#------------------------------------------------------------------------------
#$Date: 2022-01-18 12:40:19 +0200 (Tue, 18 Jan 2022) $
#$Revision: 272103 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/60/1566024.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_1566024
loop_
_publ_author_name
'Karmakar, Gourab'
'Tyagi, Adish'
'Kedarnath, G.'
'Naveen Kumar, N.'
'Phadnis, Prasad P.'
'Mishra, Ratikanta'
'Kumar, Mukesh'
_publ_section_title
;
 Preparation and characterization of colloidal Pd17Se15 nanoparticles from
 a novel Pd(II) pyridyl selenoether molecular precursor
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120668
_journal_paper_doi               10.1016/j.ica.2021.120668
_journal_volume                  529
_journal_year                    2022
_chemical_formula_moiety         'C14 H12 Cl2 N2 O4 Pd Se2'
_chemical_formula_sum            'C14 H12 Cl2 N2 O4 Pd Se2'
_chemical_formula_weight         607.48
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   25.3661(9)
_cell_length_b                   25.3661(9)
_cell_length_c                   17.4250(11)
_cell_measurement_reflns_used    3053
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.2870
_cell_measurement_theta_min      5.4560
_cell_volume                     9709.8(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1600
_diffrn_detector_type            Titan
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -66.00  33.00   1.00    5.00    --  -43.29  19.00-150.00   99
  2  ω     78.00 153.00   1.00   35.00    --  102.90  61.00 120.00   75
  3  ω    100.00 130.00   1.00   35.00    --  102.90 -61.00 -30.00   30
  4  ω     40.00  75.00   1.00   35.00    --  102.90 -61.00 -30.00   35
  5  ω     20.00  48.00   1.00   35.00    --  102.90 -95.00   0.00   28
  6  ω     25.00  91.00   1.00   35.00    --  102.90 -95.00 -30.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0323479000
_diffrn_orient_matrix_UB_12      -0.0369563000
_diffrn_orient_matrix_UB_13      0.0132076000
_diffrn_orient_matrix_UB_21      -0.0469954000
_diffrn_orient_matrix_UB_22      -0.0510244000
_diffrn_orient_matrix_UB_23      -0.0520094000
_diffrn_orient_matrix_UB_31      0.0407209000
_diffrn_orient_matrix_UB_32      0.0308059000
_diffrn_orient_matrix_UB_33      -0.0702903000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6493
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.047
_diffrn_reflns_theta_min         3.485
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.256
_exptl_absorpt_correction_T_max  0.441
_exptl_absorpt_correction_T_min  0.095
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_description       needle
_exptl_crystal_F_000             5220
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0867
_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)+(0.1102P)²+248.3120P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2256
_refine_ls_wR_factor_ref         0.2493
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1511
_reflns_number_total             2076
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2022-529-120668.cif
_cod_data_source_block           prasad3_1
_cod_original_cell_volume        9709.9(9)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               1566024
_chemical_oxdiff_formula         'C14 H12 Cl2 N2 O4 Pd Se2'
_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.
;
_reflns_odcompleteness_completeness 97.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.593
_oxdiff_exptl_absorpt_empirical_full_min 0.279
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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 0.66820(4) 0.6667 0.4167 0.0547(4) Uani 1 2 d S T P . .
Se1 Se 0.64431(8) 0.55726(7) 0.30075(10) 0.0881(6) Uani 1 1 d . . . . .
Cl1 Cl 0.75862(15) 0.6667 0.4167 0.0795(14) Uani 1 2 d S T P . .
Cl2 Cl 0.57808(15) 0.6667 0.4167 0.0746(13) Uani 1 2 d S T P . .
O1 O 0.6518(13) 0.4452(12) 0.250(2) 0.31(2) Uani 1 1 d . . . . .
O2 O 0.5745(11) 0.3986(10) 0.1886(18) 0.229(11) Uani 1 1 d . . . . .
N1 N 0.6226(4) 0.5775(4) 0.4512(6) 0.057(2) Uani 1 1 d . . . . .
C1 C 0.6027(6) 0.5653(6) 0.5224(8) 0.068(3) Uani 1 1 d . . . . .
H1 H 0.6108 0.5974 0.5551 0.081 Uiso 1 1 calc R . . . .
C2 C 0.5711(7) 0.5081(6) 0.5495(9) 0.084(4) Uani 1 1 d . . . . .
H2 H 0.5584 0.5006 0.6005 0.101 Uiso 1 1 calc R . . . .
C3 C 0.5580(7) 0.4610(6) 0.4999(12) 0.102(6) Uani 1 1 d . . . . .
H3 H 0.5356 0.4209 0.5167 0.123 Uiso 1 1 calc R . . . .
C4 C 0.5781(7) 0.4732(6) 0.4254(10) 0.087(4) Uani 1 1 d . . . . .
H4 H 0.5694 0.4414 0.3917 0.104 Uiso 1 1 calc R . . . .
C5 C 0.6116(5) 0.5331(5) 0.4003(8) 0.069(3) Uani 1 1 d . . . . .
C6 C 0.5867(6) 0.4855(7) 0.2424(10) 0.082(4) Uani 1 1 d . . . . .
H6A H 0.5481 0.4655 0.2693 0.099 Uiso 1 1 calc R . . . .
H6B H 0.5799 0.4984 0.1928 0.099 Uiso 1 1 calc R . . . .
C7 C 0.6078(8) 0.4418(8) 0.2308(14) 0.112(6) 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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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'
Se Se -0.7943 1.1372 '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
-3 4 -11 0.3272
15 -2 0 0.0591
1 -4 11 0.1932
-15 2 0 0.0450
8 -1 -9 0.3017
-4 16 0 0.0363
-8 0 9 0.1858
4 -16 0 0.0311
-16 9 0 0.0420
16 -9 0 0.0514
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
Cl2 Pd1 Cl1 180.0 . .
N1 Pd1 Cl1 90.7(2) . .
N1 Pd1 Cl1 90.7(2) 11_565 .
N1 Pd1 Cl2 89.3(2) . .
N1 Pd1 Cl2 89.3(2) 11_565 .
N1 Pd1 N1 178.6(5) 11_565 .
C5 Se1 C6 100.0(6) . .
C1 N1 Pd1 118.3(8) . .
C1 N1 C5 121.9(10) . .
C5 N1 Pd1 119.7(8) . .
N1 C1 H1 118.8 . .
N1 C1 C2 122.5(13) . .
C2 C1 H1 118.8 . .
C1 C2 H2 121.0 . .
C1 C2 C3 118.1(15) . .
C3 C2 H2 121.0 . .
C2 C3 H3 120.1 . .
C4 C3 C2 119.9(13) . .
C4 C3 H3 120.1 . .
C3 C4 H4 120.0 . .
C3 C4 C5 120.0(14) . .
C5 C4 H4 120.0 . .
N1 C5 Se1 117.4(8) . .
N1 C5 C4 117.7(13) . .
C4 C5 Se1 125.0(11) . .
Se1 C6 H6A 109.0 . .
Se1 C6 H6B 109.0 . .
H6A C6 H6B 107.8 . .
C7 C6 Se1 112.9(11) . .
C7 C6 H6A 109.0 . .
C7 C6 H6B 109.0 . .
O1 C7 O2 117(2) . .
O1 C7 C6 129(2) . .
O2 C7 C6 114(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Cl1 2.294(4) .
Pd1 Cl2 2.286(4) .
Pd1 N1 2.049(8) .
Pd1 N1 2.049(8) 11_565
Se1 C5 1.888(14) .
Se1 C6 1.955(14) .
O1 C7 1.12(3) .
O2 C7 1.24(3) .
N1 C1 1.317(16) .
N1 C5 1.348(16) .
C1 H1 0.9300 .
C1 C2 1.345(17) .
C2 H2 0.9300 .
C2 C3 1.37(2) .
C3 H3 0.9300 .
C3 C4 1.37(2) .
C4 H4 0.9300 .
C4 C5 1.390(16) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C7 1.47(2) .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.0316 4.4456 -10.8658 -0.4059 0.4808 0.7773
15.0038 -1.6176 0.2002 0.5478 -0.6330 0.5471
1.3057 -4.2804 10.8978 0.3444 -0.4097 -0.8447
-15.0184 1.6610 -0.3103 -0.5513 0.6372 -0.5386
8.4093 -1.1797 -9.4334 0.1910 0.1556 0.9692
-4.2008 15.8848 0.1548 -0.7209 -0.6211 0.3074
-8.1417 0.3174 9.3791 -0.1512 -0.1214 -0.9810
4.2008 -15.8848 -0.1548 0.7209 0.6211 -0.3074
-15.9903 8.9869 0.0082 -0.8493 0.2925 -0.3749
15.9903 -8.9869 -0.0082 0.8493 -0.2925 0.3749
