#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/83/7008371.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_7008371
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
;
synthesis as described
;
_chemical_formula_moiety         ' C21 H22 Cl P Pd S '
_chemical_formula_sum            'C21 H22 Cl P Pd S'
_chemical_formula_weight         479.30
_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
_cell_angle_alpha                101.530(2)
_cell_angle_beta                 97.460(2)
_cell_angle_gamma                116.200(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7350(10)
_cell_length_b                   9.2150(10)
_cell_length_c                   14.7010(10)
_cell_measurement_reflns_used    8187
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     1007.81(18)
_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 0.996
_diffrn_measured_fraction_theta_max 0.987
_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  0.02
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8328
_diffrn_reflns_theta_full        25.331
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_min         2.679
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.13
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0815
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000626
_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:
2.03 0.311 1.71
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0653
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0568
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                3219
_reflns_number_total             4579
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b502195b.txt
_cod_data_source_block           1
_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 2.4.1 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 '
_cod_original_formula_sum        ' C21 H22 Cl P Pd S '
_cod_database_code               7008371
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_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 0.28047(5) -0.13322(5) 0.71931(3) 0.0219 1.0000 Uani . . . . . .
Cl1 Cl 0.24520(19) -0.40896(16) 0.69938(10) 0.0326 1.0000 Uani . . . . . .
S1 S 0.14833(16) -0.20320(14) 0.54967(8) 0.0237 1.0000 Uani . . . . . .
P1 P 0.30039(16) 0.11897(14) 0.74832(9) 0.0207 1.0000 Uani . . . . . .
C1 C 0.3778(8) -0.0764(7) 0.8652(4) 0.0341 1.0000 Uani . . . . . .
C2 C 0.1981(7) -0.3495(6) 0.4763(4) 0.0307 1.0000 Uani . . . . . .
C3 C 0.2354(6) -0.0229(6) 0.5064(3) 0.0212 1.0000 Uani . . . . . .
C4 C 0.2964(7) -0.0278(7) 0.4231(4) 0.0303 1.0000 Uani . . . . . .
C5 C 0.3554(7) 0.1128(7) 0.3894(4) 0.0305 1.0000 Uani . . . . . .
C6 C 0.3540(7) 0.2575(7) 0.4372(4) 0.0307 1.0000 Uani . . . . . .
C7 C 0.2947(7) 0.2618(6) 0.5208(4) 0.0258 1.0000 Uani . . . . . .
C8 C 0.2334(6) 0.1214(6) 0.5563(4) 0.0251 1.0000 Uani . . . . . .
C9 C 0.1680(6) 0.1329(6) 0.6455(3) 0.0219 1.0000 Uani . . . . . .
C10 C 0.5196(6) 0.2920(6) 0.7688(3) 0.0222 1.0000 Uani . . . . . .
C11 C 0.6671(6) 0.2672(6) 0.7867(4) 0.0251 1.0000 Uani . . . . . .
C12 C 0.8330(7) 0.3948(7) 0.7932(4) 0.0324 1.0000 Uani . . . . . .
C13 C 0.8550(7) 0.5488(7) 0.7830(4) 0.0353 1.0000 Uani . . . . . .
C14 C 0.7130(9) 0.5760(7) 0.7684(4) 0.0383 1.0000 Uani . . . . . .
C15 C 0.5430(7) 0.4493(6) 0.7608(4) 0.0322 1.0000 Uani . . . . . .
C16 C 0.2015(7) 0.1729(7) 0.8423(4) 0.0267 1.0000 Uani . . . . . .
C17 C 0.2763(7) 0.3313(7) 0.9091(4) 0.0360 1.0000 Uani . . . . . .
C18 C 0.1841(9) 0.3641(8) 0.9734(4) 0.0426 1.0000 Uani . . . . . .
C19 C 0.0191(9) 0.2417(8) 0.9725(4) 0.0404 1.0000 Uani . . . . . .
C20 C -0.0561(8) 0.0853(8) 0.9058(5) 0.0409 1.0000 Uani . . . . . .
C21 C 0.0340(8) 0.0508(7) 0.8419(4) 0.0375 1.0000 Uani . . . . . .
H41 H 0.2976 -0.1320 0.3881 0.0355 1.0000 Uiso . . . . . .
H51 H 0.3992 0.1095 0.3298 0.0376 1.0000 Uiso . . . . . .
H61 H 0.3952 0.3580 0.4121 0.0364 1.0000 Uiso . . . . . .
H71 H 0.2959 0.3671 0.5561 0.0320 1.0000 Uiso . . . . . .
H91 H 0.1683 0.2435 0.6641 0.0244 1.0000 Uiso . . . . . .
H92 H 0.0448 0.0384 0.6307 0.0244 1.0000 Uiso . . . . . .
H111 H 0.6517 0.1567 0.7947 0.0293 1.0000 Uiso . . . . . .
H121 H 0.9373 0.3762 0.8054 0.0363 1.0000 Uiso . . . . . .
H131 H 0.9749 0.6401 0.7862 0.0369 1.0000 Uiso . . . . . .
H141 H 0.7312 0.6887 0.7630 0.0418 1.0000 Uiso . . . . . .
H151 H 0.4401 0.4703 0.7499 0.0357 1.0000 Uiso . . . . . .
H171 H 0.3960 0.4212 0.9108 0.0378 1.0000 Uiso . . . . . .
H181 H 0.2382 0.4782 1.0211 0.0466 1.0000 Uiso . . . . . .
H191 H -0.0453 0.2660 1.0198 0.0523 1.0000 Uiso . . . . . .
H201 H -0.1766 -0.0034 0.9038 0.0467 1.0000 Uiso . . . . . .
H211 H -0.0215 -0.0636 0.7945 0.0417 1.0000 Uiso . . . . . .
H21 H 0.1536 -0.4561 0.4956 0.0370 1.0000 Uiso . . . . . .
H22 H 0.3285 -0.2983 0.4848 0.0370 1.0000 Uiso . . . . . .
H23 H 0.1400 -0.3754 0.4075 0.0370 1.0000 Uiso . . . . . .
H11 H 0.3872 -0.1741 0.8796 0.0417 1.0000 Uiso . . . . . .
H12 H 0.2964 -0.0534 0.9001 0.0417 1.0000 Uiso . . . . . .
H13 H 0.4969 0.0258 0.8863 0.0417 1.0000 Uiso . . . . . .
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 ' 0.0020 0.0020 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
'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
'Cl ' 0.1320 0.1590 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
'S ' 0.1100 0.1240 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
'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
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 . S1 . 91.05(5) yes
Cl1 . Pd1 . P1 . 174.74(5) yes
S1 . Pd1 . P1 . 92.09(4) yes
Cl1 . Pd1 . C1 . 89.51(16) yes
S1 . Pd1 . C1 . 176.44(18) yes
P1 . Pd1 . C1 . 87.10(16) yes
Pd1 . S1 . C2 . 112.37(19) yes
Pd1 . S1 . C3 . 111.61(16) yes
C2 . S1 . C3 . 103.7(2) yes
Pd1 . P1 . C9 . 110.48(15) yes
Pd1 . P1 . C10 . 115.19(16) yes
C9 . P1 . C10 . 105.1(2) yes
Pd1 . P1 . C16 . 116.29(17) yes
C9 . P1 . C16 . 99.8(2) yes
C10 . P1 . C16 . 108.4(2) yes
Pd1 . C1 . H11 . 109.468 no
Pd1 . C1 . H12 . 109.468 no
H11 . C1 . H12 . 109.476 no
Pd1 . C1 . H13 . 109.467 no
H11 . C1 . H13 . 109.474 no
H12 . C1 . H13 . 109.475 no
S1 . C2 . H21 . 109.467 no
S1 . C2 . H22 . 109.466 no
H21 . C2 . H22 . 109.474 no
S1 . C2 . H23 . 109.468 no
H21 . C2 . H23 . 109.476 no
H22 . C2 . H23 . 109.476 no
S1 . C3 . C4 . 121.4(4) yes
S1 . C3 . C8 . 117.6(4) yes
C4 . C3 . C8 . 120.9(4) yes
C3 . C4 . C5 . 119.6(5) yes
C3 . C4 . H41 . 120.196 no
C5 . C4 . H41 . 120.196 no
C4 . C5 . C6 . 120.7(5) yes
C4 . C5 . H51 . 119.665 no
C6 . C5 . H51 . 119.669 no
C5 . C6 . C7 . 119.3(5) yes
C5 . C6 . H61 . 120.351 no
C7 . C6 . H61 . 120.351 no
C6 . C7 . C8 . 121.3(5) yes
C6 . C7 . H71 . 119.332 no
C8 . C7 . H71 . 119.333 no
C7 . C8 . C3 . 118.2(5) yes
C7 . C8 . C9 . 118.8(4) yes
C3 . C8 . C9 . 123.1(4) yes
C8 . C9 . P1 . 114.4(3) yes
C8 . C9 . H91 . 108.231 no
P1 . C9 . H91 . 108.232 no
C8 . C9 . H92 . 108.231 no
P1 . C9 . H92 . 108.232 no
H91 . C9 . H92 . 109.466 no
P1 . C10 . C11 . 120.4(4) yes
P1 . C10 . C15 . 120.1(4) yes
C11 . C10 . C15 . 119.5(4) yes
C10 . C11 . C12 . 120.3(5) yes
C10 . C11 . H111 . 119.845 no
C12 . C11 . H111 . 119.843 no
C11 . C12 . C13 . 120.0(5) yes
C11 . C12 . H121 . 119.985 no
C13 . C12 . H121 . 119.987 no
C12 . C13 . C14 . 120.2(5) yes
C12 . C13 . H131 . 119.922 no
C14 . C13 . H131 . 119.920 no
C13 . C14 . C15 . 121.3(5) yes
C13 . C14 . H141 . 119.355 no
C15 . C14 . H141 . 119.355 no
C10 . C15 . C14 . 118.7(5) yes
C10 . C15 . H151 . 120.644 no
C14 . C15 . H151 . 120.645 no
P1 . C16 . C17 . 124.1(4) yes
P1 . C16 . C21 . 117.2(4) yes
C17 . C16 . C21 . 118.5(5) yes
C16 . C17 . C18 . 119.8(5) yes
C16 . C17 . H171 . 120.090 no
C18 . C17 . H171 . 120.090 no
C17 . C18 . C19 . 121.0(5) yes
C17 . C18 . H181 . 119.504 no
C19 . C18 . H181 . 119.502 no
C18 . C19 . C20 . 119.3(5) yes
C18 . C19 . H191 . 120.335 no
C20 . C19 . H191 . 120.333 no
C19 . C20 . C21 . 120.3(6) yes
C19 . C20 . H201 . 119.843 no
C21 . C20 . H201 . 119.843 no
C16 . C21 . C20 . 121.0(5) yes
C16 . C21 . H211 . 119.476 no
C20 . C21 . H211 . 119.477 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 . 2.3717(13) yes
Pd1 . S1 . 2.4331(13) yes
Pd1 . P1 . 2.2001(12) yes
Pd1 . C1 . 2.069(6) yes
S1 . C2 . 1.797(5) yes
S1 . C3 . 1.781(4) yes
P1 . C9 . 1.842(5) yes
P1 . C10 . 1.806(5) yes
P1 . C16 . 1.821(5) yes
C1 . H11 . 1.000 no
C1 . H12 . 1.000 no
C1 . H13 . 1.000 no
C2 . H21 . 1.000 no
C2 . H22 . 1.000 no
C2 . H23 . 1.000 no
C3 . C4 . 1.399(7) yes
C3 . C8 . 1.393(7) yes
C4 . C5 . 1.387(8) yes
C4 . H41 . 1.000 no
C5 . C6 . 1.383(8) yes
C5 . H51 . 1.000 no
C6 . C7 . 1.394(7) yes
C6 . H61 . 1.000 no
C7 . C8 . 1.401(7) yes
C7 . H71 . 1.000 no
C8 . C9 . 1.499(7) yes
C9 . H91 . 1.000 no
C9 . H92 . 1.000 no
C10 . C11 . 1.406(7) yes
C10 . C15 . 1.404(7) yes
C11 . C12 . 1.380(7) yes
C11 . H111 . 1.000 no
C12 . C13 . 1.388(8) yes
C12 . H121 . 1.000 no
C13 . C14 . 1.369(9) yes
C13 . H131 . 1.000 no
C14 . C15 . 1.398(8) yes
C14 . H141 . 1.000 no
C15 . H151 . 1.000 no
C16 . C17 . 1.393(7) yes
C16 . C21 . 1.396(8) yes
C17 . C18 . 1.390(8) yes
C17 . H171 . 1.000 no
C18 . C19 . 1.380(9) yes
C18 . H181 . 1.000 no
C19 . C20 . 1.379(9) yes
C19 . H191 . 1.000 no
C20 . C21 . 1.377(8) yes
C20 . H201 . 1.000 no
C21 . H211 . 1.000 no
