#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:09:52 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179914 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/09/7020917.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_7020917
loop_
_publ_author_name
'Safin, Damir A.'
'Babashkina, Maria G.'
'Garcia, Yann'
_publ_section_title
;
 First paramagnetic Pd(II) complex with a PdN4S2 coordination core.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              902
_journal_page_last               905
_journal_paper_doi               10.1039/c2dt32505e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C24 H38 N6 O4 P2 Pd S4'
_chemical_formula_sum            'C24 H38 N6 O4 P2 Pd S4'
_chemical_formula_weight         771.18
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.870(9)
_cell_angle_beta                 94.830(9)
_cell_angle_gamma                107.321(6)
_cell_formula_units_Z            1
_cell_length_a                   7.9596(12)
_cell_length_b                   10.4276(15)
_cell_length_c                   11.7207(18)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     833.3(2)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens CCD three-circle diffractometer'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20545
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_correction_T_min  0.6552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         5080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0242P)²+0.2479P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                3920
_reflns_number_total             5080
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c2dt32505e.txt
_cod_data_source_block           safin96
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7020917
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 1.0000 0.5000 1.0000 0.02063(7) Uani 1 2 d S
P1 P 0.76361(7) 0.50181(6) 0.76407(5) 0.02111(12) Uani 1 1 d .
S1 S 0.72202(7) 0.50951(6) 0.93179(5) 0.02470(13) Uani 1 1 d .
S2 S 0.99180(8) 0.29789(7) 0.82082(5) 0.03054(14) Uani 1 1 d .
O1 O 0.9378(2) 0.63016(16) 0.77568(14) 0.0257(3) Uani 1 1 d .
O2 O 0.60875(19) 0.53227(16) 0.70021(14) 0.0247(3) Uani 1 1 d .
N1 N 0.7765(2) 0.35196(19) 0.66255(16) 0.0242(4) Uani 1 1 d .
N2 N 0.8554(3) 0.1440(2) 0.58066(17) 0.0243(4) Uani 1 1 d .
H2 H 0.933(3) 0.107(3) 0.593(2) 0.034(7) Uiso 1 1 d .
C1 C 0.8611(3) 0.2699(2) 0.68078(19) 0.0222(4) Uani 1 1 d .
C2 C 0.9648(3) 0.7879(2) 0.8515(2) 0.0291(5) Uani 1 1 d .
H2A H 0.8811 0.7954 0.9109 0.035 Uiso 1 1 calc R
C3 C 0.9221(4) 0.8507(3) 0.7616(3) 0.0480(7) Uani 1 1 d .
H3A H 0.7952 0.7974 0.7157 0.072 Uiso 1 1 calc R
H3B H 0.9999 0.8386 0.7007 0.072 Uiso 1 1 calc R
H3C H 0.9433 0.9569 0.8098 0.072 Uiso 1 1 calc R
C4 C 1.1567(3) 0.8628(3) 0.9270(3) 0.0434(7) Uani 1 1 d .
H4A H 1.1751 0.8178 0.9842 0.065 Uiso 1 1 calc R
H4B H 1.1818 0.9694 0.9771 0.065 Uiso 1 1 calc R
H4C H 1.2385 0.8503 0.8689 0.065 Uiso 1 1 calc R
C5 C 0.4193(3) 0.4829(3) 0.7079(2) 0.0328(6) Uani 1 1 d .
H5 H 0.4022 0.4190 0.7543 0.039 Uiso 1 1 calc R
C6 C 0.3079(4) 0.3913(4) 0.5741(3) 0.0618(9) Uani 1 1 d .
H6A H 0.3417 0.3040 0.5329 0.093 Uiso 1 1 calc R
H6B H 0.3298 0.4517 0.5267 0.093 Uiso 1 1 calc R
H6C H 0.1796 0.3584 0.5755 0.093 Uiso 1 1 calc R
C7 C 0.3796(4) 0.6183(4) 0.7814(4) 0.0657(10) Uani 1 1 d .
H7A H 0.4571 0.6708 0.8673 0.099 Uiso 1 1 calc R
H7B H 0.2526 0.5893 0.7865 0.099 Uiso 1 1 calc R
H7C H 0.4030 0.6841 0.7389 0.099 Uiso 1 1 calc R
C11 C 0.7457(3) 0.0699(2) 0.4571(2) 0.0227(4) Uani 1 1 d .
N12 N 0.7916(2) -0.0401(2) 0.38011(17) 0.0245(4) Uani 1 1 d .
C13 C 0.6878(3) -0.1220(3) 0.2621(2) 0.0290(5) Uani 1 1 d .
H13 H 0.7189 -0.2010 0.2058 0.035 Uiso 1 1 calc R
C14 C 0.5397(3) -0.0996(3) 0.2173(2) 0.0296(5) Uani 1 1 d .
H14 H 0.4699 -0.1614 0.1329 0.036 Uiso 1 1 calc R
C15 C 0.4957(3) 0.0151(3) 0.2984(2) 0.0353(6) Uani 1 1 d .
H15 H 0.3937 0.0338 0.2706 0.042 Uiso 1 1 calc R
C16 C 0.5998(3) 0.1031(3) 0.4203(2) 0.0337(6) Uani 1 1 d .
H16 H 0.5725 0.1841 0.4774 0.040 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 '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'
Pd Pd -0.9988 1.0072 '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'
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
S2 Pd1 S2 180.0 2_767 .
S2 Pd1 S1 97.93(2) 2_767 2_767
S2 Pd1 S1 82.07(2) . 2_767
S2 Pd1 S1 82.07(2) 2_767 .
S2 Pd1 S1 97.93(2) . .
S1 Pd1 S1 180.0 2_767 .
O2 P1 O1 103.02(8) . .
O2 P1 N1 107.28(9) . .
O1 P1 N1 105.52(9) . .
O2 P1 S1 108.96(6) . .
O1 P1 S1 113.32(6) . .
N1 P1 S1 117.62(7) . .
P1 S1 Pd1 95.86(3) . .
C1 S2 Pd1 115.05(8) . .
C2 O1 P1 121.40(14) . .
C5 O2 P1 125.69(13) . .
C1 N1 P1 128.52(16) . .
C1 N2 C11 129.53(18) . .
C1 N2 H2 115.6(17) . .
C11 N2 H2 114.8(17) . .
N1 C1 N2 119.71(19) . .
N1 C1 S2 128.84(17) . .
N2 C1 S2 111.43(15) . .
O1 C2 C4 106.77(18) . .
O1 C2 C3 107.97(19) . .
C4 C2 C3 113.6(2) . .
O1 C2 H2A 109.5 . .
C4 C2 H2A 109.5 . .
C3 C2 H2A 109.5 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O2 C5 C7 107.4(2) . .
O2 C5 C6 107.2(2) . .
C7 C5 C6 114.8(2) . .
O2 C5 H5 109.1 . .
C7 C5 H5 109.1 . .
C6 C5 H5 109.1 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N12 C11 C16 123.3(2) . .
N12 C11 N2 112.78(18) . .
C16 C11 N2 123.8(2) . .
C11 N12 C13 116.74(18) . .
N12 C13 C14 124.4(2) . .
N12 C13 H13 117.8 . .
C14 C13 H13 117.8 . .
C13 C14 C15 117.8(2) . .
C13 C14 H14 121.1 . .
C15 C14 H14 121.1 . .
C14 C15 C16 119.8(2) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
C15 C16 C11 118.0(2) . .
C15 C16 H16 121.0 . .
C11 C16 H16 121.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 S2 2.3046(7) 2_767
Pd1 S2 2.3046(7) .
Pd1 S1 2.3321(6) 2_767
Pd1 S1 2.3322(6) .
P1 O2 1.5630(14) .
P1 O1 1.5664(16) .
P1 N1 1.5933(19) .
P1 S1 1.9958(8) .
S2 C1 1.738(2) .
O1 C2 1.471(3) .
O2 C5 1.464(3) .
N1 C1 1.301(3) .
N2 C1 1.364(3) .
N2 C11 1.405(3) .
N2 H2 0.85(3) .
C2 C4 1.500(3) .
C2 C3 1.505(3) .
C2 H2A 1.0000 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C7 1.483(4) .
C5 C6 1.502(4) .
C5 H5 1.0000 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C11 N12 1.328(3) .
C11 C16 1.388(3) .
N12 C13 1.339(3) .
C13 C14 1.369(3) .
C13 H13 0.9500 .
C14 C15 1.370(3) .
C14 H14 0.9500 .
C15 C16 1.378(3) .
C15 H15 0.9500 .
C16 H16 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 N12 0.85(3) 2.52(3) 3.356(3) 167(2) 2_756
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
_geom_torsion_site_symmetry_1
O2 P1 S1 Pd1 -170.97(6) .
O1 P1 S1 Pd1 -56.92(7) .
N1 P1 S1 Pd1 66.74(8) .
S2 Pd1 S1 P1 130.10(3) 2_767
S2 Pd1 S1 P1 -49.90(3) .
S1 Pd1 S2 C1 -153.57(9) 2_767
S1 Pd1 S2 C1 26.43(9) .
O2 P1 O1 C2 61.26(16) .
N1 P1 O1 C2 173.63(15) .
S1 P1 O1 C2 -56.31(16) .
O1 P1 O2 C5 -156.56(17) .
N1 P1 O2 C5 92.37(18) .
S1 P1 O2 C5 -35.96(18) .
O2 P1 N1 C1 -166.02(19) .
O1 P1 N1 C1 84.6(2) .
S1 P1 N1 C1 -42.9(2) .
P1 N1 C1 N2 179.75(16) .
P1 N1 C1 S2 -1.4(3) .
C11 N2 C1 N1 -11.5(4) .
C11 N2 C1 S2 169.46(19) .
Pd1 S2 C1 N1 4.3(2) .
Pd1 S2 C1 N2 -176.75(13) .
P1 O1 C2 C4 135.83(18) .
P1 O1 C2 C3 -101.7(2) .
P1 O2 C5 C7 113.3(2) .
P1 O2 C5 C6 -122.9(2) .
C1 N2 C11 N12 172.8(2) .
C1 N2 C11 C16 -9.9(4) .
C16 C11 N12 C13 -0.8(3) .
N2 C11 N12 C13 176.51(19) .
C11 N12 C13 C14 -0.2(3) .
N12 C13 C14 C15 0.5(4) .
C13 C14 C15 C16 0.1(4) .
C14 C15 C16 C11 -1.0(4) .
N12 C11 C16 C15 1.4(4) .
N2 C11 C16 C15 -175.6(2) .
