#------------------------------------------------------------------------------
#$Date: 2024-06-28 04:46:26 +0300 (Fri, 28 Jun 2024) $
#$Revision: 292634 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312530.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_2312530
loop_
_publ_author_name
'Blake, Alexander J.'
'Castellano, Carlo'
'Lippolis, Vito'
'Podda, Enrico'
'Schröder, Martin'
_publ_section_title
;
Formation of extended polyiodides at large cation templates.
;
_journal_coeditor_code VP3036
_journal_issue 7
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624004194
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Pd2 I2 (C12 H26 N2 S4)] (I)2, 5I2'
_chemical_formula_moiety 'C12 H26 I2 N2 Pd2 S4 2+, 2(I -), 5(I2)'
_chemical_formula_sum 'C12 H26 I14 N2 Pd2 S4'
_chemical_formula_weight 2315.99
_chemical_name_systematic
;
(\m-1,4,10,13-Tetrathia-7,16-diazacyclooctadecane)bis[iodidopalladium(II)]
diiodide penta(diiodine)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha 90
_cell_angle_beta 100.170(13)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 21.609(4)
_cell_length_b 8.198(3)
_cell_length_c 24.151(3)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 220(2)
_cell_measurement_theta_max 20
_cell_measurement_theta_min 5
_cell_volume 4211.1(18)
_computing_cell_refinement
;
STADI4 (Stoe & Cie, 1996)
;
_computing_data_collection
;
STADI4 (Stoe & Cie, 1996)
;
_computing_data_reduction
;
REDU4 (Stoe & Cie, 1996)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 1997)
;
_diffrn_ambient_temperature 220(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device 'STOE STADI4 4-circle'
_diffrn_measurement_method
;
Scan width (omega) = 1.64 - 2.20, scan ratio 2theta:omega = 1.00
I(Net) and sigma(I) from profile fitting (Clegg, 1981)
;
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0289
_diffrn_reflns_av_unetI/netI 0.0356
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 4584
_diffrn_reflns_theta_full 25.022
_diffrn_reflns_theta_max 25.022
_diffrn_reflns_theta_min 2.663
_diffrn_standards_decay_% 5.0
_diffrn_standards_interval_count 60
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 11.328
_exptl_absorpt_correction_T_max 0.3056
_exptl_absorpt_correction_T_min 0.2217
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details
;
(REDU4; Stoe & Cie, 1996)
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 3.653
_exptl_crystal_description column
_exptl_crystal_F_000 4040
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.13
_refine_diff_density_max 1.349
_refine_diff_density_min -1.615
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.079
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 163
_refine_ls_number_reflns 3715
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.079
_refine_ls_R_factor_all 0.0634
_refine_ls_R_factor_gt 0.0506
_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/[\s^2^(Fo^2^)+(0.0681P)^2^+91.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1239
_refine_ls_wR_factor_ref 0.1361
_reflns_number_gt 3059
_reflns_number_total 3715
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vp3036.cif
_cod_data_source_block I
_cod_database_code 2312530
_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 0.157
_shelx_estimated_absorpt_t_max 0.321
_shelx_hkl_file
;
-24 0 1 1.31 1.92 0
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-24 0 6 2.58 2.10 0
-24 0 7 1.75 2.16 0
-24 0 8 68.95 5.54 0
-24 0 9 3.11 2.63 0
-24 0 10 6.83 3.04 0
-24 0 11 0.76 2.33 0
-24 0 12 28.84 4.32 0
-24 0 13 2.40 2.58 0
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-22 0 18 61.67 5.74 0
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-22 0 9 -3.74 1.85 0
-22 0 8 -1.44 2.00 0
-22 0 7 5.69 2.28 0
-22 0 6 117.30 6.35 0
-22 0 5 0.07 2.16 0
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-22 0 1 0.38 1.79 0
-20 0 1 4.77 2.37 0
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-20 0 21 2.88 2.88 0
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-16 0 5 0.91 1.89 0
-16 0 6 469.85 9.89 0
-16 0 7 2.92 2.36 0
-16 0 8 1587.35 18.71 0
-16 0 9 3.80 2.37 0
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-16 0 11 1.74 2.05 0
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-16 0 18 -0.88 2.08 0
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-16 0 20 -3.67 1.89 0
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-16 0 24 84.82 6.54 0
-16 0 25 2.71 2.80 0
-14 0 26 250.15 10.42 0
-14 0 25 1.67 2.73 0
-14 0 24 34.87 4.50 0
-14 0 23 -1.45 2.43 0
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-2 0 15 2.52 2.02 0
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-2 0 11 -2.21 1.79 0
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-2 0 7 -1.50 1.60 0
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-2 0 5 1.45 1.44 0
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-2 0 3 -0.65 0.97 0
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0 0 20 126.91 6.24 0
0 0 21 0.62 2.26 0
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0 0 23 7.22 2.89 0
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2 0 21 0.49 2.41 0
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2 0 12 16.84 2.39 0
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2 0 9 3.78 1.88 0
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2 0 6 7.48 1.93 0
2 0 5 1.19 1.70 0
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4 0 3 1.10 1.53 0
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4 0 7 5.56 2.02 0
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4 0 9 2.84 2.03 0
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6 0 15 0.12 2.44 0
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6 0 3 3.70 1.65 0
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6 0 1 -0.03 1.37 0
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8 0 0 392.11 6.14 0
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8 0 11 0.10 1.85 0
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8 0 13 2.46 2.33 0
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8 0 25 -0.53 2.82 0
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10 0 13 -1.29 1.97 0
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12 0 1 3.40 1.53 0
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12 0 3 1.64 1.59 0
12 0 4 237.12 6.60 0
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12 0 7 3.24 2.16 0
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12 0 9 4.51 2.36 0
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7 1 -15 -1.95 1.67 0
7 1 -14 8.24 2.23 0
7 1 -13 235.21 6.72 0
7 1 -12 2.96 1.98 0
7 1 -11 787.95 11.24 0
7 1 -10 128.26 4.89 0
7 1 -9 54.71 3.37 0
7 1 -8 302.09 6.54 0
7 1 -7 4.38 1.83 0
7 1 -6 49.49 2.96 0
7 1 -5 99.92 3.67 0
7 1 -4 2530.10 15.37 0
7 1 -3 138.10 3.90 0
7 1 -2 1954.93 12.95 0
7 1 -1 4805.71 20.74 0
9 1 -1 17.53 2.14 0
9 1 -2 47.74 2.90 0
9 1 -3 22.75 2.32 0
9 1 -4 1640.34 13.61 0
9 1 -5 30.23 2.56 0
9 1 -6 516.53 8.19 0
9 1 -7 1913.66 15.65 0
9 1 -8 861.52 11.03 0
9 1 -9 21.51 2.55 0
9 1 -10 7.78 2.22 0
9 1 -11 24.62 2.76 0
9 1 -12 11.89 2.40 0
9 1 -13 3.78 1.98 0
9 1 -14 534.03 10.77 0
9 1 -15 84.65 4.81 0
9 1 -16 220.39 7.40 0
9 1 -17 117.18 5.78 0
9 1 -18 9.41 2.72 0
9 1 -19 0.25 2.12 0
9 1 -20 181.10 7.37 0
9 1 -21 98.89 5.83 0
9 1 -22 46.12 4.33 0
9 1 -23 -0.75 2.03 0
9 1 -24 6.94 2.70 0
9 1 -25 17.33 3.42 0
9 1 -26 1.64 2.60 0
9 1 -27 28.22 4.11 0
9 1 -28 12.15 3.35 0
11 1 -27 97.28 6.90 0
11 1 -26 20.79 3.77 0
11 1 -25 21.99 3.78 0
11 1 -24 7.70 2.92 0
11 1 -23 11.93 3.12 0
11 1 -22 14.16 3.37 0
11 1 -21 0.48 2.32 0
11 1 -20 477.54 12.00 0
11 1 -19 58.59 4.75 0
11 1 -18 226.61 8.36 0
11 1 -17 1242.32 18.06 0
11 1 -16 1048.82 16.07 0
11 1 -15 60.48 4.55 0
11 1 -14 272.01 8.13 0
11 1 -13 705.61 12.14 0
11 1 -12 2.97 1.99 0
11 1 -11 1271.25 15.23 0
11 1 -10 1.85 2.07 0
11 1 -9 818.85 11.67 0
11 1 -8 313.87 7.27 0
11 1 -7 8.04 1.99 0
11 1 -6 107.62 4.46 0
11 1 -5 1028.25 12.13 0
11 1 -4 570.47 9.03 0
11 1 -3 237.63 5.88 0
11 1 -2 65.58 3.53 0
11 1 -1 0.74 1.66 0
13 1 -1 512.80 9.30 0
13 1 -2 82.98 4.15 0
13 1 -3 63.84 3.61 0
13 1 -4 4.30 1.80 0
13 1 -5 30.05 2.79 0
13 1 -6 10.11 2.18 0
13 1 -7 576.13 10.37 0
13 1 -8 12.78 2.44 0
13 1 -9 302.68 7.87 0
13 1 -10 149.08 5.79 0
13 1 -11 3.89 2.00 0
13 1 -12 44.13 3.73 0
13 1 -13 168.50 6.62 0
13 1 -14 16.33 2.89 0
13 1 -15 12.33 2.68 0
13 1 -16 6.79 2.63 0
13 1 -17 2.36 2.45 0
13 1 -18 16.53 3.42 0
13 1 -19 33.52 4.14 0
13 1 -20 263.16 9.61 0
13 1 -21 7.86 3.14 0
13 1 -22 8.73 2.97 0
13 1 -23 124.33 7.21 0
13 1 -24 -0.27 2.35 0
13 1 -25 4.86 2.91 0
13 1 -26 10.25 3.42 0
15 1 -25 5.50 3.05 0
15 1 -24 13.39 3.51 0
15 1 -23 31.14 4.54 0
15 1 -22 56.21 5.34 0
15 1 -21 74.54 5.92 0
15 1 -20 68.70 5.56 0
15 1 -19 12.34 3.29 0
15 1 -18 15.80 3.42 0
15 1 -17 5.05 2.48 0
15 1 -16 3.05 2.57 0
15 1 -15 93.29 5.68 0
15 1 -14 18.36 3.27 0
15 1 -13 12.08 2.59 0
15 1 -12 54.36 4.28 0
15 1 -11 70.40 4.70 0
15 1 -10 6.36 2.28 0
15 1 -9 153.18 6.41 0
15 1 -8 131.64 5.88 0
15 1 -7 14.88 2.57 0
15 1 -6 307.21 7.85 0
15 1 -5 356.28 8.65 0
15 1 -4 41.91 3.42 0
15 1 -3 51.03 3.65 0
15 1 -2 333.10 7.98 0
15 1 -1 893.37 13.19 0
17 1 -1 773.17 12.96 0
17 1 -2 29.06 3.22 0
17 1 -3 23.69 3.03 0
17 1 -4 50.65 3.86 0
17 1 -5 63.04 4.44 0
17 1 -6 363.43 9.50 0
17 1 -7 9.73 2.52 0
17 1 -8 0.36 2.06 0
17 1 -9 1.97 2.27 0
17 1 -10 8.45 2.59 0
17 1 -11 31.96 3.81 0
17 1 -12 293.46 9.23 0
17 1 -13 448.98 11.31 0
17 1 -14 216.36 8.49 0
17 1 -15 6.44 2.83 0
17 1 -16 78.91 5.63 0
17 1 -17 27.34 3.98 0
17 1 -18 90.45 6.16 0
17 1 -19 27.04 4.19 0
17 1 -20 30.18 4.43 0
17 1 -21 91.89 6.45 0
17 1 -22 7.73 3.21 0
17 1 -23 -0.04 2.61 0
17 1 -24 9.25 3.52 0
19 1 -22 5.68 3.22 0
19 1 -21 17.33 3.82 0
19 1 -20 16.58 3.83 0
19 1 -19 10.55 3.20 0
19 1 -18 96.56 6.69 0
19 1 -17 9.86 3.33 0
19 1 -16 54.21 5.07 0
19 1 -15 1.51 2.72 0
19 1 -14 8.34 2.75 0
19 1 -13 1.61 2.56 0
19 1 -12 34.56 4.10 0
19 1 -11 19.45 3.34 0
19 1 -10 2.21 2.40 0
19 1 -9 148.10 6.97 0
19 1 -8 8.12 2.61 0
19 1 -7 270.15 8.69 0
19 1 -6 17.10 3.15 0
19 1 -5 91.50 5.31 0
19 1 -4 21.17 3.04 0
19 1 -3 21.04 3.11 0
19 1 -2 2.09 1.88 0
19 1 -1 8.84 2.42 0
21 1 -1 -2.55 1.83 0
21 1 -2 -0.39 2.00 0
21 1 -3 60.80 4.68 0
21 1 -4 13.35 2.83 0
21 1 -5 237.60 8.65 0
21 1 -6 87.55 5.77 0
21 1 -7 45.05 4.37 0
21 1 -8 43.21 4.35 0
21 1 -9 62.39 5.04 0
21 1 -10 2.28 2.52 0
21 1 -11 169.22 8.17 0
21 1 -12 51.73 5.17 0
21 1 -13 304.71 10.94 0
21 1 -14 2.49 2.45 0
21 1 -15 24.40 4.03 0
21 1 -16 2.32 2.71 0
21 1 -17 115.29 7.22 0
21 1 -18 23.21 4.19 0
21 1 -19 51.03 5.36 0
21 1 -20 13.54 3.68 0
23 1 -16 -1.71 2.37 0
23 1 -15 0.04 3.03 0
23 1 -14 28.88 4.68 0
23 1 -13 3.95 2.79 0
23 1 -12 3.75 2.87 0
23 1 -11 3.22 2.86 0
23 1 -10 88.04 6.28 0
23 1 -9 106.68 6.61 0
23 1 -8 14.37 3.28 0
23 1 -7 1.72 2.49 0
23 1 -6 0.42 2.40 0
23 1 -5 21.01 3.52 0
23 1 -4 22.51 3.60 0
23 1 -3 51.73 4.83 0
23 1 -2 75.83 5.48 0
23 1 -1 113.50 6.54 0
25 1 -1 13.06 3.39 0
25 1 -2 6.27 2.91 0
25 1 -3 35.67 4.51 0
25 1 -4 3.99 2.72 0
25 1 -5 48.43 4.96 0
25 1 -6 8.88 3.04 0
25 1 -7 31.44 4.55 0
25 1 -8 21.19 4.00 0
25 1 -9 2.92 2.66 0
25 1 -10 12.97 3.37 0
24 2 -12 57.82 5.92 0
24 2 -11 3.80 2.92 0
24 2 -10 27.35 4.41 0
24 2 -9 60.63 5.43 0
24 2 -8 3.17 2.81 0
24 2 -7 6.01 2.83 0
24 2 -6 3.23 2.44 0
24 2 -5 -4.29 1.89 0
24 2 -4 69.27 5.60 0
24 2 -3 1.59 2.51 0
24 2 -2 11.97 3.24 0
24 2 -1 8.88 3.25 0
22 2 -1 -0.03 2.52 0
22 2 -2 35.09 4.44 0
22 2 -3 57.67 5.14 0
22 2 -4 62.71 5.36 0
22 2 -5 15.23 3.03 0
22 2 -6 45.75 4.47 0
22 2 -7 20.53 3.66 0
22 2 -8 77.91 6.17 0
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 50346
_shelx_res_file
;
TITL PDNSI9 #365 for VL/MS in C2/c
i.res
created by SHELXL-2018/3 at 15:09:24 on 10-Jan-2024
REM PDNSI9 #365 for VL/MS in C2/c
REM 163 parameters refined using 0 restraints
CELL 0.71073 21.609 8.198 24.151 90 100.17 90
ZERR 4 0.004 0.003 0.003 0 0.013 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N S Pd I
UNIT 48 104 8 16 8 56
EQIV $1 1-X,-1+Y,0.5-Z
L.S. 10
PLAN 17
SIZE 0.26 0.14 0.13
TEMP -53(2)
CONF
FREE I6 I3
FREE I4 I3
BIND I3 I7_$1
FREE I3 I2
BOND
MORE -1
BOND $H
fmap -2
acta
OMIT -4 180
OMIT 2 2 7
REM
REM
REM
WGHT 0.068100 91.853203
FVAR 0.06428
PD 5 0.745577 0.209756 0.410953 11.00000 0.02773 0.03165 =
0.01914 0.00310 0.00175 0.00144
I 6 0.743550 -0.070579 0.458432 11.00000 0.04458 0.03852 =
0.03563 0.00559 0.00660 0.00073
N1 3 0.747210 0.422408 0.364544 11.00000 0.03604 0.03639 =
0.02491 0.00666 0.00365 0.00540
AFIX 13
H1 2 0.745717 0.388974 0.324940 11.00000 -1.20000
AFIX 0
C2 1 0.691441 0.521687 0.365795 11.00000 0.04002 0.03377 =
0.03162 0.01115 0.00201 0.00505
AFIX 23
H2A 2 0.689655 0.611209 0.338668 11.00000 -1.20000
H2B 2 0.693364 0.568860 0.403345 11.00000 -1.20000
AFIX 0
C3 1 0.633374 0.416160 0.351193 11.00000 0.03272 0.04130 =
0.02057 0.00741 -0.00297 0.00993
AFIX 23
H3A 2 0.628665 0.382092 0.311775 11.00000 -1.20000
H3B 2 0.596243 0.480422 0.355395 11.00000 -1.20000
AFIX 0
S4 4 0.637304 0.237103 0.395463 11.00000 0.02749 0.04457 =
0.01826 0.00054 -0.00112 0.00187
C5 1 0.622116 0.330337 0.460954 11.00000 0.03127 0.03444 =
0.01850 -0.00022 0.00506 0.00583
AFIX 23
H5A 2 0.654611 0.411792 0.474030 11.00000 -1.20000
H5B 2 0.581340 0.385964 0.453828 11.00000 -1.20000
AFIX 0
C6 1 0.621996 0.202586 0.505793 11.00000 0.03184 0.03840 =
0.01455 -0.00435 -0.00416 -0.00021
AFIX 23
H6A 2 0.650767 0.114176 0.500145 11.00000 -1.20000
H6B 2 0.579687 0.156393 0.502622 11.00000 -1.20000
AFIX 0
S7 4 0.645732 0.287744 0.574790 11.00000 0.02960 0.03672 =
0.01887 0.00069 0.00481 0.00307
C8 1 0.638627 0.108722 0.617514 11.00000 0.02970 0.04234 =
0.02740 -0.00481 0.00463 -0.00026
AFIX 23
H8A 2 0.637648 0.143110 0.656212 11.00000 -1.20000
H8B 2 0.598808 0.053577 0.603074 11.00000 -1.20000
AFIX 0
C9 1 0.692150 -0.009966 0.617716 11.00000 0.04769 0.02742 =
0.02644 0.00043 0.01107 -0.00437
AFIX 23
H9A 2 0.688681 -0.099724 0.643794 11.00000 -1.20000
H9B 2 0.690389 -0.055880 0.580004 11.00000 -1.20000
AFIX 0
I1 6 0.174110 0.491100 0.276320 11.00000 0.07072 0.06094 =
0.02750 -0.00296 -0.00026 0.00726
I2 6 0.304156 0.447291 0.299335 11.00000 0.07355 0.04511 =
0.02427 -0.00444 0.01277 -0.00623
I3 6 0.446473 0.358476 0.331096 11.00000 0.05159 0.08445 =
0.05376 -0.00748 0.00959 -0.00545
I4 6 0.443215 0.285027 0.460911 11.00000 0.03101 0.04775 =
0.06656 -0.01412 -0.00235 0.00199
I5 6 0.454210 0.210535 0.573861 11.00000 0.04830 0.07400 =
0.06166 -0.01116 0.00798 0.00605
PART -1
I6 6 0.480621 0.709181 0.271882 10.50000 0.06122 0.09613 =
0.04651 -0.00942 -0.00214 0.02543
I7 6 0.506580 1.000491 0.222478 10.50000 0.05775 0.10240 =
0.04509 -0.00409 0.00265 0.02833
HKLF 4
REM PDNSI9 #365 for VL/MS in C2/c
REM wR2 = 0.1361, GooF = S = 1.079, Restrained GooF = 1.079 for all data
REM R1 = 0.0506 for 3059 Fo > 4sig(Fo) and 0.0634 for all 3715 data
REM 163 parameters refined using 0 restraints
END
WGHT 0.0681 90.6646
REM Highest difference peak 1.349, deepest hole -1.615, 1-sigma level 0.274
Q1 1 0.7290 -0.0625 0.4296 11.00000 0.05 -1.61
Q2 1 0.7602 -0.0367 0.4868 11.00000 0.05 -1.41
Q3 1 0.2820 0.3483 0.2940 11.00000 0.05 1.35
Q4 1 0.7706 -0.0760 0.4549 11.00000 0.05 -1.34
Q5 1 0.5270 1.1072 0.2185 11.00000 0.05 1.33
Q6 1 0.3359 0.3619 0.2998 11.00000 0.05 1.32
Q7 1 0.7612 -0.0916 0.4794 11.00000 0.05 -1.31
Q8 1 0.4523 0.1373 0.5884 11.00000 0.05 1.30
Q9 1 0.2830 0.5421 0.2956 11.00000 0.05 1.29
Q10 1 0.4719 0.2863 0.5799 11.00000 0.05 1.27
Q11 1 0.7237 0.1045 0.4108 11.00000 0.05 1.22
Q12 1 0.1452 0.5425 0.2393 11.00000 0.05 -1.20
Q13 1 0.3289 0.4891 0.3392 11.00000 0.05 -1.20
Q14 1 0.7734 0.2729 0.4539 11.00000 0.05 -1.19
Q15 1 0.7172 -0.1983 0.4512 11.00000 0.05 1.18
Q16 1 0.7239 0.2525 0.3720 11.00000 0.05 -1.18
Q17 1 0.1963 0.4138 0.2678 11.00000 0.05 1.17
;
_shelx_res_checksum 95310
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_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 Pd 0.74558(4) 0.20976(10) 0.41095(3) 0.0265(2) Uani d 1 . .
I I 0.74355(4) -0.07058(10) 0.45843(3) 0.0396(2) Uani d 1 . .
N N1 0.7472(4) 0.4224(12) 0.3645(4) 0.033(2) Uani d 1 . .
H H1 0.745717 0.388974 0.324940 0.039 Uiso calc 1 . .
C C2 0.6914(6) 0.5217(15) 0.3658(5) 0.036(3) Uani d 1 . .
H H2A 0.689655 0.611209 0.338668 0.043 Uiso calc 1 . .
H H2B 0.693364 0.568860 0.403345 0.043 Uiso calc 1 . .
C C3 0.6334(5) 0.4162(15) 0.3512(4) 0.032(3) Uani d 1 . .
H H3A 0.628665 0.382092 0.311775 0.039 Uiso calc 1 . .
H H3B 0.596243 0.480422 0.355395 0.039 Uiso calc 1 . .
S S4 0.63730(13) 0.2371(4) 0.39546(11) 0.0307(6) Uani d 1 . .
C C5 0.6221(5) 0.3303(14) 0.4610(4) 0.028(2) Uani d 1 . .
H H5A 0.654611 0.411792 0.474030 0.034 Uiso calc 1 . .
H H5B 0.581340 0.385964 0.453828 0.034 Uiso calc 1 . .
C C6 0.6220(5) 0.2026(14) 0.5058(4) 0.029(2) Uani d 1 . .
H H6A 0.650767 0.114176 0.500145 0.035 Uiso calc 1 . .
H H6B 0.579687 0.156393 0.502622 0.035 Uiso calc 1 . .
S S7 0.64573(13) 0.2877(4) 0.57479(11) 0.0283(6) Uani d 1 . .
C C8 0.6386(5) 0.1087(15) 0.6175(5) 0.033(3) Uani d 1 . .
H H8A 0.637648 0.143110 0.656212 0.040 Uiso calc 1 . .
H H8B 0.598808 0.053577 0.603074 0.040 Uiso calc 1 . .
C C9 0.6921(6) -0.0100(14) 0.6177(5) 0.033(3) Uani d 1 . .
H H9A 0.688681 -0.099724 0.643794 0.040 Uiso calc 1 . .
H H9B 0.690389 -0.055880 0.580004 0.040 Uiso calc 1 . .
I I1 0.17411(5) 0.49110(13) 0.27632(4) 0.0541(3) Uani d 1 . .
I I2 0.30416(5) 0.44729(11) 0.29934(3) 0.0471(3) Uani d 1 . .
I I3 0.44647(5) 0.35848(16) 0.33110(4) 0.0632(3) Uani d 1 . .
I I4 0.44322(4) 0.28503(11) 0.46091(4) 0.0498(3) Uani d 1 . .
I I5 0.45421(5) 0.21053(14) 0.57386(5) 0.0615(3) Uani d 1 . .
I I6 0.48062(11) 0.7092(3) 0.27188(9) 0.0694(6) Uani d 0.5 A -1
I I7 0.50658(10) 1.0005(3) 0.22248(9) 0.0692(6) Uani d 0.5 A -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
Pd 0.0277(4) 0.0317(5) 0.0191(4) 0.0014(4) 0.0018(3) 0.0031(3)
I 0.0446(5) 0.0385(5) 0.0356(4) 0.0007(4) 0.0066(3) 0.0056(3)
N1 0.036(5) 0.036(5) 0.025(5) 0.005(4) 0.004(4) 0.007(4)
C2 0.040(6) 0.034(6) 0.032(6) 0.005(5) 0.002(5) 0.011(5)
C3 0.033(6) 0.041(7) 0.021(5) 0.010(5) -0.003(4) 0.007(5)
S4 0.0275(13) 0.0446(17) 0.0183(12) 0.0019(12) -0.0011(10) 0.0005(12)
C5 0.031(5) 0.034(6) 0.019(5) 0.006(5) 0.005(4) 0.000(5)
C6 0.032(6) 0.038(6) 0.015(5) 0.000(5) -0.004(4) -0.004(5)
S7 0.0296(13) 0.0367(15) 0.0189(12) 0.0031(12) 0.0048(10) 0.0007(11)
C8 0.030(6) 0.042(7) 0.027(6) 0.000(5) 0.005(5) -0.005(5)
C9 0.048(7) 0.027(6) 0.026(6) -0.004(5) 0.011(5) 0.000(5)
I1 0.0707(6) 0.0609(6) 0.0275(4) 0.0073(5) -0.0003(4) -0.0030(4)
I2 0.0735(6) 0.0451(5) 0.0243(4) -0.0062(4) 0.0128(4) -0.0044(3)
I3 0.0516(6) 0.0845(8) 0.0538(6) -0.0055(5) 0.0096(5) -0.0075(5)
I4 0.0310(4) 0.0478(5) 0.0666(6) 0.0020(4) -0.0023(4) -0.0141(5)
I5 0.0483(5) 0.0740(7) 0.0617(6) 0.0060(5) 0.0080(5) -0.0112(5)
I6 0.0612(12) 0.0961(17) 0.0465(11) 0.0254(12) -0.0021(9) -0.0094(11)
I7 0.0578(12) 0.1024(18) 0.0451(10) 0.0283(12) 0.0026(9) -0.0041(11)
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'
S S 0.1246 0.1234 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.0660
0.00 0.00 1.00 0.0660
0.00 1.00 1.00 0.0680
1.00 -1.00 0.00 0.0680
-1.00 0.00 0.00 0.1280
1.00 0.00 0.00 0.1280
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 Pd I . . 173.8(3) ?
N1 Pd S4 . . 86.8(3) ?
N1 Pd S7 . 7_656 87.7(3) ?
S4 Pd I . . 93.57(8) ?
S7 Pd I 7_656 . 92.20(8) ?
S7 Pd S4 7_656 . 173.88(11) ?
Pd N1 H1 . . 106.8 ?
C2 N1 Pd . . 111.4(7) ?
C2 N1 H1 . . 106.8 ?
C2 N1 C9 . 7_656 114.4(9) ?
C9 N1 Pd 7_656 . 110.3(7) ?
C9 N1 H1 7_656 . 106.8 ?
N1 C2 H2A . . 109.8 ?
N1 C2 H2B . . 109.8 ?
N1 C2 C3 . . 109.3(10) ?
H2A C2 H2B . . 108.3 ?
C3 C2 H2A . . 109.8 ?
C3 C2 H2B . . 109.8 ?
C2 C3 H3A . . 109.2 ?
C2 C3 H3B . . 109.2 ?
C2 C3 S4 . . 112.1(7) ?
H3A C3 H3B . . 107.9 ?
S4 C3 H3A . . 109.2 ?
S4 C3 H3B . . 109.2 ?
C3 S4 Pd . . 96.6(4) ?
C3 S4 C5 . . 100.0(5) ?
C5 S4 Pd . . 103.3(4) ?
S4 C5 H5A . . 109.5 ?
S4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 108.1 ?
C6 C5 S4 . . 110.7(8) ?
C6 C5 H5A . . 109.5 ?
C6 C5 H5B . . 109.5 ?
C5 C6 H6A . . 109.4 ?
C5 C6 H6B . . 109.4 ?
C5 C6 S7 . . 111.1(8) ?
H6A C6 H6B . . 108.0 ?
S7 C6 H6A . . 109.4 ?
S7 C6 H6B . . 109.4 ?
C6 S7 Pd . 7_656 104.9(4) ?
C6 S7 C8 . . 100.0(5) ?
C8 S7 Pd . 7_656 96.2(4) ?
S7 C8 H8A . . 109.1 ?
S7 C8 H8B . . 109.1 ?
H8A C8 H8B . . 107.9 ?
C9 C8 S7 . . 112.4(8) ?
C9 C8 H8A . . 109.1 ?
C9 C8 H8B . . 109.1 ?
N1 C9 C8 7_656 . 109.0(9) ?
N1 C9 H9A 7_656 . 109.9 ?
N1 C9 H9B 7_656 . 109.9 ?
C8 C9 H9A . . 109.9 ?
C8 C9 H9B . . 109.9 ?
H9A C9 H9B . . 108.3 ?
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
Pd I . 2.5722(14) ?
Pd N1 . 2.076(9) ?
Pd S4 . 2.314(3) ?
Pd S7 7_656 2.313(3) ?
N1 H1 . 0.9900 ?
N1 C2 . 1.459(15) ?
N1 C9 7_656 1.489(16) ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
C2 C3 . 1.514(17) ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 S4 . 1.809(11) ?
S4 C5 . 1.838(10) ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C5 C6 . 1.507(15) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 S7 . 1.796(10) ?
S7 C8 . 1.816(12) ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 C9 . 1.511(16) ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
I1 I2 . 2.7899(15) ?
I3 I7 2_645 3.432(3) ?
I4 I5 . 2.7644(16) ?
I6 I7 . 2.771(4) ?
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
Pd N1 C2 C3 . . . . -49.8(11) ?
Pd S4 C5 C6 . . . . -81.5(8) ?
Pd S7 C8 C9 7_656 . . . -30.4(8) ?
N1 C2 C3 S4 . . . . 53.8(11) ?
C2 C3 S4 Pd . . . . -29.9(9) ?
C2 C3 S4 C5 . . . . 74.9(9) ?
C3 S4 C5 C6 . . . . 179.2(8) ?
S4 C5 C6 S7 . . . . 151.6(6) ?
C5 C6 S7 Pd . . . 7_656 -82.2(8) ?
C5 C6 S7 C8 . . . . 178.6(8) ?
C6 S7 C8 C9 . . . . 76.0(9) ?
S7 C8 C9 N1 . . . 7_656 54.5(11) ?
C9 N1 C2 C3 7_656 . . . -175.8(9) ?