Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2001

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X-Sun-Content-Lines: 851

data_global

_journal_coden_Cambridge     186 


loop_
_publ_author_name
'A.Slawin'
'J.Woollins'
'Qingzhi Zhang'

_publ_contact_author_name     	'Prof J Woollins'  
_publ_contact_author_address 
;
Department of Chemistry
University of St Andrews
St Andrews
Fife
KY16 9ST
UNITED KINGDOM
;

_publ_contact_author_email JDW3@ST-AND.AC.UK

data_5

_database_code_CSD	165075

_audit_creation_method SHELXL
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_formula_moiety 'C18 H22 Cl2 N O2 P Pd S'
_chemical_formula_structural 'C18 H22 Cl2 N O2 P Pd S'
_chemical_formula_analytical 'C18 H22 Cl2 N O2 P Pd S'
_chemical_formula_sum 'C18 H22 Cl2 N O2 P Pd S'
_chemical_formula_weight 524.70
_chemical_melting_point ?
_chemical_compound_source ?
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'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M P2(1)2(1)2(1)
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'
_cell_length_a 8.87370(10)
_cell_length_b 13.5627(2)
_cell_length_c 17.52930(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2109.67(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 123
_cell_measurement_theta_min 12
_cell_measurement_theta_max 168
_exptl_crystal_description prism
_exptl_crystal_colour yellow
_exptl_crystal_size_max .25
_exptl_crystal_size_mid .1
_exptl_crystal_size_min .1
_exptl_crystal_density_meas   ?
_exptl_crystal_density_diffrn 1.652
_exptl_crystal_density_method ?
_exptl_crystal_F_000 1056
_exptl_absorpt_coefficient_mu 1.320
_exptl_absorpt_correction_type sadabs
_exptl_absorpt_correction_T_min 0.814969
_exptl_absorpt_correction_T_max 1.000000
_exptl_special_details
;
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device SMART
_diffrn_measurement_method CCD
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 9249
_diffrn_reflns_av_R_equivalents 0.0180
_diffrn_reflns_av_sigmaI/netI 0.0207
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 1.90
_diffrn_reflns_theta_max 23.27
_reflns_number_total 3023
_reflns_number_observed 2887
_reflns_observed_criterion >2sigma(I)
_computing_data_collection SMART
_computing_cell_refinement SMART/SAINT
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 13 with very
negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors
R are based on F, with F set to zero for negative F^2^. The observed
criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs
etc. and is
not relevant to the choice of reflections for refinement. R-factors
based on F^2^ are statistically about twice as large as those based
on F, and R-factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.0074P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment riding
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0016(2)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.01(2)
_refine_ls_number_reflns 3010
_refine_ls_number_parameters 240
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0189
_refine_ls_R_factor_obs 0.0168
_refine_ls_wR_factor_all 0.0454
_refine_ls_wR_factor_obs 0.0423
_refine_ls_goodness_of_fit_all 1.008
_refine_ls_goodness_of_fit_obs 1.021
_refine_ls_restrained_S_all 1.071
_refine_ls_restrained_S_obs 1.021
_refine_ls_shift/esd_max 0.004
_refine_ls_shift/esd_mean 0.001
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
Pd1 Pd 0.02645(2) 0.805632(13) 0.147454(11) 0.03114(8) Uani 1 d . .
Cl1 Cl 0.28544(8) 0.81212(6) 0.13963(5) 0.0527(2) Uani 1 d . .
Cl2 Cl 0.00495(10) 0.95989(5) 0.08543(4) 0.0551(2) Uani 1 d . .
P1 P 0.03792(9) 0.65920(4) 0.20749(3) 0.02859(15) Uani 1 d . .
N1 N -0.0378(3) 0.66752(14) 0.29363(11) 0.0347(5) Uani 1 d D .
H1N H -0.0310(29) 0.6132(12) 0.3297(10) 0.031(6) Uiso 1 d D .
C1 C -0.1335(3) 0.7498(2) 0.31821(15) 0.0324(6) Uani 1 d . .
H1A H -0.0958(3) 0.8094(2) 0.29310(15) 0.039 Uiso 1 calc R .
C2 C -0.1163(3) 0.7646(2) 0.4035(2) 0.0369(7) Uani 1 d . .
O2 O -0.0455(3) 0.7128(2) 0.44546(11) 0.0599(6) Uani 1 d . .
O3 O -0.1946(3) 0.8421(2) 0.42549(12) 0.0580(6) Uani 1 d . .
C3 C -0.1933(5) 0.8659(3) 0.5053(2) 0.0661(10) Uani 1 d . .
H3A H -0.2536(5) 0.9235(3) 0.5140(2) 0.099 Uiso 1 calc R .
H3B H -0.0916(5) 0.8784(3) 0.5213(2) 0.099 Uiso 1 calc R .
H3C H -0.2337(5) 0.8116(3) 0.5339(2) 0.099 Uiso 1 calc R .
C4 C -0.2994(3) 0.7387(2) 0.2966(2) 0.0427(7) Uani 1 d . .
H4A H -0.3408(3) 0.6826(2) 0.3238(2) 0.051 Uiso 1 calc R .
H4B H -0.3534(3) 0.7970(2) 0.3135(2) 0.051 Uiso 1 calc R .
C5 C -0.3269(3) 0.7249(2) 0.2125(2) 0.0397(7) Uani 1 d . .
H5A H -0.4344(3) 0.7273(2) 0.2023(2) 0.048 Uiso 1 calc R .
H5B H -0.2901(3) 0.6606(2) 0.1968(2) 0.048 Uiso 1 calc R .
S5 S -0.23164(8) 0.82076(5) 0.15741(5) 0.0442(2) Uani 1 d . .
C6 C -0.3096(4) 0.7959(4) 0.0648(2) 0.0761(12) Uani 1 d . .
H6A H -0.2691(4) 0.8418(4) 0.0285(2) 0.114 Uiso 1 calc R .
H6B H -0.4172(4) 0.8028(4) 0.0667(2) 0.114 Uiso 1 calc R .
H6C H -0.2843(4) 0.7299(4) 0.0497(2) 0.114 Uiso 1 calc R .
C7 C 0.2188(3) 0.6005(2) 0.2238(2) 0.0340(6) Uani 1 d . .
C8 C 0.2828(3) 0.5959(2) 0.2949(2) 0.0410(7) Uani 1 d . .
H8A H 0.2358(3) 0.6266(2) 0.3359(2) 0.049 Uiso 1 calc R .
C9 C 0.4182(4) 0.5456(2) 0.3059(2) 0.0536(9) Uani 1 d . .
H9A H 0.4596(4) 0.5415(2) 0.3546(2) 0.064 Uiso 1 calc R .
C10 C 0.4897(4) 0.5027(2) 0.2461(2) 0.0553(8) Uani 1 d . .
H10A H 0.5794(4) 0.4687(2) 0.2538(2) 0.066 Uiso 1 calc R .
C11 C 0.4287(4) 0.5097(2) 0.1736(2) 0.0569(9) Uani 1 d . .
H11A H 0.4793(4) 0.4822(2) 0.1323(2) 0.068 Uiso 1 calc R .
C12 C 0.2937(4) 0.5571(2) 0.1623(2) 0.0478(8) Uani 1 d . .
H12A H 0.2522(4) 0.5603(2) 0.1136(2) 0.057 Uiso 1 calc R .
C13 C -0.0599(3) 0.5647(2) 0.1517(2) 0.0318(6) Uani 1 d . .
C14 C -0.0852(3) 0.5785(2) 0.07431(15) 0.0429(7) Uani 1 d . .
H14A H -0.0498(3) 0.6352(2) 0.05045(15) 0.052 Uiso 1 calc R .
C15 C -0.1622(4) 0.5088(3) 0.0326(2) 0.0544(9) Uani 1 d . .
H15A H -0.1789(4) 0.5184(3) -0.0193(2) 0.065 Uiso 1 calc R .
C16 C -0.2145(4) 0.4249(3) 0.0678(2) 0.0583(9) Uani 1 d . .
H16A H -0.2685(4) 0.3786(3) 0.0398(2) 0.070 Uiso 1 calc R .
C17 C -0.1873(3) 0.4090(2) 0.1447(2) 0.0512(8) Uani 1 d . .
H17A H -0.2201(3) 0.3512(2) 0.1679(2) 0.061 Uiso 1 calc R .
C18 C -0.1109(3) 0.4797(2) 0.1867(2) 0.0391(7) Uani 1 d . .
H18A H -0.0939(3) 0.4699(2) 0.2385(2) 0.047 Uiso 1 calc R .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.03072(12) 0.02822(11) 0.03447(11) 0.00188(8) 0.00312(9)
0.00144(9)
Cl1 0.0329(4) 0.0531(4) 0.0722(5) 0.0112(5) 0.0030(4) -0.0056(3)
Cl2 0.0608(6) 0.0400(4) 0.0645(5) 0.0181(3) 0.0131(4) 0.0075(4)
P1 0.0274(4) 0.0279(3) 0.0305(3) -0.0016(2) 0.0006(3) 0.0020(3)
N1 0.0405(13) 0.0313(11) 0.0321(11) 0.0011(9) 0.0029(11) 0.0080(10)
C1 0.034(2) 0.0283(14) 0.0348(14) -0.0030(11) 0.0054(12) -0.0007(12)
C2 0.040(2) 0.0311(15) 0.040(2) -0.0027(13) 0.0115(14) -0.0069(13)
O2 0.089(2) 0.0505(12) 0.0406(11) -0.0022(10) -0.0010(12) 0.0117(14)
O3 0.072(2) 0.0564(14) 0.0454(13) -0.0120(10) 0.0104(12) 0.0193(12)
C3 0.087(3) 0.066(2) 0.045(2) -0.022(2) 0.018(2) -0.003(2)
C4 0.030(2) 0.046(2) 0.052(2) 0.0015(14) 0.0110(14) -0.0004(13)
C5 0.025(2) 0.042(2) 0.052(2) 0.0022(13) -0.0023(13) -0.0020(12)
S5 0.0351(4) 0.0444(4) 0.0530(4) 0.0111(4) 0.0042(3) 0.0106(3)
C6 0.046(2) 0.123(3) 0.059(2) 0.025(2) -0.008(2) 0.014(2)
C7 0.031(2) 0.0271(14) 0.044(2) -0.0025(12) -0.0007(13) -0.0023(12)
C8 0.036(2) 0.046(2) 0.041(2) 0.0049(13) -0.0013(14) 0.0014(14)
C9 0.036(2) 0.063(2) 0.062(2) 0.019(2) -0.009(2) -0.003(2)
C10 0.031(2) 0.045(2) 0.090(3) 0.012(2) -0.006(2) 0.0020(14)
C11 0.038(2) 0.048(2) 0.084(3) -0.017(2) 0.010(2) 0.0054(14)
C12 0.038(2) 0.052(2) 0.053(2) -0.0116(15) -0.0013(15) 0.0065(14)
C13 0.0245(15) 0.0328(13) 0.0381(14) -0.0030(12) -0.0003(13) 0.0059(10)
C14 0.044(2) 0.048(2) 0.037(2) -0.0028(13) -0.0012(13) 0.0015(14)
C15 0.055(2) 0.065(2) 0.043(2) -0.016(2) -0.012(2) 0.004(2)
C16 0.041(2) 0.059(2) 0.075(3) -0.030(2) -0.014(2) 0.003(2)
C17 0.041(2) 0.038(2) 0.074(2) -0.012(2) -0.005(2) -0.0011(13)
C18 0.038(2) 0.035(2) 0.044(2) -0.0023(13) -0.0023(13) 0.0058(13)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s.planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are
only used when they are defined by crystal symmetry. An approximate
(isotropic)
treatment of cell esds is used for estimating esds involving l.s.planes.
;
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 P1 2.2500(6) . ?
Pd1 Cl1 2.3039(8) . ?
Pd1 S5 2.3060(8) . ?
Pd1 Cl2 2.3655(7) . ?
P1 N1 1.656(2) . ?
P1 C7 1.814(3) . ?
P1 C13 1.831(2) . ?
N1 C1 1.467(3) . ?
C1 C2 1.517(4) . ?
C1 C4 1.528(4) . ?
C2 O2 1.195(4) . ?
C2 O3 1.317(4) . ?
O3 C3 1.435(4) . ?
C4 C5 1.507(4) . ?
C5 S5 1.827(3) . ?
S5 C6 1.797(4) . ?
C7 C8 1.371(4) . ?
C7 C12 1.397(4) . ?
C8 C9 1.395(4) . ?
C9 C10 1.357(5) . ?
C10 C11 1.386(5) . ?
C11 C12 1.373(5) . ?
C13 C18 1.382(4) . ?
C13 C14 1.387(4) . ?
C14 C15 1.377(4) . ?
C15 C16 1.375(5) . ?
C16 C17 1.386(5) . ?
C17 C18 1.387(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
P1 Pd1 Cl1 90.94(3) . . ?
P1 Pd1 S5 95.05(3) . . ?
Cl1 Pd1 S5 172.65(3) . . ?
P1 Pd1 Cl2 177.92(3) . . ?
Cl1 Pd1 Cl2 91.11(3) . . ?
S5 Pd1 Cl2 82.88(3) . . ?
N1 P1 C7 104.20(12) . . ?
N1 P1 C13 110.03(12) . . ?
C7 P1 C13 101.32(11) . . ?
N1 P1 Pd1 110.36(8) . . ?
C7 P1 Pd1 120.07(9) . . ?
C13 P1 Pd1 110.26(9) . . ?
C1 N1 P1 123.7(2) . . ?
N1 C1 C2 109.4(2) . . ?
N1 C1 C4 114.3(2) . . ?
C2 C1 C4 110.7(2) . . ?
O2 C2 O3 124.5(3) . . ?
O2 C2 C1 125.5(3) . . ?
O3 C2 C1 110.0(3) . . ?
C2 O3 C3 117.4(3) . . ?
C5 C4 C1 114.2(2) . . ?
C4 C5 S5 110.7(2) . . ?
C6 S5 C5 99.5(2) . . ?
C6 S5 Pd1 107.30(13) . . ?
C5 S5 Pd1 115.88(10) . . ?
C8 C7 C12 119.0(3) . . ?
C8 C7 P1 122.0(2) . . ?
C12 C7 P1 119.0(2) . . ?
C7 C8 C9 120.3(3) . . ?
C10 C9 C8 120.4(3) . . ?
C9 C10 C11 119.8(3) . . ?
C12 C11 C10 120.4(3) . . ?
C11 C12 C7 120.1(3) . . ?
C18 C13 C14 119.5(2) . . ?
C18 C13 P1 120.1(2) . . ?
C14 C13 P1 120.3(2) . . ?
C15 C14 C13 120.5(3) . . ?
C16 C15 C14 119.8(3) . . ?
C15 C16 C17 120.5(3) . . ?
C18 C17 C16 119.5(3) . . ?
C13 C18 C17 120.1(3) . . ?
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
Cl1 Pd1 P1 N1 118.72(10) . . . . ?
S5 Pd1 P1 N1 -57.01(10) . . . . ?
Cl2 Pd1 P1 N1 -50.6(8) . . . . ?
Cl1 Pd1 P1 C7 -2.42(11) . . . . ?
S5 Pd1 P1 C7 -178.16(10) . . . . ?
Cl2 Pd1 P1 C7 -171.7(8) . . . . ?
Cl1 Pd1 P1 C13 -119.52(9) . . . . ?
S5 Pd1 P1 C13 64.75(9) . . . . ?
Cl2 Pd1 P1 C13 71.2(8) . . . . ?
C7 P1 N1 C1 145.4(2) . . . . ?
C13 P1 N1 C1 -106.7(2) . . . . ?
Pd1 P1 N1 C1 15.2(2) . . . . ?
P1 N1 C1 C2 -150.4(2) . . . . ?
P1 N1 C1 C4 84.8(3) . . . . ?
N1 C1 C2 O2 -5.5(4) . . . . ?
C4 C1 C2 O2 121.3(3) . . . . ?
N1 C1 C2 O3 176.2(2) . . . . ?
C4 C1 C2 O3 -57.0(3) . . . . ?
O2 C2 O3 C3 0.6(5) . . . . ?
C1 C2 O3 C3 178.9(3) . . . . ?
N1 C1 C4 C5 -56.6(3) . . . . ?
C2 C1 C4 C5 179.3(2) . . . . ?
C1 C4 C5 S5 -51.6(3) . . . . ?
C4 C5 S5 C6 -171.2(2) . . . . ?
C4 C5 S5 Pd1 74.1(2) . . . . ?
P1 Pd1 S5 C6 -105.1(2) . . . . ?
Cl1 Pd1 S5 C6 110.4(3) . . . . ?
Cl2 Pd1 S5 C6 75.1(2) . . . . ?
P1 Pd1 S5 C5 4.97(11) . . . . ?
Cl1 Pd1 S5 C5 -139.5(2) . . . . ?
Cl2 Pd1 S5 C5 -174.80(11) . . . . ?
N1 P1 C7 C8 -16.8(3) . . . . ?
C13 P1 C7 C8 -131.1(2) . . . . ?
Pd1 P1 C7 C8 107.3(2) . . . . ?
N1 P1 C7 C12 162.0(2) . . . . ?
C13 P1 C7 C12 47.8(3) . . . . ?
Pd1 P1 C7 C12 -73.8(2) . . . . ?
C12 C7 C8 C9 -2.3(4) . . . . ?
P1 C7 C8 C9 176.6(2) . . . . ?
C7 C8 C9 C10 1.6(5) . . . . ?
C8 C9 C10 C11 0.6(5) . . . . ?
C9 C10 C11 C12 -2.1(5) . . . . ?
C10 C11 C12 C7 1.4(5) . . . . ?
C8 C7 C12 C11 0.8(5) . . . . ?
P1 C7 C12 C11 -178.1(2) . . . . ?
N1 P1 C13 C18 -36.6(2) . . . . ?
C7 P1 C13 C18 73.2(2) . . . . ?
Pd1 P1 C13 C18 -158.6(2) . . . . ?
N1 P1 C13 C14 142.5(2) . . . . ?
C7 P1 C13 C14 -107.6(2) . . . . ?
Pd1 P1 C13 C14 20.6(2) . . . . ?
C18 C13 C14 C15 0.9(4) . . . . ?
P1 C13 C14 C15 -178.3(2) . . . . ?
C13 C14 C15 C16 0.0(5) . . . . ?
C14 C15 C16 C17 -1.4(5) . . . . ?
C15 C16 C17 C18 2.0(5) . . . . ?
C14 C13 C18 C17 -0.3(4) . . . . ?
P1 C13 C18 C17 178.9(2) . . . . ?
C16 C17 C18 C13 -1.1(4) . . . . ?
_refine_diff_density_max 0.407
_refine_diff_density_min -0.210
_refine_diff_density_rms 0.038

data_7

_database_code_CSD	165076

_audit_creation_method SHELXL
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_formula_moiety 
'C32 H34 Cl2 N2 O4 P2 Pd2 S2.[C H2 Cl2]0.5'
_chemical_formula_structural 'C32.50 H35 Cl3 N2 O4 P2 Pd2 S2'
_chemical_formula_analytical 'C32.50 H35 Cl3 N2 O4 P2 Pd2 S2'
_chemical_formula_sum 'C32.50 H35 Cl3 N2 O4 P2 Pd2 S2'
_chemical_formula_weight 962.84
_chemical_melting_point ?
_chemical_compound_source ?
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'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M P2(1)2(1)2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
_cell_length_a 11.86210(10)
_cell_length_b 18.7870(3)
_cell_length_c 9.1333(2)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2035.39(6)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 94
_cell_measurement_theta_min 12
_cell_measurement_theta_max 168
_exptl_crystal_description prism
_exptl_crystal_colour orange
_exptl_crystal_size_max .14
_exptl_crystal_size_mid .2
_exptl_crystal_size_min .4
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.571
_exptl_crystal_density_method ?
_exptl_crystal_F_000 962
_exptl_absorpt_coefficient_mu 1.297
_exptl_absorpt_correction_type sadabs
_exptl_absorpt_correction_T_min 0.683248
_exptl_absorpt_correction_T_max 1.000000
_exptl_special_details
;
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device SMART
_diffrn_measurement_method CCD
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 9025
_diffrn_reflns_av_R_equivalents 0.0277
_diffrn_reflns_av_sigmaI/netI 0.0310
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_theta_min 2.03
_diffrn_reflns_theta_max 23.25
_reflns_number_total 2928
_reflns_number_observed 2695
_reflns_observed_criterion >2sigma(I)
_computing_data_collection SMART
_computing_cell_refinement SMART/SAINT
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 45 with very
negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors
R are based on F, with F set to zero for negative F^2^. The observed
criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc.
and is
not relevant to the choice of reflections for refinement. R-factors
based on F^2^ are statistically about twice as large as those based on F,
and R-factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+1.6788P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment riding
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0017(7)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.06(5)
_refine_ls_number_reflns 2883
_refine_ls_number_parameters 227
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0422
_refine_ls_R_factor_obs 0.0344
_refine_ls_wR_factor_all 0.1154
_refine_ls_wR_factor_obs 0.0875
_refine_ls_goodness_of_fit_all 1.129
_refine_ls_goodness_of_fit_obs 1.135
_refine_ls_restrained_S_all 1.446
_refine_ls_restrained_S_obs 1.134
_refine_ls_shift/esd_max 4.562
_refine_ls_shift/esd_mean 0.351
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
Pd1 Pd 0.93851(4) 0.06870(2) 0.81479(5) 0.0325(2) Uani 1 d . .
Cl1 Cl 1.0083(2) 0.17246(9) 0.7094(2) 0.0558(5) Uani 1 d . .
P1 P 0.77151(13) 0.08837(8) 0.7063(2) 0.0333(4) Uani 1 d . .
N1 N 0.6846(5) 0.0191(3) 0.7225(6) 0.0369(13) Uani 1 d D .
H1N H 0.6039(17) 0.0213(38) 0.6997(80) 0.053(19) Uiso 1 d D .
C1 C 0.7293(5) -0.0534(3) 0.7069(7) 0.0317(13) Uani 1 d . .
H1A H 0.7925(5) -0.0527(3) 0.6378(7) 0.038 Uiso 1 calc R .
C2 C 0.6369(6) -0.0992(3) 0.6453(7) 0.0351(15) Uani 1 d . .
O2 O 0.5443(4) -0.0787(3) 0.6132(6) 0.0535(12) Uani 1 d . .
O3 O 0.6687(4) -0.1671(2) 0.6327(6) 0.0519(13) Uani 1 d . .
C3 C 0.5838(7) -0.2158(4) 0.5736(9) 0.057(2) Uani 1 d . .
H3A H 0.6144(7) -0.2630(4) 0.5688(9) 0.086 Uiso 1 calc R .
H3B H 0.5624(7) -0.2005(4) 0.4772(9) 0.086 Uiso 1 calc R .
H3C H 0.5187(7) -0.2157(4) 0.6361(9) 0.086 Uiso 1 calc R .
C4 C 0.7705(6) -0.0823(4) 0.8536(7) 0.043(2) Uani 1 d . .
H4A H 0.7918(6) -0.1318(4) 0.8407(7) 0.051 Uiso 1 calc R .
H4B H 0.7084(6) -0.0810(4) 0.9225(7) 0.051 Uiso 1 calc R .
S4 S 0.88907(13) -0.03477(8) 0.9327(2) 0.0340(4) Uani 1 d . .
C7 C 0.7842(6) 0.1072(4) 0.5127(7) 0.039(2) Uani 1 d . .
C8 C 0.7022(6) 0.1450(4) 0.4345(8) 0.051(2) Uani 1 d . .
H8A H 0.6413(6) 0.1644(4) 0.4847(8) 0.061 Uiso 1 calc R .
C9 C 0.7095(7) 0.1541(5) 0.2871(9) 0.066(2) Uani 1 d . .
H9A H 0.6542(7) 0.1801(5) 0.2386(9) 0.079 Uiso 1 calc R .
C10 C 0.7974(8) 0.1253(5) 0.2087(10) 0.073(2) Uani 1 d . .
H10A H 0.8012(8) 0.1312(5) 0.1077(10) 0.087 Uiso 1 calc R .
C11 C 0.8799(8) 0.0875(5) 0.2822(9) 0.069(2) Uani 1 d . .
H11A H 0.9401(8) 0.0681(5) 0.2305(9) 0.083 Uiso 1 calc R .
C12 C 0.8732(7) 0.0783(4) 0.4337(8) 0.049(2) Uani 1 d . .
H12A H 0.9288(7) 0.0525(4) 0.4821(8) 0.059 Uiso 1 calc R .
C13 C 0.6927(6) 0.1608(3) 0.7870(7) 0.038(2) Uani 1 d . .
C14 C 0.6042(6) 0.1473(4) 0.8871(7) 0.045(2) Uani 1 d . .
H14A H 0.5835(6) 0.1007(4) 0.9089(7) 0.054 Uiso 1 calc R .
C15 C 0.5489(8) 0.2034(5) 0.9519(8) 0.066(2) Uani 1 d . .
H15A H 0.4922(8) 0.1949(5) 1.0199(8) 0.079 Uiso 1 calc R .
C16 C 0.5776(8) 0.2724(4) 0.9160(9) 0.066(2) Uani 1 d . .
H16A H 0.5380(8) 0.3101(4) 0.9572(9) 0.079 Uiso 1 calc R .
C17 C 0.6616(8) 0.2854(4) 0.8225(13) 0.074(2) Uani 1 d . .
H17A H 0.6811(8) 0.3323(4) 0.8016(13) 0.089 Uiso 1 calc R .
C18 C 0.7203(8) 0.2306(4) 0.7561(9) 0.058(2) Uani 1 d . .
H18A H 0.7783(8) 0.2407(4) 0.6908(9) 0.069 Uiso 1 calc R .
C20 C 0.5000 0.0000 0.2920(21) 0.060(6) Uani 0.50 d SP .
H20A H 0.4553 -0.0307 0.3546(21) 0.072 Uiso 0.25 calc PR .
H20B H 0.5447 0.0307 0.3546(21) 0.072 Uiso 0.25 calc PR .
Cl20 Cl 0.5833(8) -0.0484(6) 0.1956(12) 0.239(7) Uani 0.50 d P .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0344(3) 0.0292(3) 0.0337(3) -0.0004(2) -0.0029(2) 0.0002(2)
Cl1 0.0573(10) 0.0429(9) 0.0673(12) 0.0176(9) -0.0222(10) -0.0141(8)
P1 0.0336(8) 0.0290(8) 0.0372(9) -0.0003(7) -0.0026(7) 0.0007(6)
N1 0.031(3) 0.029(3) 0.051(3) 0.006(2) -0.005(2) -0.004(2)
C1 0.029(3) 0.028(3) 0.037(3) -0.001(3) 0.002(3) -0.003(2)
C2 0.035(4) 0.032(3) 0.038(4) 0.006(3) 0.000(3) 0.007(3)
O2 0.048(3) 0.038(3) 0.074(3) -0.006(2) -0.013(2) 0.003(2)
O3 0.043(3) 0.034(3) 0.079(3) -0.016(2) -0.009(2) -0.003(2)
C3 0.054(5) 0.038(4) 0.080(5) -0.019(4) -0.007(4) -0.004(3)
C4 0.045(4) 0.034(4) 0.049(4) 0.001(3) -0.006(3) 0.010(3)
S4 0.0362(8) 0.0380(8) 0.0277(7) 0.0027(6) 0.0031(7) 0.0005(7)
C7 0.043(4) 0.043(4) 0.032(3) -0.005(3) -0.009(3) -0.014(3)
C8 0.037(4) 0.074(5) 0.041(4) 0.003(4) -0.004(3) 0.010(3)
C9 0.054(5) 0.095(6) 0.048(5) 0.020(4) -0.018(4) -0.001(4)
C10 0.076(6) 0.094(7) 0.047(5) 0.007(5) -0.005(5) -0.008(5)
C11 0.075(6) 0.079(6) 0.053(5) -0.016(4) 0.013(4) 0.004(5)
C12 0.061(4) 0.045(4) 0.042(4) -0.007(3) 0.002(3) 0.008(4)
C13 0.041(4) 0.038(4) 0.036(4) 0.001(3) -0.009(3) 0.011(3)
C14 0.044(4) 0.048(4) 0.043(4) 0.005(3) 0.003(3) 0.010(3)
C15 0.071(6) 0.079(6) 0.049(4) -0.013(4) 0.012(4) 0.021(5)
C16 0.086(7) 0.048(5) 0.062(5) -0.023(4) -0.010(5) 0.027(5)
C17 0.078(6) 0.040(4) 0.104(7) -0.018(5) 0.008(7) 0.002(4)
C18 0.068(5) 0.034(4) 0.070(5) -0.013(3) 0.008(4) 0.000(4)
C20 0.097(18) 0.055(12) 0.027(10) 0.000 0.000 -0.015(12)
Cl20 0.194(9) 0.306(12) 0.219(10) -0.207(10) 0.152(8) -0.124(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s.planes)
are estimated using the full covariance matrix. The cell esds aretaken
into account individually in the estimation of esds in distances,angles
and torsion angles; correlations between esds in cell parameters areonly
used when they are defined by crystal symmetry. An approximate(isotropic)
treatment of cell esds is used for estimating esds involving l.s.planes.
;
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 P1 2.246(2) . ?
Pd1 S4 2.298(2) . ?
Pd1 Cl1 2.326(2) . ?
Pd1 S4 2.398(2) 2_755 ?
Pd1 Pd1 2.9652(9) 2_755 ?
P1 N1 1.667(5) . ?
P1 C13 1.808(6) . ?
P1 C7 1.809(7) . ?
N1 C1 1.469(8) . ?
C1 C2 1.502(9) . ?
C1 C4 1.526(9) . ?
C2 O2 1.200(8) . ?
C2 O3 1.335(8) . ?
O3 C3 1.463(8) . ?
C4 S4 1.816(7) . ?
S4 Pd1 2.398(2) 2_755 ?
C7 C12 1.390(10) . ?
C7 C8 1.401(10) . ?
C8 C9 1.360(11) . ?
C9 C10 1.375(12) . ?
C10 C11 1.384(13) . ?
C11 C12 1.397(12) . ?
C13 C18 1.380(10) . ?
C13 C14 1.415(10) . ?
C14 C15 1.375(11) . ?
C15 C16 1.379(13) . ?
C16 C17 1.335(13) . ?
C17 C18 1.384(12) . ?
C20 Cl20 1.606(12) 2_655 ?
C20 Cl20 1.606(12) . ?
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
P1 Pd1 S4 96.94(6) . . ?
P1 Pd1 Cl1 89.62(6) . . ?
S4 Pd1 Cl1 173.42(6) . . ?
P1 Pd1 S4 173.94(6) . 2_755 ?
S4 Pd1 S4 77.43(7) . 2_755 ?
Cl1 Pd1 S4 96.04(6) . 2_755 ?
P1 Pd1 Pd1 125.26(4) . 2_755 ?
S4 Pd1 Pd1 52.35(4) . 2_755 ?
Cl1 Pd1 Pd1 123.68(6) . 2_755 ?
S4 Pd1 Pd1 49.37(4) 2_755 2_755 ?
N1 P1 C13 103.4(3) . . ?
N1 P1 C7 106.9(3) . . ?
C13 P1 C7 107.1(3) . . ?
N1 P1 Pd1 112.2(2) . . ?
C13 P1 Pd1 113.6(2) . . ?
C7 P1 Pd1 112.9(2) . . ?
C1 N1 P1 119.5(4) . . ?
N1 C1 C2 107.7(5) . . ?
N1 C1 C4 111.1(5) . . ?
C2 C1 C4 111.0(5) . . ?
O2 C2 O3 122.9(6) . . ?
O2 C2 C1 125.2(6) . . ?
O3 C2 C1 111.9(5) . . ?
C2 O3 C3 115.8(5) . . ?
C1 C4 S4 115.0(5) . . ?
C4 S4 Pd1 115.3(2) . . ?
C4 S4 Pd1 110.6(2) . 2_755 ?
Pd1 S4 Pd1 78.28(5) . 2_755 ?
C12 C7 C8 117.5(6) . . ?
C12 C7 P1 119.6(5) . . ?
C8 C7 P1 122.7(5) . . ?
C9 C8 C7 121.7(7) . . ?
C8 C9 C10 120.9(8) . . ?
C9 C10 C11 119.1(8) . . ?
C10 C11 C12 120.2(8) . . ?
C7 C12 C11 120.6(7) . . ?
C18 C13 C14 118.6(6) . . ?
C18 C13 P1 120.6(6) . . ?
C14 C13 P1 120.8(5) . . ?
C15 C14 C13 119.6(7) . . ?
C16 C15 C14 120.0(8) . . ?
C17 C16 C15 120.6(8) . . ?
C16 C17 C18 121.3(8) . . ?
C13 C18 C17 119.9(8) . . ?
Cl20 C20 Cl20 113.5(15) 2_655 . ?
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
S4 Pd1 P1 N1 -9.9(2) . . . . ?
Cl1 Pd1 P1 N1 170.7(2) . . . . ?
S4 Pd1 P1 N1 11.7(7) 2_755 . . . ?
Pd1 Pd1 P1 N1 38.2(2) 2_755 . . . ?
S4 Pd1 P1 C13 107.0(2) . . . . ?
Cl1 Pd1 P1 C13 -72.5(3) . . . . ?
S4 Pd1 P1 C13 128.5(6) 2_755 . . . ?
Pd1 Pd1 P1 C13 155.1(2) 2_755 . . . ?
S4 Pd1 P1 C7 -130.8(2) . . . . ?
Cl1 Pd1 P1 C7 49.7(2) . . . . ?
S4 Pd1 P1 C7 -109.3(6) 2_755 . . . ?
Pd1 Pd1 P1 C7 -82.7(2) 2_755 . . . ?
C13 P1 N1 C1 -163.1(5) . . . . ?
C7 P1 N1 C1 84.0(5) . . . . ?
Pd1 P1 N1 C1 -40.4(5) . . . . ?
P1 N1 C1 C2 -149.6(4) . . . . ?
P1 N1 C1 C4 88.6(6) . . . . ?
N1 C1 C2 O2 1.1(9) . . . . ?
C4 C1 C2 O2 123.0(7) . . . . ?
N1 C1 C2 O3 -177.5(5) . . . . ?
C4 C1 C2 O3 -55.7(7) . . . . ?
O2 C2 O3 C3 1.2(9) . . . . ?
C1 C2 O3 C3 179.9(6) . . . . ?
N1 C1 C4 S4 -64.2(6) . . . . ?
C2 C1 C4 S4 176.0(4) . . . . ?
C1 C4 S4 Pd1 8.3(5) . . . . ?
C1 C4 S4 Pd1 -78.1(5) . . . 2_755 ?
P1 Pd1 S4 C4 22.5(3) . . . . ?
Cl1 Pd1 S4 C4 -162.2(6) . . . . ?
S4 Pd1 S4 C4 -155.3(3) 2_755 . . . ?
Pd1 Pd1 S4 C4 -107.4(3) 2_755 . . . ?
P1 Pd1 S4 Pd1 129.83(5) . . . 2_755 ?
Cl1 Pd1 S4 Pd1 -54.8(6) . . . 2_755 ?
S4 Pd1 S4 Pd1 -47.89(6) 2_755 . . 2_755 ?
Pd1 Pd1 S4 Pd1 0.0 2_755 . . 2_755 ?
N1 P1 C7 C12 -94.6(6) . . . . ?
C13 P1 C7 C12 155.1(5) . . . . ?
Pd1 P1 C7 C12 29.3(6) . . . . ?
N1 P1 C7 C8 79.7(6) . . . . ?
C13 P1 C7 C8 -30.7(7) . . . . ?
Pd1 P1 C7 C8 -156.5(5) . . . . ?
C12 C7 C8 C9 -0.8(11) . . . . ?
P1 C7 C8 C9 -175.1(6) . . . . ?
C7 C8 C9 C10 1.0(13) . . . . ?
C8 C9 C10 C11 -0.8(14) . . . . ?
C9 C10 C11 C12 0.6(14) . . . . ?
C8 C7 C12 C11 0.5(11) . . . . ?
P1 C7 C12 C11 175.0(6) . . . . ?
C10 C11 C12 C7 -0.4(12) . . . . ?
N1 P1 C13 C18 -160.3(6) . . . . ?
C7 P1 C13 C18 -47.6(7) . . . . ?
Pd1 P1 C13 C18 77.8(6) . . . . ?
N1 P1 C13 C14 22.0(6) . . . . ?
C7 P1 C13 C14 134.7(5) . . . . ?
Pd1 P1 C13 C14 -99.9(5) . . . . ?
C18 C13 C14 C15 -0.6(10) . . . . ?
P1 C13 C14 C15 177.1(6) . . . . ?
C13 C14 C15 C16 1.9(12) . . . . ?
C14 C15 C16 C17 -2.5(14) . . . . ?
C15 C16 C17 C18 1.7(15) . . . . ?
C14 C13 C18 C17 -0.1(12) . . . . ?
P1 C13 C18 C17 -177.9(7) . . . . ?
C16 C17 C18 C13 -0.4(15) . . . . ?

_refine_diff_density_max 0.709
_refine_diff_density_min -0.477
_refine_diff_density_rms 0.086