#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:21:07 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179891 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/87/7018740.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_7018740
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 H46 Cl2 N4 O9 P2 Pd2 S4'
_chemical_formula_sum            'C30 H46 Cl2 N4 O9 P2 Pd2 S4'
_chemical_formula_weight         1080.59
_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                106.140(9)
_cell_angle_beta                 99.678(7)
_cell_angle_gamma                108.160(10)
_cell_formula_units_Z            1
_cell_length_a                   8.6119(9)
_cell_length_b                   11.1471(14)
_cell_length_c                   13.3906(9)
_cell_measurement_reflns_used    3261
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7052
_cell_measurement_theta_min      2.0506
_cell_volume                     1126.7(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection       MAR
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '120 images, ΔΦ 2.0°'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6570
_diffrn_reflns_theta_full        21.75
_diffrn_reflns_theta_max         21.75
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The unit cell contains 1 H2O molecule which has been
treated as a diffuse contribution to the overall
scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.141
_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     240
_refine_ls_number_reflns         2535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0654
_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)+(0.1124P)²+3.7458P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1819
_reflns_number_gt                1990
_reflns_number_total             2535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12466a.txt
_cod_data_source_block           safin87
_cod_database_code               7018740
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 0.48603(9) -0.05073(8) 0.11121(6) 0.0433(4) Uani 1 1 d .
Cl2 Cl 0.5375(3) -0.2257(2) 0.1601(2) 0.0490(7) Uani 1 1 d .
S3 S 0.4515(4) 0.0304(3) 0.2826(2) 0.0586(8) Uani 1 1 d .
P4 P 0.4280(3) 0.2061(3) 0.2919(2) 0.0479(8) Uani 1 1 d .
O5 O 0.2472(9) 0.1952(7) 0.2362(6) 0.0545(19) Uani 1 1 d .
C6 C 0.0899(14) 0.1082(12) 0.2511(10) 0.065(3) Uani 1 1 d .
H6 H 0.1199 0.0707 0.3062 0.078 Uiso 1 1 calc R
C7 C -0.005(2) 0.1970(17) 0.290(2) 0.151(10) Uani 1 1 d .
H7A H 0.0646 0.2682 0.3566 0.227 Uiso 1 1 calc R
H7B H -0.1083 0.1441 0.3004 0.227 Uiso 1 1 calc R
H7C H -0.0325 0.2351 0.2362 0.227 Uiso 1 1 calc R
C8 C -0.0094(19) -0.0043(17) 0.1453(14) 0.120(7) Uani 1 1 d .
H8A H -0.0327 0.0327 0.0904 0.181 Uiso 1 1 calc R
H8B H -0.1147 -0.0592 0.1524 0.181 Uiso 1 1 calc R
H8C H 0.0556 -0.0585 0.1253 0.181 Uiso 1 1 calc R
O9 O 0.4560(9) 0.2883(7) 0.4133(6) 0.056(2) Uani 1 1 d .
C10 C 0.5938(17) 0.3122(14) 0.5057(9) 0.070(4) Uani 1 1 d .
H10 H 0.6105 0.2283 0.5025 0.084 Uiso 1 1 calc R
C11 C 0.548(3) 0.364(3) 0.6007(15) 0.194(12) Uani 1 1 d .
H11A H 0.4846 0.4185 0.5887 0.292 Uiso 1 1 calc R
H11B H 0.6496 0.4190 0.6595 0.292 Uiso 1 1 calc R
H11C H 0.4803 0.2912 0.6184 0.292 Uiso 1 1 calc R
C12 C 0.754(3) 0.418(2) 0.5102(17) 0.172(11) Uani 1 1 d .
H12A H 0.7350 0.4984 0.5120 0.259 Uiso 1 1 calc R
H12B H 0.7905 0.3860 0.4474 0.259 Uiso 1 1 calc R
H12C H 0.8409 0.4365 0.5742 0.259 Uiso 1 1 calc R
N13 N 0.5592(11) 0.3014(8) 0.2455(7) 0.047(2) Uani 1 1 d .
C14 C 0.5767(12) 0.2659(10) 0.1487(9) 0.046(3) Uani 1 1 d .
N15 N 0.6946(11) 0.3416(8) 0.1167(7) 0.048(2) Uani 1 1 d .
H15 H 0.6982 0.3064 0.0517 0.058 Uiso 1 1 calc R
C16 C 0.8161(14) 0.4740(10) 0.1764(9) 0.049(3) Uani 1 1 d .
C17 C 0.7735(15) 0.5658(11) 0.2496(11) 0.067(4) Uani 1 1 d .
H17 H 0.6675 0.5385 0.2625 0.080 Uiso 1 1 calc R
C18 C 0.8888(17) 0.6984(12) 0.3036(12) 0.080(4) Uani 1 1 d .
H18 H 0.8598 0.7602 0.3516 0.096 Uiso 1 1 calc R
C19 C 1.0460(16) 0.7366(12) 0.2850(10) 0.067(3) Uani 1 1 d .
H19 H 1.1240 0.8248 0.3210 0.080 Uiso 1 1 calc R
C20 C 1.0891(15) 0.6461(11) 0.2138(10) 0.059(3) Uani 1 1 d .
H20 H 1.1948 0.6741 0.2006 0.071 Uiso 1 1 calc R
C21 C 0.9756(13) 0.5125(11) 0.1610(9) 0.048(3) Uani 1 1 d .
S21 S 0.4329(3) 0.1068(3) 0.0460(2) 0.0440(7) Uani 1 1 d .
C22 C 1.0290(15) 0.4140(12) 0.0862(9) 0.050(3) Uani 1 1 d .
O23 O 0.9345(10) 0.3046(9) 0.0228(7) 0.071(2) Uani 1 1 d .
O24 O 1.1945(9) 0.4627(8) 0.0975(7) 0.068(2) Uani 1 1 d .
C25 C 1.2609(16) 0.3755(13) 0.0334(11) 0.074(4) Uani 1 1 d .
H25A H 1.2336 0.2932 0.0485 0.111 Uiso 1 1 calc R
H25B H 1.3822 0.4195 0.0508 0.111 Uiso 1 1 calc R
H25C H 1.2112 0.3555 -0.0419 0.111 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'
Pd Pd -0.9988 1.0072 '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'
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
S21 Pd1 S21 81.72(10) . 2_655
S21 Pd1 S3 98.15(10) . .
S21 Pd1 S3 170.43(11) 2_655 .
S21 Pd1 Cl2 174.23(10) . .
S21 Pd1 Cl2 92.99(9) 2_655 .
S3 Pd1 Cl2 87.45(10) . .
P4 S3 Pd1 104.37(15) . .
O5 P4 O9 102.9(4) . .
O5 P4 N13 105.7(4) . .
O9 P4 N13 107.7(4) . .
O5 P4 S3 115.5(3) . .
O9 P4 S3 108.5(3) . .
N13 P4 S3 115.6(3) . .
C6 O5 P4 122.5(7) . .
O5 C6 C8 108.3(10) . .
O5 C6 C7 107.0(11) . .
C8 C6 C7 112.8(14) . .
O5 C6 H6 109.6 . .
C8 C6 H6 109.6 . .
C7 C6 H6 109.6 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C10 O9 P4 126.9(7) . .
C11 C10 O9 107.3(12) . .
C11 C10 C12 106.6(18) . .
O9 C10 C12 110.8(12) . .
C11 C10 H10 110.7 . .
O9 C10 H10 110.7 . .
C12 C10 H10 110.7 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C14 N13 P4 125.4(7) . .
N13 C14 N15 123.8(9) . .
N13 C14 S21 120.9(8) . .
N15 C14 S21 115.3(8) . .
C14 N15 C16 127.9(8) . .
C14 N15 H15 116.0 . .
C16 N15 H15 116.0 . .
C21 C16 C17 119.9(10) . .
C21 C16 N15 119.9(9) . .
C17 C16 N15 120.2(9) . .
C16 C17 C18 120.4(11) . .
C16 C17 H17 119.8 . .
C18 C17 H17 119.8 . .
C19 C18 C17 119.1(11) . .
C19 C18 H18 120.5 . .
C17 C18 H18 120.5 . .
C20 C19 C18 120.7(11) . .
C20 C19 H19 119.7 . .
C18 C19 H19 119.7 . .
C19 C20 C21 120.6(11) . .
C19 C20 H20 119.7 . .
C21 C20 H20 119.7 . .
C16 C21 C20 119.2(10) . .
C16 C21 C22 121.4(10) . .
C20 C21 C22 119.4(10) . .
C14 S21 Pd1 103.4(4) . .
C14 S21 Pd1 114.4(4) . 2_655
Pd1 S21 Pd1 98.28(10) . 2_655
O23 C22 O24 123.1(11) . .
O23 C22 C21 125.0(10) . .
O24 C22 C21 111.8(10) . .
C22 O24 C25 116.7(9) . .
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 S21 2.298(3) .
Pd1 S21 2.311(3) 2_655
Pd1 S3 2.328(3) .
Pd1 Cl2 2.363(3) .
S3 P4 2.004(4) .
P4 O5 1.561(8) .
P4 O9 1.563(7) .
P4 N13 1.626(9) .
O5 C6 1.481(12) .
C6 C8 1.499(18) .
C6 C7 1.510(19) .
C6 H6 0.9800 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
O9 C10 1.462(14) .
C10 C11 1.42(2) .
C10 C12 1.49(2) .
C10 H10 0.9800 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
N13 C14 1.295(13) .
C14 N15 1.319(13) .
C14 S21 1.809(10) .
N15 C16 1.419(13) .
N15 H15 0.8600 .
C16 C21 1.376(14) .
C16 C17 1.392(15) .
C17 C18 1.394(16) .
C17 H17 0.9300 .
C18 C19 1.374(17) .
C18 H18 0.9300 .
C19 C20 1.372(16) .
C19 H19 0.9300 .
C20 C21 1.396(15) .
C20 H20 0.9300 .
C21 C22 1.509(16) .
S21 Pd1 2.312(3) 2_655
C22 O23 1.201(13) .
C22 O24 1.322(13) .
O24 C25 1.433(13) .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
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
S21 Pd1 S3 P4 -7.87(17) . .
Cl2 Pd1 S3 P4 173.52(16) . .
Pd1 S3 P4 O5 81.1(3) . .
Pd1 S3 P4 O9 -164.1(3) . .
Pd1 S3 P4 N13 -43.0(4) . .
O9 P4 O5 C6 -71.7(8) . .
N13 P4 O5 C6 175.4(8) . .
S3 P4 O5 C6 46.3(8) . .
P4 O5 C6 C8 -112.6(11) . .
P4 O5 C6 C7 125.6(13) . .
O5 P4 O9 C10 170.5(9) . .
N13 P4 O9 C10 -78.1(10) . .
S3 P4 O9 C10 47.7(10) . .
P4 O9 C10 C11 -167.2(14) . .
P4 O9 C10 C12 76.8(16) . .
O5 P4 N13 C14 -72.9(10) . .
O9 P4 N13 C14 177.6(9) . .
S3 P4 N13 C14 56.2(10) . .
P4 N13 C14 N15 -173.8(8) . .
P4 N13 C14 S21 7.9(13) . .
N13 C14 N15 C16 -3.2(17) . .
S21 C14 N15 C16 175.2(8) . .
C14 N15 C16 C21 145.8(11) . .
C14 N15 C16 C17 -35.1(17) . .
C21 C16 C17 C18 3.0(19) . .
N15 C16 C17 C18 -176.1(12) . .
C16 C17 C18 C19 -1(2) . .
C17 C18 C19 C20 0(2) . .
C18 C19 C20 C21 -2(2) . .
C17 C16 C21 C20 -4.2(17) . .
N15 C16 C21 C20 174.9(10) . .
C17 C16 C21 C22 177.2(11) . .
N15 C16 C21 C22 -3.7(16) . .
C19 C20 C21 C16 3.6(17) . .
C19 C20 C21 C22 -177.8(11) . .
N13 C14 S21 Pd1 -65.1(9) . .
N15 C14 S21 Pd1 116.4(8) . .
N13 C14 S21 Pd1 -170.9(7) . 2_655
N15 C14 S21 Pd1 10.7(9) . 2_655
S21 Pd1 S21 C14 -117.7(4) 2_655 .
S3 Pd1 S21 C14 52.6(4) . .
S21 Pd1 S21 Pd1 0.000(1) 2_655 2_655
S3 Pd1 S21 Pd1 170.34(11) . 2_655
C16 C21 C22 O23 12.2(18) . .
C20 C21 C22 O23 -166.4(11) . .
C16 C21 C22 O24 -168.4(10) . .
C20 C21 C22 O24 13.1(15) . .
O23 C22 O24 C25 -2.9(17) . .
C21 C22 O24 C25 177.6(10) . .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.004 0.000 0.500 96 8 ' '
