#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:16:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179807 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/03/7010315.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_7010315
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            'C31 H38 Cl N2 O4 P Pd S'
_chemical_formula_weight         707.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7346(2)
_cell_length_b                   14.3998(3)
_cell_length_c                   20.3434(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3144.60(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18439
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       'Plate-like crystal fragment'
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.401
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_obs          0.0379
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0552P)²+0.9022P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1025
_refine_ls_wR_factor_obs         0.0891
_reflns_number_observed          5694
_reflns_number_total             6426
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b007970g.txt
_cod_data_source_block           kf1a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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^)+(0.0552P)^2^+0.9022P] 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^)+(0.0552P)^2^+0.9022P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7010315
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd Pd 0.67096(3) 0.18256(2) 0.155821(14) 0.03115(9) Uani 1 d . .
C1 C 0.4958(4) 0.1364(3) 0.1410(2) 0.0320(9) Uani 1 d . .
C2 C 0.3864(4) 0.1608(3) 0.1758(2) 0.0360(10) Uani 1 d . .
H2A H 0.3932(4) 0.1960(3) 0.2140(2) 0.043 Uiso 1 calc R .
C3 C 0.2720(4) 0.1341(3) 0.1548(3) 0.0428(9) Uani 1 d . .
H3A H 0.2016(4) 0.1536(3) 0.1777(3) 0.051 Uiso 1 calc R .
C4 C 0.2580(4) 0.0773(3) 0.0987(2) 0.0383(10) Uani 1 d . .
C5 C 0.1397(4) 0.0439(4) 0.0788(2) 0.0518(12) Uani 1 d . .
H5A H 0.0688(4) 0.0639(4) 0.1009(2) 0.062 Uiso 1 calc R .
C6 C 0.1276(5) -0.0168(4) 0.0278(3) 0.0630(15) Uani 1 d . .
H6A H 0.0494(5) -0.0385(4) 0.0155(3) 0.076 Uiso 1 calc R .
C7 C 0.2345(5) -0.0462(4) -0.0058(3) 0.0587(14) Uani 1 d . .
H7A H 0.2266(5) -0.0891(4) -0.0397(3) 0.070 Uiso 1 calc R .
C8 C 0.3494(5) -0.0137(3) 0.0098(2) 0.0471(11) Uani 1 d . .
H8A H 0.4180(5) -0.0324(3) -0.0147(2) 0.056 Uiso 1 calc R .
C9 C 0.3661(4) 0.0493(3) 0.0637(2) 0.0365(9) Uani 1 d . .
C10 C 0.4844(4) 0.0840(3) 0.0841(2) 0.0351(9) Uani 1 d . .
C11 C 0.6033(4) 0.0636(3) 0.0472(2) 0.0413(10) Uani 1 d . .
H11A H 0.5837(4) 0.0508(3) 0.0010(2) 0.050 Uiso 1 calc R .
N12 N 0.6824(4) 0.1508(3) 0.0516(2) 0.0414(8) Uani 1 d . .
C13 C 0.6711(6) -0.0201(4) 0.0768(3) 0.0640(14) Uani 1 d . .
H13A H 0.7462(6) -0.0317(4) 0.0526(3) 0.096 Uiso 1 calc R .
H13B H 0.6181(6) -0.0737(4) 0.0746(3) 0.096 Uiso 1 calc R .
H13C H 0.6914(6) -0.0074(4) 0.1219(3) 0.096 Uiso 1 calc R .
C14 C 0.6236(6) 0.2264(4) 0.0133(3) 0.065(2) Uani 1 d . .
H14A H 0.5411(6) 0.2376(4) 0.0298(3) 0.098 Uiso 1 calc R .
H14B H 0.6190(6) 0.2087(4) -0.0321(3) 0.098 Uiso 1 calc R .
H14C H 0.6725(6) 0.2819(4) 0.0175(3) 0.098 Uiso 1 calc R .
C15 C 0.8079(5) 0.1353(5) 0.0254(3) 0.078(2) Uani 1 d . .
H15A H 0.8477(5) 0.0864(5) 0.0497(3) 0.117 Uiso 1 calc R .
H15B H 0.8559(5) 0.1913(5) 0.0295(3) 0.117 Uiso 1 calc R .
H15C H 0.8024(5) 0.1181(5) -0.0201(3) 0.117 Uiso 1 calc R .
P16 P 0.65238(8) 0.18013(7) 0.26366(4) 0.0288(2) Uani 1 d . .
C17 C 0.5983(4) 0.0702(3) 0.2972(2) 0.0356(9) Uani 1 d . .
C18 C 0.4874(5) 0.0617(3) 0.3317(2) 0.0485(11) Uani 1 d . .
H18A H 0.4357(5) 0.1128(3) 0.3378(2) 0.058 Uiso 1 calc R .
C19 C 0.4551(5) -0.0246(4) 0.3567(2) 0.0602(15) Uani 1 d . .
H19A H 0.3811(5) -0.0313(4) 0.3800(2) 0.072 Uiso 1 calc R .
C20 C 0.5309(6) -0.1002(3) 0.3476(3) 0.0641(14) Uani 1 d . .
H20A H 0.5086(6) -0.1574(3) 0.3653(3) 0.077 Uiso 1 calc R .
C21 C 0.6399(5) -0.0920(3) 0.3124(3) 0.0617(15) Uani 1 d . .
H21A H 0.6914(5) -0.1432(3) 0.3062(3) 0.074 Uiso 1 calc R .
C22 C 0.6719(5) -0.0063(3) 0.2864(3) 0.0516(11) Uani 1 d . .
H22A H 0.7440(5) -0.0005(3) 0.2614(3) 0.062 Uiso 1 calc R .
C23 C 0.5932(4) 0.2764(3) 0.3155(2) 0.0322(9) Uani 1 d . .
H23A H 0.5037(4) 0.2890(3) 0.3118(2) 0.039 Uiso 1 calc R .
C24 C 0.6374(4) 0.2436(3) 0.3830(2) 0.0317(9) Uani 1 d . .
C25 C 0.7515(4) 0.2077(3) 0.3784(2) 0.0354(10) Uani 1 d . .
C26 C 0.7976(4) 0.2089(3) 0.3072(2) 0.0313(9) Uani 1 d . .
H26A H 0.8688(4) 0.1685(3) 0.2977(2) 0.038 Uiso 1 calc R .
C27 C 0.8139(3) 0.3125(3) 0.2879(2) 0.0317(8) Uani 1 d . .
H27A H 0.8656(3) 0.3422(3) 0.3215(2) 0.038 Uiso 1 calc R .
C28 C 0.6794(4) 0.3551(3) 0.2926(2) 0.0353(9) Uani 1 d . .
H28A H 0.6780(4) 0.4060(3) 0.3238(2) 0.042 Uiso 1 calc R .
H28B H 0.6530(4) 0.3783(3) 0.2500(2) 0.042 Uiso 1 calc R .
C29 C 0.5572(5) 0.2523(4) 0.4423(2) 0.0486(12) Uani 1 d . .
H29A H 0.4798(5) 0.2811(4) 0.4304(2) 0.073 Uiso 1 calc R .
H29B H 0.5988(5) 0.2896(4) 0.4746(2) 0.073 Uiso 1 calc R .
H29C H 0.5412(5) 0.1917(4) 0.4601(2) 0.073 Uiso 1 calc R .
C30 C 0.8329(5) 0.1705(4) 0.4320(2) 0.0590(13) Uani 1 d . .
H30A H 0.9101(5) 0.1493(4) 0.4136(2) 0.088 Uiso 1 calc R .
H30B H 0.7915(5) 0.1196(4) 0.4534(2) 0.088 Uiso 1 calc R .
H30C H 0.8491(5) 0.2186(4) 0.4635(2) 0.088 Uiso 1 calc R .
C31 C 0.8750(4) 0.3291(3) 0.2216(2) 0.0360(9) Uani 1 d . .
N32 N 0.9324(4) 0.4083(3) 0.2125(2) 0.0462(9) Uani 1 d . .
C33 C 0.9438(6) 0.4800(4) 0.2645(3) 0.065(2) Uani 1 d . .
H33A H 0.9890(6) 0.5323(4) 0.2476(3) 0.098 Uiso 1 calc R .
H33B H 0.9875(6) 0.4545(4) 0.3015(3) 0.098 Uiso 1 calc R .
H33C H 0.8622(6) 0.4995(4) 0.2780(3) 0.098 Uiso 1 calc R .
C34 C 0.9943(6) 0.4311(4) 0.1502(3) 0.072(2) Uani 1 d . .
H34A H 1.0308(6) 0.4919(4) 0.1532(3) 0.108 Uiso 1 calc R .
H34B H 0.9344(6) 0.4302(4) 0.1152(3) 0.108 Uiso 1 calc R .
H34C H 1.0584(6) 0.3863(4) 0.1414(3) 0.108 Uiso 1 calc R .
S35 S 0.87429(11) 0.24856(9) 0.15984(6) 0.0523(3) Uani 1 d . .
Cl1 Cl 1.16246(11) 0.25443(9) 0.33983(7) 0.0542(3) Uani 1 d . .
O1 O 1.0938(5) 0.3139(5) 0.3808(3) 0.111(2) Uani 1 d . .
O2 O 1.2869(4) 0.2582(5) 0.3495(4) 0.144(3) Uani 1 d . .
O3 O 1.1196(7) 0.1638(4) 0.3461(5) 0.164(3) Uani 1 d . .
O4 O 1.1327(8) 0.2746(8) 0.2766(3) 0.190(4) Uani 1 d . .
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'
O O 0.0106 0.0060 '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
C1 Pd N12 80.61(15) . . ?
C1 Pd P16 93.41(11) . . ?
N12 Pd P16 166.80(10) . . ?
C1 Pd S35 172.24(11) . . ?
N12 Pd S35 93.78(10) . . ?
P16 Pd S35 93.16(4) . . ?
C10 C1 C2 118.7(4) . . ?
C10 C1 Pd 112.8(3) . . ?
C2 C1 Pd 128.0(3) . . ?
C3 C2 C1 121.5(4) . . ?
C2 C3 C4 121.1(4) . . ?
C3 C4 C5 121.6(4) . . ?
C3 C4 C9 118.9(4) . . ?
C5 C4 C9 119.5(4) . . ?
C6 C5 C4 121.4(5) . . ?
C5 C6 C7 119.1(5) . . ?
C8 C7 C6 121.8(5) . . ?
C7 C8 C9 120.7(5) . . ?
C4 C9 C10 118.8(4) . . ?
C4 C9 C8 117.4(4) . . ?
C10 C9 C8 123.8(4) . . ?
C1 C10 C9 120.8(4) . . ?
C1 C10 C11 116.5(4) . . ?
C9 C10 C11 122.6(4) . . ?
C10 C11 N12 106.4(3) . . ?
C10 C11 C13 111.1(4) . . ?
N12 C11 C13 111.3(4) . . ?
C15 N12 C14 108.2(5) . . ?
C15 N12 C11 111.5(4) . . ?
C14 N12 C11 109.8(4) . . ?
C15 N12 Pd 116.0(3) . . ?
C14 N12 Pd 109.6(3) . . ?
C11 N12 Pd 101.6(2) . . ?
C17 P16 C26 106.6(2) . . ?
C17 P16 C23 109.1(2) . . ?
C26 P16 C23 81.3(2) . . ?
C17 P16 Pd 114.60(14) . . ?
C26 P16 Pd 113.53(13) . . ?
C23 P16 Pd 125.83(14) . . ?
C22 C17 C18 120.2(4) . . ?
C22 C17 P16 117.0(4) . . ?
C18 C17 P16 122.8(3) . . ?
C17 C18 C19 118.7(5) . . ?
C20 C19 C18 120.9(5) . . ?
C19 C20 C21 120.4(5) . . ?
C20 C21 C22 119.1(5) . . ?
C17 C22 C21 120.7(5) . . ?
C24 C23 C28 108.3(3) . . ?
C24 C23 P16 100.0(3) . . ?
C28 C23 P16 99.9(3) . . ?
C25 C24 C29 128.4(4) . . ?
C25 C24 C23 110.1(4) . . ?
C29 C24 C23 121.5(4) . . ?
C24 C25 C30 128.7(4) . . ?
C24 C25 C26 111.0(4) . . ?
C30 C25 C26 120.3(4) . . ?
C25 C26 C27 106.7(3) . . ?
C25 C26 P16 100.3(3) . . ?
C27 C26 P16 101.0(2) . . ?
C31 C27 C26 115.2(3) . . ?
C31 C27 C28 112.9(3) . . ?
C26 C27 C28 104.8(3) . . ?
C23 C28 C27 106.5(3) . . ?
N32 C31 C27 117.9(4) . . ?
N32 C31 S35 119.2(3) . . ?
C27 C31 S35 122.9(3) . . ?
C31 N32 C34 122.1(4) . . ?
C31 N32 C33 122.9(4) . . ?
C34 N32 C33 115.0(4) . . ?
C31 S35 Pd 107.44(14) . . ?
O2 Cl1 O4 111.2(6) . . ?
O2 Cl1 O3 110.6(4) . . ?
O4 Cl1 O3 102.1(6) . . ?
O2 Cl1 O1 114.1(4) . . ?
O4 Cl1 O1 108.0(5) . . ?
O3 Cl1 O1 110.2(4) . . ?
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
Pd C1 2.017(4) . ?
Pd N12 2.172(3) . ?
Pd P16 2.2031(9) . ?
Pd S35 2.3820(11) . ?
C1 C10 1.386(5) . ?
C1 C2 1.417(6) . ?
C2 C3 1.357(6) . ?
C3 C4 1.412(7) . ?
C4 C5 1.417(6) . ?
C4 C9 1.421(6) . ?
C5 C6 1.363(8) . ?
C6 C7 1.401(8) . ?
C7 C8 1.356(7) . ?
C8 C9 1.434(6) . ?
C9 C10 1.427(6) . ?
C10 C11 1.510(6) . ?
C11 N12 1.518(6) . ?
C11 C13 1.531(7) . ?
N12 C15 1.466(6) . ?
N12 C14 1.480(7) . ?
P16 C17 1.818(4) . ?
P16 C26 1.840(4) . ?
P16 C23 1.854(4) . ?
C17 C22 1.374(7) . ?
C17 C18 1.387(6) . ?
C18 C19 1.387(7) . ?
C19 C20 1.372(8) . ?
C20 C21 1.377(8) . ?
C21 C22 1.386(7) . ?
C23 C24 1.527(6) . ?
C23 C28 1.536(6) . ?
C24 C25 1.333(6) . ?
C24 C29 1.488(6) . ?
C25 C30 1.496(6) . ?
C25 C26 1.531(6) . ?
C26 C27 1.552(5) . ?
C27 C31 1.517(5) . ?
C27 C28 1.571(6) . ?
C31 N32 1.309(6) . ?
C31 S35 1.711(4) . ?
N32 C34 1.469(6) . ?
N32 C33 1.484(6) . ?
Cl1 O2 1.351(5) . ?
Cl1 O4 1.356(7) . ?
Cl1 O3 1.389(6) . ?
Cl1 O1 1.404(5) . ?
