#------------------------------------------------------------------------------
#$Date: 2016-09-07 18:11:00 +0300 (Wed, 07 Sep 2016) $
#$Revision: 186259 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/66/4086645.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_4086645
loop_
_publ_author_name
'Behnia, Ava'
'Boyle, Paul D.'
'Blacquiere, Johanna M.'
'Puddephatt, Richard J.'
_publ_section_title
;
 Selective Oxygen Atom Insertion into an Aryl--Palladium Bond
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2645
_journal_paper_doi               10.1021/acs.organomet.6b00387
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C23 H30 I2 N2 O Pd'
_chemical_formula_weight         710.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   19.207(4)
_cell_length_b                   19.213(4)
_cell_length_c                   29.230(6)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    173
_cell_measurement_theta_max      31.50
_cell_measurement_theta_min      3.19
_cell_volume                     10620(4)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  SHELXL-2014
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            114328
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.599
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.039
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       prism
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         19308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0220P)²+7.0504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12797
_reflns_number_total             19308
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00387_si_003.cif
_cod_data_source_block           complex_2b
_cod_depositor_comments
'Adding full bibliography for 4086643--4086646.cif.'
_cod_database_code               4086645
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.806
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'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Pd1 Pd 0.72530(2) 0.43470(2) 0.75091(2) 0.02389(5) Uani 1 1 d . . .
I1A I 0.61558(2) 0.46923(2) 0.69166(2) 0.03335(5) Uani 1 1 d . . .
I2A I 0.64651(2) 0.40030(2) 0.80969(2) 0.03475(5) Uani 1 1 d . . .
N1A N 0.81927(11) 0.40826(12) 0.79320(8) 0.0243(5) Uani 1 1 d . . .
N2A N 0.79743(11) 0.46126(12) 0.70894(8) 0.0246(5) Uani 1 1 d . . .
C1A C 0.87365(14) 0.41949(14) 0.77452(9) 0.0265(6) Uani 1 1 d . . .
H1A H 0.9199 0.4080 0.7901 0.032 Uiso 1 1 calc R U .
C2A C 0.86185(14) 0.45070(14) 0.72831(9) 0.0263(6) Uani 1 1 d . . .
H2A H 0.9002 0.4627 0.7132 0.032 Uiso 1 1 calc R U .
C3A C 0.82855(13) 0.37519(15) 0.83822(9) 0.0250(5) Uani 1 1 d . . .
C4A C 0.83088(13) 0.30267(15) 0.84061(9) 0.0267(6) Uani 1 1 d . . .
C5A C 0.83713(14) 0.27185(16) 0.88395(10) 0.0327(6) Uani 1 1 d . . .
H5A H 0.8387 0.2225 0.8862 0.039 Uiso 1 1 calc R U .
C6A C 0.84124(15) 0.31129(18) 0.92436(10) 0.0374(7) Uani 1 1 d . . .
C7A C 0.83842(15) 0.38274(17) 0.92055(10) 0.0370(7) Uani 1 1 d . . .
H7A H 0.8413 0.4099 0.9480 0.044 Uiso 1 1 calc R U .
C8A C 0.83144(14) 0.41674(16) 0.87772(10) 0.0319(6) Uani 1 1 d . . .
C9A C 0.82585(16) 0.25953(16) 0.79732(10) 0.0343(7) Uani 1 1 d . . .
H9A1 H 0.8262 0.2100 0.8055 0.051 Uiso 1 1 calc R U .
H9A2 H 0.8662 0.2698 0.7820 0.051 Uiso 1 1 calc R U .
H9A3 H 0.7818 0.2706 0.7762 0.051 Uiso 1 1 calc R U .
C10A C 0.8466(2) 0.2752(2) 0.97098(13) 0.0603(11) Uani 1 1 d . . .
H10A H 0.8804 0.2366 0.9727 0.091 Uiso 1 1 calc R U .
H10B H 0.8001 0.2571 0.9744 0.091 Uiso 1 1 calc R U .
H10C H 0.8629 0.3085 0.9960 0.091 Uiso 1 1 calc R U .
C11A C 0.82529(18) 0.49470(16) 0.87455(11) 0.0408(7) Uani 1 1 d . . .
H11A H 0.8616 0.5130 0.8580 0.061 Uiso 1 1 calc R U .
H11B H 0.8320 0.5145 0.9059 0.061 Uiso 1 1 calc R U .
H11C H 0.7783 0.5073 0.8576 0.061 Uiso 1 1 calc R U .
C12A C 0.78316(13) 0.49183(15) 0.66311(9) 0.0257(6) Uani 1 1 d . . .
C13A C 0.76620(14) 0.44731(16) 0.62504(10) 0.0323(6) Uani 1 1 d . . .
C14A C 0.75096(16) 0.47837(19) 0.58142(11) 0.0398(7) Uani 1 1 d . . .
H14A H 0.7401 0.4493 0.5548 0.048 Uiso 1 1 calc R U .
C15A C 0.75085(16) 0.54958(19) 0.57502(11) 0.0409(8) Uani 1 1 d . . .
C16A C 0.76697(14) 0.59110(17) 0.61442(11) 0.0362(7) Uani 1 1 d . . .
H16A H 0.7666 0.6402 0.6108 0.043 Uiso 1 1 calc R U .
C17A C 0.78352(13) 0.56348(15) 0.65883(10) 0.0280(6) Uani 1 1 d . . .
C18A C 0.76129(18) 0.36998(17) 0.63039(12) 0.0433(8) Uani 1 1 d . . .
H18A H 0.7487 0.3484 0.5997 0.065 Uiso 1 1 calc R U .
H18B H 0.7249 0.3591 0.6490 0.065 Uiso 1 1 calc R U .
H18C H 0.8070 0.3519 0.6460 0.065 Uiso 1 1 calc R U .
C19A C 0.7322(2) 0.5810(2) 0.52690(13) 0.0630(11) Uani 1 1 d . . .
H19A H 0.6818 0.5930 0.5206 0.094 Uiso 1 1 calc R U .
H19B H 0.7423 0.5473 0.5038 0.094 Uiso 1 1 calc R U .
H19C H 0.7604 0.6232 0.5252 0.094 Uiso 1 1 calc R U .
C20A C 0.79996(16) 0.60963(16) 0.70082(11) 0.0367(7) Uani 1 1 d . . .
H20A H 0.7689 0.5976 0.7229 0.055 Uiso 1 1 calc R U .
H20B H 0.7923 0.6584 0.6914 0.055 Uiso 1 1 calc R U .
H20C H 0.8494 0.6031 0.7156 0.055 Uiso 1 1 calc R U .
Pd2 Pd 0.5000 0.70989(2) 0.7500 0.02370(6) Uani 1 2 d S T P
I1B I 0.45069(2) 0.80402(2) 0.69072(2) 0.03423(5) Uani 1 1 d . . .
N1B N 0.46238(11) 0.62680(12) 0.70775(7) 0.0244(5) Uani 1 1 d . . .
C1B C 0.47798(13) 0.56732(15) 0.72689(9) 0.0253(5) Uani 1 1 d . . .
H1B H 0.4616 0.5252 0.7117 0.030 Uiso 1 1 calc R U .
C2B C 0.41771(13) 0.62932(14) 0.66235(9) 0.0251(5) Uani 1 1 d . . .
C3B C 0.44963(15) 0.63653(15) 0.62315(10) 0.0304(6) Uani 1 1 d . . .
C4B C 0.40508(16) 0.64023(16) 0.58045(10) 0.0375(7) Uani 1 1 d . . .
H4B H 0.4253 0.6444 0.5532 0.045 Uiso 1 1 calc R U .
C5B C 0.33193(16) 0.63813(17) 0.57605(10) 0.0372(7) Uani 1 1 d . . .
C6B C 0.30333(15) 0.63195(16) 0.61609(10) 0.0335(6) Uani 1 1 d . . .
H6B H 0.2533 0.6310 0.6135 0.040 Uiso 1 1 calc R U .
C7B C 0.34484(13) 0.62701(14) 0.65993(9) 0.0257(5) Uani 1 1 d . . .
C8B C 0.52834(15) 0.64235(19) 0.62673(11) 0.0405(8) Uani 1 1 d . . .
H8B1 H 0.5449 0.6854 0.6431 0.061 Uiso 1 1 calc R U .
H8B2 H 0.5403 0.6431 0.5955 0.061 Uiso 1 1 calc R U .
H8B3 H 0.5512 0.6023 0.6439 0.061 Uiso 1 1 calc R U .
C9B C 0.2847(2) 0.6439(2) 0.52914(12) 0.0637(12) Uani 1 1 d . . .
H9B1 H 0.2633 0.6903 0.5257 0.096 Uiso 1 1 calc R U .
H9B2 H 0.2474 0.6086 0.5266 0.096 Uiso 1 1 calc R U .
H9B3 H 0.3128 0.6365 0.5046 0.096 Uiso 1 1 calc R U .
C10B C 0.31223(14) 0.62050(17) 0.70278(10) 0.0339(7) Uani 1 1 d . . .
H10D H 0.2606 0.6208 0.6940 0.051 Uiso 1 1 calc R U .
H10E H 0.3273 0.6597 0.7236 0.051 Uiso 1 1 calc R U .
H10F H 0.3275 0.5768 0.7187 0.051 Uiso 1 1 calc R U .
Pd3 Pd 1.0000 0.66003(2) 0.7500 0.02416(6) Uani 1 2 d S T P
I1C I 0.98018(2) 0.56584(2) 0.80874(2) 0.03392(5) Uani 1 1 d . . .
N1C N 0.98459(11) 0.74305(12) 0.79207(8) 0.0251(5) Uani 1 1 d . . .
C1C C 0.99042(13) 0.80200(14) 0.77319(9) 0.0270(6) Uani 1 1 d . . .
H1C H 0.9827 0.8442 0.7885 0.032 Uiso 1 1 calc R U .
C2C C 0.96584(14) 0.74040(14) 0.83768(9) 0.0267(6) Uani 1 1 d . . .
C3C C 1.01963(15) 0.73342(16) 0.87636(10) 0.0322(6) Uani 1 1 d . . .
C4C C 0.99920(17) 0.72997(17) 0.91950(11) 0.0392(7) Uani 1 1 d . . .
H4C H 1.0349 0.7269 0.9464 0.047 Uiso 1 1 calc R U .
C5C C 0.92964(18) 0.73080(17) 0.92513(11) 0.0416(7) Uani 1 1 d . . .
C6C C 0.87795(16) 0.73621(16) 0.88576(11) 0.0361(7) Uani 1 1 d . . .
H6C H 0.8297 0.7363 0.8892 0.043 Uiso 1 1 calc R U .
C7C C 0.89447(14) 0.74149(15) 0.84165(10) 0.0299(6) Uani 1 1 d . . .
C8C C 1.09604(15) 0.72793(19) 0.87147(12) 0.0427(8) Uani 1 1 d . . .
H8C1 H 1.1032 0.6855 0.8543 0.064 Uiso 1 1 calc R U .
H8C2 H 1.1256 0.7261 0.9024 0.064 Uiso 1 1 calc R U .
H8C3 H 1.1092 0.7686 0.8546 0.064 Uiso 1 1 calc R U .
C9C C 0.9101(2) 0.7242(2) 0.97309(13) 0.0650(11) Uani 1 1 d . . .
H9C1 H 0.9012 0.6752 0.9794 0.097 Uiso 1 1 calc R U .
H9C2 H 0.8675 0.7515 0.9744 0.097 Uiso 1 1 calc R U .
H9C3 H 0.9491 0.7416 0.9965 0.097 Uiso 1 1 calc R U .
C10C C 0.83808(14) 0.74695(18) 0.79885(11) 0.0380(7) Uani 1 1 d . . .
H10G H 0.8424 0.7917 0.7835 0.057 Uiso 1 1 calc R U .
H10H H 0.7913 0.7437 0.8078 0.057 Uiso 1 1 calc R U .
H10I H 0.8438 0.7090 0.7774 0.057 Uiso 1 1 calc R U .
O1S O 0.88366(18) 0.46415(17) 0.50487(10) 0.0808(9) Uani 1 1 d . . .
C1S C 0.9230(2) 0.4776(2) 0.54076(14) 0.0572(10) Uani 1 1 d . . .
C2S C 0.9526(3) 0.5480(3) 0.55049(18) 0.0910(17) Uani 1 1 d . . .
H2S1 H 0.9373 0.5667 0.5783 0.137 Uiso 1 1 calc R U .
H2S2 H 0.9359 0.5785 0.5240 0.137 Uiso 1 1 calc R U .
H2S3 H 1.0044 0.5457 0.5557 0.137 Uiso 1 1 calc R U .
C3S C 0.9423(3) 0.4235(3) 0.57738(17) 0.0816(14) Uani 1 1 d . . .
H3S1 H 0.9165 0.3804 0.5677 0.122 Uiso 1 1 calc R U .
H3S2 H 0.9296 0.4399 0.6066 0.122 Uiso 1 1 calc R U .
H3S3 H 0.9932 0.4146 0.5818 0.122 Uiso 1 1 calc R U .
O2S O 0.46528(17) 0.38283(19) 0.50471(11) 0.0826(10) Uani 1 1 d . . .
C4S C 0.4881(2) 0.4125(2) 0.54049(14) 0.0582(10) Uani 1 1 d . . .
C5S C 0.4446(3) 0.4231(3) 0.57740(17) 0.0847(15) Uani 1 1 d . . .
H5S1 H 0.4011 0.3956 0.5701 0.127 Uiso 1 1 calc R U .
H5S2 H 0.4326 0.4725 0.5790 0.127 Uiso 1 1 calc R U .
H5S3 H 0.4715 0.4081 0.6074 0.127 Uiso 1 1 calc R U .
C6S C 0.5615(3) 0.4387(3) 0.55054(18) 0.0931(17) Uani 1 1 d . . .
H6S1 H 0.5833 0.4338 0.5228 0.140 Uiso 1 1 calc R U .
H6S2 H 0.5887 0.4117 0.5761 0.140 Uiso 1 1 calc R U .
H6S3 H 0.5614 0.4878 0.5594 0.140 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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1A Pd1 N2A 79.03(9) . .
N1A Pd1 I2A 95.27(6) . .
N2A Pd1 I2A 174.20(6) . .
N1A Pd1 I1A 174.22(6) . .
N2A Pd1 I1A 95.28(6) . .
I2A Pd1 I1A 90.437(17) . .
C1A N1A C3A 118.9(2) . .
C1A N1A Pd1 113.37(18) . .
C3A N1A Pd1 127.55(16) . .
C2A N2A C12A 119.0(2) . .
C2A N2A Pd1 113.17(19) . .
C12A N2A Pd1 127.75(16) . .
N1A C1A C2A 117.3(2) . .
N1A C1A H1A 121.4 . .
C2A C1A H1A 121.4 . .
N2A C2A C1A 117.1(2) . .
N2A C2A H2A 121.5 . .
C1A C2A H2A 121.5 . .
C4A C3A C8A 122.2(3) . .
C4A C3A N1A 118.9(2) . .
C8A C3A N1A 118.9(3) . .
C5A C4A C3A 118.0(3) . .
C5A C4A C9A 121.2(3) . .
C3A C4A C9A 120.8(2) . .
C4A C5A C6A 121.7(3) . .
C4A C5A H5A 119.1 . .
C6A C5A H5A 119.1 . .
C7A C6A C5A 118.5(3) . .
C7A C6A C10A 121.6(3) . .
C5A C6A C10A 119.9(3) . .
C6A C7A C8A 122.3(3) . .
C6A C7A H7A 118.8 . .
C8A C7A H7A 118.8 . .
C3A C8A C7A 117.2(3) . .
C3A C8A C11A 121.8(3) . .
C7A C8A C11A 121.0(3) . .
C4A C9A H9A1 109.5 . .
C4A C9A H9A2 109.5 . .
H9A1 C9A H9A2 109.5 . .
C4A C9A H9A3 109.5 . .
H9A1 C9A H9A3 109.5 . .
H9A2 C9A H9A3 109.5 . .
C6A C10A H10A 109.5 . .
C6A C10A H10B 109.5 . .
H10A C10A H10B 109.5 . .
C6A C10A H10C 109.5 . .
H10A C10A H10C 109.5 . .
H10B C10A H10C 109.5 . .
C8A C11A H11A 109.5 . .
C8A C11A H11B 109.5 . .
H11A C11A H11B 109.5 . .
C8A C11A H11C 109.5 . .
H11A C11A H11C 109.5 . .
H11B C11A H11C 109.5 . .
C17A C12A C13A 122.8(3) . .
C17A C12A N2A 119.1(2) . .
C13A C12A N2A 118.0(3) . .
C14A C13A C12A 116.7(3) . .
C14A C13A C18A 120.9(3) . .
C12A C13A C18A 122.3(3) . .
C15A C14A C13A 123.0(3) . .
C15A C14A H14A 118.5 . .
C13A C14A H14A 118.5 . .
C14A C15A C16A 117.5(3) . .
C14A C15A C19A 121.0(3) . .
C16A C15A C19A 121.5(3) . .
C17A C16A C15A 122.5(3) . .
C17A C16A H16A 118.8 . .
C15A C16A H16A 118.8 . .
C12A C17A C16A 117.5(3) . .
C12A C17A C20A 121.2(3) . .
C16A C17A C20A 121.3(3) . .
C13A C18A H18A 109.5 . .
C13A C18A H18B 109.5 . .
H18A C18A H18B 109.5 . .
C13A C18A H18C 109.5 . .
H18A C18A H18C 109.5 . .
H18B C18A H18C 109.5 . .
C15A C19A H19A 109.5 . .
C15A C19A H19B 109.5 . .
H19A C19A H19B 109.5 . .
C15A C19A H19C 109.5 . .
H19A C19A H19C 109.5 . .
H19B C19A H19C 109.5 . .
C17A C20A H20A 109.5 . .
C17A C20A H20B 109.5 . .
H20A C20A H20B 109.5 . .
C17A C20A H20C 109.5 . .
H20A C20A H20C 109.5 . .
H20B C20A H20C 109.5 . .
N1B Pd2 N1B 79.05(12) 2_656 .
N1B Pd2 I1B 95.25(6) 2_656 2_656
N1B Pd2 I1B 174.14(6) . 2_656
N1B Pd2 I1B 174.14(6) 2_656 .
N1B Pd2 I1B 95.25(6) . .
I1B Pd2 I1B 90.48(2) 2_656 .
C1B N1B C2B 119.0(2) . .
C1B N1B Pd2 113.32(18) . .
C2B N1B Pd2 127.55(17) . .
N1B C1B C1B 117.08(15) . 2_656
N1B C1B H1B 121.5 . .
C1B C1B H1B 121.5 2_656 .
C7B C2B C3B 122.9(2) . .
C7B C2B N1B 118.4(2) . .
C3B C2B N1B 118.7(2) . .
C4B C3B C2B 116.9(3) . .
C4B C3B C8B 121.0(3) . .
C2B C3B C8B 122.1(3) . .
C3B C4B C5B 122.5(3) . .
C3B C4B H4B 118.7 . .
C5B C4B H4B 118.7 . .
C6B C5B C4B 118.0(3) . .
C6B C5B C9B 120.7(3) . .
C4B C5B C9B 121.3(3) . .
C5B C6B C7B 122.5(3) . .
C5B C6B H6B 118.7 . .
C7B C6B H6B 118.7 . .
C6B C7B C2B 117.1(3) . .
C6B C7B C10B 121.3(2) . .
C2B C7B C10B 121.6(2) . .
C3B C8B H8B1 109.5 . .
C3B C8B H8B2 109.5 . .
H8B1 C8B H8B2 109.5 . .
C3B C8B H8B3 109.5 . .
H8B1 C8B H8B3 109.5 . .
H8B2 C8B H8B3 109.5 . .
C5B C9B H9B1 109.5 . .
C5B C9B H9B2 109.5 . .
H9B1 C9B H9B2 109.5 . .
C5B C9B H9B3 109.5 . .
H9B1 C9B H9B3 109.5 . .
H9B2 C9B H9B3 109.5 . .
C7B C10B H10D 109.5 . .
C7B C10B H10E 109.5 . .
H10D C10B H10E 109.5 . .
C7B C10B H10F 109.5 . .
H10D C10B H10F 109.5 . .
H10E C10B H10F 109.5 . .
N1C Pd3 N1C 78.97(13) 2_756 .
N1C Pd3 I1C 95.32(6) 2_756 2_756
N1C Pd3 I1C 174.25(6) . 2_756
N1C Pd3 I1C 174.25(6) 2_756 .
N1C Pd3 I1C 95.32(6) . .
I1C Pd3 I1C 90.40(2) 2_756 .
C1C N1C C2C 119.2(2) . .
C1C N1C Pd3 113.34(19) . .
C2C N1C Pd3 127.44(18) . .
N1C C1C C1C 117.14(16) . 2_756
N1C C1C H1C 121.4 . .
C1C C1C H1C 121.4 2_756 .
C7C C2C C3C 122.1(3) . .
C7C C2C N1C 118.9(2) . .
C3C C2C N1C 118.8(2) . .
C4C C3C C2C 117.0(3) . .
C4C C3C C8C 121.3(3) . .
C2C C3C C8C 121.7(3) . .
C5C C4C C3C 122.9(3) . .
C5C C4C H4C 118.5 . .
C3C C4C H4C 118.5 . .
C4C C5C C6C 118.2(3) . .
C4C C5C C9C 120.8(3) . .
C6C C5C C9C 121.1(3) . .
C7C C6C C5C 122.1(3) . .
C7C C6C H6C 119.0 . .
C5C C6C H6C 119.0 . .
C6C C7C C2C 117.7(3) . .
C6C C7C C10C 121.9(3) . .
C2C C7C C10C 120.4(3) . .
C3C C8C H8C1 109.5 . .
C3C C8C H8C2 109.5 . .
H8C1 C8C H8C2 109.5 . .
C3C C8C H8C3 109.5 . .
H8C1 C8C H8C3 109.5 . .
H8C2 C8C H8C3 109.5 . .
C5C C9C H9C1 109.5 . .
C5C C9C H9C2 109.5 . .
H9C1 C9C H9C2 109.5 . .
C5C C9C H9C3 109.5 . .
H9C1 C9C H9C3 109.5 . .
H9C2 C9C H9C3 109.5 . .
C7C C10C H10G 109.5 . .
C7C C10C H10H 109.5 . .
H10G C10C H10H 109.5 . .
C7C C10C H10I 109.5 . .
H10G C10C H10I 109.5 . .
H10H C10C H10I 109.5 . .
O1S C1S C2S 121.6(4) . .
O1S C1S C3S 120.8(4) . .
C2S C1S C3S 117.5(4) . .
C1S C2S H2S1 109.5 . .
C1S C2S H2S2 109.5 . .
H2S1 C2S H2S2 109.5 . .
C1S C2S H2S3 109.5 . .
H2S1 C2S H2S3 109.5 . .
H2S2 C2S H2S3 109.5 . .
C1S C3S H3S1 109.5 . .
C1S C3S H3S2 109.5 . .
H3S1 C3S H3S2 109.5 . .
C1S C3S H3S3 109.5 . .
H3S1 C3S H3S3 109.5 . .
H3S2 C3S H3S3 109.5 . .
O2S C4S C6S 121.6(4) . .
O2S C4S C5S 121.9(4) . .
C6S C4S C5S 116.5(4) . .
C4S C5S H5S1 109.5 . .
C4S C5S H5S2 109.5 . .
H5S1 C5S H5S2 109.5 . .
C4S C5S H5S3 109.5 . .
H5S1 C5S H5S3 109.5 . .
H5S2 C5S H5S3 109.5 . .
C4S C6S H6S1 109.5 . .
C4S C6S H6S2 109.5 . .
H6S1 C6S H6S2 109.5 . .
C4S C6S H6S3 109.5 . .
H6S1 C6S H6S3 109.5 . .
H6S2 C6S H6S3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1A 2.065(2) .
Pd1 N2A 2.069(2) .
Pd1 I2A 2.5668(5) .
Pd1 I1A 2.5700(5) .
N1A C1A 1.279(3) .
N1A C3A 1.444(3) .
N2A C2A 1.284(3) .
N2A C12A 1.444(3) .
C1A C2A 1.459(4) .
C1A H1A 0.9500 .
C2A H2A 0.9500 .
C3A C4A 1.395(4) .
C3A C8A 1.397(4) .
C4A C5A 1.384(4) .
C4A C9A 1.502(4) .
C5A C6A 1.394(4) .
C5A H5A 0.9500 .
C6A C7A 1.378(5) .
C6A C10A 1.516(4) .
C7A C8A 1.398(4) .
C7A H7A 0.9500 .
C8A C11A 1.504(4) .
C9A H9A1 0.9800 .
C9A H9A2 0.9800 .
C9A H9A3 0.9800 .
C10A H10A 0.9800 .
C10A H10B 0.9800 .
C10A H10C 0.9800 .
C11A H11A 0.9800 .
C11A H11B 0.9800 .
C11A H11C 0.9800 .
C12A C17A 1.382(4) .
C12A C13A 1.396(4) .
C13A C14A 1.392(4) .
C13A C18A 1.499(4) .
C14A C15A 1.381(5) .
C14A H14A 0.9500 .
C15A C16A 1.391(5) .
C15A C19A 1.515(5) .
C16A C17A 1.387(4) .
C16A H16A 0.9500 .
C17A C20A 1.502(4) .
C18A H18A 0.9800 .
C18A H18B 0.9800 .
C18A H18C 0.9800 .
C19A H19A 0.9800 .
C19A H19B 0.9800 .
C19A H19C 0.9800 .
C20A H20A 0.9800 .
C20A H20B 0.9800 .
C20A H20C 0.9800 .
Pd2 N1B 2.070(2) 2_656
Pd2 N1B 2.070(2) .
Pd2 I1B 2.5682(5) 2_656
Pd2 I1B 2.5682(4) .
N1B C1B 1.285(3) .
N1B C2B 1.450(3) .
C1B C1B 1.463(5) 2_656
C1B H1B 0.9500 .
C2B C7B 1.390(4) .
C2B C3B 1.398(4) .
C3B C4B 1.386(4) .
C3B C8B 1.501(4) .
C4B C5B 1.389(4) .
C4B H4B 0.9500 .
C5B C6B 1.382(4) .
C5B C9B 1.510(4) .
C6B C7B 1.389(4) .
C6B H6B 0.9500 .
C7B C10B 1.500(4) .
C8B H8B1 0.9800 .
C8B H8B2 0.9800 .
C8B H8B3 0.9800 .
C9B H9B1 0.9800 .
C9B H9B2 0.9800 .
C9B H9B3 0.9800 .
C10B H10D 0.9800 .
C10B H10E 0.9800 .
C10B H10F 0.9800 .
Pd3 N1C 2.067(2) 2_756
Pd3 N1C 2.067(2) .
Pd3 I1C 2.5682(5) 2_756
Pd3 I1C 2.5682(4) .
N1C C1C 1.273(3) .
N1C C2C 1.442(3) .
C1C C1C 1.466(6) 2_756
C1C H1C 0.9500 .
C2C C7C 1.396(4) .
C2C C3C 1.398(4) .
C3C C4C 1.386(4) .
C3C C8C 1.503(4) .
C4C C5C 1.375(5) .
C4C H4C 0.9500 .
C5C C6C 1.386(5) .
C5C C9C 1.518(5) .
C6C C7C 1.384(4) .
C6C H6C 0.9500 .
C7C C10C 1.508(4) .
C8C H8C1 0.9800 .
C8C H8C2 0.9800 .
C8C H8C3 0.9800 .
C9C H9C1 0.9800 .
C9C H9C2 0.9800 .
C9C H9C3 0.9800 .
C10C H10G 0.9800 .
C10C H10H 0.9800 .
C10C H10I 0.9800 .
O1S C1S 1.209(4) .
C1S C2S 1.476(6) .
C1S C3S 1.492(6) .
C2S H2S1 0.9800 .
C2S H2S2 0.9800 .
C2S H2S3 0.9800 .
C3S H3S1 0.9800 .
C3S H3S2 0.9800 .
C3S H3S3 0.9800 .
O2S C4S 1.204(5) .
C4S C6S 1.478(6) .
C4S C5S 1.489(6) .
C5S H5S1 0.9800 .
C5S H5S2 0.9800 .
C5S H5S3 0.9800 .
C6S H6S1 0.9800 .
C6S H6S2 0.9800 .
C6S H6S3 0.9800 .
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
C1A H1A I1B 0.95 3.16 4.017(3) 150.6 4_646
C2A H2A I1C 0.95 3.18 4.052(3) 152.8 2_756
C1B H1B I2A 0.95 3.16 4.033(3) 152.9 2_656
C1C H1C I1A 0.95 3.17 4.032(3) 151.6 4_656
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_4
C3A N1A C1A C2A 177.8(2) .
Pd1 N1A C1A C2A 2.1(3) .
C12A N2A C2A C1A -179.8(2) .
Pd1 N2A C2A C1A 2.8(3) .
N1A C1A C2A N2A -3.4(4) .
C1A N1A C3A C4A -85.1(3) .
Pd1 N1A C3A C4A 89.9(3) .
C1A N1A C3A C8A 97.9(3) .
Pd1 N1A C3A C8A -87.1(3) .
C8A C3A C4A C5A -0.8(4) .
N1A C3A C4A C5A -177.6(2) .
C8A C3A C4A C9A 178.5(2) .
N1A C3A C4A C9A 1.7(4) .
C3A C4A C5A C6A -0.2(4) .
C9A C4A C5A C6A -179.4(3) .
C4A C5A C6A C7A 0.5(4) .
C4A C5A C6A C10A 178.8(3) .
C5A C6A C7A C8A 0.2(5) .
C10A C6A C7A C8A -178.1(3) .
C4A C3A C8A C7A 1.4(4) .
N1A C3A C8A C7A 178.2(2) .
C4A C3A C8A C11A -176.9(3) .
N1A C3A C8A C11A -0.1(4) .
C6A C7A C8A C3A -1.1(4) .
C6A C7A C8A C11A 177.3(3) .
C2A N2A C12A C17A -85.6(3) .
Pd1 N2A C12A C17A 91.3(3) .
C2A N2A C12A C13A 97.4(3) .
Pd1 N2A C12A C13A -85.6(3) .
C17A C12A C13A C14A 1.6(4) .
N2A C12A C13A C14A 178.4(2) .
C17A C12A C13A C18A -175.8(3) .
N2A C12A C13A C18A 1.0(4) .
C12A C13A C14A C15A -1.2(4) .
C18A C13A C14A C15A 176.2(3) .
C13A C14A C15A C16A 0.1(5) .
C13A C14A C15A C19A -178.5(3) .
C14A C15A C16A C17A 0.7(4) .
C19A C15A C16A C17A 179.3(3) .
C13A C12A C17A C16A -0.8(4) .
N2A C12A C17A C16A -177.6(2) .
C13A C12A C17A C20A 178.1(3) .
N2A C12A C17A C20A 1.3(4) .
C15A C16A C17A C12A -0.4(4) .
C15A C16A C17A C20A -179.3(3) .
C2B N1B C1B C1B -178.8(3) 2_656
Pd2 N1B C1B C1B -3.3(4) 2_656
C1B N1B C2B C7B 84.0(3) .
Pd2 N1B C2B C7B -90.7(3) .
C1B N1B C2B C3B -98.3(3) .
Pd2 N1B C2B C3B 87.0(3) .
C7B C2B C3B C4B -1.1(4) .
N1B C2B C3B C4B -178.7(3) .
C7B C2B C3B C8B 177.0(3) .
N1B C2B C3B C8B -0.6(4) .
C2B C3B C4B C5B 1.0(5) .
C8B C3B C4B C5B -177.1(3) .
C3B C4B C5B C6B -0.1(5) .
C3B C4B C5B C9B 178.6(3) .
C4B C5B C6B C7B -0.8(5) .
C9B C5B C6B C7B -179.5(3) .
C5B C6B C7B C2B 0.7(4) .
C5B C6B C7B C10B 179.9(3) .
C3B C2B C7B C6B 0.3(4) .
N1B C2B C7B C6B 177.8(2) .
C3B C2B C7B C10B -178.9(3) .
N1B C2B C7B C10B -1.3(4) .
C2C N1C C1C C1C 180.0(3) 2_756
Pd3 N1C C1C C1C -2.5(4) 2_756
C1C N1C C2C C7C 86.1(3) .
Pd3 N1C C2C C7C -91.0(3) .
C1C N1C C2C C3C -96.9(3) .
Pd3 N1C C2C C3C 86.0(3) .
C7C C2C C3C C4C -2.2(4) .
N1C C2C C3C C4C -179.0(3) .
C7C C2C C3C C8C 176.2(3) .
N1C C2C C3C C8C -0.6(4) .
C2C C3C C4C C5C 2.2(5) .
C8C C3C C4C C5C -176.2(3) .
C3C C4C C5C C6C -0.8(5) .
C3C C4C C5C C9C 177.7(3) .
C4C C5C C6C C7C -0.7(5) .
C9C C5C C6C C7C -179.3(3) .
C5C C6C C7C C2C 0.7(4) .
C5C C6C C7C C10C 179.6(3) .
C3C C2C C7C C6C 0.8(4) .
N1C C2C C7C C6C 177.6(3) .
C3C C2C C7C C10C -178.2(3) .
N1C C2C C7C C10C -1.3(4) .
