#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:05:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179714 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/16/7001603.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_7001603
loop_
_publ_author_name
'Cao, Lingyun'
'Jennings, Michael C.'
'Puddephatt, Richard J.'
_publ_section_title
;
 A dipalladium complex with a single hydroxo bridge and its
 methylpalladium precursor
;
_journal_issue                   26
_journal_name_full               'Dalton Transactions'
_journal_page_first              5171
_journal_page_last               5176
_journal_paper_doi               10.1039/b906038c
_journal_year                    2009
_chemical_formula_sum            'C14 H16 F3 N3 O3 Pd S'
_chemical_formula_weight         469.76
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.961(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9817(7)
_cell_length_b                   6.9983(4)
_cell_length_c                   14.1109(10)
_cell_measurement_reflns_used    2404
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.70
_cell_volume                     843.74(10)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8825
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  0.8832
_exptl_absorpt_correction_T_min  0.7012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.987
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.369
_refine_ls_extinction_coef       0.063(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0431
_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)+(0.0754P)²+0.6403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                1486
_reflns_number_total             1609
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b906038c.txt
_cod_data_source_block           1b
_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      P2(1)/m
_cod_database_code               7001603
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_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
Pd Pd 0.94180(5) 0.7500 0.72024(3) 0.0310(3) Uani 1 2 d S . .
N11 N 1.0153(6) 0.7500 0.5988(4) 0.0273(11) Uani 1 2 d S A .
C12 C 0.9305(8) 0.7500 0.5007(5) 0.0379(16) Uani 1 2 d S . .
H12A H 0.8196 0.7500 0.4834 0.045 Uiso 1 2 calc SR A .
C13 C 0.9962(9) 0.7500 0.4260(5) 0.0391(16) Uani 1 2 d S . .
H13A H 0.9325 0.7500 0.3584 0.047 Uiso 1 2 calc SR . .
C14 C 1.1578(8) 0.7500 0.4502(5) 0.0366(16) Uani 1 2 d S . .
H14A H 1.2066 0.7500 0.3993 0.044 Uiso 1 2 calc SR A .
C15 C 1.2463(7) 0.7500 0.5489(5) 0.0325(15) Uani 1 2 d S A .
H15A H 1.3573 0.7500 0.5668 0.039 Uiso 1 2 calc SR . .
C16 C 1.1734(7) 0.7500 0.6222(5) 0.0270(13) Uani 1 2 d S . .
C17 C 1.2643(8) 0.780(2) 0.7320(5) 0.018(3) Uani 0.50 1 d P A -1
H17A H 1.3714 0.7276 0.7465 0.026 Uiso 0.50 1 calc PR A -1
H17B H 1.2724 0.9180 0.7478 0.026 Uiso 0.50 1 calc PR A -1
N18 N 1.1787(8) 0.6784(11) 0.7946(5) 0.0281(16) Uani 0.50 1 d P A -1
H18A H 1.1955 0.5471 0.7969 0.042 Uiso 0.50 1 calc PR A -1
C19 C 1.2126(8) 0.764(9) 0.8963(5) 0.028(5) Uani 0.50 1 d P A -1
H19A H 1.2430 0.8992 0.8947 0.043 Uiso 0.50 1 calc PR A -1
H19B H 1.3011 0.6949 0.9435 0.043 Uiso 0.50 1 calc PR A -1
C20 C 1.0693(7) 0.7500 0.9316(5) 0.0316(14) Uani 1 2 d S . .
C21 C 1.0824(8) 0.7500 1.0305(5) 0.0376(15) Uani 1 2 d S A .
H21A H 1.1832 0.7500 1.0787 0.045 Uiso 1 2 calc SR . .
C22 C 0.9503(8) 0.7500 1.0616(5) 0.0414(17) Uani 1 2 d S . .
H22A H 0.9590 0.7500 1.1304 0.050 Uiso 1 2 calc SR A .
C23 C 0.8055(9) 0.7500 0.9895(6) 0.0447(18) Uani 1 2 d S A .
H23A H 0.7125 0.7500 1.0082 0.054 Uiso 1 2 calc SR . .
C24 C 0.7973(8) 0.7500 0.8904(6) 0.0428(17) Uani 1 2 d S . .
H24A H 0.6972 0.7500 0.8414 0.051 Uiso 1 2 calc SR A .
N25 N 0.9264(6) 0.7500 0.8601(4) 0.0343(13) Uani 1 2 d S A .
C26 C 0.7110(8) 0.7500 0.6458(6) 0.0480(19) Uani 1 2 d S A .
H26A H 0.6715 0.8815 0.6392 0.072 Uiso 0.50 1 calc PR . .
H26B H 0.6555 0.6739 0.6826 0.072 Uiso 0.50 1 calc PR . .
H26C H 0.6935 0.6946 0.5795 0.072 Uiso 0.50 1 calc PR . .
O31 O 1.2811(5) 0.2500 0.7906(3) 0.0376(11) Uani 1 2 d S . .
O32 O 1.5185(4) 0.4240(5) 0.8748(3) 0.0445(9) Uani 1 1 d . . .
S33 S 1.45104(18) 0.2500 0.82721(12) 0.0311(4) Uani 1 2 d S . .
C34 C 1.5045(8) 0.2500 0.7126(5) 0.0350(15) Uani 1 2 d S . .
F35 F 1.4459(4) 0.4018(5) 0.6561(2) 0.0528(9) Uani 1 1 d . . .
F36 F 1.6582(5) 0.2500 0.7307(3) 0.0536(12) Uani 1 2 d S . .
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'
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
C26 Pd N11 96.4(3) . . ?
C26 Pd N25 98.0(3) . . ?
N11 Pd N25 165.6(2) . . ?
C26 Pd N18 166.3(2) . 4_575 ?
N11 Pd N18 83.1(2) . 4_575 ?
N25 Pd N18 82.9(2) . 4_575 ?
C26 Pd N18 166.3(2) . . ?
N11 Pd N18 83.1(2) . . ?
N25 Pd N18 82.9(2) . . ?
N18 Pd N18 27.3(4) 4_575 . ?
C16 N11 C12 117.6(6) . . ?
C16 N11 Pd 112.7(4) . . ?
C12 N11 Pd 129.7(5) . . ?
C13 C12 N11 123.4(6) . . ?
C13 C12 H12A 118.3 . . ?
N11 C12 H12A 118.3 . . ?
C12 C13 C14 118.9(6) . . ?
C12 C13 H13A 120.6 . . ?
C14 C13 H13A 120.6 . . ?
C15 C14 C13 119.0(6) . . ?
C15 C14 H14A 120.5 . . ?
C13 C14 H14A 120.5 . . ?
C14 C15 C16 119.8(6) . . ?
C14 C15 H15A 120.1 . . ?
C16 C15 H15A 120.1 . . ?
N11 C16 C15 121.4(6) . . ?
N11 C16 C17 116.0(6) . . ?
C15 C16 C17 122.0(6) . . ?
N11 C16 C17 116.0(6) . 4_575 ?
C15 C16 C17 122.0(6) . 4_575 ?
C17 C16 C17 15.7(11) . 4_575 ?
N18 C17 C16 108.6(7) . . ?
N18 C17 H17A 110.0 . . ?
C16 C17 H17A 110.0 . . ?
N18 C17 H17B 110.0 . . ?
C16 C17 H17B 110.0 . . ?
H17A C17 H17B 108.3 . . ?
C19 N18 C17 112.5(17) . . ?
C19 N18 Pd 104.9(9) . . ?
C17 N18 Pd 102.3(5) . . ?
C19 N18 H18A 112.2 . . ?
C17 N18 H18A 112.2 . . ?
Pd N18 H18A 112.2 . . ?
N18 C19 C20 110.3(17) . . ?
N18 C19 H19A 109.6 . . ?
C20 C19 H19A 109.6 . . ?
N18 C19 H19B 109.6 . . ?
C20 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C21 C20 N25 121.4(6) . . ?
C21 C20 C19 121.4(6) . 4_575 ?
N25 C20 C19 117.1(6) . 4_575 ?
C21 C20 C19 121.4(6) . . ?
N25 C20 C19 117.1(6) . . ?
C19 C20 C19 7(5) 4_575 . ?
C20 C21 C22 120.8(6) . . ?
C20 C21 H21A 119.6 . . ?
C22 C21 H21A 119.6 . . ?
C23 C22 C21 118.1(6) . . ?
C23 C22 H22A 121.0 . . ?
C21 C22 H22A 121.0 . . ?
C24 C23 C22 119.4(7) . . ?
C24 C23 H23A 120.3 . . ?
C22 C23 H23A 120.3 . . ?
N25 C24 C23 122.5(6) . . ?
N25 C24 H24A 118.7 . . ?
C23 C24 H24A 118.7 . . ?
C24 N25 C20 117.9(6) . . ?
C24 N25 Pd 129.2(5) . . ?
C20 N25 Pd 113.0(4) . . ?
Pd C26 H26A 109.5 . . ?
Pd C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Pd C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O32 S33 O32 116.5(3) . 4_565 ?
O32 S33 O31 114.38(16) . . ?
O32 S33 O31 114.38(16) 4_565 . ?
O32 S33 C34 103.11(19) . . ?
O32 S33 C34 103.11(19) 4_565 . ?
O31 S33 C34 102.7(3) . . ?
F36 C34 F35 108.1(4) . 4_565 ?
F36 C34 F35 108.1(4) . . ?
F35 C34 F35 105.4(5) 4_565 . ?
F36 C34 S33 111.9(5) . . ?
F35 C34 S33 111.5(4) 4_565 . ?
F35 C34 S33 111.5(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 C26 2.015(7) . ?
Pd N11 2.017(5) . ?
Pd N25 2.020(6) . ?
Pd N18 2.122(7) 4_575 ?
Pd N18 2.122(7) . ?
N11 C16 1.355(8) . ?
N11 C12 1.360(9) . ?
C12 C13 1.356(10) . ?
C12 H12A 0.9500 . ?
C13 C14 1.384(10) . ?
C13 H13A 0.9500 . ?
C14 C15 1.374(10) . ?
C14 H14A 0.9500 . ?
C15 C16 1.384(9) . ?
C15 H15A 0.9500 . ?
C16 C17 1.527(9) . ?
C16 C17 1.527(9) 4_575 ?
C17 N18 1.515(12) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
N18 C19 1.50(3) . ?
N18 H18A 0.9300 . ?
C19 C20 1.519(10) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.364(9) . ?
C20 N25 1.366(8) . ?
C20 C19 1.519(10) 4_575 ?
C21 C22 1.386(9) . ?
C21 H21A 0.9500 . ?
C22 C23 1.382(10) . ?
C22 H22A 0.9500 . ?
C23 C24 1.378(11) . ?
C23 H23A 0.9500 . ?
C24 N25 1.354(8) . ?
C24 H24A 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O31 S33 1.453(5) . ?
O32 S33 1.432(4) . ?
S33 O32 1.432(4) 4_565 ?
S33 C34 1.824(7) . ?
C34 F36 1.324(8) . ?
C34 F35 1.335(5) 4_565 ?
C34 F35 1.335(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N18 H18A O31 0.93 2.23 3.141(8) 167.1 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C26 Pd N11 C16 180.000(2) . . . . ?
N25 Pd N11 C16 0.000(4) . . . . ?
N18 Pd N11 C16 13.8(2) 4_575 . . . ?
N18 Pd N11 C16 -13.8(2) . . . . ?
C26 Pd N11 C12 0.000(2) . . . . ?
N25 Pd N11 C12 180.000(3) . . . . ?
N18 Pd N11 C12 -166.2(2) 4_575 . . . ?
N18 Pd N11 C12 166.2(2) . . . . ?
C16 N11 C12 C13 0.000(3) . . . . ?
Pd N11 C12 C13 180.000(2) . . . . ?
N11 C12 C13 C14 0.000(3) . . . . ?
C12 C13 C14 C15 0.000(3) . . . . ?
C13 C14 C15 C16 0.000(2) . . . . ?
C12 N11 C16 C15 0.000(3) . . . . ?
Pd N11 C16 C15 180.000(2) . . . . ?
C12 N11 C16 C17 171.3(6) . . . . ?
Pd N11 C16 C17 -8.7(6) . . . . ?
C12 N11 C16 C17 -171.3(6) . . . 4_575 ?
Pd N11 C16 C17 8.7(6) . . . 4_575 ?
C14 C15 C16 N11 0.000(3) . . . . ?
C14 C15 C16 C17 -170.7(7) . . . . ?
C14 C15 C16 C17 170.7(7) . . . 4_575 ?
N11 C16 C17 N18 36.9(10) . . . . ?
C15 C16 C17 N18 -151.9(5) . . . . ?
C17 C16 C17 N18 -56.9(8) 4_575 . . . ?
C16 C17 N18 C19 -154.9(17) . . . . ?
C16 C17 N18 Pd -42.9(9) . . . . ?
C26 Pd N18 C19 -123(2) . . . . ?
N11 Pd N18 C19 149(2) . . . . ?
N25 Pd N18 C19 -28(2) . . . . ?
N18 Pd N18 C19 61(2) 4_575 . . . ?
C26 Pd N18 C17 119.8(12) . . . . ?
N11 Pd N18 C17 31.4(6) . . . . ?
N25 Pd N18 C17 -145.2(6) . . . . ?
N18 Pd N18 C17 -56.9(6) 4_575 . . . ?
C17 N18 C19 C20 146(2) . . . . ?
Pd N18 C19 C20 36(3) . . . . ?
N18 C19 C20 C21 155.5(16) . . . . ?
N18 C19 C20 N25 -29(4) . . . . ?
N18 C19 C20 C19 63(3) . . . 4_575 ?
N25 C20 C21 C22 0.000(5) . . . . ?
C19 C20 C21 C22 -176(3) 4_575 . . . ?
C19 C20 C21 C22 176(3) . . . . ?
C20 C21 C22 C23 0.000(5) . . . . ?
C21 C22 C23 C24 0.000(6) . . . . ?
C22 C23 C24 N25 0.000(5) . . . . ?
C23 C24 N25 C20 0.000(5) . . . . ?
C23 C24 N25 Pd 180.000(4) . . . . ?
C21 C20 N25 C24 0.000(5) . . . . ?
C19 C20 N25 C24 176(3) 4_575 . . . ?
C19 C20 N25 C24 -176(3) . . . . ?
C21 C20 N25 Pd 180.000(3) . . . . ?
C19 C20 N25 Pd -4(3) 4_575 . . . ?
C19 C20 N25 Pd 4(3) . . . . ?
C26 Pd N25 C24 0.000(3) . . . . ?
N11 Pd N25 C24 180.000(5) . . . . ?
N18 Pd N25 C24 166.2(2) 4_575 . . . ?
N18 Pd N25 C24 -166.2(2) . . . . ?
C26 Pd N25 C20 180.000(3) . . . . ?
N11 Pd N25 C20 0.000(6) . . . . ?
N18 Pd N25 C20 -13.8(2) 4_575 . . . ?
N18 Pd N25 C20 13.8(2) . . . . ?
O32 S33 C34 F36 60.85(16) . . . . ?
O32 S33 C34 F36 -60.85(16) 4_565 . . . ?
O31 S33 C34 F36 180.000(2) . . . . ?
O32 S33 C34 F35 -177.9(4) . . . 4_565 ?
O32 S33 C34 F35 60.4(4) 4_565 . . 4_565 ?
O31 S33 C34 F35 -58.8(4) . . . 4_565 ?
O32 S33 C34 F35 -60.4(4) . . . . ?
O32 S33 C34 F35 177.9(4) 4_565 . . . ?
O31 S33 C34 F35 58.8(4) . . . . ?
