#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:32:26 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179185 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/31/4313162.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_4313162
loop_
_publ_author_name
'U. Anandhi'
'Todd Holbert'
'Dennis Lueng'
'Paul R. Sharp'
_publ_contact_author
;
 Paul R. Sharp
 Department of Chemistry
 University of Missouri
 Columbia, MO  65211
;
_publ_contact_author_email       SharpP@missouri.edu
_publ_contact_author_fax         573-882-2754
_publ_contact_author_phone       573-882-7715
_publ_section_title
;
 Platinum and Palladium Imido and Oxo Complexes with Small Natural Bite
 Angle Diphosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1282
_journal_page_last               1295
_journal_paper_doi               10.1021/ic025987f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C27 H23 F6 N O6 P2 Pd S2'
_chemical_formula_weight         803.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.873(5)
_cell_angle_beta                 102.687(5)
_cell_angle_gamma                116.755(4)
_cell_formula_units_Z            1
_cell_length_a                   9.048(3)
_cell_length_b                   9.051(3)
_cell_length_c                   11.395(3)
_cell_measurement_temperature    173(2)
_cell_volume                     782.6(4)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
 ORTEP (Johnson, 1976), ORTEP 3 for Windows
 L. J. Farrugia, 1997' 
;
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement
;
 SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to
 SHELX-97 and POV-Ray, 1999
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.866
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5001
_diffrn_reflns_theta_full        28.66
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).   
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.997
_refine_diff_density_min         -1.871
_refine_diff_density_rms         0.207
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_coef       0.001(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         4131
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1289P)²+1.2490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1634
_reflns_number_gt                4036
_reflns_number_total             4131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025987f-2_s1_3.cif
_cod_data_source_block           Pd(OTf)2(dppma)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 '
_cod_database_code               4313162
loop_
_symmetry_equiv_pos_as_xyz
'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_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 0.06061(2) 0.68561(2) 0.83540(2) 0.01773(18) Uani 1 1 d . . .
S1 S 0.2660(3) 0.6047(3) 1.0714(2) 0.0246(4) Uani 1 1 d . . .
S2 S 0.2281(3) 0.7669(3) 0.6068(2) 0.0251(4) Uiso 1 1 d . . .
P1 P -0.1263(3) 0.6594(3) 0.9407(2) 0.0193(5) Uani 1 1 d . . .
P2 P -0.1541(3) 0.7125(3) 0.7207(2) 0.0186(5) Uani 1 1 d . . .
F1 F 0.0024(10) 0.4543(10) 0.4696(8) 0.061(2) Uani 1 1 d . . .
F2 F 0.1725(15) 0.6141(14) 0.3800(7) 0.073(3) Uani 1 1 d . . .
F3 F 0.2687(13) 0.5104(12) 0.5164(8) 0.069(2) Uani 1 1 d . . .
F4 F 0.4116(16) 0.9265(12) 1.1885(12) 0.090(3) Uani 1 1 d . . .
F5 F 0.4865(13) 0.7767(13) 1.2941(8) 0.080(3) Uani 1 1 d . . .
F6 F 0.5878(9) 0.8475(13) 1.1451(9) 0.075(3) Uani 1 1 d . . .
O1 O 0.2209(9) 0.7017(9) 0.7200(7) 0.0228(15) Uani 1 1 d . . .
O2 O 0.1035(11) 0.8174(11) 0.5666(8) 0.0405(17) Uani 1 1 d . . .
O3 O 0.4066(10) 0.8832(12) 0.6172(8) 0.0447(19) Uani 1 1 d . . .
O4 O 0.2597(10) 0.6581(11) 0.9561(7) 0.0291(17) Uani 1 1 d . . .
O5 O 0.1203(9) 0.5746(11) 1.1137(7) 0.0384(17) Uani 1 1 d . . .
O6 O 0.3227(11) 0.4823(11) 1.0743(8) 0.0444(19) Uani 1 1 d . . .
N1 N -0.2575(9) 0.6866(8) 0.8282(6) 0.0192(13) Uani 1 1 d . . .
C1 C -0.0649(10) 0.8225(11) 1.0806(8) 0.0224(15) Uani 1 1 d . . .
C2 C -0.0404(12) 0.9848(12) 1.0672(9) 0.0294(18) Uani 1 1 d . . .
H2 H -0.0527 1.0061 0.9872 0.035 Uiso 1 1 calc R . .
C3 C 0.0013(14) 1.1108(13) 1.1706(10) 0.037(2) Uani 1 1 d . . .
H3 H 0.0169 1.2195 1.1624 0.044 Uiso 1 1 calc R . .
C4 C 0.0205(14) 1.0793(14) 1.2868(11) 0.041(2) Uani 1 1 d . . .
H4 H 0.0481 1.1668 1.3579 0.049 Uiso 1 1 calc R . .
C5 C 0.0003(13) 0.9239(13) 1.3015(9) 0.035(2) Uani 1 1 d . . .
H5 H 0.0152 0.9052 1.3822 0.042 Uiso 1 1 calc R . .
C6 C -0.0420(14) 0.7935(14) 1.1978(10) 0.028(2) Uani 1 1 d . . .
H6 H -0.0550 0.6861 1.2075 0.033 Uiso 1 1 calc R . .
C7 C -0.2511(10) 0.4493(10) 0.9585(8) 0.0222(16) Uani 1 1 d . . .
C8 C -0.3825(11) 0.4162(11) 1.0141(9) 0.0264(17) Uani 1 1 d . . .
H8 H -0.3952 0.5078 1.0526 0.032 Uiso 1 1 calc R . .
C9 C -0.4943(13) 0.2479(13) 1.0124(9) 0.036(2) Uani 1 1 d . . .
H9 H -0.5853 0.2232 1.0483 0.044 Uiso 1 1 calc R . .
C10 C -0.4706(15) 0.1159(12) 0.9569(11) 0.042(3) Uani 1 1 d . . .
H10 H -0.5441 0.0014 0.9579 0.050 Uiso 1 1 calc R . .
C11 C -0.3438(15) 0.1480(13) 0.9011(11) 0.040(2) Uani 1 1 d . . .
H11 H -0.3328 0.0558 0.8614 0.048 Uiso 1 1 calc R . .
C12 C -0.2309(12) 0.3159(12) 0.9027(9) 0.0295(18) Uani 1 1 d . . .
H12 H -0.1408 0.3391 0.8660 0.035 Uiso 1 1 calc R . .
C13 C -0.1004(11) 0.9183(11) 0.6963(8) 0.0239(16) Uani 1 1 d . . .
C14 C 0.0666(13) 1.0603(13) 0.7666(10) 0.036(2) Uani 1 1 d . . .
H14 H 0.1515 1.0426 0.8185 0.043 Uiso 1 1 calc R . .
C15 C 0.1054(17) 1.2240(14) 0.7596(13) 0.049(3) Uani 1 1 d . . .
H15 H 0.2148 1.3194 0.8104 0.059 Uiso 1 1 calc R . .
C16 C -0.013(2) 1.2503(15) 0.6797(14) 0.057(4) Uani 1 1 d . . .
H16 H 0.0178 1.3628 0.6718 0.068 Uiso 1 1 calc R . .
C17 C -0.175(2) 1.1139(16) 0.6111(13) 0.052(3) Uani 1 1 d . . .
H17 H -0.2579 1.1340 0.5586 0.062 Uiso 1 1 calc R . .
C18 C -0.2210(14) 0.9470(15) 0.6175(11) 0.036(2) Uani 1 1 d . . .
H18 H -0.3330 0.8536 0.5688 0.043 Uiso 1 1 calc R . .
C19 C -0.3009(10) 0.5454(10) 0.5798(8) 0.0231(16) Uani 1 1 d . . .
C20 C -0.3060(14) 0.5779(15) 0.4615(10) 0.033(2) Uani 1 1 d . . .
H20 H -0.2322 0.6888 0.4543 0.040 Uiso 1 1 calc R . .
C21 C -0.4233(16) 0.4415(17) 0.3552(10) 0.046(3) Uani 1 1 d . . .
H21 H -0.4294 0.4599 0.2746 0.056 Uiso 1 1 calc R . .
C22 C -0.5298(15) 0.2809(15) 0.3661(11) 0.044(3) Uani 1 1 d . . .
H22 H -0.6099 0.1907 0.2929 0.053 Uiso 1 1 calc R . .
C23 C -0.5218(14) 0.2488(13) 0.4834(12) 0.044(3) Uani 1 1 d . . .
H23 H -0.5922 0.1365 0.4899 0.053 Uiso 1 1 calc R . .
C24 C -0.4091(13) 0.3838(12) 0.5907(10) 0.034(2) Uani 1 1 d . . .
H24 H -0.4064 0.3651 0.6709 0.041 Uiso 1 1 calc R . .
C25 C -0.4266(12) 0.6734(13) 0.8201(9) 0.0251(19) Uani 1 1 d . . .
H25A H -0.5175 0.5521 0.7928 0.038 Uiso 1 1 calc R . .
H25B H -0.4526 0.7327 0.7597 0.038 Uiso 1 1 calc R . .
H25C H -0.4230 0.7267 0.9023 0.038 Uiso 1 1 calc R . .
C26 C 0.1668(16) 0.5775(17) 0.4860(12) 0.039(3) Uani 1 1 d . . .
C27 C 0.4499(18) 0.8000(18) 1.1840(14) 0.046(3) Uiso 1 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'
F F 0.0171 0.0103 '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'
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
O1 Pd1 O4 79.7(3) . . ?
O1 Pd1 P2 104.3(2) . . ?
O4 Pd1 P2 176.1(3) . . ?
O1 Pd1 P1 175.0(2) . . ?
O4 Pd1 P1 104.7(2) . . ?
P2 Pd1 P1 71.39(10) . . ?
O6 S1 O5 117.2(5) . . ?
O6 S1 O4 112.8(5) . . ?
O5 S1 O4 114.6(4) . . ?
O6 S1 C27 103.6(6) . . ?
O5 S1 C27 105.1(6) . . ?
O4 S1 C27 101.1(6) . . ?
O2 S2 O3 117.6(5) . . ?
O2 S2 O1 114.7(5) . . ?
O3 S2 O1 110.3(5) . . ?
O2 S2 C26 105.9(5) . . ?
O3 S2 C26 103.8(6) . . ?
O1 S2 C26 102.7(5) . . ?
N1 P1 C7 107.2(4) . . ?
N1 P1 C1 106.0(4) . . ?
C7 P1 C1 110.7(4) . . ?
N1 P1 Pd1 93.5(3) . . ?
C7 P1 Pd1 115.7(3) . . ?
C1 P1 Pd1 120.8(3) . . ?
N1 P1 P2 39.3(3) . . ?
C7 P1 P2 120.9(3) . . ?
C1 P1 P2 123.4(3) . . ?
Pd1 P1 P2 54.21(8) . . ?
N1 P2 C13 107.6(4) . . ?
N1 P2 C19 107.7(4) . . ?
C13 P2 C19 110.7(4) . . ?
N1 P2 Pd1 93.5(3) . . ?
C13 P2 Pd1 117.3(3) . . ?
C19 P2 Pd1 117.7(3) . . ?
N1 P2 P1 39.1(3) . . ?
C13 P2 P1 122.5(3) . . ?
C19 P2 P1 122.7(3) . . ?
Pd1 P2 P1 54.41(8) . . ?
S2 O1 Pd1 130.1(5) . . ?
S1 O4 Pd1 130.3(5) . . ?
C25 N1 P1 129.1(6) . . ?
C25 N1 P2 129.0(6) . . ?
P1 N1 P2 101.6(4) . . ?
C6 C1 C2 120.1(9) . . ?
C6 C1 P1 122.3(7) . . ?
C2 C1 P1 117.6(7) . . ?
C3 C2 C1 119.5(9) . . ?
C2 C3 C4 119.9(10) . . ?
C5 C4 C3 121.2(10) . . ?
C4 C5 C6 120.0(10) . . ?
C1 C6 C5 119.2(10) . . ?
C12 C7 C8 120.6(7) . . ?
C12 C7 P1 118.9(7) . . ?
C8 C7 P1 120.0(7) . . ?
C9 C8 C7 119.5(9) . . ?
C8 C9 C10 119.0(9) . . ?
C11 C10 C9 121.5(9) . . ?
C10 C11 C12 120.0(10) . . ?
C7 C12 C11 119.4(9) . . ?
C18 C13 C14 118.9(9) . . ?
C18 C13 P2 122.3(7) . . ?
C14 C13 P2 118.6(7) . . ?
C15 C14 C13 119.9(11) . . ?
C16 C15 C14 120.6(12) . . ?
C15 C16 C17 120.1(10) . . ?
C16 C17 C18 121.0(12) . . ?
C17 C18 C13 119.3(12) . . ?
C24 C19 C20 121.2(8) . . ?
C24 C19 P2 118.0(7) . . ?
C20 C19 P2 120.8(7) . . ?
C21 C20 C19 117.9(10) . . ?
C22 C21 C20 120.9(11) . . ?
C21 C22 C23 121.0(9) . . ?
C24 C23 C22 119.2(10) . . ?
C19 C24 C23 119.9(10) . . ?
F2 C26 F3 109.3(12) . . ?
F2 C26 F1 108.0(11) . . ?
F3 C26 F1 106.7(11) . . ?
F2 C26 S2 110.7(10) . . ?
F3 C26 S2 111.9(8) . . ?
F1 C26 S2 110.0(10) . . ?
F5 C27 F6 109.7(12) . . ?
F5 C27 F4 110.3(14) . . ?
F6 C27 F4 107.1(12) . . ?
F5 C27 S1 111.4(10) . . ?
F6 C27 S1 109.2(10) . . ?
F4 C27 S1 109.1(10) . . ?
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 O1 2.134(8) . ?
Pd1 O4 2.146(7) . ?
Pd1 P2 2.222(2) . ?
Pd1 P1 2.228(3) . ?
S1 O6 1.416(8) . ?
S1 O5 1.426(8) . ?
S1 O4 1.460(8) . ?
S1 C27 1.825(14) . ?
S2 O2 1.408(8) . ?
S2 O3 1.443(7) . ?
S2 O1 1.492(8) . ?
S2 C26 1.818(14) . ?
P1 N1 1.671(7) . ?
P1 C7 1.790(8) . ?
P1 C1 1.805(9) . ?
P1 P2 2.596(4) . ?
P2 N1 1.678(8) . ?
P2 C13 1.780(8) . ?
P2 C19 1.794(9) . ?
F1 C26 1.349(15) . ?
F2 C26 1.301(16) . ?
F3 C26 1.327(15) . ?
F4 C27 1.336(18) . ?
F5 C27 1.296(17) . ?
F6 C27 1.324(17) . ?
N1 C25 1.461(11) . ?
C1 C6 1.386(14) . ?
C1 C2 1.419(13) . ?
C2 C3 1.371(14) . ?
C3 C4 1.383(16) . ?
C4 C5 1.373(16) . ?
C5 C6 1.396(14) . ?
C7 C12 1.392(13) . ?
C7 C8 1.402(13) . ?
C8 C9 1.392(13) . ?
C9 C10 1.399(17) . ?
C10 C11 1.369(18) . ?
C11 C12 1.393(14) . ?
C13 C18 1.398(13) . ?
C13 C14 1.419(13) . ?
C14 C15 1.379(16) . ?
C15 C16 1.37(2) . ?
C16 C17 1.38(2) . ?
C17 C18 1.393(15) . ?
C19 C24 1.388(13) . ?
C19 C20 1.415(14) . ?
C20 C21 1.401(15) . ?
C21 C22 1.377(19) . ?
C22 C23 1.400(18) . ?
C23 C24 1.396(14) . ?
