#------------------------------------------------------------------------------
#$Date: 2020-05-28 01:51:11 +0300 (Thu, 28 May 2020) $
#$Revision: 252395 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/50/4135031.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_4135031
loop_
_publ_author_name
'Zhou, Xue-Quan'
'Xiao, Ming'
'Vadde, Ramu'
'Hilgendorf, Jonathan'
'Li, Xuezhao'
'Papadopoulou, Panagiota'
'Siegler, Maxime A.'
'Kros, Alexander'
'Sun, Wen'
'Bonnet, Sylvestre'
_publ_section_title
;
 The self-assembly of a cyclometalated palladium photosensitizer into
 proteins-stabilized nanorods triggered drug uptake in vitro and in vivo.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01369
_journal_year                    2020
_chemical_formula_moiety         'C22 H17 N4 Pd, F6 P'
_chemical_formula_sum            'C22 H17 F6 N4 P Pd'
_chemical_formula_weight         588.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                111.199(3)
_cell_angle_beta                 98.922(3)
_cell_angle_gamma                94.144(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0794(2)
_cell_length_b                   12.4486(4)
_cell_length_c                   12.4689(4)
_cell_measurement_reflns_used    7723
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.94
_cell_measurement_theta_min      6.36
_cell_volume                     1002.24(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12084
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.845
_diffrn_reflns_theta_min         3.846
_exptl_absorpt_coefficient_mu    8.930
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_description       needle
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0203
_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)+(0.0288P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3974
_reflns_number_total             4342
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c01369_si_003.cif
_cod_data_source_block           2_PF6
_cod_database_code               4135031
_shelx_shelxl_version_number     2018/3
_twin_information
;

 * * * CRYSALIS TWIN DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * *
Laue class: 1bar - Friedel mate is equivalent
Lattice type: P-lattice 
DC PROFFITRRPTWIN INFO: Step 1 - Loading orientation matrices (UB) of 2 components
 
DC PROFFITRRPTWIN INFO: Loading UB component 1
 
DC PROFFITRRPTWIN INFO: Loading UB component 2
 
DC PROFFITRRPTWIN INFO: Step 2 - Computing crossed twin laws
 
Twin law determination (relative to component 1)
Matrix 1 is taken from component 1 (   7.077   12.448   12.462   111.22    98.89    94.15)
Matrix 2 is taken from component 2 (   7.073   12.460   12.437   111.26    98.26    94.57)
Twin analysis: Component 1 with component 2
TL  =UB[1]-1*UB[2]:   1.0004  -0.0002  -0.0005    -0.2680  -0.9996  -0.0003    -0.5260  -0.0002  -1.0003   det 1.000653
TL-1=UB[2]*UB[1]-1:   0.9993  -0.0002  -0.0005    -0.2677  -1.0003   0.0004    -0.5254   0.0003  -0.9995   det 0.999348
Rot= 179.9827 deg around the following vectors: 
Reciprocal space (hkl): 0.9591 -0.1285 -0.2523
Direct space (uvw)    : 1.0000 -0.0012 0.0025
 
DC PROFFITRRPTWIN INFO: Step 3 - Loading reflections of 2 components
 
DC PROFFITRRPTWIN ALL INFO: Component 1
DC PROFFITRRPTWIN INFO: Face list of component 1 
  1:   0.3454   2.5188  -8.0471  d=   0.0141
  2:  -0.0776  -4.8609  -4.0418  d=   0.0207
  3:   4.5627   0.1502  -2.0533  d=   0.0757
  4:   0.0776   4.8609   4.0418  d=   0.0155
  5:  -4.3525  -1.6165   0.7225  d=   0.0590
  6:  -0.0024  -5.0015   7.9962  d=   0.0151
  7:   0.9961  -6.9948  -1.9952  d=   0.0405
  8:  -0.0019  -4.0023   7.9958  d=   0.0125
  9:   3.9968  -1.0041   1.0040  d=   0.0714
 10:   0.0024   5.0015  -7.9962  d=   0.0135
DC PROFFITRRPTWIN ALL INFO: Component 2
DC PROFFITRRPTWIN INFO: Face list of component 2 
  1:   0.3483  -2.6151   7.8621  d=   0.0141
  2:  -0.0746   4.8816   4.0788  d=   0.0207
  3:   4.5604  -1.3726  -0.3451  d=   0.0757
  4:   0.0746  -4.8816  -4.0788  d=   0.0155
  5:  -4.3494   2.7826   1.5643  d=   0.0590
  6:  -0.0049   5.0067  -7.9921  d=   0.0151
  7:   0.9980   6.7294   1.4685  d=   0.0405
  8:  -0.0047   4.0070  -7.9917  d=   0.0125
  9:   3.9937  -0.0653  -3.1038  d=   0.0714
 10:   0.0049  -5.0067   7.9921  d=   0.0135
 
DC PROFFITRRPTWIN INFO: Step 4 - Analysing composite reflections of 2 components
 
Component 1: 13120 observations read
Component 2: 13141 observations read

23995 composite observations collected (21796 fully isolated, 2199 overlapped), 58 skipped due to one or more missing parts


OVERLAP STATISTICS

2 COMPONENTS

COMPONENTS 1, 2
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |        872 |     3.6 <--- ALMOST SEPARATED
   0.20 - 0.40  |         72 |     0.3
   0.40 - 0.60  |          3 |     0.0
   0.60 - 0.80  |         21 |     0.1
   0.80 - 1.00  |       1231 |     5.1 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |       2199 |     9.2

 
DC PROFFITRRPTWIN INFO: Step 5 - Scaling data & analysing twin ratios of 2 components
 
Computed twin ratios:
Twin 1: 87.90% (6829 common observations, 2077 merged)
Twin 2: 12.10% (5823 common observations, 2077 merged)

Preparing data for SCALE3 ABSPACK...

SCALING COMPONENT 1

11830 of 13087 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-619174.0625 max=4319006.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=380.6988 max=15293.3662


SCALING COMPONENT 2

11851 of 13107 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-835853.4375 max=4319006.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=312.3031 max=15293.3662

Computed twin ratios:
Twin 1: 87.98% (6829 common observations, 2077 merged)
Twin 2: 12.02% (5823 common observations, 2077 merged)

DC PROFFITRRPTWIN INFO: Determining HKLF4 overlap threshold for completeness requirement (>=80.0%)
DC PROFFITRRPTWIN INFO: HKLF4 overlap threshold kept - 0.40

DC PROFFITRRPTWIN INFO: Step 6 - Decomposed intensities statistics (HKLF4)
 
COMPONENT 1

 
Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only!
	Mean F2 and F2/sig(F2) are given for all measured values!
Note: The RsigmaA values are computed for all measured values!

Help: For more information about computations of rint and rsigma please look into Crysalis help: 
 file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html
 

Statistics vs intensity - point group symmetry: P-1
                       #        #        #      average    mean      mean        
          intensity measured   kept    unique  redundancy   F2     F2/sig(F2)   Rint   Rsigma
---------------------------------------------------------------------------------------------
   4286979-   176534     1208     1208      358    3.4    333844.08    60.94    0.015    0.016
    176037-   106046     1248     1248      358    3.5    135033.71    41.83    0.019    0.021
    105996-    75881     1255     1255      358    3.5     89502.66    36.45    0.024    0.026
     75845-    54789     1169     1169      358    3.3     64756.02    31.37    0.027    0.029
     54768-    39257     1169     1169      358    3.3     46429.85    27.00    0.030    0.033
     39183-    26533     1183     1183      358    3.3     32650.20    21.21    0.037    0.039
     26522-    16018     1109     1109      358    3.1     21075.45    15.79    0.044    0.046
     16015-     7911     1158     1158      358    3.2     11984.56     9.93    0.065    0.067
      7894-     2548     1149     1149      358    3.2      4940.42     4.67    0.111    0.115
      2539-    -4884     1182     1182      367    3.2      1033.14     1.06    0.383    0.428
-------------------------------------------------------------------------------------------
   4286979-    -4884    11830    11830     3589    3.3     75814.16    25.40    0.023    0.024
 

Statistics vs resolution - point group symmetry: P-1
resolu-      #        #        #               average    mean      mean          
tion(A)   measured   kept    unique           redundancy   F2     F2/sig(F2)   Rint   Rsigma   RsigmaA
------------------------------------------------------------------------------------------------------
 inf-1.68     1171     1171      358             3.3    214006.93    41.86    0.015    0.016     0.018
1.68-1.36      881      881      358             2.5    117392.24    21.71    0.024    0.025     0.035
1.36-1.19     1769     1769      358             4.9     85529.07    24.26    0.028    0.032     0.034
1.19-1.09     1495     1495      358             4.2     63432.14    22.72    0.026    0.028     0.035
1.09-1.01     1286     1286      358             3.6     62073.63    24.47    0.021    0.023     0.033
1.01-0.96     1216     1216      358             3.4     53189.79    23.63    0.021    0.024     0.035
0.96-0.91     1154     1154      358             3.2     48060.02    23.41    0.027    0.029     0.035
0.91-0.87     1082     1082      358             3.0     36424.26    22.15    0.026    0.028     0.038
0.87-0.84      957      957      358             2.7     34051.40    23.97    0.029    0.031     0.035
0.84-0.81      819      819      367             2.2     30231.86    26.09    0.029    0.031     0.032
------------------------------------------------------------------------------------------------------
 inf-0.81    11830    11830     3589             3.3     75814.16    25.40    0.023    0.024     0.030
 

Statistics vs resolution (taking redundancy into account) - point group symmetry: P-1
resolu-      #        #        #       %       average    mean      mean          
tion(A)    kept     theory   unique complete  redundancy   F2     F2/sig(F2)   Rint  RsigmaB
--------------------------------------------------------------------------------------------
 inf-1.68     1171      438      358   81.7      3.3    214006.93    76.80    0.015    0.010
1.68-1.36      881      400      358   89.5      2.5    117392.24    35.26    0.024    0.022
1.36-1.19     1769      395      358   90.6      4.9     85529.07    49.61    0.028    0.017
1.19-1.09     1495      387      358   92.5      4.2     63432.14    45.29    0.026    0.017
1.09-1.01     1286      387      358   92.5      3.6     62073.63    48.08    0.021    0.018
1.01-0.96     1216      381      358   94.0      3.4     53189.79    44.95    0.021    0.019
0.96-0.91     1154      386      358   92.7      3.2     48060.02    44.21    0.027    0.020
0.91-0.87     1082      384      358   93.2      3.0     36424.26    40.55    0.026    0.022
0.87-0.84      957      380      358   94.2      2.7     34051.40    41.37    0.029    0.022
0.84-0.81      819      405      367   90.6      2.2     30231.86    41.38    0.029    0.021
--------------------------------------------------------------------------------------------
 inf-0.81    11830     3944     3589   91.0      3.3     75814.16    47.45    0.023    0.017
DC PROFFITRRPTWIN INFO: Step 7 - Generating output files
 
HKLF 4
Reflections read=13087, from those 11830 with overlapping factor < 0.400 written to file D:\Data\xs1926a\twin_abs_twin1_hklf4.hkl, 1257 skipped
Use the HKLF 4 file(s) for structure solution.

HKLF 5 merged
RINT ANALYSIS FOR ALL HKLF5 REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2          13087     12084      4358     2.77     25.85     0.017     0.031

RINT ANALYSIS FOR OVERLAPPED REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2           2199      1882       876     2.15     28.07     0.021     0.032

RINT ANALYSIS FOR ISOLATED REFLECTIONS
 Component measured     kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
     1       10888     10202      3482     2.93     25.22     0.017     0.031
     2           0         0         0     0.00      0.00     0.000     0.000

4358 merged reflections saved into file: D:\Data\xs1926a\twin_abs_twin1_hklf5.hkl

Use this hkl file in SHELXL with BASF instruction, which has (components minus 1) entries, and HKLF 5 instruction.
E.g. Two component twin: 'BASF n2' in .ins file, BASF n1 can be computed as n1 = 1.0 - n2.
E.g. Three component twin: 'BASF n2 n3' in .ins file, BASF n1 can be computed as n1 = 1.0 - (n2 + n3).

BASF 0.12024 
;
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.773
_oxdiff_exptl_absorpt_empirical_full_max 1.438
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_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_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 0.20900(2) 0.45335(2) 0.51582(2) 0.01411(5) Uani 1 1 d . . . . .
C1 C 0.1538(3) 0.5129(2) 0.77122(19) 0.0196(4) Uani 1 1 d . . . . .
H1 H 0.155160 0.591549 0.778343 0.024 Uiso 1 1 calc R U . A 1
C2 C 0.1339(3) 0.4859(2) 0.86801(19) 0.0227(4) Uani 1 1 d . . . . .
H2 H 0.125189 0.545314 0.940134 0.027 Uiso 1 1 calc R U . . .
C3 C 0.1269(3) 0.3715(2) 0.8580(2) 0.0249(5) Uani 1 1 d . . . . .
H3 H 0.113285 0.350860 0.922927 0.030 Uiso 1 1 calc R U . . .
C4 C 0.1401(3) 0.2872(2) 0.7513(2) 0.0234(4) Uani 1 1 d . . . . .
H4 H 0.134116 0.207933 0.742499 0.028 Uiso 1 1 calc R U . . .
C5 C 0.1620(3) 0.31871(19) 0.65734(19) 0.0188(4) Uani 1 1 d . . . . .
C6 C 0.1721(3) 0.2322(2) 0.54133(19) 0.0190(4) Uani 1 1 d . . . . .
C7 C 0.1755(3) 0.1155(2) 0.5193(2) 0.0235(4) Uani 1 1 d . . . . .
H7 H 0.177539 0.086814 0.580404 0.028 Uiso 1 1 calc R U . . .
C8 C 0.1758(3) 0.0412(2) 0.4050(2) 0.0251(5) Uani 1 1 d . . . . .
H8 H 0.180330 -0.039329 0.387621 0.030 Uiso 1 1 calc R U . . .
C9 C 0.1696(3) 0.0835(2) 0.3171(2) 0.0246(5) Uani 1 1 d . . . . .
H9 H 0.166005 0.032410 0.238658 0.030 Uiso 1 1 calc R U . . .
C10 C 0.1686(3) 0.20375(19) 0.34489(19) 0.0187(4) Uani 1 1 d . . . . .
C11 C 0.0831(4) 0.1597(2) 0.1355(2) 0.0280(5) Uani 1 1 d . . . . .
H11A H 0.186859 0.118005 0.104132 0.042 Uiso 1 1 calc R U . . .
H11B H 0.031077 0.199605 0.084957 0.042 Uiso 1 1 calc R U . . .
H11C H -0.019904 0.104268 0.138175 0.042 Uiso 1 1 calc R U . . .
C12 C 0.2389(3) 0.3558(2) 0.26262(19) 0.0196(4) Uani 1 1 d . . . . .
C13 C 0.2998(3) 0.3646(2) 0.16316(19) 0.0239(5) Uani 1 1 d . . . . .
H13 H 0.300320 0.296410 0.096547 0.029 Uiso 1 1 calc R U . . .
C14 C 0.3582(3) 0.4721(2) 0.1630(2) 0.0249(5) Uani 1 1 d . . . . .
H14 H 0.400046 0.478258 0.096423 0.030 Uiso 1 1 calc R U . . .
C15 C 0.3562(3) 0.5717(2) 0.2598(2) 0.0221(4) Uani 1 1 d . . . . .
H15 H 0.388405 0.646677 0.258753 0.026 Uiso 1 1 calc R U . . .
C16 C 0.3061(3) 0.5593(2) 0.35850(19) 0.0184(4) Uani 1 1 d . . . . .
C17 C 0.3097(3) 0.65635(19) 0.46898(19) 0.0183(4) Uani 1 1 d . . . . .
C18 C 0.3455(3) 0.7725(2) 0.4805(2) 0.0235(4) Uani 1 1 d . . . . .
H18 H 0.361859 0.790563 0.414451 0.028 Uiso 1 1 calc R U . . .
C19 C 0.3569(3) 0.8609(2) 0.5890(2) 0.0263(5) Uani 1 1 d . . . . .
H19 H 0.377342 0.939999 0.597230 0.032 Uiso 1 1 calc R U . . .
C20 C 0.3384(3) 0.8332(2) 0.6853(2) 0.0260(5) Uani 1 1 d . . . . .
H20 H 0.351371 0.893373 0.760413 0.031 Uiso 1 1 calc R U . . .
C21 C 0.3007(3) 0.7174(2) 0.6724(2) 0.0219(4) Uani 1 1 d . . . . .
H21 H 0.290064 0.699938 0.739513 0.026 Uiso 1 1 calc R U . B 1
N1 N 0.1713(2) 0.43252(17) 0.66758(16) 0.0165(4) Uani 0.82(3) 1 d . . P C 1
C22 C 0.2783(3) 0.62669(18) 0.56408(19) 0.0182(4) Uani 0.82(3) 1 d . . P C 1
N1' N 0.2783(3) 0.62669(18) 0.56408(19) 0.0182(4) Uani 0.18(3) 1 d . . P C 2
C22' C 0.1713(2) 0.43252(17) 0.66758(16) 0.0165(4) Uani 0.18(3) 1 d . . P C 2
N2 N 0.1713(2) 0.27573(16) 0.45559(16) 0.0176(3) Uani 1 1 d . . . . .
N3 N 0.1605(3) 0.24645(17) 0.25556(16) 0.0210(4) Uani 1 1 d . . . . .
N4 N 0.2511(2) 0.45225(16) 0.35972(15) 0.0166(3) Uani 1 1 d . . . . .
P1 P 0.41387(8) 0.81757(5) 0.09295(5) 0.02077(12) Uani 1 1 d . . . . .
F1 F 0.1917(2) 0.78494(18) 0.09465(17) 0.0443(4) Uani 1 1 d . . . . .
F2 F 0.4521(3) 0.68812(13) 0.07896(14) 0.0363(3) Uani 1 1 d . . . . .
F3 F 0.6361(2) 0.84938(15) 0.09176(15) 0.0357(3) Uani 1 1 d . . . . .
F4 F 0.3758(2) 0.94600(13) 0.10608(14) 0.0354(3) Uani 1 1 d . . . . .
F5 F 0.3619(2) 0.77629(14) -0.04667(12) 0.0340(3) Uani 1 1 d . . . . .
F6 F 0.4653(3) 0.85767(15) 0.23302(13) 0.0381(4) Uani 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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N4 Pd1 N1' 82.33(8) . . ?
N4 Pd1 C22 82.33(8) . . ?
N4 Pd1 N2 92.04(7) . . ?
N1' Pd1 N2 171.96(8) . . ?
C22 Pd1 N2 171.96(8) . . ?
N4 Pd1 N1 172.67(7) . . ?
C22 Pd1 N1 104.52(8) . . ?
N2 Pd1 N1 80.88(7) . . ?
N4 Pd1 C22' 172.67(7) . . ?
N1' Pd1 C22' 104.52(8) . . ?
N2 Pd1 C22' 80.88(7) . . ?
C22' C1 C2 123.0(2) . . ?
N1 C1 C2 123.0(2) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.1(2) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 118.8(2) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C3 C4 C5 120.0(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C22' C5 C4 121.3(2) . . ?
N1 C5 C4 121.3(2) . . ?
C22' C5 C6 116.56(19) . . ?
N1 C5 C6 116.56(19) . . ?
C4 C5 C6 122.2(2) . . ?
N2 C6 C7 122.1(2) . . ?
N2 C6 C5 114.63(19) . . ?
C7 C6 C5 123.2(2) . . ?
C6 C7 C8 118.0(2) . . ?
C6 C7 H7 121.0 . . ?
C8 C7 H7 121.0 . . ?
C9 C8 C7 120.4(2) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 119.1(2) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 N3 120.5(2) . . ?
N2 C10 C9 120.4(2) . . ?
N3 C10 C9 119.1(2) . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 N3 121.8(2) . . ?
N4 C12 C13 119.7(2) . . ?
N3 C12 C13 118.5(2) . . ?
C14 C13 C12 119.8(2) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 120.1(2) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C16 118.4(2) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
N4 C16 C15 121.5(2) . . ?
N4 C16 C17 114.27(19) . . ?
C15 C16 C17 124.2(2) . . ?
C18 C17 N1' 121.6(2) . . ?
C18 C17 C22 121.6(2) . . ?
C18 C17 C16 122.1(2) . . ?
N1' C17 C16 116.28(19) . . ?
C22 C17 C16 116.28(19) . . ?
C19 C18 C17 119.6(2) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C20 C19 C18 119.6(2) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 120.2(2) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
N1' C21 C20 121.9(2) . . ?
C22 C21 C20 121.9(2) . . ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
C1 N1 C5 117.82(19) . . ?
C1 N1 Pd1 129.51(16) . . ?
C5 N1 Pd1 112.67(14) . . ?
C21 C22 C17 116.9(2) . . ?
C21 C22 Pd1 131.16(17) . . ?
C17 C22 Pd1 111.90(15) . . ?
C21 N1' C17 116.9(2) . . ?
C21 N1' Pd1 131.16(17) . . ?
C17 N1' Pd1 111.90(15) . . ?
C1 C22' C5 117.82(19) . . ?
C1 C22' Pd1 129.51(16) . . ?
C5 C22' Pd1 112.67(14) . . ?
C10 N2 C6 119.85(19) . . ?
C10 N2 Pd1 125.57(15) . . ?
C6 N2 Pd1 114.12(15) . . ?
C10 N3 C12 128.24(19) . . ?
C10 N3 C11 115.4(2) . . ?
C12 N3 C11 115.74(19) . . ?
C12 N4 C16 120.09(19) . . ?
C12 N4 Pd1 124.94(15) . . ?
C16 N4 Pd1 114.86(14) . . ?
F4 P1 F3 90.51(9) . . ?
F4 P1 F5 90.03(9) . . ?
F3 P1 F5 90.39(9) . . ?
F4 P1 F1 89.90(10) . . ?
F3 P1 F1 179.52(10) . . ?
F5 P1 F1 89.85(10) . . ?
F4 P1 F2 179.68(9) . . ?
F3 P1 F2 89.45(9) . . ?
F5 P1 F2 89.66(9) . . ?
F1 P1 F2 90.14(10) . . ?
F4 P1 F6 90.49(9) . . ?
F3 P1 F6 89.89(9) . . ?
F5 P1 F6 179.41(10) . . ?
F1 P1 F6 89.87(10) . . ?
F2 P1 F6 89.82(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 N4 2.0096(18) . ?
Pd1 N1' 2.019(2) . ?
Pd1 C22 2.019(2) . ?
Pd1 N2 2.0435(18) . ?
Pd1 N1 2.0544(18) . ?
Pd1 C22' 2.0544(18) . ?
C1 C22' 1.349(3) . ?
C1 N1 1.349(3) . ?
C1 C2 1.389(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.380(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(3) . ?
C4 H4 0.9500 . ?
C5 C22' 1.371(3) . ?
C5 N1 1.371(3) . ?
C5 C6 1.474(3) . ?
C6 N2 1.362(3) . ?
C6 C7 1.380(3) . ?
C7 C8 1.391(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.373(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.410(3) . ?
C9 H9 0.9500 . ?
C10 N2 1.343(3) . ?
C10 N3 1.393(3) . ?
C11 N3 1.482(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N4 1.348(3) . ?
C12 N3 1.399(3) . ?
C12 C13 1.412(3) . ?
C13 C14 1.372(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(3) . ?
C15 H15 0.9500 . ?
C16 N4 1.367(3) . ?
C16 C17 1.462(3) . ?
C17 C18 1.400(3) . ?
C17 N1' 1.406(3) . ?
C17 C22 1.406(3) . ?
C18 C19 1.388(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.386(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.392(3) . ?
C20 H20 0.9500 . ?
C21 N1' 1.389(3) . ?
C21 C22 1.389(3) . ?
C21 H21 0.9500 . ?
P1 F4 1.5945(15) . ?
P1 F3 1.5981(16) . ?
P1 F5 1.5992(14) . ?
P1 F1 1.6010(17) . ?
P1 F2 1.6046(15) . ?
P1 F6 1.6056(15) . ?
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
C22' C1 C2 C3 -1.6(3) . . . . ?
N1 C1 C2 C3 -1.6(3) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C2 C3 C4 C5 0.7(3) . . . . ?
C3 C4 C5 C22' 0.1(3) . . . . ?
C3 C4 C5 N1 0.1(3) . . . . ?
C3 C4 C5 C6 -178.5(2) . . . . ?
C22' C5 C6 N2 -5.8(3) . . . . ?
N1 C5 C6 N2 -5.8(3) . . . . ?
C4 C5 C6 N2 172.81(19) . . . . ?
C22' C5 C6 C7 176.2(2) . . . . ?
N1 C5 C6 C7 176.2(2) . . . . ?
C4 C5 C6 C7 -5.1(3) . . . . ?
N2 C6 C7 C8 -0.8(3) . . . . ?
C5 C6 C7 C8 177.0(2) . . . . ?
C6 C7 C8 C9 -1.1(3) . . . . ?
C7 C8 C9 C10 1.8(3) . . . . ?
C8 C9 C10 N2 -0.8(3) . . . . ?
C8 C9 C10 N3 -179.4(2) . . . . ?
N4 C12 C13 C14 -4.5(3) . . . . ?
N3 C12 C13 C14 173.1(2) . . . . ?
C12 C13 C14 C15 -0.4(3) . . . . ?
C13 C14 C15 C16 4.1(3) . . . . ?
C14 C15 C16 N4 -3.0(3) . . . . ?
C14 C15 C16 C17 176.02(19) . . . . ?
N4 C16 C17 C18 -174.11(19) . . . . ?
C15 C16 C17 C18 6.8(3) . . . . ?
N4 C16 C17 N1' 6.9(3) . . . . ?
C15 C16 C17 N1' -172.1(2) . . . . ?
N4 C16 C17 C22 6.9(3) . . . . ?
C15 C16 C17 C22 -172.1(2) . . . . ?
N1' C17 C18 C19 2.2(3) . . . . ?
C22 C17 C18 C19 2.2(3) . . . . ?
C16 C17 C18 C19 -176.7(2) . . . . ?
C17 C18 C19 C20 1.9(3) . . . . ?
C18 C19 C20 C21 -2.6(4) . . . . ?
C19 C20 C21 N1' -0.8(4) . . . . ?
C19 C20 C21 C22 -0.8(4) . . . . ?
C2 C1 N1 C5 2.3(3) . . . . ?
C2 C1 N1 Pd1 -178.25(16) . . . . ?
C4 C5 N1 C1 -1.6(3) . . . . ?
C6 C5 N1 C1 177.10(18) . . . . ?
C4 C5 N1 Pd1 178.93(16) . . . . ?
C6 C5 N1 Pd1 -2.4(2) . . . . ?
C20 C21 C22 C17 4.6(3) . . . . ?
C20 C21 C22 Pd1 -176.05(17) . . . . ?
C18 C17 C22 C21 -5.3(3) . . . . ?
C16 C17 C22 C21 173.63(18) . . . . ?
C18 C17 C22 Pd1 175.23(16) . . . . ?
C16 C17 C22 Pd1 -5.8(2) . . . . ?
C20 C21 N1' C17 4.6(3) . . . . ?
C20 C21 N1' Pd1 -176.05(17) . . . . ?
C18 C17 N1' C21 -5.3(3) . . . . ?
C16 C17 N1' C21 173.63(18) . . . . ?
C18 C17 N1' Pd1 175.23(16) . . . . ?
C16 C17 N1' Pd1 -5.8(2) . . . . ?
C2 C1 C22' C5 2.3(3) . . . . ?
C2 C1 C22' Pd1 -178.25(16) . . . . ?
C4 C5 C22' C1 -1.6(3) . . . . ?
C6 C5 C22' C1 177.10(18) . . . . ?
C4 C5 C22' Pd1 178.93(16) . . . . ?
C6 C5 C22' Pd1 -2.4(2) . . . . ?
N3 C10 N2 C6 177.59(18) . . . . ?
C9 C10 N2 C6 -1.0(3) . . . . ?
N3 C10 N2 Pd1 -10.6(3) . . . . ?
C9 C10 N2 Pd1 170.75(15) . . . . ?
C7 C6 N2 C10 1.8(3) . . . . ?
C5 C6 N2 C10 -176.11(18) . . . . ?
C7 C6 N2 Pd1 -170.84(17) . . . . ?
C5 C6 N2 Pd1 11.2(2) . . . . ?
N2 C10 N3 C12 32.2(3) . . . . ?
C9 C10 N3 C12 -149.2(2) . . . . ?
N2 C10 N3 C11 -157.16(19) . . . . ?
C9 C10 N3 C11 21.5(3) . . . . ?
N4 C12 N3 C10 -33.3(3) . . . . ?
C13 C12 N3 C10 149.1(2) . . . . ?
N4 C12 N3 C11 156.10(19) . . . . ?
C13 C12 N3 C11 -21.5(3) . . . . ?
N3 C12 N4 C16 -171.88(18) . . . . ?
C13 C12 N4 C16 5.7(3) . . . . ?
N3 C12 N4 Pd1 12.0(3) . . . . ?
C13 C12 N4 Pd1 -170.41(15) . . . . ?
C15 C16 N4 C12 -2.0(3) . . . . ?
C17 C16 N4 C12 178.95(18) . . . . ?
C15 C16 N4 Pd1 174.50(16) . . . . ?
C17 C16 N4 Pd1 -4.6(2) . . . . ?
