#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:49:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179130 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/92/4309293.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_4309293
loop_
_publ_author_name
'Kallol Ray'
'Thomas Weyhermüller'
'Frank Neese'
'Karl Wieghardt'
_publ_section_title
;
Electronic Structure of Square Planar Bis(benzene-1,2-dithiolato)metal
Complexes [M(L)2]z (z= 2-, 1-, 0; M = Ni, Pd, Pt, Cu, Au): An
Experimental, Density Functional, and Correlated ab Initio Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5345
_journal_page_last               5360
_journal_paper_doi               10.1021/ic0507565
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[C16 H36 N]+, [C28 H40 Pd S4]-'
_chemical_formula_sum            'C44 H76 N Pd S4'
_chemical_formula_weight         853.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.79(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.438(2)
_cell_length_b                   10.1521(8)
_cell_length_c                   18.098(2)
_cell_measurement_temperature    200(2)
_cell_volume                     4737.0(8)
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.468
_diffrn_measured_fraction_theta_max 0.468
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '770 images at 1.0 deg in ω and 70 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27273
_diffrn_reflns_theta_full        23.81
_diffrn_reflns_theta_max         23.81
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.9773
_exptl_absorpt_correction_T_min  0.9436
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0534
_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
'w=1/[σ²(Fo²)+(0.0078P)²+11.0479P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                2931
_reflns_number_total             3629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0507565si20050512_085424.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0078P)^2^+11.0479P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0078P)^2^+11.0479P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4737.0(7)
_cod_database_code               4309293
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 0.0000 0.0000 0.02807(11) Uani 1 d S . .
S1 S 0.58734(3) 0.01124(8) 0.03246(4) 0.03350(19) Uani 1 d . . .
S2 S 0.50528(3) -0.21706(8) 0.02924(5) 0.0348(2) Uani 1 d . . .
C1 C 0.60901(11) -0.1490(3) 0.05764(16) 0.0282(7) Uani 1 d . . .
C2 C 0.57192(11) -0.2487(3) 0.05538(16) 0.0285(7) Uani 1 d . . .
C3 C 0.58665(12) -0.3796(3) 0.07331(17) 0.0335(8) Uani 1 d . . .
H3 H 0.5607 -0.4451 0.0714 0.040 Uiso 1 calc R . .
C4 C 0.63812(12) -0.4144(3) 0.09368(17) 0.0310(8) Uani 1 d . . .
C5 C 0.67488(12) -0.3143(3) 0.09608(17) 0.0334(8) Uani 1 d . . .
H5 H 0.7105 -0.3380 0.1099 0.040 Uiso 1 calc R . .
C6 C 0.66295(12) -0.1827(3) 0.07965(18) 0.0323(7) Uani 1 d . . .
C7 C 0.70652(12) -0.0797(3) 0.0862(2) 0.0430(9) Uani 1 d . . .
C8 C 0.70188(13) 0.0227(3) 0.1471(2) 0.0540(10) Uani 1 d . . .
H8A H 0.7296 0.0881 0.1511 0.081 Uiso 1 calc R . .
H8B H 0.7049 -0.0216 0.1960 0.081 Uiso 1 calc R . .
H8C H 0.6681 0.0668 0.1330 0.081 Uiso 1 calc R . .
C9 C 0.70552(14) -0.0130(4) 0.0097(2) 0.0588(10) Uani 1 d . . .
H9A H 0.6722 0.0319 -0.0079 0.088 Uiso 1 calc R . .
H9B H 0.7099 -0.0797 -0.0275 0.088 Uiso 1 calc R . .
H9C H 0.7338 0.0513 0.0157 0.088 Uiso 1 calc R . .
C10 C 0.76096(13) -0.1422(3) 0.1124(3) 0.0655(13) Uani 1 d . . .
H10A H 0.7665 -0.2071 0.0749 0.098 Uiso 1 calc R . .
H10B H 0.7634 -0.1858 0.1614 0.098 Uiso 1 calc R . .
H10C H 0.7875 -0.0733 0.1176 0.098 Uiso 1 calc R . .
C11 C 0.65442(12) -0.5589(3) 0.10884(18) 0.0342(8) Uani 1 d . . .
C12 C 0.71077(15) -0.5711(4) 0.1528(2) 0.0655(12) Uani 1 d . . .
H12A H 0.7339 -0.5362 0.1220 0.098 Uiso 1 calc R . .
H12B H 0.7190 -0.6640 0.1643 0.098 Uiso 1 calc R . .
H12C H 0.7155 -0.5210 0.2001 0.098 Uiso 1 calc R . .
C13 C 0.61982(16) -0.6269(4) 0.1541(3) 0.0693(13) Uani 1 d . . .
H13A H 0.6311 -0.7184 0.1639 0.104 Uiso 1 calc R . .
H13B H 0.5838 -0.6251 0.1252 0.104 Uiso 1 calc R . .
H13C H 0.6223 -0.5809 0.2024 0.104 Uiso 1 calc R . .
C14 C 0.64895(16) -0.6295(3) 0.0331(2) 0.0575(11) Uani 1 d . . .
H14A H 0.6703 -0.5849 0.0028 0.086 Uiso 1 calc R . .
H14B H 0.6125 -0.6280 0.0057 0.086 Uiso 1 calc R . .
H14C H 0.6605 -0.7210 0.0420 0.086 Uiso 1 calc R . .
N20 N 0.5000 -0.0535(4) -0.2500 0.0425(10) Uani 1 d S . .
C21 C 0.45889(14) 0.0313(4) -0.22672(19) 0.0501(10) Uani 1 d . . .
H21A H 0.4758 0.0859 -0.1829 0.060 Uiso 1 calc R . .
H21B H 0.4339 -0.0273 -0.2095 0.060 Uiso 1 calc R . .
C22 C 0.42893(16) 0.1219(4) -0.2879(2) 0.0570(11) Uani 1 d . . .
H22A H 0.4533 0.1850 -0.3031 0.068 Uiso 1 calc R . .
H22B H 0.4131 0.0687 -0.3330 0.068 Uiso 1 calc R . .
C23 C 0.38750(19) 0.1963(5) -0.2623(2) 0.0865(16) Uani 1 d . . .
H23A H 0.4039 0.2519 -0.2186 0.104 Uiso 1 calc R . .
H23B H 0.3646 0.1325 -0.2443 0.104 Uiso 1 calc R . .
C24 C 0.35445(18) 0.2831(5) -0.3215(3) 0.0832(15) Uani 1 d . . .
H24A H 0.3765 0.3478 -0.3395 0.125 Uiso 1 calc R . .
H24B H 0.3288 0.3292 -0.2994 0.125 Uiso 1 calc R . .
H24C H 0.3366 0.2289 -0.3642 0.125 Uiso 1 calc R . .
C25 C 0.52440(14) -0.1385(4) -0.18202(18) 0.0450(9) Uani 1 d . . .
H25A H 0.4971 -0.1949 -0.1691 0.054 Uiso 1 calc R . .
H25B H 0.5375 -0.0800 -0.1382 0.054 Uiso 1 calc R . .
C26 C 0.56878(14) -0.2264(4) -0.1935(2) 0.0586(11) Uani 1 d . . .
H26A H 0.5587 -0.2705 -0.2434 0.070 Uiso 1 calc R . .
H26B H 0.5996 -0.1712 -0.1939 0.070 Uiso 1 calc R . .
C27 C 0.58299(15) -0.3305(4) -0.1317(2) 0.0593(11) Uani 1 d . . .
H27A H 0.6159 -0.3728 -0.1361 0.071 Uiso 1 calc R . .
H27B H 0.5890 -0.2865 -0.0817 0.071 Uiso 1 calc R . .
C28 C 0.54275(18) -0.4355(4) -0.1344(3) 0.0808(14) Uani 1 d . . .
H28A H 0.5109 -0.3959 -0.1252 0.121 Uiso 1 calc R . .
H28B H 0.5556 -0.5018 -0.0954 0.121 Uiso 1 calc R . .
H28C H 0.5354 -0.4774 -0.1844 0.121 Uiso 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'
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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Pd1 S1 180.0 . 5_655 ?
S1 Pd1 S2 88.96(3) . . ?
S1 Pd1 S2 91.04(3) 5_655 . ?
S1 Pd1 S2 91.04(3) . 5_655 ?
S1 Pd1 S2 88.96(3) 5_655 5_655 ?
S2 Pd1 S2 180.0 . 5_655 ?
C1 S1 Pd1 106.13(10) . . ?
C2 S2 Pd1 104.37(10) . . ?
C2 C1 C6 118.7(3) . . ?
C2 C1 S1 118.4(2) . . ?
C6 C1 S1 122.8(2) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 S2 116.6(2) . . ?
C1 C2 S2 122.0(2) . . ?
C4 C3 C2 120.9(3) . . ?
C3 C4 C5 117.4(3) . . ?
C3 C4 C11 121.0(3) . . ?
C5 C4 C11 121.5(3) . . ?
C6 C5 C4 124.6(3) . . ?
C5 C6 C1 117.0(3) . . ?
C5 C6 C7 120.4(3) . . ?
C1 C6 C7 122.7(3) . . ?
C9 C7 C8 111.1(3) . . ?
C9 C7 C6 111.5(3) . . ?
C8 C7 C6 109.7(3) . . ?
C9 C7 C10 106.7(3) . . ?
C8 C7 C10 105.8(3) . . ?
C6 C7 C10 112.0(3) . . ?
C13 C11 C14 108.8(3) . . ?
C13 C11 C12 108.4(3) . . ?
C14 C11 C12 108.4(3) . . ?
C13 C11 C4 110.5(3) . . ?
C14 C11 C4 108.7(3) . . ?
C12 C11 C4 111.9(3) . . ?
C21 N20 C21 110.8(4) 2_654 . ?
C21 N20 C25 107.35(18) 2_654 2_654 ?
C21 N20 C25 110.1(2) . 2_654 ?
C21 N20 C25 110.1(2) 2_654 . ?
C21 N20 C25 107.35(18) . . ?
C25 N20 C25 111.1(4) 2_654 . ?
N20 C21 C22 115.5(3) . . ?
C23 C22 C21 112.5(3) . . ?
C22 C23 C24 115.3(4) . . ?
N20 C25 C26 115.0(3) . . ?
C27 C26 C25 112.2(3) . . ?
C28 C27 C26 114.3(3) . . ?
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 S1 2.2560(8) . ?
Pd1 S1 2.2560(8) 5_655 ?
Pd1 S2 2.2633(8) . ?
Pd1 S2 2.2633(8) 5_655 ?
S1 C1 1.751(3) . ?
S2 C2 1.750(3) . ?
C1 C2 1.404(4) . ?
C1 C6 1.435(4) . ?
C2 C3 1.402(4) . ?
C3 C4 1.375(4) . ?
C4 C5 1.400(4) . ?
C4 C11 1.536(4) . ?
C5 C6 1.389(4) . ?
C6 C7 1.541(4) . ?
C7 C9 1.536(5) . ?
C7 C8 1.540(5) . ?
C7 C10 1.548(4) . ?
C11 C13 1.522(5) . ?
C11 C14 1.526(5) . ?
C11 C12 1.530(5) . ?
N20 C21 1.518(4) 2_654 ?
N20 C21 1.518(4) . ?
N20 C25 1.524(4) 2_654 ?
N20 C25 1.524(4) . ?
C21 C22 1.520(5) . ?
C22 C23 1.487(5) . ?
C23 C24 1.508(5) . ?
C25 C26 1.525(5) . ?
C26 C27 1.524(5) . ?
C27 C28 1.499(6) . ?
