#------------------------------------------------------------------------------
#$Date: 2019-11-08 02:29:49 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224772 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/80/7058049.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_7058049
loop_
_publ_author_name
'Saxena, Priya'
'Thomas, Jisha Mary'
'Sivasankar, Chinnappan'
'Thirupathi, Natesan'
_publ_section_title
;
 Syntheses and structural aspects of six-membered palladacyclic complexes
 derived from N,N′,N′′-triarylguanidines with N- or
 S-thiocyanate ligands
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2307
_journal_paper_doi               10.1039/C8NJ04167A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C46 H44 N8 Pd2 S2'
_chemical_formula_sum            'C46 H44 N8 Pd2 S2'
_chemical_formula_weight         985.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0567(6)
_cell_length_b                   16.0971(7)
_cell_length_c                   18.9179(10)
_cell_measurement_reflns_used    4371
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.90
_cell_volume                     4280.6(3)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'OLEX 2-2.1'
_computing_publication_material  'WINGX V1.80.01'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.3703
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Sapphire-3 CCD detector'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19693
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.898
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  0.8131
_exptl_absorpt_correction_T_min  0.7987
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0480P)²+5.6208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3655
_reflns_number_total             4371
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj04167a2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to
'empirical' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7058049--7058061.cif.
;
_cod_database_code               7058049
_shelx_shelxl_version_number     2016/6
_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   0.799
_shelx_estimated_absorpt_t_max   0.813
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
N1 N 0.8525(2) 0.2035(2) 0.60976(18) 0.0494(8) Uani 1 1 d . .
N2 N 0.8393(3) 0.3079(2) 0.6932(2) 0.0737(12) Uani 1 1 d . .
H2 H 0.871543 0.339646 0.665567 0.088 Uiso 1 1 calc R U
N3 N 0.7844(3) 0.1758(2) 0.71860(19) 0.0620(10) Uani 1 1 d . .
H3 H 0.796342 0.181803 0.762887 0.074 Uiso 1 1 calc R U
N4 N 0.9886(3) 0.0938(2) 0.5274(2) 0.0543(8) Uani 1 1 d . .
C1 C 0.8266(3) 0.2281(3) 0.6716(2) 0.0528(10) Uani 1 1 d . .
C2 C 0.8818(3) 0.2623(2) 0.5581(2) 0.0488(9) Uani 1 1 d . .
C3 C 0.9735(3) 0.2947(3) 0.5590(3) 0.0650(12) Uani 1 1 d . .
H3A H 1.016533 0.278267 0.593668 0.078 Uiso 1 1 calc R U
C4 C 1.0002(4) 0.3518(3) 0.5079(3) 0.0812(16) Uani 1 1 d . .
H4 H 1.061105 0.374360 0.508325 0.097 Uiso 1 1 calc R U
C5 C 0.9377(6) 0.3744(4) 0.4577(4) 0.098(2) Uani 1 1 d . .
H5 H 0.955743 0.413559 0.424173 0.118 Uiso 1 1 calc R U
C6 C 0.8487(5) 0.3413(4) 0.4548(4) 0.0947(19) Uani 1 1 d . .
H6 H 0.807302 0.356636 0.418693 0.114 Uiso 1 1 calc R U
C7 C 0.8195(4) 0.2841(3) 0.5060(3) 0.0651(12) Uani 1 1 d . .
C8 C 0.7232(4) 0.2470(4) 0.5043(4) 0.104(2) Uani 1 1 d . .
H8A H 0.728466 0.187514 0.503203 0.156 Uiso 1 1 calc R U
H8B H 0.690087 0.265761 0.462943 0.156 Uiso 1 1 calc R U
H8C H 0.688655 0.263487 0.545781 0.156 Uiso 1 1 calc R U
C9 C 0.8047(3) 0.3446(3) 0.7570(2) 0.0568(11) Uani 1 1 d . .
C10 C 0.7203(4) 0.3859(4) 0.7573(3) 0.0837(15) Uani 1 1 d . .
H10 H 0.682283 0.386357 0.717046 0.100 Uiso 1 1 calc R U
C11 C 0.6910(6) 0.4273(4) 0.8176(5) 0.109(2) Uani 1 1 d . .
H11 H 0.633464 0.455831 0.817931 0.131 Uiso 1 1 calc R U
C12 C 0.7458(6) 0.4262(4) 0.8754(4) 0.104(2) Uani 1 1 d . .
H12 H 0.725600 0.453416 0.916112 0.124 Uiso 1 1 calc R U
C13 C 0.8286(6) 0.3867(5) 0.8755(3) 0.0971(19) Uani 1 1 d . .
H13 H 0.865694 0.387077 0.916161 0.116 Uiso 1 1 calc R U
C14 C 0.8611(4) 0.3447(4) 0.8158(3) 0.0736(14) Uani 1 1 d . .
C15 C 0.9564(5) 0.3012(6) 0.8166(4) 0.132(3) Uani 1 1 d . .
H15A H 0.951889 0.250115 0.790581 0.198 Uiso 1 1 calc R U
H15B H 0.974427 0.289533 0.864483 0.198 Uiso 1 1 calc R U
H15C H 1.003398 0.336332 0.795073 0.198 Uiso 1 1 calc R U
C16 C 0.7207(3) 0.1113(2) 0.6970(2) 0.0510(9) Uani 1 1 d . .
C17 C 0.7379(3) 0.0653(2) 0.6355(2) 0.0489(9) Uani 1 1 d . .
C18 C 0.6665(3) 0.0108(2) 0.6143(3) 0.0555(10) Uani 1 1 d . .
H18 H 0.673333 -0.018328 0.572159 0.067 Uiso 1 1 calc R U
C19 C 0.5857(3) -0.0008(3) 0.6545(3) 0.0622(12) Uani 1 1 d . .
H19 H 0.538925 -0.037266 0.638863 0.075 Uiso 1 1 calc R U
C20 C 0.5735(3) 0.0403(3) 0.7167(3) 0.0649(12) Uani 1 1 d . .
H20 H 0.519850 0.029741 0.744021 0.078 Uiso 1 1 calc R U
C21 C 0.6403(3) 0.0981(3) 0.7397(3) 0.0579(11) Uani 1 1 d . .
C22 C 0.6242(4) 0.1450(4) 0.8066(3) 0.0903(18) Uani 1 1 d . .
H22A H 0.617114 0.202983 0.796125 0.135 Uiso 1 1 calc R U
H22B H 0.677518 0.137173 0.837560 0.135 Uiso 1 1 calc R U
H22C H 0.567469 0.124876 0.829128 0.135 Uiso 1 1 calc R U
C23 C 0.9491(3) -0.0805(2) 0.5093(2) 0.0513(10) Uani 1 1 d . .
Pd1 Pd 0.85979(2) 0.07979(2) 0.58355(2) 0.04714(12) Uani 1 1 d . .
S1 S 0.85771(9) -0.06248(7) 0.56280(9) 0.0728(4) Uani 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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
C1 N1 C2 120.2(3) .
C1 N1 Pd1 122.1(3) .
C2 N1 Pd1 117.7(2) .
C1 N2 C9 126.8(4) .
C1 N2 H2 116.6 .
C9 N2 H2 116.6 .
C1 N3 C16 122.3(4) .
C1 N3 H3 118.8 .
C16 N3 H3 118.8 .
C23 N4 Pd1 161.2(3) 5_756
N1 C1 N2 121.7(4) .
N1 C1 N3 121.8(4) .
N2 C1 N3 116.4(4) .
C7 C2 C3 120.5(4) .
C7 C2 N1 118.8(4) .
C3 C2 N1 120.7(4) .
C4 C3 C2 119.4(5) .
C4 C3 H3A 120.3 .
C2 C3 H3A 120.3 .
C5 C4 C3 119.7(5) .
C5 C4 H4 120.1 .
C3 C4 H4 120.1 .
C4 C5 C6 121.6(6) .
C4 C5 H5 119.2 .
C6 C5 H5 119.2 .
C5 C6 C7 119.9(6) .
C5 C6 H6 120.0 .
C7 C6 H6 120.0 .
C2 C7 C6 118.8(5) .
C2 C7 C8 119.9(5) .
C6 C7 C8 121.3(6) .
C7 C8 H8A 109.5 .
C7 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C7 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C10 C9 C14 120.1(5) .
C10 C9 N2 120.2(5) .
C14 C9 N2 119.4(5) .
C9 C10 C11 119.9(6) .
C9 C10 H10 120.1 .
C11 C10 H10 120.1 .
C12 C11 C10 119.8(6) .
C12 C11 H11 120.1 .
C10 C11 H11 120.1 .
C13 C12 C11 120.8(6) .
C13 C12 H12 119.6 .
C11 C12 H12 119.6 .
C12 C13 C14 121.3(6) .
C12 C13 H13 119.3 .
C14 C13 H13 119.3 .
C9 C14 C13 118.1(6) .
C9 C14 C15 121.4(5) .
C13 C14 C15 120.5(6) .
C14 C15 H15A 109.5 .
C14 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
C14 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
C17 C16 C21 122.4(4) .
C17 C16 N3 120.9(4) .
C21 C16 N3 116.6(4) .
C18 C17 C16 116.6(4) .
C18 C17 Pd1 123.6(3) .
C16 C17 Pd1 119.8(3) .
C19 C18 C17 121.3(4) .
C19 C18 H18 119.3 .
C17 C18 H18 119.3 .
C20 C19 C18 121.0(4) .
C20 C19 H19 119.5 .
C18 C19 H19 119.5 .
C19 C20 C21 120.7(4) .
C19 C20 H20 119.7 .
C21 C20 H20 119.7 .
C20 C21 C16 117.6(4) .
C20 C21 C22 120.1(4) .
C16 C21 C22 122.3(4) .
C21 C22 H22A 109.5 .
C21 C22 H22B 109.5 .
H22A C22 H22B 109.5 .
C21 C22 H22C 109.5 .
H22A C22 H22C 109.5 .
H22B C22 H22C 109.5 .
N4 C23 S1 179.2(4) 5_756
C17 Pd1 N1 87.22(14) .
C17 Pd1 N4 179.19(15) .
N1 Pd1 N4 93.47(12) .
C17 Pd1 S1 87.53(11) .
N1 Pd1 S1 174.44(9) .
N4 Pd1 S1 91.79(9) .
C23 S1 Pd1 105.40(12) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.287(5) .
N1 C2 1.421(5) .
N1 Pd1 2.055(3) .
N2 C1 1.360(5) .
N2 C9 1.429(5) .
N2 H2 0.8600 .
N3 C1 1.360(5) .
N3 C16 1.430(5) .
N3 H3 0.8600 .
N4 C23 1.138(5) 5_756
N4 Pd1 2.112(4) .
C2 C7 1.366(7) .
C2 C3 1.391(6) .
C3 C4 1.386(7) .
C3 H3A 0.9300 .
C4 C5 1.343(9) .
C4 H4 0.9300 .
C5 C6 1.362(9) .
C5 H5 0.9300 .
C6 C7 1.397(8) .
C6 H6 0.9300 .
C7 C8 1.480(8) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C10 1.361(7) .
C9 C14 1.366(7) .
C10 C11 1.384(9) .
C10 H10 0.9300 .
C11 C12 1.339(10) .
C11 H11 0.9300 .
C12 C13 1.325(10) .
C12 H12 0.9300 .
C13 C14 1.393(8) .
C13 H13 0.9300 .
C14 C15 1.512(9) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 C17 1.400(6) .
C16 C21 1.406(6) .
C17 C18 1.392(6) .
C17 Pd1 1.989(4) .
C18 C19 1.379(6) .
C18 H18 0.9300 .
C19 C20 1.360(7) .
C19 H19 0.9300 .
C20 C21 1.392(7) .
C20 H20 0.9300 .
C21 C22 1.490(7) .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 S1 1.660(4) .
Pd1 S1 2.3237(12) .
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
C2 N1 C1 N2 -9.7(7)
Pd1 N1 C1 N2 167.0(4)
C2 N1 C1 N3 169.7(4)
Pd1 N1 C1 N3 -13.6(6)
C9 N2 C1 N1 172.7(5)
C9 N2 C1 N3 -6.7(8)
C16 N3 C1 N1 -34.9(7)
C16 N3 C1 N2 144.5(4)
C1 N1 C2 C7 -101.8(5)
Pd1 N1 C2 C7 81.4(4)
C1 N1 C2 C3 80.6(5)
Pd1 N1 C2 C3 -96.3(4)
C7 C2 C3 C4 2.2(7)
N1 C2 C3 C4 179.8(4)
C2 C3 C4 C5 -0.7(8)
C3 C4 C5 C6 -1.3(10)
C4 C5 C6 C7 1.9(10)
C3 C2 C7 C6 -1.7(7)
N1 C2 C7 C6 -179.3(5)
C3 C2 C7 C8 177.9(5)
N1 C2 C7 C8 0.3(7)
C5 C6 C7 C2 -0.4(9)
C5 C6 C7 C8 -180.0(6)
C1 N2 C9 C10 -93.9(7)
C1 N2 C9 C14 92.3(6)
C14 C9 C10 C11 -0.7(8)
N2 C9 C10 C11 -174.5(5)
C9 C10 C11 C12 -0.3(10)
C10 C11 C12 C13 0.9(12)
C11 C12 C13 C14 -0.5(12)
C10 C9 C14 C13 1.1(8)
N2 C9 C14 C13 174.9(5)
C10 C9 C14 C15 -178.4(6)
N2 C9 C14 C15 -4.6(8)
C12 C13 C14 C9 -0.5(10)
C12 C13 C14 C15 179.0(7)
C1 N3 C16 C17 38.7(6)
C1 N3 C16 C21 -140.2(4)
C21 C16 C17 C18 6.3(6)
N3 C16 C17 C18 -172.6(4)
C21 C16 C17 Pd1 -173.7(3)
N3 C16 C17 Pd1 7.5(5)
C16 C17 C18 C19 -4.0(6)
Pd1 C17 C18 C19 176.0(3)
C17 C18 C19 C20 -0.4(7)
C18 C19 C20 C21 2.9(7)
C19 C20 C21 C16 -0.7(7)
C19 C20 C21 C22 177.7(5)
C17 C16 C21 C20 -4.0(7)
N3 C16 C21 C20 174.9(4)
C17 C16 C21 C22 177.6(5)
N3 C16 C21 C22 -3.5(7)
