#------------------------------------------------------------------------------
#$Date: 2024-05-04 04:52:50 +0300 (Sat, 04 May 2024) $
#$Revision: 291492 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023118.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_2023118
loop_
_publ_author_name
'Zakharchenko, Borys V.'
'Khomenko, Dmytro M.'
'Doroshchuk, Roman O.'
'Bargan, Alexandra'
'Vassilyeva, Olga Yu.'
'Lampeka, Rostyslav D.'
_publ_section_title
;
Crystal structure of
bis{2-[5-(3,4,5-trimethoxyphenyl)-4H-1,2,4-triazol-3-yl]pyridine}palladium(II)
bis(trifluoroacetate) trifluoroacetic acid disolvate
;
_journal_coeditor_code JW2005
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S205698902400392X
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac
'[Pd (C16 H16 N4 O3)2] (C2 F3 O2)2, 2C2 H F3 O2'
_chemical_formula_moiety
'C32 H32 N8 O6 Pd 2+, 2(C2 F3 O2 -), 2(C2 H F3 O2)'
_chemical_formula_sum 'C40 H34 F12 N8 O14 Pd'
_chemical_formula_weight 1185.15
_chemical_name_systematic
'Bis{2-[5-(3,4,5-trimethoxyphenyl)-4H-1,2,4-triazol-3-yl]pyridine}palladium(II) bis(trifluoroacetate) trifluoroacetic acid disolvate'
_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 mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 93.384(4)
_cell_angle_beta 98.121(3)
_cell_angle_gamma 94.090(4)
_cell_formula_units_Z 1
_cell_length_a 8.6173(4)
_cell_length_b 10.6265(6)
_cell_length_c 13.1312(4)
_cell_measurement_reflns_used 3996
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.8300
_cell_measurement_theta_min 1.6200
_cell_volume 1184.45(9)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0260
_diffrn_reflns_av_unetI/netI 0.0490
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 9462
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 26.728
_diffrn_reflns_theta_min 1.926
_diffrn_standards_decay_% ' '
_diffrn_standards_interval_count ' '
_diffrn_standards_interval_time ' '
_diffrn_standards_number ' '
_exptl_absorpt_coefficient_mu 0.513
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.96779
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour 'clear light yellow'
_exptl_crystal_density_diffrn 1.662
_exptl_crystal_description irregular
_exptl_crystal_F_000 596
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.3
_refine_diff_density_max 0.386
_refine_diff_density_min -0.454
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 444
_refine_ls_number_reflns 5010
_refine_ls_number_restraints 382
_refine_ls_restrained_S_all 1.101
_refine_ls_R_factor_all 0.0466
_refine_ls_R_factor_gt 0.0415
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.5877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0910
_refine_ls_wR_factor_ref 0.0953
_reflns_number_gt 4615
_reflns_number_total 5010
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jw2005.cif
_cod_data_source_block I
_cod_original_cell_volume 1184.46(9)
_cod_database_code 2023118
_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 0.821
_shelx_estimated_absorpt_t_max 0.861
_shelx_hkl_file
;
-10 -4 -2 0.92 1.23
-10 -4 -1 1.87 1.80
-10 -4 0 7.94 2.69
-10 -4 1 9.28 2.73
-10 -4 2 23.65 4.25
-10 -4 3 8.51 2.73
-10 -4 4 2.08 1.68
-10 -3 -4 2.95 1.75
-10 -3 -3 0.30 1.39
-10 -3 -2 2.96 1.97
-10 -3 -1 14.75 3.36
-10 -3 0 11.09 2.93
-10 -3 1 10.93 2.96
-10 -3 2 8.55 2.85
-10 -3 3 7.59 2.76
-10 -3 4 1.28 1.70
-10 -3 5 8.79 2.70
-10 -3 6 16.72 3.60
-10 -3 7 5.41 2.43
-10 -2 -5 1.26 1.48
-10 -2 -4 2.51 1.81
-10 -2 -3 1.72 1.66
-10 -2 -2 8.52 2.76
-10 -2 -1 6.22 2.29
-10 -2 0 5.44 2.28
-10 -2 1 9.63 2.69
-10 -2 2 16.76 3.66
-10 -2 3 17.52 3.56
-10 -2 4 45.77 5.69
-10 -2 5 29.78 4.59
-10 -2 6 30.47 4.74
-10 -2 7 29.88 4.63
-10 -2 8 16.00 3.64
-10 -1 -5 4.43 2.29
-10 -1 -4 14.77 3.35
-10 -1 -3 18.95 3.90
-10 -1 -2 8.48 2.75
-10 -1 -1 5.56 2.19
-10 -1 0 8.27 2.68
-10 -1 1 8.86 2.84
-10 -1 2 5.93 2.50
-10 -1 3 8.12 2.58
-10 -1 4 7.11 2.55
-10 -1 5 2.19 1.77
-10 -1 6 3.27 1.72
-10 -1 7 8.91 2.70
-10 -1 8 11.07 2.88
-10 -1 9 5.08 1.94
-10 -1 10 9.32 2.88
-10 0 -7 7.38 2.56
-10 0 -5 0.24 1.07
-10 0 -4 1.88 1.57
-10 0 -3 1.42 1.89
-10 0 -2 -0.36 1.44
-10 0 -1 2.44 1.95
-10 0 0 -0.15 1.67
-10 0 1 8.86 2.77
-10 0 2 1.72 1.48
-10 0 3 12.96 2.92
-10 0 4 6.23 2.20
-10 0 5 0.67 1.34
-10 0 6 2.34 1.38
-10 0 7 10.71 2.76
-10 0 8 0.09 1.29
-10 0 9 6.16 2.21
-10 0 10 2.14 1.61
-10 0 11 2.36 1.72
-10 1 -7 0.23 1.14
-10 1 -6 6.42 2.33
-10 1 -5 6.56 2.41
-10 1 -5 6.79 2.67
-10 1 -4 3.90 1.91
-10 1 -4 4.44 2.01
-10 1 -3 6.58 2.56
-10 1 -3 5.27 2.18
-10 1 -2 1.17 1.36
-10 1 -2 1.81 1.34
-10 1 -1 -0.09 1.47
-10 1 0 6.00 2.36
-10 1 1 16.73 3.59
-10 1 2 24.08 4.00
-10 1 3 24.73 4.09
-10 1 4 3.97 1.89
-10 1 5 -3.49 1.81
-10 1 6 6.10 2.24
-10 1 7 15.67 3.26
-10 1 8 28.62 4.25
-10 1 9 9.91 2.74
-10 1 10 18.03 3.47
-10 1 11 0.58 1.59
-10 2 -6 -2.35 1.77
-10 2 -5 0.29 1.61
-10 2 -4 7.37 2.56
-10 2 -4 0.10 1.64
-10 2 -3 3.74 2.25
-10 2 -3 0.12 1.33
-10 2 -2 5.83 2.39
-10 2 -2 8.45 2.76
-10 2 -1 5.29 2.33
-10 2 -1 12.35 3.07
-10 2 0 22.70 4.04
-10 2 0 27.56 4.39
-10 2 1 15.87 3.54
-10 2 2 27.18 4.39
-10 2 3 9.56 2.73
-10 2 4 1.89 1.68
-10 2 5 0.92 1.25
-10 2 6 14.85 3.33
-10 2 7 20.75 3.77
-10 2 8 15.29 3.31
-10 2 9 17.23 3.41
-10 2 10 7.15 2.45
-10 3 -5 1.98 1.76
-10 3 -4 5.75 2.30
-10 3 -3 -0.13 1.27
-10 3 -2 2.29 1.89
-10 3 -1 1.28 1.37
-10 3 0 1.27 1.58
-10 3 0 6.04 2.36
-10 3 1 0.21 1.50
-10 3 1 0.72 1.44
-10 3 2 2.00 1.70
-10 3 3 2.15 1.46
-10 3 4 3.21 1.85
-10 3 5 14.53 3.26
-10 3 6 24.47 4.10
-10 3 7 15.92 3.37
-10 3 8 14.91 3.31
-10 3 9 17.20 3.42
-10 3 10 4.93 2.07
-10 4 -3 6.14 2.28
-10 4 -2 7.59 2.62
-10 4 -1 11.94 3.18
-10 4 0 12.28 3.08
-10 4 1 14.02 3.33
-10 4 2 12.56 3.05
-10 4 2 5.97 2.53
-10 4 3 13.21 3.25
-10 4 4 9.64 2.57
-10 4 5 7.43 2.42
-10 4 6 2.39 1.59
-10 4 7 4.09 1.92
-10 4 8 6.39 2.14
-10 4 9 4.76 1.85
-10 5 -1 10.37 2.99
-10 5 0 6.78 2.51
-10 5 1 7.24 2.30
-10 5 2 10.01 3.11
-10 5 3 7.15 2.51
-10 5 3 9.71 2.80
-10 5 4 6.57 2.23
-10 5 5 5.48 2.30
-10 5 6 6.04 2.35
-10 5 7 8.85 2.51
-10 5 8 7.26 2.41
-10 6 1 5.32 2.34
-10 6 2 6.04 2.59
-10 6 3 7.99 2.69
-10 6 4 5.78 2.26
-10 6 4 4.80 2.25
-10 6 5 -0.04 1.05
-10 6 6 1.52 1.12
-10 6 7 15.26 3.37
-10 6 8 17.51 3.58
-10 7 5 -0.46 1.10
-10 7 6 4.40 1.93
-10 7 7 4.45 2.30
-9 -7 -4 12.24 3.03
-9 -7 -3 7.38 2.38
-9 -7 -2 12.95 3.20
-9 -7 -1 5.52 2.41
-9 -7 0 8.48 2.65
-9 -7 1 5.96 2.36
-9 -6 -5 5.82 2.19
-9 -6 -4 21.21 3.84
-9 -6 -3 31.22 4.58
-9 -6 -2 11.86 2.92
-9 -6 -1 4.40 2.33
-9 -6 0 5.50 2.15
-9 -6 1 10.74 2.95
-9 -6 2 11.41 3.20
-9 -6 3 7.07 2.46
-9 -6 4 12.46 3.13
-9 -6 5 15.44 3.44
-9 -6 6 8.83 3.07
-9 -5 -6 4.99 2.08
-9 -5 -5 1.61 1.63
-9 -5 -4 7.92 2.48
-9 -5 -3 15.17 3.35
-9 -5 -2 1.11 1.31
-9 -5 -1 2.68 1.74
-9 -5 0 7.77 2.43
-9 -5 1 3.28 1.63
-9 -5 2 8.93 2.74
-9 -5 3 26.12 4.36
-9 -5 4 14.38 3.36
-9 -5 5 21.85 3.99
-9 -5 6 24.06 4.25
-9 -5 7 12.94 3.30
-9 -5 8 11.86 3.10
-9 -4 -6 9.21 2.64
-9 -4 -5 4.96 2.13
-9 -4 -4 18.23 3.40
-9 -4 -3 10.41 2.79
-9 -4 -2 -0.35 1.01
-9 -4 -1 1.13 1.15
-9 -4 0 4.74 2.09
-9 -4 1 22.91 3.99
-9 -4 2 31.81 4.58
-9 -4 3 36.41 4.91
-9 -4 4 37.19 4.93
-9 -4 5 9.64 2.61
-9 -4 6 8.74 2.53
-9 -4 7 11.40 2.94
-9 -4 8 15.78 3.47
-9 -4 9 7.61 2.61
-9 -4 10 8.26 2.73
-9 -3 -7 3.83 2.00
-9 -3 -6 3.17 1.82
-9 -3 -5 4.65 1.86
-9 -3 -4 7.80 2.46
-9 -3 -3 7.01 2.32
-9 -3 -2 14.92 3.17
-9 -3 -1 25.08 3.97
-9 -3 0 26.22 4.06
-9 -3 1 15.78 3.20
-9 -3 2 23.16 3.87
-9 -3 3 8.87 2.67
-9 -3 4 -0.24 1.26
-9 -3 5 -1.40 1.29
-9 -3 6 4.82 2.06
-9 -3 7 10.02 2.84
-9 -3 8 20.73 3.86
-9 -3 9 15.87 3.33
-9 -3 10 14.17 3.35
-9 -3 11 35.39 5.23
-9 -2 -8 -1.05 1.24
-9 -2 -7 1.55 1.51
-9 -2 -6 6.31 2.12
-9 -2 -5 7.89 2.37
-9 -2 -4 8.94 2.38
-9 -2 -3 15.10 3.35
-9 -2 -2 10.94 2.72
-9 -2 -1 19.56 3.52
-9 -2 0 5.73 2.21
-9 -2 1 42.24 5.06
-9 -2 2 17.49 3.33
-9 -2 3 49.06 5.49
-9 -2 4 66.14 6.30
-9 -2 5 75.82 6.79
-9 -2 6 32.53 4.57
-9 -2 7 23.73 3.91
-9 -2 8 17.81 3.52
-9 -2 9 18.56 3.68
-9 -2 10 7.90 2.54
-9 -2 11 14.58 3.19
-9 -2 12 14.87 3.40
-9 -2 13 6.61 2.62
-9 -1 -9 2.59 1.47
-9 -1 -8 2.19 1.62
-9 -1 -7 2.87 1.63
-9 -1 -6 10.39 2.74
-9 -1 -5 9.80 2.68
-9 -1 -4 5.78 2.15
-9 -1 -3 8.33 2.52
-9 -1 -2 5.69 2.11
-9 -1 -1 6.48 2.00
-9 -1 0 4.61 1.97
-9 -1 1 2.57 1.75
-9 -1 2 17.87 3.42
-9 -1 3 21.75 3.62
-9 -1 4 18.27 3.31
-9 -1 5 11.60 2.65
-9 -1 6 -4.61 1.84
-9 -1 7 3.27 1.84
-9 -1 8 17.49 3.34
-9 -1 9 7.32 2.31
-9 -1 10 18.04 3.45
-9 -1 11 10.18 2.72
-9 -1 12 1.39 1.58
-9 0 -9 3.49 1.86
-9 0 -8 8.40 2.66
-9 0 -8 10.80 2.72
-9 0 -7 12.39 2.95
-9 0 -7 12.12 3.07
-9 0 -6 6.41 1.96
-9 0 -6 10.17 2.56
-9 0 -5 4.89 1.97
-9 0 -5 6.57 2.22
-9 0 -4 15.52 3.16
-9 0 -4 9.98 2.71
-9 0 -3 15.59 3.05
-9 0 -3 12.43 3.13
-9 0 -2 23.59 3.93
-9 0 -1 -2.39 1.52
-9 0 0 10.00 2.57
-9 0 1 7.95 2.17
-9 0 2 7.41 2.41
-9 0 3 13.65 2.91
-9 0 4 22.57 3.77
-9 0 5 3.24 1.64
-9 0 6 3.63 1.71
-9 0 7 10.91 2.63
-9 0 8 36.71 4.72
-9 0 9 10.16 2.68
-9 0 10 6.20 2.18
-9 0 11 9.42 2.51
-9 0 12 7.51 2.43
-9 1 -9 1.70 1.42
-9 1 -9 -0.46 1.19
-9 1 -8 5.07 2.16
-9 1 -8 2.81 1.45
-9 1 -7 5.30 2.06
-9 1 -7 4.83 2.09
-9 1 -6 4.68 2.01
-9 1 -6 4.96 2.09
-9 1 -5 10.67 2.71
-9 1 -5 9.09 2.61
-9 1 -4 20.80 3.84
-9 1 -4 14.66 3.06
-9 1 -3 6.81 2.29
-9 1 -3 5.70 2.31
-9 1 -2 10.45 2.69
-9 1 -2 5.94 2.41
-9 1 -1 3.74 1.48
-9 1 -1 3.91 1.86
-9 1 0 7.24 2.44
-9 1 1 6.37 2.04
-9 1 2 22.11 3.67
-9 1 3 20.26 3.52
-9 1 4 21.53 3.52
-9 1 5 2.51 1.67
-9 1 6 3.02 1.65
-9 1 7 15.85 3.04
-9 1 8 9.47 2.58
-9 1 9 9.06 2.55
-9 1 10 26.77 4.02
-9 1 11 8.40 2.35
-9 2 -9 1.92 1.62
-9 2 -8 3.06 1.87
-9 2 -7 2.58 1.16
-9 2 -6 4.94 2.00
-9 2 -5 0.42 1.47
-9 2 -4 2.82 1.77
-9 2 -3 15.14 3.21
-9 2 -2 3.74 1.64
-9 2 -1 15.31 3.08
-9 2 0 27.49 4.26
-9 2 0 28.08 4.17
-9 2 1 38.49 4.74
-9 2 1 29.71 4.30
-9 2 2 36.25 4.61
-9 2 3 29.52 4.21
-9 2 4 11.35 2.87
-9 2 5 4.06 1.61
-9 2 6 13.48 2.87
-9 2 7 54.99 5.56
-9 2 8 57.31 5.70
-9 2 9 51.36 5.36
-9 2 10 15.87 3.04
-9 2 11 21.80 3.55
-9 3 -8 -1.55 1.42
-9 3 -7 1.86 1.53
-9 3 -6 0.56 1.20
-9 3 -5 3.63 1.84
-9 3 -4 1.62 1.70
-9 3 -3 3.54 1.66
-9 3 -2 7.45 2.54
-9 3 -1 19.11 3.45
-9 3 0 12.41 3.03
-9 3 1 19.88 3.59
-9 3 2 12.17 2.82
-9 3 2 12.74 2.93
-9 3 3 12.39 2.85
-9 3 4 12.22 2.81
-9 3 5 14.49 3.03
-9 3 6 28.38 3.98
-9 3 7 26.32 3.79
-9 3 8 4.82 1.92
-9 3 9 6.71 2.14
-9 3 10 10.80 2.63
-9 4 -7 25.39 4.24
-9 4 -6 44.63 5.62
-9 4 -5 26.59 4.34
-9 4 -4 24.46 4.07
-9 4 -3 15.18 3.33
-9 4 -2 11.41 2.86
-9 4 -1 13.83 3.02
-9 4 0 21.55 3.75
-9 4 1 16.23 3.37
-9 4 2 11.32 2.78
-9 4 3 10.31 2.73
-9 4 3 16.81 3.37
-9 4 4 35.71 4.66
-9 4 5 13.91 2.90
-9 4 6 4.61 1.97
-9 4 7 -2.19 1.52
-9 4 8 5.76 1.93
-9 4 9 7.70 2.26
-9 5 -6 12.75 3.21
-9 5 -5 6.65 2.54
-9 5 -4 2.52 1.72
-9 5 -3 0.72 1.30
-9 5 -2 9.11 2.64
-9 5 -1 8.79 2.74
-9 5 0 20.19 3.66
-9 5 1 10.23 2.91
-9 5 2 6.38 2.27
-9 5 3 10.31 2.73
-9 5 4 3.43 1.63
-9 5 5 1.47 1.51
-9 5 6 0.53 0.99
-9 5 7 10.36 2.59
-9 5 8 9.51 2.42
-9 5 9 21.54 3.55
-9 6 -5 5.91 2.33
-9 6 -4 3.68 2.04
-9 6 -3 4.72 2.03
-9 6 -2 3.07 1.99
-9 6 -1 3.29 1.88
-9 6 0 4.42 2.07
-9 6 1 3.56 1.85
-9 6 2 3.81 1.85
-9 6 3 13.50 3.12
-9 6 4 31.98 4.62
-9 6 5 52.08 5.77
-9 6 6 24.43 3.82
-9 6 7 30.50 4.30
-9 6 8 37.30 4.60
-9 7 -3 0.50 1.39
-9 7 -2 3.48 1.94
-9 7 -1 5.63 2.28
-9 7 0 2.04 1.66
-9 7 1 8.35 2.73
-9 7 2 5.83 2.30
-9 7 3 7.72 2.50
-9 7 4 -0.18 1.40
-9 7 5 0.85 1.46
-9 7 6 3.83 1.99
-9 7 7 2.10 1.48
-9 8 -1 9.44 2.95
-9 8 0 8.71 2.66
-9 8 1 20.09 3.85
-9 8 2 21.54 3.96
-9 8 3 3.04 1.99
-9 8 4 12.36 3.08
-9 8 5 11.55 3.03
-9 8 6 17.18 3.47
-9 9 3 9.29 2.71
-9 9 4 3.26 1.88
-9 9 5 16.03 3.54
-9 9 6 10.47 2.83
-8 -9 -3 9.34 2.81
-8 -9 -2 9.03 2.77
-8 -9 -1 7.51 2.76
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7 -4 5 30.66 3.22
7 -4 6 26.23 3.12
7 -4 7 11.52 2.35
7 -4 8 2.71 1.31
7 -4 9 1.77 1.33
7 -4 10 7.41 2.25
7 -4 11 7.93 2.32
7 -4 12 5.93 2.39
7 -3 -14 11.78 2.87
7 -3 -13 16.73 3.27
7 -3 -12 6.37 2.29
7 -3 -11 27.42 3.83
7 -3 -10 33.94 4.20
7 -3 -9 8.00 2.16
7 -3 -8 -0.45 1.13
7 -3 -7 10.92 2.45
7 -3 -6 92.83 6.46
7 -3 -5 72.85 5.55
7 -3 -4 8.45 2.11
7 -3 -3 58.49 4.78
7 -3 -2 36.23 3.78
7 -3 -1 43.60 2.67
7 -3 -1 46.39 4.18
7 -3 0 31.56 2.39
7 -3 0 25.74 3.10
7 -3 0 26.59 2.14
7 -3 1 42.01 2.90
7 -3 1 43.87 3.99
7 -3 1 36.67 2.68
7 -3 2 83.76 4.31
7 -3 3 90.33 4.76
7 -3 4 127.21 6.01
7 -3 5 193.71 7.97
7 -3 6 46.45 4.03
7 -3 7 2.06 1.16
7 -3 8 0.78 0.94
7 -3 9 5.14 1.73
7 -3 10 0.70 1.11
7 -3 11 4.84 1.98
7 -3 12 5.37 1.89
7 -2 -15 9.88 2.70
7 -2 -14 13.06 2.97
7 -2 -13 12.51 2.88
7 -2 -12 14.40 2.94
7 -2 -11 29.12 3.96
7 -2 -10 14.64 2.72
7 -2 -9 24.13 3.49
7 -2 -8 44.67 4.59
7 -2 -7 98.61 6.64
7 -2 -6 -0.83 1.25
7 -2 -5 58.78 4.91
7 -2 -4 11.12 2.22
7 -2 -3 11.91 2.33
7 -2 -2 35.78 1.96
7 -2 -2 36.14 3.69
7 -2 -1 48.23 2.41
7 -2 -1 53.64 4.42
7 -2 -1 47.58 2.34
7 -2 0 44.82 4.05
7 -2 0 39.76 2.28
7 -2 0 37.05 2.27
7 -2 1 28.98 2.18
7 -2 1 41.59 2.51
7 -2 2 20.68 1.95
7 -2 3 15.25 1.83
7 -2 4 30.95 2.79
7 -2 5 2.11 0.98
7 -2 6 0.05 0.86
7 -2 7 2.12 1.03
7 -2 8 4.20 1.58
7 -2 9 4.99 1.68
7 -2 10 9.05 2.38
7 -2 11 2.57 1.52
7 -2 12 5.26 2.04
7 -1 -15 13.54 2.92
7 -1 -14 13.28 2.88
7 -1 -13 21.50 3.59
7 -1 -12 33.36 4.31
7 -1 -11 64.08 5.74
7 -1 -11 59.50 4.45
7 -1 -10 97.46 6.90
7 -1 -10 82.71 4.96
7 -1 -9 126.77 7.98
7 -1 -9 135.73 5.99
7 -1 -8 62.18 5.35
7 -1 -7 0.59 0.92
7 -1 -6 33.64 3.84
7 -1 -5 33.46 3.78
7 -1 -4 90.01 6.01
7 -1 -4 69.77 2.27
7 -1 -3 166.08 8.18
7 -1 -2 128.57 7.11
7 -1 -1 76.50 2.07
7 -1 0 35.31 1.71
7 -1 1 26.14 1.76
7 -1 2 16.85 1.61
7 -1 3 0.06 0.52
7 -1 4 0.63 0.61
7 -1 5 8.80 1.52
7 -1 6 8.67 1.72
7 -1 7 6.69 1.67
7 -1 8 10.66 2.05
7 -1 9 4.22 1.53
7 -1 10 1.48 1.12
7 -1 11 8.02 2.25
7 -1 12 7.28 2.36
7 0 -15 14.58 3.01
7 0 -14 1.41 1.18
7 0 -13 8.18 2.14
7 0 -12 43.79 4.80
7 0 -11 25.74 3.67
7 0 -10 33.86 4.06
7 0 -9 8.53 1.38
7 0 -9 7.74 2.22
7 0 -8 45.62 2.85
7 0 -8 49.72 4.73
7 0 -7 1.42 1.07
7 0 -7 1.57 0.51
7 0 -6 9.52 0.93
7 0 -6 10.33 2.31
7 0 -5 140.98 7.70
7 0 -4 81.70 5.73
7 0 3 36.07 2.46
7 0 4 13.31 1.68
7 0 5 7.35 1.46
7 0 6 22.70 2.63
7 0 7 10.29 1.96
7 0 8 4.06 1.36
7 0 9 2.13 1.06
7 1 -15 12.93 2.84
7 1 -14 9.20 2.27
7 1 -13 14.20 2.89
7 1 -12 15.77 2.84
7 1 -11 1.13 1.16
7 1 -10 29.63 3.90
7 1 -9 63.61 5.49
7 1 -8 1.66 0.95
7 1 -7 9.92 2.19
7 1 -6 59.62 5.04
8 -11 -2 9.50 2.67
8 -11 -1 8.58 2.51
8 -11 0 11.09 2.66
8 -11 1 14.51 3.17
8 -10 -4 -0.33 1.40
8 -10 -3 -2.20 1.60
8 -10 -2 1.66 1.41
8 -10 -1 14.81 3.03
8 -10 0 15.42 2.89
8 -10 0 12.48 2.71
8 -10 1 2.24 1.53
8 -10 2 3.47 1.64
8 -10 3 0.89 1.03
8 -10 4 1.87 1.30
8 -9 -6 14.16 3.33
8 -9 -5 17.94 3.42
8 -9 -4 -2.58 1.57
8 -9 -3 6.46 2.13
8 -9 -2 25.91 3.95
8 -9 -1 19.88 3.34
8 -9 0 5.43 1.90
8 -9 0 5.68 1.87
8 -9 1 4.48 1.71
8 -9 1 4.01 1.64
8 -9 2 6.95 2.08
8 -9 3 9.34 2.31
8 -9 4 6.30 1.98
8 -9 5 10.93 2.62
8 -9 6 10.68 2.69
8 -8 -7 41.72 5.31
8 -8 -6 25.97 4.12
8 -8 -5 20.23 3.55
8 -8 -4 18.52 3.32
8 -8 -3 18.86 3.30
8 -8 -2 24.42 3.62
8 -8 -1 21.22 3.43
8 -8 0 16.26 2.73
8 -8 0 14.90 2.80
8 -8 1 22.31 3.12
8 -8 1 15.48 2.86
8 -8 2 9.98 2.32
8 -8 2 14.65 2.69
8 -8 3 9.07 2.24
8 -8 4 14.05 2.68
8 -8 5 9.53 2.27
8 -8 6 1.58 1.29
8 -8 7 1.76 1.29
8 -8 8 0.35 1.35
8 -7 -8 21.55 3.86
8 -7 -7 15.93 3.22
8 -7 -6 28.99 4.24
8 -7 -5 21.52 3.54
8 -7 -4 11.19 2.71
8 -7 -3 13.16 2.77
8 -7 -2 18.07 3.10
8 -7 -1 5.23 1.53
8 -7 -1 5.41 1.87
8 -7 0 4.11 1.42
8 -7 0 4.60 1.59
8 -7 1 2.26 0.99
8 -7 1 1.66 1.07
8 -7 2 8.91 2.03
8 -7 2 1.90 1.39
8 -7 3 4.59 1.55
8 -7 3 5.45 1.57
8 -7 4 8.08 1.98
8 -7 5 5.38 1.57
8 -7 6 3.65 1.56
8 -7 7 2.06 1.33
8 -7 8 5.72 2.11
8 -7 9 1.23 1.35
8 -6 -10 19.69 3.69
8 -6 -9 13.89 3.13
8 -6 -8 26.10 4.03
8 -6 -7 12.09 2.87
8 -6 -6 3.16 1.77
8 -6 -5 7.93 2.35
8 -6 -4 10.45 2.49
8 -6 -3 7.39 2.04
8 -6 -2 4.27 1.80
8 -6 -1 9.65 1.82
8 -6 -1 10.60 2.50
8 -6 0 25.80 2.86
8 -6 0 25.21 3.53
8 -6 1 23.00 2.84
8 -6 1 34.50 3.86
8 -6 2 21.79 2.82
8 -6 2 16.52 2.71
8 -6 3 14.27 2.33
8 -6 3 11.62 2.28
8 -6 4 6.03 1.70
8 -6 5 2.24 1.21
8 -6 6 1.19 1.12
8 -6 7 7.70 2.16
8 -6 8 1.78 1.31
8 -6 9 3.64 1.70
8 -6 10 1.77 1.52
8 -5 -11 16.89 3.60
8 -5 -10 32.22 4.60
8 -5 -9 51.65 5.71
8 -5 -8 6.62 2.24
8 -5 -7 0.20 1.02
8 -5 -6 2.06 1.50
8 -5 -5 15.40 2.95
8 -5 -4 11.14 2.58
8 -5 -3 12.14 2.54
8 -5 -2 22.25 2.42
8 -5 -2 17.07 3.00
8 -5 -1 37.42 3.12
8 -5 -1 32.23 3.89
8 -5 0 52.03 3.75
8 -5 0 47.57 4.64
8 -5 1 17.16 2.25
8 -5 1 19.45 2.87
8 -5 2 5.52 1.44
8 -5 2 4.94 1.50
8 -5 3 2.92 1.05
8 -5 4 1.04 0.79
8 -5 5 1.98 1.14
8 -5 6 10.99 2.27
8 -5 7 9.97 2.33
8 -5 8 -0.69 1.14
8 -5 9 0.75 1.13
8 -5 10 -3.67 1.77
8 -4 -12 5.23 2.27
8 -4 -11 23.16 4.04
8 -4 -10 16.03 3.17
8 -4 -9 15.17 3.11
8 -4 -8 6.55 2.24
8 -4 -7 14.14 2.94
8 -4 -6 10.36 2.52
8 -4 -5 31.54 3.95
8 -4 -4 46.29 4.71
8 -4 -3 25.93 3.52
8 -4 -2 44.81 3.07
8 -4 -2 50.87 4.81
8 -4 -1 54.81 3.43
8 -4 -1 56.62 5.02
8 -4 0 21.95 3.20
8 -4 0 19.78 2.10
8 -4 1 13.64 1.86
8 -4 1 14.20 2.49
8 -4 2 5.74 1.33
8 -4 3 10.27 1.76
8 -4 4 15.09 2.24
8 -4 5 19.27 2.69
8 -4 6 38.79 3.93
8 -4 7 15.67 2.69
8 -4 8 6.62 1.95
8 -4 9 -1.39 1.32
8 -4 10 7.11 2.17
8 -4 11 4.39 1.96
8 -3 -12 10.42 2.69
8 -3 -11 3.92 1.81
8 -3 -10 12.11 2.79
8 -3 -9 21.38 3.56
8 -3 -8 19.74 3.48
8 -3 -7 17.25 3.13
8 -3 -6 52.76 5.25
8 -3 -5 37.57 4.30
8 -3 -4 38.62 4.30
8 -3 -3 69.29 5.76
8 -3 -2 22.55 1.84
8 -3 -2 27.24 3.56
8 -3 -1 52.99 4.77
8 -3 -1 47.74 2.76
8 -3 0 22.25 3.12
8 -3 0 18.91 1.83
8 -3 1 6.09 1.12
8 -3 2 26.68 2.49
8 -3 3 3.80 1.05
8 -3 4 5.99 1.35
8 -3 5 9.97 1.94
8 -3 6 5.29 1.48
8 -3 7 -0.11 0.89
8 -3 8 1.05 1.00
8 -3 9 2.45 1.51
8 -3 10 1.77 1.17
8 -2 -13 3.56 1.46
8 -2 -12 6.57 2.37
8 -2 -11 28.27 4.17
8 -2 -10 46.20 5.21
8 -2 -9 18.08 3.33
8 -2 -8 70.26 6.17
8 -2 -7 65.30 5.77
8 -2 -6 32.01 4.05
8 -2 -5 30.96 3.89
8 -2 -4 12.89 2.59
8 -2 -3 4.50 1.56
8 -2 -2 8.70 2.10
8 -2 -1 1.57 1.24
8 -2 3 25.25 2.39
8 -2 4 27.48 2.69
8 -2 5 24.81 2.77
8 -2 6 21.21 2.75
8 -2 7 9.58 2.05
8 -2 8 3.05 1.32
8 -1 -13 7.42 2.04
8 -1 -12 25.01 3.90
8 -1 -11 21.94 3.62
8 -1 -10 33.47 4.40
8 -1 -9 41.19 4.73
8 -1 -8 30.80 4.16
8 -1 -7 21.23 3.42
8 -1 -6 13.32 2.63
8 -1 -5 7.09 2.09
8 -1 -4 78.26 6.04
8 -1 -3 35.51 4.04
8 0 -14 8.46 2.46
8 0 -13 3.40 1.69
8 0 -12 8.66 2.31
8 0 -11 44.38 5.06
8 0 -10 25.31 3.77
8 0 -9 62.25 5.86
8 0 -8 47.02 5.00
8 0 -7 5.43 1.96
8 0 -6 0.28 1.22
8 0 -5 56.62 5.22
8 1 -14 8.53 2.53
8 1 -13 7.37 2.34
8 1 -12 10.37 2.52
8 1 -11 9.00 2.42
8 1 -10 9.56 2.39
8 1 -9 22.16 3.53
9 -10 -1 10.17 2.74
9 -9 -3 9.94 2.69
9 -9 -2 11.14 2.81
9 -9 -1 15.64 3.24
9 -9 0 11.80 2.79
9 -8 -5 16.17 3.32
9 -8 -4 12.71 3.22
9 -8 -3 0.98 1.42
9 -8 -2 16.19 3.17
9 -8 -1 16.70 3.18
9 -8 0 13.85 2.87
9 -8 1 7.25 2.11
9 -7 -6 3.84 2.03
9 -7 -5 0.24 1.28
9 -7 -4 5.03 2.06
9 -7 -3 4.73 1.98
9 -7 -2 5.40 1.99
9 -7 -1 6.15 2.14
9 -7 0 2.14 1.66
9 -7 1 3.19 1.65
9 -7 2 4.15 1.50
9 -6 -7 31.60 4.72
9 -6 -6 30.90 4.46
9 -6 -5 46.26 5.34
9 -6 -4 30.14 4.31
9 -6 -3 12.21 2.78
9 -6 -2 5.90 2.06
9 -6 -1 5.53 1.91
9 -6 0 3.35 1.62
9 -6 1 4.42 1.72
9 -6 2 2.05 1.60
9 -5 -8 16.21 3.45
9 -5 -7 8.20 2.39
9 -5 -6 1.15 1.35
9 -5 -5 1.01 1.47
9 -5 -4 2.29 1.57
9 -5 -3 6.80 2.26
9 -5 -2 8.36 2.38
9 -5 -1 9.46 2.35
9 -5 0 20.59 3.30
9 -5 1 9.89 2.37
9 -4 -9 8.53 2.85
9 -4 -8 15.17 3.25
9 -4 -7 0.93 1.23
9 -4 -6 1.63 1.49
9 -4 -5 23.14 3.75
9 -4 -4 30.07 4.16
9 -4 -3 11.41 2.64
9 -4 -2 15.76 2.94
9 -4 -1 16.31 2.97
9 -4 0 20.34 3.36
9 -3 -10 12.80 3.02
9 -3 -9 5.09 2.30
9 -3 -8 9.48 2.57
9 -3 -7 26.92 4.09
9 -3 -6 30.50 4.31
9 -3 -5 13.83 2.83
9 -3 -4 3.92 1.57
9 -3 -3 13.29 2.77
9 -3 -2 9.77 2.41
9 -3 -1 14.32 2.95
9 -2 -11 11.36 2.88
9 -2 -10 23.55 4.01
9 -2 -9 59.93 6.16
9 -2 -8 63.22 6.21
9 -2 -7 59.01 5.91
9 -2 -6 6.76 2.28
9 -2 -5 7.22 2.35
9 -2 -4 11.69 2.77
9 -2 -3 26.49 3.88
9 -1 -11 13.55 3.09
9 -1 -10 27.71 4.38
9 -1 -9 8.55 2.73
9 -1 -8 14.85 3.04
9 -1 -7 16.66 3.26
9 -1 -6 4.83 1.83
9 -1 -5 1.90 1.69
9 0 -11 8.64 2.75
9 0 -10 9.06 2.61
9 0 -9 9.54 2.73
9 0 -8 38.83 4.85
10 -8 -1 4.62 2.14
10 -8 0 1.47 1.50
10 -7 -3 4.56 2.20
10 -7 -2 5.00 2.25
10 -7 -1 3.01 1.82
10 -7 0 0.91 1.35
10 -7 1 4.71 1.83
10 -6 -4 3.77 2.04
10 -6 -3 8.17 2.65
10 -6 -2 -1.08 1.65
10 -6 -1 5.13 2.06
10 -6 0 9.01 2.56
10 -6 1 8.27 2.46
10 -5 -6 4.43 1.94
10 -5 -5 8.55 2.63
10 -5 -4 2.74 1.81
10 -5 -3 10.93 2.89
10 -5 -2 9.43 2.70
10 -5 -1 9.66 2.65
10 -5 0 11.97 2.80
10 -4 -6 6.90 2.44
10 -4 -5 8.03 2.48
10 -4 -4 11.27 2.91
10 -4 -3 12.06 2.90
10 -4 -2 4.46 1.94
10 -3 -7 13.13 3.06
10 -3 -6 16.97 3.55
10 -3 -5 18.47 3.45
10 -3 -4 4.80 2.10
10 -3 -3 2.98 2.07
10 -2 -8 16.13 3.51
10 -2 -7 16.31 3.54
10 -2 -6 11.62 3.03
10 -2 -5 1.17 1.57
10 -1 -8 18.20 3.64
10 -1 -7 14.41 3.41
0 0 0 0.00 0.00
TITL shI_3396_ in P1
REM P1 (#1 in standard setting)
CELL 0.71073 8.617349 10.626534 13.131190 93.3842 98.1206 94.0898
ZERR 2.00 0.000386 0.000595 0.000406 0.0035 0.0031 0.0041
LATT -1
SFAC C H N O Pd
UNIT 60.00 60.00 16.00 12.00 2.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 52414
_shelx_res_file
;
TITL shi_3396__a.res in P-1
jw2005_attached2.res
created by SHELXL-2018/3 at 15:18:59 on 08-Mar-2024
REM Old TITL shI_3396_ in P1 #1
REM SHELXT solution in P-1
REM R1 0.160, Rweak 0.045, Alpha 0.079, Orientation as input
REM Formula found by SHELXT: C58 N14 O4 Pd
CELL 0.71073 8.617349 10.626534 13.13119 93.3842 98.1206 94.0898
ZERR 1 0.000386 0.000595 0.000406 0.0035 0.0031 0.0041
LATT 1
SFAC C H F N O Pd
UNIT 40 34 12 8 14 1
EQIV $1 2-X,2-Y,1-Z
EQIV $2 1-X,1-Y,1-Z
EQIV $3 1-X,-Y,1-Z
EQIV $4 2-X,1-Y,-Z
EQIV $5 1+X,1+Y,+Z
EQIV $6 2-X,1-Y,1-Z
SIMU 0.01 0.02 2 C20 > O5X
RIGU C20 > O5X
FLAT C19 C20 O4 O5
FLAT C19 C20X O4 O5X
SIMU 0.01 0.02 2 C18 > O6X
RIGU C18 O6X
FLAT C17 C18 O6 O7
FLAT C17 C18X O7X O6X
L.S. 19
PLAN 5
SIZE 0.3 0.3 0.4
CONF
HTAB O6 F6
HTAB O6 O5
HTAB O6X F6X
HTAB O6X O5X
HTAB N4 O4
HTAB C15 N3_$2
HTAB C15 O1
HTAB C15 O3_$3
HTAB C14 O7
HTAB C4 F6_$4
HTAB C4 O4
HTAB C9 O4
HTAB C2 O7_$5
HTAB C2 O7X_$5
HTAB C1 N3_$1
HTAB C16 F4_$6
LIST 6
htab
BOND $H
MORE -1
fmap 2
acta 52
SHEL 99 0.79
OMIT 0 0 1
OMIT 2 0 1
REM
REM
REM
WGHT 0.039500 0.587700
FVAR 0.39949 0.52979 0.58736
PD1 6 1.000000 1.000000 0.500000 10.50000 0.04096 0.01711 =
0.02989 -0.00184 0.01369 -0.00198
SAME 0.01 0.04 C19 C20 F5 F6 F4 O5
SAME 0.01 0.04 C19 C20 F6 F4 F5 O5
SAME 0.02 0.04 C19 C20X F4X F5X F6X O5X
C19 1 0.889363 0.430165 0.153516 11.00000 0.06382 0.03956 =
0.04315 -0.01022 0.01976 -0.00768
PART 1
C20 1 0.965468 0.346983 0.079134 21.00000 0.11023 0.07709 =
0.05762 -0.03403 0.03517 0.00506
F4 3 1.109623 0.385817 0.070525 21.00000 0.07394 0.14391 =
0.10465 -0.06423 0.03236 0.00770
F5 3 0.950849 0.229411 0.100523 21.00000 0.18909 0.08577 =
0.15272 -0.01401 0.05668 0.04252
F6 3 0.897290 0.352706 -0.016961 21.00000 0.11115 0.15289 =
0.05151 -0.05666 0.02131 -0.00703
O5 5 0.745214 0.425163 0.139578 21.00000 0.05899 0.07941 =
0.05728 -0.00978 0.01292 -0.01445
PART 2
C20X 1 0.967613 0.330066 0.096275 -21.00000 0.10836 0.06256 =
0.07006 -0.02845 0.02268 0.00015
F4X 3 0.995193 0.356322 0.008034 -21.00000 0.18715 0.13037 =
0.10107 -0.01350 0.07942 0.02212
F5X 3 1.092128 0.289790 0.146253 -21.00000 0.10286 0.08923 =
0.13327 -0.04626 0.00106 0.04911
F6X 3 0.868979 0.224563 0.072185 -21.00000 0.12408 0.06675 =
0.11506 -0.05826 0.00050 -0.01144
O5X 5 0.749772 0.441496 0.122571 -21.00000 0.07648 0.07193 =
0.07277 -0.01469 0.02094 -0.01155
PART 0
O4 5 0.977910 0.489569 0.223786 11.00000 0.07077 0.05207 =
0.04831 -0.02169 0.01274 -0.00241
SAME 0.01 0.04 C17 C18 F2 F3 F1 O7 O6
SAME 0.01 0.04 C17 C18 F3 F1 F2 O7 O6
SAME 0.01 0.04 C17 C18X > O6X
C17 1 0.453011 0.237731 0.020552 11.00000 0.05271 0.07511 =
0.06317 0.00432 0.00895 -0.00778
PART 1
C18 1 0.349246 0.163733 -0.067808 31.00000 0.07855 0.11734 =
0.08284 -0.01871 0.01297 -0.02394
F1 3 0.305348 0.229636 -0.147525 31.00000 0.12364 0.18559 =
0.08320 0.00998 -0.02360 -0.02527
F2 3 0.426161 0.072053 -0.104348 31.00000 0.15117 0.13105 =
0.13200 -0.05794 0.00118 -0.00581
F3 3 0.216155 0.115813 -0.040968 31.00000 0.06763 0.14170 =
0.13071 -0.01003 0.00396 -0.04519
O7 5 0.441781 0.209304 0.104625 31.00000 0.09944 0.12269 =
0.07471 0.04011 0.00573 -0.03532
O6 5 0.540428 0.325654 -0.009266 31.00000 0.09706 0.11591 =
0.05944 0.02187 -0.00213 -0.04621
AFIX 3
H6 2 0.613798 0.359574 0.035314 31.00000 -1.20000
AFIX 0
PART 2
C18X 1 0.343777 0.169003 -0.067623 -31.00000 0.08576 0.12232 =
0.08790 -0.01899 0.01007 -0.02277
F1X 3 0.416597 0.129270 -0.143839 -31.00000 0.12522 0.15053 =
0.08858 -0.04153 0.01706 -0.01798
F2X 3 0.244317 0.247546 -0.108572 -31.00000 0.08734 0.17569 =
0.11507 -0.02196 -0.03050 0.01166
F3X 3 0.277607 0.064345 -0.037789 -31.00000 0.13171 0.12889 =
0.14717 -0.00788 0.01679 -0.06411
O7X 5 0.427791 0.240628 0.106209 -31.00000 0.09870 0.07561 =
0.06454 -0.01164 0.03880 -0.00651
O6X 5 0.574010 0.287845 -0.011976 -31.00000 0.06213 0.11575 =
0.05736 -0.01327 0.01291 -0.02837
AFIX 3
H6X 2 0.646340 0.324285 0.033784 -31.00000 -1.20000
AFIX 0
PART 0
O1 5 0.590299 0.367635 0.695904 11.00000 0.09192 0.03842 =
0.05825 0.00275 0.04063 -0.00968
O2 5 0.609368 0.156523 0.574179 11.00000 0.05381 0.02807 =
0.07164 0.01208 0.01543 -0.00502
O3 5 0.708608 0.167461 0.395657 11.00000 0.08820 0.02080 =
0.05222 -0.00735 0.01596 -0.00981
N4 4 0.910280 0.643704 0.375121 11.00000 0.04124 0.02061 =
0.02883 -0.00580 0.00836 -0.00524
AFIX 43
H4 2 0.916011 0.589624 0.324689 11.00000 -1.20000
AFIX 0
N3 4 0.856104 0.727960 0.522368 11.00000 0.04626 0.01960 =
0.03450 0.00096 0.01478 -0.00370
N2 4 0.930803 0.816917 0.472119 11.00000 0.04099 0.01811 =
0.03225 -0.00173 0.01394 -0.00239
N1 4 1.078526 0.964882 0.362656 11.00000 0.04288 0.02064 =
0.03108 -0.00123 0.01308 -0.00223
C10 1 0.711944 0.279681 0.451738 11.00000 0.04884 0.02321 =
0.04191 -0.00133 0.00566 -0.00442
C15 1 0.452927 0.129798 0.584438 11.00000 0.05377 0.04199 =
0.14329 0.00567 0.02629 -0.01463
AFIX 137
H15A 2 0.387704 0.144900 0.521519 11.00000 -1.50000
H15B 2 0.426681 0.183175 0.640017 11.00000 -1.50000
H15C 2 0.435939 0.042788 0.598890 11.00000 -1.50000
AFIX 0
C7 1 0.844515 0.623078 0.462137 11.00000 0.03712 0.02024 =
0.03317 -0.00099 0.00677 -0.00116
C12 1 0.650800 0.383762 0.607131 11.00000 0.04654 0.03222 =
0.04600 0.00444 0.01621 -0.00219
C14 1 0.755830 0.169898 0.296321 11.00000 0.10488 0.03818 =
0.04600 -0.00933 0.01204 -0.00126
AFIX 137
H14A 2 0.687992 0.219861 0.253864 11.00000 -1.50000
H14B 2 0.749120 0.085221 0.265300 11.00000 -1.50000
H14C 2 0.862275 0.206258 0.302706 11.00000 -1.50000
AFIX 0
C4 1 1.099522 0.804399 0.231502 11.00000 0.05282 0.03068 =
0.03220 -0.00640 0.01129 -0.00396
AFIX 43
H4A 2 1.077270 0.721198 0.204347 11.00000 -1.20000
AFIX 0
C9 1 0.773241 0.394327 0.422772 11.00000 0.04940 0.02443 =
0.03514 -0.00050 0.00873 -0.00458
AFIX 43
H9 2 0.813638 0.398525 0.360914 11.00000 -1.20000
AFIX 0
C2 1 1.214985 1.012029 0.223419 11.00000 0.07081 0.04030 =
0.04230 0.00028 0.03007 -0.00792
AFIX 43
H2 2 1.272046 1.071011 0.190832 11.00000 -1.20000
AFIX 0
C13 1 0.710838 0.497610 0.578318 11.00000 0.05064 0.02381 =
0.04066 -0.00262 0.01346 -0.00271
AFIX 43
H13 2 0.709298 0.571194 0.620054 11.00000 -1.20000
AFIX 0
C1 1 1.160099 1.046706 0.313978 11.00000 0.05831 0.02410 =
0.04032 -0.00112 0.01975 -0.00539
AFIX 43
H1 2 1.180841 1.129773 0.341708 11.00000 -1.20000
AFIX 0
C3 1 1.184673 0.890239 0.182134 11.00000 0.07027 0.04528 =
0.03489 -0.00698 0.02720 -0.00600
AFIX 43
H3 2 1.221162 0.865472 0.121268 11.00000 -1.20000
AFIX 0
C5 1 1.048451 0.843711 0.320961 11.00000 0.03409 0.02480 =
0.02886 0.00031 0.00550 0.00098
C11 1 0.651986 0.273429 0.543952 11.00000 0.04196 0.02387 =
0.04881 0.00670 0.00669 -0.00524
C8 1 0.773448 0.502302 0.487161 11.00000 0.03911 0.02163 =
0.03524 0.00110 0.00615 -0.00294
C16 1 0.579439 0.477550 0.761256 11.00000 0.09302 0.05729 =
0.05871 -0.00327 0.04034 0.00129
AFIX 137
H16A 2 0.519452 0.536517 0.723050 11.00000 -1.50000
H16B 2 0.683090 0.516035 0.786165 11.00000 -1.50000
H16C 2 0.528455 0.454170 0.818594 11.00000 -1.50000
AFIX 0
C6 1 0.963908 0.765931 0.384996 11.00000 0.03694 0.02092 =
0.02907 -0.00331 0.00705 -0.00164
HKLF 4
REM shi_3396__a.res in P-1
REM wR2 = 0.0953, GooF = S = 1.040, Restrained GooF = 1.101 for all data
REM R1 = 0.0415 for 4615 Fo > 4sig(Fo) and 0.0466 for all 5010 data
REM 444 parameters refined using 382 restraints
END
WGHT 0.0395 0.5877
REM Instructions for potential hydrogen bonds
HTAB O6 F6
HTAB O6 O5
HTAB O6X F6X
HTAB O6X O5X
HTAB N4 O4
HTAB C15 N3_$2
HTAB C15 O1
HTAB C15 O3_$3
HTAB C4 F6_$4
HTAB C4 O4
HTAB C9 O4
HTAB C2 O7_$5
HTAB C2 O7X_$5
HTAB C1 N3_$1
HTAB C16 F4_$6
REM Highest difference peak 0.386, deepest hole -0.454, 1-sigma level 0.069
Q1 1 0.9213 0.2643 0.0154 11.00000 0.05 0.39
Q2 1 1.1236 0.3399 0.1198 11.00000 0.05 0.38
Q3 1 1.0373 0.2550 0.1591 11.00000 0.05 0.33
Q4 1 0.6067 0.1787 0.3499 11.00000 0.05 0.33
Q5 1 1.0821 0.3003 0.1986 11.00000 0.05 0.33
;
_shelx_res_checksum 8377
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd1 1.000000 1.000000 0.500000 0.02885(10) Uani d 1 . .
C C19 0.8894(4) 0.4302(3) 0.1535(2) 0.0488(8) Uani d 1 . .
C C20 0.9655(9) 0.3470(9) 0.0791(6) 0.081(2) Uani d 0.530(6) A 1
F F4 1.1096(6) 0.3858(7) 0.0705(5) 0.109(2) Uani d 0.530(6) A 1
F F5 0.9508(14) 0.2294(9) 0.1005(8) 0.139(3) Uani d 0.530(6) A 1
F F6 0.8973(9) 0.3527(8) -0.0170(4) 0.108(2) Uani d 0.530(6) A 1
O O5 0.7452(12) 0.425(3) 0.140(2) 0.066(4) Uani d 0.530(6) A 1
C C20X 0.9676(14) 0.3301(10) 0.0963(10) 0.081(2) Uani d 0.470(6) A 2
F F4X 0.9952(15) 0.3563(10) 0.0080(8) 0.134(3) Uani d 0.470(6) A 2
F F5X 1.0921(8) 0.2898(7) 0.1463(6) 0.110(3) Uani d 0.470(6) A 2
F F6X 0.8690(10) 0.2246(8) 0.0722(7) 0.107(3) Uani d 0.470(6) A 2
O O5X 0.7498(15) 0.441(3) 0.123(3) 0.074(6) Uani d 0.470(6) A 2
O O4 0.9779(3) 0.4896(2) 0.22379(16) 0.0580(6) Uani d 1 . .
C C17 0.4530(4) 0.2377(4) 0.0206(3) 0.0643(10) Uani d 1 . .
C C18 0.3492(9) 0.1637(9) -0.0678(6) 0.095(2) Uani d 0.587(17) B 1
F F1 0.3053(15) 0.2296(12) -0.1475(7) 0.136(3) Uani d 0.587(17) B 1
F F2 0.4262(13) 0.0721(12) -0.1043(11) 0.143(3) Uani d 0.587(17) B 1
F F3 0.2162(9) 0.1158(12) -0.0410(7) 0.118(3) Uani d 0.587(17) B 1
O O7 0.442(2) 0.2093(17) 0.1046(6) 0.100(5) Uani d 0.587(17) B 1
O O6 0.5404(17) 0.3257(15) -0.0093(13) 0.094(5) Uani d 0.587(17) B 1
H H6 0.613798 0.359574 0.035314 0.113 Uiso d 0.587(17) B 1
C C18X 0.3438(13) 0.1690(10) -0.0676(7) 0.101(3) Uani d 0.413(17) B 2
F F1X 0.4166(17) 0.1293(19) -0.1438(10) 0.125(4) Uani d 0.413(17) B 2
F F2X 0.2443(16) 0.2475(14) -0.1086(13) 0.132(4) Uani d 0.413(17) B 2
F F3X 0.278(2) 0.0643(15) -0.0378(12) 0.141(4) Uani d 0.413(17) B 2
O O7X 0.428(3) 0.241(2) 0.1062(8) 0.078(4) Uani d 0.413(17) B 2
O O6X 0.574(2) 0.288(2) -0.0120(18) 0.081(5) Uani d 0.413(17) B 2
H H6X 0.646340 0.324285 0.033784 0.097 Uiso d 0.413(17) B 2
O O1 0.5903(3) 0.3676(2) 0.69590(17) 0.0607(7) Uani d 1 . .
O O2 0.6094(3) 0.15652(19) 0.57418(17) 0.0506(5) Uani d 1 . .
O O3 0.7086(3) 0.16746(19) 0.39566(16) 0.0543(6) Uani d 1 . .
N N4 0.9103(3) 0.6437(2) 0.37512(15) 0.0306(5) Uani d 1 . .
H H4 0.916011 0.589624 0.324689 0.037 Uiso calc 1 . .
N N3 0.8561(3) 0.7280(2) 0.52237(16) 0.0329(5) Uani d 1 . .
N N2 0.9308(3) 0.81692(19) 0.47212(15) 0.0300(5) Uani d 1 . .
N N1 1.0785(3) 0.9649(2) 0.36266(15) 0.0311(5) Uani d 1 . .
C C10 0.7119(3) 0.2797(3) 0.4517(2) 0.0386(6) Uani d 1 . .
C C15 0.4529(4) 0.1298(4) 0.5844(4) 0.0795(13) Uani d 1 . .
H H15A 0.387704 0.144900 0.521519 0.119 Uiso calc 1 . .
H H15B 0.426681 0.183175 0.640017 0.119 Uiso calc 1 . .
H H15C 0.435939 0.042788 0.598890 0.119 Uiso calc 1 . .
C C7 0.8445(3) 0.6231(2) 0.46214(19) 0.0303(6) Uani d 1 . .
C C12 0.6508(3) 0.3838(3) 0.6071(2) 0.0409(7) Uani d 1 . .
C C14 0.7558(5) 0.1699(3) 0.2963(2) 0.0638(10) Uani d 1 . .
H H14A 0.687992 0.219861 0.253864 0.096 Uiso calc 1 . .
H H14B 0.749120 0.085221 0.265300 0.096 Uiso calc 1 . .
H H14C 0.862275 0.206258 0.302706 0.096 Uiso calc 1 . .
C C4 1.0995(3) 0.8044(3) 0.2315(2) 0.0388(7) Uani d 1 . .
H H4A 1.077270 0.721198 0.204347 0.047 Uiso calc 1 . .
C C9 0.7732(3) 0.3943(3) 0.4228(2) 0.0365(6) Uani d 1 . .
H H9 0.813638 0.398525 0.360914 0.044 Uiso calc 1 . .
C C2 1.2150(4) 1.0120(3) 0.2234(2) 0.0497(8) Uani d 1 . .
H H2 1.272046 1.071011 0.190832 0.060 Uiso calc 1 . .
C C13 0.7108(3) 0.4976(3) 0.5783(2) 0.0382(6) Uani d 1 . .
H H13 0.709298 0.571194 0.620054 0.046 Uiso calc 1 . .
C C1 1.1601(4) 1.0467(3) 0.3140(2) 0.0403(7) Uani d 1 . .
H H1 1.180841 1.129773 0.341708 0.048 Uiso calc 1 . .
C C3 1.1847(4) 0.8902(3) 0.1821(2) 0.0492(8) Uani d 1 . .
H H3 1.221162 0.865472 0.121268 0.059 Uiso calc 1 . .
C C5 1.0485(3) 0.8437(2) 0.32096(18) 0.0293(5) Uani d 1 . .
C C11 0.6520(3) 0.2734(3) 0.5440(2) 0.0384(6) Uani d 1 . .
C C8 0.7734(3) 0.5023(2) 0.4872(2) 0.0322(6) Uani d 1 . .
C C16 0.5794(5) 0.4776(4) 0.7613(3) 0.0674(11) Uani d 1 . .
H H16A 0.519452 0.536517 0.723050 0.101 Uiso calc 1 . .
H H16B 0.683090 0.516035 0.786165 0.101 Uiso calc 1 . .
H H16C 0.528455 0.454170 0.818594 0.101 Uiso calc 1 . .
C C6 0.9639(3) 0.7659(2) 0.38500(18) 0.0292(5) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pd1 0.04096(18) 0.01711(15) 0.02989(16) -0.00198(11) 0.01369(12) -0.00184(10)
C19 0.064(2) 0.0396(18) 0.0431(17) -0.0077(16) 0.0198(16) -0.0102(14)
C20 0.110(4) 0.077(4) 0.058(4) 0.005(4) 0.035(4) -0.034(4)
F4 0.074(3) 0.144(5) 0.105(4) 0.008(3) 0.032(3) -0.064(4)
F5 0.189(8) 0.086(5) 0.153(7) 0.043(5) 0.057(6) -0.014(5)
F6 0.111(5) 0.153(5) 0.052(3) -0.007(4) 0.021(3) -0.057(3)
O5 0.059(5) 0.079(9) 0.057(6) -0.014(4) 0.013(4) -0.010(5)
C20X 0.108(5) 0.063(5) 0.070(5) 0.000(4) 0.023(4) -0.028(4)
F4X 0.187(8) 0.130(5) 0.101(6) 0.022(6) 0.079(6) -0.014(5)
F5X 0.103(4) 0.089(5) 0.133(5) 0.049(4) 0.001(4) -0.046(4)
F6X 0.124(6) 0.067(4) 0.115(5) -0.011(4) 0.001(4) -0.058(3)
O5X 0.076(7) 0.072(9) 0.073(12) -0.012(5) 0.021(5) -0.015(8)
O4 0.0708(16) 0.0521(15) 0.0483(13) -0.0024(12) 0.0127(11) -0.0217(11)
C17 0.053(2) 0.075(3) 0.063(2) -0.0078(19) 0.0090(18) 0.004(2)
C18 0.079(5) 0.117(5) 0.083(5) -0.024(4) 0.013(4) -0.019(4)
F1 0.124(6) 0.186(7) 0.083(4) -0.025(5) -0.024(4) 0.010(5)
F2 0.151(6) 0.131(7) 0.132(7) -0.006(5) 0.001(5) -0.058(5)
F3 0.068(4) 0.142(7) 0.131(4) -0.045(4) 0.004(3) -0.010(5)
O7 0.099(7) 0.123(11) 0.075(6) -0.035(7) 0.006(5) 0.040(6)
O6 0.097(8) 0.116(9) 0.059(5) -0.046(7) -0.002(5) 0.022(6)
C18X 0.086(6) 0.122(6) 0.088(6) -0.023(6) 0.010(5) -0.019(5)
F1X 0.125(6) 0.151(9) 0.089(6) -0.018(7) 0.017(5) -0.042(6)
F2X 0.087(6) 0.176(7) 0.115(7) 0.012(6) -0.031(5) -0.022(6)
F3X 0.132(8) 0.129(8) 0.147(7) -0.064(6) 0.017(7) -0.008(6)
O7X 0.099(8) 0.076(8) 0.065(7) -0.007(6) 0.039(6) -0.012(5)
O6X 0.062(6) 0.116(12) 0.057(6) -0.028(7) 0.013(5) -0.013(7)
O1 0.0919(18) 0.0384(13) 0.0582(14) -0.0097(12) 0.0406(13) 0.0027(10)
O2 0.0538(13) 0.0281(11) 0.0716(15) -0.0050(10) 0.0154(11) 0.0121(10)
O3 0.0882(17) 0.0208(11) 0.0522(13) -0.0098(11) 0.0160(11) -0.0074(9)
N4 0.0412(13) 0.0206(11) 0.0288(11) -0.0052(9) 0.0084(9) -0.0058(8)
N3 0.0463(13) 0.0196(11) 0.0345(11) -0.0037(9) 0.0148(10) 0.0010(9)
N2 0.0410(13) 0.0181(11) 0.0323(11) -0.0024(9) 0.0139(9) -0.0017(8)
N1 0.0429(13) 0.0206(11) 0.0311(11) -0.0022(9) 0.0131(9) -0.0012(8)
C10 0.0488(17) 0.0232(14) 0.0419(15) -0.0044(12) 0.0057(13) -0.0013(11)
C15 0.054(2) 0.042(2) 0.143(4) -0.0146(17) 0.026(2) 0.006(2)
C7 0.0371(15) 0.0202(13) 0.0332(13) -0.0012(11) 0.0068(11) -0.0010(10)
C12 0.0465(17) 0.0322(16) 0.0460(16) -0.0022(13) 0.0162(13) 0.0044(13)
C14 0.105(3) 0.0382(19) 0.0460(19) -0.0013(19) 0.0120(18) -0.0093(15)
C4 0.0528(18) 0.0307(15) 0.0322(14) -0.0040(13) 0.0113(12) -0.0064(11)
C9 0.0494(17) 0.0244(14) 0.0351(14) -0.0046(12) 0.0087(12) -0.0005(11)
C2 0.071(2) 0.0403(18) 0.0423(16) -0.0079(16) 0.0301(15) 0.0003(13)
C13 0.0506(17) 0.0238(14) 0.0407(15) -0.0027(12) 0.0135(13) -0.0026(11)
C1 0.0583(19) 0.0241(14) 0.0403(15) -0.0054(13) 0.0197(13) -0.0011(11)
C3 0.070(2) 0.0453(19) 0.0349(15) -0.0060(16) 0.0272(15) -0.0070(13)
C5 0.0341(14) 0.0248(13) 0.0289(12) 0.0010(11) 0.0055(10) 0.0003(10)
C11 0.0420(16) 0.0239(14) 0.0488(16) -0.0052(12) 0.0067(13) 0.0067(12)
C8 0.0391(15) 0.0216(13) 0.0352(14) -0.0029(11) 0.0061(11) 0.0011(10)
C16 0.093(3) 0.057(2) 0.059(2) 0.001(2) 0.040(2) -0.0033(18)
C6 0.0369(14) 0.0209(13) 0.0291(12) -0.0016(10) 0.0071(10) -0.0033(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Pd1 N2 . 2_776 180.00(12) ?
N2 Pd1 N1 . 2_776 100.35(8) y
N2 Pd1 N1 2_776 . 100.35(8) ?
N2 Pd1 N1 2_776 2_776 79.65(8) ?
N2 Pd1 N1 . . 79.65(8) y
N1 Pd1 N1 2_776 . 180.00(12) ?
O5 C19 C20 . . 116.4(14) ?
O5X C19 C20X . . 116.7(16) ?
O4 C19 C20 . . 116.6(4) ?
O4 C19 O5 . . 126.9(14) ?
O4 C19 C20X . . 113.6(6) ?
O4 C19 O5X . . 129.6(17) ?
F4 C20 C19 . . 114.3(6) ?
F4 C20 F6 . . 100.3(7) ?
F5 C20 C19 . . 110.6(7) ?
F5 C20 F4 . . 112.8(8) ?
F5 C20 F6 . . 107.0(9) ?
F6 C20 C19 . . 111.1(6) ?
F4X C20X C19 . . 115.2(10) ?
F4X C20X F5X . . 108.9(11) ?
F4X C20X F6X . . 100.6(11) ?
F5X C20X C19 . . 116.1(9) ?
F5X C20X F6X . . 103.9(9) ?
F6X C20X C19 . . 110.5(9) ?
O7 C17 C18 . . 117.9(10) ?
O7 C17 O6 . . 129.6(11) ?
O6 C17 C18 . . 112.5(9) ?
O7X C17 C18X . . 123.2(13) ?
O7X C17 O6X . . 126.8(15) ?
O6X C17 C18X . . 110.0(12) ?
F1 C18 C17 . . 114.7(7) ?
F1 C18 F2 . . 105.2(8) ?
F1 C18 F3 . . 104.8(8) ?
F2 C18 C17 . . 109.5(7) ?
F2 C18 F3 . . 109.9(8) ?
F3 C18 C17 . . 112.4(6) ?
C17 O6 H6 . . 116.1 ?
F1X C18X C17 . . 113.1(9) ?
F1X C18X F2X . . 105.1(10) ?
F1X C18X F3X . . 103.9(10) ?
F2X C18X C17 . . 109.2(8) ?
F3X C18X C17 . . 110.4(9) ?
F3X C18X F2X . . 114.9(12) ?
C17 O6X H6X . . 116.5 ?
C12 O1 C16 . . 117.7(2) ?
C11 O2 C15 . . 117.5(3) ?
C10 O3 C14 . . 117.7(2) ?
C7 N4 H4 . . 127.3 ?
C6 N4 H4 . . 127.3 ?
C6 N4 C7 . . 105.5(2) ?
C7 N3 N2 . . 105.36(19) ?
N3 N2 Pd1 . . 135.44(16) ?
C6 N2 Pd1 . . 114.75(16) ?
C6 N2 N3 . . 109.8(2) ?
C1 N1 Pd1 . . 126.23(18) ?
C1 N1 C5 . . 118.4(2) ?
C5 N1 Pd1 . . 115.29(16) ?
O3 C10 C9 . . 124.2(3) ?
O3 C10 C11 . . 115.4(2) ?
C11 C10 C9 . . 120.4(3) ?
O2 C15 H15A . . 109.5 ?
O2 C15 H15B . . 109.5 ?
O2 C15 H15C . . 109.5 ?
H15A C15 H15B . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
N4 C7 C8 . . 125.5(2) ?
N3 C7 N4 . . 110.5(2) ?
N3 C7 C8 . . 123.9(2) ?
O1 C12 C13 . . 124.8(3) ?
O1 C12 C11 . . 115.1(3) ?
C13 C12 C11 . . 120.0(2) ?
O3 C14 H14A . . 109.5 ?
O3 C14 H14B . . 109.5 ?
O3 C14 H14C . . 109.5 ?
H14A C14 H14B . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C3 C4 H4A . . 120.6 ?
C5 C4 H4A . . 120.6 ?
C5 C4 C3 . . 118.8(3) ?
C10 C9 H9 . . 120.4 ?
C8 C9 C10 . . 119.1(2) ?
C8 C9 H9 . . 120.4 ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
C3 C2 C1 . . 119.4(3) ?
C12 C13 H13 . . 120.1 ?
C12 C13 C8 . . 119.8(3) ?
C8 C13 H13 . . 120.1 ?
N1 C1 C2 . . 121.9(3) ?
N1 C1 H1 . . 119.0 ?
C2 C1 H1 . . 119.0 ?
C4 C3 H3 . . 120.3 ?
C2 C3 C4 . . 119.4(3) ?
C2 C3 H3 . . 120.3 ?
N1 C5 C4 . . 122.1(2) ?
N1 C5 C6 . . 111.5(2) ?
C4 C5 C6 . . 126.3(2) ?
O2 C11 C10 . . 117.9(3) ?
O2 C11 C12 . . 122.1(3) ?
C10 C11 C12 . . 119.6(2) ?
C9 C8 C7 . . 120.7(2) ?
C13 C8 C7 . . 118.3(2) ?
C13 C8 C9 . . 120.9(2) ?
O1 C16 H16A . . 109.5 ?
O1 C16 H16B . . 109.5 ?
O1 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N4 C6 C5 . . 132.4(2) ?
N2 C6 N4 . . 108.8(2) ?
N2 C6 C5 . . 118.8(2) ?
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
Pd1 N2 . 1.991(2) y
Pd1 N2 2_776 1.991(2) ?
Pd1 N1 . 2.037(2) y
Pd1 N1 2_776 2.037(2) ?
C19 C20 . 1.526(9) ?
C19 O5 . 1.227(11) ?
C19 C20X . 1.517(11) ?
C19 O5X . 1.231(13) ?
C19 O4 . 1.223(4) ?
C20 F4 . 1.303(7) ?
C20 F5 . 1.298(7) ?
C20 F6 . 1.321(7) ?
C20X F4X . 1.258(12) ?
C20X F5X . 1.290(12) ?
C20X F6X . 1.351(11) ?
C17 C18 . 1.504(7) ?
C17 O7 . 1.177(7) ?
C17 O6 . 1.273(7) ?
C17 C18X . 1.501(8) ?
C17 O7X . 1.174(8) ?
C17 O6X . 1.275(8) ?
C18 F1 . 1.320(6) ?
C18 F2 . 1.321(6) ?
C18 F3 . 1.323(6) ?
O6 H6 . 0.8428 ?
C18X F1X . 1.319(7) ?
C18X F2X . 1.321(7) ?
C18X F3X . 1.319(7) ?
O6X H6X . 0.8555 ?
O1 C12 . 1.357(3) ?
O1 C16 . 1.425(4) ?
O2 C15 . 1.385(4) ?
O2 C11 . 1.367(3) ?
O3 C10 . 1.360(3) ?
O3 C14 . 1.421(4) ?
N4 H4 . 0.8600 ?
N4 C7 . 1.367(3) ?
N4 C6 . 1.340(3) ?
N3 N2 . 1.360(3) ?
N3 C7 . 1.317(3) ?
N2 C6 . 1.313(3) ?
N1 C1 . 1.328(3) ?
N1 C5 . 1.362(3) ?
C10 C9 . 1.388(4) ?
C10 C11 . 1.385(4) ?
C15 H15A . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15C . 0.9600 ?
C7 C8 . 1.458(3) ?
C12 C13 . 1.376(4) ?
C12 C11 . 1.397(4) ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
C4 H4A . 0.9300 ?
C4 C3 . 1.378(4) ?
C4 C5 . 1.365(3) ?
C9 H9 . 0.9300 ?
C9 C8 . 1.384(4) ?
C2 H2 . 0.9300 ?
C2 C1 . 1.380(4) ?
C2 C3 . 1.366(4) ?
C13 H13 . 0.9300 ?
C13 C8 . 1.383(4) ?
C1 H1 . 0.9300 ?
C3 H3 . 0.9300 ?
C5 C6 . 1.446(3) ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
C16 H16C . 0.9600 ?
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
_geom_hbond_publ_flag
O6 H6 F6 . 0.84 2.63 3.085(15) 114.9 yes
O6 H6 O5 . 0.84 1.73 2.56(3) 171.5 yes
O6X H6X F6X . 0.86 2.27 2.77(3) 117.7 yes
O6X H6X O5X . 0.86 1.76 2.58(4) 159.8 yes
N4 H4 O4 . 0.86 1.81 2.655(3) 166.1 yes
C15 H15A N3 2_666 0.96 2.59 3.334(5) 134.1 yes
C15 H15B O1 . 0.96 2.35 2.929(5) 118.4 yes
C15 H15C O3 2_656 0.96 2.49 3.400(4) 158.3 yes
C14 H14A O7 . 0.96 2.67 3.492(17) 144.2 yes
C4 H4A F6 2_765 0.93 2.58 3.193(6) 123.7 yes
C4 H4A O4 . 0.93 2.59 3.425(4) 150.2 yes
C9 H9 O4 . 0.93 2.63 3.510(4) 158.3 yes
C2 H2 O7 1_665 0.93 2.44 3.363(14) 174.0 yes
C2 H2 O7X 1_665 0.93 2.57 3.498(19) 177.7 yes
C1 H1 N3 2_776 0.93 2.34 3.146(3) 144.6 yes
C16 H16B F4 2_766 0.96 2.52 3.400(7) 151.7 yes
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 N2 C6 N4 . . . . -179.45(16) ?
Pd1 N2 C6 C5 . . . . 1.7(3) ?
Pd1 N1 C1 C2 . . . . 176.7(2) ?
Pd1 N1 C5 C4 . . . . -177.2(2) ?
Pd1 N1 C5 C6 . . . . 0.6(3) ?
O5 C19 C20 F4 . . . . 156.2(17) ?
O5 C19 C20 F5 . . . . -75.1(18) ?
O5 C19 C20 F6 . . . . 43.6(18) ?
O5X C19 C20X F4X . . . . 73(2) ?
O5X C19 C20X F5X . . . . -158(2) ?
O5X C19 C20X F6X . . . . -40(2) ?
O4 C19 C20 F4 . . . . -27.5(8) ?
O4 C19 C20 F5 . . . . 101.2(8) ?
O4 C19 C20 F6 . . . . -140.1(6) ?
O4 C19 C20X F4X . . . . -106.0(11) ?
O4 C19 C20X F5X . . . . 22.9(12) ?
O4 C19 C20X F6X . . . . 140.8(9) ?
O7 C17 C18 F1 . . . . 147.3(16) ?
O7 C17 C18 F2 . . . . -94.6(16) ?
O7 C17 C18 F3 . . . . 27.8(18) ?
O6 C17 C18 F1 . . . . -31.6(16) ?
O6 C17 C18 F2 . . . . 86.4(15) ?
O6 C17 C18 F3 . . . . -151.2(15) ?
O7X C17 C18X F1X . . . . -151.8(19) ?
O7X C17 C18X F2X . . . . 91.5(19) ?
O7X C17 C18X F3X . . . . -36(2) ?
O6X C17 C18X F1X . . . . 27(2) ?
O6X C17 C18X F2X . . . . -89.8(19) ?
O6X C17 C18X F3X . . . . 142.9(19) ?
O1 C12 C13 C8 . . . . 178.3(3) ?
O1 C12 C11 O2 . . . . -6.0(4) ?
O1 C12 C11 C10 . . . . -179.7(3) ?
O3 C10 C9 C8 . . . . -178.6(3) ?
O3 C10 C11 O2 . . . . 5.8(4) ?
O3 C10 C11 C12 . . . . 179.8(3) ?
N4 C7 C8 C9 . . . . 2.5(4) ?
N4 C7 C8 C13 . . . . -179.5(3) ?
N3 N2 C6 N4 . . . . 0.9(3) ?
N3 N2 C6 C5 . . . . -178.0(2) ?
N3 C7 C8 C9 . . . . -176.4(3) ?
N3 C7 C8 C13 . . . . 1.6(4) ?
N2 N3 C7 N4 . . . . 0.1(3) ?
N2 N3 C7 C8 . . . . 179.1(2) ?
N1 C5 C6 N4 . . . . 179.9(3) ?
N1 C5 C6 N2 . . . . -1.5(3) ?
C10 C9 C8 C7 . . . . 176.6(3) ?
C10 C9 C8 C13 . . . . -1.3(4) ?
C15 O2 C11 C10 . . . . -118.1(4) ?
C15 O2 C11 C12 . . . . 68.1(4) ?
C7 N4 C6 N2 . . . . -0.8(3) ?
C7 N4 C6 C5 . . . . 177.9(3) ?
C7 N3 N2 Pd1 . . . . 179.9(2) ?
C7 N3 N2 C6 . . . . -0.6(3) ?
C12 C13 C8 C7 . . . . -176.4(3) ?
C12 C13 C8 C9 . . . . 1.6(4) ?
C14 O3 C10 C9 . . . . -6.8(5) ?
C14 O3 C10 C11 . . . . 174.6(3) ?
C4 C5 C6 N4 . . . . -2.4(5) ?
C4 C5 C6 N2 . . . . 176.2(3) ?
C9 C10 C11 O2 . . . . -172.8(3) ?
C9 C10 C11 C12 . . . . 1.2(5) ?
C13 C12 C11 O2 . . . . 172.9(3) ?
C13 C12 C11 C10 . . . . -0.8(5) ?
C1 N1 C5 C4 . . . . 0.1(4) ?
C1 N1 C5 C6 . . . . 177.9(2) ?
C1 C2 C3 C4 . . . . 0.2(5) ?
C3 C4 C5 N1 . . . . 0.2(4) ?
C3 C4 C5 C6 . . . . -177.2(3) ?
C3 C2 C1 N1 . . . . 0.1(5) ?
C5 N1 C1 C2 . . . . -0.3(4) ?
C5 C4 C3 C2 . . . . -0.3(5) ?
C11 C10 C9 C8 . . . . -0.1(4) ?
C11 C12 C13 C8 . . . . -0.5(5) ?
C16 O1 C12 C13 . . . . 3.9(5) ?
C16 O1 C12 C11 . . . . -177.2(3) ?
C6 N4 C7 N3 . . . . 0.4(3) ?
C6 N4 C7 C8 . . . . -178.5(2) ?