#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/43/2214391.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214391
loop_
_publ_author_name
'Hai-Ping Huang'
'Li-Xia Liu'
_publ_section_title
;Bis(μ-4-benzyl-3,5-diphenylpyrazolato-κ²N:N')bis[(4,4'-dimethyl-2,2'-bipyridine-κ²N,N')palladium(II)]
 bis(hexafluorophosphate) diethyl ether monosolvate monohydrate
;
_journal_coeditor_code           SI2018
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1875
_journal_page_last               m1876
_journal_paper_doi               10.1107/S1600536807028401
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Pd2 (C22 H17 N2)2 (C12 H12 N2)2] (P F6)2 , C4 H10 O , H2 O'
_chemical_formula_moiety
'C68 H58 N8 Pd2 2+ , 2F6 P - , C4 H10 O , H2 O'
_chemical_formula_sum            'C72 H70 F12 N8 O2 P2 Pd2'
_chemical_formula_weight         1582.10
_chemical_name_systematic
;
Bis(μ-4-benzyl-3,5-diphenylpyrazolato-κ²N:N')bis[(4,4'-\
dimethyl-2,2'-bipyridine-κ²N,N')palladium(II)]
bis(hexafluoridophosphate) diethyl ether monosolvate monohydrate
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   22.1138(3)
_cell_length_b                   22.1138(3)
_cell_length_c                   12.8884(2)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.930
_cell_measurement_theta_min      2.427
_cell_volume                     5458.29(13)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47040
_diffrn_reflns_theta_full        28.290
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.06
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.8080
_exptl_absorpt_correction_T_min  0.7556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.739
_refine_ls_abs_structure_details 'Flack (1983), with 4168 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         9007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0449
_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)+(0.0859P)²+2.0829P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1435
_reflns_number_gt                8156
_reflns_number_total             9007
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            si2018.cif
_cod_data_source_block           I
_cod_database_code               2214391
_cod_database_fobs_code          2214391
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 0.5436(3) 0.8913(3) 1.0360(4) 0.0499(10) Uani d . 1
H H1 0.5219 0.9138 1.0659 0.060 Uiso calc R 1
C C2 0.5767(3) 0.8665(3) 1.0993(4) 0.0590(13) Uani d . 1
H H2 0.5777 0.8732 1.1706 0.071 Uiso calc R 1
C C3 0.6080(3) 0.8319(3) 1.0572(4) 0.0600(13) Uani d . 1
C C4 0.6420(5) 0.8022(5) 1.1256(6) 0.095(3) Uani d . 1
H H4A 0.6909 0.8355 1.1322 0.142 Uiso calc R 1
H H4B 0.6362 0.7600 1.0952 0.142 Uiso calc R 1
H H4C 0.6206 0.7921 1.1929 0.142 Uiso calc R 1
C C5 0.6071(3) 0.8259(3) 0.9514(5) 0.0577(12) Uani d . 1
H H5 0.6284 0.8033 0.9208 0.069 Uiso calc R 1
C C6 0.5751(2) 0.8527(2) 0.8887(4) 0.0439(9) Uani d . 1
C C7 0.5768(2) 0.8544(2) 0.7752(4) 0.0422(9) Uani d . 1
C C8 0.6115(3) 0.8291(3) 0.7153(4) 0.0525(11) Uani d . 1
H H8 0.6319 0.8060 0.7471 0.063 Uiso calc R 1
C C9 0.6160(3) 0.8379(3) 0.6094(4) 0.0580(13) Uani d . 1
C C10 0.6557(5) 0.8132(5) 0.5452(6) 0.089(2) Uani d . 1
H H10A 0.6379 0.7643 0.5576 0.133 Uiso calc R 1
H H10B 0.7042 0.8389 0.5637 0.133 Uiso calc R 1
H H10C 0.6505 0.8204 0.4731 0.133 Uiso calc R 1
C C11 0.5847(3) 0.8732(3) 0.5659(4) 0.0591(13) Uani d . 1
H H11 0.5870 0.8809 0.4947 0.071 Uiso calc R 1
C C12 0.5500(3) 0.8965(3) 0.6292(4) 0.0508(11) Uani d . 1
H H12 0.5295 0.9201 0.5992 0.061 Uiso calc R 1
C C13 0.4209(2) 0.9453(2) 0.6460(4) 0.0422(9) Uani d . 1
C C14 0.3722(2) 0.8706(2) 0.6242(4) 0.0468(10) Uani d . 1
C C15 0.3780(3) 0.8400(3) 0.5326(5) 0.0652(14) Uani d . 1
H H15 0.4128 0.8663 0.4847 0.078 Uiso calc R 1
C C16 0.3309(5) 0.7694(4) 0.5139(7) 0.084(2) Uani d . 1
H H16 0.3354 0.7484 0.4542 0.101 Uiso calc R 1
C C17 0.2784(5) 0.7310(3) 0.5822(7) 0.088(2) Uani d . 1
H H17 0.2472 0.6841 0.5685 0.106 Uiso calc R 1
C C18 0.2716(4) 0.7611(4) 0.6711(8) 0.086(2) Uani d . 1
H H18 0.2352 0.7349 0.7169 0.103 Uiso calc R 1
C C19 0.3187(3) 0.8307(3) 0.6929(5) 0.0620(12) Uani d . 1
H H19 0.3143 0.8506 0.7539 0.074 Uiso calc R 1
C C20 0.4195(2) 0.9389(2) 1.0197(4) 0.0403(9) Uani d . 1
C C21 0.3762(2) 0.8629(2) 1.0408(4) 0.0455(10) Uani d . 1
C C22 0.3518(3) 0.8147(3) 0.9600(5) 0.0589(13) Uani d . 1
H H22 0.3615 0.8299 0.8916 0.071 Uiso calc R 1
C C23 0.3129(3) 0.7436(3) 0.9820(6) 0.0715(17) Uani d . 1
H H23 0.2971 0.7116 0.9278 0.086 Uiso calc R 1
C C24 0.2976(3) 0.7204(3) 1.0813(7) 0.082(2) Uani d . 1
H H24 0.2704 0.6728 1.0944 0.098 Uiso calc R 1
C C25 0.3214(3) 0.7660(4) 1.1609(6) 0.0725(18) Uani d . 1
H H25 0.3114 0.7495 1.2287 0.087 Uiso calc R 1
C C26 0.3609(3) 0.8374(3) 1.1428(5) 0.0591(13) Uani d . 1
H H26 0.3772 0.8683 1.1984 0.071 Uiso calc R 1
C C27 0.4274(2) 1.0032(3) 0.5939(3) 0.0429(8) Uani d . 1
C C28 0.3809(3) 1.0019(3) 0.5084(4) 0.0528(11) Uani d . 1
H H28A 0.3642 0.9587 0.4699 0.063 Uiso calc R 1
H H28B 0.4085 1.0401 0.4613 0.063 Uiso calc R 1
C C29 0.3190(3) 1.0073(2) 0.5424(4) 0.0498(11) Uani d . 1
C C30 0.2880(3) 0.9856(3) 0.6380(5) 0.0644(14) Uani d . 1
H H30 0.3081 0.9699 0.6865 0.077 Uiso calc R 1
C C31 0.2275(4) 0.9864(5) 0.6643(9) 0.096(3) Uani d . 1
H H31 0.2067 0.9696 0.7286 0.115 Uiso calc R 1
C C32 0.1984(5) 1.0118(6) 0.5953(11) 0.117(4) Uani d . 1
H H32 0.1591 1.0145 0.6138 0.140 Uiso calc R 1
C C33 0.2280(5) 1.0335(5) 0.4983(11) 0.108(4) Uani d . 1
H H33 0.2079 1.0494 0.4501 0.130 Uiso calc R 1
C C34 0.2877(4) 1.0314(3) 0.4731(6) 0.0742(19) Uani d . 1
H H34 0.3075 1.0466 0.4078 0.089 Uiso calc R 1
C C35 0.0657(19) 0.0584(18) 0.794(3) 0.282(17) Uani d . 1
H H35A 0.0256 0.0564 0.8277 0.338 Uiso calc R 1
H H35B 0.0548 0.0504 0.7204 0.338 Uiso calc R 1
C C36 0.1279(17) 0.1337(17) 0.806(2) 0.267(14) Uani d . 1
H H36A 0.1342 0.1462 0.8782 0.401 Uiso calc R 1
H H36B 0.1185 0.1654 0.7682 0.401 Uiso calc R 1
H H36C 0.1696 0.1359 0.7795 0.401 Uiso calc R 1
F F1 0.5517(4) 1.0008(4) 0.4557(3) 0.1223(19) Uani d . 1
F F2 0.5204(7) 0.9199(4) 0.3331(6) 0.185(4) Uani d . 1
F F3 0.4871(6) 1.0000 0.3333 0.220(9) Uani d S 1
F F4 0.6205(7) 1.0000 0.3333 0.218(7) Uani d S 1
F F5 0.8020(4) 1.0593(5) 0.8395(10) 0.098(3) Uani d P 0.50
F F6 0.8550(5) 1.0000 0.8333 0.174(5) Uani d S 1
F F7 0.7642(6) 0.9347(7) 0.9591(14) 0.270(7) Uani d . 1
F F8 0.7129(6) 0.9957(7) 0.9187(15) 0.158(6) Uani d P 0.50
F F9 0.8204(7) 1.0540(8) 0.9732(17) 0.173(7) Uani d P 0.50
N N1 0.5419(2) 0.8839(2) 0.9324(3) 0.0409(7) Uani d . 1
N N2 0.5449(2) 0.8865(2) 0.7307(3) 0.0405(7) Uani d . 1
N N3 0.46707(19) 0.96654(19) 0.7249(3) 0.0386(7) Uani d . 1
N N4 0.46601(18) 0.96287(19) 0.9408(3) 0.0384(7) Uani d . 1
O O1 0.0732(17) 0.0000 0.8333 0.290(15) Uani d S 1
O O2 0.2246(11) 0.2246(11) 1.0000 0.332(17) Uani d S 1
H H2A 0.2470 0.2505 0.9373 0.398 Uiso d R 1
P P1 0.55322(12) 1.0000 0.3333 0.0683(6) Uani d S 1
P P2 0.7837(3) 0.9967(3) 0.8965(6) 0.122(2) Uani d P 0.50
Pd Pd1 0.500203(16) 0.921712(16) 0.83157(2) 0.03555(10) Uani d . 1
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 121.9(4) ?
N1 C1 H1 . . 119.0 ?
C2 C1 H1 . . 119.0 ?
C3 C2 C1 . . 120.2(5) ?
C3 C2 H2 . . 119.9 ?
C1 C2 H2 . . 119.9 ?
C5 C3 C2 . . 117.3(5) ?
C5 C3 C4 . . 121.8(5) ?
C2 C3 C4 . . 120.9(6) ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
C3 C5 C6 . . 121.6(5) ?
C3 C5 H5 . . 119.2 ?
C6 C5 H5 . . 119.2 ?
N1 C6 C5 . . 119.8(5) ?
N1 C6 C7 . . 114.6(4) ?
C5 C6 C7 . . 125.5(4) ?
N2 C7 C8 . . 121.0(4) ?
N2 C7 C6 . . 115.0(4) ?
C8 C7 C6 . . 124.0(4) ?
C9 C8 C7 . . 120.7(5) ?
C9 C8 H8 . . 119.7 ?
C7 C8 H8 . . 119.7 ?
C8 C9 C11 . . 117.2(5) ?
C8 C9 C10 . . 120.8(6) ?
C11 C9 C10 . . 121.9(6) ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C12 C11 C9 . . 119.6(5) ?
C12 C11 H11 . . 120.2 ?
C9 C11 H11 . . 120.2 ?
N2 C12 C11 . . 122.6(5) ?
N2 C12 H12 . . 118.7 ?
C11 C12 H12 . . 118.7 ?
N3 C13 C27 . . 109.4(4) ?
N3 C13 C14 . . 122.2(4) ?
C27 C13 C14 . . 128.4(4) ?
C19 C14 C15 . . 119.2(5) ?
C19 C14 C13 . . 120.1(5) ?
C15 C14 C13 . . 120.6(5) ?
C14 C15 C16 . . 119.2(7) ?
C14 C15 H15 . . 120.4 ?
C16 C15 H15 . . 120.4 ?
C17 C16 C15 . . 120.8(7) ?
C17 C16 H16 . . 119.6 ?
C15 C16 H16 . . 119.6 ?
C16 C17 C18 . . 120.2(6) ?
C16 C17 H17 . . 119.9 ?
C18 C17 H17 . . 119.9 ?
C17 C18 C19 . . 120.2(7) ?
C17 C18 H18 . . 119.9 ?
C19 C18 H18 . . 119.9 ?
C14 C19 C18 . . 120.3(6) ?
C14 C19 H19 . . 119.9 ?
C18 C19 H19 . . 119.9 ?
N4 C20 C27 . 5_676 108.2(4) ?
N4 C20 C21 . . 121.0(4) ?
C27 C20 C21 5_676 . 130.7(4) ?
C22 C21 C26 . . 117.9(5) ?
C22 C21 C20 . . 120.9(5) ?
C26 C21 C20 . . 121.1(5) ?
C21 C22 C23 . . 119.8(6) ?
C21 C22 H22 . . 120.1 ?
C23 C22 H22 . . 120.1 ?
C24 C23 C22 . . 121.0(7) ?
C24 C23 H23 . . 119.5 ?
C22 C23 H23 . . 119.5 ?
C25 C24 C23 . . 120.4(6) ?
C25 C24 H24 . . 119.8 ?
C23 C24 H24 . . 119.8 ?
C24 C25 C26 . . 120.6(6) ?
C24 C25 H25 . . 119.7 ?
C26 C25 H25 . . 119.7 ?
C25 C26 C21 . . 120.2(6) ?
C25 C26 H26 . . 119.9 ?
C21 C26 H26 . . 119.9 ?
C13 C27 C20 . 5_676 105.0(4) ?
C13 C27 C28 . . 125.7(4) ?
C20 C27 C28 5_676 . 129.0(4) ?
C27 C28 C29 . . 115.5(4) ?
C27 C28 H28A . . 108.4 ?
C29 C28 H28A . . 108.4 ?
C27 C28 H28B . . 108.4 ?
C29 C28 H28B . . 108.4 ?
H28A C28 H28B . . 107.5 ?
C30 C29 C34 . . 116.9(6) ?
C30 C29 C28 . . 123.3(5) ?
C34 C29 C28 . . 119.6(6) ?
C29 C30 C31 . . 122.0(7) ?
C29 C30 H30 . . 119.0 ?
C31 C30 H30 . . 119.0 ?
C32 C31 C30 . . 120.0(10) ?
C32 C31 H31 . . 120.0 ?
C30 C31 H31 . . 120.0 ?
C31 C32 C33 . . 119.3(8) ?
C31 C32 H32 . . 120.4 ?
C33 C32 H32 . . 120.4 ?
C34 C33 C32 . . 119.8(7) ?
C34 C33 H33 . . 120.1 ?
C32 C33 H33 . . 120.1 ?
C33 C34 C29 . . 121.9(8) ?
C33 C34 H34 . . 119.0 ?
C29 C34 H34 . . 119.0 ?
O1 C35 C36 . . 119(4) ?
O1 C35 H35A . . 107.7 ?
C36 C35 H35A . . 107.7 ?
O1 C35 H35B . . 107.7 ?
C36 C35 H35B . . 107.7 ?
H35A C35 H35B . . 107.1 ?
C35 C36 H36A . . 109.5 ?
C35 C36 H36B . . 109.5 ?
H36A C36 H36B . . 109.5 ?
C35 C36 H36C . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
F3 P1 F4 . . 180.000(4) ?
F3 P1 F2 . . 95.9(5) ?
F4 P1 F2 . . 84.1(5) ?
F3 P1 F2 . 5_675 95.9(5) ?
F4 P1 F2 . 5_675 84.1(5) ?
F2 P1 F2 . 5_675 168.1(10) ?
F3 P1 F1 . 5_675 88.5(3) ?
F4 P1 F1 . 5_675 91.5(3) ?
F2 P1 F1 . 5_675 89.5(4) ?
F2 P1 F1 5_675 5_675 90.8(4) ?
F3 P1 F1 . . 88.5(3) ?
F4 P1 F1 . . 91.5(3) ?
F2 P1 F1 . . 90.8(4) ?
F2 P1 F1 5_675 . 89.5(4) ?
F1 P1 F1 5_675 . 177.0(6) ?
F5 P2 F5 5_676 . 105.5(7) ?
F5 P2 F7 5_676 . 76.7(8) ?
F5 P2 F7 . . 177.0(10) ?
F5 P2 F9 5_676 . 174.8(8) ?
F5 P2 F9 . . 75.4(8) ?
F7 P2 F9 . . 102.3(11) ?
F5 P2 F8 5_676 . 84.6(8) ?
F5 P2 F8 . . 84.6(7) ?
F7 P2 F8 . . 93.6(8) ?
F9 P2 F8 . . 90.4(9) ?
F5 P2 P2 5_676 5_676 55.5(6) ?
F5 P2 P2 . 5_676 54.8(6) ?
F7 P2 P2 . 5_676 128.0(10) ?
F9 P2 P2 . 5_676 127.2(8) ?
F8 P2 P2 . 5_676 100.4(7) ?
F5 P2 F6 5_676 . 85.0(5) ?
F5 P2 F6 . . 84.7(5) ?
F7 P2 F6 . . 97.7(7) ?
F9 P2 F6 . . 100.2(6) ?
F8 P2 F6 . . 162.5(9) ?
P2 P2 F6 5_676 . 62.1(3) ?
P2 F5 P2 5_676 . 69.7(7) ?
P2 F6 P2 5_676 . 55.9(6) ?
C1 N1 C6 . . 119.0(4) ?
C1 N1 Pd1 . . 125.9(3) ?
C6 N1 Pd1 . . 115.0(3) ?
C12 N2 C7 . . 118.8(4) ?
C12 N2 Pd1 . . 126.4(3) ?
C7 N2 Pd1 . . 114.5(3) ?
C13 N3 N4 . 5_676 108.4(3) ?
C13 N3 Pd1 . . 137.3(3) ?
N4 N3 Pd1 5_676 . 114.1(3) y
N3 N4 C20 5_676 . 109.0(3) ?
N3 N4 Pd1 5_676 . 113.9(3) y
C20 N4 Pd1 . . 137.0(3) ?
C35 O1 C35 . 5_556 113(4) ?
H2A O2 H2A . 4_557 113.30(10) ?
N1 Pd1 N2 . . 80.80(10) y
N1 Pd1 N4 . . 95.20(10) ?
N2 Pd1 N4 . . 173.5(2) ?
N1 Pd1 N3 . . 174.7(2) ?
N2 Pd1 N3 . . 96.80(10) ?
N4 Pd1 N3 . . 86.80(10) y
N1 Pd1 Pd1 . 5_676 110.59(12) ?
N2 Pd1 Pd1 . 5_676 110.18(11) ?
N4 Pd1 Pd1 . 5_676 66.34(11) ?
N3 Pd1 Pd1 . 5_676 65.68(11) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.343(6) ?
C1 C2 . 1.378(7) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.375(8) ?
C2 H2 . 0.9300 ?
C3 C5 . 1.370(8) ?
C3 C4 . 1.506(7) ?
C4 H4A . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
C5 C6 . 1.388(6) ?
C5 H5 . 0.9300 ?
C6 N1 . 1.356(6) ?
C6 C7 . 1.464(7) ?
C7 N2 . 1.355(5) ?
C7 C8 . 1.387(6) ?
C8 C9 . 1.375(8) ?
C8 H8 . 0.9300 ?
C9 C11 . 1.394(8) ?
C9 C10 . 1.495(8) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 C12 . 1.384(7) ?
C11 H11 . 0.9300 ?
C12 N2 . 1.321(6) ?
C12 H12 . 0.9300 ?
C13 N3 . 1.349(6) ?
C13 C27 . 1.388(7) ?
C13 C14 . 1.480(6) ?
C14 C19 . 1.385(8) ?
C14 C15 . 1.397(8) ?
C15 C16 . 1.398(10) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.362(12) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.372(12) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.389(9) ?
C18 H18 . 0.9300 ?
C19 H19 . 0.9300 ?
C20 N4 . 1.352(6) ?
C20 C27 5_676 1.409(6) ?
C20 C21 . 1.484(6) ?
C21 C22 . 1.392(8) ?
C21 C26 . 1.403(7) ?
C22 C23 . 1.392(8) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.356(11) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.348(12) ?
C24 H24 . 0.9300 ?
C25 C26 . 1.390(9) ?
C25 H25 . 0.9300 ?
C26 H26 . 0.9300 ?
C27 C20 5_676 1.409(6) ?
C27 C28 . 1.497(6) ?
C28 C29 . 1.499(8) ?
C28 H28A . 0.9700 ?
C28 H28B . 0.9700 ?
C29 C30 . 1.375(9) ?
C29 C34 . 1.389(7) ?
C30 C31 . 1.387(9) ?
C30 H30 . 0.9300 ?
C31 C32 . 1.373(14) ?
C31 H31 . 0.9300 ?
C32 C33 . 1.382(16) ?
C32 H32 . 0.9300 ?
C33 C34 . 1.382(13) ?
C33 H33 . 0.9300 ?
C34 H34 . 0.9300 ?
C35 O1 . 1.47(4) ?
C35 C36 . 1.55(4) ?
C35 H35A . 0.9700 ?
C35 H35B . 0.9700 ?
C36 H36A . 0.9600 ?
C36 H36B . 0.9600 ?
C36 H36C . 0.9600 ?
P1 F3 . 1.462(15) ?
P1 F4 . 1.489(15) ?
P1 F2 . 1.542(8) ?
P1 F2 5_675 1.542(8) ?
P1 F1 5_675 1.577(4) ?
P1 F1 . 1.577(4) ?
P2 F5 5_676 1.425(13) ?
P2 F5 . 1.436(12) ?
P2 F7 . 1.458(13) ?
P2 F9 . 1.49(2) ?
P2 F8 . 1.582(13) ?
P2 P2 5_676 1.634(15) ?
P2 F6 . 1.744(11) ?
F5 P2 5_676 1.425(12) ?
F6 P2 5_676 1.744(11) ?
N1 Pd1 . 2.002(3) y
N2 Pd1 . 2.010(3) y
N3 N4 5_676 1.352(5) y
N3 Pd1 . 2.033(3) y
N4 N3 5_676 1.352(5) ?
N4 Pd1 . 2.017(3) y
O1 C35 5_556 1.47(4) ?
O2 H2A . 0.9713 ?
Pd1 Pd1 5_676 2.9989(6) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C1 H1 F1 5_676 0.93 2.50 3.228(8) 135
C12 H12 F1 . 0.93 2.44 3.200(8) 139
C36 H36A O2 . 0.96 2.45 3.25(3) 141
C36 H36B F7 3_564 0.96 2.31 3.04(4) 133
C36 H36C F9 3_564 0.96 2.19 2.95(3) 135
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N1 C1 C2 C3 . . -1.2(10)
C1 C2 C3 C5 . . 2.4(10)
C1 C2 C3 C4 . . -177.7(7)
C2 C3 C5 C6 . . -0.8(9)
C4 C3 C5 C6 . . 179.3(7)
C3 C5 C6 N1 . . -2.0(9)
C3 C5 C6 C7 . . 174.2(6)
N1 C6 C7 N2 . . -0.3(6)
C5 C6 C7 N2 . . -176.6(5)
N1 C6 C7 C8 . . 176.2(5)
C5 C6 C7 C8 . . -0.2(8)
N2 C7 C8 C9 . . 1.9(8)
C6 C7 C8 C9 . . -174.3(5)
C7 C8 C9 C11 . . 0.2(8)
C7 C8 C9 C10 . . 177.6(6)
C8 C9 C11 C12 . . -1.0(9)
C10 C9 C11 C12 . . -178.4(6)
C9 C11 C12 N2 . . -0.3(9)
N3 C13 C14 C19 . . 68.4(6)
C27 C13 C14 C19 . . -111.3(6)
N3 C13 C14 C15 . . -114.1(6)
C27 C13 C14 C15 . . 66.2(7)
C19 C14 C15 C16 . . -1.9(9)
C13 C14 C15 C16 . . -179.4(6)
C14 C15 C16 C17 . . 2.1(11)
C15 C16 C17 C18 . . -0.6(12)
C16 C17 C18 C19 . . -1.0(12)
C15 C14 C19 C18 . . 0.3(9)
C13 C14 C19 C18 . . 177.9(6)
C17 C18 C19 C14 . . 1.2(11)
N4 C20 C21 C22 . . -35.4(7)
C27 C20 C21 C22 5_676 . 147.6(5)
N4 C20 C21 C26 . . 142.2(5)
C27 C20 C21 C26 5_676 . -34.9(7)
C26 C21 C22 C23 . . 0.7(8)
C20 C21 C22 C23 . . 178.3(5)
C21 C22 C23 C24 . . 0.7(9)
C22 C23 C24 C25 . . -1.7(10)
C23 C24 C25 C26 . . 1.3(10)
C24 C25 C26 C21 . . 0.1(9)
C22 C21 C26 C25 . . -1.1(8)
C20 C21 C26 C25 . . -178.7(5)
N3 C13 C27 C20 . 5_676 -0.3(5)
C14 C13 C27 C20 . 5_676 179.4(5)
N3 C13 C27 C28 . . -173.6(4)
C14 C13 C27 C28 . . 6.1(8)
C13 C27 C28 C29 . . 90.3(6)
C20 C27 C28 C29 5_676 . -81.4(6)
C27 C28 C29 C30 . . -27.2(7)
C27 C28 C29 C34 . . 156.9(5)
C34 C29 C30 C31 . . 1.1(9)
C28 C29 C30 C31 . . -175.0(6)
C29 C30 C31 C32 . . -2.5(12)
C30 C31 C32 C33 . . 3.0(14)
C31 C32 C33 C34 . . -2.2(14)
C32 C33 C34 C29 . . 0.8(12)
C30 C29 C34 C33 . . -0.2(9)
C28 C29 C34 C33 . . 176.0(6)
F5 P2 F5 P2 5_676 5_676 -23.9(8)
F9 P2 F5 P2 . 5_676 161.4(7)
F8 P2 F5 P2 . 5_676 -106.8(8)
F6 P2 F5 P2 . 5_676 59.4(4)
F5 P2 F6 P2 5_676 5_676 53.3(5)
F5 P2 F6 P2 . 5_676 -52.8(5)
F7 P2 F6 P2 . 5_676 129.1(9)
F9 P2 F6 P2 . 5_676 -126.9(8)
F8 P2 F6 P2 . 5_676 -0.5(18)
C2 C1 N1 C6 . . -1.7(8)
C2 C1 N1 Pd1 . . -176.6(4)
C5 C6 N1 C1 . . 3.3(7)
C7 C6 N1 C1 . . -173.3(4)
C5 C6 N1 Pd1 . . 178.7(4)
C7 C6 N1 Pd1 . . 2.1(5)
C11 C12 N2 C7 . . 2.4(8)
C11 C12 N2 Pd1 . . 176.8(4)
C8 C7 N2 C12 . . -3.2(7)
C6 C7 N2 C12 . . 173.4(4)
C8 C7 N2 Pd1 . . -178.3(4)
C6 C7 N2 Pd1 . . -1.7(5)
C27 C13 N3 N4 . 5_676 0.6(5)
C14 C13 N3 N4 . 5_676 -179.1(4)
C27 C13 N3 Pd1 . . -173.7(3)
C14 C13 N3 Pd1 . . 6.6(7)
C27 C20 N4 N3 5_676 5_676 0.5(5)
C21 C20 N4 N3 . 5_676 -177.2(4)
C27 C20 N4 Pd1 5_676 . 175.6(3)
C21 C20 N4 Pd1 . . -2.0(7)
C36 C35 O1 C35 . 5_556 147(3)
C1 N1 Pd1 N2 . . 172.7(5)
C6 N1 Pd1 N2 . . -2.4(3)
C1 N1 Pd1 N4 . . -2.1(4)
C6 N1 Pd1 N4 . . -177.2(3)
C1 N1 Pd1 Pd1 . 5_676 64.5(4)
C6 N1 Pd1 Pd1 . 5_676 -110.6(3)
C12 N2 Pd1 N1 . . -172.4(5)
C7 N2 Pd1 N1 . . 2.2(3)
C12 N2 Pd1 N3 . . 2.8(5)
C7 N2 Pd1 N3 . . 177.4(3)
C12 N2 Pd1 Pd1 . 5_676 -63.7(4)
C7 N2 Pd1 Pd1 . 5_676 110.9(3)
N3 N4 Pd1 N1 5_676 . 111.1(3)
C20 N4 Pd1 N1 . . -63.9(5)
N3 N4 Pd1 N3 5_676 . -63.9(3)
C20 N4 Pd1 N3 . . 121.1(4)
N3 N4 Pd1 Pd1 5_676 5_676 0.9(2)
C20 N4 Pd1 Pd1 . 5_676 -174.1(5)
C13 N3 Pd1 N2 . . 65.8(5)
N4 N3 Pd1 N2 5_676 . -108.3(3)
C13 N3 Pd1 N4 . . -119.6(5)
N4 N3 Pd1 N4 5_676 . 66.3(3)
C13 N3 Pd1 Pd1 . 5_676 174.9(5)
N4 N3 Pd1 Pd1 5_676 5_676 0.9(2)
