#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322366.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_4322366
loop_
_publ_author_name
'Sudeep Bhattacharyya'
'Timothy J. R. Weakley'
'Muktimoy Chaudhury'
_publ_contact_author_address
;Department of Chemistry,
University of Oregon,
Eugene, OR 97403-1253
USA
;
_publ_contact_author_email       tweakley@oregon.uoregon.edu
_publ_contact_author_fax         01(541)3464643
_publ_contact_author_name        'Dr Timothy J. R. Weakley'
_publ_contact_author_phone       01(541)3464620
_publ_section_title
;
 Palladium(II)-Induced Activation of Carbon-Nitrogen Single Bond of
 Coordinated N4S Ligand. Characterization of Product with Modified Ligand
 Structure: Kinetics versus Thermodynamic Considerations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5453
_journal_page_last               5456
_journal_paper_doi               10.1021/ic9813720
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C21 H31 N6 Pd S2 1+, Cl O4 1-'
_chemical_formula_sum            'C21 H31 Cl N6 O4 Pd S2'
_chemical_formula_weight         637.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                96.818(7)
_cell_angle_beta                 107.694(7)
_cell_angle_gamma                104.520(6)
_cell_formula_units_Z            2
_cell_length_a                   8.8449(5)
_cell_length_b                   11.2219(8)
_cell_length_c                   14.466(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      30.0
_cell_volume                     1294.32(17)
_computing_cell_refinement       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_collection       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'TEXSAN (Molecular Structure Corp., 1989)'
_computing_publication_material  'TEXSAN (Molecular Structure Corp., 1989)'
_computing_structure_refinement  'TEXSAN (Molecular Structure Corp., 1989)'
_computing_structure_solution    'TEXSAN (Molecular Structure Corp., 1989)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.10644
_diffrn_orient_matrix_UB_12      0.00486
_diffrn_orient_matrix_UB_13      -0.01235
_diffrn_orient_matrix_UB_21      -0.06203
_diffrn_orient_matrix_UB_22      -0.02210
_diffrn_orient_matrix_UB_23      -0.07319
_diffrn_orient_matrix_UB_31      0.01823
_diffrn_orient_matrix_UB_32      0.09142
_diffrn_orient_matrix_UB_33      -0.00088
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0081
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4868
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0.70
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.0
_exptl_absorpt_correction_T_max  1.198
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'DIFABS (Walker & Stuart, 1983)'
_exptl_crystal_colour            rose-red
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             652.00
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.44
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.38
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4100
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.029
_refine_ls_shift/esd_max         0.069
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fₒ²/[σ²(I)+(0.02I)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.038
_reflns_number_observed          4100
_reflns_number_total             4546
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            ic9813720_1.cif
_cod_data_source_block           IC9813720
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1294.3(4)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C21 H31 Cl N6 O4 Pd S2 '
_cod_database_code               4322366
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Pd 0.23988(3) 0.17275(2) 0.18751(2) 0.03664(7) Uij ? ?
Cl 0.1222(1) 0.44306(8) 0.77436(7) 0.0591(3) Uij ? ?
S1 0.1614(1) -0.03241(7) 0.11838(6) 0.0482(2) Uij ? ?
S2 0.1669(1) -0.20586(9) -0.05010(7) 0.0628(3) Uij ? ?
O1 0.1564(4) 0.5592(3) 0.7440(3) 0.103(1) Uij ? ?
O2 0.2186(4) 0.3735(3) 0.7453(2) 0.094(1) Uij ? ?
O3 0.1784(6) 0.4686(4) 0.8792(3) 0.134(2) Uij ? ?
O4 -0.0474(4) 0.3794(4) 0.7304(4) 0.151(2) Uij ? ?
N1 0.3220(3) 0.2357(3) 0.0848(2) 0.0446(7) Uij ? ?
N2 0.3254(3) 0.3609(2) 0.2627(2) 0.0419(7) Uij ? ?
N3 0.1484(3) 0.2650(2) 0.3462(2) 0.0437(7) Uij ? ?
N4 0.1512(3) 0.1513(2) 0.3012(2) 0.0418(7) Uij ? ?
N5 0.5291(3) 0.3192(2) 0.4044(2) 0.0447(7) Uij ? ?
N6 0.4925(4) 0.3341(3) 0.4907(2) 0.0542(8) Uij ? ?
C1 0.2114(4) -0.0498(3) 0.0134(2) 0.0464(9) Uij ? ?
C2 0.2798(4) 0.0411(3) -0.0292(2) 0.0484(9) Uij ? ?
C3 0.3134(5) 0.0090(4) -0.1245(3) 0.068(1) Uij ? ?
C4 0.3916(6) 0.1356(5) -0.1460(3) 0.080(2) Uij ? ?
C5 0.4046(5) 0.2392(4) -0.0639(3) 0.064(1) Uij ? ?
C6 0.3311(4) 0.1737(3) 0.0047(2) 0.0460(9) Uij ? ?
C7 0.3930(5) 0.3749(3) 0.1101(3) 0.056(1) Uij ? ?
C8 0.3221(5) 0.4312(3) 0.1809(3) 0.055(1) Uij ? ?
C9 0.1989(4) 0.3754(3) 0.3070(3) 0.051(1) Uij ? ?
C10 0.0783(5) 0.3645(4) 0.4836(3) 0.072(1) Uij ? ?
C11 0.0933(4) 0.2542(3) 0.4223(3) 0.055(1) Uij ? ?
C12 0.0603(5) 0.1312(4) 0.4268(3) 0.062(1) Uij ? ?
C13 0.0976(4) 0.0686(3) 0.3518(3) 0.051(1) Uij ? ?
C14 0.0860(6) -0.0666(4) 0.3265(3) 0.073(1) Uij ? ?
C15 0.4989(4) 0.4023(3) 0.3389(2) 0.0474(9) Uij ? ?
C16 0.6379(5) 0.1802(4) 0.3102(3) 0.068(1) Uij ? ?
C17 0.5875(4) 0.2182(3) 0.3942(2) 0.0508(9) Uij ? ?
C18 0.5878(5) 0.1667(4) 0.4751(3) 0.066(1) Uij ? ?
C19 0.5293(5) 0.2407(3) 0.5334(3) 0.060(1) Uij ? ?
C20 0.5052(7) 0.2259(5) 0.6295(3) 0.089(2) Uij ? ?
C21 0.1057(6) -0.3023(4) 0.0290(3) 0.080(1) Uij ? ?
H1 0.3881 -0.0400 -0.1159 0.082 Uiso ? ?
H2 0.2125 -0.0360 -0.1772 0.082 Uiso ? ?
H3 0.4994 0.1401 -0.1476 0.096 Uiso ? ?
H4 0.3237 0.1446 -0.2081 0.096 Uiso ? ?
H5 0.5178 0.2869 -0.0294 0.077 Uiso ? ?
H6 0.3435 0.2933 -0.0907 0.077 Uiso ? ?
H7 0.5106 0.3971 0.1404 0.068 Uiso ? ?
H8 0.3664 0.4067 0.0512 0.068 Uiso ? ?
H9 0.2104 0.4268 0.1458 0.066 Uiso ? ?
H10 0.3866 0.5168 0.2086 0.066 Uiso ? ?
H11 0.2449 0.4483 0.3590 0.061 Uiso ? ?
H12 0.1049 0.3836 0.2576 0.061 Uiso ? ?
H13 0.1850 0.4250 0.5149 0.086 Uiso ? ?
H14 0.0054 0.4013 0.4422 0.086 Uiso ? ?
H15 0.0350 0.3374 0.5327 0.086 Uiso ? ?
H16 0.0188 0.0939 0.4732 0.074 Uiso ? ?
H17 0.0448 -0.1103 0.3704 0.087 Uiso ? ?
H18 0.0125 -0.1020 0.2601 0.087 Uiso ? ?
H19 0.1933 -0.0737 0.3328 0.087 Uiso ? ?
H20 0.5760 0.4092 0.3048 0.057 Uiso ? ?
H21 0.5166 0.4825 0.3775 0.057 Uiso ? ?
H22 0.6729 0.1074 0.3177 0.081 Uiso ? ?
H23 0.5463 0.1619 0.2500 0.081 Uiso ? ?
H24 0.7272 0.2468 0.3085 0.081 Uiso ? ?
H25 0.6211 0.0948 0.4893 0.079 Uiso ? ?
H26 0.5704 0.3003 0.6786 0.107 Uiso ? ?
H27 0.3910 0.2116 0.6215 0.107 Uiso ? ?
H28 0.5389 0.1563 0.6498 0.107 Uiso ? ?
H29 0.0097 -0.2883 0.0389 0.096 Uiso ? ?
H30 0.0809 -0.3883 -0.0008 0.096 Uiso ? ?
H31 0.1938 -0.2818 0.0911 0.096 Uiso ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 42 0.002 0.002 'Cromer & Waber (1974)'
H 0 62 0.000 0.000 'Cromer & Waber (1974)'
Cl 0 2 0.132 0.159 'Cromer & Waber (1974)'
N 0 12 0.004 0.003 'Cromer & Waber (1974)'
O 0 8 0.008 0.006 'Cromer & Waber (1974)'
Pd 0 2 -1.177 1.007 'Cromer & Waber (1974)'
S 0 4 0.110 0.124 'Cromer & Waber (1974)'
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Pd N1 96.74(8) ? ? ? yes
S1 Pd N2 175.24(7) ? ? ? yes
S1 Pd N4 96.44(7) ? ? ? yes
N1 Pd N2 86.0(1) ? ? ? yes
N1 Pd N4 165.9(1) ? ? ? yes
N2 Pd N4 81.25(10) ? ? ? yes
O1 Cl O2 108.0(2) ? ? ? no
O1 Cl O3 108.0(3) ? ? ? no
O1 Cl O4 109.0(2) ? ? ? no
O2 Cl O3 106.8(2) ? ? ? no
O2 Cl O4 111.4(3) ? ? ? no
O3 Cl O4 113.4(3) ? ? ? no
Pd S1 C1 109.2(1) ? ? ? yes
C1 S2 C21 105.1(2) ? ? ? no
Pd N1 C6 130.1(2) ? ? ? no
Pd N1 C7 111.5(2) ? ? ? yes
C6 N1 C7 118.3(3) ? ? ? yes
Pd N2 C8 102.9(2) ? ? ? yes
Pd N2 C9 104.9(2) ? ? ? np
Pd N2 C15 115.2(2) ? ? ? yes
C8 N2 C9 111.5(3) ? ? ? no
C8 N2 C15 109.7(2) ? ? ? no
C9 N2 C15 112.3(2) ? ? ? no
N4 N3 C9 119.0(2) ? ? ? no
N4 N3 C11 111.6(3) ? ? ? no
C9 N3 C11 129.4(3) ? ? ? no
Pd N4 N3 110.3(2) ? ? ? no
Pd N4 C13 144.1(2) ? ? ? no
N3 N4 C13 105.5(2) ? ? ? no
N6 N5 C15 119.4(3) ? ? ? no
N6 N5 C17 111.5(3) ? ? ? no
C15 N5 C17 129.1(3) ? ? ? no
N5 N6 C19 104.8(3) ? ? ? no
S1 C1 S2 116.4(2) ? ? ? no
S1 C1 C2 128.7(3) ? ? ? yes
S2 C1 C2 114.9(2) ? ? ? no
C1 C2 C3 121.9(3) ? ? ? no
C1 C2 C6 128.1(3) ? ? ? no
C3 C2 C6 110.0(3) ? ? ? no
C2 C3 C4 105.4(3) ? ? ? no
C3 C4 C5 108.2(3) ? ? ? no
C4 C5 C6 105.9(3) ? ? ? no
N1 C6 C2 127.1(3) ? ? ? no
N1 C6 C5 122.4(3) ? ? ? no
C2 C6 C5 110.4(3) ? ? ? no
N1 C7 C8 110.1(3) ? ? ? no
N2 C8 C7 110.5(3) ? ? ? no
N2 C9 N3 108.9(2) ? ? ? no
N3 C11 C10 122.2(3) ? ? ? no
N3 C11 C12 105.8(3) ? ? ? no
C10 C11 C12 132.0(3) ? ? ? no
C11 C12 C13 108.4(3) ? ? ? no
N4 C13 C12 108.7(3) ? ? ? no
N4 C13 C14 121.9(3) ? ? ? no
C12 C13 C14 129.4(3) ? ? ? no
N2 C15 N5 114.4(2) ? ? ? no
N5 C17 C16 123.6(3) ? ? ? no
N5 C17 C18 106.3(3) ? ? ? no
C16 C17 C18 130.1(3) ? ? ? no
C17 C18 C19 106.8(3) ? ? ? no
N6 C19 C18 110.6(3) ? ? ? no
N6 C19 C20 120.4(3) ? ? ? no
C18 C19 C20 129.0(4) ? ? ? no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.2389(8) ? ? yes
Pd N1 1.970(2) ? ? yes
Pd N2 2.090(2) ? ? yes
Pd N4 2.039(2) ? ? yes
Cl O1 1.415(3) ? ? no
Cl O2 1.410(3) ? ? no
Cl O3 1.413(4) ? ? no
Cl O4 1.393(4) ? ? no
S1 C1 1.709(3) ? ? yes
S2 C1 1.766(3) ? ? no
S2 C21 1.774(5) ? ? no
N1 C6 1.315(4) ? ? yes
N1 C7 1.483(4) ? ? no
N2 C8 1.495(4) ? ? no
N2 C9 1.480(4) ? ? no
N2 C15 1.510(4) ? ? no
N3 N4 1.371(3) ? ? no
N3 C9 1.449(4) ? ? no
N3 C11 1.339(4) ? ? no
N4 C13 1.332(4) ? ? no
N5 N6 1.384(4) ? ? no
N5 C15 1.421(4) ? ? no
N5 C17 1.369(4) ? ? no
N6 C19 1.337(4) ? ? no
C1 C2 1.361(5) ? ? yes
C2 C3 1.517(5) ? ? no
C2 C6 1.419(5) ? ? yes
C3 C4 1.528(6) ? ? no
C4 C5 1.515(6) ? ? no
C5 C6 1.508(5) ? ? no
C7 C8 1.509(5) ? ? no
C10 C11 1.493(5) ? ? no
C11 C12 1.351(5) ? ? no
C12 C13 1.390(5) ? ? no
C13 C14 1.488(5) ? ? no
C16 C17 1.470(5) ? ? no
C17 C18 1.364(5) ? ? no
C18 C19 1.408(5) ? ? no
C19 C20 1.492(5) ? ? no
