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#$Date: 2016-03-25 12:16:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179807 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/03/7010317.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_7010317
loop_
_publ_author_name
'Leung, Pak-Hing'
'Qin, Ying'
'He, Guosen'
'Mok, K. F.'
'Vittal, Jagadese J.'
_publ_section_title
;
 Coordination chemistry, reactivities, and stereoelectronic properties
 of chelating phosphine ligands containing thioamide substituents
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              309
_journal_paper_doi               10.1039/b007970g
_journal_year                    2001
_chemical_formula_sum            'C15 H16 Cl2 N P Pd S'
_chemical_formula_weight         450.62
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.122(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1583(2)
_cell_length_b                   12.3121(2)
_cell_length_c                   14.4431(2)
_cell_measurement_reflns_used    6753
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.06
_cell_volume                     1788.28(5)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_method       'ω scans'
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11162
_diffrn_reflns_theta_full        29.34
_diffrn_reflns_theta_max         29.34
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  0.8918
_exptl_absorpt_correction_T_min  0.7236
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'rectangular shape, cut'
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0291
_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)+(0.0319P)²+0.0295P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                3531
_reflns_number_total             4415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007970g.txt
_cod_data_source_block           089
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010317
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.385198(17) 0.324938(14) 0.494347(13) 0.03210(7) Uani 1 1 d . . .
Cl1 Cl 0.18529(6) 0.27196(6) 0.40677(5) 0.05271(18) Uani 1 1 d . . .
Cl2 Cl 0.28757(7) 0.38781(6) 0.62452(5) 0.05584(19) Uani 1 1 d . . .
S1 S 0.59891(7) 0.36426(6) 0.55882(5) 0.04948(18) Uani 1 1 d . . .
C1 C 0.6596(2) 0.32460(18) 0.45996(17) 0.0349(5) Uani 1 1 d . . .
N1 N 0.7815(2) 0.33482(17) 0.44382(16) 0.0423(5) Uani 1 1 d . . .
C2 C 0.8798(3) 0.3909(3) 0.5113(2) 0.0614(8) Uani 1 1 d . . .
H2A H 0.9674 0.3773 0.4963 0.092 Uiso 1 1 calc R . .
H2B H 0.8738 0.3646 0.5732 0.092 Uiso 1 1 calc R . .
H2C H 0.8624 0.4676 0.5087 0.092 Uiso 1 1 calc R . .
C3 C 0.8240(3) 0.2994(3) 0.3554(2) 0.0719(10) Uani 1 1 d . . .
H3A H 0.9121 0.2697 0.3676 0.108 Uiso 1 1 calc R . .
H3B H 0.8237 0.3605 0.3140 0.108 Uiso 1 1 calc R . .
H3C H 0.7638 0.2450 0.3268 0.108 Uiso 1 1 calc R . .
P1 P 0.50886(6) 0.27235(5) 0.38849(4) 0.02987(13) Uani 1 1 d . . .
C4 C 0.4843(2) 0.33874(18) 0.27591(17) 0.0331(5) Uani 1 1 d . . .
C5 C 0.5393(3) 0.3012(2) 0.19867(18) 0.0448(6) Uani 1 1 d . . .
H5 H 0.5889 0.2374 0.2027 0.054 Uiso 1 1 calc R . .
C6 C 0.5196(3) 0.3593(3) 0.1161(2) 0.0578(8) Uani 1 1 d . . .
H6 H 0.5552 0.3345 0.0641 0.069 Uiso 1 1 calc R . .
C7 C 0.4471(3) 0.4543(3) 0.1110(2) 0.0709(10) Uani 1 1 d . . .
H7 H 0.4342 0.4932 0.0553 0.085 Uiso 1 1 calc R . .
C8 C 0.3939(4) 0.4921(3) 0.1868(2) 0.0728(10) Uani 1 1 d . . .
H8 H 0.3463 0.5569 0.1828 0.087 Uiso 1 1 calc R . .
C9 C 0.4110(3) 0.4338(2) 0.2691(2) 0.0486(7) Uani 1 1 d . . .
H9 H 0.3732 0.4585 0.3202 0.058 Uiso 1 1 calc R . .
C10 C 0.5320(2) 0.12915(19) 0.37217(17) 0.0350(5) Uani 1 1 d . . .
C11 C 0.6245(3) 0.0701(2) 0.4323(2) 0.0479(6) Uani 1 1 d . . .
H11 H 0.6789 0.1052 0.4803 0.058 Uiso 1 1 calc R . .
C12 C 0.6358(3) -0.0409(2) 0.4205(2) 0.0600(8) Uani 1 1 d . . .
H12 H 0.6978 -0.0803 0.4607 0.072 Uiso 1 1 calc R . .
C13 C 0.5556(3) -0.0929(2) 0.3498(2) 0.0605(8) Uani 1 1 d . . .
H13 H 0.5649 -0.1672 0.3414 0.073 Uiso 1 1 calc R . .
C14 C 0.4622(3) -0.0364(2) 0.2917(2) 0.0604(8) Uani 1 1 d . . .
H14 H 0.4070 -0.0726 0.2447 0.073 Uiso 1 1 calc R . .
C15 C 0.4496(3) 0.0754(2) 0.3026(2) 0.0492(7) Uani 1 1 d . . .
H15 H 0.3857 0.1138 0.2632 0.059 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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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
P1 Pd1 S1 75.18(2) . . ?
P1 Pd1 Cl1 94.56(2) . . ?
S1 Pd1 Cl1 169.73(3) . . ?
P1 Pd1 Cl2 170.14(3) . . ?
S1 Pd1 Cl2 95.00(3) . . ?
Cl1 Pd1 Cl2 95.25(3) . . ?
C1 S1 Pd1 91.89(9) . . ?
N1 C1 S1 126.1(2) . . ?
N1 C1 P1 132.3(2) . . ?
S1 C1 P1 101.52(12) . . ?
C1 N1 C2 120.2(2) . . ?
C1 N1 C3 122.1(2) . . ?
C2 N1 C3 117.5(2) . . ?
C10 P1 C4 109.26(11) . . ?
C10 P1 C1 107.62(11) . . ?
C4 P1 C1 110.22(11) . . ?
C10 P1 Pd1 118.42(8) . . ?
C4 P1 Pd1 118.10(8) . . ?
C1 P1 Pd1 91.07(8) . . ?
C9 C4 C5 119.8(2) . . ?
C9 C4 P1 116.83(18) . . ?
C5 C4 P1 123.35(19) . . ?
C6 C5 C4 119.5(3) . . ?
C7 C6 C5 119.8(3) . . ?
C8 C7 C6 121.0(3) . . ?
C7 C8 C9 119.7(3) . . ?
C8 C9 C4 120.2(3) . . ?
C15 C10 C11 119.3(2) . . ?
C15 C10 P1 119.2(2) . . ?
C11 C10 P1 121.3(2) . . ?
C12 C11 C10 120.0(3) . . ?
C13 C12 C11 120.1(3) . . ?
C14 C13 C12 120.5(3) . . ?
C13 C14 C15 120.0(3) . . ?
C10 C15 C14 120.0(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 P1 2.2086(6) . ?
Pd1 S1 2.2899(7) . ?
Pd1 Cl1 2.3288(7) . ?
Pd1 Cl2 2.3758(7) . ?
S1 C1 1.705(3) . ?
C1 N1 1.298(3) . ?
C1 P1 1.838(2) . ?
N1 C2 1.466(3) . ?
N1 C3 1.471(4) . ?
P1 C10 1.799(2) . ?
P1 C4 1.805(2) . ?
C4 C9 1.384(3) . ?
C4 C5 1.395(3) . ?
C5 C6 1.381(4) . ?
C6 C7 1.378(4) . ?
C7 C8 1.369(5) . ?
C8 C9 1.379(4) . ?
C10 C15 1.383(4) . ?
C10 C11 1.391(4) . ?
C11 C12 1.383(4) . ?
C12 C13 1.372(5) . ?
C13 C14 1.365(5) . ?
C14 C15 1.393(4) . ?
