#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:52:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179081 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/43/4304376.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_4304376
loop_
_publ_author_name
'José Ruiz'
'María Dolores Villa'
'Natalia Cutillas'
'Concepción de Haro'
'Delia Bautista'
'Virtudes Moreno'
'Laura Valencia'
_publ_section_title
;
Palladium(II) and Platinum(II) Organometallic Complexes with
4,7-dihydro-5-methyl-7-oxo[1,2,4]triazolo[1,5-a]pyrimidine. Antitumor
Activity of the Platinum Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4490
_journal_page_last               4505
_journal_paper_doi               10.1021/ic701873b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C78 H92 Cl2 F20 N8 O2 Pd2'
_chemical_formula_weight         1837.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.718(2)
_cell_angle_beta                 108.812(2)
_cell_angle_gamma                110.224(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2953(7)
_cell_length_b                   17.0706(8)
_cell_length_c                   17.9758(8)
_cell_measurement_reflns_used    8217
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.23
_cell_volume                     4049.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44817
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.8781
_exptl_absorpt_correction_T_min  0.8157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.202
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         16452
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0775P)²+10.0383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                14724
_reflns_number_total             16452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701873b-file001_5.cif
_cod_data_source_block           md470s
_cod_database_code               4304376
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.220482(17) 0.852527(14) 0.359669(13) 0.01716(7) Uani 1 1 d . . .
Pd2 Pd 0.095297(18) 0.673892(15) 0.189165(14) 0.01980(8) Uani 1 1 d . . .
N4 N 0.2077(2) 0.76049(17) 0.15808(16) 0.0221(6) Uani 1 1 d . . .
N3 N 0.2801(2) 0.88541(17) 0.27019(16) 0.0207(5) Uani 1 1 d . . .
N1 N 0.3831(2) 0.97662(18) 0.22121(18) 0.0255(6) Uani 1 1 d . . .
N14 N 0.3033(2) 0.77422(17) 0.39052(16) 0.0197(5) Uani 1 1 d . . .
N13 N 0.2089(2) 0.64987(17) 0.27601(16) 0.0221(6) Uani 1 1 d . . .
N11 N 0.3027(2) 0.57335(19) 0.31949(19) 0.0288(6) Uani 1 1 d . . .
N7 N 0.6799(2) 0.58162(19) 0.46424(19) 0.0282(6) Uani 1 1 d . . .
N9 N 0.6768(2) 1.0032(2) 0.15253(18) 0.0326(7) Uani 1 1 d . . .
O1 O 0.39055(19) 0.93180(17) 0.07000(15) 0.0316(6) Uani 1 1 d . . .
O2 O 0.46723(19) 0.62888(17) 0.46698(17) 0.0322(6) Uani 1 1 d . . .
F1 F 0.22945(16) 0.96872(13) 0.52422(12) 0.0309(4) Uani 1 1 d . . .
F2 F 0.13228(17) 0.92146(14) 0.62161(12) 0.0333(5) Uani 1 1 d . . .
F3 F 0.01821(17) 0.75259(15) 0.60387(13) 0.0336(5) Uani 1 1 d . . .
F4 F -0.00483(16) 0.63261(13) 0.47953(13) 0.0299(4) Uani 1 1 d . . .
F5 F 0.09272(14) 0.67793(12) 0.38105(11) 0.0237(4) Uani 1 1 d . . .
F6 F 0.32078(15) 1.05386(13) 0.41729(13) 0.0302(4) Uani 1 1 d . . .
F7 F 0.2491(2) 1.17427(14) 0.39510(15) 0.0410(6) Uani 1 1 d . . .
F8 F 0.0470(2) 1.13057(16) 0.32003(16) 0.0459(6) Uani 1 1 d . . .
F9 F -0.08127(18) 0.96110(17) 0.26825(16) 0.0455(6) Uani 1 1 d . . .
F10 F -0.01068(15) 0.83893(14) 0.28703(13) 0.0323(5) Uani 1 1 d . . .
F11 F -0.07170(16) 0.67410(15) 0.26364(14) 0.0373(5) Uani 1 1 d . . .
F12 F -0.2135(2) 0.5470(2) 0.28517(17) 0.0612(8) Uani 1 1 d . . .
F13 F -0.2451(2) 0.3805(2) 0.23352(19) 0.0727(10) Uani 1 1 d . . .
F14 F -0.1287(2) 0.34427(16) 0.16023(17) 0.0629(8) Uani 1 1 d . . .
F15 F 0.01702(19) 0.47152(14) 0.13920(14) 0.0404(5) Uani 1 1 d . . .
F16 F 0.06184(16) 0.84293(13) 0.16837(12) 0.0319(5) Uani 1 1 d . . .
F17 F -0.0883(2) 0.87373(18) 0.06917(17) 0.0546(7) Uani 1 1 d . . .
F18 F -0.2423(2) 0.7467(2) -0.05538(18) 0.0628(8) Uani 1 1 d . . .
F19 F -0.2420(2) 0.58656(18) -0.07871(16) 0.0623(8) Uani 1 1 d . . .
F20 F -0.09782(19) 0.55138(14) 0.02412(14) 0.0439(6) Uani 1 1 d . . .
C41 C 0.1625(2) 0.8260(2) 0.44452(19) 0.0206(6) Uani 1 1 d . . .
C46 C 0.1710(3) 0.8841(2) 0.5088(2) 0.0238(7) Uani 1 1 d . . .
C45 C 0.1231(3) 0.8611(2) 0.5612(2) 0.0260(7) Uani 1 1 d . . .
C44 C 0.0643(3) 0.7761(2) 0.5524(2) 0.0267(7) Uani 1 1 d . . .
C43 C 0.0541(2) 0.7156(2) 0.4900(2) 0.0237(7) Uani 1 1 d . . .
C42 C 0.1034(2) 0.7415(2) 0.43882(19) 0.0213(6) Uani 1 1 d . . .
C51 C 0.1594(3) 0.9397(2) 0.34720(19) 0.0221(6) Uani 1 1 d . . .
C52 C 0.2198(3) 1.0265(2) 0.3759(2) 0.0256(7) Uani 1 1 d . . .
C53 C 0.1850(3) 1.0909(2) 0.3669(2) 0.0300(8) Uani 1 1 d . . .
C54 C 0.0827(3) 1.0686(3) 0.3294(2) 0.0327(8) Uani 1 1 d . . .
C55 C 0.0189(3) 0.9837(3) 0.3029(2) 0.0314(8) Uani 1 1 d . . .
C56 C 0.0576(3) 0.9210(2) 0.3126(2) 0.0263(7) Uani 1 1 d . . .
C21 C -0.0173(3) 0.5801(2) 0.2036(2) 0.0267(7) Uani 1 1 d . . .
C22 C -0.0802(3) 0.5940(3) 0.2381(2) 0.0323(8) Uani 1 1 d . . .
C23 C -0.1560(3) 0.5286(3) 0.2491(2) 0.0435(11) Uani 1 1 d . . .
C24 C -0.1721(3) 0.4444(3) 0.2233(3) 0.0485(12) Uani 1 1 d . . .
C25 C -0.1125(3) 0.4268(3) 0.1866(2) 0.0445(11) Uani 1 1 d . . .
C26 C -0.0371(3) 0.4940(2) 0.1775(2) 0.0329(8) Uani 1 1 d . . .
C31 C -0.0131(3) 0.6944(2) 0.1050(2) 0.0258(7) Uani 1 1 d . . .
C32 C -0.0146(3) 0.7757(2) 0.1104(2) 0.0293(7) Uani 1 1 d . . .
C33 C -0.0901(3) 0.7944(3) 0.0591(3) 0.0403(9) Uani 1 1 d . . .
C34 C -0.1673(3) 0.7299(3) -0.0041(3) 0.0449(10) Uani 1 1 d . . .
C35 C -0.1676(3) 0.6496(3) -0.0154(2) 0.0440(11) Uani 1 1 d . . .
C36 C -0.0917(3) 0.6326(2) 0.0390(2) 0.0337(8) Uani 1 1 d . . .
C3A C 0.2672(2) 0.8425(2) 0.19786(19) 0.0203(6) Uani 1 1 d . . .
C2 C 0.3502(2) 0.9649(2) 0.2797(2) 0.0237(7) Uani 1 1 d . . .
H2 H 0.3741 1.0096 0.3264 0.028 Uiso 1 1 calc R . .
N8 N 0.3285(2) 0.89744(17) 0.16811(17) 0.0222(6) Uani 1 1 d . . .
C7 C 0.3364(2) 0.8765(2) 0.0934(2) 0.0252(7) Uani 1 1 d . . .
C6 C 0.2770(3) 0.7884(2) 0.0555(2) 0.0288(7) Uani 1 1 d . . .
H6 H 0.2790 0.7656 0.0060 0.035 Uiso 1 1 calc R . .
C5 C 0.2165(3) 0.7344(2) 0.0876(2) 0.0267(7) Uani 1 1 d . . .
C8 C 0.1565(3) 0.6414(2) 0.0437(2) 0.0376(9) Uani 1 1 d . . .
H8A H 0.1627 0.6053 0.0825 0.045 Uiso 1 1 calc R . .
H8B H 0.1822 0.6270 0.0032 0.045 Uiso 1 1 calc R . .
H8C H 0.0854 0.6314 0.0168 0.045 Uiso 1 1 calc R . .
C13A C 0.2822(2) 0.6964(2) 0.34836(19) 0.0198(6) Uani 1 1 d . . .
C12 C 0.2267(3) 0.5776(2) 0.2630(2) 0.0287(7) Uani 1 1 d . . .
H12 H 0.1859 0.5329 0.2153 0.034 Uiso 1 1 calc R . .
N18 N 0.3383(2) 0.64949(18) 0.37471(17) 0.0226(6) Uani 1 1 d . . .
C17 C 0.4228(2) 0.6762(2) 0.4480(2) 0.0250(7) Uani 1 1 d . . .
C16 C 0.4441(3) 0.7591(2) 0.4900(2) 0.0258(7) Uani 1 1 d . . .
H16 H 0.5004 0.7847 0.5400 0.031 Uiso 1 1 calc R . .
C15 C 0.3865(2) 0.8049(2) 0.4615(2) 0.0229(6) Uani 1 1 d . . .
C18 C 0.4159(3) 0.8930(2) 0.5088(2) 0.0307(8) Uani 1 1 d . . .
H18A H 0.4156 0.9322 0.4726 0.037 Uiso 1 1 calc R . .
H18B H 0.4836 0.9126 0.5508 0.037 Uiso 1 1 calc R . .
H18C H 0.3678 0.8920 0.5342 0.037 Uiso 1 1 calc R . .
C61 C 0.5818(3) 0.5137(3) 0.4001(3) 0.0346(8) Uani 1 1 d . . .
H61A H 0.5612 0.4619 0.4213 0.042 Uiso 1 1 calc R . .
H61B H 0.5285 0.5361 0.3910 0.042 Uiso 1 1 calc R . .
C62 C 0.5880(3) 0.4876(3) 0.3196(3) 0.0393(9) Uani 1 1 d . . .
H62A H 0.6201 0.5400 0.3027 0.047 Uiso 1 1 calc R . .
H62B H 0.6315 0.4551 0.3264 0.047 Uiso 1 1 calc R . .
C63 C 0.4863(3) 0.4330(3) 0.2536(3) 0.0541(12) Uani 1 1 d . . .
H63A H 0.4433 0.4659 0.2452 0.065 Uiso 1 1 calc R . .
H63B H 0.4531 0.3811 0.2708 0.065 Uiso 1 1 calc R . .
C64 C 0.4960(4) 0.4057(4) 0.1742(3) 0.0723(17) Uani 1 1 d . . .
H64A H 0.5228 0.4566 0.1544 0.087 Uiso 1 1 calc R . .
H64B H 0.4295 0.3668 0.1340 0.087 Uiso 1 1 calc R . .
H64C H 0.5418 0.3761 0.1831 0.087 Uiso 1 1 calc R . .
C65 C 0.6644(3) 0.5870(2) 0.5438(2) 0.0322(8) Uani 1 1 d . . .
H65A H 0.6147 0.6127 0.5403 0.039 Uiso 1 1 calc R . .
H65B H 0.6346 0.5278 0.5503 0.039 Uiso 1 1 calc R . .
C66 C 0.7575(3) 0.6379(2) 0.6183(2) 0.0323(8) Uani 1 1 d . . .
H66A H 0.7921 0.6958 0.6112 0.039 Uiso 1 1 calc R . .
H66B H 0.8045 0.6087 0.6274 0.039 Uiso 1 1 calc R . .
C67 C 0.7273(4) 0.6456(3) 0.6907(3) 0.0442(10) Uani 1 1 d . . .
H67A H 0.6816 0.6760 0.6815 0.053 Uiso 1 1 calc R . .
H67B H 0.6900 0.5873 0.6956 0.053 Uiso 1 1 calc R . .
C68 C 0.8176(5) 0.6935(4) 0.7687(3) 0.0676(16) Uani 1 1 d . . .
H68A H 0.8638 0.6644 0.7774 0.081 Uiso 1 1 calc R . .
H68B H 0.7951 0.6947 0.8139 0.081 Uiso 1 1 calc R . .
H68C H 0.8523 0.7524 0.7654 0.081 Uiso 1 1 calc R . .
C69 C 0.6946(3) 0.6668(2) 0.4390(2) 0.0332(8) Uani 1 1 d . . .
H69A H 0.6605 0.6533 0.3794 0.040 Uiso 1 1 calc R . .
H69B H 0.6588 0.6943 0.4622 0.040 Uiso 1 1 calc R . .
C70 C 0.8005(3) 0.7325(2) 0.4617(2) 0.0309(8) Uani 1 1 d . . .
H70A H 0.8375 0.7084 0.4366 0.037 Uiso 1 1 calc R . .
H70B H 0.8369 0.7481 0.5212 0.037 Uiso 1 1 calc R . .
C71 C 0.7952(3) 0.8125(3) 0.4318(2) 0.0347(8) Uani 1 1 d . . .
H71A H 0.7560 0.7954 0.3727 0.042 Uiso 1 1 calc R . .
H71B H 0.7590 0.8363 0.4579 0.042 Uiso 1 1 calc R . .
C72 C 0.8992(3) 0.8823(3) 0.4497(3) 0.0410(9) Uani 1 1 d . . .
H72A H 0.9385 0.8995 0.5081 0.049 Uiso 1 1 calc R . .
H72B H 0.8915 0.9322 0.4305 0.049 Uiso 1 1 calc R . .
H72C H 0.9343 0.8599 0.4219 0.049 Uiso 1 1 calc R . .
C73 C 0.7675(3) 0.5562(2) 0.4712(2) 0.0255(7) Uani 1 1 d . . .
H73A H 0.7770 0.5543 0.4192 0.031 Uiso 1 1 calc R . .
H73B H 0.8297 0.6009 0.5134 0.031 Uiso 1 1 calc R . .
C74 C 0.7532(3) 0.4699(2) 0.4922(2) 0.0285(7) Uani 1 1 d . . .
H74A H 0.6989 0.4235 0.4458 0.034 Uiso 1 1 calc R . .
H74B H 0.7326 0.4677 0.5391 0.034 Uiso 1 1 calc R . .
C75 C 0.8506(3) 0.4553(2) 0.5126(2) 0.0296(7) Uani 1 1 d . . .
H75A H 0.8789 0.4704 0.4711 0.036 Uiso 1 1 calc R . .
H75B H 0.8346 0.3936 0.5104 0.036 Uiso 1 1 calc R . .
C76 C 0.9304(3) 0.5080(2) 0.5961(2) 0.0325(8) Uani 1 1 d . . .
H76A H 0.9485 0.5694 0.5982 0.039 Uiso 1 1 calc R . .
H76B H 0.9905 0.4955 0.6060 0.039 Uiso 1 1 calc R . .
H76C H 0.9033 0.4930 0.6377 0.039 Uiso 1 1 calc R . .
C81 C 0.6351(3) 1.0690(2) 0.1678(2) 0.0335(8) Uani 1 1 d . A .
H81A H 0.5627 1.0381 0.1572 0.040 Uiso 1 1 calc R . .
H81B H 0.6396 1.1050 0.1281 0.040 Uiso 1 1 calc R . .
C82 C 0.6867(3) 1.1283(3) 0.2524(2) 0.0400(9) Uani 1 1 d . . .
H82A H 0.6891 1.0935 0.2933 0.048 Uiso 1 1 calc R A .
H82B H 0.7568 1.1658 0.2613 0.048 Uiso 1 1 calc R . .
C83 C 0.6294(3) 1.1834(3) 0.2623(3) 0.0453(10) Uani 1 1 d . A .
H83A H 0.5601 1.1455 0.2551 0.054 Uiso 1 1 calc R . .
H83B H 0.6244 1.2158 0.2195 0.054 Uiso 1 1 calc R . .
C84 C 0.6806(4) 1.2468(3) 0.3453(3) 0.0539(12) Uani 1 1 d . . .
H84A H 0.6875 1.2151 0.3879 0.065 Uiso 1 1 calc R A .
H84B H 0.6394 1.2787 0.3498 0.065 Uiso 1 1 calc R . .
H84C H 0.7474 1.2871 0.3511 0.065 Uiso 1 1 calc R . .
C85 C 0.6751(3) 0.9469(3) 0.2131(2) 0.0303(8) Uani 1 1 d . A .
H85A H 0.7002 0.9035 0.1992 0.036 Uiso 1 1 calc R . .
H85B H 0.7231 0.9833 0.2674 0.036 Uiso 1 1 calc R . .
C86 C 0.5738(3) 0.9003(2) 0.2183(2) 0.0300(8) Uani 1 1 d . . .
H86A H 0.5430 0.9415 0.2254 0.036 Uiso 1 1 calc R A .
H86B H 0.5278 0.8558 0.1677 0.036 Uiso 1 1 calc R . .
C87 C 0.5887(3) 0.8588(3) 0.2895(3) 0.0446(11) Uani 1 1 d . A .
H87A H 0.6358 0.9037 0.3395 0.053 Uiso 1 1 calc R . .
H87B H 0.6198 0.8181 0.2819 0.053 Uiso 1 1 calc R . .
C88 C 0.4903(4) 0.8107(4) 0.2998(3) 0.0551(13) Uani 1 1 d . . .
H88A H 0.4565 0.8495 0.3032 0.066 Uiso 1 1 calc R A .
H88B H 0.5049 0.7900 0.3494 0.066 Uiso 1 1 calc R . .
H88C H 0.4464 0.7617 0.2532 0.066 Uiso 1 1 calc R . .
C89A C 0.7872(6) 1.0326(7) 0.1575(5) 0.030(2) Uiso 0.538(15) 1 d P A 1
C90A C 0.8090(6) 1.0920(6) 0.1012(5) 0.0313(19) Uiso 0.538(15) 1 d P A 1
C91A C 0.9219(7) 1.1094(7) 0.1090(6) 0.053(3) Uiso 0.538(15) 1 d P A 1
C92A C 0.9508(9) 1.1602(9) 0.0523(8) 0.069(3) Uiso 0.538(15) 1 d P A 1
C89B C 0.7858(6) 1.0574(7) 0.1661(5) 0.021(2) Uiso 0.462(15) 1 d P A 2
C90B C 0.8031(6) 1.1235(7) 0.1148(5) 0.031(2) Uiso 0.462(15) 1 d P A 2
C91B C 0.9170(7) 1.1512(7) 0.1245(6) 0.040(3) Uiso 0.462(15) 1 d P A 2
C92B C 0.9506(12) 1.2030(12) 0.0687(10) 0.075(4) Uiso 0.462(15) 1 d P A 2
C93 C 0.6092(3) 0.9486(3) 0.0669(2) 0.0360(9) Uani 1 1 d . A .
H93A H 0.5393 0.9219 0.0643 0.043 Uiso 1 1 calc R . .
H93B H 0.6098 0.9871 0.0292 0.043 Uiso 1 1 calc R . .
C94 C 0.6369(3) 0.8783(4) 0.0370(3) 0.0517(12) Uani 1 1 d . . .
H94A H 0.6416 0.8414 0.0760 0.062 Uiso 1 1 calc R A .
H94B H 0.7035 0.9041 0.0332 0.062 Uiso 1 1 calc R . .
C95 C 0.5575(4) 0.8237(4) -0.0461(3) 0.0548(13) Uani 1 1 d . A .
H95A H 0.5486 0.8619 -0.0833 0.066 Uiso 1 1 calc R . .
H95B H 0.5821 0.7839 -0.0682 0.066 Uiso 1 1 calc R . .
C96 C 0.4556(4) 0.7716(3) -0.0431(3) 0.0515(11) Uani 1 1 d . . .
H96A H 0.4648 0.7378 -0.0024 0.062 Uiso 1 1 calc R A .
H96B H 0.4103 0.7329 -0.0962 0.062 Uiso 1 1 calc R . .
H96C H 0.4263 0.8107 -0.0286 0.062 Uiso 1 1 calc R . .
C99 C 0.7151(5) 0.8920(4) 0.8436(4) 0.0725(16) Uiso 1 1 d . . .
H99A H 0.6779 0.9242 0.8585 0.087 Uiso 1 1 calc R . .
H99B H 0.7276 0.8572 0.8836 0.087 Uiso 1 1 calc R . .
Cl1 Cl 0.82987(14) 0.96413(15) 0.84617(12) 0.0950(6) Uani 1 1 d . . .
Cl2 Cl 0.64124(17) 0.82314(11) 0.74582(16) 0.1015(7) Uani 1 1 d . . .
C101 C 0.4944(7) 0.3725(6) 0.8793(6) 0.104(3) Uiso 1 1 d D . .
C102 C 0.4091(7) 0.3350(5) 0.8066(6) 0.105(3) Uiso 1 1 d D . .
H102 H 0.4219 0.3251 0.7589 0.126 Uiso 1 1 calc R . .
C103 C 0.3059(6) 0.3101(5) 0.7954(5) 0.0850(19) Uiso 1 1 d D . .
H103 H 0.2526 0.2807 0.7443 0.102 Uiso 1 1 calc R . .
C104 C 0.2881(7) 0.3318(6) 0.8651(5) 0.101(2) Uiso 1 1 d D . .
H104 H 0.2215 0.3232 0.8603 0.121 Uiso 1 1 calc R . .
C105 C 0.3672(6) 0.3662(5) 0.9421(5) 0.095(2) Uiso 1 1 d D . .
H105 H 0.3527 0.3721 0.9894 0.114 Uiso 1 1 calc R . .
C106 C 0.4689(7) 0.3920(6) 0.9485(6) 0.102(2) Uiso 1 1 d D . .
H106 H 0.5219 0.4227 0.9995 0.123 Uiso 1 1 calc R . .
C107 C 0.5923(5) 0.3822(5) 0.8790(4) 0.0769(17) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 '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
C51 Pd1 C41 86.02(13) . . ?
C51 Pd1 N3 91.51(11) . . ?
C41 Pd1 N3 177.48(11) . . ?
C51 Pd1 N14 170.80(12) . . ?
C41 Pd1 N14 91.58(11) . . ?
N3 Pd1 N14 90.78(10) . . ?
C31 Pd2 C21 86.58(14) . . ?
C31 Pd2 N4 90.91(12) . . ?
C21 Pd2 N4 171.84(12) . . ?
C31 Pd2 N13 178.77(13) . . ?
C21 Pd2 N13 93.11(12) . . ?
N4 Pd2 N13 89.24(11) . . ?
C3A N4 C5 115.4(3) . . ?
C3A N4 Pd2 126.2(2) . . ?
C5 N4 Pd2 118.2(2) . . ?
C3A N3 C2 103.1(3) . . ?
C3A N3 Pd1 134.5(2) . . ?
C2 N3 Pd1 122.3(2) . . ?
C2 N1 N8 101.4(3) . . ?
C13A N14 C15 115.1(3) . . ?
C13A N14 Pd1 127.0(2) . . ?
C15 N14 Pd1 117.9(2) . . ?
C13A N13 C12 103.4(3) . . ?
C13A N13 Pd2 133.6(2) . . ?
C12 N13 Pd2 122.8(2) . . ?
C12 N11 N18 101.8(3) . . ?
C73 N7 C65 110.3(3) . . ?
C73 N7 C69 112.2(3) . . ?
C65 N7 C69 110.0(3) . . ?
C73 N7 C61 110.6(3) . . ?
C65 N7 C61 106.7(3) . . ?
C69 N7 C61 106.8(3) . . ?
C81 N9 C85 111.3(3) . . ?
C81 N9 C89B 103.9(5) . . ?
C85 N9 C89B 109.2(4) . . ?
C81 N9 C93 106.1(3) . . ?
C85 N9 C93 110.1(3) . . ?
C89B N9 C93 116.0(4) . . ?
C81 N9 C89A 120.3(5) . . ?
C85 N9 C89A 102.2(4) . . ?
C89B N9 C89A 16.6(4) . . ?
C93 N9 C89A 106.5(4) . . ?
C42 C41 C46 113.8(3) . . ?
C42 C41 Pd1 118.9(2) . . ?
C46 C41 Pd1 127.3(2) . . ?
F1 C46 C45 115.5(3) . . ?
F1 C46 C41 120.8(3) . . ?
C45 C46 C41 123.7(3) . . ?
F2 C45 C44 119.0(3) . . ?
F2 C45 C46 120.7(3) . . ?
C44 C45 C46 120.2(3) . . ?
F3 C44 C43 120.7(3) . . ?
F3 C44 C45 120.9(3) . . ?
C43 C44 C45 118.4(3) . . ?
F4 C43 C44 119.2(3) . . ?
F4 C43 C42 121.4(3) . . ?
C44 C43 C42 119.4(3) . . ?
F5 C42 C43 115.7(3) . . ?
F5 C42 C41 119.8(3) . . ?
C43 C42 C41 124.4(3) . . ?
C56 C51 C52 114.3(3) . . ?
C56 C51 Pd1 125.3(3) . . ?
C52 C51 Pd1 120.5(2) . . ?
F6 C52 C53 115.1(3) . . ?
F6 C52 C51 120.4(3) . . ?
C53 C52 C51 124.4(3) . . ?
F7 C53 C54 120.3(3) . . ?
F7 C53 C52 120.9(3) . . ?
C54 C53 C52 118.8(3) . . ?
F8 C54 C55 121.0(4) . . ?
F8 C54 C53 119.8(4) . . ?
C55 C54 C53 119.2(3) . . ?
F9 C55 C54 119.7(3) . . ?
F9 C55 C56 120.4(4) . . ?
C54 C55 C56 119.9(3) . . ?
F10 C56 C51 120.8(3) . . ?
F10 C56 C55 116.0(3) . . ?
C51 C56 C55 123.2(3) . . ?
C22 C21 C26 114.6(3) . . ?
C22 C21 Pd2 124.5(3) . . ?
C26 C21 Pd2 120.9(3) . . ?
F11 C22 C21 120.9(3) . . ?
F11 C22 C23 115.4(4) . . ?
C21 C22 C23 123.6(4) . . ?
F12 C23 C24 119.8(4) . . ?
F12 C23 C22 120.4(4) . . ?
C24 C23 C22 119.8(4) . . ?
F13 C24 C23 120.4(5) . . ?
F13 C24 C25 120.7(5) . . ?
C23 C24 C25 118.9(4) . . ?
F14 C25 C24 119.2(4) . . ?
F14 C25 C26 121.3(5) . . ?
C24 C25 C26 119.5(4) . . ?
F15 C26 C25 116.0(4) . . ?
F15 C26 C21 120.4(3) . . ?
C25 C26 C21 123.6(4) . . ?
C36 C31 C32 113.9(3) . . ?
C36 C31 Pd2 125.6(3) . . ?
C32 C31 Pd2 120.6(3) . . ?
F16 C32 C33 115.7(3) . . ?
F16 C32 C31 119.8(3) . . ?
C33 C32 C31 124.5(4) . . ?
F17 C33 C34 119.8(4) . . ?
F17 C33 C32 121.4(4) . . ?
C34 C33 C32 118.8(4) . . ?
F18 C34 C35 120.5(4) . . ?
F18 C34 C33 119.9(4) . . ?
C35 C34 C33 119.6(4) . . ?
F19 C35 C34 119.8(4) . . ?
F19 C35 C36 120.3(4) . . ?
C34 C35 C36 119.9(4) . . ?
F20 C36 C31 120.5(3) . . ?
F20 C36 C35 116.4(3) . . ?
C31 C36 C35 123.1(4) . . ?
N4 C3A N3 129.5(3) . . ?
N4 C3A N8 122.5(3) . . ?
N3 C3A N8 107.9(3) . . ?
N1 C2 N3 116.6(3) . . ?
C3A N8 N1 111.0(3) . . ?
C3A N8 C7 125.1(3) . . ?
N1 N8 C7 123.9(3) . . ?
O1 C7 N8 120.4(3) . . ?
O1 C7 C6 129.0(3) . . ?
N8 C7 C6 110.6(3) . . ?
C5 C6 C7 122.7(3) . . ?
N4 C5 C6 123.5(3) . . ?
N4 C5 C8 117.3(3) . . ?
C6 C5 C8 119.3(3) . . ?
N14 C13A N13 129.9(3) . . ?
N14 C13A N18 122.7(3) . . ?
N13 C13A N18 107.3(3) . . ?
N11 C12 N13 116.4(3) . . ?
N11 N18 C13A 111.1(3) . . ?
N11 N18 C17 123.9(3) . . ?
C13A N18 C17 125.0(3) . . ?
O2 C17 N18 120.2(3) . . ?
O2 C17 C16 129.1(3) . . ?
N18 C17 C16 110.7(3) . . ?
C15 C16 C17 122.9(3) . . ?
N14 C15 C16 123.6(3) . . ?
N14 C15 C18 117.2(3) . . ?
C16 C15 C18 119.2(3) . . ?
C62 C61 N7 114.7(3) . . ?
C63 C62 C61 113.1(4) . . ?
C62 C63 C64 111.5(4) . . ?
C66 C65 N7 115.7(3) . . ?
C65 C66 C67 109.0(3) . . ?
C68 C67 C66 112.2(4) . . ?
C70 C69 N7 118.7(3) . . ?
C69 C70 C71 108.7(3) . . ?
C72 C71 C70 112.9(3) . . ?
C74 C73 N7 113.7(3) . . ?
C73 C74 C75 110.9(3) . . ?
C74 C75 C76 113.3(3) . . ?
N9 C81 C82 116.0(3) . . ?
C83 C82 C81 110.2(3) . . ?
C82 C83 C84 112.4(4) . . ?
C86 C85 N9 116.3(3) . . ?
C87 C86 C85 109.1(3) . . ?
C86 C87 C88 112.8(3) . . ?
C90A C89A N9 112.6(6) . . ?
C89A C90A C91A 105.6(7) . . ?
C92A C91A C90A 111.7(8) . . ?
N9 C89B C90B 116.9(6) . . ?
C89B C90B C91B 105.2(7) . . ?
C92B C91B C90B 117.3(9) . . ?
C94 C93 N9 116.1(3) . . ?
C93 C94 C95 110.4(4) . . ?
C96 C95 C94 112.9(4) . . ?
Cl1 C99 Cl2 110.5(4) . . ?
C102 C101 C107 119.2(8) . . ?
C102 C101 C106 112.5(8) . . ?
C107 C101 C106 128.1(8) . . ?
C101 C102 C103 128.1(9) . . ?
C104 C103 C102 115.6(8) . . ?
C103 C104 C105 121.2(8) . . ?
C104 C105 C106 119.7(8) . . ?
C105 C106 C101 122.1(9) . . ?
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 C51 2.009(3) . ?
Pd1 C41 2.012(3) . ?
Pd1 N3 2.123(3) . ?
Pd1 N14 2.136(3) . ?
Pd2 C31 2.012(3) . ?
Pd2 C21 2.014(3) . ?
Pd2 N4 2.117(3) . ?
Pd2 N13 2.120(3) . ?
N4 C3A 1.341(4) . ?
N4 C5 1.364(4) . ?
N3 C3A 1.346(4) . ?
N3 C2 1.360(4) . ?
N1 C2 1.308(5) . ?
N1 N8 1.372(4) . ?
N14 C13A 1.338(4) . ?
N14 C15 1.371(4) . ?
N13 C13A 1.348(4) . ?
N13 C12 1.366(4) . ?
N11 C12 1.304(5) . ?
N11 N18 1.370(4) . ?
N7 C73 1.518(4) . ?
N7 C65 1.523(5) . ?
N7 C69 1.530(5) . ?
N7 C61 1.530(5) . ?
N9 C81 1.512(5) . ?
N9 C85 1.524(5) . ?
N9 C89B 1.524(8) . ?
N9 C93 1.526(5) . ?
N9 C89A 1.555(9) . ?
O1 C7 1.232(4) . ?
O2 C17 1.231(4) . ?
F1 C46 1.353(4) . ?
F2 C45 1.356(4) . ?
F3 C44 1.346(4) . ?
F4 C43 1.346(4) . ?
F5 C42 1.351(4) . ?
F6 C52 1.359(4) . ?
F7 C53 1.347(4) . ?
F8 C54 1.350(4) . ?
F9 C55 1.347(4) . ?
F10 C56 1.347(4) . ?
F11 C22 1.346(5) . ?
F12 C23 1.346(5) . ?
F13 C24 1.342(5) . ?
F14 C25 1.350(5) . ?
F15 C26 1.357(5) . ?
F16 C32 1.348(4) . ?
F17 C33 1.338(5) . ?
F18 C34 1.357(5) . ?
F19 C35 1.350(5) . ?
F20 C36 1.350(5) . ?
C41 C42 1.384(5) . ?
C41 C46 1.386(5) . ?
C46 C45 1.378(5) . ?
C45 C44 1.378(5) . ?
C44 C43 1.376(5) . ?
C43 C42 1.382(5) . ?
C51 C56 1.379(5) . ?
C51 C52 1.382(5) . ?
C52 C53 1.380(5) . ?
C53 C54 1.380(6) . ?
C54 C55 1.366(6) . ?
C55 C56 1.391(5) . ?
C21 C22 1.371(5) . ?
C21 C26 1.391(5) . ?
C22 C23 1.388(5) . ?
C23 C24 1.374(7) . ?
C24 C25 1.375(7) . ?
C25 C26 1.384(5) . ?
C31 C36 1.386(5) . ?
C31 C32 1.391(5) . ?
C32 C33 1.383(5) . ?
C33 C34 1.372(6) . ?
C34 C35 1.366(7) . ?
C35 C36 1.394(6) . ?
C3A N8 1.365(4) . ?
N8 C7 1.408(4) . ?
C7 C6 1.415(5) . ?
C6 C5 1.379(5) . ?
C5 C8 1.503(5) . ?
C13A N18 1.375(4) . ?
N18 C17 1.410(4) . ?
C17 C16 1.411(5) . ?
C16 C15 1.383(5) . ?
C15 C18 1.489(5) . ?
C61 C62 1.513(6) . ?
C62 C63 1.511(6) . ?
C63 C64 1.527(8) . ?
C65 C66 1.502(6) . ?
C66 C67 1.523(5) . ?
C67 C68 1.511(8) . ?
C69 C70 1.509(5) . ?
C70 C71 1.534(5) . ?
C71 C72 1.529(6) . ?
C73 C74 1.517(5) . ?
C74 C75 1.529(5) . ?
C75 C76 1.531(5) . ?
C81 C82 1.527(6) . ?
C82 C83 1.522(6) . ?
C83 C84 1.533(6) . ?
C85 C86 1.517(5) . ?
C86 C87 1.516(5) . ?
C87 C88 1.525(6) . ?
C89A C90A 1.535(11) . ?
C90A C91A 1.603(12) . ?
C91A C92A 1.480(16) . ?
C89B C90B 1.534(12) . ?
C90B C91B 1.584(13) . ?
C91B C92B 1.499(18) . ?
C93 C94 1.508(7) . ?
C94 C95 1.531(6) . ?
C95 C96 1.525(7) . ?
C99 Cl1 1.745(7) . ?
C99 Cl2 1.771(7) . ?
C101 C102 1.406(12) . ?
C101 C107 1.452(11) . ?
C101 C106 1.459(12) . ?
C102 C103 1.423(11) . ?
C103 C104 1.407(11) . ?
C104 C105 1.411(11) . ?
C105 C106 1.424(11) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C65 H65A O2 0.99 2.34 3.243(4) 150.8 .
C81 H81A O1 0.99 2.48 3.383(4) 151.5 .
C93 H93A O1 0.99 2.37 3.276(5) 151.5 .
C85 H85B F2 0.99 2.35 3.317(4) 164.5 2_676
C93 H93B O1 0.99 2.36 3.351(5) 174.5 2_675
C73 H73A F12 0.99 2.45 3.442(4) 175.6 1_655
C65 H65B O2 0.99 2.51 3.485(5) 166.7 2_666
