1 1 d . . . . .
H14 H 0.803036 0.718967 0.030530 0.137 Uiso 1 1 calc R . . . .
C13 C 0.7752(6) 0.6899(3) 0.1304(3) 0.0764(13) Uani 1 1 d . . . . .
H13 H 0.842198 0.725221 0.152336 0.092 Uiso 1 1 calc R . . . .
C18 C 0.7113(3) 0.30211(18) 0.2374(2) 0.0468(7) Uani 1 1 d . . . . .
C19 C 0.6551(4) 0.2734(2) 0.1717(3) 0.0628(10) Uani 1 1 d . . . . .
H19 H 0.639435 0.306877 0.132559 0.075 Uiso 1 1 calc R . . . .
C20 C 0.6215(5) 0.1926(3) 0.1646(4) 0.0833(15) Uani 1 1 d . . . . .
H20 H 0.582800 0.172451 0.120651 0.100 Uiso 1 1 calc R . . . .
C21 C 0.6460(6) 0.1443(3) 0.2223(4) 0.094(2) Uani 1 1 d . . . . .
H21 H 0.626558 0.090820 0.217373 0.113 Uiso 1 1 calc R . . . .
C22 C 0.6984(5) 0.1737(3) 0.2868(4) 0.0844(17) Uani 1 1 d . . . . .
H22 H 0.711410 0.139818 0.325701 0.101 Uiso 1 1 calc R . . . .
C23 C 0.7338(4) 0.2535(2) 0.2972(3) 0.0621(10) Uani 1 1 d . . . . .
C24 C 0.7895(4) 0.2819(2) 0.36998(15) 0.0744(10) Uani 1 1 d . U . . .
C25 C 0.7259(4) 0.2509(2) 0.4268(2) 0.116(2) Uani 1 1 d G U . . .
H25 H 0.651434 0.214655 0.418410 0.139 Uiso 1 1 calc R . . . .
C26 C 0.7738(6) 0.2741(3) 0.49617(18) 0.150(3) Uani 1 1 d G U . . .
H26 H 0.731248 0.253311 0.534184 0.180 Uiso 1 1 calc R . . . .
C27 C 0.8851(6) 0.3282(3) 0.50871(13) 0.146(3) Uani 1 1 d G U . . .
H27 H 0.917121 0.343719 0.555122 0.175 Uiso 1 1 calc R . . . .
C28 C 0.9487(4) 0.3592(3) 0.4519(2) 0.118(2) Uani 1 1 d G U . . .
H28 H 1.023180 0.395473 0.460288 0.142 Uiso 1 1 calc R . . . .
C29 C 0.9009(3) 0.3361(2) 0.38253(16) 0.0806(11) Uani 1 1 d G U . . .
H29 H 0.943368 0.356818 0.344514 0.097 Uiso 1 1 calc R . . . .
C30 C 0.5354(7) 0.4383(3) 0.4147(3) 0.0826(15) Uani 1 1 d . . . . .
H30A H 0.608969 0.419074 0.440478 0.099 Uiso 1 1 d R . . A 1
H30B H 0.539059 0.485084 0.397598 0.099 Uiso 1 1 d R . . A 1
H30C H 0.590679 0.463904 0.446258 0.099 Uiso 1 1 d R . . B 2
H30D H 0.570399 0.401754 0.390378 0.099 Uiso 1 1 d R . . B 2
C31 C 0.4126(7) 0.3946(4) 0.4009(3) 0.0744(16) Uani 0.75 1 d . . P C 1
H31 H 0.409145 0.344051 0.419474 0.089 Uiso 0.75 1 d R . P C 1
C33 C 0.2917(6) 0.4258(3) 0.3597(3) 0.0863(17) Uani 1 1 d . . . . .
H33A H 0.214937 0.397982 0.351189 0.104 Uiso 1 1 d R . . C 1
H33B H 0.294537 0.472542 0.342429 0.104 Uiso 1 1 d R . . C 1
H33C H 0.204867 0.442862 0.358059 0.104 Uiso 1 1 d R . . C 2
H33D H 0.311687 0.388342 0.331899 0.104 Uiso 1 1 d R . . C 2
C32 C 0.392(2) 0.4555(13) 0.4038(11) 0.0744(16) Uani 0.25 1 d . . P C 2
H32 H 0.361985 0.495674 0.432059 0.089 Uiso 0.25 1 d R . P C 2
Cl2 Cl 0.8953(10) 0.0618(4) 0.4919(4) 0.337(4) Uani 1 1 d D U . . .
C34 C 0.960(4) -0.0274(16) 0.463(2) 0.337(4) Uani 0.5 1 d D U P . .
H34A H 0.889214 -0.062923 0.465594 0.404 Uiso 1 1 d R . . . .
H34B H 0.977964 -0.020553 0.417794 0.404 Uiso 1 1 d 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 2.3797(10) . ?
Pd1 C1 2.047(3) . ?
Pd1 C30 2.096(5) . ?
Pd1 C31 2.133(5) . ?
Pd1 C33 2.203(4) . ?
Pd1 C32 2.207(18) . ?
N1 C2 1.398(4) . ?
N1 C1 1.359(4) . ?
N1 C6 1.441(4) . ?
N2 C3 1.400(4) . ?
N2 C1 1.341(4) . ?
N2 C18 1.439(4) . ?
C2 C3 1.351(5) . ?
C2 C4 1.492(5) . ?
C3 C5 1.488(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.381(5) . ?
C6 C11 1.393(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.382(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.379(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.372(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.398(5) . ?
C11 C12 1.475(5) . ?
C12 C17 1.389(6) . ?
C12 C13 1.398(5) . ?
C17 H17 0.9300 . ?
C17 C16 1.390(6) . ?
C16 H16 0.9300 . ?
C16 C15 1.385(10) . ?
C15 H15 0.9300 . ?
C15 C14 1.368(11) . ?
C14 H14 0.9300 . ?
C14 C13 1.368(8) . ?
C13 H13 0.9300 . ?
C18 C19 1.379(6) . ?
C18 C23 1.394(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.413(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.362(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.354(9) . ?
C22 H22 0.9300 . ?
C22 C23 1.404(6) . ?
C23 C24 1.493(6) . ?
C24 C25 1.3900 . ?
C24 C29 1.3900 . ?
C25 H25 0.9300 . ?
C25 C26 1.3900 . ?
C26 H26 0.9300 . ?
C26 C27 1.3900 . ?
C27 H27 0.9300 . ?
C27 C28 1.3900 . ?
C28 H28 0.9300 . ?
C28 C29 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30A 0.8599 . ?
C30 H30B 0.8599 . ?
C30 H30C 0.8599 . ?
C30 H30D 0.8600 . ?
C30 C31 1.368(9) . ?
C30 C32 1.37(2) . ?
C33 H33A 0.8599 . ?
C33 H33B 0.8601 . ?
C33 H33C 0.8601 . ?
C33 H33D 0.8599 . ?
C33 C32 1.28(2) . ?
Cl2 C34 1.745(5) . ?
C34 H34A 0.9036 . ?
C34 H34B 0.8919 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 Cl1 93.01(9) . . ?
C1 Pd1 C30 101.31(19) . . ?
C1 Pd1 C31 132.8(2) . . ?
C1 Pd1 C33 169.1(2) . . ?
C1 Pd1 C32 135.8(6) . . ?
C30 Pd1 Cl1 165.25(17) . . ?
C30 Pd1 C31 37.7(2) . . ?
C30 Pd1 C33 67.8(2) . . ?
C30 Pd1 C32 36.9(6) . . ?
C33 Pd1 Cl1 97.80(18) . . ?
C33 Pd1 C32 33.8(6) . . ?
C2 N1 C6 123.4(3) . . ?
C1 N1 C2 111.5(2) . . ?
C1 N1 C6 125.0(3) . . ?
C3 N2 C18 121.6(2) . . ?
C1 N2 C3 112.5(2) . . ?
C1 N2 C18 125.7(2) . . ?
N1 C2 C4 123.3(3) . . ?
C3 C2 N1 106.4(3) . . ?
C3 C2 C4 130.2(3) . . ?
N2 C3 C5 123.1(3) . . ?
C2 C3 N2 105.7(3) . . ?
C2 C3 C5 131.1(3) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C1 Pd1 130.7(2) . . ?
N2 C1 Pd1 125.3(2) . . ?
N2 C1 N1 103.9(3) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 117.0(3) . . ?
C7 C6 C11 122.0(3) . . ?
C11 C6 N1 120.8(3) . . ?
C6 C7 H7 120.2 . . ?
C6 C7 C8 119.6(4) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.8(4) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.1(3) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 119.1 . . ?
C9 C10 C11 121.8(4) . . ?
C11 C10 H10 119.1 . . ?
C6 C11 C10 116.7(3) . . ?
C6 C11 C12 123.6(3) . . ?
C10 C11 C12 119.7(3) . . ?
C17 C12 C11 120.9(3) . . ?
C17 C12 C13 118.7(4) . . ?
C13 C12 C11 120.3(4) . . ?
C12 C17 H17 119.8 . . ?
C12 C17 C16 120.4(4) . . ?
C16 C17 H17 119.8 . . ?
C17 C16 H16 120.1 . . ?
C15 C16 C17 119.7(6) . . ?
C15 C16 H16 120.1 . . ?
C16 C15 H15 120.1 . . ?
C14 C15 C16 119.7(5) . . ?
C14 C15 H15 120.1 . . ?
C15 C14 H14 119.4 . . ?
C13 C14 C15 121.3(6) . . ?
C13 C14 H14 119.4 . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.2(5) . . ?
C14 C13 H13 119.9 . . ?
C19 C18 N2 117.4(3) . . ?
C19 C18 C23 121.5(4) . . ?
C23 C18 N2 121.0(3) . . ?
C18 C19 H19 120.4 . . ?
C18 C19 C20 119.1(5) . . ?
C20 C19 H19 120.4 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.7(5) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.4(4) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 118.8 . . ?
C21 C22 C23 122.4(5) . . ?
C23 C22 H22 118.8 . . ?
C18 C23 C22 116.7(5) . . ?
C18 C23 C24 123.8(3) . . ?
C22 C23 C24 119.5(4) . . ?
C25 C24 C23 116.9(3) . . ?
C25 C24 C29 120.0 . . ?
C29 C24 C23 123.1(3) . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 120.0 . . ?
C25 C26 C27 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 120.0 . . ?
C29 C28 H28 120.0 . . ?
C24 C29 H29 120.0 . . ?
C28 C29 C24 120.0 . . ?
C28 C29 H29 120.0 . . ?
Cl2 C34 Cl2 116(2) 3_756 . ?
Cl2 C34 H34A 106.1 . . ?
Cl2 C34 H34B 107.4 . . ?
H34A C34 H34B 111.4 . . ?


_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 2.727
_oxdiff_exptl_absorpt_empirical_full_min 0.526
_vrf_PLAT410_I                   
;
PROBLEM: Short Intra H...H Contact H33B     ..H32       .       1.78 Ang.  
RESPONSE: H32 and H33B are PART 2 and PART 1 respectively as H atoms connected
to disordered central C atoms of the allyl moiety. Checkcif should not report this
error message.
;
####################################################################### 
# 
# 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_lk2078
_database_code_depnum_ccdc_archive 'CCDC 2250210'
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi'
;Aix Marseille University CNRS
France
;
_audit_update_record             
;
2023-03-20 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2018-01-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H33 Cl N2 Pd'
_chemical_formula_sum            'C26 H33 Cl N2 Pd'
_chemical_formula_weight         515.39
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      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                   9.6459(2)
_cell_length_b                   21.2509(3)
_cell_length_c                   12.3138(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.214(2)
_cell_angle_gamma                90
_cell_volume                     2509.30(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31514
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.8180
_cell_measurement_theta_min      3.9120
_shelx_estimated_absorpt_T_max   0.934
_shelx_estimated_absorpt_T_min   0.875
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.18b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            75805
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.608
_diffrn_reflns_theta_min         3.193
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  83.00   1.00   10.00    --    8.41  38.00-180.00   99
  2  ω    -20.00  49.00   1.00   10.00    --    8.41 -99.00-120.00   69
  3  ω    -20.00  82.00   1.00   10.00    --    8.41  57.00-150.00  102
  4  ω    -16.00  83.00   1.00   10.00    --    8.41  38.00   0.00   99
  5  ω    -24.00  85.00   1.00   10.00    --    8.41  77.00  30.00  109
  6  ω    -41.00  24.00   1.00   10.00    --   -7.78  81.00  70.00   65
  7  ω    -20.00  49.00   1.00   10.00    --    8.41 -99.00 -30.00   69
  8  ω    -64.00  37.00   1.00   10.00    --    8.41 -57.00-180.00  101
  9  ω    -20.00  49.00   1.00   10.00    --    8.41 -99.00-180.00   69
 10  ω    -20.00  49.00   1.00   10.00    --    8.41 -99.00 -90.00   69
 11  ω    -64.00  37.00   1.00   10.00    --    8.41 -57.00 120.00  101
 12  ω    -64.00  37.00   1.00   10.00    --    8.41 -57.00  60.00  101
 13  ω    -20.00  49.00   1.00   10.00    --    8.41 -99.00  30.00   69
 14  ω    -64.00 -39.00   1.00   10.00    --    8.41 -57.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0327488000
_diffrn_orient_matrix_UB_12      0.0284022000
_diffrn_orient_matrix_UB_13      -0.0134827000
_diffrn_orient_matrix_UB_21      0.0242266000
_diffrn_orient_matrix_UB_22      0.0046654000
_diffrn_orient_matrix_UB_23      0.0558818000
_diffrn_orient_matrix_UB_31      0.0617558000
_diffrn_orient_matrix_UB_32      -0.0168918000
_diffrn_orient_matrix_UB_33      -0.0072485000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5140
_reflns_number_total             6070
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         6070
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0329P)²+1.3851P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0735
_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 Riding coordinates:
 C24(H24A,H24B), C25(H25), C26(H26A,H26B)
2.b Ternary CH refined with riding coordinates:
 C12(H12), C21(H21)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.52887(2) 0.40098(2) 0.59713(2) 0.03558(6) Uani 1 1 d . . . . .
Cl1 Cl 0.65865(7) 0.37778(3) 0.44919(5) 0.06027(16) Uani 1 1 d . . . . .
N1 N 0.80995(16) 0.37815(8) 0.73653(13) 0.0337(3) Uani 1 1 d . . . . .
N2 N 0.67658(16) 0.29792(7) 0.73190(13) 0.0329(3) Uani 1 1 d . . . . .
C1 C 0.67893(19) 0.35927(9) 0.70227(16) 0.0322(4) Uani 1 1 d . . . . .
C2 C 0.8909(2) 0.32833(10) 0.78295(16) 0.0368(4) Uani 1 1 d . . . . .
C3 C 0.8077(2) 0.27791(9) 0.77949(16) 0.0366(4) Uani 1 1 d . . . . .
C4 C 1.0413(2) 0.33515(12) 0.8256(2) 0.0532(6) Uani 1 1 d . . . . .
H4A H 1.093747 0.347537 0.767255 0.080 Uiso 1 1 calc GR . . . .
H4B H 1.075905 0.295668 0.855196 0.080 Uiso 1 1 calc GR . . . .
H4C H 1.050632 0.366607 0.881910 0.080 Uiso 1 1 calc GR . . . .
C5 C 0.8371(3) 0.21098(11) 0.8109(2) 0.0549(6) Uani 1 1 d . . . . .
H5A H 0.783915 0.199568 0.869462 0.082 Uiso 1 1 calc GR . . . .
H5B H 0.934692 0.206108 0.834350 0.082 Uiso 1 1 calc GR . . . .
H5C H 0.811560 0.184236 0.749151 0.082 Uiso 1 1 calc GR . . . .
C6 C 0.5522(2) 0.26030(9) 0.71576(16) 0.0343(4) Uani 1 1 d . . . . .
C7 C 0.5088(2) 0.24081(11) 0.61006(18) 0.0463(5) Uani 1 1 d . . . . .
H7 H 0.561591 0.250421 0.553408 0.056 Uiso 1 1 calc R . . . .
C8 C 0.3862(3) 0.20696(12) 0.5896(2) 0.0562(6) Uani 1 1 d . . . . .
H8 H 0.356975 0.193093 0.519196 0.067 Uiso 1 1 calc R . . . .
C9 C 0.3082(3) 0.19395(11) 0.6733(2) 0.0549(6) Uani 1 1 d . . . . .
H9 H 0.225090 0.171756 0.659360 0.066 Uiso 1 1 calc R . . . .
C10 C 0.3519(2) 0.21344(10) 0.7776(2) 0.0471(5) Uani 1 1 d . . . . .
H10 H 0.297197 0.204154 0.833268 0.057 Uiso 1 1 calc R . . . .
C11 C 0.4760(2) 0.24683(9) 0.80275(17) 0.0363(4) Uani 1 1 d . . . . .
C12 C 0.5219(2) 0.26654(11) 0.91964(18) 0.0445(5) Uani 1 1 d . . . . .
H12 H 0.616368 0.283758 0.921791 0.053 Uiso 1 1 calc R . . . .
C13 C 0.5276(3) 0.21068(14) 0.9974(2) 0.0704(8) Uani 1 1 d . . . . .
H13A H 0.434678 0.196104 1.003901 0.106 Uiso 1 1 calc GR . . . .
H13B H 0.570884 0.223323 1.067898 0.106 Uiso 1 1 calc GR . . . .
H13C H 0.580913 0.177398 0.969425 0.106 Uiso 1 1 calc GR . . . .
C14 C 0.4286(4) 0.31785(17) 0.9578(3) 0.0927(11) Uani 1 1 d . . . . .
H14A H 0.431890 0.354091 0.911643 0.139 Uiso 1 1 calc GR . . . .
H14B H 0.460551 0.329174 1.031805 0.139 Uiso 1 1 calc GR . . . .
H14C H 0.334451 0.302695 0.954204 0.139 Uiso 1 1 calc GR . . . .
C15 C 0.8619(2) 0.44132(9) 0.72694(17) 0.0359(4) Uani 1 1 d . . . . .
C16 C 0.9551(2) 0.45197(11) 0.65092(19) 0.0464(5) Uani 1 1 d . . . . .
H16 H 0.976556 0.419689 0.604562 0.056 Uiso 1 1 calc R . . . .
C17 C 1.0164(3) 0.51046(13) 0.6437(2) 0.0588(7) Uani 1 1 d . . . . .
H17 H 1.080143 0.517596 0.593568 0.071 Uiso 1 1 calc R . . . .
C18 C 0.9819(3) 0.55746(13) 0.7110(3) 0.0668(8) Uani 1 1 d . . . . .
H18 H 1.023009 0.596865 0.707112 0.080 Uiso 1 1 calc R . . . .
C19 C 0.8876(3) 0.54728(12) 0.7843(2) 0.0654(7) Uani 1 1 d . . . . .
H19 H 0.865164 0.580343 0.828648 0.078 Uiso 1 1 calc R . . . .
C20 C 0.8237(2) 0.48887(11) 0.7949(2) 0.0486(5) Uani 1 1 d . . . . .
C21 C 0.7210(3) 0.47915(14) 0.8785(2) 0.0676(7) Uani 1 1 d . . . . .
H21 H 0.673654 0.438963 0.861559 0.081 Uiso 1 1 calc R . . . .
C22 C 0.6099(4) 0.5301(2) 0.8697(4) 0.1188(16) Uani 1 1 d . . . . .
H22A H 0.650675 0.569236 0.895831 0.178 Uiso 1 1 calc GR . . . .
H22B H 0.536788 0.518620 0.912856 0.178 Uiso 1 1 calc GR . . . .
H22C H 0.572102 0.534757 0.794706 0.178 Uiso 1 1 calc GR . . . .
C23 C 0.7948(5) 0.4741(3) 0.9935(3) 0.1240(17) Uani 1 1 d . . . . .
H23A H 0.866654 0.442783 0.995145 0.186 Uiso 1 1 calc GR . . . .
H23B H 0.728795 0.462416 1.042909 0.186 Uiso 1 1 calc GR . . . .
H23C H 0.835598 0.514018 1.015088 0.186 Uiso 1 1 calc GR . . . .
C24 C 0.3403(3) 0.43667(13) 0.5014(2) 0.0619(7) Uani 1 1 d . . . . .
H24A H 0.346576 0.393888 0.486792 0.074 Uiso 1 1 d R . . . .
H24B H 0.328336 0.465368 0.444152 0.074 Uiso 1 1 d R . . . .
C25 C 0.3488(3) 0.45747(15) 0.6076(3) 0.0700(8) Uani 1 1 d . . . . .
H25 H 0.342427 0.500390 0.620845 0.084 Uiso 1 1 d R . . . .
C26 C 0.3667(3) 0.41647(16) 0.6954(3) 0.0730(9) Uani 1 1 d . . . . .
H26A H 0.373274 0.373417 0.683383 0.088 Uiso 1 1 d R . . . .
H26B H 0.372064 0.431987 0.766303 0.088 Uiso 1 1 d 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 2.3712(6) . ?
Pd1 C1 2.0376(19) . ?
Pd1 C24 2.193(2) . ?
Pd1 H24A 2.1079 . ?
Pd1 C25 2.126(2) . ?
Pd1 C26 2.105(3) . ?
Pd1 H26A 2.0172 . ?
N1 C1 1.349(2) . ?
N1 C2 1.400(2) . ?
N1 C15 1.442(2) . ?
N2 C1 1.355(2) . ?
N2 C3 1.401(2) . ?
N2 C6 1.438(2) . ?
C2 C3 1.337(3) . ?
C2 C4 1.495(3) . ?
C3 C5 1.493(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.387(3) . ?
C6 C11 1.393(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.383(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.369(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.372(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.397(3) . ?
C11 C12 1.518(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.522(3) . ?
C12 C14 1.520(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.384(3) . ?
C15 C20 1.387(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.383(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.362(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.365(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.398(3) . ?
C20 C21 1.519(4) . ?
C21 H21 0.9800 . ?
C21 C22 1.519(5) . ?
C21 C23 1.518(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9300 . ?
C24 H24B 0.9299 . ?
C24 C25 1.374(4) . ?
C25 H25 0.9299 . ?
C25 C26 1.385(4) . ?
C26 H26A 0.9299 . ?
C26 H26B 0.9299 . ?

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 H24A 87.9 . . ?
Cl1 Pd1 H26A 146.0 . . ?
C1 Pd1 Cl1 89.99(6) . . ?
C1 Pd1 C24 169.39(10) . . ?
C1 Pd1 H24A 149.8 . . ?
C1 Pd1 C25 137.38(11) . . ?
C1 Pd1 C26 102.94(10) . . ?
C1 Pd1 H26A 93.3 . . ?
C24 Pd1 Cl1 97.76(8) . . ?
C24 Pd1 H24A 24.9 . . ?
C24 Pd1 H26A 76.3 . . ?
H24A Pd1 H26A 72.7 . . ?
C25 Pd1 Cl1 131.78(9) . . ?
C25 Pd1 C24 37.06(11) . . ?
C25 Pd1 H24A 56.6 . . ?
C25 Pd1 H26A 58.2 . . ?
C26 Pd1 Cl1 164.00(10) . . ?
C26 Pd1 C24 68.28(12) . . ?
C26 Pd1 H24A 76.2 . . ?
C26 Pd1 C25 38.21(11) . . ?
C26 Pd1 H26A 26.0 . . ?
C1 N1 C2 111.41(16) . . ?
C1 N1 C15 124.99(16) . . ?
C2 N1 C15 123.61(16) . . ?
C1 N2 C3 111.36(16) . . ?
C1 N2 C6 122.40(16) . . ?
C3 N2 C6 126.24(16) . . ?
N1 C1 Pd1 130.26(13) . . ?
N1 C1 N2 104.14(15) . . ?
N2 C1 Pd1 123.95(14) . . ?
N1 C2 C4 123.18(19) . . ?
C3 C2 N1 106.64(17) . . ?
C3 C2 C4 130.18(19) . . ?
N2 C3 C5 122.35(18) . . ?
C2 C3 N2 106.37(17) . . ?
C2 C3 C5 131.19(19) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N2 117.29(18) . . ?
C7 C6 C11 121.98(19) . . ?
C11 C6 N2 120.66(17) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.4(2) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.8(2) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.4(2) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.0 . . ?
C9 C10 C11 122.0(2) . . ?
C11 C10 H10 119.0 . . ?
C6 C11 C10 116.4(2) . . ?
C6 C11 C12 123.25(18) . . ?
C10 C11 C12 120.34(19) . . ?
C11 C12 H12 107.7 . . ?
C11 C12 C13 111.6(2) . . ?
C11 C12 C14 111.7(2) . . ?
C13 C12 H12 107.7 . . ?
C14 C12 H12 107.7 . . ?
C14 C12 C13 110.3(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N1 117.67(19) . . ?
C16 C15 C20 121.5(2) . . ?
C20 C15 N1 120.75(18) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.2(2) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.5 . . ?
C18 C17 C16 119.1(2) . . ?
C18 C17 H17 120.5 . . ?
C17 C18 H18 119.7 . . ?
C17 C18 C19 120.6(2) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 118.9 . . ?
C18 C19 C20 122.3(3) . . ?
C20 C19 H19 118.9 . . ?
C15 C20 C19 116.2(2) . . ?
C15 C20 C21 123.0(2) . . ?
C19 C20 C21 120.7(2) . . ?
C20 C21 H21 107.3 . . ?
C20 C21 C22 111.2(3) . . ?
C22 C21 H21 107.3 . . ?
C23 C21 C20 111.5(3) . . ?
C23 C21 H21 107.3 . . ?
C23 C21 C22 111.9(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Pd1 C24 H24A 72.5 . . ?
Pd1 C24 H24B 131.5 . . ?
H24A C24 H24B 120.0 . . ?
C25 C24 Pd1 68.85(14) . . ?
C25 C24 H24A 120.0 . . ?
C25 C24 H24B 120.0 . . ?
Pd1 C25 H25 129.4 . . ?
C24 C25 Pd1 74.09(15) . . ?
C24 C25 H25 119.0 . . ?
C24 C25 C26 122.0(3) . . ?
C26 C25 Pd1 70.04(15) . . ?
C26 C25 H25 119.0 . . ?
Pd1 C26 H26A 71.8 . . ?
Pd1 C26 H26B 128.8 . . ?
C25 C26 Pd1 71.75(16) . . ?
C25 C26 H26A 120.0 . . ?
C25 C26 H26B 120.0 . . ?
H26A C26 H26B 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 C24 C25 C26 -53.4(2) . . . . ?
N1 C2 C3 N2 -0.6(2) . . . . ?
N1 C2 C3 C5 176.1(2) . . . . ?
N1 C15 C16 C17 -175.2(2) . . . . ?
N1 C15 C20 C19 175.6(2) . . . . ?
N1 C15 C20 C21 -3.2(3) . . . . ?
N2 C6 C7 C8 -177.1(2) . . . . ?
N2 C6 C11 C10 175.96(17) . . . . ?
N2 C6 C11 C12 -4.1(3) . . . . ?
C1 N1 C2 C3 -1.3(2) . . . . ?
C1 N1 C2 C4 178.6(2) . . . . ?
C1 N1 C15 C16 -108.1(2) . . . . ?
C1 N1 C15 C20 74.4(3) . . . . ?
C1 N2 C3 C2 2.3(2) . . . . ?
C1 N2 C3 C5 -174.7(2) . . . . ?
C1 N2 C6 C7 74.6(2) . . . . ?
C1 N2 C6 C11 -102.5(2) . . . . ?
C2 N1 C1 Pd1 -162.85(15) . . . . ?
C2 N1 C1 N2 2.6(2) . . . . ?
C2 N1 C15 C16 71.7(3) . . . . ?
C2 N1 C15 C20 -105.8(2) . . . . ?
C3 N2 C1 Pd1 163.67(13) . . . . ?
C3 N2 C1 N1 -3.0(2) . . . . ?
C3 N2 C6 C7 -106.0(2) . . . . ?
C3 N2 C6 C11 76.8(3) . . . . ?
C4 C2 C3 N2 179.6(2) . . . . ?
C4 C2 C3 C5 -3.8(4) . . . . ?
C6 N2 C1 Pd1 -16.9(3) . . . . ?
C6 N2 C1 N1 176.46(17) . . . . ?
C6 N2 C3 C2 -177.13(18) . . . . ?
C6 N2 C3 C5 5.9(3) . . . . ?
C6 C7 C8 C9 1.0(4) . . . . ?
C6 C11 C12 C13 -125.9(2) . . . . ?
C6 C11 C12 C14 110.1(3) . . . . ?
C7 C6 C11 C10 -1.0(3) . . . . ?
C7 C6 C11 C12 178.9(2) . . . . ?
C7 C8 C9 C10 -1.0(4) . . . . ?
C8 C9 C10 C11 -0.1(4) . . . . ?
C9 C10 C11 C6 1.1(3) . . . . ?
C9 C10 C11 C12 -178.9(2) . . . . ?
C10 C11 C12 C13 54.1(3) . . . . ?
C10 C11 C12 C14 -69.9(3) . . . . ?
C11 C6 C7 C8 0.0(3) . . . . ?
C15 N1 C1 Pd1 17.0(3) . . . . ?
C15 N1 C1 N2 -177.58(17) . . . . ?
C15 N1 C2 C3 178.88(18) . . . . ?
C15 N1 C2 C4 -1.2(3) . . . . ?
C15 C16 C17 C18 -1.1(4) . . . . ?
C15 C20 C21 C22 -130.8(3) . . . . ?
C15 C20 C21 C23 103.6(3) . . . . ?
C16 C15 C20 C19 -1.8(3) . . . . ?
C16 C15 C20 C21 179.4(2) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
C17 C18 C19 C20 0.8(5) . . . . ?
C18 C19 C20 C15 0.3(4) . . . . ?
C18 C19 C20 C21 179.1(3) . . . . ?
C19 C20 C21 C22 50.5(4) . . . . ?
C19 C20 C21 C23 -75.1(4) . . . . ?
C20 C15 C16 C17 2.2(3) . . . . ?
C24 C25 C26 Pd1 55.2(2) . . . . ?


_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 0.745
####################################################################### 
# 
# 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_lk4061meso
_database_code_depnum_ccdc_archive 'CCDC 2250214'
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi'
;Aix Marseille University CNRS
France
;
_audit_update_record             
;
2023-03-20 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2019-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C50 H49 Cl N2 Pd, C6 H13.5'
_chemical_formula_sum            'C56 H62.50 Cl N2 Pd'
_chemical_formula_weight         905.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c50 h50 Cl2 n2 Pd1'
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      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                   9.9780(2)
_cell_length_b                   33.5142(7)
_cell_length_c                   15.1164(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.002(2)
_cell_angle_gamma                90
_cell_volume                     5051.91(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    30503
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.8480
_cell_measurement_theta_min      3.3410
_shelx_estimated_absorpt_T_max   0.964
_shelx_estimated_absorpt_T_min   0.804
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1902
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            93978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.635
_diffrn_reflns_theta_min         2.780
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  33.00   1.00   30.00    --   -7.86 -99.00   0.00   53
  2  ω    -32.00  66.00   1.00   30.00    --   -7.86  38.00-120.00   98
  3  ω    -16.00  83.00   1.00   30.00    --    8.41  38.00-150.00   99
  4  ω    -64.00  37.00   1.00   30.00    --    8.41 -57.00  60.00  101
  5  ω    -64.00  37.00   1.00   30.00    --    8.41 -57.00 -90.00  101
  6  ω    -32.00  66.00   1.00   30.00    --   -7.86  38.00 150.00   98
  7  ω    -20.00  33.00   1.00   30.00    --   -7.86 -99.00 -60.00   53
  8  ω    -20.00  33.00   1.00   30.00    --   -7.86 -99.00-150.00   53
  9  ω    -20.00  27.00   1.00   30.00    --    8.41 -99.00  30.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0469881000
_diffrn_orient_matrix_UB_12      0.0079096000
_diffrn_orient_matrix_UB_13      0.0315931000
_diffrn_orient_matrix_UB_21      0.0356494000
_diffrn_orient_matrix_UB_22      0.0090304000
_diffrn_orient_matrix_UB_23      -0.0345277000
_diffrn_orient_matrix_UB_31      -0.0397580000
_diffrn_orient_matrix_UB_32      0.0174385000
_diffrn_orient_matrix_UB_33      0.0035436000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7854
_reflns_number_total             11759
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         11759
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0632
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0721P)²+6.4445P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1800
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C59-C60
 1.45 with sigma of 0.02
 C60-C61
 1.45 with sigma of 0.02
 C61-C62
 1.45 with sigma of 0.02
 C62-C56
 1.45 with sigma of 0.02
 C56-C57
 1.45 with sigma of 0.02
 C52-C53
 1.45 with sigma of 0.02
 C53-C54
 1.45 with sigma of 0.02
 C54-C55
 1.45 with sigma of 0.02
 C55-C56
 1.45 with sigma of 0.02
 C57-C58
 1.54 with sigma of 0.02
 C51-C52
 1.54 with sigma of 0.02
 C51-C59
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim
C59 \\sim C60 \\sim C61 \\sim C62: within 1.7A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Pd1 \\sim C48 \\sim C49 \\sim C50: within 2.3A with sigma of 0.005 and sigma
for terminal atoms of 0.01
4. Others
 Fixed Sof: C51(0.75) H51A(0.5) H51B(0.5) H51C(0.5) H51D(0.25) H51E(0.25)
 H51F(0.25) C52(0.5) H52A(0.5) H52B(0.5) C53(0.5) H53A(0.5) H53B(0.5) C54(0.5)
 H54A(0.5) H54B(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.75) H56B(0.5) H56A(0.5)
 H56D(0.25) H56C(0.25) C57(0.75) H57A(0.75) H57B(0.75) C58(0.75) H58A(0.75)
 H58B(0.75) H58C(0.75) C59(0.25) H59A(0.25) H59B(0.25) C60(0.25) H60A(0.25)
 H60B(0.25) C61(0.25) H61A(0.25) H61B(0.25) C62(0.25) H62A(0.25) H62B(0.25)
5.a Riding coordinates:
 C48(H48B,H48A), C49(H49), C50(H50B,H50A)
5.b Ternary CH refined with riding coordinates:
 C14(H14), C35(H35)
5.c Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56B,
 H56A), C56(H56D,H56C), C57(H57A,H57B), C59(H59A,H59B), C60(H60A,H60B),
 C61(H61A,H61B), C62(H62A,H62B)
5.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C31(H31), C37(H37), C38(H38),
  C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47)
5.e Idealised Me refined with riding coordinates:
 C51(H51A,H51B,H51C), C51(H51D,H51E,H51F), C58(H58A,H58B,H58C)
5.f Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.65486(3) 0.37129(2) 0.11984(2) 0.05656(13) Uani 1 1 d . U . . .
Cl1 Cl 0.78107(10) 0.35617(4) 0.24989(9) 0.0686(3) Uani 1 1 d . . . . .
N1 N 0.3992(3) 0.39396(9) 0.21755(19) 0.0435(7) Uani 1 1 d . . . . .
N2 N 0.3893(3) 0.33389(9) 0.16826(18) 0.0408(6) Uani 1 1 d . . . . .
C1 C 0.4708(4) 0.36628(10) 0.1733(2) 0.0411(8) Uani 1 1 d . . . . .
C2 C 0.2651(4) 0.34177(12) 0.2063(2) 0.0472(9) Uani 1 1 d . . . . .
C3 C 0.2714(4) 0.37945(12) 0.2367(2) 0.0478(9) Uani 1 1 d . . . . .
C4 C 0.1521(4) 0.31284(14) 0.2087(3) 0.0640(11) Uani 1 1 d . . . . .
H4A H 0.150155 0.296991 0.155794 0.096 Uiso 1 1 calc GR . . . .
H4B H 0.069027 0.327089 0.212557 0.096 Uiso 1 1 calc GR . . . .
H4C H 0.164184 0.295764 0.259374 0.096 Uiso 1 1 calc GR . . . .
C5 C 0.1662(4) 0.40329(15) 0.2813(3) 0.0671(12) Uani 1 1 d . . . . .
H5A H 0.173811 0.399045 0.344077 0.101 Uiso 1 1 calc GR . . . .
H5B H 0.079030 0.395001 0.259640 0.101 Uiso 1 1 calc GR . . . .
H5C H 0.178458 0.431104 0.268728 0.101 Uiso 1 1 calc GR . . . .
C6 C 0.4387(4) 0.43523(11) 0.2276(3) 0.0473(9) Uani 1 1 d . . . . .
C7 C 0.5107(3) 0.44794(10) 0.3030(2) 0.0408(8) Uani 1 1 d . . . . .
C8 C 0.5433(4) 0.48848(11) 0.3088(3) 0.0495(9) Uani 1 1 d . . . . .
H8 H 0.592356 0.497491 0.358265 0.059 Uiso 1 1 calc R . . . .
C9 C 0.5052(4) 0.51572(12) 0.2437(3) 0.0574(10) Uani 1 1 d . . . . .
C10 C 0.4327(5) 0.50190(14) 0.1706(3) 0.0682(12) Uani 1 1 d . . . . .
H10 H 0.406110 0.519848 0.126482 0.082 Uiso 1 1 calc R . . . .
C11 C 0.3979(5) 0.46170(13) 0.1610(3) 0.0629(11) Uani 1 1 d . . . . .
C12 C 0.5438(6) 0.55910(13) 0.2519(4) 0.0778(14) Uani 1 1 d . . . . .
H12A H 0.551691 0.566271 0.313374 0.117 Uiso 1 1 calc GR . . . .
H12B H 0.476034 0.575272 0.222939 0.117 Uiso 1 1 calc GR . . . .
H12C H 0.628057 0.563381 0.224712 0.117 Uiso 1 1 calc GR . . . .
C13 C 0.3180(7) 0.44816(18) 0.0802(4) 0.099(2) Uani 1 1 d . . . . .
H13A H 0.365012 0.427014 0.051711 0.148 Uiso 1 1 calc GR . . . .
H13B H 0.306187 0.470137 0.039920 0.148 Uiso 1 1 calc GR . . . .
H13C H 0.231922 0.438710 0.097372 0.148 Uiso 1 1 calc GR . . . .
C14 C 0.5503(3) 0.41915(10) 0.3776(2) 0.0394(7) Uani 1 1 d . . . . .
H14 H 0.579961 0.394455 0.349590 0.047 Uiso 1 1 calc R . . . .
C15 C 0.6693(3) 0.43450(10) 0.4352(2) 0.0416(8) Uani 1 1 d . . . . .
C16 C 0.6574(4) 0.44877(12) 0.5195(3) 0.0503(9) Uani 1 1 d . . . . .
H16 H 0.573672 0.448875 0.544603 0.060 Uiso 1 1 calc R . . . .
C17 C 0.7674(4) 0.46304(13) 0.5682(3) 0.0574(10) Uani 1 1 d . . . . .
H17 H 0.756551 0.472958 0.624923 0.069 Uiso 1 1 calc R . . . .
C18 C 0.8911(4) 0.46262(13) 0.5334(3) 0.0617(11) Uani 1 1 d . . . . .
H18 H 0.965230 0.471836 0.566360 0.074 Uiso 1 1 calc R . . . .
C19 C 0.9055(4) 0.44848(15) 0.4493(3) 0.0708(13) Uani 1 1 d . . . . .
H19 H 0.989779 0.448375 0.424833 0.085 Uiso 1 1 calc R . . . .
C20 C 0.7958(4) 0.43436(14) 0.4004(3) 0.0588(10) Uani 1 1 d . . . . .
H20 H 0.807060 0.424677 0.343456 0.071 Uiso 1 1 calc R . . . .
C21 C 0.4312(3) 0.40830(11) 0.4327(2) 0.0425(8) Uani 1 1 d . . . . .
C22 C 0.4039(4) 0.36895(12) 0.4526(3) 0.0592(11) Uani 1 1 d . . . . .
H22 H 0.456146 0.348777 0.429324 0.071 Uiso 1 1 calc R . . . .
C23 C 0.2999(5) 0.35924(18) 0.5065(4) 0.0820(15) Uani 1 1 d . . . . .
H23 H 0.282576 0.332538 0.518300 0.098 Uiso 1 1 calc R . . . .
C24 C 0.2227(5) 0.3878(2) 0.5425(4) 0.0849(16) Uani 1 1 d . . . . .
H24 H 0.153979 0.380916 0.579609 0.102 Uiso 1 1 calc R . . . .
C25 C 0.2481(4) 0.42736(18) 0.5228(3) 0.0705(13) Uani 1 1 d . . . . .
H25 H 0.195832 0.447305 0.546898 0.085 Uiso 1 1 calc R . . . .
C26 C 0.3502(4) 0.43751(13) 0.4679(3) 0.0540(10) Uani 1 1 d . . . . .
H26 H 0.364936 0.464188 0.454319 0.065 Uiso 1 1 calc R . . . .
C27 C 0.4120(3) 0.30025(11) 0.1101(2) 0.0409(8) Uani 1 1 d . . . . .
C28 C 0.4954(3) 0.26858(10) 0.1365(2) 0.0390(7) Uani 1 1 d . . . . .
C29 C 0.5114(4) 0.23804(11) 0.0757(2) 0.0455(8) Uani 1 1 d . . . . .
H29 H 0.566826 0.216739 0.091655 0.055 Uiso 1 1 calc R . . . .
C30 C 0.4489(4) 0.23772(12) -0.0075(2) 0.0499(9) Uani 1 1 d . . . . .
C31 C 0.3668(4) 0.26945(13) -0.0299(2) 0.0557(10) Uani 1 1 d . . . . .
H31 H 0.323259 0.269673 -0.085340 0.067 Uiso 1 1 calc R . . . .
C32 C 0.3469(4) 0.30092(12) 0.0271(2) 0.0519(9) Uani 1 1 d . . . . .
C33 C 0.4703(5) 0.20369(15) -0.0708(3) 0.0725(13) Uani 1 1 d . . . . .
H33A H 0.562602 0.203006 -0.086509 0.109 Uiso 1 1 calc GR . . . .
H33B H 0.414401 0.207429 -0.123108 0.109 Uiso 1 1 calc GR . . . .
H33C H 0.447340 0.178982 -0.042943 0.109 Uiso 1 1 calc GR . . . .
C34 C 0.2565(6) 0.33506(15) -0.0029(3) 0.0765(14) Uani 1 1 d . . . . .
H34A H 0.212505 0.345895 0.047212 0.115 Uiso 1 1 calc GR . . . .
H34B H 0.190521 0.325426 -0.045410 0.115 Uiso 1 1 calc GR . . . .
H34C H 0.309347 0.355466 -0.029444 0.115 Uiso 1 1 calc GR . . . .
C35 C 0.5667(3) 0.26725(11) 0.2279(2) 0.0403(8) Uani 1 1 d . . . . .
H35 H 0.604088 0.293884 0.239071 0.048 Uiso 1 1 calc R . . . .
C36 C 0.6853(3) 0.23782(11) 0.2302(2) 0.0417(8) Uani 1 1 d . . . . .
C37 C 0.6690(4) 0.19789(11) 0.2529(3) 0.0511(9) Uani 1 1 d . . . . .
H37 H 0.585109 0.188745 0.268713 0.061 Uiso 1 1 calc R . . . .
C38 C 0.7754(5) 0.17183(13) 0.2523(3) 0.0612(11) Uani 1 1 d . . . . .
H38 H 0.762237 0.145155 0.266530 0.073 Uiso 1 1 calc R . . . .
C39 C 0.9002(5) 0.18461(15) 0.2309(3) 0.0663(12) Uani 1 1 d . . . . .
H39 H 0.971814 0.166859 0.231090 0.080 Uiso 1 1 calc R . . . .
C40 C 0.9186(4) 0.22393(14) 0.2093(3) 0.0626(11) Uani 1 1 d . . . . .
H40 H 1.003486 0.232866 0.195154 0.075 Uiso 1 1 calc R . . . .
C41 C 0.8121(4) 0.25049(13) 0.2083(3) 0.0514(9) Uani 1 1 d . . . . .
H41 H 0.825800 0.276998 0.192855 0.062 Uiso 1 1 calc R . . . .
C42 C 0.4743(4) 0.25804(11) 0.3033(2) 0.0460(8) Uani 1 1 d . . . . .
C43 C 0.5164(5) 0.26876(14) 0.3886(3) 0.0636(11) Uani 1 1 d . . . . .
H43 H 0.595958 0.282877 0.397547 0.076 Uiso 1 1 calc R . . . .
C44 C 0.4416(7) 0.25872(18) 0.4602(3) 0.0851(17) Uani 1 1 d . . . . .
H44 H 0.471783 0.265658 0.517004 0.102 Uiso 1 1 calc R . . . .
C45 C 0.3231(7) 0.23864(19) 0.4481(3) 0.0897(18) Uani 1 1 d . . . . .
H45 H 0.272002 0.232432 0.496552 0.108 Uiso 1 1 calc R . . . .
C46 C 0.2802(5) 0.22773(17) 0.3652(4) 0.0788(14) Uani 1 1 d . . . . .
H46 H 0.200367 0.213656 0.357080 0.095 Uiso 1 1 calc R . . . .
C47 C 0.3554(4) 0.23759(13) 0.2926(3) 0.0599(10) Uani 1 1 d . . . . .
H47 H 0.324946 0.230261 0.236051 0.072 Uiso 1 1 calc R . . . .
C48 C 0.8269(7) 0.3755(2) 0.0343(4) 0.1052(15) Uani 1 1 d . U . . .
H48B H 0.821566 0.352553 0.059338 0.126 Uiso 1 1 d R . . . .
H48A H 0.902386 0.387853 0.034028 0.126 Uiso 1 1 d R . . . .
C49 C 0.7195(7) 0.3911(3) -0.0034(4) 0.1143(14) Uani 1 1 d . U . . .
H49 H 0.736501 0.415894 -0.028412 0.137 Uiso 1 1 d R . . . .
C50 C 0.5953(7) 0.3806(2) -0.0154(4) 0.1110(15) Uani 1 1 d . U . . .
H50B H 0.569454 0.358076 0.005464 0.133 Uiso 1 1 d R . . . .
H50A H 0.538694 0.395836 -0.043056 0.133 Uiso 1 1 d R . . . .
C51 C 0.2137(8) 0.1634(3) 0.0935(6) 0.102(2) Uani 0.75 1 d D U P . .
H51A H 0.214058 0.162719 0.030069 0.153 Uiso 0.5 1 calc R . P A 1
H51B H 0.217116 0.190643 0.113315 0.153 Uiso 0.5 1 calc R . P A 1
H51C H 0.133266 0.151085 0.113349 0.153 Uiso 0.5 1 calc R . P A 1
H51D H 0.222035 0.146913 0.042143 0.153 Uiso 0.25 1 calc R . P B 2
H51E H 0.279657 0.184272 0.092968 0.153 Uiso 0.25 1 calc R . P B 2
H51F H 0.125671 0.175002 0.093176 0.153 Uiso 0.25 1 calc R . P B 2
C52 C 0.3343(12) 0.1411(4) 0.1312(9) 0.106(2) Uani 0.5 1 d D U P C 1
H52A H 0.356539 0.120207 0.089884 0.128 Uiso 0.5 1 calc R . P C 1
H52B H 0.409578 0.159464 0.134613 0.128 Uiso 0.5 1 calc R . P C 1
C53 C 0.3204(15) 0.1235(5) 0.2164(11) 0.114(2) Uani 0.5 1 d D U P C 1
H53A H 0.242307 0.106283 0.214787 0.137 Uiso 0.5 1 calc R . P C 1
H53B H 0.305756 0.144422 0.259359 0.137 Uiso 0.5 1 calc R . P C 1
C54 C 0.4388(15) 0.1002(5) 0.2447(12) 0.125(2) Uani 0.5 1 d D U P C 1
H54A H 0.470538 0.086378 0.193084 0.150 Uiso 0.5 1 calc R . P C 1
H54B H 0.508391 0.118899 0.263405 0.150 Uiso 0.5 1 calc R . P C 1
C55 C 0.4269(16) 0.0715(5) 0.3133(12) 0.137(2) Uani 0.5 1 d D U P C 1
H55A H 0.360423 0.052273 0.292378 0.164 Uiso 0.5 1 calc R . P C 1
H55B H 0.388572 0.085322 0.362822 0.164 Uiso 0.5 1 calc R . P C 1
C56 C 0.5413(13) 0.0486(4) 0.3492(9) 0.152(2) Uani 0.75 1 d D U P . .
H56B H 0.621527 0.064769 0.345338 0.182 Uiso 0.5 1 calc R . P C 1
H56A H 0.527676 0.043436 0.411364 0.182 Uiso 0.5 1 calc R . P C 1
H56D H 0.618508 0.053754 0.388299 0.182 Uiso 0.25 1 calc R . P C 2
H56C H 0.464661 0.045304 0.386238 0.182 Uiso 0.25 1 calc R . P C 2
C57 C 0.5632(14) 0.0118(4) 0.3062(10) 0.167(3) Uani 0.75 1 d D U P C .
H57A H 0.476236 0.000321 0.290929 0.201 Uiso 0.75 1 calc R . P . .
H57B H 0.606584 0.017454 0.251195 0.201 Uiso 0.75 1 calc R . P . .
C58 C 0.6397(15) -0.0173(4) 0.3521(10) 0.183(4) Uani 0.75 1 d D U P . .
H58A H 0.684520 -0.033790 0.310382 0.274 Uiso 0.75 1 calc R . P C .
H58B H 0.581699 -0.033560 0.386459 0.274 Uiso 0.75 1 calc R . P . .
H58C H 0.704957 -0.004531 0.390636 0.274 Uiso 0.75 1 calc R . P . .
C59 C 0.235(2) 0.1387(7) 0.1750(15) 0.108(2) Uani 0.25 1 d D U P C 2
H59A H 0.205372 0.153969 0.225184 0.129 Uiso 0.25 1 calc R . P C 2
H59B H 0.178064 0.115302 0.169612 0.129 Uiso 0.25 1 calc R . P C 2
C60 C 0.368(2) 0.1258(10) 0.194(2) 0.114(2) Uani 0.25 1 d D U P C 2
H60A H 0.424432 0.149129 0.201542 0.137 Uiso 0.25 1 calc R . P C 2
H60B H 0.398639 0.111152 0.143256 0.137 Uiso 0.25 1 calc R . P C 2
C61 C 0.386(3) 0.1006(11) 0.272(2) 0.125(2) Uani 0.25 1 d D U P C 2
H61A H 0.324100 0.078364 0.265538 0.150 Uiso 0.25 1 calc R . P C 2
H61B H 0.357519 0.116020 0.322725 0.150 Uiso 0.25 1 calc R . P C 2
C62 C 0.518(3) 0.0843(8) 0.295(2) 0.135(2) Uani 0.25 1 d D U P C 2
H62A H 0.568492 0.105631 0.323767 0.162 Uiso 0.25 1 calc R . P C 2
H62B H 0.560384 0.079298 0.239181 0.162 Uiso 0.25 1 calc R . P C 2


_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 2.3526(13) . ?
Pd1 C1 2.039(4) . ?
Pd1 C48 2.189(5) . ?
Pd1 H48B 2.0258 . ?
Pd1 C49 2.101(6) . ?
Pd1 C50 2.131(6) . ?
Pd1 H50B 1.9516 . ?
N1 C1 1.361(5) . ?
N1 C3 1.404(5) . ?
N1 C6 1.445(5) . ?
N2 C1 1.357(4) . ?
N2 C2 1.410(5) . ?
N2 C27 1.452(4) . ?
C2 C3 1.344(5) . ?
C2 C4 1.488(5) . ?
C3 C5 1.497(5) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.392(5) . ?
C6 C11 1.392(6) . ?
C7 C8 1.399(5) . ?
C7 C14 1.526(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.385(6) . ?
C9 C10 1.380(6) . ?
C9 C12 1.508(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.397(6) . ?
C11 C13 1.505(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14 0.9800 . ?
C14 C15 1.536(5) . ?
C14 C21 1.519(5) . ?
C15 C16 1.370(5) . ?
C15 C20 1.384(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.385(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.358(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.369(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.383(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(5) . ?
C21 C26 1.387(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.380(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.354(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.385(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.379(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.398(5) . ?
C27 C32 1.393(5) . ?
C28 C29 1.388(5) . ?
C28 C35 1.532(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.383(5) . ?
C30 C31 1.378(6) . ?
C30 C33 1.508(6) . ?
C31 H31 0.9300 . ?
C31 C32 1.381(6) . ?
C32 C34 1.516(6) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35 0.9800 . ?
C35 C36 1.540(5) . ?
C35 C42 1.523(5) . ?
C36 C37 1.393(5) . ?
C36 C41 1.385(5) . ?
C37 H37 0.9300 . ?
C37 C38 1.375(6) . ?
C38 H38 0.9300 . ?
C38 C39 1.366(6) . ?
C39 H39 0.9300 . ?
C39 C40 1.372(7) . ?
C40 H40 0.9300 . ?
C40 C41 1.386(6) . ?
C41 H41 0.9300 . ?
C42 C43 1.389(5) . ?
C42 C47 1.375(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.377(7) . ?
C44 H44 0.9300 . ?
C44 C45 1.367(8) . ?
C45 H45 0.9300 . ?
C45 C46 1.360(8) . ?
C46 H46 0.9300 . ?
C46 C47 1.392(6) . ?
C47 H47 0.9300 . ?
C48 H48B 0.8594 . ?
C48 H48A 0.8602 . ?
C48 C49 1.305(9) . ?
C49 H49 0.9305 . ?
C49 C50 1.296(9) . ?
C50 H50B 0.8599 . ?
C50 H50A 0.8600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C51 H51D 0.9600 . ?
C51 H51E 0.9600 . ?
C51 H51F 0.9600 . ?
C51 C52 1.510(13) . ?
C51 C59 1.494(17) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.428(14) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C53 C54 1.468(15) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 C55 1.421(15) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C55 C56 1.465(14) . ?
C56 H56B 0.9700 . ?
C56 H56A 0.9700 . ?
C56 H56D 0.9700 . ?
C56 H56C 0.9700 . ?
C56 C57 1.413(13) . ?
C56 C62 1.465(18) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C57 C58 1.408(13) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 C60 1.412(18) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C60 C61 1.459(19) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C61 C62 1.459(18) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?

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 H48B 83.5 . . ?
Cl1 Pd1 H50B 153.6 . . ?
C1 Pd1 Cl1 96.57(10) . . ?
C1 Pd1 C48 167.1(2) . . ?
C1 Pd1 H48B 156.7 . . ?
C1 Pd1 C49 133.3(2) . . ?
C1 Pd1 C50 99.6(2) . . ?
C1 Pd1 H50B 87.8 . . ?
C48 Pd1 Cl1 95.73(19) . . ?
C48 Pd1 H48B 23.1 . . ?
C48 Pd1 H50B 79.5 . . ?
H48B Pd1 H50B 82.5 . . ?
C49 Pd1 Cl1 129.6(2) . . ?
C49 Pd1 C48 35.3(2) . . ?
C49 Pd1 H48B 54.2 . . ?
C49 Pd1 C50 35.7(2) . . ?
C49 Pd1 H50B 54.8 . . ?
C50 Pd1 Cl1 162.94(19) . . ?
C50 Pd1 C48 67.8(3) . . ?
C50 Pd1 H48B 79.5 . . ?
C50 Pd1 H50B 23.8 . . ?
C1 N1 C3 111.2(3) . . ?
C1 N1 C6 123.9(3) . . ?
C3 N1 C6 123.8(3) . . ?
C1 N2 C2 111.2(3) . . ?
C1 N2 C27 123.3(3) . . ?
C2 N2 C27 123.4(3) . . ?
N1 C1 Pd1 129.4(3) . . ?
N2 C1 Pd1 126.2(3) . . ?
N2 C1 N1 104.4(3) . . ?
N2 C2 C4 124.4(4) . . ?
C3 C2 N2 106.5(3) . . ?
C3 C2 C4 129.1(4) . . ?
N1 C3 C5 124.3(4) . . ?
C2 C3 N1 106.7(3) . . ?
C2 C3 C5 129.0(4) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 120.7(3) . . ?
C7 C6 C11 121.8(4) . . ?
C11 C6 N1 117.5(3) . . ?
C6 C7 C8 117.4(3) . . ?
C6 C7 C14 121.6(3) . . ?
C8 C7 C14 120.9(3) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 C7 122.6(4) . . ?
C9 C8 H8 118.7 . . ?
C8 C9 C12 120.9(4) . . ?
C10 C9 C8 118.1(4) . . ?
C10 C9 C12 121.0(4) . . ?
C9 C10 H10 119.0 . . ?
C9 C10 C11 121.9(4) . . ?
C11 C10 H10 119.0 . . ?
C6 C11 C10 118.3(4) . . ?
C6 C11 C13 121.9(4) . . ?
C10 C11 C13 119.8(4) . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C14 H14 106.8 . . ?
C7 C14 C15 112.5(3) . . ?
C15 C14 H14 106.8 . . ?
C21 C14 C7 111.7(3) . . ?
C21 C14 H14 106.8 . . ?
C21 C14 C15 111.9(3) . . ?
C16 C15 C14 123.6(3) . . ?
C16 C15 C20 117.7(3) . . ?
C20 C15 C14 118.7(3) . . ?
C15 C16 H16 119.3 . . ?
C15 C16 C17 121.5(4) . . ?
C17 C16 H16 119.3 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.3(4) . . ?
C18 C17 H17 119.8 . . ?
C17 C18 H18 120.4 . . ?
C17 C18 C19 119.3(4) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.5(4) . . ?
C20 C19 H19 119.7 . . ?
C15 C20 H20 119.6 . . ?
C19 C20 C15 120.7(4) . . ?
C19 C20 H20 119.6 . . ?
C22 C21 C14 120.8(3) . . ?
C22 C21 C26 117.9(4) . . ?
C26 C21 C14 121.2(3) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.7(4) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.4(5) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 120.7 . . ?
C23 C24 C25 118.6(4) . . ?
C25 C24 H24 120.7 . . ?
C24 C25 H25 119.7 . . ?
C26 C25 C24 120.7(5) . . ?
C26 C25 H25 119.7 . . ?
C21 C26 H26 119.7 . . ?
C25 C26 C21 120.6(4) . . ?
C25 C26 H26 119.7 . . ?
C28 C27 N2 121.4(3) . . ?
C32 C27 N2 117.1(3) . . ?
C32 C27 C28 121.6(3) . . ?
C27 C28 C35 122.1(3) . . ?
C29 C28 C27 116.9(3) . . ?
C29 C28 C35 121.0(3) . . ?
C28 C29 H29 118.4 . . ?
C30 C29 C28 123.3(4) . . ?
C30 C29 H29 118.4 . . ?
C29 C30 C33 120.9(4) . . ?
C31 C30 C29 117.6(3) . . ?
C31 C30 C33 121.5(4) . . ?
C30 C31 H31 118.9 . . ?
C30 C31 C32 122.2(3) . . ?
C32 C31 H31 118.9 . . ?
C27 C32 C34 122.4(4) . . ?
C31 C32 C27 118.5(4) . . ?
C31 C32 C34 119.1(4) . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C28 C35 H35 107.0 . . ?
C28 C35 C36 111.8(3) . . ?
C36 C35 H35 107.0 . . ?
C42 C35 C28 114.1(3) . . ?
C42 C35 H35 107.0 . . ?
C42 C35 C36 109.7(3) . . ?
C37 C36 C35 121.6(3) . . ?
C41 C36 C35 120.4(3) . . ?
C41 C36 C37 118.0(3) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 C36 120.8(4) . . ?
C38 C37 H37 119.6 . . ?
C37 C38 H38 119.6 . . ?
C39 C38 C37 120.9(4) . . ?
C39 C38 H38 119.6 . . ?
C38 C39 H39 120.4 . . ?
C38 C39 C40 119.3(4) . . ?
C40 C39 H39 120.4 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.7(4) . . ?
C41 C40 H40 119.7 . . ?
C36 C41 C40 120.5(4) . . ?
C36 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C43 C42 C35 118.2(4) . . ?
C47 C42 C35 123.7(3) . . ?
C47 C42 C43 118.0(4) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 C42 120.7(5) . . ?
C44 C43 H43 119.6 . . ?
C43 C44 H44 119.8 . . ?
C45 C44 C43 120.4(5) . . ?
C45 C44 H44 119.8 . . ?
C44 C45 H45 120.1 . . ?
C46 C45 C44 119.9(5) . . ?
C46 C45 H45 120.1 . . ?
C45 C46 H46 119.9 . . ?
C45 C46 C47 120.1(5) . . ?
C47 C46 H46 119.9 . . ?
C42 C47 C46 120.8(4) . . ?
C42 C47 H47 119.6 . . ?
C46 C47 H47 119.6 . . ?
Pd1 C48 H48B 67.7 . . ?
Pd1 C48 H48A 137.6 . . ?
H48B C48 H48A 120.0 . . ?
C49 C48 Pd1 68.6(4) . . ?
C49 C48 H48B 119.3 . . ?
C49 C48 H48A 120.7 . . ?
Pd1 C49 H49 135.1 . . ?
C48 C49 Pd1 76.1(4) . . ?
C48 C49 H49 112.2 . . ?
C50 C49 Pd1 73.5(4) . . ?
C50 C49 C48 135.9(8) . . ?
C50 C49 H49 111.9 . . ?
Pd1 C50 H50B 66.3 . . ?
Pd1 C50 H50A 135.2 . . ?
C49 C50 Pd1 70.9(4) . . ?
C49 C50 H50B 119.1 . . ?
C49 C50 H50A 121.0 . . ?
H50B C50 H50A 120.0 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
H51D C51 H51E 109.5 . . ?
H51D C51 H51F 109.5 . . ?
H51E C51 H51F 109.5 . . ?
C52 C51 H51A 109.5 . . ?
C52 C51 H51B 109.5 . . ?
C52 C51 H51C 109.5 . . ?
C59 C51 H51D 109.5 . . ?
C59 C51 H51E 109.5 . . ?
C59 C51 H51F 109.5 . . ?
C51 C52 H52A 108.2 . . ?
C51 C52 H52B 108.2 . . ?
H52A C52 H52B 107.4 . . ?
C53 C52 C51 116.3(11) . . ?
C53 C52 H52A 108.2 . . ?
C53 C52 H52B 108.2 . . ?
C52 C53 H53A 109.1 . . ?
C52 C53 H53B 109.1 . . ?
C52 C53 C54 112.4(13) . . ?
H53A C53 H53B 107.9 . . ?
C54 C53 H53A 109.1 . . ?
C54 C53 H53B 109.1 . . ?
C53 C54 H54A 107.6 . . ?
C53 C54 H54B 107.6 . . ?
H54A C54 H54B 107.0 . . ?
C55 C54 C53 119.1(14) . . ?
C55 C54 H54A 107.6 . . ?
C55 C54 H54B 107.6 . . ?
C54 C55 H55A 106.6 . . ?
C54 C55 H55B 106.6 . . ?
C54 C55 C56 122.7(14) . . ?
C56 C55 H55A 106.6 . . ?
C56 C55 H55B 106.6 . . ?
C55 C56 H56B 108.6 . . ?
C55 C56 H56A 108.6 . . ?
H56B C56 H56A 107.6 . . ?
H56D C56 H56C 107.1 . . ?
C57 C56 C55 114.7(13) . . ?
C57 C56 H56B 108.6 . . ?
C57 C56 H56A 108.6 . . ?
C57 C56 H56D 107.7 . . ?
C57 C56 H56C 107.7 . . ?
C57 C56 C62 118.6(19) . . ?
C62 C56 H56D 107.7 . . ?
C62 C56 H56C 107.7 . . ?
C56 C57 H57A 107.8 . . ?
C56 C57 H57B 107.8 . . ?
H57A C57 H57B 107.1 . . ?
C58 C57 C56 118.0(14) . . ?
C58 C57 H57A 107.8 . . ?
C58 C57 H57B 107.8 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C51 C59 H59A 108.2 . . ?
C51 C59 H59B 108.2 . . ?
H55A C55a H55B 106.6 . . ?
H59A C59 H59B 107.4 . . ?
C60 C59 C51 116(2) . . ?
C60 C59 H59A 108.2 . . ?
C60 C59 H59B 108.2 . . ?
C59 C60 H60A 108.4 . . ?
C59 C60 H60B 108.4 . . ?
C59 C60 C61 115(2) . . ?
H60A C60 H60B 107.5 . . ?
C61 C60 H60A 108.4 . . ?
C61 C60 H60B 108.4 . . ?
C60 C61 H61A 107.5 . . ?
C60 C61 H61B 107.5 . . ?
C60 C61 C62 119(2) . . ?
H61A C61 H61B 107.0 . . ?
C62 C61 H61A 107.5 . . ?
C62 C61 H61B 107.5 . . ?
C56 C62 H62A 106.3 . . ?
C56 C62 H62B 106.3 . . ?
C61 C62 C56 124(2) . . ?
C61 C62 H62A 106.3 . . ?
C61 C62 H62B 106.3 . . ?
H62A C62 H62B 106.4 . . ?

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
Pd1 C48 C49 C50 -47.4(9) . . . . ?
N1 C6 C7 C8 -178.9(3) . . . . ?
N1 C6 C7 C14 -0.2(5) . . . . ?
N1 C6 C11 C10 178.6(4) . . . . ?
N1 C6 C11 C13 -1.2(7) . . . . ?
N2 C2 C3 N1 -0.4(4) . . . . ?
N2 C2 C3 C5 178.5(4) . . . . ?
N2 C27 C28 C29 -179.5(3) . . . . ?
N2 C27 C28 C35 0.5(5) . . . . ?
N2 C27 C32 C31 179.7(3) . . . . ?
N2 C27 C32 C34 0.4(6) . . . . ?
C1 N1 C3 C2 1.9(4) . . . . ?
C1 N1 C3 C5 -177.2(4) . . . . ?
C1 N1 C6 C7 -94.9(4) . . . . ?
C1 N1 C6 C11 87.3(4) . . . . ?
C1 N2 C2 C3 -1.1(4) . . . . ?
C1 N2 C2 C4 177.9(4) . . . . ?
C1 N2 C27 C28 86.4(4) . . . . ?
C1 N2 C27 C32 -93.7(4) . . . . ?
C2 N2 C1 Pd1 -175.2(2) . . . . ?
C2 N2 C1 N1 2.2(4) . . . . ?
C2 N2 C27 C28 -111.6(4) . . . . ?
C2 N2 C27 C32 68.3(4) . . . . ?
C3 N1 C1 Pd1 174.8(3) . . . . ?
C3 N1 C1 N2 -2.5(4) . . . . ?
C3 N1 C6 C7 98.0(4) . . . . ?
C3 N1 C6 C11 -79.8(5) . . . . ?
C4 C2 C3 N1 -179.4(4) . . . . ?
C4 C2 C3 C5 -0.4(7) . . . . ?
C6 N1 C1 Pd1 6.3(5) . . . . ?
C6 N1 C1 N2 -171.0(3) . . . . ?
C6 N1 C3 C2 170.4(3) . . . . ?
C6 N1 C3 C5 -8.6(6) . . . . ?
C6 C7 C8 C9 0.8(6) . . . . ?
C6 C7 C14 C15 158.6(3) . . . . ?
C6 C7 C14 C21 -74.6(4) . . . . ?
C7 C6 C11 C10 0.8(7) . . . . ?
C7 C6 C11 C13 -179.0(5) . . . . ?
C7 C8 C9 C10 -0.1(6) . . . . ?
C7 C8 C9 C12 -179.3(4) . . . . ?
C7 C14 C15 C16 107.1(4) . . . . ?
C7 C14 C15 C20 -72.3(4) . . . . ?
C7 C14 C21 C22 131.3(4) . . . . ?
C7 C14 C21 C26 -51.6(4) . . . . ?
C8 C7 C14 C15 -22.8(4) . . . . ?
C8 C7 C14 C21 104.0(4) . . . . ?
C8 C9 C10 C11 -0.3(7) . . . . ?
C9 C10 C11 C6 -0.1(7) . . . . ?
C9 C10 C11 C13 179.7(5) . . . . ?
C11 C6 C7 C8 -1.2(6) . . . . ?
C11 C6 C7 C14 177.5(4) . . . . ?
C12 C9 C10 C11 178.9(5) . . . . ?
C14 C7 C8 C9 -177.9(3) . . . . ?
C14 C15 C16 C17 -178.7(4) . . . . ?
C14 C15 C20 C19 179.0(4) . . . . ?
C14 C21 C22 C23 176.6(4) . . . . ?
C14 C21 C26 C25 -175.5(3) . . . . ?
C15 C14 C21 C22 -101.6(4) . . . . ?
C15 C14 C21 C26 75.5(4) . . . . ?
C15 C16 C17 C18 -1.0(6) . . . . ?
C16 C15 C20 C19 -0.5(6) . . . . ?
C16 C17 C18 C19 0.9(7) . . . . ?
C17 C18 C19 C20 -0.7(8) . . . . ?
C18 C19 C20 C15 0.4(7) . . . . ?
C20 C15 C16 C17 0.7(6) . . . . ?
C21 C14 C15 C16 -19.5(5) . . . . ?
C21 C14 C15 C20 161.1(3) . . . . ?
C21 C22 C23 C24 -0.9(8) . . . . ?
C22 C21 C26 C25 1.7(6) . . . . ?
C22 C23 C24 C25 1.2(8) . . . . ?
C23 C24 C25 C26 -0.2(8) . . . . ?
C24 C25 C26 C21 -1.3(7) . . . . ?
C26 C21 C22 C23 -0.6(6) . . . . ?
C27 N2 C1 Pd1 -11.3(5) . . . . ?
C27 N2 C1 N1 166.1(3) . . . . ?
C27 N2 C2 C3 -165.0(3) . . . . ?
C27 N2 C2 C4 14.0(5) . . . . ?
C27 C28 C29 C30 -0.4(5) . . . . ?
C27 C28 C35 C36 -161.2(3) . . . . ?
C27 C28 C35 C42 73.5(4) . . . . ?
C28 C27 C32 C31 -0.4(6) . . . . ?
C28 C27 C32 C34 -179.7(4) . . . . ?
C28 C29 C30 C31 -0.2(6) . . . . ?
C28 C29 C30 C33 179.9(4) . . . . ?
C28 C35 C36 C37 -90.1(4) . . . . ?
C28 C35 C36 C41 89.1(4) . . . . ?
C28 C35 C42 C43 -159.2(3) . . . . ?
C28 C35 C42 C47 24.8(5) . . . . ?
C29 C28 C35 C36 18.7(4) . . . . ?
C29 C28 C35 C42 -106.5(4) . . . . ?
C29 C30 C31 C32 0.5(6) . . . . ?
C30 C31 C32 C27 -0.3(6) . . . . ?
C30 C31 C32 C34 179.1(4) . . . . ?
C32 C27 C28 C29 0.7(5) . . . . ?
C32 C27 C28 C35 -179.4(3) . . . . ?
C33 C30 C31 C32 -179.6(4) . . . . ?
C35 C28 C29 C30 179.7(3) . . . . ?
C35 C36 C37 C38 178.2(3) . . . . ?
C35 C36 C41 C40 -179.2(3) . . . . ?
C35 C42 C43 C44 -175.4(4) . . . . ?
C35 C42 C47 C46 175.5(4) . . . . ?
C36 C35 C42 C43 74.5(4) . . . . ?
C36 C35 C42 C47 -101.5(4) . . . . ?
C36 C37 C38 C39 1.2(6) . . . . ?
C37 C36 C41 C40 0.0(5) . . . . ?
C37 C38 C39 C40 -0.5(7) . . . . ?
C38 C39 C40 C41 -0.5(7) . . . . ?
C39 C40 C41 C36 0.7(6) . . . . ?
C41 C36 C37 C38 -1.0(5) . . . . ?
C42 C35 C36 C37 37.5(4) . . . . ?
C42 C35 C36 C41 -143.3(3) . . . . ?
C42 C43 C44 C45 -1.2(8) . . . . ?
C43 C42 C47 C46 -0.4(7) . . . . ?
C43 C44 C45 C46 1.4(9) . . . . ?
C44 C45 C46 C47 -1.1(9) . . . . ?
C45 C46 C47 C42 0.6(8) . . . . ?
C47 C42 C43 C44 0.7(7) . . . . ?
C48 C49 C50 Pd1 48.1(9) . . . . ?
C51 C52 C53 C54 176.0(12) . . . . ?
C51 C59 C60 C61 -178(3) . . . . ?
C52 C53 C54 C55 -161.3(15) . . . . ?
C53 C54 C55 C56 -176.4(15) . . . . ?
C54 C55 C56 C57 -91(2) . . . . ?
C55 C56 C57 C58 -159.8(14) . . . . ?
C57 C56 C62 C61 98(3) . . . . ?
C59 C60 C61 C62 177(3) . . . . ?
C60 C61 C62 C56 -157(3) . . . . ?
C62 C56 C57 C58 153.1(18) . . . . ?


_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 2.578
_oxdiff_exptl_absorpt_empirical_full_min 0.348
####################################################################### 
# 
# 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_lk31202nd
_audit_block_doi                 10.5517/ccdc.csd.cc26sbr3
_database_code_depnum_ccdc_archive 'CCDC 2049185'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/adsc.202100491 2021
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi '
;Aix Marseille University
France
;
_audit_update_record             
;
2020-12-08 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2020-07-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H45 Cl N2 Pd'
_chemical_formula_sum            'C44 H45 Cl N2 Pd'
_chemical_formula_weight         743.67
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c44 h45 Cl1 n2 Pd1'
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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   13.6877(3)
_cell_length_b                   16.4427(3)
_cell_length_c                   16.8054(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3782.27(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21489
_cell_measurement_temperature    295
_cell_measurement_theta_max      25.3840
_cell_measurement_theta_min      3.8360
_shelx_estimated_absorpt_T_max   0.932
_shelx_estimated_absorpt_T_min   0.851
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55929
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.994
_diffrn_reflns_theta_min         3.224
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00  77.00   1.00   15.00    --   -9.59   3.00-143.00  175
  2  ω    -20.00  31.00   1.00   15.00    --   -9.59 -99.00  90.00   51
  3  ω    -34.00  65.00   1.00   15.00    --   -9.59  38.00  60.00   99
  4  ω    -20.00  31.00   1.00   15.00    --   -9.59 -99.00  30.00   51
  5  ω    -14.00  84.00   1.00   15.00    --   10.05  38.00 -90.00   98
  6  ω      6.00  41.00   1.00   15.00    --   10.05-132.00-147.00   35
  7  ω    -66.00  43.00   1.00   15.00    --   10.05 -77.00 -60.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0205352000
_diffrn_orient_matrix_UB_12      0.0018995000
_diffrn_orient_matrix_UB_13      0.0387066000
_diffrn_orient_matrix_UB_21      0.0475752000
_diffrn_orient_matrix_UB_22      -0.0008019000
_diffrn_orient_matrix_UB_23      -0.0167223000
_diffrn_orient_matrix_UB_31      -0.0000745000
_diffrn_orient_matrix_UB_32      0.0430840000
_diffrn_orient_matrix_UB_33      -0.0020278000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.865
_reflns_number_gt                7145
_reflns_number_total             9003
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_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         0.575
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         9003
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0479
_refine_ls_restrained_S_all      1.029
_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)+(0.0489P)²+1.5191P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1192
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.04(4)
 -0.04(4)
2. 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
3.a Riding coordinates:
 C36(H36A,H36B), C37(H37), C38(H38)
3.b Ternary CH refined with riding coordinates:
 C14(H14)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C31(H31), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44)
3.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.49124(3) 0.56980(2) 0.52227(2) 0.05331(14) Uani 1 1 d . . . . .
Cl1 Cl 0.53410(14) 0.55839(12) 0.65743(9) 0.0844(5) Uani 1 1 d . . . . .
N1 N 0.6742(3) 0.5332(3) 0.4297(3) 0.0504(10) Uani 1 1 d . . . . .
N2 N 0.6886(3) 0.6506(3) 0.4809(3) 0.0544(10) Uani 1 1 d . . . . .
C1 C 0.6272(3) 0.5863(3) 0.4771(3) 0.0482(11) Uani 1 1 d . . . . .
C2 C 0.7719(4) 0.6379(4) 0.4347(4) 0.0605(14) Uani 1 1 d . . . . .
C3 C 0.7630(4) 0.5640(4) 0.4019(3) 0.0580(13) Uani 1 1 d . . . . .
C4 C 0.8499(5) 0.7006(4) 0.4260(5) 0.087(2) Uani 1 1 d . . . . .
H4A H 0.824015 0.747164 0.398866 0.131 Uiso 1 1 calc GR . . . .
H4B H 0.903221 0.678364 0.395891 0.131 Uiso 1 1 calc GR . . . .
H4C H 0.872810 0.716467 0.477735 0.131 Uiso 1 1 calc GR . . . .
C5 C 0.8297(5) 0.5194(4) 0.3474(4) 0.0796(19) Uani 1 1 d . . . . .
H5A H 0.876726 0.489554 0.378111 0.119 Uiso 1 1 calc GR . . . .
H5B H 0.862899 0.557490 0.313637 0.119 Uiso 1 1 calc GR . . . .
H5C H 0.792465 0.482329 0.315325 0.119 Uiso 1 1 calc GR . . . .
C6 C 0.6285(4) 0.4580(3) 0.4029(3) 0.0507(12) Uani 1 1 d . . . . .
C7 C 0.5875(4) 0.4574(4) 0.3273(3) 0.0620(14) Uani 1 1 d . . . . .
C8 C 0.5383(5) 0.3879(4) 0.3045(4) 0.0687(16) Uani 1 1 d . . . . .
H8 H 0.511248 0.385659 0.253767 0.082 Uiso 1 1 calc R . . . .
C9 C 0.5276(5) 0.3215(4) 0.3541(4) 0.0700(16) Uani 1 1 d . . . . .
C10 C 0.5719(4) 0.3239(4) 0.4288(4) 0.0597(14) Uani 1 1 d . . . . .
H10 H 0.566642 0.278946 0.462151 0.072 Uiso 1 1 calc R . . . .
C11 C 0.6232(4) 0.3912(3) 0.4546(3) 0.0523(12) Uani 1 1 d . . . . .
C12 C 0.5962(6) 0.5296(5) 0.2721(4) 0.084(2) Uani 1 1 d . . . . .
H12A H 0.587320 0.578873 0.301931 0.126 Uiso 1 1 calc GR . . . .
H12B H 0.547065 0.526078 0.231514 0.126 Uiso 1 1 calc GR . . . .
H12C H 0.659724 0.529785 0.247917 0.126 Uiso 1 1 calc GR . . . .
C13 C 0.4698(6) 0.2473(4) 0.3279(5) 0.093(2) Uani 1 1 d . . . . .
H13A H 0.401459 0.256745 0.336642 0.140 Uiso 1 1 calc GR . . . .
H13B H 0.490412 0.200827 0.358080 0.140 Uiso 1 1 calc GR . . . .
H13C H 0.481111 0.237505 0.272309 0.140 Uiso 1 1 calc GR . . . .
C14 C 0.6756(4) 0.3939(3) 0.5339(3) 0.0521(12) Uani 1 1 d . . . . .
H14 H 0.657642 0.445451 0.559232 0.063 Uiso 1 1 calc R . . . .
C15 C 0.7859(4) 0.3959(3) 0.5217(3) 0.0553(12) Uani 1 1 d . . . . .
C16 C 0.8419(4) 0.4500(4) 0.5646(4) 0.0645(14) Uani 1 1 d . . . . .
H16 H 0.811797 0.485089 0.600441 0.077 Uiso 1 1 calc R . . . .
C17 C 0.9428(6) 0.4528(5) 0.5551(5) 0.087(2) Uani 1 1 d . . . . .
H17 H 0.979134 0.489793 0.584691 0.104 Uiso 1 1 calc R . . . .
C18 C 0.9882(6) 0.4035(7) 0.5046(6) 0.106(3) Uani 1 1 d . . . . .
H18 H 1.055717 0.405690 0.499152 0.127 Uiso 1 1 calc R . . . .
C19 C 0.9353(6) 0.3499(6) 0.4610(6) 0.105(3) Uani 1 1 d . . . . .
H19 H 0.966718 0.315268 0.425512 0.126 Uiso 1 1 calc R . . . .
C20 C 0.8336(5) 0.3463(4) 0.4691(4) 0.0781(18) Uani 1 1 d . . . . .
H20 H 0.797988 0.309749 0.438349 0.094 Uiso 1 1 calc R . . . .
C21 C 0.6479(5) 0.3257(4) 0.5927(3) 0.0658(16) Uani 1 1 d . . . . .
C22 C 0.5725(7) 0.3383(5) 0.6438(5) 0.096(3) Uani 1 1 d . . . . .
H22 H 0.537365 0.386634 0.640779 0.116 Uiso 1 1 calc R . . . .
C23 C 0.5465(9) 0.2804(7) 0.7006(5) 0.132(4) Uani 1 1 d . . . . .
H23 H 0.495830 0.290681 0.736042 0.159 Uiso 1 1 calc R . . . .
C24 C 0.5956(11) 0.2093(8) 0.7037(6) 0.132(5) Uani 1 1 d . . . . .
H24 H 0.579215 0.170809 0.741968 0.159 Uiso 1 1 calc R . . . .
C25 C 0.6686(9) 0.1934(6) 0.6515(8) 0.129(4) Uani 1 1 d . . . . .
H25 H 0.700528 0.143473 0.652376 0.155 Uiso 1 1 calc R . . . .
C26 C 0.6950(6) 0.2524(5) 0.5971(6) 0.100(3) Uani 1 1 d . . . . .
H26 H 0.746358 0.242000 0.562353 0.120 Uiso 1 1 calc R . . . .
C27 C 0.6680(3) 0.7246(3) 0.5244(4) 0.0530(12) Uani 1 1 d . . . . .
C28 C 0.6167(4) 0.7856(4) 0.4855(4) 0.0627(14) Uani 1 1 d . . . . .
C29 C 0.5998(4) 0.8565(4) 0.5281(5) 0.0735(18) Uani 1 1 d . . . . .
H29 H 0.565342 0.898179 0.503265 0.088 Uiso 1 1 calc R . . . .
C30 C 0.6308(4) 0.8686(4) 0.6043(5) 0.0728(18) Uani 1 1 d . . . . .
C31 C 0.6817(5) 0.8058(4) 0.6398(4) 0.0708(16) Uani 1 1 d . . . . .
H31 H 0.702892 0.812686 0.691905 0.085 Uiso 1 1 calc R . . . .
C32 C 0.7027(4) 0.7332(3) 0.6020(4) 0.0580(13) Uani 1 1 d . . . . .
C33 C 0.5807(6) 0.7762(4) 0.4020(4) 0.083(2) Uani 1 1 d . . . . .
H33A H 0.632082 0.754694 0.369342 0.124 Uiso 1 1 calc GR . . . .
H33B H 0.560922 0.828307 0.381795 0.124 Uiso 1 1 calc GR . . . .
H33C H 0.525982 0.739719 0.401270 0.124 Uiso 1 1 calc GR . . . .
C34 C 0.6128(6) 0.9470(4) 0.6492(6) 0.102(3) Uani 1 1 d . . . . .
H34A H 0.671432 0.979056 0.649381 0.152 Uiso 1 1 calc GR . . . .
H34B H 0.594330 0.934693 0.702994 0.152 Uiso 1 1 calc GR . . . .
H34C H 0.561324 0.976909 0.623791 0.152 Uiso 1 1 calc GR . . . .
C35 C 0.7595(6) 0.6674(4) 0.6417(5) 0.085(2) Uani 1 1 d . . . . .
H35A H 0.718814 0.620230 0.647938 0.128 Uiso 1 1 calc GR . . . .
H35B H 0.780944 0.685729 0.693041 0.128 Uiso 1 1 calc GR . . . .
H35C H 0.815236 0.653727 0.609725 0.128 Uiso 1 1 calc GR . . . .
C36 C 0.4146(4) 0.5863(5) 0.4151(4) 0.086(2) Uani 1 1 d . . . . .
H36A H 0.428680 0.634005 0.432734 0.104 Uiso 1 1 d R . . . .
H36B H 0.434490 0.571505 0.368724 0.104 Uiso 1 1 d R . . . .
C37 C 0.3599(5) 0.5347(6) 0.4622(5) 0.090(2) Uani 1 1 d . . . . .
H37 H 0.344674 0.483184 0.443130 0.108 Uiso 1 1 d R . . . .
C38 C 0.3275(4) 0.5559(5) 0.5353(5) 0.090(2) Uani 1 1 d . . . . .
H38 H 0.336455 0.609941 0.549977 0.108 Uiso 1 1 d R . . . .
C39 C 0.2806(4) 0.5024(4) 0.5932(4) 0.0697(17) Uani 1 1 d . . . . .
C40 C 0.2357(6) 0.5383(5) 0.6574(5) 0.094(2) Uani 1 1 d . . . . .
H40 H 0.239812 0.594358 0.664108 0.113 Uiso 1 1 calc R . . . .
C41 C 0.1834(6) 0.4912(7) 0.7133(5) 0.105(3) Uani 1 1 d . . . . .
H41 H 0.153799 0.515391 0.757136 0.126 Uiso 1 1 calc R . . . .
C42 C 0.1774(6) 0.4107(6) 0.7016(5) 0.099(2) Uani 1 1 d . . . . .
H42 H 0.140789 0.379358 0.736815 0.118 Uiso 1 1 calc R . . . .
C43 C 0.2225(7) 0.3742(6) 0.6408(7) 0.112(3) Uani 1 1 d . . . . .
H43 H 0.218925 0.318007 0.635231 0.135 Uiso 1 1 calc R . . . .
C44 C 0.2745(7) 0.4199(6) 0.5861(6) 0.107(3) Uani 1 1 d . . . . .
H44 H 0.305812 0.394041 0.544041 0.129 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 2.3534(17) . ?
Pd1 C1 2.028(5) . ?
Pd1 C36 2.102(6) . ?
Pd1 H36A 2.0278 . ?
Pd1 C37 2.141(7) . ?
Pd1 C38 2.264(6) . ?
N1 C1 1.345(6) . ?
N1 C3 1.397(6) . ?
N1 C6 1.458(7) . ?
N2 C1 1.352(6) . ?
N2 C2 1.395(7) . ?
N2 C27 1.448(7) . ?
C2 C3 1.340(9) . ?
C2 C4 1.492(8) . ?
C3 C5 1.486(8) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.389(8) . ?
C6 C11 1.402(7) . ?
C7 C8 1.381(9) . ?
C7 C12 1.511(9) . ?
C8 H8 0.9300 . ?
C8 C9 1.381(9) . ?
C9 C10 1.395(9) . ?
C9 C13 1.519(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.381(8) . ?
C11 C14 1.514(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14 0.9800 . ?
C14 C15 1.523(7) . ?
C14 C21 1.542(8) . ?
C15 C16 1.378(8) . ?
C15 C20 1.369(8) . ?
C16 H16 0.9300 . ?
C16 C17 1.391(9) . ?
C17 H17 0.9300 . ?
C17 C18 1.328(12) . ?
C18 H18 0.9300 . ?
C18 C19 1.355(13) . ?
C19 H19 0.9300 . ?
C19 C20 1.400(11) . ?
C20 H20 0.9300 . ?
C21 C22 1.358(10) . ?
C21 C26 1.369(10) . ?
C22 H22 0.9300 . ?
C22 C23 1.395(12) . ?
C23 H23 0.9300 . ?
C23 C24 1.350(16) . ?
C24 H24 0.9300 . ?
C24 C25 1.354(16) . ?
C25 H25 0.9300 . ?
C25 C26 1.382(12) . ?
C26 H26 0.9300 . ?
C27 C28 1.387(7) . ?
C27 C32 1.396(9) . ?
C28 C29 1.388(9) . ?
C28 C33 1.495(9) . ?
C29 H29 0.9300 . ?
C29 C30 1.363(10) . ?
C30 C31 1.381(9) . ?
C30 C34 1.514(9) . ?
C31 H31 0.9300 . ?
C31 C32 1.382(8) . ?
C32 C35 1.491(8) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.8600 . ?
C36 H36B 0.8602 . ?
C36 C37 1.382(10) . ?
C37 H37 0.9301 . ?
C37 C38 1.351(11) . ?
C38 H38 0.9300 . ?
C38 C39 1.460(10) . ?
C39 C40 1.376(10) . ?
C39 C44 1.363(11) . ?
C40 H40 0.9300 . ?
C40 C41 1.413(12) . ?
C41 H41 0.9300 . ?
C41 C42 1.341(12) . ?
C42 H42 0.9300 . ?
C42 C43 1.336(12) . ?
C43 H43 0.9300 . ?
C43 C44 1.385(12) . ?
C44 H44 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pd1 H36A 149.6 . . ?
C1 Pd1 Cl1 98.23(15) . . ?
C1 Pd1 C36 96.9(2) . . ?
C1 Pd1 H36A 92.3 . . ?
C1 Pd1 C37 129.1(3) . . ?
C1 Pd1 C38 163.4(3) . . ?
C36 Pd1 Cl1 164.10(19) . . ?
C36 Pd1 H36A 23.9 . . ?
C36 Pd1 C37 38.0(3) . . ?
C36 Pd1 C38 66.5(3) . . ?
C37 Pd1 Cl1 130.0(2) . . ?
C37 Pd1 H36A 55.7 . . ?
C37 Pd1 C38 35.6(3) . . ?
C38 Pd1 Cl1 98.4(2) . . ?
C38 Pd1 H36A 72.9 . . ?
C1 N1 C3 112.3(4) . . ?
C1 N1 C6 121.9(4) . . ?
C3 N1 C6 125.3(5) . . ?
C1 N2 C2 111.4(5) . . ?
C1 N2 C27 124.1(4) . . ?
C2 N2 C27 124.5(4) . . ?
N1 C1 Pd1 125.0(3) . . ?
N1 C1 N2 103.7(4) . . ?
N2 C1 Pd1 131.1(4) . . ?
N2 C2 C4 122.4(6) . . ?
C3 C2 N2 106.9(5) . . ?
C3 C2 C4 130.6(6) . . ?
N1 C3 C5 124.2(6) . . ?
C2 C3 N1 105.6(5) . . ?
C2 C3 C5 130.2(5) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 117.5(5) . . ?
C7 C6 C11 122.7(5) . . ?
C11 C6 N1 119.7(4) . . ?
C6 C7 C12 121.6(6) . . ?
C8 C7 C6 117.2(5) . . ?
C8 C7 C12 121.3(6) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 C7 122.6(6) . . ?
C9 C8 H8 118.7 . . ?
C8 C9 C10 118.4(6) . . ?
C8 C9 C13 121.0(6) . . ?
C10 C9 C13 120.6(6) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 C9 121.7(6) . . ?
C11 C10 H10 119.1 . . ?
C6 C11 C14 119.9(5) . . ?
C10 C11 C6 117.4(5) . . ?
C10 C11 C14 122.8(5) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14 106.8 . . ?
C11 C14 C15 110.6(4) . . ?
C11 C14 C21 115.2(4) . . ?
C15 C14 H14 106.8 . . ?
C15 C14 C21 110.3(5) . . ?
C21 C14 H14 106.8 . . ?
C16 C15 C14 119.6(5) . . ?
C20 C15 C14 123.2(5) . . ?
C20 C15 C16 117.2(6) . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.9(7) . . ?
C17 C16 H16 119.6 . . ?
C16 C17 H17 119.4 . . ?
C18 C17 C16 121.2(8) . . ?
C18 C17 H17 119.4 . . ?
C17 C18 H18 120.2 . . ?
C17 C18 C19 119.5(7) . . ?
C19 C18 H18 120.2 . . ?
C18 C19 H19 119.8 . . ?
C18 C19 C20 120.4(8) . . ?
C20 C19 H19 119.8 . . ?
C15 C20 C19 120.8(8) . . ?
C15 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C22 C21 C14 118.8(6) . . ?
C22 C21 C26 117.2(7) . . ?
C26 C21 C14 124.0(7) . . ?
C21 C22 H22 119.3 . . ?
C21 C22 C23 121.5(9) . . ?
C23 C22 H22 119.3 . . ?
C22 C23 H23 120.3 . . ?
C24 C23 C22 119.4(10) . . ?
C24 C23 H23 120.3 . . ?
C23 C24 H24 119.7 . . ?
C23 C24 C25 120.6(10) . . ?
C25 C24 H24 119.7 . . ?
C24 C25 H25 120.5 . . ?
C24 C25 C26 119.1(11) . . ?
C26 C25 H25 120.5 . . ?
C21 C26 C25 122.1(10) . . ?
C21 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C28 C27 N2 118.0(5) . . ?
C28 C27 C32 122.6(5) . . ?
C32 C27 N2 119.4(5) . . ?
C27 C28 C29 116.7(6) . . ?
C27 C28 C33 122.3(6) . . ?
C29 C28 C33 121.0(6) . . ?
C28 C29 H29 118.2 . . ?
C30 C29 C28 123.7(6) . . ?
C30 C29 H29 118.2 . . ?
C29 C30 C31 117.0(6) . . ?
C29 C30 C34 122.8(7) . . ?
C31 C30 C34 120.2(7) . . ?
C30 C31 H31 118.2 . . ?
C30 C31 C32 123.5(7) . . ?
C32 C31 H31 118.2 . . ?
C27 C32 C35 121.5(5) . . ?
C31 C32 C27 116.5(5) . . ?
C31 C32 C35 122.0(6) . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.5 . . ?
C28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
C30 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Pd1 C36 H36A 73.2 . . ?
Pd1 C36 H36B 125.6 . . ?
H36A C36 H36B 120.0 . . ?
C37 C36 Pd1 72.5(4) . . ?
C37 C36 H36A 118.9 . . ?
C37 C36 H36B 121.1 . . ?
Pd1 C37 H37 126.6 . . ?
C36 C37 Pd1 69.5(4) . . ?
C36 C37 H37 118.9 . . ?
C38 C37 Pd1 77.2(4) . . ?
C38 C37 C36 122.8(8) . . ?
C38 C37 H37 118.4 . . ?
Pd1 C38 H38 78.4 . . ?
C37 C38 Pd1 67.2(4) . . ?
C37 C38 H38 116.3 . . ?
C37 C38 C39 126.4(8) . . ?
C39 C38 Pd1 124.1(5) . . ?
C39 C38 H38 117.2 . . ?
C40 C39 C38 117.4(7) . . ?
C44 C39 C38 124.6(7) . . ?
C44 C39 C40 117.9(7) . . ?
C39 C40 H40 119.6 . . ?
C39 C40 C41 120.8(8) . . ?
C41 C40 H40 119.6 . . ?
C40 C41 H41 120.8 . . ?
C42 C41 C40 118.4(9) . . ?
C42 C41 H41 120.8 . . ?
C41 C42 H42 119.1 . . ?
C43 C42 C41 121.8(9) . . ?
C43 C42 H42 119.1 . . ?
C42 C43 H43 119.9 . . ?
C42 C43 C44 120.1(9) . . ?
C44 C43 H43 119.9 . . ?
C39 C44 C43 120.9(8) . . ?
C39 C44 H44 119.5 . . ?
C43 C44 H44 119.5 . . ?

_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 3.628
_oxdiff_exptl_absorpt_empirical_full_min 0.760
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.04(4)
2 -0.04(4)

####################################################################### 
# 
# 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_lk315221st
_database_code_depnum_ccdc_archive 'CCDC 2250215'
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi'
;Aix Marseille University CNRS
France
;
_audit_update_record             
;
2023-03-20 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2018-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H35 Cl N2 Pd'
_chemical_formula_sum            'C27 H35 Cl N2 Pd'
_chemical_formula_weight         529.42
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c27 h35 Cl1 n2 Pd1'
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           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   8.91439(18)
_cell_length_b                   11.5588(2)
_cell_length_c                   13.5263(3)
_cell_angle_alpha                70.3306(19)
_cell_angle_beta                 83.4315(17)
_cell_angle_gamma                80.1947(16)
_cell_volume                     1290.81(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    25403
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.2850
_cell_measurement_theta_min      3.5310
_shelx_estimated_absorpt_T_max   0.959
_shelx_estimated_absorpt_T_min   0.752
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48191
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.023
_diffrn_reflns_theta_min         2.781
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00  12.00   1.00   30.00    --   -7.86  89.00  55.00   57
  2  ω    -24.00  85.00   1.00   30.00    --    8.41  77.00 150.00  109
  3  ω    -16.00  83.00   1.00   30.00    --    8.41  38.00  90.00   99
  4  ω    -20.00  82.00   1.00   30.00    --    8.41  57.00 -90.00  102
  5  ω    -20.00  49.00   1.00   30.00    --    8.41 -99.00 -90.00   69
  6  ω    -15.00  53.00   1.00   30.00    --    8.41-105.00  -8.95   68
  7  ω    -65.00  42.00   1.00   30.00    --   10.00 -73.00 136.27  107
  8  ω    -20.00  33.00   1.00   30.00    --   -7.86 -99.00 -90.00   53
  9  ω    -81.00 -37.00   1.00   30.00    --   -7.86 151.00  94.83   44
 10  ω    -70.00 -29.00   1.00   30.00    --   -7.86 135.00 154.18   41
 11  ω    -81.00 -37.00   1.00   30.00    --   -7.86 151.00-142.38   44
 12  ω    -83.00 -38.00   1.00   30.00    --   -7.86 153.00 -79.97   45
 13  ω    -65.00 -24.00   1.00   30.00    --   -7.86 126.00  -4.28   41
 14  ω    -16.00  83.00   1.00   30.00    --    8.41  38.00 -30.00   99
 15  ω    -66.00  33.00   1.00   30.00    --    8.41 -38.00 -60.00   99
 16  ω    -66.00  33.00   1.00   30.00    --    8.41 -38.00  60.00   99
 17  ω    -80.00  42.00   1.00   30.00    --    8.41   0.00-180.00  122
 18  ω    -16.00  83.00   1.00   30.00    --    8.41  38.00 150.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0089701000
_diffrn_orient_matrix_UB_12      -0.0444757000
_diffrn_orient_matrix_UB_13      0.0507648000
_diffrn_orient_matrix_UB_21      -0.0707099000
_diffrn_orient_matrix_UB_22      -0.0191603000
_diffrn_orient_matrix_UB_23      -0.0021102000
_diffrn_orient_matrix_UB_31      0.0382698000
_diffrn_orient_matrix_UB_32      -0.0445816000
_diffrn_orient_matrix_UB_33      -0.0230519000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.773
_reflns_number_gt                10067
_reflns_number_total             11387
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 
;
 Flack x determined using 4268 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         11387
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0347
_refine_ls_restrained_S_all      1.073
_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)+(0.0420P)²+0.2023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0846
_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. Uiso/Uaniso restraints and constraints
C22 \\sim C24: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01
C22 \\sim C23: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01
C49 \\sim C50: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
3.a Riding coordinates:
 C26(H26), C53(H53)
3.b Ternary CH refined with riding coordinates:
 C22(H22), C49(H49)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C17(H17), C18(H18), C19(H19), C20(H20),
 C34(H34), C35(H35), C36(H36), C37(H37), C44(H44), C45(H45), C46(H46), C47(H47)
3.d X=CH2 refined with riding coordinates:
 C25(H25A,H25B), C27(H27A,H27B), C52(H52A,H52B), C54(H54A,H54B)
3.e Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.80063(3) 0.54998(2) 0.84300(2) 0.03782(16) Uani 1 1 d . . . . .
Cl1 Cl 0.5383(4) 0.5338(3) 0.8945(3) 0.0653(9) Uani 1 1 d . . . . .
N1 N 0.8997(9) 0.3289(7) 1.0307(6) 0.0332(16) Uani 1 1 d . . . . .
N2 N 0.8541(9) 0.4903(7) 1.0759(6) 0.038(2) Uani 1 1 d . . . . .
C1 C 0.8645(12) 0.4510(10) 0.9929(8) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.8844(11) 0.3908(9) 1.1693(8) 0.040(2) Uani 1 1 d . . . . .
C3 C 0.9099(11) 0.2894(9) 1.1384(8) 0.041(2) Uani 1 1 d . . . . .
C4 C 0.8884(16) 0.4063(12) 1.2704(10) 0.070(4) Uani 1 1 d . . . . .
H4A H 0.971630 0.350254 1.307232 0.105 Uiso 1 1 calc GR . . . .
H4B H 0.794263 0.388759 1.310630 0.105 Uiso 1 1 calc GR . . . .
H4C H 0.902159 0.490128 1.260496 0.105 Uiso 1 1 calc GR . . . .
C5 C 0.9441(15) 0.1536(10) 1.2056(8) 0.061(3) Uani 1 1 d . . . . .
H5A H 0.880881 0.105579 1.187004 0.092 Uiso 1 1 calc GR . . . .
H5B H 0.923623 0.146191 1.278513 0.092 Uiso 1 1 calc GR . . . .
H5C H 1.049483 0.123442 1.193519 0.092 Uiso 1 1 calc GR . . . .
C6 C 0.9181(12) 0.2482(9) 0.9649(8) 0.039(2) Uani 1 1 d . . . . .
C7 C 0.7819(13) 0.2347(10) 0.9336(9) 0.050(3) Uani 1 1 d . . . . .
H7 H 0.690162 0.273348 0.955378 0.059 Uiso 1 1 calc R . . . .
C8 C 0.7831(14) 0.1643(11) 0.8708(10) 0.055(3) Uani 1 1 d . . . . .
H8 H 0.692085 0.156093 0.848064 0.066 Uiso 1 1 calc R . . A 2
C9 C 0.9183(18) 0.1056(14) 0.8410(12) 0.066(4) Uani 1 1 d . . . . .
H9 H 0.918918 0.056645 0.798692 0.079 Uiso 1 1 calc R . . . .
C10 C 1.0521(13) 0.1186(10) 0.8730(9) 0.053(2) Uani 1 1 d . . . . .
H10 H 1.142638 0.076672 0.852847 0.064 Uiso 1 1 calc R . . . .
C11 C 1.0577(12) 0.1916(9) 0.9341(8) 0.041(2) Uani 1 1 d . . . . .
C12 C 1.2221(10) 0.2101(10) 0.9561(8) 0.055(3) Uani 1 1 d . . . . .
C13 C 1.2303(6) 0.3009(6) 1.0136(5) 0.0600(15) Uani 1 1 d . . . . .
H13A H 1.176234 0.380420 0.976759 0.090 Uiso 1 1 calc GR . . . .
H13B H 1.335020 0.308608 1.016722 0.090 Uiso 1 1 calc GR . . . .
H13C H 1.184816 0.271019 1.083673 0.090 Uiso 1 1 calc GR . . . .
C14 C 1.3072(9) 0.2620(9) 0.8486(7) 0.067(2) Uani 1 1 d . . . . .
H14A H 1.311567 0.206100 0.809258 0.101 Uiso 1 1 calc GR . . . .
H14B H 1.408844 0.270902 0.858925 0.101 Uiso 1 1 calc GR . . . .
H14C H 1.254213 0.341556 0.810605 0.101 Uiso 1 1 calc GR . . . .
C15 C 1.3045(15) 0.0798(12) 1.0129(10) 0.073(3) Uani 1 1 d . . . . .
H15A H 1.249520 0.043997 1.078540 0.109 Uiso 1 1 calc GR . . . .
H15B H 1.405986 0.085994 1.026018 0.109 Uiso 1 1 calc GR . . . .
H15C H 1.309534 0.028105 0.969654 0.109 Uiso 1 1 calc GR . . . .
C16 C 0.8114(11) 0.6186(8) 1.0736(7) 0.036(2) Uani 1 1 d . . . . .
C17 C 0.6598(13) 0.6555(10) 1.0887(9) 0.052(3) Uani 1 1 d . . . . .
H17 H 0.588399 0.602845 1.095473 0.062 Uiso 1 1 calc R . . . .
C18 C 0.6142(14) 0.7780(10) 1.0939(9) 0.068(4) Uani 1 1 d . . . . .
H18 H 0.512259 0.806198 1.107081 0.081 Uiso 1 1 calc R . . . .
C19 C 0.7243(18) 0.8535(12) 1.0789(12) 0.068(4) Uani 1 1 d . . . . .
H19 H 0.696051 0.934522 1.079433 0.082 Uiso 1 1 calc R . . . .
C20 C 0.8696(15) 0.8122(11) 1.0637(11) 0.065(3) Uani 1 1 d . . . . .
H20 H 0.941634 0.864234 1.057246 0.078 Uiso 1 1 calc R . . . .
C21 C 0.9207(14) 0.6922(11) 1.0568(10) 0.052(3) Uani 1 1 d . . . . .
C22 C 1.0924(17) 0.6569(16) 1.0286(15) 0.092(4) Uani 1 1 d . U . . .
H22 H 1.108417 0.572710 1.024335 0.111 Uiso 1 1 calc R . . . .
C23 C 1.1487(18) 0.7430(15) 0.9270(14) 0.105(4) Uani 1 1 d . U . . .
H23A H 1.090097 0.744037 0.871367 0.158 Uiso 1 1 calc GR . . . .
H23B H 1.254171 0.715375 0.912621 0.158 Uiso 1 1 calc GR . . . .
H23C H 1.138147 0.825161 0.931605 0.158 Uiso 1 1 calc GR . . . .
C24 C 1.1834(17) 0.6585(15) 1.1169(15) 0.155(6) Uani 1 1 d . U . . .
H24A H 1.138217 0.725827 1.141884 0.232 Uiso 1 1 calc GR . . . .
H24B H 1.286648 0.669185 1.090781 0.232 Uiso 1 1 calc GR . . . .
H24C H 1.182748 0.581465 1.173540 0.232 Uiso 1 1 calc GR . . . .
C25 C 0.7800(13) 0.6422(11) 0.6739(9) 0.059(3) Uani 1 1 d . . . . .
H25A H 0.754713 0.562699 0.690580 0.071 Uiso 1 1 calc R . . . .
H25B H 0.714513 0.710529 0.636234 0.071 Uiso 1 1 calc R . . . .
C26 C 0.9143(14) 0.6586(13) 0.7051(8) 0.093(5) Uani 1 1 d . . . . .
H26 H 0.935307 0.739304 0.688551 0.111 Uiso 1 1 d R . . . .
C27 C 1.0197(15) 0.5616(12) 0.7620(10) 0.066(4) Uani 1 1 d . . . . .
H27A H 1.000951 0.479978 0.781027 0.079 Uiso 1 1 calc R . . . .
H27B H 1.108584 0.578770 0.780798 0.079 Uiso 1 1 calc R . . . .
Pd2 Pd 0.61724(3) -0.01590(2) 0.63943(2) 0.03878(17) Uani 1 1 d . . . . .
Cl2 Cl 0.8807(3) -0.0034(3) 0.5924(3) 0.0614(9) Uani 1 1 d . . . . .
N3 N 0.5631(9) 0.0455(7) 0.4057(6) 0.0356(18) Uani 1 1 d . . . . .
N4 N 0.5200(10) 0.2119(7) 0.4497(7) 0.0414(19) Uani 1 1 d . . . . .
C28 C 0.5604(11) 0.0829(9) 0.4927(8) 0.033(2) Uani 1 1 d . . . . .
C29 C 0.5101(12) 0.2507(10) 0.3395(8) 0.046(3) Uani 1 1 d . . . . .
C30 C 0.5394(12) 0.1454(10) 0.3145(8) 0.045(2) Uani 1 1 d . . . . .
C31 C 0.4760(14) 0.3799(10) 0.2746(9) 0.063(3) Uani 1 1 d . . . . .
H31A H 0.375049 0.394857 0.250573 0.094 Uiso 1 1 calc GR . . . .
H31B H 0.548481 0.397513 0.215142 0.094 Uiso 1 1 calc GR . . . .
H31C H 0.481993 0.432670 0.315323 0.094 Uiso 1 1 calc GR . . . .
C32 C 0.5401(14) 0.1311(13) 0.2067(9) 0.058(3) Uani 1 1 d . . . . .
H32A H 0.631913 0.079564 0.194467 0.088 Uiso 1 1 calc GR . . . .
H32B H 0.535428 0.211218 0.153653 0.088 Uiso 1 1 calc GR . . . .
H32C H 0.453303 0.093335 0.204052 0.088 Uiso 1 1 calc GR . . . .
C33 C 0.6001(11) -0.0808(9) 0.4095(8) 0.042(2) Uani 1 1 d . . . . .
C34 C 0.7556(13) -0.1246(10) 0.3991(9) 0.052(3) Uani 1 1 d . . . . .
H34 H 0.826147 -0.071851 0.393976 0.063 Uiso 1 1 calc R . . . .
C35 C 0.8073(14) -0.2401(12) 0.3961(10) 0.065(3) Uani 1 1 d . . . . .
H35 H 0.911382 -0.266522 0.389822 0.078 Uiso 1 1 calc R . . . .
C36 C 0.7045(15) -0.3175(12) 0.4025(10) 0.061(4) Uani 1 1 d . . . . .
H36 H 0.738320 -0.396433 0.398225 0.073 Uiso 1 1 calc R . . . .
C37 C 0.5474(16) -0.2785(11) 0.4155(9) 0.062(3) Uani 1 1 d . . . . .
H37 H 0.479750 -0.334390 0.423244 0.075 Uiso 1 1 calc R . . . .
C38 C 0.4892(13) -0.1595(11) 0.4174(9) 0.045(3) Uani 1 1 d . . . . .
C39 C 0.3189(13) -0.1264(11) 0.4320(10) 0.055(2) Uani 1 1 d . . . . .
C40 C 0.2433(14) -0.1481(12) 0.3417(12) 0.104(4) Uani 1 1 d . . . . .
H40A H 0.284323 -0.099368 0.274788 0.156 Uiso 1 1 calc GR . . . .
H40B H 0.135053 -0.123761 0.347422 0.156 Uiso 1 1 calc GR . . . .
H40C H 0.264311 -0.234347 0.347716 0.156 Uiso 1 1 calc GR . . . .
C41 C 0.2646(17) -0.2127(14) 0.5383(13) 0.109(5) Uani 1 1 d . . . . .
H41A H 0.299958 -0.297340 0.542629 0.163 Uiso 1 1 calc GR . . . .
H41B H 0.155201 -0.199892 0.545397 0.163 Uiso 1 1 calc GR . . . .
H41C H 0.304658 -0.194884 0.593763 0.163 Uiso 1 1 calc GR . . . .
C42 C 0.2512(6) 0.0072(6) 0.4277(6) 0.0685(18) Uani 1 1 d . . . . .
H42A H 0.291478 0.027281 0.481822 0.103 Uiso 1 1 calc GR . . . .
H42B H 0.142203 0.013246 0.438443 0.103 Uiso 1 1 calc GR . . . .
H42C H 0.277861 0.064077 0.360236 0.103 Uiso 1 1 calc GR . . . .
C43 C 0.5131(11) 0.2896(9) 0.5128(8) 0.037(2) Uani 1 1 d . . . . .
C44 C 0.6476(13) 0.2944(9) 0.5529(9) 0.048(3) Uani 1 1 d . . . . .
H44 H 0.738266 0.249614 0.536320 0.057 Uiso 1 1 calc R . . . .
C45 C 0.6478(15) 0.3666(11) 0.6182(10) 0.056(3) Uani 1 1 d . . . . .
H45 H 0.737035 0.368555 0.646761 0.067 Uiso 1 1 calc R . . . .
C46 C 0.5121(16) 0.4346(12) 0.6391(10) 0.051(3) Uani 1 1 d . . . . .
H46 H 0.509250 0.483035 0.682214 0.061 Uiso 1 1 calc R . . . .
C47 C 0.3821(13) 0.4308(11) 0.5964(9) 0.051(2) Uani 1 1 d . . . . .
H47 H 0.293218 0.479587 0.610097 0.061 Uiso 1 1 calc R . . . .
C48 C 0.3745(13) 0.3566(10) 0.5321(8) 0.045(2) Uani 1 1 d . . . . .
C49 C 0.2246(11) 0.3501(9) 0.4981(8) 0.053(2) Uani 1 1 d . U . . .
H49 H 0.246260 0.313394 0.441489 0.064 Uiso 1 1 calc R . . . .
C50 C 0.1318(11) 0.2651(10) 0.5840(8) 0.083(3) Uani 1 1 d . U . . .
H50A H 0.194826 0.187847 0.615524 0.125 Uiso 1 1 calc GR . . . .
H50B H 0.047144 0.249886 0.554485 0.125 Uiso 1 1 calc GR . . . .
H50C H 0.094650 0.303502 0.636604 0.125 Uiso 1 1 calc GR . . . .
C51 C 0.1294(16) 0.4751(12) 0.4525(11) 0.086(4) Uani 1 1 d . . . . .
H51A H 0.100251 0.512748 0.506493 0.129 Uiso 1 1 calc GR . . . .
H51B H 0.039632 0.464290 0.425498 0.129 Uiso 1 1 calc GR . . . .
H51C H 0.187991 0.527674 0.396621 0.129 Uiso 1 1 calc GR . . . .
C52 C 0.4063(15) -0.0319(15) 0.7216(11) 0.072(4) Uani 1 1 d . . . . .
H52A H 0.427078 0.049062 0.703506 0.086 Uiso 1 1 calc R . . . .
H52B H 0.318350 -0.047340 0.700180 0.086 Uiso 1 1 calc R . . . .
C53 C 0.5039(13) -0.1271(7) 0.7789(8) 0.060(3) Uani 1 1 d . . . . .
H53 H 0.483365 -0.207998 0.795846 0.072 Uiso 1 1 d R . . . .
C54 C 0.6322(18) -0.1041(13) 0.8099(9) 0.074(4) Uani 1 1 d . . . . .
H54A H 0.652535 -0.022969 0.791685 0.089 Uiso 1 1 calc R . . . .
H54B H 0.699683 -0.169417 0.849398 0.089 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 2.383(3) . ?
Pd1 C1 2.056(11) . ?
Pd1 C25 2.188(12) . ?
Pd1 C26 2.122(11) . ?
Pd1 C27 2.129(11) . ?
N1 C1 1.324(13) . ?
N1 C3 1.380(12) . ?
N1 C6 1.471(12) . ?
N2 C1 1.334(13) . ?
N2 C2 1.410(12) . ?
N2 C16 1.457(10) . ?
C2 C3 1.349(14) . ?
C2 C4 1.442(16) . ?
C3 C5 1.524(14) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.380(15) . ?
C6 C11 1.393(14) . ?
C7 H7 0.9300 . ?
C7 C8 1.358(15) . ?
C8 H8 0.9300 . ?
C8 C9 1.368(19) . ?
C9 H9 0.9300 . ?
C9 C10 1.362(19) . ?
C10 H10 0.9300 . ?
C10 C11 1.376(15) . ?
C11 C12 1.590(14) . ?
C12 C13 1.516(11) . ?
C12 C14 1.538(12) . ?
C12 C15 1.541(16) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.360(14) . ?
C16 C21 1.352(16) . ?
C17 H17 0.9300 . ?
C17 C18 1.428(14) . ?
C18 H18 0.9300 . ?
C18 C19 1.376(18) . ?
C19 H19 0.9300 . ?
C19 C20 1.320(19) . ?
C20 H20 0.9300 . ?
C20 C21 1.415(15) . ?
C21 C22 1.553(19) . ?
C22 H22 0.9800 . ?
C22 C23 1.49(2) . ?
C22 C24 1.53(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9300 . ?
C25 H25B 0.9300 . ?
C25 C26 1.376(19) . ?
C26 H26 0.9299 . ?
C26 C27 1.400(17) . ?
C27 H27A 0.9300 . ?
C27 H27B 0.9300 . ?
Pd2 Cl2 2.377(3) . ?
Pd2 C28 2.002(11) . ?
Pd2 C52 2.075(13) . ?
Pd2 C53 2.146(9) . ?
Pd2 C54 2.195(12) . ?
N3 C28 1.380(13) . ?
N3 C30 1.385(12) . ?
N3 C33 1.425(12) . ?
N4 C28 1.404(13) . ?
N4 C29 1.414(13) . ?
N4 C43 1.423(13) . ?
C29 C30 1.346(15) . ?
C29 C31 1.455(15) . ?
C30 C32 1.521(15) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.401(14) . ?
C33 C38 1.426(15) . ?
C34 H34 0.9300 . ?
C34 C35 1.348(15) . ?
C35 H35 0.9300 . ?
C35 C36 1.362(17) . ?
C36 H36 0.9300 . ?
C36 C37 1.406(19) . ?
C37 H37 0.9300 . ?
C37 C38 1.393(16) . ?
C38 C39 1.508(17) . ?
C39 C40 1.567(15) . ?
C39 C41 1.529(17) . ?
C39 C42 1.544(13) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C44 1.388(14) . ?
C43 C48 1.389(14) . ?
C44 H44 0.9300 . ?
C44 C45 1.406(16) . ?
C45 H45 0.9300 . ?
C45 C46 1.381(18) . ?
C46 H46 0.9300 . ?
C46 C47 1.366(17) . ?
C47 H47 0.9300 . ?
C47 C48 1.426(15) . ?
C48 C49 1.484(16) . ?
C49 H49 0.9800 . ?
C49 C50 1.513(12) . ?
C49 C51 1.513(15) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9300 . ?
C52 H52B 0.9300 . ?
C52 C53 1.350(17) . ?
C53 H53 0.9298 . ?
C53 C54 1.358(19) . ?
C54 H54A 0.9300 . ?
C54 H54B 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 Cl1 91.9(3) . . ?
C1 Pd1 C25 168.4(4) . . ?
C1 Pd1 C26 134.0(5) . . ?
C1 Pd1 C27 99.7(5) . . ?
C25 Pd1 Cl1 98.7(3) . . ?
C26 Pd1 Cl1 132.9(3) . . ?
C26 Pd1 C25 37.2(5) . . ?
C26 Pd1 C27 38.4(4) . . ?
C27 Pd1 Cl1 166.0(4) . . ?
C27 Pd1 C25 69.2(5) . . ?
C1 N1 C3 111.2(8) . . ?
C1 N1 C6 123.1(9) . . ?
C3 N1 C6 125.7(8) . . ?
C1 N2 C2 111.5(8) . . ?
C1 N2 C16 125.5(8) . . ?
C2 N2 C16 123.0(8) . . ?
N1 C1 Pd1 125.5(8) . . ?
N1 C1 N2 105.4(9) . . ?
N2 C1 Pd1 128.2(8) . . ?
N2 C2 C4 123.7(9) . . ?
C3 C2 N2 104.2(8) . . ?
C3 C2 C4 132.1(10) . . ?
N1 C3 C5 123.9(9) . . ?
C2 C3 N1 107.7(8) . . ?
C2 C3 C5 128.4(9) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 113.5(9) . . ?
C7 C6 C11 121.9(9) . . ?
C11 C6 N1 124.6(9) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.4(10) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.9(12) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.3(13) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.0 . . ?
C9 C10 C11 122.1(12) . . ?
C11 C10 H10 119.0 . . ?
C6 C11 C12 126.5(9) . . ?
C10 C11 C6 116.2(10) . . ?
C10 C11 C12 117.1(9) . . ?
C13 C12 C11 117.7(7) . . ?
C13 C12 C14 105.0(7) . . ?
C13 C12 C15 111.8(8) . . ?
C14 C12 C11 107.2(8) . . ?
C14 C12 C15 108.4(8) . . ?
C15 C12 C11 106.5(9) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 115.9(9) . . ?
C21 C16 N2 119.6(9) . . ?
C21 C16 C17 124.5(10) . . ?
C16 C17 H17 121.2 . . ?
C16 C17 C18 117.6(11) . . ?
C18 C17 H17 121.2 . . ?
C17 C18 H18 120.7 . . ?
C19 C18 C17 118.6(11) . . ?
C19 C18 H18 120.7 . . ?
C18 C19 H19 119.6 . . ?
C20 C19 C18 120.8(11) . . ?
C20 C19 H19 119.6 . . ?
C19 C20 H20 118.6 . . ?
C19 C20 C21 122.9(12) . . ?
C21 C20 H20 118.6 . . ?
C16 C21 C20 115.5(10) . . ?
C16 C21 C22 125.7(11) . . ?
C20 C21 C22 118.8(12) . . ?
C21 C22 H22 108.8 . . ?
C23 C22 C21 113.1(14) . . ?
C23 C22 H22 108.8 . . ?
C23 C22 C24 109.1(14) . . ?
C24 C22 C21 108.1(13) . . ?
C24 C22 H22 108.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Pd1 C25 H25A 72.2 . . ?
Pd1 C25 H25B 131.8 . . ?
H25A C25 H25B 120.0 . . ?
C26 C25 Pd1 68.8(7) . . ?
C26 C25 H25A 120.0 . . ?
C26 C25 H25B 120.0 . . ?
Pd1 C26 H26 128.7 . . ?
C25 C26 Pd1 74.0(7) . . ?
C25 C26 H26 118.0 . . ?
C25 C26 C27 124.1(13) . . ?
C27 C26 Pd1 71.0(6) . . ?
C27 C26 H26 117.9 . . ?
Pd1 C27 H27A 71.9 . . ?
Pd1 C27 H27B 130.1 . . ?
C26 C27 Pd1 70.5(7) . . ?
C26 C27 H27A 120.0 . . ?
C26 C27 H27B 120.0 . . ?
H27A C27 H27B 120.0 . . ?
C28 Pd2 Cl2 91.9(3) . . ?
C28 Pd2 C52 102.5(5) . . ?
C28 Pd2 C53 135.8(4) . . ?
C28 Pd2 C54 167.6(5) . . ?
C52 Pd2 Cl2 163.9(4) . . ?
C52 Pd2 C53 37.3(5) . . ?
C52 Pd2 C54 66.5(6) . . ?
C53 Pd2 Cl2 131.0(3) . . ?
C53 Pd2 C54 36.4(5) . . ?
C54 Pd2 Cl2 98.4(4) . . ?
C28 N3 C30 111.9(8) . . ?
C28 N3 C33 123.1(8) . . ?
C30 N3 C33 124.7(8) . . ?
C28 N4 C29 112.2(9) . . ?
C28 N4 C43 120.5(9) . . ?
C29 N4 C43 126.7(8) . . ?
N3 C28 Pd2 129.8(7) . . ?
N3 C28 N4 101.8(9) . . ?
N4 C28 Pd2 128.2(8) . . ?
N4 C29 C31 123.6(10) . . ?
C30 C29 N4 104.9(9) . . ?
C30 C29 C31 131.5(10) . . ?
N3 C30 C32 123.0(10) . . ?
C29 C30 N3 108.9(9) . . ?
C29 C30 C32 127.9(10) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 C38 123.8(9) . . ?
C34 C33 N3 116.1(9) . . ?
C34 C33 C38 119.9(10) . . ?
C33 C34 H34 118.6 . . ?
C35 C34 C33 122.7(11) . . ?
C35 C34 H34 118.6 . . ?
C34 C35 H35 120.5 . . ?
C34 C35 C36 118.9(11) . . ?
C36 C35 H35 120.5 . . ?
C35 C36 H36 119.9 . . ?
C35 C36 C37 120.3(12) . . ?
C37 C36 H36 119.9 . . ?
C36 C37 H37 118.7 . . ?
C38 C37 C36 122.6(12) . . ?
C38 C37 H37 118.7 . . ?
C33 C38 C39 125.8(10) . . ?
C37 C38 C33 115.5(11) . . ?
C37 C38 C39 118.7(11) . . ?
C38 C39 C40 108.0(10) . . ?
C38 C39 C41 108.2(11) . . ?
C38 C39 C42 119.5(9) . . ?
C41 C39 C40 109.5(11) . . ?
C41 C39 C42 106.8(9) . . ?
C42 C39 C40 104.4(9) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 N4 117.6(9) . . ?
C44 C43 C48 122.8(10) . . ?
C48 C43 N4 119.6(9) . . ?
C43 C44 H44 119.8 . . ?
C43 C44 C45 120.4(10) . . ?
C45 C44 H44 119.8 . . ?
C44 C45 H45 120.8 . . ?
C46 C45 C44 118.4(11) . . ?
C46 C45 H45 120.8 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 C45 120.0(12) . . ?
C47 C46 H46 120.0 . . ?
C46 C47 H47 118.0 . . ?
C46 C47 C48 124.0(12) . . ?
C48 C47 H47 118.0 . . ?
C43 C48 C47 114.4(10) . . ?
C43 C48 C49 126.0(9) . . ?
C47 C48 C49 119.5(10) . . ?
C48 C49 H49 106.5 . . ?
C48 C49 C50 112.7(9) . . ?
C48 C49 C51 114.2(10) . . ?
C50 C49 H49 106.5 . . ?
C50 C49 C51 110.0(10) . . ?
C51 C49 H49 106.5 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
Pd2 C52 H52A 70.1 . . ?
Pd2 C52 H52B 127.8 . . ?
H52A C52 H52B 120.0 . . ?
C53 C52 Pd2 74.2(7) . . ?
C53 C52 H52A 120.0 . . ?
C53 C52 H52B 120.0 . . ?
Pd2 C53 H53 129.2 . . ?
C52 C53 Pd2 68.5(7) . . ?
C52 C53 H53 119.6 . . ?
C52 C53 C54 119.8(10) . . ?
C54 C53 Pd2 73.7(6) . . ?
C54 C53 H53 120.6 . . ?
Pd2 C54 H54A 71.3 . . ?
Pd2 C54 H54B 131.7 . . ?
C53 C54 Pd2 69.8(7) . . ?
C53 C54 H54A 120.0 . . ?
C53 C54 H54B 120.0 . . ?
H54A C54 H54B 120.0 . . ?


_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 2.427
_oxdiff_exptl_absorpt_empirical_full_min 0.469
####################################################################### 
# 
# 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_lk2087b
_database_code_depnum_ccdc_archive 'CCDC 2250213'
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi'
;Aix Marseille University CNRS
France
;
_audit_update_record             
;
2023-03-20 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2018-01-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H29 Cl N2 Pd'
_chemical_formula_sum            'C32 H29 Cl N2 Pd'
_chemical_formula_weight         583.42
_chemical_absolute_configuration unk
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   18.4645(5)
_cell_length_b                   10.3454(3)
_cell_length_c                   14.2625(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2724.46(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9262
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.2030
_cell_measurement_theta_min      3.6140
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.819
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.18b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25700
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.604
_diffrn_reflns_theta_min         3.284
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  82.00   1.00   15.00    --    8.41  57.00-120.00  102
  2  ω    -24.00  85.00   1.00   15.00    --    8.41  77.00 -30.00  109
  3  ω    -20.00  49.00   1.00   15.00    --    8.41 -99.00  60.00   69
  4  ω    -64.00 -39.00   1.00   15.00    --    8.41 -57.00 -90.00   25
  5  ω    -20.00  49.00   1.00   15.00    --    8.41 -99.00-150.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0112909000
_diffrn_orient_matrix_UB_12      -0.0368694000
_diffrn_orient_matrix_UB_13      0.0392954000
_diffrn_orient_matrix_UB_21      0.0088336000
_diffrn_orient_matrix_UB_22      -0.0522672000
_diffrn_orient_matrix_UB_23      -0.0300825000
_diffrn_orient_matrix_UB_31      0.0356309000
_diffrn_orient_matrix_UB_32      0.0246970000
_diffrn_orient_matrix_UB_33      -0.0049924000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                5176
_reflns_number_total             6064
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_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         1.940
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.19(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6064
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0592
_refine_ls_restrained_S_all      1.075
_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)+(0.1231P)²+1.4530P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1795
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.81(7)
 0.19(7)
2. 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
3.a Riding coordinates:
 C30(H30A,H30B), C31(H31), C32(H32A,H32B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.29863(3) 0.26542(5) 0.67141(8) 0.0414(2) Uani 1 1 d . . . . .
Cl1 Cl 0.34129(8) 0.41402(17) 0.79420(12) 0.0292(4) Uani 1 1 d . . . . .
N1 N 0.1863(4) 0.4450(7) 0.5804(5) 0.0354(14) Uani 1 1 d . . . . .
N2 N 0.2930(3) 0.4990(7) 0.5383(5) 0.0327(14) Uani 1 1 d . . . . .
C1 C 0.2573(4) 0.4088(8) 0.5906(6) 0.0355(17) Uani 1 1 d . . . . .
C2 C 0.1786(4) 0.5543(8) 0.5272(6) 0.0386(17) Uani 1 1 d . . . . .
C3 C 0.2457(5) 0.5891(9) 0.4989(6) 0.0413(19) Uani 1 1 d . . . . .
C4 C 0.1094(5) 0.6236(11) 0.5097(9) 0.056(2) Uani 1 1 d . . . . .
H4A H 0.075279 0.565620 0.481136 0.085 Uiso 1 1 calc GR . . . .
H4B H 0.117989 0.695421 0.468499 0.085 Uiso 1 1 calc GR . . . .
H4C H 0.090123 0.654589 0.568012 0.085 Uiso 1 1 calc GR . . . .
C5 C 0.2727(6) 0.7041(12) 0.4459(9) 0.060(3) Uani 1 1 d . . . . .
H5A H 0.307313 0.750006 0.483471 0.089 Uiso 1 1 calc GR . . . .
H5B H 0.232767 0.760053 0.431370 0.089 Uiso 1 1 calc GR . . . .
H5C H 0.295315 0.676059 0.388797 0.089 Uiso 1 1 calc GR . . . .
C6 C 0.1277(5) 0.3765(10) 0.6297(7) 0.042(2) Uani 1 1 d . . . . .
C7 C 0.1334(5) 0.3736(11) 0.7254(8) 0.048(2) Uani 1 1 d . . . . .
H7 H 0.172261 0.412515 0.755750 0.058 Uiso 1 1 calc R . . . .
C8 C 0.0781(6) 0.3093(13) 0.7771(9) 0.055(3) Uani 1 1 d . . . . .
H8 H 0.081007 0.301899 0.842021 0.066 Uiso 1 1 calc R . . . .
C9 C 0.0225(9) 0.2605(13) 0.7307(15) 0.077(5) Uani 1 1 d . . . . .
H9 H -0.014880 0.223778 0.765282 0.093 Uiso 1 1 calc R . . . .
C10 C 0.0161(7) 0.2604(11) 0.6319(12) 0.060(3) Uani 1 1 d . . . . .
H10 H -0.022484 0.220106 0.601837 0.072 Uiso 1 1 calc R . . . .
C11 C 0.0704(5) 0.3237(12) 0.5815(9) 0.053(3) Uani 1 1 d . . . . .
C12 C 0.0621(5) 0.3253(9) 0.4777(8) 0.049(2) Uani 1 1 d . . . . .
C13 C -0.0041(5) 0.3630(11) 0.4374(10) 0.061(3) Uani 1 1 d . . . . .
H13 H -0.042379 0.387471 0.475868 0.073 Uiso 1 1 calc R . . . .
C14 C -0.0127(6) 0.3641(12) 0.3405(9) 0.062(3) Uani 1 1 d . . . . .
H14 H -0.056727 0.390215 0.315176 0.074 Uiso 1 1 calc R . . . .
C15 C 0.0422(6) 0.3274(13) 0.2816(9) 0.068(3) Uani 1 1 d . . . . .
H15 H 0.035940 0.327344 0.216877 0.081 Uiso 1 1 calc R . . . .
C16 C 0.1082(6) 0.2901(13) 0.3221(9) 0.063(3) Uani 1 1 d . . . . .
H16 H 0.146681 0.265829 0.283862 0.076 Uiso 1 1 calc R . . . .
C17 C 0.1165(5) 0.2890(10) 0.4186(8) 0.051(2) Uani 1 1 d . . . . .
H17 H 0.160517 0.262686 0.443847 0.062 Uiso 1 1 calc R . . . .
C18 C 0.3710(4) 0.5057(8) 0.5255(6) 0.0367(16) Uani 1 1 d . . . . .
C19 C 0.4123(5) 0.5655(10) 0.5926(6) 0.046(2) Uani 1 1 d . . . . .
H19 H 0.390671 0.592261 0.648242 0.056 Uiso 1 1 calc R . . . .
C20 C 0.4840(6) 0.5863(11) 0.5794(8) 0.055(2) Uani 1 1 d . . . . .
H20 H 0.510681 0.628771 0.625399 0.066 Uiso 1 1 calc R . . . .
C21 C 0.5173(5) 0.5460(11) 0.5000(8) 0.058(3) Uani 1 1 d . . . . .
H21 H 0.566706 0.559179 0.491734 0.070 Uiso 1 1 calc R . . . .
C22 C 0.4757(5) 0.4830(9) 0.4291(7) 0.047(2) Uani 1 1 d . . . . .
H22 H 0.497918 0.457633 0.373595 0.056 Uiso 1 1 calc R . . . .
C23 C 0.4027(4) 0.4592(8) 0.4420(6) 0.0388(17) Uani 1 1 d . . . . .
C24 C 0.3614(5) 0.3871(9) 0.3678(6) 0.0430(19) Uani 1 1 d . . . . .
C25 C 0.3665(7) 0.4178(10) 0.2745(7) 0.055(2) Uani 1 1 d . . . . .
H25 H 0.390943 0.492748 0.257186 0.066 Uiso 1 1 calc R . . . .
C26 C 0.3367(7) 0.3416(14) 0.2059(8) 0.068(3) Uani 1 1 d . . . . .
H26 H 0.343133 0.361296 0.142854 0.082 Uiso 1 1 calc R . . . .
C27 C 0.2969(6) 0.2346(16) 0.2332(12) 0.073(5) Uani 1 1 d . . . . .
H27 H 0.274942 0.183496 0.187668 0.088 Uiso 1 1 calc R . . . .
C28 C 0.2893(6) 0.2026(13) 0.3258(9) 0.057(3) Uani 1 1 d . . . . .
H28 H 0.262061 0.131018 0.343455 0.069 Uiso 1 1 calc R . . . .
C29 C 0.3226(6) 0.2786(11) 0.3922(8) 0.051(2) Uani 1 1 d . . . . .
H29 H 0.318874 0.256051 0.455138 0.061 Uiso 1 1 calc R . . . .
C30 C 0.3297(9) 0.0856(13) 0.7377(9) 0.075(4) Uani 1 1 d . . . . .
H30A H 0.368675 0.060707 0.765456 0.090 Uiso 1 1 d R . . . .
H30B H 0.296525 0.124937 0.768906 0.090 Uiso 1 1 d R . . . .
C31 C 0.3205(10) 0.0645(13) 0.6484(10) 0.082(4) Uani 1 1 d . . . . .
H31 H 0.357297 0.021804 0.616451 0.098 Uiso 1 1 d R . . . .
C32 C 0.2613(11) 0.0995(12) 0.5985(12) 0.090(5) Uani 1 1 d . . . . .
H32A H 0.258222 0.082703 0.539575 0.108 Uiso 1 1 d R . . . .
H32B H 0.226442 0.139143 0.626395 0.108 Uiso 1 1 d 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 2.460(2) . ?
Pd1 C1 2.027(9) . ?
Pd1 C30 2.164(12) . ?
Pd1 H30B 2.0117 . ?
Pd1 C31 2.142(14) . ?
Pd1 C32 2.122(14) . ?
Pd1 H32B 1.9738 . ?
N1 C1 1.372(10) . ?
N1 C2 1.370(12) . ?
N1 C6 1.471(12) . ?
N2 C1 1.365(11) . ?
N2 C3 1.395(11) . ?
N2 C18 1.453(9) . ?
C2 C3 1.353(13) . ?
C2 C4 1.486(13) . ?
C3 C5 1.494(14) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.369(13) . ?
C6 C11 1.374(13) . ?
C7 H7 0.9300 . ?
C7 C8 1.425(16) . ?
C8 H8 0.9300 . ?
C8 C9 1.32(2) . ?
C9 H9 0.9300 . ?
C9 C10 1.41(2) . ?
C10 H10 0.9300 . ?
C10 C11 1.397(17) . ?
C11 C12 1.488(16) . ?
C12 C13 1.404(14) . ?
C12 C17 1.365(14) . ?
C13 H13 0.9300 . ?
C13 C14 1.392(18) . ?
C14 H14 0.9300 . ?
C14 C15 1.371(18) . ?
C15 H15 0.9300 . ?
C15 C16 1.403(17) . ?
C16 H16 0.9300 . ?
C16 C17 1.384(18) . ?
C17 H17 0.9300 . ?
C18 C19 1.372(12) . ?
C18 C23 1.412(12) . ?
C19 H19 0.9300 . ?
C19 C20 1.355(14) . ?
C20 H20 0.9300 . ?
C20 C21 1.355(15) . ?
C21 H21 0.9300 . ?
C21 C22 1.427(14) . ?
C22 H22 0.9300 . ?
C22 C23 1.382(12) . ?
C23 C24 1.502(12) . ?
C24 C25 1.372(14) . ?
C24 C29 1.376(15) . ?
C25 H25 0.9300 . ?
C25 C26 1.371(17) . ?
C26 H26 0.9300 . ?
C26 C27 1.38(2) . ?
C27 H27 0.9300 . ?
C27 C28 1.37(2) . ?
C28 H28 0.9300 . ?
C28 C29 1.377(16) . ?
C29 H29 0.9300 . ?
C30 H30A 0.8600 . ?
C30 H30B 0.8601 . ?
C30 C31 1.30(2) . ?
C31 H31 0.9299 . ?
C31 C32 1.35(2) . ?
C32 H32A 0.8600 . ?
C32 H32B 0.8600 . ?

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 H30B 88.0 . . ?
Cl1 Pd1 H32B 149.5 . . ?
C1 Pd1 Cl1 93.9(2) . . ?
C1 Pd1 C30 167.7(5) . . ?
C1 Pd1 H30B 156.1 . . ?
C1 Pd1 C31 133.9(5) . . ?
C1 Pd1 C32 101.0(6) . . ?
C1 Pd1 H32B 92.6 . . ?
C30 Pd1 Cl1 98.1(4) . . ?
C30 Pd1 H30B 23.4 . . ?
C30 Pd1 H32B 75.7 . . ?
H30B Pd1 H32B 74.6 . . ?
C31 Pd1 Cl1 130.9(5) . . ?
C31 Pd1 C30 35.2(6) . . ?
C31 Pd1 H30B 53.8 . . ?
C31 Pd1 H32B 55.6 . . ?
C32 Pd1 Cl1 163.4(4) . . ?
C32 Pd1 C30 66.8(6) . . ?
C32 Pd1 H30B 75.4 . . ?
C32 Pd1 C31 37.0(6) . . ?
C32 Pd1 H32B 23.9 . . ?
C1 N1 C6 121.4(7) . . ?
C2 N1 C1 112.6(7) . . ?
C2 N1 C6 125.9(7) . . ?
C1 N2 C3 112.1(6) . . ?
C1 N2 C18 125.4(7) . . ?
C3 N2 C18 122.5(7) . . ?
N1 C1 Pd1 128.3(6) . . ?
N2 C1 Pd1 129.0(6) . . ?
N2 C1 N1 102.5(7) . . ?
N1 C2 C4 125.5(8) . . ?
C3 C2 N1 106.9(8) . . ?
C3 C2 C4 127.5(9) . . ?
N2 C3 C5 121.8(8) . . ?
C2 C3 N2 106.0(8) . . ?
C2 C3 C5 131.9(9) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 115.5(9) . . ?
C7 C6 C11 123.3(11) . . ?
C11 C6 N1 121.2(9) . . ?
C6 C7 H7 120.9 . . ?
C6 C7 C8 118.2(11) . . ?
C8 C7 H7 120.9 . . ?
C7 C8 H8 120.8 . . ?
C9 C8 C7 118.3(13) . . ?
C9 C8 H8 120.8 . . ?
C8 C9 H9 117.8 . . ?
C8 C9 C10 124.4(14) . . ?
C10 C9 H9 117.8 . . ?
C9 C10 H10 121.6 . . ?
C11 C10 C9 116.9(15) . . ?
C11 C10 H10 121.6 . . ?
C6 C11 C10 118.8(12) . . ?
C6 C11 C12 124.9(10) . . ?
C10 C11 C12 116.2(10) . . ?
C13 C12 C11 120.0(10) . . ?
C17 C12 C11 122.3(9) . . ?
C17 C12 C13 117.6(10) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.5(10) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 119.3 . . ?
C15 C14 C13 121.5(10) . . ?
C15 C14 H14 119.3 . . ?
C14 C15 H15 121.1 . . ?
C14 C15 C16 117.8(12) . . ?
C16 C15 H15 121.1 . . ?
C15 C16 H16 119.7 . . ?
C17 C16 C15 120.5(11) . . ?
C17 C16 H16 119.7 . . ?
C12 C17 C16 122.0(10) . . ?
C12 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
C19 C18 N2 119.0(7) . . ?
C19 C18 C23 120.8(7) . . ?
C23 C18 N2 120.1(7) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 C18 121.2(9) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.7(9) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 120.4 . . ?
C20 C21 C22 119.2(8) . . ?
C22 C21 H21 120.4 . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.8(9) . . ?
C23 C22 H22 119.6 . . ?
C18 C23 C24 123.6(7) . . ?
C22 C23 C18 117.1(8) . . ?
C22 C23 C24 119.3(8) . . ?
C25 C24 C23 122.2(9) . . ?
C25 C24 C29 118.0(10) . . ?
C29 C24 C23 119.4(9) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 C24 122.1(11) . . ?
C26 C25 H25 119.0 . . ?
C25 C26 H26 120.9 . . ?
C25 C26 C27 118.2(12) . . ?
C27 C26 H26 120.9 . . ?
C26 C27 H27 119.4 . . ?
C28 C27 C26 121.2(12) . . ?
C28 C27 H27 119.4 . . ?
C27 C28 H28 120.7 . . ?
C27 C28 C29 118.7(13) . . ?
C29 C28 H28 120.7 . . ?
C24 C29 C28 121.6(11) . . ?
C24 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
Pd1 C30 H30A 132.9 . . ?
Pd1 C30 H30B 68.3 . . ?
H30A C30 H30B 120.0 . . ?
C31 C30 Pd1 71.5(8) . . ?
C31 C30 H30A 120.6 . . ?
C31 C30 H30B 119.4 . . ?
Pd1 C31 H31 132.4 . . ?
C30 C31 Pd1 73.3(9) . . ?
C30 C31 H31 117.6 . . ?
C30 C31 C32 125.1(16) . . ?
C32 C31 Pd1 70.7(8) . . ?
C32 C31 H31 117.4 . . ?
Pd1 C32 H32A 131.6 . . ?
Pd1 C32 H32B 68.3 . . ?
C31 C32 Pd1 72.3(9) . . ?
C31 C32 H32A 120.8 . . ?
C31 C32 H32B 119.2 . . ?
H32A C32 H32B 120.0 . . ?


_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 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.788
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.81(7)
2 0.19(7)

####################################################################### 
# 
# 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_lk41062meso
_database_code_depnum_ccdc_archive 'CCDC 2250212'
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi'
;Aix Marseille University CNRS
France
;
_audit_update_record             
;
2023-03-20 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2020-01-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H41 Cl N2 Pd, C0.5 Cl1, 0.5(C3 H6)'
_chemical_formula_sum            'C48 H44.50 Cl2 N2 Pd'
_chemical_formula_weight         826.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c46 h42 Cl1 n2 Pd1'
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                   11.0273(2)
_cell_length_b                   11.7303(2)
_cell_length_c                   17.0058(2)
_cell_angle_alpha                102.2810(10)
_cell_angle_beta                 101.4300(10)
_cell_angle_gamma                91.4670(10)
_cell_volume                     2101.51(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    48773
_cell_measurement_temperature    295
_cell_measurement_theta_max      27.5810
_cell_measurement_theta_min      3.3670
_shelx_estimated_absorpt_T_max   0.953
_shelx_estimated_absorpt_T_min   0.869
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             853
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            94003
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.583
_diffrn_reflns_theta_min         2.799
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00 -24.00   1.00   10.00    --   -8.02 126.00-159.85   41
  2  ω    -67.00 -27.00   1.00   10.00    --   -8.02 129.00 -46.44   40
  3  ω    -24.00  84.00   1.00   10.00    --    8.25  77.00 -30.00  108
  4  ω    -16.00  83.00   1.00   10.00    --    8.25  38.00 120.00   99
  5  ω    -66.00  33.00   1.00   10.00    --    8.25 -38.00 -60.00   99
  6  ω    -16.00  83.00   1.00   10.00    --    8.25  38.00-120.00   99
  7  ω    -66.00  33.00   1.00   10.00    --    8.25 -38.00  60.00   99
  8  ω    -20.00  49.00   1.00   10.00    --    8.25 -99.00-180.00   69
  9  ω    -62.00 -20.00   1.00   10.00    --   -8.02 121.00   7.61   42
 10  ω    -67.00 -27.00   1.00   10.00    --   -8.02 129.00 126.18   40
 11  ω    -75.00 -33.00   1.00   10.00    --   -8.02 142.00  48.63   42
 12  ω    -77.00 -34.00   1.00   10.00    --   -8.02 145.00 -99.87   43
 13  ω    -63.00 -22.00   1.00   10.00    --   -8.02 123.00-121.09   41
 14  ω    -80.00  96.00   1.00   10.00    --    8.25   0.00-180.00  176
 15  ω    -66.00  33.00   1.00   10.00    --    8.25 -38.00-150.00   99
 16  ω    -80.00  96.00   1.00   10.00    --    8.25   0.00-120.00  176
 17  ω    -80.00  96.00   1.00   10.00    --    8.25   0.00 -90.00  176
 18  ω    -80.00  96.00   1.00   10.00    --    8.25   0.00-150.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0086965000
_diffrn_orient_matrix_UB_12      0.0589202000
_diffrn_orient_matrix_UB_13      0.0175769000
_diffrn_orient_matrix_UB_21      0.0651997000
_diffrn_orient_matrix_UB_22      0.0119998000
_diffrn_orient_matrix_UB_23      0.0122425000
_diffrn_orient_matrix_UB_31      0.0012305000
_diffrn_orient_matrix_UB_32      0.0152716000
_diffrn_orient_matrix_UB_33      -0.0380270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8531
_reflns_number_total             9686
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         9686
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0656P)²+1.0817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1193
_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. Restrained distances
 C50-C49
 1.54 with sigma of 0.005
 C49-C48
 1.54 with sigma of 0.005
 C53-C52
 1.54 with sigma of 0.005
 C52-C51
 1.54 with sigma of 0.005
 C50-C48_$1
 1.54 with sigma of 0.005
 C48-C50_$1
 1.54 with sigma of 0.005
 C47-Cl2
 1.7 with sigma of 0.005
 C47-Cl3
 1.7 with sigma of 0.005
 C47-Cl4
 1.7 with sigma of 0.005
 C47-Cl5
 1.7 with sigma of 0.005
 C47-Cl6
 1.7 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C47 \\sim Cl2: within 1.8A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C50) = Uanis(C53)
Uanis(C52) = Uanis(C49)
Uanis(C48) = Uanis(C51)
4. Rigid body (RIGU) restrains
 C48, C49, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C51, C52, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl2, Cl3, Cl4, Cl5, Cl6, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cl2(0.2) Cl3(0.2) Cl4(0.2) Cl5(0.2) Cl6(0.2) C47(0.5) C48(0.25)
 H48A(0.25) H48B(0.25) C49(0.25) H49A(0.25) H49B(0.25) C50(0.25) H50A(0.25)
 H50B(0.25) C51(0.25) H51B(0.25) H51A(0.25) C52(0.25) H52A(0.25) H52B(0.25)
 C53(0.25) H53B(0.25) H53A(0.25)
6.a Riding coordinates:
 C45(H45)
6.b Ternary CH refined with riding coordinates:
 C12(H12), C31(H31)
6.c Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51B,H51A), C52(H52A,
 H52B), C53(H53B,H53A)
6.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43)
6.e X=CH2 refined with riding coordinates:
 C44(H44A,H44B), C46(H46A,H46B)
6.f Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.46834(2) 0.80580(2) 0.90808(2) 0.04461(8) Uani 1 1 d . . . . .
Cl1 Cl 0.68499(7) 0.79086(7) 0.94860(5) 0.0706(2) Uani 1 1 d . . . . .
N1 N 0.51689(18) 0.78820(17) 0.73435(12) 0.0430(4) Uani 1 1 d . . . . .
N2 N 0.46293(18) 0.62119(17) 0.75223(11) 0.0427(4) Uani 1 1 d . . . . .
C1 C 0.4751(2) 0.7367(2) 0.78876(14) 0.0413(5) Uani 1 1 d . . . . .
C2 C 0.5352(2) 0.7057(2) 0.66545(15) 0.0496(6) Uani 1 1 d . . . . .
C3 C 0.5022(2) 0.6007(2) 0.67703(15) 0.0492(5) Uani 1 1 d . . . . .
C4 C 0.5862(3) 0.7389(3) 0.5980(2) 0.0708(8) Uani 1 1 d . . . . .
H4A H 0.523401 0.772770 0.564209 0.106 Uiso 1 1 calc GR . . . .
H4B H 0.612050 0.670476 0.565088 0.106 Uiso 1 1 calc GR . . . .
H4C H 0.656046 0.794689 0.621190 0.106 Uiso 1 1 calc GR . . . .
C5 C 0.5087(3) 0.4799(3) 0.6272(2) 0.0703(8) Uani 1 1 d . . . . .
H5A H 0.536077 0.428835 0.663393 0.105 Uiso 1 1 calc GR . . . .
H5B H 0.566041 0.482077 0.591723 0.105 Uiso 1 1 calc GR . . . .
H5C H 0.427976 0.451404 0.594520 0.105 Uiso 1 1 calc GR . . . .
C6 C 0.5400(2) 0.9123(2) 0.74594(14) 0.0443(5) Uani 1 1 d . . . . .
C7 C 0.6585(3) 0.9628(3) 0.78163(18) 0.0586(6) Uani 1 1 d . . . . .
H7 H 0.721229 0.916693 0.798994 0.070 Uiso 1 1 calc R . . . .
C8 C 0.6833(3) 1.0810(3) 0.79140(19) 0.0658(8) Uani 1 1 d . . . . .
H8 H 0.762980 1.114709 0.815189 0.079 Uiso 1 1 calc R . . . .
C9 C 0.5910(3) 1.1490(3) 0.76614(18) 0.0627(7) Uani 1 1 d . . . . .
H9 H 0.608381 1.228851 0.772542 0.075 Uiso 1 1 calc R . . . .
C10 C 0.4721(3) 1.1001(2) 0.73121(18) 0.0569(6) Uani 1 1 d . . . . .
H10 H 0.410079 1.147348 0.714643 0.068 Uiso 1 1 calc R . . . .
C11 C 0.4442(2) 0.9798(2) 0.72049(15) 0.0460(5) Uani 1 1 d . . . . .
C12 C 0.3147(2) 0.9228(2) 0.67994(16) 0.0475(5) Uani 1 1 d . . . . .
H12 H 0.307285 0.852323 0.701423 0.057 Uiso 1 1 calc R . . . .
C13 C 0.2110(2) 0.9981(2) 0.70454(18) 0.0530(6) Uani 1 1 d . . . . .
C14 C 0.2209(3) 1.0553(3) 0.7859(2) 0.0716(8) Uani 1 1 d . . . . .
H14 H 0.292250 1.050560 0.824377 0.086 Uiso 1 1 calc R . . . .
C15 C 0.1265(4) 1.1193(4) 0.8107(3) 0.0919(13) Uani 1 1 d . . . . .
H15 H 0.134132 1.157768 0.865364 0.110 Uiso 1 1 calc R . . . .
C16 C 0.0215(4) 1.1253(4) 0.7538(4) 0.1073(17) Uani 1 1 d . . . . .
H16 H -0.042058 1.168661 0.770431 0.129 Uiso 1 1 calc R . . . .
C17 C 0.0082(4) 1.0700(4) 0.6743(4) 0.1009(14) Uani 1 1 d . . . . .
H17 H -0.063976 1.074975 0.636557 0.121 Uiso 1 1 calc R . . . .
C18 C 0.1042(3) 1.0045(3) 0.6488(2) 0.0721(8) Uani 1 1 d . . . . .
H18 H 0.095214 0.965483 0.594045 0.087 Uiso 1 1 calc R . . . .
C19 C 0.3014(2) 0.8803(2) 0.58730(17) 0.0521(6) Uani 1 1 d . . . . .
C20 C 0.3455(3) 0.9466(3) 0.53892(19) 0.0636(7) Uani 1 1 d . . . . .
H20 H 0.384453 1.020515 0.563248 0.076 Uiso 1 1 calc R . . . .
C21 C 0.3322(3) 0.9043(4) 0.4550(2) 0.0755(9) Uani 1 1 d . . . . .
H21 H 0.362395 0.949765 0.423504 0.091 Uiso 1 1 calc R . . . .
C22 C 0.2747(4) 0.7960(4) 0.4182(2) 0.0834(10) Uani 1 1 d . . . . .
H22 H 0.266578 0.767344 0.361875 0.100 Uiso 1 1 calc R . . . .
C23 C 0.2293(5) 0.7300(4) 0.4647(2) 0.0952(13) Uani 1 1 d . . . . .
H23 H 0.189220 0.656708 0.439870 0.114 Uiso 1 1 calc R . . . .
C24 C 0.2428(4) 0.7720(3) 0.5485(2) 0.0750(9) Uani 1 1 d . . . . .
H24 H 0.211778 0.726116 0.579395 0.090 Uiso 1 1 calc R . . . .
C25 C 0.4236(2) 0.5332(2) 0.79097(14) 0.0456(5) Uani 1 1 d . . . . .
C26 C 0.5093(3) 0.5071(2) 0.85494(17) 0.0569(6) Uani 1 1 d . . . . .
H26 H 0.589162 0.543134 0.869524 0.068 Uiso 1 1 calc R . . . .
C27 C 0.4750(3) 0.4268(3) 0.89686(18) 0.0675(8) Uani 1 1 d . . . . .
H27 H 0.531904 0.408741 0.939866 0.081 Uiso 1 1 calc R . . . .
C28 C 0.3586(4) 0.3746(3) 0.8755(2) 0.0721(9) Uani 1 1 d . . . . .
H28 H 0.336046 0.320785 0.903984 0.087 Uiso 1 1 calc R . . . .
C29 C 0.2731(3) 0.4005(3) 0.8115(2) 0.0677(8) Uani 1 1 d . . . . .
H29 H 0.193619 0.363694 0.797577 0.081 Uiso 1 1 calc R . . . .
C30 C 0.3037(3) 0.4809(2) 0.76742(16) 0.0517(6) Uani 1 1 d . . . . .
C31 C 0.2098(2) 0.5099(2) 0.69628(16) 0.0531(6) Uani 1 1 d . . . . .
H31 H 0.246929 0.578800 0.683535 0.064 Uiso 1 1 calc R . . . .
C32 C 0.1857(2) 0.4160(2) 0.61652(17) 0.0528(6) Uani 1 1 d . . . . .
C33 C 0.1927(4) 0.2981(3) 0.6119(2) 0.0743(9) Uani 1 1 d . . . . .
H33 H 0.217520 0.270893 0.659670 0.089 Uiso 1 1 calc R . . . .
C34 C 0.1630(4) 0.2196(3) 0.5365(2) 0.0828(10) Uani 1 1 d . . . . .
H34 H 0.168053 0.140016 0.534540 0.099 Uiso 1 1 calc R . . . .
C35 C 0.1264(3) 0.2564(3) 0.4651(2) 0.0701(8) Uani 1 1 d . . . . .
H35 H 0.105896 0.202597 0.414946 0.084 Uiso 1 1 calc R . . . .
C36 C 0.1204(3) 0.3723(3) 0.4685(2) 0.0732(8) Uani 1 1 d . . . . .
H36 H 0.097432 0.398984 0.420347 0.088 Uiso 1 1 calc R . . . .
C37 C 0.1486(3) 0.4512(3) 0.54410(19) 0.0669(8) Uani 1 1 d . . . . .
H37 H 0.142025 0.530506 0.545681 0.080 Uiso 1 1 calc R . . . .
C38 C 0.0881(3) 0.5465(3) 0.71982(17) 0.0607(7) Uani 1 1 d . . . . .
C39 C -0.0071(3) 0.4665(4) 0.7195(2) 0.0759(9) Uani 1 1 d . . . . .
H39 H 0.002307 0.386768 0.704365 0.091 Uiso 1 1 calc R . . . .
C40 C -0.1168(4) 0.5050(5) 0.7417(3) 0.0997(14) Uani 1 1 d . . . . .
H40 H -0.180098 0.450637 0.741052 0.120 Uiso 1 1 calc R . . . .
C41 C -0.1320(5) 0.6216(6) 0.7643(3) 0.1113(18) Uani 1 1 d . . . . .
H41 H -0.204140 0.646844 0.780790 0.134 Uiso 1 1 calc R . . . .
C42 C -0.0397(5) 0.7013(5) 0.7625(3) 0.1116(18) Uani 1 1 d . . . . .
H42 H -0.050679 0.780822 0.776648 0.134 Uiso 1 1 calc R . . . .
C43 C 0.0693(4) 0.6648(3) 0.7400(2) 0.0794(10) Uani 1 1 d . . . . .
H43 H 0.130402 0.719836 0.738354 0.095 Uiso 1 1 calc R . . . .
C44 C 0.2762(3) 0.8160(3) 0.9035(2) 0.0708(8) Uani 1 1 d . . . . .
H44A H 0.293625 0.737736 0.894275 0.085 Uiso 1 1 calc R . . . .
H44B H 0.216062 0.841729 0.865800 0.085 Uiso 1 1 calc R . . . .
C45 C 0.3406(3) 0.8956(3) 0.9744(2) 0.0682(8) Uani 1 1 d . . . . .
H45 H 0.322244 0.973599 0.983111 0.082 Uiso 1 1 d R . . . .
C46 C 0.4300(3) 0.8606(3) 1.03132(18) 0.0692(8) Uani 1 1 d . . . . .
H46A H 0.449006 0.782731 1.023411 0.083 Uiso 1 1 calc R . . . .
H46B H 0.471405 0.914760 1.077754 0.083 Uiso 1 1 calc R . . . .
Cl2 Cl -0.0225(15) 1.1209(11) 1.0091(11) 0.195(4) Uani 0.2 1 d D U P A 5
Cl3 Cl -0.0611(10) 1.0926(13) 0.9624(9) 0.179(6) Uani 0.2 1 d D U P A 4
Cl4 Cl -0.067(2) 1.021(3) 0.9193(10) 0.212(15) Uani 0.2 1 d D U P A 3
Cl5 Cl -0.0236(14) 1.0029(15) 0.9179(7) 0.122(4) Uani 0.2 1 d D U P A 2
Cl6 Cl -0.0075(17) 0.9427(18) 0.9169(7) 0.170(6) Uani 0.2 1 d D U P A 1
C47 C -0.0462(17) 0.9781(11) 1.0097(6) 0.189(4) Uani 0.5 1 d D U P . .
C48 C 0.1535(14) 0.5203(15) 1.015(2) 0.108(5) Uani 0.25 1 d D U P B 1
H48A H 0.210121 0.536409 0.981324 0.130 Uiso 0.25 1 calc R . P B 1
H48B H 0.201378 0.516126 1.068782 0.130 Uiso 0.25 1 calc R . P B 1
C49 C 0.0752(13) 0.4057(17) 0.975(2) 0.126(5) Uani 0.25 1 d D U P B 1
H49A H 0.118366 0.345405 0.997675 0.151 Uiso 0.25 1 calc R . P B 1
H49B H 0.080232 0.389638 0.917062 0.151 Uiso 0.25 1 calc R . P B 1
C50 C -0.0616(12) 0.3838(16) 0.9761(19) 0.128(6) Uani 0.25 1 d D U P B 1
H50A H -0.063103 0.344523 1.020663 0.153 Uiso 0.25 1 calc R . P B 1
H50B H -0.097168 0.327354 0.925600 0.153 Uiso 0.25 1 calc R . P B 1
C51 C 0.1174(14) 0.4940(18) 1.020(2) 0.108(5) Uani 0.25 1 d D U P C 2
H51B H 0.140286 0.481141 1.075710 0.130 Uiso 0.25 1 calc R . P C 2
H51A H 0.191503 0.483943 0.997705 0.130 Uiso 0.25 1 calc R . P C 2
C52 C 0.0285(13) 0.3884(18) 0.972(2) 0.126(5) Uani 0.25 1 d D U P C 2
H52A H 0.044567 0.322403 0.997852 0.151 Uiso 0.25 1 calc R . P C 2
H52B H 0.040664 0.366242 0.916212 0.151 Uiso 0.25 1 calc R . P C 2
C53 C -0.1049(14) 0.4224(18) 0.9723(19) 0.128(6) Uani 0.25 1 d D U P C 2
H53B H -0.157362 0.381812 0.920539 0.153 Uiso 0.25 1 calc R . P C 2
H53A H -0.132876 0.394380 1.015853 0.153 Uiso 0.25 1 calc R . P C 2


_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 2.3735(8) . ?
Pd1 C1 2.035(2) . ?
Pd1 C44 2.113(3) . ?
Pd1 C45 2.136(3) . ?
Pd1 C46 2.186(3) . ?
N1 C1 1.352(3) . ?
N1 C2 1.404(3) . ?
N1 C6 1.437(3) . ?
N2 C1 1.356(3) . ?
N2 C3 1.405(3) . ?
N2 C25 1.438(3) . ?
C2 C3 1.340(4) . ?
C2 C4 1.489(4) . ?
C3 C5 1.500(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.385(4) . ?
C6 C11 1.392(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.374(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.369(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.381(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.401(4) . ?
C11 C12 1.525(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.532(4) . ?
C12 C19 1.524(4) . ?
C13 C14 1.384(5) . ?
C13 C18 1.373(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.380(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.367(7) . ?
C16 H16 0.9300 . ?
C16 C17 1.347(7) . ?
C17 H17 0.9300 . ?
C17 C18 1.408(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.389(4) . ?
C19 C24 1.378(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.385(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.368(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.369(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.381(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.386(3) . ?
C25 C30 1.389(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.383(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.355(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.384(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.396(4) . ?
C30 C31 1.533(3) . ?
C31 H31 0.9800 . ?
C31 C32 1.527(4) . ?
C31 C38 1.522(4) . ?
C32 C33 1.373(4) . ?
C32 C37 1.371(4) . ?
C33 H33 0.9300 . ?
C33 C34 1.383(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.364(5) . ?
C35 H35 0.9300 . ?
C35 C36 1.352(5) . ?
C36 H36 0.9300 . ?
C36 C37 1.388(4) . ?
C37 H37 0.9300 . ?
C38 C39 1.388(5) . ?
C38 C43 1.388(5) . ?
C39 H39 0.9300 . ?
C39 C40 1.395(6) . ?
C40 H40 0.9300 . ?
C40 C41 1.364(7) . ?
C41 H41 0.9300 . ?
C41 C42 1.373(8) . ?
C42 H42 0.9300 . ?
C42 C43 1.384(6) . ?
C43 H43 0.9300 . ?
C44 H44A 0.9300 . ?
C44 H44B 0.9300 . ?
C44 C45 1.406(4) . ?
C45 H45 0.9300 . ?
C45 C46 1.374(5) . ?
C46 H46A 0.9300 . ?
C46 H46B 0.9300 . ?
Cl2 C47 1.692(5) . ?
Cl2 C47 1.42(2) 2_577 ?
Cl3 C47 1.520(19) 2_577 ?
Cl3 C47 1.703(5) . ?
Cl4 C47 1.56(2) 2_577 ?
Cl4 C47 1.691(5) . ?
Cl5 C47 1.29(2) 2_577 ?
Cl5 C47 1.711(5) . ?
Cl6 C47 1.687(5) . ?
Cl6 C47 1.40(2) 2_577 ?
C47 Cl2 1.42(2) 2_577 ?
C47 Cl3 1.520(19) 2_577 ?
C47 Cl4 1.56(2) 2_577 ?
C47 Cl5 1.29(2) 2_577 ?
C47 Cl6 1.40(2) 2_577 ?
C47 C47 1.26(3) 2_577 ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 C49 1.530(5) . ?
C48 C50 1.536(4) 2_567 ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 C50 1.530(5) . ?
C50 C48 1.536(4) 2_567 ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 H51B 0.9700 . ?
C51 H51A 0.9700 . ?
C51 C52 1.533(5) . ?
C51 C53 0.98(3) 2_567 ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.534(5) . ?
C53 C51 0.98(3) 2_567 ?
C53 H53B 0.9700 . ?
C53 H53A 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 Cl1 90.42(7) . . ?
C1 Pd1 C44 102.80(11) . . ?
C1 Pd1 C45 137.61(12) . . ?
C1 Pd1 C46 169.72(11) . . ?
C44 Pd1 Cl1 165.24(10) . . ?
C44 Pd1 C45 38.65(12) . . ?
C44 Pd1 C46 68.70(14) . . ?
C45 Pd1 Cl1 130.55(10) . . ?
C45 Pd1 C46 37.05(13) . . ?
C46 Pd1 Cl1 97.43(10) . . ?
C1 N1 C2 111.8(2) . . ?
C1 N1 C6 123.93(19) . . ?
C2 N1 C6 124.3(2) . . ?
C1 N2 C3 111.4(2) . . ?
C1 N2 C25 122.44(19) . . ?
C3 N2 C25 126.0(2) . . ?
N1 C1 Pd1 128.98(17) . . ?
N1 C1 N2 103.95(19) . . ?
N2 C1 Pd1 125.75(17) . . ?
N1 C2 C4 122.7(3) . . ?
C3 C2 N1 106.2(2) . . ?
C3 C2 C4 131.0(3) . . ?
N2 C3 C5 122.5(3) . . ?
C2 C3 N2 106.5(2) . . ?
C2 C3 C5 130.9(3) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 119.1(2) . . ?
C7 C6 C11 121.0(2) . . ?
C11 C6 N1 119.9(2) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(3) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.0(3) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 119.7 . . ?
C8 C9 C10 120.5(3) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.6(3) . . ?
C11 C10 H10 119.7 . . ?
C6 C11 C10 117.7(2) . . ?
C6 C11 C12 120.5(2) . . ?
C10 C11 C12 121.8(2) . . ?
C11 C12 H12 105.9 . . ?
C11 C12 C13 113.1(2) . . ?
C13 C12 H12 105.9 . . ?
C19 C12 C11 111.3(2) . . ?
C19 C12 H12 105.9 . . ?
C19 C12 C13 113.9(2) . . ?
C14 C13 C12 119.6(3) . . ?
C18 C13 C12 121.5(3) . . ?
C18 C13 C14 118.7(3) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 121.0(4) . . ?
C15 C14 H14 119.5 . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.2(4) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 119.3 . . ?
C17 C16 C15 121.4(4) . . ?
C17 C16 H16 119.3 . . ?
C16 C17 H17 120.2 . . ?
C16 C17 C18 119.6(4) . . ?
C18 C17 H17 120.2 . . ?
C13 C18 C17 120.1(4) . . ?
C13 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 C12 122.8(2) . . ?
C24 C19 C12 119.6(3) . . ?
C24 C19 C20 117.6(3) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 120.9(3) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.3(3) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.2 . . ?
C21 C22 C23 119.6(3) . . ?
C23 C22 H22 120.2 . . ?
C22 C23 H23 119.9 . . ?
C22 C23 C24 120.2(4) . . ?
C24 C23 H23 119.9 . . ?
C19 C24 C23 121.5(3) . . ?
C19 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C26 C25 N2 116.7(2) . . ?
C26 C25 C30 121.9(3) . . ?
C30 C25 N2 121.3(2) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 C25 119.3(3) . . ?
C27 C26 H26 120.4 . . ?
C26 C27 H27 119.9 . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.5(3) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 119.4 . . ?
C28 C29 C30 121.3(3) . . ?
C30 C29 H29 119.4 . . ?
C25 C30 C29 116.8(2) . . ?
C25 C30 C31 121.5(2) . . ?
C29 C30 C31 121.7(3) . . ?
C30 C31 H31 105.8 . . ?
C32 C31 C30 114.9(2) . . ?
C32 C31 H31 105.8 . . ?
C38 C31 C30 113.1(2) . . ?
C38 C31 H31 105.8 . . ?
C38 C31 C32 110.6(2) . . ?
C33 C32 C31 125.0(3) . . ?
C37 C32 C31 117.6(3) . . ?
C37 C32 C33 117.3(3) . . ?
C32 C33 H33 119.8 . . ?
C32 C33 C34 120.5(3) . . ?
C34 C33 H33 119.8 . . ?
C33 C34 H34 119.3 . . ?
C35 C34 C33 121.4(3) . . ?
C35 C34 H34 119.3 . . ?
C34 C35 H35 120.5 . . ?
C36 C35 C34 119.0(3) . . ?
C36 C35 H35 120.5 . . ?
C35 C36 H36 120.1 . . ?
C35 C36 C37 119.8(3) . . ?
C37 C36 H36 120.1 . . ?
C32 C37 C36 122.1(3) . . ?
C32 C37 H37 119.0 . . ?
C36 C37 H37 119.0 . . ?
C39 C38 C31 122.9(3) . . ?
C39 C38 C43 118.3(3) . . ?
C43 C38 C31 118.8(3) . . ?
C38 C39 H39 119.8 . . ?
C38 C39 C40 120.4(4) . . ?
C40 C39 H39 119.8 . . ?
C39 C40 H40 119.7 . . ?
C41 C40 C39 120.6(5) . . ?
C41 C40 H40 119.7 . . ?
C40 C41 H41 120.3 . . ?
C40 C41 C42 119.4(4) . . ?
C42 C41 H41 120.3 . . ?
C41 C42 H42 119.6 . . ?
C41 C42 C43 120.8(5) . . ?
C43 C42 H42 119.6 . . ?
C38 C43 H43 119.8 . . ?
C42 C43 C38 120.4(4) . . ?
C42 C43 H43 119.8 . . ?
Pd1 C44 H44A 71.3 . . ?
Pd1 C44 H44B 129.6 . . ?
H44A C44 H44B 120.0 . . ?
C45 C44 Pd1 71.58(19) . . ?
C45 C44 H44A 120.0 . . ?
C45 C44 H44B 120.0 . . ?
Pd1 C45 H45 130.5 . . ?
C44 C45 Pd1 69.76(18) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 Pd1 73.43(19) . . ?
C46 C45 C44 121.5(3) . . ?
C46 C45 H45 119.2 . . ?
Pd1 C46 H46A 71.5 . . ?
Pd1 C46 H46B 131.8 . . ?
C45 C46 Pd1 69.52(17) . . ?
C45 C46 H46A 120.0 . . ?
C45 C46 H46B 120.0 . . ?
H46A C46 H46B 120.0 . . ?
C47 Cl2 C47 46.8(13) 2_577 . ?
C47 Cl3 C47 45.6(11) 2_577 . ?
C47 Cl4 C47 45.5(10) 2_577 . ?
C47 Cl5 C47 47.2(13) 2_577 . ?
C47 Cl6 C47 47.1(12) 2_577 . ?
Cl2 C47 Cl2 133.2(13) 2_577 . ?
Cl3 C47 Cl3 134.4(11) 2_577 . ?
Cl4 C47 Cl4 134.5(10) 2_577 . ?
Cl5 C47 Cl5 132.8(13) 2_577 . ?
Cl6 C47 Cl6 132.9(12) 2_577 . ?
C47 C47 Cl2 55.1(10) 2_577 . ?
C47 C47 Cl2 78.1(12) 2_577 2_577 ?
C47 C47 Cl3 74.8(14) 2_577 2_577 ?
C47 C47 Cl3 59.5(8) 2_577 . ?
C47 C47 Cl4 61.6(9) 2_577 . ?
C47 C47 Cl4 72.9(15) 2_577 2_577 ?
C47 C47 Cl5 48.4(9) 2_577 . ?
C47 C47 Cl5 84.4(18) 2_577 2_577 ?
C47 C47 Cl6 78.5(16) 2_577 2_577 ?
C47 C47 Cl6 54.4(10) 2_577 . ?
H48A C48 H48B 108.7 . . ?
C49 C48 H48A 110.5 . . ?
C49 C48 H48B 110.5 . . ?
C49 C48 C50 106.2(15) . 2_567 ?
C50 C48 H48A 110.5 2_567 . ?
C50 C48 H48B 110.5 2_567 . ?
C48 C49 H49A 106.1 . . ?
C48 C49 H49B 106.1 . . ?
C48 C49 C50 124.9(14) . . ?
H49A C49 H49B 106.3 . . ?
C50 C49 H49A 106.1 . . ?
C50 C49 H49B 106.1 . . ?
C48 C50 H50A 106.2 2_567 . ?
C48 C50 H50B 106.2 2_567 . ?
C49 C50 C48 124.5(16) . 2_567 ?
C49 C50 H50A 106.2 . . ?
C49 C50 H50B 106.2 . . ?
H50A C50 H50B 106.4 . . ?
H51B C51 H51A 105.8 . . ?
C52 C51 H51B 104.9 . . ?
C52 C51 H51A 104.9 . . ?
C53 C51 H51B 104.9 2_567 . ?
C53 C51 H51A 104.9 2_567 . ?
C53 C51 C52 130(2) 2_567 . ?
C51 C52 H52A 110.0 . . ?
C51 C52 H52B 110.0 . . ?
C51 C52 C53 108.4(13) . . ?
H52A C52 H52B 108.4 . . ?
C53 C52 H52A 110.0 . . ?
C53 C52 H52B 110.0 . . ?
C51 C53 C52 116(2) 2_567 . ?
C51 C53 H53B 108.3 2_567 . ?
C51 C53 H53A 108.3 2_567 . ?
C52 C53 H53B 108.3 . . ?
C52 C53 H53A 108.3 . . ?
H53B C53 H53A 107.4 . . ?

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
Pd1 C44 C45 C46 -54.4(3) . . . . ?
N1 C2 C3 N2 0.7(3) . . . . ?
N1 C2 C3 C5 -175.9(3) . . . . ?
N1 C6 C7 C8 178.4(2) . . . . ?
N1 C6 C11 C10 -178.4(2) . . . . ?
N1 C6 C11 C12 -0.3(3) . . . . ?
N2 C25 C26 C27 177.2(2) . . . . ?
N2 C25 C30 C29 -177.1(3) . . . . ?
N2 C25 C30 C31 3.1(4) . . . . ?
C1 N1 C2 C3 0.9(3) . . . . ?
C1 N1 C2 C4 -177.2(3) . . . . ?
C1 N1 C6 C7 93.6(3) . . . . ?
C1 N1 C6 C11 -87.1(3) . . . . ?
C1 N2 C3 C2 -2.1(3) . . . . ?
C1 N2 C3 C5 174.8(2) . . . . ?
C1 N2 C25 C26 -74.0(3) . . . . ?
C1 N2 C25 C30 103.4(3) . . . . ?
C2 N1 C1 Pd1 165.16(17) . . . . ?
C2 N1 C1 N2 -2.1(3) . . . . ?
C2 N1 C6 C7 -86.2(3) . . . . ?
C2 N1 C6 C11 93.0(3) . . . . ?
C3 N2 C1 Pd1 -165.24(16) . . . . ?
C3 N2 C1 N1 2.6(2) . . . . ?
C3 N2 C25 C26 100.9(3) . . . . ?
C3 N2 C25 C30 -81.8(3) . . . . ?
C4 C2 C3 N2 178.6(3) . . . . ?
C4 C2 C3 C5 2.0(5) . . . . ?
C6 N1 C1 Pd1 -14.7(3) . . . . ?
C6 N1 C1 N2 178.0(2) . . . . ?
C6 N1 C2 C3 -179.3(2) . . . . ?
C6 N1 C2 C4 2.7(4) . . . . ?
C6 C7 C8 C9 0.2(4) . . . . ?
C6 C11 C12 C13 142.9(2) . . . . ?
C6 C11 C12 C19 -87.2(3) . . . . ?
C7 C6 C11 C10 0.8(4) . . . . ?
C7 C6 C11 C12 178.9(2) . . . . ?
C7 C8 C9 C10 0.4(5) . . . . ?
C8 C9 C10 C11 -0.4(5) . . . . ?
C9 C10 C11 C6 -0.2(4) . . . . ?
C9 C10 C11 C12 -178.3(3) . . . . ?
C10 C11 C12 C13 -39.0(3) . . . . ?
C10 C11 C12 C19 90.8(3) . . . . ?
C11 C6 C7 C8 -0.9(4) . . . . ?
C11 C12 C13 C14 -42.7(3) . . . . ?
C11 C12 C13 C18 141.5(3) . . . . ?
C11 C12 C19 C20 -43.8(3) . . . . ?
C11 C12 C19 C24 136.6(3) . . . . ?
C12 C13 C14 C15 -176.9(3) . . . . ?
C12 C13 C18 C17 176.9(3) . . . . ?
C12 C19 C20 C21 179.5(3) . . . . ?
C12 C19 C24 C23 -179.7(4) . . . . ?
C13 C12 C19 C20 85.6(3) . . . . ?
C13 C12 C19 C24 -94.0(3) . . . . ?
C13 C14 C15 C16 0.4(6) . . . . ?
C14 C13 C18 C17 1.1(5) . . . . ?
C14 C15 C16 C17 0.2(7) . . . . ?
C15 C16 C17 C18 -0.1(7) . . . . ?
C16 C17 C18 C13 -0.6(6) . . . . ?
C18 C13 C14 C15 -1.0(5) . . . . ?
C19 C12 C13 C14 -171.2(2) . . . . ?
C19 C12 C13 C18 13.0(3) . . . . ?
C19 C20 C21 C22 0.2(5) . . . . ?
C20 C19 C24 C23 0.6(5) . . . . ?
C20 C21 C22 C23 0.6(6) . . . . ?
C21 C22 C23 C24 -0.8(7) . . . . ?
C22 C23 C24 C19 0.2(7) . . . . ?
C24 C19 C20 C21 -0.8(5) . . . . ?
C25 N2 C1 Pd1 10.3(3) . . . . ?
C25 N2 C1 N1 178.1(2) . . . . ?
C25 N2 C3 C2 -177.5(2) . . . . ?
C25 N2 C3 C5 -0.5(4) . . . . ?
C25 C26 C27 C28 0.0(5) . . . . ?
C25 C30 C31 C32 104.7(3) . . . . ?
C25 C30 C31 C38 -127.0(3) . . . . ?
C26 C25 C30 C29 0.2(4) . . . . ?
C26 C25 C30 C31 -179.7(3) . . . . ?
C26 C27 C28 C29 0.1(5) . . . . ?
C27 C28 C29 C30 -0.1(5) . . . . ?
C28 C29 C30 C25 -0.1(5) . . . . ?
C28 C29 C30 C31 179.8(3) . . . . ?
C29 C30 C31 C32 -75.2(4) . . . . ?
C29 C30 C31 C38 53.1(4) . . . . ?
C30 C25 C26 C27 -0.1(4) . . . . ?
C30 C31 C32 C33 30.4(4) . . . . ?
C30 C31 C32 C37 -152.9(3) . . . . ?
C30 C31 C38 C39 -83.4(3) . . . . ?
C30 C31 C38 C43 98.7(3) . . . . ?
C31 C32 C33 C34 176.7(3) . . . . ?
C31 C32 C37 C36 -177.8(3) . . . . ?
C31 C38 C39 C40 180.0(3) . . . . ?
C31 C38 C43 C42 -179.3(3) . . . . ?
C32 C31 C38 C39 47.1(4) . . . . ?
C32 C31 C38 C43 -130.7(3) . . . . ?
C32 C33 C34 C35 0.1(6) . . . . ?
C33 C32 C37 C36 -0.9(5) . . . . ?
C33 C34 C35 C36 0.6(6) . . . . ?
C34 C35 C36 C37 -1.5(5) . . . . ?
C35 C36 C37 C32 1.6(6) . . . . ?
C37 C32 C33 C34 0.0(5) . . . . ?
C38 C31 C32 C33 -99.2(3) . . . . ?
C38 C31 C32 C37 77.5(3) . . . . ?
C38 C39 C40 C41 -0.2(6) . . . . ?
C39 C38 C43 C42 2.7(5) . . . . ?
C39 C40 C41 C42 2.1(7) . . . . ?
C40 C41 C42 C43 -1.5(7) . . . . ?
C41 C42 C43 C38 -0.9(6) . . . . ?
C43 C38 C39 C40 -2.2(5) . . . . ?
C44 C45 C46 Pd1 52.7(3) . . . . ?
C47 Cl2 C47 Cl2 0.000(2) 2_577 . . 2_577 ?
C47 Cl3 C47 Cl3 0.001(1) 2_577 . . 2_577 ?
C47 Cl4 C47 Cl4 0.000(4) 2_577 . . 2_577 ?
C47 Cl5 C47 Cl5 0.000(3) 2_577 . . 2_577 ?
C47 Cl6 C47 Cl6 0.003(3) 2_577 . . 2_577 ?
C48 C49 C50 C48 27(5) . . . 2_567 ?
C50 C48 C49 C50 -23(4) 2_567 . . . ?
C51 C52 C53 C51 25(5) . . . 2_567 ?
C53 C51 C52 C53 -29(5) 2_567 . . . ?


_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.749
####################################################################### 
# 
# 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_lk2069
_audit_block_doi                 10.5517/ccdc.csd.cc26sbs4
_database_code_depnum_ccdc_archive 'CCDC 2049186'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/adsc.202100491 2021
loop_
_audit_author_name
_audit_author_address
'Michel Giorgi '
;Aix Marseille University
France
;
_audit_update_record             
;
2020-12-08 deposited with the CCDC.	2023-05-08 downloaded from the CCDC.
;
_audit_creation_date             2018-01-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H31 Cl N2 Pd'
_chemical_formula_sum            'C21 H31 Cl N2 Pd'
_chemical_formula_weight         453.33
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   17.2249(3)
_cell_length_b                   14.0349(3)
_cell_length_c                   18.3854(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4444.67(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    17066
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.6340
_cell_measurement_theta_min      3.9820
_shelx_estimated_absorpt_T_max   0.910
_shelx_estimated_absorpt_T_min   0.802
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.18b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47668
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.621
_diffrn_reflns_theta_min         3.241
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  83.00   1.00   13.50    --    8.41  38.00-150.00   99
  2  ω    -20.00  49.00   1.00   13.50    --    8.41 -99.00  90.00   69
  3  ω    -16.00  83.00   1.00   13.50    --    8.41  38.00 -60.00   99
  4  ω    -16.00  35.00   1.00   13.50    --    8.41  38.00  30.00   51
  5  ω    -68.00  41.00   1.00   13.50    --    8.41 -77.00-120.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0315764000
_diffrn_orient_matrix_UB_12      0.0156243000
_diffrn_orient_matrix_UB_13      -0.0216876000
_diffrn_orient_matrix_UB_21      0.0263940000
_diffrn_orient_matrix_UB_22      0.0165962000
_diffrn_orient_matrix_UB_23      -0.0267794000
_diffrn_orient_matrix_UB_31      -0.0012375000
_diffrn_orient_matrix_UB_32      -0.0451003000
_diffrn_orient_matrix_UB_33      -0.0173654000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3959
_reflns_number_total             5147
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_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         0.577
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5147
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.075
_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)+(0.0223P)²+4.2023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0737
_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. Uiso/Uaniso restraints and constraints
C19 \\sim C20: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01
C20 \\sim C21: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01
3.a Riding coordinates:
 C19(H19A,H19B), C20(H20), C21(H21A,H21B)
3.b Ternary CH refined with riding coordinates:
 C4(H4), C16(H16)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B)
3.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14)
3.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.43890(2) 0.12921(2) 0.57712(2) 0.04074(7) Uani 1 1 d . . . . .
Cl1 Cl 0.37460(4) -0.00325(5) 0.62853(5) 0.0648(2) Uani 1 1 d . . . . .
N9 N 0.27872(11) 0.20321(15) 0.53993(12) 0.0468(5) Uani 1 1 d . . . . .
N12 N 0.32842(12) 0.27387(14) 0.63338(12) 0.0460(5) Uani 1 1 d . . . . .
C1 C 0.34149(14) 0.20912(16) 0.58096(13) 0.0399(5) Uani 1 1 d . . . . .
C2 C 0.21837(16) 0.2719(2) 0.56160(16) 0.0579(7) Uani 1 1 d . . . . .
H2A H 0.167708 0.241925 0.564305 0.070 Uiso 1 1 calc R . . . .
H2B H 0.215999 0.325361 0.528244 0.070 Uiso 1 1 calc R . . . .
C3 C 0.24647(16) 0.3025(2) 0.63584(16) 0.0600(8) Uani 1 1 d . . . . .
H3A H 0.241098 0.370683 0.642586 0.072 Uiso 1 1 calc R . . . .
H3B H 0.218758 0.269525 0.674276 0.072 Uiso 1 1 calc R . . . .
C4 C 0.27189(15) 0.1433(2) 0.47513(15) 0.0513(7) Uani 1 1 d . . . . .
H4 H 0.322268 0.112542 0.467332 0.062 Uiso 1 1 calc R . . . .
C5 C 0.2122(2) 0.0654(2) 0.48553(17) 0.0698(9) Uani 1 1 d . . . . .
H5A H 0.161961 0.093885 0.495275 0.084 Uiso 1 1 calc R . . . .
H5B H 0.226431 0.026822 0.527209 0.084 Uiso 1 1 calc R . . . .
C6 C 0.2066(3) 0.0021(3) 0.4181(2) 0.0930(13) Uani 1 1 d . . . . .
H6A H 0.255171 -0.031680 0.411397 0.112 Uiso 1 1 calc R . . . .
H6B H 0.165863 -0.044730 0.425093 0.112 Uiso 1 1 calc R . . . .
C7 C 0.1894(2) 0.0595(4) 0.3517(2) 0.1000(14) Uani 1 1 d . . . . .
H7A H 0.138063 0.087299 0.355960 0.120 Uiso 1 1 calc R . . . .
H7B H 0.189643 0.018144 0.309421 0.120 Uiso 1 1 calc R . . . .
C8 C 0.2481(3) 0.1373(4) 0.34146(19) 0.1105(16) Uani 1 1 d . . . . .
H8A H 0.233774 0.175428 0.299570 0.133 Uiso 1 1 calc R . . . .
H8B H 0.298513 0.109116 0.331808 0.133 Uiso 1 1 calc R . . . .
C9 C 0.2539(2) 0.2014(3) 0.40819(16) 0.0796(10) Uani 1 1 d . . . . .
H9A H 0.294367 0.248388 0.400744 0.096 Uiso 1 1 calc R . . . .
H9B H 0.205154 0.234896 0.415022 0.096 Uiso 1 1 calc R . . . .
C10 C 0.38075(15) 0.29097(18) 0.69270(14) 0.0477(6) Uani 1 1 d . . . . .
C11 C 0.39636(19) 0.2178(2) 0.74036(17) 0.0650(8) Uani 1 1 d . . . . .
H11 H 0.372649 0.158798 0.734427 0.078 Uiso 1 1 calc R . . . .
C12 C 0.4476(2) 0.2328(3) 0.7971(2) 0.0904(13) Uani 1 1 d . . . . .
H12 H 0.458219 0.183798 0.829736 0.108 Uiso 1 1 calc R . . . .
C13 C 0.4826(2) 0.3192(3) 0.8054(2) 0.0951(13) Uani 1 1 d . . . . .
H13 H 0.517743 0.328848 0.843023 0.114 Uiso 1 1 calc R . . . .
C14 C 0.4659(2) 0.3913(3) 0.7584(2) 0.0784(10) Uani 1 1 d . . . . .
H14 H 0.489818 0.450035 0.765140 0.094 Uiso 1 1 calc R . . . .
C15 C 0.41450(18) 0.3802(2) 0.70083(16) 0.0573(7) Uani 1 1 d . . . . .
C16 C 0.3977(2) 0.4623(2) 0.64987(19) 0.0666(8) Uani 1 1 d . . . . .
H16 H 0.360866 0.439468 0.613188 0.080 Uiso 1 1 calc R . . . .
C17 C 0.3593(3) 0.5449(3) 0.6899(2) 0.0992(13) Uani 1 1 d . . . . .
H17A H 0.311432 0.523724 0.711121 0.149 Uiso 1 1 calc GR . . . .
H17B H 0.348974 0.595644 0.656174 0.149 Uiso 1 1 calc GR . . . .
H17C H 0.393332 0.567488 0.727458 0.149 Uiso 1 1 calc GR . . . .
C18 C 0.4699(3) 0.4955(3) 0.6101(3) 0.1028(14) Uani 1 1 d . . . . .
H18A H 0.509393 0.511683 0.644876 0.154 Uiso 1 1 calc GR . . . .
H18B H 0.457692 0.550478 0.581258 0.154 Uiso 1 1 calc GR . . . .
H18C H 0.488413 0.445372 0.579136 0.154 Uiso 1 1 calc GR . . . .
C19 C 0.55946(16) 0.0752(3) 0.5787(2) 0.0732(9) Uani 1 1 d . U . . .
H19A H 0.546241 0.089663 0.626490 0.088 Uiso 1 1 d R . . . .
H19B H 0.580191 0.015843 0.567430 0.088 Uiso 1 1 d R . . . .
C20 C 0.54864(18) 0.1403(3) 0.5259(2) 0.0783(9) Uani 1 1 d . U . . .
H20 H 0.562337 0.124113 0.478543 0.094 Uiso 1 1 d R . . . .
C21 C 0.51752(17) 0.2317(2) 0.5383(2) 0.0758(9) Uani 1 1 d . U . . .
H21A H 0.503372 0.249695 0.585172 0.091 Uiso 1 1 d R . . . .
H21B H 0.511212 0.274005 0.499862 0.091 Uiso 1 1 d 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 2.3614(7) . ?
Pd1 C1 2.019(2) . ?
Pd1 C19 2.211(3) . ?
Pd1 H19A 2.1332 . ?
Pd1 C20 2.118(3) . ?
Pd1 C21 2.100(3) . ?
Pd1 H21A 2.0285 . ?
N9 C1 1.321(3) . ?
N9 C2 1.473(3) . ?
N9 C4 1.463(3) . ?
N12 C1 1.344(3) . ?
N12 C3 1.468(3) . ?
N12 C10 1.435(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.510(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4 0.9800 . ?
C4 C5 1.513(4) . ?
C4 C9 1.508(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.529(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.491(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.500(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.525(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.376(4) . ?
C10 C15 1.388(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.383(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.362(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.360(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.390(4) . ?
C15 C16 1.514(4) . ?
C16 H16 0.9800 . ?
C16 C17 1.524(5) . ?
C16 C18 1.516(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9300 . ?
C19 H19B 0.9299 . ?
C19 C20 1.347(5) . ?
C20 H20 0.9301 . ?
C20 C21 1.408(5) . ?
C21 H21A 0.9300 . ?
C21 H21B 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pd1 H19A 91.8 . . ?
Cl1 Pd1 H21A 152.1 . . ?
C1 Pd1 Cl1 91.92(7) . . ?
C1 Pd1 C19 166.02(12) . . ?
C1 Pd1 H19A 148.2 . . ?
C1 Pd1 C20 135.74(13) . . ?
C1 Pd1 C21 99.63(11) . . ?
C1 Pd1 H21A 89.4 . . ?
C19 Pd1 Cl1 99.53(10) . . ?
C19 Pd1 H19A 24.6 . . ?
C19 Pd1 H21A 76.7 . . ?
H19A Pd1 H21A 73.2 . . ?
C20 Pd1 Cl1 130.91(11) . . ?
C20 Pd1 C19 36.17(13) . . ?
C20 Pd1 H19A 55.6 . . ?
C20 Pd1 H21A 58.8 . . ?
C21 Pd1 Cl1 167.81(10) . . ?
C21 Pd1 C19 68.50(13) . . ?
C21 Pd1 H19A 76.3 . . ?
C21 Pd1 C20 39.00(13) . . ?
C21 Pd1 H21A 26.0 . . ?
C1 N9 C2 112.5(2) . . ?
C1 N9 C4 124.6(2) . . ?
C4 N9 C2 122.7(2) . . ?
C1 N12 C3 111.6(2) . . ?
C1 N12 C10 123.6(2) . . ?
C10 N12 C3 122.3(2) . . ?
N9 C1 Pd1 128.70(18) . . ?
N9 C1 N12 108.4(2) . . ?
N12 C1 Pd1 122.68(17) . . ?
N9 C2 H2A 111.4 . . ?
N9 C2 H2B 111.4 . . ?
N9 C2 C3 101.8(2) . . ?
H2A C2 H2B 109.3 . . ?
C3 C2 H2A 111.4 . . ?
C3 C2 H2B 111.4 . . ?
N12 C3 C2 101.7(2) . . ?
N12 C3 H3A 111.4 . . ?
N12 C3 H3B 111.4 . . ?
C2 C3 H3A 111.4 . . ?
C2 C3 H3B 111.4 . . ?
H3A C3 H3B 109.3 . . ?
N9 C4 H4 107.5 . . ?
N9 C4 C5 111.5(2) . . ?
N9 C4 C9 111.8(2) . . ?
C5 C4 H4 107.5 . . ?
C9 C4 H4 107.5 . . ?
C9 C4 C5 110.7(2) . . ?
C4 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
C4 C5 C6 111.1(3) . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C7 C6 C5 111.3(3) . . ?
C7 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
C6 C7 C8 111.2(3) . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
C7 C8 C9 111.8(3) . . ?
H8A C8 H8B 107.9 . . ?
C9 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
C4 C9 C8 110.6(3) . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 N12 118.8(2) . . ?
C11 C10 C15 121.5(3) . . ?
C15 C10 N12 119.7(2) . . ?
C10 C11 H11 120.3 . . ?
C10 C11 C12 119.5(3) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.1(3) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 118.8 . . ?
C13 C14 C15 122.3(3) . . ?
C15 C14 H14 118.8 . . ?
C10 C15 C14 116.8(3) . . ?
C10 C15 C16 122.7(3) . . ?
C14 C15 C16 120.5(3) . . ?
C15 C16 H16 107.5 . . ?
C15 C16 C17 111.4(3) . . ?
C15 C16 C18 112.0(3) . . ?
C17 C16 H16 107.5 . . ?
C18 C16 H16 107.5 . . ?
C18 C16 C17 110.8(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Pd1 C19 H19A 73.0 . . ?
Pd1 C19 H19B 131.7 . . ?
H19A C19 H19B 120.0 . . ?
C20 C19 Pd1 68.15(18) . . ?
C20 C19 H19A 120.0 . . ?
C20 C19 H19B 120.0 . . ?
Pd1 C20 H20 128.7 . . ?
C19 C20 Pd1 75.68(19) . . ?
C19 C20 H20 118.3 . . ?
C19 C20 C21 123.6(4) . . ?
C21 C20 Pd1 69.83(17) . . ?
C21 C20 H20 118.1 . . ?
Pd1 C21 H21A 72.7 . . ?
Pd1 C21 H21B 128.3 . . ?
C20 C21 Pd1 71.17(18) . . ?
C20 C21 H21A 119.8 . . ?
C20 C21 H21B 120.2 . . ?
H21A C21 H21B 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 C19 C20 C21 53.4(3) . . . . ?
N9 C2 C3 N12 18.8(3) . . . . ?
N9 C4 C5 C6 -178.9(3) . . . . ?
N9 C4 C9 C8 179.3(3) . . . . ?
N12 C10 C11 C12 179.0(3) . . . . ?
N12 C10 C15 C14 -178.6(3) . . . . ?
N12 C10 C15 C16 0.9(4) . . . . ?
C1 N9 C2 C3 -14.9(3) . . . . ?
C1 N9 C4 C5 114.8(3) . . . . ?
C1 N9 C4 C9 -120.7(3) . . . . ?
C1 N12 C3 C2 -19.0(3) . . . . ?
C1 N12 C10 C11 -61.6(4) . . . . ?
C1 N12 C10 C15 118.3(3) . . . . ?
C2 N9 C1 Pd1 177.61(19) . . . . ?
C2 N9 C1 N12 3.5(3) . . . . ?
C2 N9 C4 C5 -72.3(3) . . . . ?
C2 N9 C4 C9 52.3(4) . . . . ?
C3 N12 C1 Pd1 -164.2(2) . . . . ?
C3 N12 C1 N9 10.4(3) . . . . ?
C3 N12 C10 C11 98.9(3) . . . . ?
C3 N12 C10 C15 -81.2(4) . . . . ?
C4 N9 C1 Pd1 -8.8(4) . . . . ?
C4 N9 C1 N12 177.1(2) . . . . ?
C4 N9 C2 C3 171.4(2) . . . . ?
C4 C5 C6 C7 -55.7(4) . . . . ?
C5 C4 C9 C8 -55.7(4) . . . . ?
C5 C6 C7 C8 55.2(5) . . . . ?
C6 C7 C8 C9 -55.7(5) . . . . ?
C7 C8 C9 C4 55.9(5) . . . . ?
C9 C4 C5 C6 55.9(4) . . . . ?
C10 N12 C1 Pd1 -1.8(3) . . . . ?
C10 N12 C1 N9 172.7(2) . . . . ?
C10 N12 C3 C2 178.4(2) . . . . ?
C10 C11 C12 C13 -0.4(6) . . . . ?
C10 C15 C16 C17 117.3(3) . . . . ?
C10 C15 C16 C18 -118.0(4) . . . . ?
C11 C10 C15 C14 1.3(5) . . . . ?
C11 C10 C15 C16 -179.2(3) . . . . ?
C11 C12 C13 C14 1.2(7) . . . . ?
C12 C13 C14 C15 -0.8(7) . . . . ?
C13 C14 C15 C10 -0.5(6) . . . . ?
C13 C14 C15 C16 -180.0(4) . . . . ?
C14 C15 C16 C17 -63.2(4) . . . . ?
C14 C15 C16 C18 61.5(4) . . . . ?
C15 C10 C11 C12 -0.9(5) . . . . ?
C19 C20 C21 Pd1 -55.9(3) . . . . ?


_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.865
