data_2010src0042

#Dr. S. L. James
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C40 H34 Cl2 P2 Pd'
_chemical_formula_weight          753.91
 
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'
 'P'  'P'   0.1023   0.0942
 '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            triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.9242(4)
_cell_length_b                    9.9428(4)
_cell_length_c                    10.4323(3)
_cell_angle_alpha                 86.305(2)
_cell_angle_beta                  67.758(2)
_cell_angle_gamma                 62.176(2)
_cell_volume                      834.69(5)
_cell_formula_units_Z             1
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3767
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Yellow
_exptl_crystal_size_max           0.36
_exptl_crystal_size_mid           0.18
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.500
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              384
_exptl_absorpt_coefficient_mu     0.841
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7517
_exptl_absorpt_correction_T_max   0.9671
_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Estimated minimum and maximum transmission: 0.6524 0.7456
The given Tmin and Tmax were generated using the SHELX SIZE command
;


_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type   
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '9.091'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             18038
_diffrn_reflns_av_R_equivalents   0.0583
_diffrn_reflns_av_sigmaI/netI     0.0513
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.69
_diffrn_reflns_theta_max          27.48
_reflns_number_total              3813
_reflns_number_gt                 3133
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX (Farrugia, 1999)'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0301P)²+0.8845P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          3813
_refine_ls_number_parameters      238
_refine_ls_number_restraints      18
_refine_ls_R_factor_all           0.0531
_refine_ls_R_factor_gt            0.0382
_refine_ls_wR_factor_ref          0.0867
_refine_ls_wR_factor_gt           0.0799
_refine_ls_goodness_of_fit_ref    1.051
_refine_ls_restrained_S_all       1.049
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
Cl1 Cl 0.14765(9) 0.23785(8) 0.44752(7) 0.03033(18) Uani 1 1 d . . .
Pd1 Pd 0.0000 0.5000 0.5000 0.02187(10) Uani 1 2 d S . .
P1 P -0.21437(8) 0.49842(8) 0.69617(7) 0.01927(16) Uani 1 1 d D . .
C1 C -0.1755(3) 0.3145(3) 0.7608(3) 0.0211(6) Uani 1 1 d . A .
C2 C -0.1778(3) 0.2917(3) 0.8949(3) 0.0234(6) Uani 1 1 d . . .
H2 H -0.2010 0.3736 0.9559 0.028 Uiso 1 1 calc R A .
C3 C -0.1463(4) 0.1491(4) 0.9392(3) 0.0309(7) Uani 1 1 d . A .
H3 H -0.1482 0.1338 1.0306 0.037 Uiso 1 1 calc R . .
C4 C -0.1125(4) 0.0305(4) 0.8514(3) 0.0345(7) Uani 1 1 d . . .
H4 H -0.0891 -0.0672 0.8817 0.041 Uiso 1 1 calc R A .
C5 C -0.1122(4) 0.0522(3) 0.7183(3) 0.0329(7) Uani 1 1 d . A .
H5 H -0.0908 -0.0297 0.6585 0.040 Uiso 1 1 calc R . .
C6 C -0.1433(3) 0.1934(3) 0.6737(3) 0.0263(6) Uani 1 1 d . . .
H6 H -0.1427 0.2081 0.5826 0.032 Uiso 1 1 calc R A .
C7 C -0.4099(3) 0.5626(3) 0.6779(3) 0.0211(6) Uani 1 1 d . A .
C8 C -0.4539(4) 0.6668(3) 0.5867(3) 0.0289(6) Uani 1 1 d . . .
H8 H -0.3812 0.7048 0.5323 0.035 Uiso 1 1 calc R A .
C9 C -0.6042(4) 0.7154(4) 0.5752(3) 0.0344(7) Uani 1 1 d . A .
H9 H -0.6341 0.7874 0.5135 0.041 Uiso 1 1 calc R . .
C10 C -0.7107(4) 0.6602(4) 0.6525(3) 0.0312(7) Uani 1 1 d . . .
H10 H -0.8135 0.6942 0.6443 0.037 Uiso 1 1 calc R A .
C11 C -0.6663(4) 0.5548(4) 0.7418(3) 0.0303(7) Uani 1 1 d . A .
H11 H -0.7383 0.5153 0.7942 0.036 Uiso 1 1 calc R . .
C12 C -0.5176(4) 0.5068(4) 0.7550(3) 0.0268(6) Uani 1 1 d . . .
H12 H -0.4886 0.4352 0.8173 0.032 Uiso 1 1 calc R A .
C13 C -0.2657(13) 0.623(2) 0.8469(18) 0.023(4) Uani 0.665(9) 1 d PD A 1
C14 C -0.4263(11) 0.7337(13) 0.9258(9) 0.0212(19) Uani 0.665(9) 1 d PD A 1
H14 H -0.5139 0.7473 0.9006 0.025 Uiso 0.665(9) 1 calc PR A 1
C15 C -0.4615(8) 0.8252(8) 1.0411(6) 0.0251(14) Uani 0.665(9) 1 d PD A 1
H15 H -0.5731 0.8994 1.0940 0.030 Uiso 0.665(9) 1 calc PR A 1
C16 C -0.3380(9) 0.8111(7) 1.0809(5) 0.0218(13) Uani 0.665(9) 1 d PD A 1
C17 C -0.1756(10) 0.7027(8) 1.0000(7) 0.0221(14) Uani 0.665(9) 1 d PD A 1
H17 H -0.0883 0.6909 1.0247 0.027 Uiso 0.665(9) 1 calc PR A 1
C18 C -0.1390(11) 0.6113(11) 0.8835(9) 0.027(2) Uani 0.665(9) 1 d PD A 1
H18 H -0.0269 0.5403 0.8282 0.033 Uiso 0.665(9) 1 calc PR A 1
C19 C -0.3807(7) 0.9058(6) 1.2073(5) 0.0292(13) Uani 0.665(9) 1 d PD A 1
H19 H -0.4906 0.9888 1.2456 0.035 Uiso 0.665(9) 1 calc PR A 1
C20 C -0.2868(7) 0.8901(6) 1.2734(5) 0.0398(16) Uani 0.665(9) 1 d PD A 1
H20A H -0.1756 0.8093 1.2403 0.048 Uiso 0.665(9) 1 calc PR A 1
H20B H -0.3297 0.9596 1.3545 0.048 Uiso 0.665(9) 1 calc PR A 1
C113 C -0.250(2) 0.621(5) 0.839(4) 0.017(7) Uiso 0.335(9) 1 d PD A 2
C114 C -0.405(2) 0.716(3) 0.939(2) 0.029(7) Uiso 0.335(9) 1 d PD A 2
H114 H -0.5014 0.7271 0.9300 0.035 Uiso 0.335(9) 1 calc PR A 2
C115 C -0.4196(16) 0.7956(16) 1.0524(13) 0.023(4) Uiso 0.335(9) 1 d PD A 2
H115 H -0.5262 0.8685 1.1163 0.028 Uiso 0.335(9) 1 calc PR A 2
C116 C -0.2817(17) 0.7696(14) 1.0729(12) 0.016(3) Uiso 0.335(9) 1 d PD A 2
C117 C -0.1271(17) 0.6729(18) 0.9739(15) 0.024(4) Uiso 0.335(9) 1 d PD A 2
H117 H -0.0312 0.6573 0.9866 0.029 Uiso 0.335(9) 1 calc PR A 2
C118 C -0.109(2) 0.599(2) 0.8568(17) 0.019(4) Uiso 0.335(9) 1 d PD A 2
H118 H -0.0012 0.5325 0.7891 0.023 Uiso 0.335(9) 1 calc PR A 2
C119 C -0.2910(14) 0.8434(12) 1.1976(9) 0.031(3) Uiso 0.335(9) 1 d PD A 2
H119 H -0.1894 0.8178 1.2048 0.037 Uiso 0.335(9) 1 calc PR A 2
C120 C -0.4264(13) 0.9397(12) 1.2970(12) 0.043(3) Uiso 0.335(9) 1 d PD A 2
H12A H -0.5306 0.9682 1.2937 0.052 Uiso 0.335(9) 1 calc PR A 2
H12B H -0.4218 0.9819 1.3734 0.052 Uiso 0.335(9) 1 calc PR A 2
 
 
_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
Cl1 Pd1 2.2917(7) . ?
Pd1 Cl1 2.2917(7) 2_566 ?
Pd1 P1 2.3336(6) . ?
Pd1 P1 2.3336(6) 2_566 ?
P1 C113 1.809(12) . ?
P1 C13 1.822(6) . ?
P1 C7 1.822(3) . ?
P1 C1 1.824(3) . ?
C1 C6 1.393(4) . ?
C1 C2 1.395(4) . ?
C2 C3 1.390(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.371(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.390(4) . ?
C7 C12 1.394(4) . ?
C8 C9 1.388(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.385(9) . ?
C13 C18 1.401(8) . ?
C14 C15 1.387(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.391(8) . ?
C16 C19 1.472(6) . ?
C17 C18 1.390(8) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.306(7) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9500 . ?
C20 H20B 0.9500 . ?
C113 C114 1.379(15) . ?
C113 C118 1.395(13) . ?
C114 C115 1.391(14) . ?
C114 H114 0.9500 . ?
C115 C116 1.367(13) . ?
C115 H115 0.9500 . ?
C116 C117 1.378(12) . ?
C116 C119 1.486(11) . ?
C117 C118 1.376(13) . ?
C117 H117 0.9500 . ?
C118 H118 0.9500 . ?
C119 C120 1.292(12) . ?
C119 H119 0.9500 . ?
C120 H12A 0.9500 . ?
C120 H12B 0.9500 . ?
 
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
Cl1 Pd1 Cl1 180.0 2_566 . ?
Cl1 Pd1 P1 85.86(2) 2_566 . ?
Cl1 Pd1 P1 94.15(2) . . ?
Cl1 Pd1 P1 94.14(2) 2_566 2_566 ?
Cl1 Pd1 P1 85.85(2) . 2_566 ?
P1 Pd1 P1 180.0 . 2_566 ?
C113 P1 C13 4.4(14) . . ?
C113 P1 C7 108.7(6) . . ?
C13 P1 C7 105.1(4) . . ?
C113 P1 C1 104.8(17) . . ?
C13 P1 C1 103.4(9) . . ?
C7 P1 C1 102.98(12) . . ?
C113 P1 Pd1 107.3(13) . . ?
C13 P1 Pd1 111.5(7) . . ?
C7 P1 Pd1 115.69(9) . . ?
C1 P1 Pd1 116.75(9) . . ?
C6 C1 C2 119.1(3) . . ?
C6 C1 P1 118.9(2) . . ?
C2 C1 P1 122.1(2) . . ?
C3 C2 C1 120.0(3) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 120.6(3) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C8 C7 C12 118.9(3) . . ?
C8 C7 P1 120.9(2) . . ?
C12 C7 P1 120.2(2) . . ?
C9 C8 C7 120.0(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.7(3) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 119.4(3) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C10 C11 C12 120.3(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 120.6(3) . . ?
C11 C12 H12 119.7 . . ?
C7 C12 H12 119.7 . . ?
C14 C13 C18 117.7(6) . . ?
C14 C13 P1 122.6(7) . . ?
C18 C13 P1 119.7(7) . . ?
C13 C14 C15 121.1(8) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C16 C15 C14 121.6(6) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C17 117.7(4) . . ?
C15 C16 C19 120.1(5) . . ?
C17 C16 C19 122.3(5) . . ?
C18 C17 C16 121.2(5) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C13 120.7(7) . . ?
C17 C18 H18 119.7 . . ?
C13 C18 H18 119.7 . . ?
C20 C19 C16 128.2(6) . . ?
C20 C19 H19 115.9 . . ?
C16 C19 H19 115.9 . . ?
C19 C20 H20A 120.0 . . ?
C19 C20 H20B 120.0 . . ?
H20A C20 H20B 120.0 . . ?
C114 C113 C118 119.9(12) . . ?
C114 C113 P1 123.5(13) . . ?
C118 C113 P1 115.8(11) . . ?
C113 C114 C115 119.6(14) . . ?
C113 C114 H114 120.2 . . ?
C115 C114 H114 120.2 . . ?
C116 C115 C114 120.6(12) . . ?
C116 C115 H115 119.7 . . ?
C114 C115 H115 119.7 . . ?
C115 C116 C117 119.3(10) . . ?
C115 C116 C119 122.7(11) . . ?
C117 C116 C119 118.0(11) . . ?
C118 C117 C116 121.3(12) . . ?
C118 C117 H117 119.3 . . ?
C116 C117 H117 119.3 . . ?
C117 C118 C113 119.0(12) . . ?
C117 C118 H118 120.5 . . ?
C113 C118 H118 120.5 . . ?
C120 C119 C116 125.1(11) . . ?
C120 C119 H119 117.4 . . ?
C116 C119 H119 117.4 . . ?
C119 C120 H12A 120.0 . . ?
C119 C120 H12B 120.0 . . ?
H12A C120 H12B 120.0 . . ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    0.517
_refine_diff_density_min   -0.794
_refine_diff_density_rms    0.090
