#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:21:07 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179891 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/87/7018741.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_7018741
loop_
_publ_author_name
'Safin, Damir A.'
'Babashkina, Maria G.'
'Robeyns, Koen'
'Garcia, Yann'
_publ_section_title
;
 Halogen anion-induced formation of [(PdLX)(2)] (X = Cl(-), Br(-), I(-))
 vs. [PdL(2)] (L = [6-MeO(O)CC(6)H(4)NHC(S)NP(S)(OiPr)(2)](-)): Reversible
 photoinduced cis/trans isomerization of [PdL(2)].
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4324
_journal_page_last               4327
_journal_paper_doi               10.1039/c2dt12466a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C30 H44 N4 O8 P2 Pd S4, C4 H8 O2'
_chemical_formula_sum            'C34 H52 N4 O10 P2 Pd S4'
_chemical_formula_weight         973.38
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.262(10)
_cell_angle_beta                 104.326(7)
_cell_angle_gamma                92.377(7)
_cell_formula_units_Z            1
_cell_length_a                   9.3910(5)
_cell_length_b                   9.6617(10)
_cell_length_c                   13.2526(14)
_cell_measurement_reflns_used    5895
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.2426
_cell_measurement_theta_min      2.2656
_cell_volume                     1074.23(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.45 (release 19-11-2010 CrysAlis171 .NET)
(compiled Nov 19 2010,18:13:43)
;
_computing_data_collection       MAR
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.45 (release 19-11-2010 CrysAlis171 .NET)
(compiled Nov 19 2010,18:13:43)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '110 images, ΔΦ 2.0°'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_radiation_source         'Rigaku Ultra 18 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0420
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8795
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.45 (release 19-11-2010 CrysAlis171 .NET)
(compiled Nov 19 2010,18:13:43)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0304
_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)+(0.0413P)²+0.9112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                3371
_reflns_number_total             3669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12466a.txt
_cod_data_source_block           safin95
_cod_original_cell_volume        1074.23(17)
_cod_database_code               7018741
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 1.0000 0.0000 1.0000 0.02397(10) Uani 1 2 d S
S2 S 0.81285(8) 0.09494(8) 1.08012(6) 0.02933(16) Uani 1 1 d .
P3 P 0.76547(7) 0.25525(7) 1.01991(6) 0.02522(16) Uani 1 1 d .
N4 N 0.7083(3) 0.2068(3) 0.88575(19) 0.0296(5) Uani 1 1 d .
C5 C 0.7589(3) 0.1105(3) 0.8090(2) 0.0271(6) Uani 1 1 d .
S6 S 0.89313(8) -0.00675(9) 0.82147(6) 0.03655(19) Uani 1 1 d .
O7 O 0.6408(2) 0.3327(2) 1.07087(15) 0.0273(4) Uani 1 1 d .
C8 C 0.4954(3) 0.2452(3) 1.0485(2) 0.0313(6) Uani 1 1 d .
H8 H 0.4892 0.1421 0.9909 0.038 Uiso 1 1 calc R
C9 C 0.3788(3) 0.3249(4) 1.0007(3) 0.0420(7) Uani 1 1 d .
H9A H 0.3891 0.4284 1.0547 0.063 Uiso 1 1 calc R
H9B H 0.2799 0.2726 0.9869 0.063 Uiso 1 1 calc R
H9C H 0.3914 0.3253 0.9296 0.063 Uiso 1 1 calc R
C10 C 0.4835(4) 0.2341(4) 1.1566(3) 0.0402(7) Uani 1 1 d .
H10A H 0.5655 0.1861 1.1847 0.060 Uiso 1 1 calc R
H10B H 0.3887 0.1740 1.1424 0.060 Uiso 1 1 calc R
H10C H 0.4885 0.3349 1.2129 0.060 Uiso 1 1 calc R
O11 O 0.8963(2) 0.3861(2) 1.06186(16) 0.0312(4) Uani 1 1 d .
C12 C 0.9766(3) 0.4673(3) 1.1824(2) 0.0330(6) Uani 1 1 d .
H12 H 0.9378 0.4220 1.2290 0.040 Uiso 1 1 calc R
C13 C 0.9488(4) 0.6271(4) 1.2136(3) 0.0516(9) Uani 1 1 d .
H13A H 0.9777 0.6676 1.1625 0.077 Uiso 1 1 calc R
H13B H 1.0075 0.6867 1.2914 0.077 Uiso 1 1 calc R
H13C H 0.8430 0.6313 1.2074 0.077 Uiso 1 1 calc R
C14 C 1.1376(4) 0.4506(4) 1.1947(3) 0.0517(9) Uani 1 1 d .
H14A H 1.1481 0.3438 1.1689 0.077 Uiso 1 1 calc R
H14B H 1.1945 0.5017 1.2741 0.077 Uiso 1 1 calc R
H14C H 1.1751 0.4954 1.1490 0.077 Uiso 1 1 calc R
N15 N 0.7080(3) 0.0932(3) 0.69859(19) 0.0305(5) Uani 1 1 d .
H15 H 0.7375 0.0176 0.6512 0.037 Uiso 1 1 calc R
C16 C 0.6171(3) 0.1748(3) 0.6477(2) 0.0274(6) Uani 1 1 d .
C17 C 0.5231(3) 0.2663(3) 0.6986(2) 0.0317(6) Uani 1 1 d .
H17 H 0.5200 0.2763 0.7720 0.038 Uiso 1 1 calc R
C18 C 0.4341(3) 0.3428(3) 0.6435(3) 0.0363(7) Uani 1 1 d .
H18 H 0.3701 0.4042 0.6791 0.044 Uiso 1 1 calc R
C19 C 0.4381(3) 0.3301(4) 0.5363(3) 0.0395(7) Uani 1 1 d .
H19 H 0.3784 0.3844 0.4994 0.047 Uiso 1 1 calc R
C20 C 0.5286(3) 0.2387(3) 0.4838(3) 0.0355(6) Uani 1 1 d .
H20 H 0.5291 0.2286 0.4098 0.043 Uiso 1 1 calc R
C21 C 0.6201(3) 0.1606(3) 0.5378(2) 0.0292(6) Uani 1 1 d .
C22 C 0.7173(3) 0.0630(3) 0.4784(2) 0.0315(6) Uani 1 1 d .
O23 O 0.8037(2) -0.0070(3) 0.51749(18) 0.0424(5) Uani 1 1 d .
O24 O 0.7015(3) 0.0602(2) 0.37473(18) 0.0420(5) Uani 1 1 d .
C25 C 0.7931(4) -0.0334(4) 0.3137(3) 0.0500(9) Uani 1 1 d .
H25A H 0.8980 0.0077 0.3521 0.075 Uiso 1 1 calc R
H25B H 0.7687 -0.0358 0.2367 0.075 Uiso 1 1 calc R
H25C H 0.7746 -0.1354 0.3110 0.075 Uiso 1 1 calc R
O31 O 0.8813(3) 0.5259(3) 0.4234(2) 0.0529(6) Uani 1 1 d .
C32 C 0.8824(4) 0.3867(4) 0.4356(3) 0.0568(9) Uani 1 1 d .
H32A H 0.8280 0.3056 0.3628 0.068 Uiso 1 1 calc R
H32B H 0.8304 0.3875 0.4922 0.068 Uiso 1 1 calc R
C33 C 1.0359(4) 0.3558(4) 0.4715(3) 0.0575(10) Uani 1 1 d .
H33A H 1.0330 0.2588 0.4809 0.069 Uiso 1 1 calc R
H33B H 1.0860 0.3481 0.4125 0.069 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'
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'
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
S6 Pd1 S6 179.999(1) 2_757 .
S6 Pd1 S2 97.80(3) 2_757 2_757
S6 Pd1 S2 82.20(3) . 2_757
S6 Pd1 S2 82.20(3) 2_757 .
S6 Pd1 S2 97.80(3) . .
S2 Pd1 S2 180.00(4) 2_757 .
P3 S2 Pd1 101.44(3) . .
O11 P3 O7 104.06(10) . .
O11 P3 N4 105.36(11) . .
O7 P3 N4 107.44(11) . .
O11 P3 S2 113.96(8) . .
O7 P3 S2 106.76(8) . .
N4 P3 S2 118.24(9) . .
C5 N4 P3 127.5(2) . .
N4 C5 N15 120.1(2) . .
N4 C5 S6 130.7(2) . .
N15 C5 S6 109.17(19) . .
C5 S6 Pd1 116.79(9) . .
C8 O7 P3 120.89(16) . .
O7 C8 C10 108.6(2) . .
O7 C8 C9 106.5(2) . .
C10 C8 C9 114.0(2) . .
O7 C8 H8 109.2 . .
C10 C8 H8 109.2 . .
C9 C8 H8 109.2 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 O11 P3 122.70(17) . .
O11 C12 C13 107.0(2) . .
O11 C12 C14 107.0(2) . .
C13 C12 C14 113.2(3) . .
O11 C12 H12 109.8 . .
C13 C12 H12 109.8 . .
C14 C12 H12 109.8 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C5 N15 C16 131.2(2) . .
C5 N15 H15 114.4 . .
C16 N15 H15 114.4 . .
C17 C16 N15 123.3(2) . .
C17 C16 C21 119.0(2) . .
N15 C16 C21 117.7(2) . .
C18 C17 C16 120.8(3) . .
C18 C17 H17 119.6 . .
C16 C17 H17 119.6 . .
C17 C18 C19 120.3(3) . .
C17 C18 H18 119.8 . .
C19 C18 H18 119.8 . .
C20 C19 C18 119.9(3) . .
C20 C19 H19 120.1 . .
C18 C19 H19 120.1 . .
C19 C20 C21 121.0(3) . .
C19 C20 H20 119.5 . .
C21 C20 H20 119.5 . .
C20 C21 C16 119.1(3) . .
C20 C21 C22 119.5(3) . .
C16 C21 C22 121.4(2) . .
O23 C22 O24 121.8(3) . .
O23 C22 C21 125.4(3) . .
O24 C22 C21 112.8(2) . .
C22 O24 C25 114.8(2) . .
O24 C25 H25A 109.5 . .
O24 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
O24 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C32 O31 C33 109.6(3) . 2_766
O31 C32 C33 111.5(3) . .
O31 C32 H32A 109.3 . .
C33 C32 H32A 109.3 . .
O31 C32 H32B 109.3 . .
C33 C32 H32B 109.3 . .
H32A C32 H32B 108.0 . .
O31 C33 C32 110.5(3) 2_766 .
O31 C33 H33A 109.6 2_766 .
C32 C33 H33A 109.6 . .
O31 C33 H33B 109.6 2_766 .
C32 C33 H33B 109.6 . .
H33A C33 H33B 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 S6 2.3058(7) 2_757
Pd1 S6 2.3059(7) .
Pd1 S2 2.3256(7) 2_757
Pd1 S2 2.3256(7) .
S2 P3 2.0029(9) .
P3 O11 1.562(2) .
P3 O7 1.5759(18) .
P3 N4 1.604(2) .
N4 C5 1.310(3) .
C5 N15 1.366(3) .
C5 S6 1.747(3) .
O7 C8 1.480(3) .
C8 C10 1.506(4) .
C8 C9 1.507(4) .
C8 H8 1.0000 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
O11 C12 1.477(3) .
C12 C13 1.499(4) .
C12 C14 1.501(4) .
C12 H12 1.0000 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
N15 C16 1.401(3) .
N15 H15 0.8800 .
C16 C17 1.394(4) .
C16 C21 1.420(4) .
C17 C18 1.385(4) .
C17 H17 0.9500 .
C18 C19 1.391(4) .
C18 H18 0.9500 .
C19 C20 1.377(4) .
C19 H19 0.9500 .
C20 C21 1.401(4) .
C20 H20 0.9500 .
C21 C22 1.494(4) .
C22 O23 1.216(3) .
C22 O24 1.334(3) .
O24 C25 1.445(4) .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
O31 C32 1.412(4) .
O31 C33 1.445(4) 2_766
C32 C33 1.481(5) .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C33 O31 1.445(4) 2_766
C33 H33A 0.9900 .
C33 H33B 0.9900 .
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_4
S6 Pd1 S2 P3 136.86(4) 2_757 .
S6 Pd1 S2 P3 -43.14(4) . .
Pd1 S2 P3 O11 -64.35(9) . .
Pd1 S2 P3 O7 -178.64(8) . .
Pd1 S2 P3 N4 60.23(11) . .
O11 P3 N4 C5 86.6(3) . .
O7 P3 N4 C5 -162.9(2) . .
S2 P3 N4 C5 -42.1(3) . .
P3 N4 C5 N15 -173.2(2) . .
P3 N4 C5 S6 4.9(4) . .
N4 C5 S6 Pd1 1.4(3) . .
N15 C5 S6 Pd1 179.73(15) . .
S2 Pd1 S6 C5 -158.20(11) 2_757 .
S2 Pd1 S6 C5 21.80(11) . .
O11 P3 O7 C8 178.98(18) . .
N4 P3 O7 C8 67.6(2) . .
S2 P3 O7 C8 -60.18(19) . .
P3 O7 C8 C10 111.2(2) . .
P3 O7 C8 C9 -125.6(2) . .
O7 P3 O11 C12 64.7(2) . .
N4 P3 O11 C12 177.56(19) . .
S2 P3 O11 C12 -51.2(2) . .
P3 O11 C12 C13 -116.3(2) . .
P3 O11 C12 C14 122.1(2) . .
N4 C5 N15 C16 8.5(4) . .
S6 C5 N15 C16 -170.0(2) . .
C5 N15 C16 C17 -20.3(5) . .
C5 N15 C16 C21 160.8(3) . .
N15 C16 C17 C18 -179.1(3) . .
C21 C16 C17 C18 -0.2(4) . .
C16 C17 C18 C19 -0.4(4) . .
C17 C18 C19 C20 1.3(5) . .
C18 C19 C20 C21 -1.5(5) . .
C19 C20 C21 C16 0.9(4) . .
C19 C20 C21 C22 -179.8(3) . .
C17 C16 C21 C20 0.0(4) . .
N15 C16 C21 C20 178.9(2) . .
C17 C16 C21 C22 -179.3(3) . .
N15 C16 C21 C22 -0.4(4) . .
C20 C21 C22 O23 178.1(3) . .
C16 C21 C22 O23 -2.6(5) . .
C20 C21 C22 O24 -1.4(4) . .
C16 C21 C22 O24 178.0(2) . .
O23 C22 O24 C25 0.7(4) . .
C21 C22 O24 C25 -179.8(3) . .
C33 O31 C32 C33 -57.4(5) 2_766 .
O31 C32 C33 O31 58.0(5) . 2_766
