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#$Date: 2024-08-05 22:50:58 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293917 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/33/7063315.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_7063315
loop_
_publ_author_name
'Kwon, Hyoung Soon'
'Park, Geon Hyeong'
'Ju, Huiyeong'
'Lee, Eunji'
'Kim, Yong-Joo'
_publ_section_title
;
 Facile formation of tetrazole--thiolato Pd(ii) and Pt(ii) complexes
 through deprotonation or oxidative addition using organic
 tetrazole--thiones
;
_journal_issue                   30
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13358
_journal_page_last               13372
_journal_paper_doi               10.1039/D4NJ01429D
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C28 H42 N8 P2 Pd S2, C H2 Cl2'
_chemical_formula_sum            'C29 H44 Cl2 N8 P2 Pd S2'
_chemical_formula_weight         808.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2024-03-07 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1391(7)
_cell_length_b                   19.4487(11)
_cell_length_c                   15.6956(8)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.37
_cell_volume                     3705.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70396
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.337
_diffrn_reflns_theta_min         2.094
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 1595 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0269P)²+2.0377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0606
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                4004
_reflns_number_total             4619
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj01429d2.cif
_cod_data_source_block           KSH-30
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7063314--7063321.cif.
;
_cod_database_code               7063315
_shelx_shelxl_version_number     2018/1
_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   0.880
_shelx_estimated_absorpt_t_max   0.941
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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 0.500000 0.53120(2) 0.750000 0.02154(9) Uani 1 2 d S T P . .
P1 P 0.42020(9) 0.61652(5) 0.67552(6) 0.0337(2) Uani 1 1 d . . . . .
S1 S 0.59475(9) 0.44784(5) 0.83425(6) 0.0356(2) Uani 1 1 d . . . . .
N1 N 0.7388(3) 0.35320(15) 0.77649(18) 0.0285(7) Uani 1 1 d . . . . .
N2 N 0.7916(3) 0.33410(18) 0.7040(2) 0.0376(8) Uani 1 1 d . . . . .
N3 N 0.7606(3) 0.37676(19) 0.6458(2) 0.0404(8) Uani 1 1 d . . . . .
N4 N 0.6887(3) 0.42374(16) 0.67726(19) 0.0349(7) Uani 1 1 d . . . . .
C1 C 0.4872(5) 0.69757(17) 0.7028(2) 0.0479(12) Uani 1 1 d . . . . .
H1A H 0.555321 0.702729 0.669987 0.057 Uiso 1 1 calc R U . . .
H1B H 0.438453 0.736172 0.689011 0.057 Uiso 1 1 calc R U . . .
C2 C 0.4345(4) 0.6074(3) 0.5607(3) 0.0497(13) Uani 1 1 d . . . . .
H2A H 0.385467 0.570843 0.540540 0.060 Uiso 1 1 calc R U . . .
H2B H 0.412598 0.650375 0.532866 0.060 Uiso 1 1 calc R U . . .
C3 C 0.5519(4) 0.5903(3) 0.5368(3) 0.0513(13) Uani 1 1 d . . . . .
H3A H 0.600413 0.626568 0.556543 0.077 Uiso 1 1 calc R U . . .
H3B H 0.557638 0.586232 0.475350 0.077 Uiso 1 1 calc R U . . .
H3C H 0.572928 0.547125 0.563082 0.077 Uiso 1 1 calc R U . . .
C4 C 0.2764(4) 0.6358(3) 0.7011(4) 0.0697(16) Uani 1 1 d . . . . .
H4A H 0.273254 0.649614 0.761135 0.084 Uiso 1 1 calc R U . . .
H4B H 0.254322 0.675821 0.667222 0.084 Uiso 1 1 calc R U . . .
C5 C 0.1970(5) 0.5841(3) 0.6886(6) 0.107(3) Uani 1 1 d . . . . .
H5A H 0.206075 0.564322 0.632267 0.161 Uiso 1 1 calc R U . . .
H5B H 0.123845 0.603829 0.693453 0.161 Uiso 1 1 calc R U . . .
H5C H 0.206237 0.548538 0.731274 0.161 Uiso 1 1 calc R U . . .
C6 C 0.6752(3) 0.40872(16) 0.7589(3) 0.0269(7) Uani 1 1 d . . . . .
C7 C 0.7626(3) 0.32106(18) 0.8560(2) 0.0273(8) Uani 1 1 d . . . . .
C8 C 0.6926(3) 0.26952(19) 0.8867(2) 0.0332(9) Uani 1 1 d . . . . .
C9 C 0.7207(4) 0.2375(2) 0.9626(3) 0.0412(11) Uani 1 1 d . . . . .
H9 H 0.675928 0.202140 0.984251 0.049 Uiso 1 1 calc R U . . .
C10 C 0.8134(4) 0.2572(2) 1.0063(3) 0.0473(12) Uani 1 1 d . . . . .
H10 H 0.831758 0.234967 1.057565 0.057 Uiso 1 1 calc R U . . .
C11 C 0.8795(4) 0.3089(2) 0.9761(3) 0.0450(11) Uani 1 1 d . . . . .
H11 H 0.941918 0.322043 1.007575 0.054 Uiso 1 1 calc R U . . .
C12 C 0.8560(3) 0.3422(2) 0.8997(3) 0.0371(9) Uani 1 1 d . . . . .
C13 C 0.5911(4) 0.2506(2) 0.8384(3) 0.0494(11) Uani 1 1 d . . . . .
H13A H 0.562110 0.207553 0.860107 0.074 Uiso 1 1 calc R U . . .
H13B H 0.609034 0.245425 0.778464 0.074 Uiso 1 1 calc R U . . .
H13C H 0.536307 0.286462 0.845063 0.074 Uiso 1 1 calc R U . . .
C14 C 0.9288(4) 0.3984(3) 0.8667(3) 0.0581(13) Uani 1 1 d . . . . .
H14A H 0.890375 0.441996 0.870373 0.087 Uiso 1 1 calc R U . . .
H14B H 0.947609 0.389094 0.807697 0.087 Uiso 1 1 calc R U . . .
H14C H 0.995592 0.400407 0.900494 0.087 Uiso 1 1 calc R U . . .
C15 C -0.1850(7) 0.500000 0.500000 0.066(2) Uani 1 2 d S T P . .
H15A H -0.232527 0.469362 0.533277 0.080 Uiso 0.5 1 calc R U P . .
H15B H -0.232532 0.530636 0.466724 0.080 Uiso 0.5 1 calc R U P . .
Cl1 Cl -0.10481(15) 0.54894(8) 0.56917(11) 0.0871(5) 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 0.0033 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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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
P1 Pd1 P1 84.91(6) 3_656 . ?
P1 Pd1 S1 175.13(4) 3_656 3_656 ?
P1 Pd1 S1 90.32(4) . 3_656 ?
P1 Pd1 S1 90.32(4) 3_656 . ?
P1 Pd1 S1 175.13(4) . . ?
S1 Pd1 S1 94.46(5) 3_656 . ?
C2 P1 C1 105.9(2) . . ?
C2 P1 C4 109.2(3) . . ?
C1 P1 C4 101.3(3) . . ?
C2 P1 Pd1 113.69(16) . . ?
C1 P1 Pd1 108.87(16) . . ?
C4 P1 Pd1 116.61(18) . . ?
C6 S1 Pd1 101.18(13) . . ?
C6 N1 N2 108.4(3) . . ?
C6 N1 C7 130.0(3) . . ?
N2 N1 C7 121.2(3) . . ?
N3 N2 N1 106.2(3) . . ?
N2 N3 N4 111.4(3) . . ?
C6 N4 N3 106.4(3) . . ?
C1 C1 P1 108.8(2) 3_656 . ?
C3 C2 P1 111.0(3) . . ?
C5 C4 P1 118.4(5) . . ?
N4 C6 N1 107.6(3) . . ?
N4 C6 S1 129.9(3) . . ?
N1 C6 S1 122.5(3) . . ?
C12 C7 C8 122.6(3) . . ?
C12 C7 N1 117.9(3) . . ?
C8 C7 N1 119.5(3) . . ?
C9 C8 C7 117.9(4) . . ?
C9 C8 C13 121.9(4) . . ?
C7 C8 C13 120.2(3) . . ?
C10 C9 C8 120.4(4) . . ?
C11 C10 C9 120.8(4) . . ?
C10 C11 C12 121.3(4) . . ?
C7 C12 C11 117.0(4) . . ?
C7 C12 C14 121.9(4) . . ?
C11 C12 C14 121.1(4) . . ?
Cl1 C15 Cl1 112.0(4) 4_566 . ?
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 P1 2.2491(10) 3_656 ?
Pd1 P1 2.2491(10) . ?
Pd1 S1 2.3875(9) 3_656 ?
Pd1 S1 2.3875(9) . ?
P1 C2 1.819(4) . ?
P1 C1 1.825(5) . ?
P1 C4 1.830(5) . ?
S1 C6 1.712(4) . ?
N1 C6 1.356(4) . ?
N1 N2 1.359(4) . ?
N1 C7 1.426(4) . ?
N2 N3 1.289(5) . ?
N3 N4 1.356(5) . ?
N4 C6 1.324(5) . ?
C1 C1 1.513(8) 3_656 ?
C2 C3 1.510(6) . ?
C4 C5 1.407(8) . ?
C7 C12 1.387(5) . ?
C7 C8 1.400(5) . ?
C8 C9 1.386(6) . ?
C8 C13 1.493(6) . ?
C9 C10 1.373(6) . ?
C10 C11 1.371(7) . ?
C11 C12 1.393(6) . ?
C12 C14 1.497(6) . ?
C15 Cl1 1.741(5) 4_566 ?
C15 Cl1 1.741(5) . ?
