#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/83/7008374.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_7008374
loop_
_publ_author_name
'Dilworth, Jonathan R.'
'von Beckh W, Carlo A Maresca'
'Pascu, Sofia I.'
_publ_section_title
;
 Synthesis, structure and catalytic activity of thioether-phosphane
 complexes of Pd(II) and Pt(II).
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2151
_journal_page_last               2161
_journal_paper_doi               10.1039/b502195b
_journal_year                    2005
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C23 H25 Cl2 P1 Pd1 S1 '
_chemical_formula_sum            'C23 H25 Cl2 P Pd S'
_chemical_formula_weight         541.80
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 109.7231(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5554(4)
_cell_length_b                   15.0824(5)
_cell_length_c                   12.7084(4)
_cell_measurement_reflns_used    4756
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2265.35(13)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2003)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2003)
;
_computing_structure_solution
;
SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
;
Nonius Kappa CCD
;
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9161
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         5.107
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.70
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3429
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001123
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
0.361 0.682E-01 0.941E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0561
_refine_ls_wR_factor_gt          0.0337
_refine_ls_wR_factor_ref         0.0337
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3429
_reflns_number_total             5117
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b502195b.txt
_cod_data_source_block           4
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C23 H25 Cl2 P1 Pd1 S1 '
_cod_database_code               7008374
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Pd1 Pd 0.80754(2) 0.319915(18) 0.12368(2) 0.0175 1.0000 Uani . . . . . .
Cl1 Cl 0.86620(8) 0.18543(6) 0.06395(7) 0.0268 1.0000 Uani . . . . . .
Cl2 Cl 0.83882(8) 0.26352(6) 0.30108(7) 0.0248 1.0000 Uani . . . . . .
S1 S 0.79688(7) 0.37982(6) -0.04583(7) 0.0192 1.0000 Uani . . . . . .
P1 P 0.75841(7) 0.44311(6) 0.19203(7) 0.0187 1.0000 Uani . . . . . .
C1 C 0.6933(3) 0.5266(2) 0.0851(3) 0.0221 1.0000 Uani . . . . . .
C2 C 0.7694(3) 0.5555(2) 0.0224(3) 0.0211 1.0000 Uani . . . . . .
C3 C 0.8019(3) 0.6442(3) 0.0282(3) 0.0277 1.0000 Uani . . . . . .
C4 C 0.8716(3) 0.6758(3) -0.0276(3) 0.0300 1.0000 Uani . . . . . .
C5 C 0.9109(3) 0.6185(3) -0.0912(3) 0.0274 1.0000 Uani . . . . . .
C6 C 0.8826(3) 0.5290(3) -0.0964(3) 0.0234 1.0000 Uani . . . . . .
C7 C 0.8129(3) 0.4972(2) -0.0400(3) 0.0197 1.0000 Uani . . . . . .
C8 C 0.6611(3) 0.3584(3) -0.1637(3) 0.0234 1.0000 Uani . . . . . .
C9 C 0.5604(3) 0.4054(3) -0.1485(3) 0.0283 1.0000 Uani . . . . . .
C10 C 0.6451(3) 0.2582(3) -0.1664(3) 0.0326 1.0000 Uani . . . . . .
C11 C 0.6808(4) 0.3911(3) -0.2692(3) 0.0349 1.0000 Uani . . . . . .
C12 C 0.6502(3) 0.4214(2) 0.2536(3) 0.0228 1.0000 Uani . . . . . .
C13 C 0.6542(3) 0.4554(3) 0.3567(3) 0.0302 1.0000 Uani . . . . . .
C14 C 0.5686(4) 0.4341(4) 0.3993(4) 0.0423 1.0000 Uani . . . . . .
C15 C 0.4801(4) 0.3800(3) 0.3411(4) 0.0433 1.0000 Uani . . . . . .
C16 C 0.4758(4) 0.3461(3) 0.2379(4) 0.0417 1.0000 Uani . . . . . .
C17 C 0.5595(4) 0.3672(3) 0.1937(3) 0.0321 1.0000 Uani . . . . . .
C18 C 0.8773(3) 0.5009(2) 0.2894(3) 0.0218 1.0000 Uani . . . . . .
C19 C 0.8640(4) 0.5849(3) 0.3285(3) 0.0305 1.0000 Uani . . . . . .
C20 C 0.9576(4) 0.6300(3) 0.3992(4) 0.0383 1.0000 Uani . . . . . .
C21 C 1.0641(4) 0.5925(3) 0.4293(3) 0.0376 1.0000 Uani . . . . . .
C22 C 1.0779(3) 0.5100(3) 0.3897(3) 0.0327 1.0000 Uani . . . . . .
C23 C 0.9846(3) 0.4631(3) 0.3212(3) 0.0260 1.0000 Uani . . . . . .
H11 H 0.6739 0.5796 0.1223 0.0267 1.0000 Uiso . U . . . .
H12 H 0.6227 0.5010 0.0307 0.0267 1.0000 Uiso . U . . . .
H31 H 0.7740 0.6862 0.0740 0.0334 1.0000 Uiso . U . . . .
H41 H 0.8935 0.7398 -0.0219 0.0356 1.0000 Uiso . U . . . .
H51 H 0.9595 0.6414 -0.1334 0.0327 1.0000 Uiso . U . . . .
H61 H 0.9126 0.4873 -0.1409 0.0280 1.0000 Uiso . U . . . .
H91 H 0.4907 0.3917 -0.2134 0.0324 1.0000 Uiso . U . . . .
H92 H 0.5739 0.4709 -0.1444 0.0324 1.0000 Uiso . U . . . .
H93 H 0.5501 0.3847 -0.0778 0.0324 1.0000 Uiso . . . . . .
H101 H 0.5737 0.2422 -0.2279 0.0370 1.0000 Uiso . U . . . .
H102 H 0.7107 0.2288 -0.1798 0.0370 1.0000 Uiso . U . . . .
H103 H 0.6404 0.2378 -0.0932 0.0370 1.0000 Uiso . . . . . .
H111 H 0.6109 0.3814 -0.3352 0.0410 1.0000 Uiso . U . . . .
H112 H 0.6993 0.4558 -0.2616 0.0410 1.0000 Uiso . U . . . .
H113 H 0.7452 0.3577 -0.2798 0.0410 1.0000 Uiso . . . . . .
H131 H 0.7180 0.4948 0.3999 0.0371 1.0000 Uiso . U . . . .
H141 H 0.5715 0.4585 0.4734 0.0537 1.0000 Uiso . U . . . .
H151 H 0.4194 0.3652 0.3727 0.0565 1.0000 Uiso . U . . . .
H161 H 0.4120 0.3064 0.1954 0.0533 1.0000 Uiso . U . . . .
H171 H 0.5551 0.3437 0.1188 0.0412 1.0000 Uiso . U . . . .
H191 H 0.7873 0.6128 0.3059 0.0344 1.0000 Uiso . U . . . .
H201 H 0.9477 0.6899 0.4284 0.0438 1.0000 Uiso . U . . . .
H211 H 1.1310 0.6253 0.4798 0.0422 1.0000 Uiso . U . . . .
H221 H 1.1552 0.4835 0.4102 0.0389 1.0000 Uiso . U . . . .
H231 H 0.9948 0.4022 0.2948 0.0311 1.0000 Uiso . U . . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 International_Tables_Vol_IV_Table_2.2B
'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058
76.8986 5.2659 International_Tables_Vol_IV_Table_2.2B
'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Pd1 . Cl2 . 91.64(3) yes
Cl1 . Pd1 . S1 . 87.84(3) yes
Cl2 . Pd1 . S1 . 173.81(3) yes
Cl1 . Pd1 . P1 . 175.99(3) yes
Cl2 . Pd1 . P1 . 84.54(3) yes
S1 . Pd1 . P1 . 95.83(3) yes
Pd1 . S1 . C7 . 112.45(12) yes
Pd1 . S1 . C8 . 115.45(12) yes
C7 . S1 . C8 . 105.30(16) yes
Pd1 . P1 . C1 . 113.44(12) yes
Pd1 . P1 . C12 . 111.38(12) yes
C1 . P1 . C12 . 103.47(16) yes
Pd1 . P1 . C18 . 113.32(13) yes
C1 . P1 . C18 . 103.60(16) yes
C12 . P1 . C18 . 110.99(17) yes
P1 . C1 . C2 . 112.9(2) yes
P1 . C1 . H11 . 108.598 no
C2 . C1 . H11 . 108.597 no
P1 . C1 . H12 . 108.598 no
C2 . C1 . H12 . 108.597 no
H11 . C1 . H12 . 109.466 no
C1 . C2 . C3 . 118.6(3) yes
C1 . C2 . C7 . 123.6(3) yes
C3 . C2 . C7 . 117.7(3) yes
C2 . C3 . C4 . 121.9(4) yes
C2 . C3 . H31 . 119.055 no
C4 . C3 . H31 . 119.055 no
C3 . C4 . C5 . 119.7(4) yes
C3 . C4 . H41 . 120.127 no
C5 . C4 . H41 . 120.126 no
C4 . C5 . C6 . 119.9(3) yes
C4 . C5 . H51 . 120.061 no
C6 . C5 . H51 . 120.061 no
C5 . C6 . C7 . 120.3(3) yes
C5 . C6 . H61 . 119.839 no
C7 . C6 . H61 . 119.839 no
S1 . C7 . C2 . 125.6(3) yes
S1 . C7 . C6 . 113.8(3) yes
C2 . C7 . C6 . 120.4(3) yes
S1 . C8 . C9 . 112.9(2) yes
S1 . C8 . C10 . 105.5(3) yes
C9 . C8 . C10 . 110.9(3) yes
S1 . C8 . C11 . 105.8(3) yes
C9 . C8 . C11 . 110.4(3) yes
C10 . C8 . C11 . 111.2(3) yes
C8 . C9 . H91 . 109.467 no
C8 . C9 . H92 . 109.467 no
H91 . C9 . H92 . 109.476 no
C8 . C9 . H93 . 109.467 no
H91 . C9 . H93 . 109.475 no
H92 . C9 . H93 . 109.476 no
C8 . C10 . H101 . 109.467 no
C8 . C10 . H102 . 109.467 no
H101 . C10 . H102 . 109.475 no
C8 . C10 . H103 . 109.467 no
H101 . C10 . H103 . 109.476 no
H102 . C10 . H103 . 109.476 no
C8 . C11 . H111 . 109.466 no
C8 . C11 . H112 . 109.467 no
H111 . C11 . H112 . 109.475 no
C8 . C11 . H113 . 109.467 no
H111 . C11 . H113 . 109.476 no
H112 . C11 . H113 . 109.476 no
P1 . C12 . C13 . 123.1(3) yes
P1 . C12 . C17 . 117.5(3) yes
C13 . C12 . C17 . 119.4(4) yes
C12 . C13 . C14 . 119.6(4) yes
C12 . C13 . H131 . 120.217 no
C14 . C13 . H131 . 120.219 no
C13 . C14 . C15 . 121.0(4) yes
C13 . C14 . H141 . 119.479 no
C15 . C14 . H141 . 119.480 no
C14 . C15 . C16 . 119.5(4) yes
C14 . C15 . H151 . 120.244 no
C16 . C15 . H151 . 120.244 no
C15 . C16 . C17 . 120.3(4) yes
C15 . C16 . H161 . 119.867 no
C17 . C16 . H161 . 119.864 no
C12 . C17 . C16 . 120.2(4) yes
C12 . C17 . H171 . 119.908 no
C16 . C17 . H171 . 119.910 no
P1 . C18 . C19 . 120.8(3) yes
P1 . C18 . C23 . 119.7(3) yes
C19 . C18 . C23 . 119.4(3) yes
C18 . C19 . C20 . 119.9(4) yes
C18 . C19 . H191 . 120.057 no
C20 . C19 . H191 . 120.058 no
C19 . C20 . C21 . 120.4(4) yes
C19 . C20 . H201 . 119.808 no
C21 . C20 . H201 . 119.806 no
C20 . C21 . C22 . 119.9(4) yes
C20 . C21 . H211 . 120.035 no
C22 . C21 . H211 . 120.035 no
C21 . C22 . C23 . 120.3(4) yes
C21 . C22 . H221 . 119.829 no
C23 . C22 . H221 . 119.828 no
C22 . C23 . C18 . 120.0(4) yes
C22 . C23 . H231 . 119.989 no
C18 . C23 . H231 . 119.987 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Cl1 . 2.3686(9) yes
Pd1 . Cl2 . 2.3157(9) yes
Pd1 . S1 . 2.2979(9) yes
Pd1 . P1 . 2.2247(9) yes
S1 . C7 . 1.780(4) yes
S1 . C8 . 1.879(3) yes
P1 . C1 . 1.830(4) yes
P1 . C12 . 1.812(4) yes
P1 . C18 . 1.809(4) yes
C1 . C2 . 1.500(5) yes
C1 . H11 . 1.000 no
C1 . H12 . 1.000 no
C2 . C3 . 1.393(5) yes
C2 . C7 . 1.412(5) yes
C3 . C4 . 1.384(5) yes
C3 . H31 . 1.000 no
C4 . C5 . 1.383(6) yes
C4 . H41 . 1.000 no
C5 . C6 . 1.392(5) yes
C5 . H51 . 1.000 no
C6 . C7 . 1.390(5) yes
C6 . H61 . 1.000 no
C8 . C9 . 1.519(5) yes
C8 . C10 . 1.523(6) yes
C8 . C11 . 1.525(5) yes
C9 . H91 . 1.000 no
C9 . H92 . 1.000 no
C9 . H93 . 1.000 no
C10 . H101 . 1.000 no
C10 . H102 . 1.000 no
C10 . H103 . 1.000 no
C11 . H111 . 1.000 no
C11 . H112 . 1.000 no
C11 . H113 . 1.000 no
C12 . C13 . 1.392(5) yes
C12 . C17 . 1.399(5) yes
C13 . C14 . 1.394(6) yes
C13 . H131 . 1.000 no
C14 . C15 . 1.375(7) yes
C14 . H141 . 1.000 no
C15 . C16 . 1.392(7) yes
C15 . H151 . 1.000 no
C16 . C17 . 1.385(6) yes
C16 . H161 . 1.000 no
C17 . H171 . 1.000 no
C18 . C19 . 1.391(5) yes
C18 . C23 . 1.392(5) yes
C19 . C20 . 1.393(6) yes
C19 . H191 . 1.000 no
C20 . C21 . 1.381(7) yes
C20 . H201 . 1.000 no
C21 . C22 . 1.376(6) yes
C21 . H211 . 1.000 no
C22 . C23 . 1.393(5) yes
C22 . H221 . 1.000 no
C23 . H231 . 1.000 no
