#------------------------------------------------------------------------------
#$Date: 2024-10-30 20:34:16 +0200 (Wed, 30 Oct 2024) $
#$Revision: 295677 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/30/7063055.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7063055
loop_
_publ_author_name
'Sinha, Nitish Kumar'
'Khan, Hilal Ahmad'
'Sivasankar, Chinnappan'
'Thirupathi, Natesan'
_publ_section_title
;
 Guanidine-centred reactivity of CNN Pd(ii) pincer complexes including
 carboxylate-assisted N--H activation and --CH2-- → --C(O)--
 oxygenation
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5710
_journal_page_last               5720
_journal_paper_doi               10.1039/D3NJ05516G
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C23 H18 F6 N4 O2 Pd'
_chemical_formula_sum            'C23 H18 F6 N4 O2 Pd'
_chemical_formula_weight         602.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-09-24 deposited with the CCDC.	2024-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.317(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2253(3)
_cell_length_b                   19.3693(3)
_cell_length_c                   17.4110(3)
_cell_measurement_reflns_used    6644
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5360
_cell_measurement_theta_min      3.5370
_cell_volume                     4789.29(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'four-circle diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67124
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.332
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         9772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0492
_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)+(0.0377P)²+5.6529P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6788
_reflns_number_total             9772
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj05516g3.cif
_cod_data_source_block           Complex-7
_cod_depositor_comments
;
Adding full bibliography for 7063048--7063056.cif.

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C46 H36 F12 N8 O4 Pd2'
_cod_original_formula_weight         1205.63
_cod_original_formula_moiety         '2(C23 H18 F6 N4 O2 Pd)'
_cod_original_formula_units_Z            4
_cod_database_code               7063055
_shelx_shelxl_version_number     2016/4
_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.
;
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C39(H39A,H39B)
1.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), N5(H5A), N6(H6A), C27(H27),
 C28(H28), C29(H29), C33(H33), C34(H34), C35(H35), C36(H36), C41(H41), C42(H42),
  C43(H43), C44(H44)
1.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C46(H46A,H46B,H46C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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'
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 0.81041(2) 0.40497(2) 0.57503(2) 0.05481(12) Uani 1 1 d . . . . .
F1 F 1.1816(2) 0.3870(2) 0.8705(2) 0.1318(16) Uani 1 1 d . . . . .
F2 F 1.1321(2) 0.4792(2) 0.8169(2) 0.1041(11) Uani 1 1 d . . . . .
F3 F 1.0838(2) 0.38328(18) 0.77468(18) 0.0940(10) Uani 1 1 d . . . . .
F4 F 0.8361(3) 0.27208(18) 0.8754(2) 0.1047(11) Uani 1 1 d . . . . .
F5 F 0.8766(3) 0.16919(17) 0.8476(2) 0.1164(13) Uani 1 1 d . . . . .
F6 F 0.9706(3) 0.25350(18) 0.8326(2) 0.1039(12) Uani 1 1 d . . . . .
O1 O 0.7423(3) 0.3653(2) 0.47862(19) 0.0842(12) Uani 1 1 d . . . . .
O2 O 0.6004(2) 0.40339(18) 0.50118(19) 0.0686(9) Uani 1 1 d . . . . .
N1 N 0.8617(3) 0.36673(19) 0.7542(2) 0.0547(9) Uani 1 1 d . . . . .
H1 H 0.861443 0.359963 0.803027 0.066 Uiso 1 1 calc R U . . .
N2 N 0.9223(2) 0.47261(17) 0.79114(18) 0.0487(9) Uani 1 1 d . . . . .
H2 H 0.935028 0.514889 0.780774 0.058 Uiso 1 1 calc R U . . .
N3 N 0.8784(2) 0.45198(18) 0.66254(18) 0.0445(8) Uani 1 1 d . . . . .
N4 N 0.8442(3) 0.4966(2) 0.5199(2) 0.0625(11) Uani 1 1 d . . . . .
C1 C 0.8862(3) 0.4314(2) 0.7333(2) 0.0450(10) Uani 1 1 d . . . . .
C2 C 0.8365(3) 0.3091(2) 0.7086(3) 0.0542(11) Uani 1 1 d . . . . .
C3 C 0.8073(3) 0.3162(2) 0.6309(3) 0.0570(12) Uani 1 1 d . . . . .
C4 C 0.7827(4) 0.2555(3) 0.5910(4) 0.0828(17) Uani 1 1 d . . . . .
H4 H 0.765043 0.257818 0.538762 0.099 Uiso 1 1 calc R U . . .
C5 C 0.7841(5) 0.1922(3) 0.6277(5) 0.100(2) Uani 1 1 d . . . . .
H5 H 0.763960 0.153048 0.600490 0.120 Uiso 1 1 calc R U . . .
C6 C 0.8139(4) 0.1864(3) 0.7015(4) 0.0907(19) Uani 1 1 d . . . . .
H6 H 0.815772 0.143258 0.724939 0.109 Uiso 1 1 calc R U . . .
C7 C 0.8418(3) 0.2441(3) 0.7433(3) 0.0669(14) Uani 1 1 d . . . . .
C8 C 0.8796(5) 0.2346(3) 0.8232(4) 0.0818(17) Uani 1 1 d . . . . .
C9 C 0.9400(3) 0.4489(2) 0.8679(2) 0.0459(10) Uani 1 1 d . . . . .
C10 C 0.8719(3) 0.4559(3) 0.9196(3) 0.0597(12) Uani 1 1 d . . . . .
H10 H 0.814032 0.475184 0.903982 0.072 Uiso 1 1 calc R U . . .
C11 C 0.8882(4) 0.4345(3) 0.9946(3) 0.0689(14) Uani 1 1 d . . . . .
H11 H 0.841138 0.439459 1.029146 0.083 Uiso 1 1 calc R U . . .
C12 C 0.9722(4) 0.4063(3) 1.0188(3) 0.0692(14) Uani 1 1 d . . . . .
H12 H 0.982777 0.391689 1.069478 0.083 Uiso 1 1 calc R U . . .
C13 C 1.0409(4) 0.3997(3) 0.9676(3) 0.0655(14) Uani 1 1 d . . . . .
H13 H 1.098455 0.380417 0.983881 0.079 Uiso 1 1 calc R U . . .
C14 C 1.0265(3) 0.4212(2) 0.8922(2) 0.0517(11) Uani 1 1 d . . . . .
C15 C 1.1056(4) 0.4180(3) 0.8390(3) 0.0742(15) Uani 1 1 d . . . . .
C16 C 0.9136(3) 0.5209(2) 0.6466(2) 0.0503(11) Uani 1 1 d . . . . .
H16A H 0.979801 0.523587 0.663104 0.060 Uiso 1 1 calc R U . . .
H16B H 0.879925 0.554624 0.675617 0.060 Uiso 1 1 calc R U . . .
C17 C 0.9015(3) 0.5377(3) 0.5620(3) 0.0572(12) Uani 1 1 d . . . . .
C18 C 0.9484(4) 0.5925(3) 0.5313(3) 0.0718(15) Uani 1 1 d . . . . .
H18 H 0.988555 0.619890 0.562370 0.086 Uiso 1 1 calc R U . . .
C19 C 0.9349(5) 0.6058(3) 0.4540(4) 0.0874(19) Uani 1 1 d . . . . .
H19 H 0.966522 0.642019 0.431760 0.105 Uiso 1 1 calc R U . . .
C20 C 0.8746(5) 0.5653(4) 0.4104(3) 0.092(2) Uani 1 1 d . . . . .
H20 H 0.862945 0.574754 0.358326 0.110 Uiso 1 1 calc R U . . .
C21 C 0.8312(4) 0.5107(3) 0.4434(3) 0.0797(17) Uani 1 1 d . . . . .
H21 H 0.791718 0.482367 0.412788 0.096 Uiso 1 1 calc R U . . .
C22 C 0.6556(4) 0.3726(3) 0.4626(3) 0.0597(12) Uani 1 1 d . . . . .
C23 C 0.6192(4) 0.3409(3) 0.3869(3) 0.100(2) Uani 1 1 d . . . . .
H23A H 0.651176 0.361318 0.345449 0.150 Uiso 1 1 calc R U . . .
H23B H 0.552774 0.349307 0.379351 0.150 Uiso 1 1 calc R U . . .
H23C H 0.630587 0.292070 0.387953 0.150 Uiso 1 1 calc R U . . .
Pd2 Pd 0.71115(2) 0.60000(2) 0.73874(2) 0.04773(11) Uani 1 1 d . . . . .
F7 F 0.5803(3) 0.3720(2) 0.9948(2) 0.1229(14) Uani 1 1 d . . . . .
F8 F 0.5045(3) 0.3790(2) 0.8883(2) 0.1185(14) Uani 1 1 d . . . . .
F9 F 0.6443(3) 0.34627(19) 0.8908(3) 0.1312(15) Uani 1 1 d . . . . .
F10 F 0.2970(3) 0.4325(4) 0.7329(3) 0.192(2) Uani 1 1 d . . . . .
F11 F 0.4264(3) 0.4825(3) 0.7606(3) 0.1453(18) Uani 1 1 d . . . . .
F12 F 0.3759(3) 0.4701(3) 0.6466(3) 0.1555(19) Uani 1 1 d . . . . .
O3 O 0.7867(2) 0.67784(15) 0.7915(2) 0.0673(9) Uani 1 1 d . . . . .
O4 O 0.9178(2) 0.61751(17) 0.8038(2) 0.0681(9) Uani 1 1 d . . . . .
N5 N 0.6248(2) 0.45057(18) 0.7762(2) 0.0509(9) Uani 1 1 d . . . . .
H5A H 0.623650 0.406758 0.784138 0.061 Uiso 1 1 calc R U . . .
N6 N 0.5690(2) 0.42365(18) 0.6538(2) 0.0513(9) Uani 1 1 d . . . . .
H6A H 0.571643 0.429867 0.605099 0.062 Uiso 1 1 calc R U . . .
N7 N 0.6382(2) 0.53085(17) 0.6783(2) 0.0463(8) Uani 1 1 d . . . . .
N8 N 0.7197(3) 0.64504(18) 0.6296(2) 0.0533(9) Uani 1 1 d . . . . .
C24 C 0.6114(3) 0.4707(2) 0.7016(3) 0.0470(10) Uani 1 1 d . . . . .
C25 C 0.6402(3) 0.4919(2) 0.8423(3) 0.0529(11) Uani 1 1 d . . . . .
C26 C 0.6773(3) 0.5585(2) 0.8369(3) 0.0521(11) Uani 1 1 d . . . . .
C27 C 0.6854(4) 0.5972(3) 0.9045(3) 0.0660(13) Uani 1 1 d . . . . .
H27 H 0.707311 0.642300 0.902195 0.079 Uiso 1 1 calc R U . . .
C28 C 0.6622(4) 0.5710(3) 0.9745(3) 0.0773(16) Uani 1 1 d . . . . .
H28 H 0.667711 0.598622 1.018179 0.093 Uiso 1 1 calc R U . . .
C29 C 0.6312(4) 0.5047(3) 0.9797(3) 0.0784(16) Uani 1 1 d . . . . .
H29 H 0.617597 0.486600 1.027224 0.094 Uiso 1 1 calc R U . . .
C30 C 0.6200(3) 0.4645(3) 0.9143(3) 0.0611(13) Uani 1 1 d . . . . .
C31 C 0.5889(5) 0.3918(4) 0.9229(4) 0.0848(17) Uani 1 1 d . . . . .
C32 C 0.5206(3) 0.3649(3) 0.6789(3) 0.0592(12) Uani 1 1 d . . . . .
C33 C 0.5608(4) 0.3013(3) 0.6711(4) 0.0857(18) Uani 1 1 d . . . . .
H33 H 0.619046 0.297633 0.649854 0.103 Uiso 1 1 calc R U . . .
C34 C 0.5155(7) 0.2424(4) 0.6947(5) 0.128(3) Uani 1 1 d . . . . .
H34 H 0.543119 0.199299 0.689564 0.154 Uiso 1 1 calc R U . . .
C35 C 0.4299(8) 0.2483(5) 0.7254(5) 0.143(5) Uani 1 1 d . . . . .
H35 H 0.399078 0.208849 0.741183 0.172 Uiso 1 1 calc R U . . .
C36 C 0.3894(5) 0.3106(5) 0.7332(4) 0.120(3) Uani 1 1 d . . . . .
H36 H 0.331465 0.313743 0.755108 0.144 Uiso 1 1 calc R U . . .
C37 C 0.4333(4) 0.3702(3) 0.7090(3) 0.0766(16) Uani 1 1 d . . . . .
C38 C 0.3850(4) 0.4374(5) 0.7157(5) 0.110(3) Uani 1 1 d . . . . .
C39 C 0.6176(3) 0.5488(2) 0.5969(2) 0.0537(11) Uani 1 1 d . . . . .
H39A H 0.549994 0.551805 0.586699 0.064 Uiso 1 1 calc R U . . .
H39B H 0.641008 0.512504 0.564680 0.064 Uiso 1 1 calc R U . . .
C40 C 0.6612(3) 0.6153(2) 0.5763(3) 0.0551(12) Uani 1 1 d . . . . .
C41 C 0.6442(4) 0.6440(3) 0.5048(3) 0.0839(17) Uani 1 1 d . . . . .
H41 H 0.602702 0.622975 0.468746 0.101 Uiso 1 1 calc R U . . .
C42 C 0.6890(5) 0.7035(3) 0.4873(4) 0.105(2) Uani 1 1 d . . . . .
H42 H 0.678182 0.723371 0.439006 0.126 Uiso 1 1 calc R U . . .
C43 C 0.7496(5) 0.7342(3) 0.5401(4) 0.094(2) Uani 1 1 d . . . . .
H43 H 0.781048 0.774601 0.528363 0.113 Uiso 1 1 calc R U . . .
C44 C 0.7631(4) 0.7042(2) 0.6107(3) 0.0699(14) Uani 1 1 d . . . . .
H44 H 0.803657 0.725371 0.647376 0.084 Uiso 1 1 calc R U . . .
C45 C 0.8723(4) 0.6693(2) 0.8115(3) 0.0531(11) Uani 1 1 d . . . . .
C46 C 0.9194(4) 0.7329(2) 0.8481(3) 0.0744(15) Uani 1 1 d . . . . .
H46A H 0.899522 0.773297 0.819713 0.112 Uiso 1 1 calc R U . . .
H46B H 0.986561 0.728276 0.847456 0.112 Uiso 1 1 calc R U . . .
H46C H 0.901860 0.737126 0.900348 0.112 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1 Pd1 N4 93.08(17) . . ?
N3 Pd1 O1 174.28(16) . . ?
N3 Pd1 N4 81.21(15) . . ?
C3 Pd1 O1 93.08(18) . . ?
C3 Pd1 N3 92.59(16) . . ?
C3 Pd1 N4 168.00(16) . . ?
C22 O1 Pd1 123.6(3) . . ?
C1 N1 H1 115.0 . . ?
C1 N1 C2 130.1(4) . . ?
C2 N1 H1 115.0 . . ?
C1 N2 H2 118.5 . . ?
C1 N2 C9 122.9(4) . . ?
C9 N2 H2 118.5 . . ?
C1 N3 Pd1 127.1(3) . . ?
C1 N3 C16 116.9(3) . . ?
C16 N3 Pd1 115.6(3) . . ?
C17 N4 Pd1 114.0(3) . . ?
C17 N4 C21 117.6(5) . . ?
C21 N4 Pd1 126.7(4) . . ?
N1 C1 N2 115.8(4) . . ?
N3 C1 N1 122.1(4) . . ?
N3 C1 N2 122.1(4) . . ?
C3 C2 N1 121.4(4) . . ?
C7 C2 N1 117.8(4) . . ?
C7 C2 C3 120.8(4) . . ?
C2 C3 Pd1 123.2(3) . . ?
C2 C3 C4 116.7(5) . . ?
C4 C3 Pd1 119.9(4) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 C3 121.3(6) . . ?
C5 C4 H4 119.4 . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.0(6) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.4(6) . . ?
C7 C6 H6 119.8 . . ?
C2 C7 C8 121.9(5) . . ?
C6 C7 C2 119.7(5) . . ?
C6 C7 C8 118.4(5) . . ?
F4 C8 F6 104.4(5) . . ?
F4 C8 C7 114.5(5) . . ?
F5 C8 F4 105.8(5) . . ?
F5 C8 F6 105.5(5) . . ?
F5 C8 C7 113.7(5) . . ?
F6 C8 C7 112.2(5) . . ?
C10 C9 N2 119.6(4) . . ?
C10 C9 C14 119.2(4) . . ?
C14 C9 N2 121.2(4) . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.5(4) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.8(5) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 H12 120.5 . . ?
C11 C12 C13 119.0(5) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 H13 119.3 . . ?
C12 C13 C14 121.4(4) . . ?
C14 C13 H13 119.3 . . ?
C9 C14 C15 120.7(4) . . ?
C13 C14 C9 119.1(4) . . ?
C13 C14 C15 120.1(4) . . ?
F1 C15 C14 112.6(5) . . ?
F2 C15 F1 106.8(5) . . ?
F2 C15 F3 105.6(5) . . ?
F2 C15 C14 112.6(5) . . ?
F3 C15 F1 105.3(5) . . ?
F3 C15 C14 113.3(5) . . ?
N3 C16 H16A 109.4 . . ?
N3 C16 H16B 109.4 . . ?
N3 C16 C17 111.3(4) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
N4 C17 C16 116.1(4) . . ?
N4 C17 C18 122.9(5) . . ?
C18 C17 C16 121.0(5) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 C17 118.8(6) . . ?
C19 C18 H18 120.6 . . ?
C18 C19 H19 120.4 . . ?
C20 C19 C18 119.1(6) . . ?
C20 C19 H19 120.4 . . ?
C19 C20 H20 120.1 . . ?
C19 C20 C21 119.7(5) . . ?
C21 C20 H20 120.1 . . ?
N4 C21 C20 121.8(6) . . ?
N4 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
O1 C22 C23 115.3(5) . . ?
O2 C22 O1 126.0(4) . . ?
O2 C22 C23 118.6(5) . . ?
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 . . ?
O3 Pd2 N8 92.51(14) . . ?
N7 Pd2 O3 174.11(15) . . ?
N7 Pd2 N8 81.66(14) . . ?
N7 Pd2 C26 92.19(16) . . ?
C26 Pd2 O3 93.42(16) . . ?
C26 Pd2 N8 169.20(15) . . ?
C45 O3 Pd2 120.2(3) . . ?
C24 N5 H5A 115.7 . . ?
C24 N5 C25 128.6(4) . . ?
C25 N5 H5A 115.7 . . ?
C24 N6 H6A 117.9 . . ?
C24 N6 C32 124.1(4) . . ?
C32 N6 H6A 117.9 . . ?
C24 N7 Pd2 126.9(3) . . ?
C24 N7 C39 117.9(3) . . ?
C39 N7 Pd2 115.1(3) . . ?
C40 N8 Pd2 112.5(3) . . ?
C40 N8 C44 118.0(4) . . ?
C44 N8 Pd2 128.6(3) . . ?
N6 C24 N5 115.2(4) . . ?
N7 C24 N5 121.9(4) . . ?
N7 C24 N6 122.8(4) . . ?
C26 C25 N5 120.7(4) . . ?
C26 C25 C30 120.4(4) . . ?
C30 C25 N5 118.9(4) . . ?
C25 C26 Pd2 123.1(3) . . ?
C27 C26 Pd2 120.0(4) . . ?
C27 C26 C25 116.9(5) . . ?
C26 C27 H27 118.8 . . ?
C28 C27 C26 122.5(5) . . ?
C28 C27 H27 118.8 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 C27 120.0(5) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 120.0(5) . . ?
C30 C29 H29 120.0 . . ?
C25 C30 C31 121.7(5) . . ?
C29 C30 C25 120.1(5) . . ?
C29 C30 C31 118.2(5) . . ?
F7 C31 F8 104.0(5) . . ?
F7 C31 F9 107.2(6) . . ?
F7 C31 C30 114.5(5) . . ?
F8 C31 C30 113.3(5) . . ?
F9 C31 F8 103.1(6) . . ?
F9 C31 C30 113.6(5) . . ?
C33 C32 N6 118.7(5) . . ?
C33 C32 C37 119.7(5) . . ?
C37 C32 N6 121.6(5) . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.5(7) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 H34 120.3 . . ?
C35 C34 C33 119.3(8) . . ?
C35 C34 H34 120.3 . . ?
C34 C35 H35 119.6 . . ?
C36 C35 C34 120.7(8) . . ?
C36 C35 H35 119.6 . . ?
C35 C36 H36 119.6 . . ?
C35 C36 C37 120.8(8) . . ?
C37 C36 H36 119.6 . . ?
C32 C37 C36 119.0(7) . . ?
C32 C37 C38 121.8(6) . . ?
C36 C37 C38 119.3(7) . . ?
F10 C38 F12 101.1(6) . . ?
F10 C38 C37 114.1(8) . . ?
F11 C38 F10 108.7(7) . . ?
F11 C38 F12 103.7(8) . . ?
F11 C38 C37 116.4(6) . . ?
F12 C38 C37 111.2(6) . . ?
N7 C39 H39A 109.2 . . ?
N7 C39 H39B 109.2 . . ?
N7 C39 C40 112.0(4) . . ?
H39A C39 H39B 107.9 . . ?
C40 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
N8 C40 C39 117.2(4) . . ?
N8 C40 C41 121.7(5) . . ?
C41 C40 C39 121.1(4) . . ?
C40 C41 H41 120.5 . . ?
C42 C41 C40 119.0(5) . . ?
C42 C41 H41 120.5 . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.4(6) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 120.8 . . ?
C42 C43 C44 118.3(5) . . ?
C44 C43 H43 120.8 . . ?
N8 C44 C43 122.6(5) . . ?
N8 C44 H44 118.7 . . ?
C43 C44 H44 118.7 . . ?
O3 C45 C46 113.8(4) . . ?
O4 C45 O3 126.6(4) . . ?
O4 C45 C46 119.5(4) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
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 O1 2.040(3) . ?
Pd1 N3 1.979(3) . ?
Pd1 N4 2.087(4) . ?
Pd1 C3 1.978(5) . ?
F1 C15 1.329(6) . ?
F2 C15 1.308(6) . ?
F3 C15 1.327(6) . ?
F4 C8 1.342(7) . ?
F5 C8 1.338(6) . ?
F6 C8 1.347(7) . ?
O1 C22 1.257(6) . ?
O2 C22 1.217(6) . ?
N1 H1 0.8600 . ?
N1 C1 1.356(5) . ?
N1 C2 1.404(5) . ?
N2 H2 0.8600 . ?
N2 C1 1.362(5) . ?
N2 C9 1.422(5) . ?
N3 C1 1.293(5) . ?
N3 C16 1.458(5) . ?
N4 C17 1.329(6) . ?
N4 C21 1.362(6) . ?
C2 C3 1.400(6) . ?
C2 C7 1.397(7) . ?
C3 C4 1.400(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.382(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.336(8) . ?
C6 H6 0.9300 . ?
C6 C7 1.379(7) . ?
C7 C8 1.472(8) . ?
C9 C10 1.367(6) . ?
C9 C14 1.386(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.377(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.359(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.366(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.381(6) . ?
C14 C15 1.500(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.509(6) . ?
C17 C18 1.377(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.373(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.361(9) . ?
C20 H20 0.9300 . ?
C20 C21 1.369(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.518(6) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
Pd2 O3 2.039(3) . ?
Pd2 N7 1.963(3) . ?
Pd2 N8 2.100(4) . ?
Pd2 C26 1.974(5) . ?
F7 C31 1.321(6) . ?
F8 C31 1.336(7) . ?
F9 C31 1.328(7) . ?
F10 C38 1.307(7) . ?
F11 C38 1.292(8) . ?
F12 C38 1.359(8) . ?
O3 C45 1.258(5) . ?
O4 C45 1.205(5) . ?
N5 H5A 0.8600 . ?
N5 C24 1.360(5) . ?
N5 C25 1.409(5) . ?
N6 H6A 0.8600 . ?
N6 C24 1.352(5) . ?
N6 C32 1.412(5) . ?
N7 C24 1.297(5) . ?
N7 C39 1.473(5) . ?
N8 C40 1.340(5) . ?
N8 C44 1.352(6) . ?
C25 C26 1.398(6) . ?
C25 C30 1.406(6) . ?
C26 C27 1.393(6) . ?
C27 H27 0.9300 . ?
C27 C28 1.377(7) . ?
C28 H28 0.9300 . ?
C28 C29 1.362(8) . ?
C29 H29 0.9300 . ?
C29 C30 1.382(7) . ?
C30 C31 1.485(8) . ?
C32 C33 1.368(7) . ?
C32 C37 1.379(7) . ?
C33 H33 0.9300 . ?
C33 C34 1.384(9) . ?
C34 H34 0.9300 . ?
C34 C35 1.362(12) . ?
C35 H35 0.9300 . ?
C35 C36 1.347(12) . ?
C36 H36 0.9300 . ?
C36 C37 1.389(9) . ?
C37 C38 1.480(10) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.482(6) . ?
C40 C41 1.372(7) . ?
C41 H41 0.9300 . ?
C41 C42 1.361(8) . ?
C42 H42 0.9300 . ?
C42 C43 1.360(8) . ?
C43 H43 0.9300 . ?
C43 C44 1.363(7) . ?
C44 H44 0.9300 . ?
C45 C46 1.525(6) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
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 O1 C22 O2 -0.4(8) . . . . ?
Pd1 O1 C22 C23 178.2(4) . . . . ?
Pd1 N3 C1 N1 12.2(6) . . . . ?
Pd1 N3 C1 N2 -169.8(3) . . . . ?
Pd1 N3 C16 C17 -7.8(4) . . . . ?
Pd1 N4 C17 C16 -14.3(5) . . . . ?
Pd1 N4 C17 C18 165.3(4) . . . . ?
Pd1 N4 C21 C20 -164.7(4) . . . . ?
Pd1 C3 C4 C5 177.0(5) . . . . ?
N1 C2 C3 Pd1 6.4(6) . . . . ?
N1 C2 C3 C4 -179.2(4) . . . . ?
N1 C2 C7 C6 177.2(5) . . . . ?
N1 C2 C7 C8 -4.9(7) . . . . ?
N2 C9 C10 C11 -178.7(4) . . . . ?
N2 C9 C14 C13 179.1(4) . . . . ?
N2 C9 C14 C15 2.4(7) . . . . ?
N3 C16 C17 N4 14.6(5) . . . . ?
N3 C16 C17 C18 -165.0(4) . . . . ?
N4 C17 C18 C19 0.6(7) . . . . ?
C1 N1 C2 C3 -18.8(7) . . . . ?
C1 N1 C2 C7 161.1(4) . . . . ?
C1 N2 C9 C10 -92.0(5) . . . . ?
C1 N2 C9 C14 90.7(5) . . . . ?
C1 N3 C16 C17 179.0(4) . . . . ?
C2 N1 C1 N2 -169.2(4) . . . . ?
C2 N1 C1 N3 8.9(7) . . . . ?
C2 C3 C4 C5 2.3(8) . . . . ?
C2 C7 C8 F4 56.2(7) . . . . ?
C2 C7 C8 F5 178.0(5) . . . . ?
C2 C7 C8 F6 -62.4(7) . . . . ?
C3 C2 C7 C6 -3.0(7) . . . . ?
C3 C2 C7 C8 175.0(5) . . . . ?
C3 C4 C5 C6 -3.7(10) . . . . ?
C4 C5 C6 C7 1.6(10) . . . . ?
C5 C6 C7 C2 1.7(9) . . . . ?
C5 C6 C7 C8 -176.3(6) . . . . ?
C6 C7 C8 F4 -125.8(6) . . . . ?
C6 C7 C8 F5 -4.0(8) . . . . ?
C6 C7 C8 F6 115.5(6) . . . . ?
C7 C2 C3 Pd1 -173.5(3) . . . . ?
C7 C2 C3 C4 0.9(7) . . . . ?
C9 N2 C1 N1 4.4(6) . . . . ?
C9 N2 C1 N3 -173.8(4) . . . . ?
C9 C10 C11 C12 0.2(8) . . . . ?
C9 C14 C15 F1 -176.9(5) . . . . ?
C9 C14 C15 F2 62.3(7) . . . . ?
C9 C14 C15 F3 -57.5(7) . . . . ?
C10 C9 C14 C13 1.7(7) . . . . ?
C10 C9 C14 C15 -175.0(5) . . . . ?
C10 C11 C12 C13 0.4(8) . . . . ?
C11 C12 C13 C14 0.1(8) . . . . ?
C12 C13 C14 C9 -1.1(8) . . . . ?
C12 C13 C14 C15 175.6(5) . . . . ?
C13 C14 C15 F1 6.4(8) . . . . ?
C13 C14 C15 F2 -114.4(5) . . . . ?
C13 C14 C15 F3 125.8(5) . . . . ?
C14 C9 C10 C11 -1.2(7) . . . . ?
C16 N3 C1 N1 -175.6(4) . . . . ?
C16 N3 C1 N2 2.4(6) . . . . ?
C16 C17 C18 C19 -179.8(4) . . . . ?
C17 N4 C21 C20 -0.5(7) . . . . ?
C17 C18 C19 C20 1.0(8) . . . . ?
C18 C19 C20 C21 -2.3(9) . . . . ?
C19 C20 C21 N4 2.2(9) . . . . ?
C21 N4 C17 C16 179.5(4) . . . . ?
C21 N4 C17 C18 -0.8(7) . . . . ?
Pd2 O3 C45 O4 -1.0(7) . . . . ?
Pd2 O3 C45 C46 178.4(3) . . . . ?
Pd2 N7 C24 N5 6.1(6) . . . . ?
Pd2 N7 C24 N6 -173.5(3) . . . . ?
Pd2 N7 C39 C40 2.8(5) . . . . ?
Pd2 N8 C40 C39 -12.9(5) . . . . ?
Pd2 N8 C40 C41 169.0(4) . . . . ?
Pd2 N8 C44 C43 -168.0(5) . . . . ?
Pd2 C26 C27 C28 179.6(4) . . . . ?
N5 C25 C26 Pd2 -0.2(6) . . . . ?
N5 C25 C26 C27 176.6(4) . . . . ?
N5 C25 C30 C29 -177.6(4) . . . . ?
N5 C25 C30 C31 4.1(7) . . . . ?
N6 C32 C33 C34 -179.7(6) . . . . ?
N6 C32 C37 C36 -179.6(5) . . . . ?
N6 C32 C37 C38 0.9(8) . . . . ?
N7 C39 C40 N8 7.1(6) . . . . ?
N7 C39 C40 C41 -174.7(5) . . . . ?
N8 C40 C41 C42 0.9(9) . . . . ?
C24 N5 C25 C26 -23.6(6) . . . . ?
C24 N5 C25 C30 158.0(4) . . . . ?
C24 N6 C32 C33 -108.0(6) . . . . ?
C24 N6 C32 C37 73.7(6) . . . . ?
C24 N7 C39 C40 -173.7(4) . . . . ?
C25 N5 C24 N6 -159.6(4) . . . . ?
C25 N5 C24 N7 20.9(7) . . . . ?
C25 C26 C27 C28 2.7(7) . . . . ?
C25 C30 C31 F7 174.6(5) . . . . ?
C25 C30 C31 F8 -66.2(7) . . . . ?
C25 C30 C31 F9 50.9(8) . . . . ?
C26 C25 C30 C29 4.0(7) . . . . ?
C26 C25 C30 C31 -174.3(5) . . . . ?
C26 C27 C28 C29 0.9(8) . . . . ?
C27 C28 C29 C30 -2.2(8) . . . . ?
C28 C29 C30 C25 -0.3(8) . . . . ?
C28 C29 C30 C31 178.1(5) . . . . ?
C29 C30 C31 F7 -3.7(8) . . . . ?
C29 C30 C31 F8 115.4(6) . . . . ?
C29 C30 C31 F9 -127.4(6) . . . . ?
C30 C25 C26 Pd2 178.1(3) . . . . ?
C30 C25 C26 C27 -5.1(6) . . . . ?
C32 N6 C24 N5 15.1(6) . . . . ?
C32 N6 C24 N7 -165.3(4) . . . . ?
C32 C33 C34 C35 0.3(11) . . . . ?
C32 C37 C38 F10 168.9(6) . . . . ?
C32 C37 C38 F11 -63.1(9) . . . . ?
C32 C37 C38 F12 55.3(8) . . . . ?
C33 C32 C37 C36 2.1(8) . . . . ?
C33 C32 C37 C38 -177.4(6) . . . . ?
C33 C34 C35 C36 -0.2(14) . . . . ?
C34 C35 C36 C37 1.0(14) . . . . ?
C35 C36 C37 C32 -2.0(11) . . . . ?
C35 C36 C37 C38 177.6(8) . . . . ?
C36 C37 C38 F10 -10.6(10) . . . . ?
C36 C37 C38 F11 117.3(7) . . . . ?
C36 C37 C38 F12 -124.2(7) . . . . ?
C37 C32 C33 C34 -1.3(9) . . . . ?
C39 N7 C24 N5 -178.0(4) . . . . ?
C39 N7 C24 N6 2.5(6) . . . . ?
C39 C40 C41 C42 -177.1(6) . . . . ?
C40 N8 C44 C43 -0.2(8) . . . . ?
C40 C41 C42 C43 -0.1(11) . . . . ?
C41 C42 C43 C44 -0.8(11) . . . . ?
C42 C43 C44 N8 1.0(10) . . . . ?
C44 N8 C40 C39 177.3(4) . . . . ?
C44 N8 C40 C41 -0.8(7) . . . . ?
