#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:18:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179784 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/80/7008074.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_7008074
loop_
_publ_author_name
'Baber, R. Angharad'
'Orpen, A. Guy'
'Pringle, Paul G.'
'Wilkinson, Matthew J.'
'Wingad, Richard L.'
_publ_section_title
;
 Special effects of ortho-isopropylphenyl groups. Diastereoisomerism in
 platinum(II) and palladium(II) complexes of helically chiral PAr3
 ligands.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              659
_journal_page_last               667
_journal_paper_doi               10.1039/b416525j
_journal_year                    2005
_chemical_formula_moiety         'C54 H66 Cl4 P2 Pd2, 4(C H Cl3)'
_chemical_formula_sum            'C58 H70 Cl16 P2 Pd2'
_chemical_formula_weight         1609.08
_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                90.563(4)
_cell_angle_beta                 94.222(4)
_cell_angle_gamma                111.771(4)
_cell_formula_units_Z            1
_cell_length_a                   12.189(3)
_cell_length_b                   12.331(3)
_cell_length_c                   12.420(3)
_cell_measurement_reflns_used    2796
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.5895
_cell_measurement_theta_min      2.47
_cell_volume                     1727.5(7)
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1998)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1998)'
_computing_structure_refinement  'Bruker SHELXTL (Bruker, 1998)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 1998)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.1052
_diffrn_reflns_av_sigmaI/netI    0.1782
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18068
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.229
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1642
_refine_ls_R_factor_gt           0.0710
_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)+(0.0914P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.2136
_reflns_number_gt                4050
_reflns_number_total             7821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b416525j.txt
_cod_data_source_block           4c.4CHCl3(averys)
_cod_database_code               7008074
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.02040(6) 0.11263(6) 0.41123(5) 0.0174(2) Uani 1 1 d . . .
Cl1 Cl 0.13970(18) 0.03013(19) 0.50501(18) 0.0252(5) Uani 1 1 d . . .
P1 P 0.17152(19) 0.25101(18) 0.33955(18) 0.0181(5) Uani 1 1 d . . .
Cl2 Cl -0.10744(18) 0.19555(19) 0.33813(18) 0.0253(5) Uani 1 1 d . . .
Cl5 Cl 0.2499(3) 0.1034(3) 0.8345(3) 0.0547(8) Uani 1 1 d . . .
Cl6 Cl 0.4206(3) 0.1381(3) 0.6752(2) 0.0583(8) Uani 1 1 d . . .
Cl7 Cl 0.4587(4) 0.0525(4) 0.8813(3) 0.0959(15) Uani 1 1 d . . .
Cl12 Cl 0.7911(4) 0.2599(3) -0.0286(3) 0.0799(12) Uani 1 1 d . . .
Cl8 Cl 0.6885(3) 0.2889(4) 0.1666(3) 0.0867(12) Uani 1 1 d . . .
Cl9 Cl 0.9064(4) 0.4612(3) 0.1143(3) 0.0875(12) Uani 1 1 d . . .
C19 C 0.3154(7) 0.2390(7) 0.3696(6) 0.0167(17) Uani 1 1 d . . .
C20 C 0.4039(8) 0.3268(7) 0.4324(7) 0.0234(19) Uani 1 1 d . . .
H20A H 0.3886 0.3927 0.4570 0.028 Uiso 1 1 calc R . .
C15 C 0.2324(7) 0.3343(7) 0.1282(7) 0.0210(18) Uani 1 1 d . . .
C1 C 0.1754(7) 0.3916(7) 0.3940(7) 0.0190(18) Uani 1 1 d . . .
C23 C 0.4514(7) 0.1383(8) 0.3593(7) 0.027(2) Uani 1 1 d . . .
H23A H 0.4687 0.0738 0.3345 0.032 Uiso 1 1 calc R . .
C6 C 0.1826(7) 0.4158(7) 0.5083(7) 0.0194(18) Uani 1 1 d . . .
C7 C 0.1977(7) 0.3344(7) 0.5960(6) 0.0215(19) Uani 1 1 d . . .
H7A H 0.2162 0.2712 0.5596 0.026 Uiso 1 1 calc R . .
C24 C 0.3393(7) 0.1411(7) 0.3316(7) 0.024(2) Uani 1 1 d . . .
C10 C 0.1524(8) 0.2548(7) 0.1925(7) 0.0219(19) Uani 1 1 d . . .
C9 C 0.0807(8) 0.2762(8) 0.6474(8) 0.034(2) Uani 1 1 d . . .
H9A H 0.0905 0.2236 0.7028 0.051 Uiso 1 1 calc R . .
H9B H 0.0188 0.2313 0.5917 0.051 Uiso 1 1 calc R . .
H9C H 0.0580 0.3363 0.6807 0.051 Uiso 1 1 calc R . .
C11 C 0.0507(7) 0.1652(7) 0.1417(7) 0.0231(19) Uani 1 1 d . . .
H11A H -0.0020 0.1088 0.1844 0.028 Uiso 1 1 calc R . .
C27 C 0.2456(9) -0.0815(8) 0.2943(8) 0.035(2) Uani 1 1 d . . .
H27A H 0.2255 -0.0909 0.3695 0.053 Uiso 1 1 calc R . .
H27B H 0.3225 -0.0884 0.2884 0.053 Uiso 1 1 calc R . .
H27C H 0.1845 -0.1422 0.2480 0.053 Uiso 1 1 calc R . .
C2 C 0.1552(7) 0.4694(8) 0.3227(7) 0.025(2) Uani 1 1 d . . .
H2A H 0.1479 0.4517 0.2473 0.029 Uiso 1 1 calc R . .
C26 C 0.2840(8) 0.0585(8) 0.1405(7) 0.030(2) Uani 1 1 d . . .
H26A H 0.2875 0.1359 0.1188 0.044 Uiso 1 1 calc R . .
H26B H 0.2234 -0.0018 0.0934 0.044 Uiso 1 1 calc R . .
H26C H 0.3613 0.0527 0.1341 0.044 Uiso 1 1 calc R . .
C25 C 0.2524(8) 0.0411(8) 0.2576(7) 0.028(2) Uani 1 1 d . . .
H25A H 0.1718 0.0440 0.2608 0.034 Uiso 1 1 calc R . .
C5 C 0.1711(7) 0.5189(7) 0.5400(8) 0.026(2) Uani 1 1 d . . .
H5A H 0.1747 0.5370 0.6150 0.032 Uiso 1 1 calc R . .
C21 C 0.5140(8) 0.3206(8) 0.4600(7) 0.027(2) Uani 1 1 d . . .
H21A H 0.5723 0.3804 0.5048 0.033 Uiso 1 1 calc R . .
C4 C 0.1545(8) 0.5964(8) 0.4670(8) 0.031(2) Uani 1 1 d . . .
H4A H 0.1494 0.6671 0.4926 0.037 Uiso 1 1 calc R . .
C14 C 0.2067(8) 0.3258(9) 0.0165(7) 0.030(2) Uani 1 1 d . . .
H14A H 0.2598 0.3797 -0.0278 0.036 Uiso 1 1 calc R . .
C12 C 0.0276(8) 0.1590(9) 0.0323(7) 0.030(2) Uani 1 1 d . . .
H12A H -0.0413 0.0994 -0.0012 0.035 Uiso 1 1 calc R . .
C13 C 0.1060(9) 0.2410(9) -0.0302(8) 0.037(3) Uani 1 1 d . . .
H13A H 0.0891 0.2379 -0.1064 0.044 Uiso 1 1 calc R . .
C3 C 0.1453(8) 0.5722(8) 0.3580(8) 0.028(2) Uani 1 1 d . . .
H3A H 0.1325 0.6247 0.3078 0.033 Uiso 1 1 calc R . .
C16 C 0.3497(7) 0.4278(7) 0.1731(7) 0.025(2) Uani 1 1 d . . .
H16A H 0.3497 0.4309 0.2536 0.030 Uiso 1 1 calc R . .
C18 C 0.4541(8) 0.3936(9) 0.1453(8) 0.034(2) Uani 1 1 d . . .
H18A H 0.4421 0.3155 0.1712 0.051 Uiso 1 1 calc R . .
H18B H 0.5283 0.4502 0.1802 0.051 Uiso 1 1 calc R . .
H18C H 0.4584 0.3932 0.0668 0.051 Uiso 1 1 calc R . .
C22 C 0.5379(8) 0.2267(8) 0.4218(8) 0.031(2) Uani 1 1 d . . .
H22A H 0.6137 0.2229 0.4385 0.037 Uiso 1 1 calc R . .
C8 C 0.2969(9) 0.3937(8) 0.6806(8) 0.035(2) Uani 1 1 d . . .
H8A H 0.3017 0.3370 0.7337 0.053 Uiso 1 1 calc R . .
H8B H 0.2821 0.4572 0.7170 0.053 Uiso 1 1 calc R . .
H8C H 0.3718 0.4256 0.6466 0.053 Uiso 1 1 calc R . .
C17 C 0.3677(9) 0.5507(8) 0.1335(9) 0.042(3) Uani 1 1 d . . .
H17A H 0.4444 0.6065 0.1646 0.062 Uiso 1 1 calc R . .
H17B H 0.3041 0.5740 0.1563 0.062 Uiso 1 1 calc R . .
H17C H 0.3662 0.5499 0.0545 0.062 Uiso 1 1 calc R . .
C28 C 0.3523(9) 0.0526(9) 0.7794(8) 0.038(2) Uani 1 1 d . . .
H28A H 0.3090 -0.0293 0.7503 0.045 Uiso 1 1 calc R . .
C29 C 0.8194(9) 0.3123(9) 0.1052(9) 0.043(3) Uani 1 1 d . . .
H29A H 0.8639 0.2697 0.1457 0.052 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'
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'
P P 0.1023 0.0942 '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
P1 Pd1 Cl2 89.83(8) . . ?
P1 Pd1 Cl1 94.52(8) . . ?
Cl2 Pd1 Cl1 172.94(8) . . ?
P1 Pd1 Cl1 177.50(9) . 2_556 ?
Cl2 Pd1 Cl1 90.19(8) . 2_556 ?
Cl1 Pd1 Cl1 85.22(8) . 2_556 ?
Pd1 Cl1 Pd1 94.78(7) . 2_556 ?
C19 P1 C10 105.7(4) . . ?
C19 P1 C1 109.9(4) . . ?
C10 P1 C1 106.7(4) . . ?
C19 P1 Pd1 114.4(3) . . ?
C10 P1 Pd1 113.8(3) . . ?
C1 P1 Pd1 106.1(3) . . ?
C20 C19 C24 118.9(7) . . ?
C20 C19 P1 119.3(6) . . ?
C24 C19 P1 121.8(6) . . ?
C21 C20 C19 121.7(8) . . ?
C21 C20 H20A 119.2 . . ?
C19 C20 H20A 119.2 . . ?
C14 C15 C10 118.9(8) . . ?
C14 C15 C16 117.3(8) . . ?
C10 C15 C16 123.7(8) . . ?
C2 C1 C6 119.3(7) . . ?
C2 C1 P1 118.5(6) . . ?
C6 C1 P1 121.6(6) . . ?
C22 C23 C24 122.0(8) . . ?
C22 C23 H23A 119.0 . . ?
C24 C23 H23A 119.0 . . ?
C5 C6 C1 116.6(8) . . ?
C5 C6 C7 118.5(7) . . ?
C1 C6 C7 124.8(7) . . ?
C8 C7 C9 110.8(7) . . ?
C8 C7 C6 113.7(7) . . ?
C9 C7 C6 109.7(7) . . ?
C8 C7 H7A 107.5 . . ?
C9 C7 H7A 107.5 . . ?
C6 C7 H7A 107.5 . . ?
C23 C24 C19 118.0(8) . . ?
C23 C24 C25 117.4(7) . . ?
C19 C24 C25 124.5(7) . . ?
C15 C10 C11 119.1(8) . . ?
C15 C10 P1 125.3(7) . . ?
C11 C10 P1 115.6(6) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C11 C10 120.8(8) . . ?
C12 C11 H11A 119.6 . . ?
C10 C11 H11A 119.6 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C3 C2 C1 122.1(8) . . ?
C3 C2 H2A 119.0 . . ?
C1 C2 H2A 119.0 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C26 C25 C24 110.5(7) . . ?
C26 C25 C27 110.7(7) . . ?
C24 C25 C27 112.8(8) . . ?
C26 C25 H25A 107.5 . . ?
C24 C25 H25A 107.5 . . ?
C27 C25 H25A 107.5 . . ?
C4 C5 C6 122.8(9) . . ?
C4 C5 H5A 118.6 . . ?
C6 C5 H5A 118.6 . . ?
C22 C21 C20 119.4(8) . . ?
C22 C21 H21A 120.3 . . ?
C20 C21 H21A 120.3 . . ?
C3 C4 C5 120.6(8) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C13 C14 C15 120.8(9) . . ?
C13 C14 H14A 119.6 . . ?
C15 C14 H14A 119.6 . . ?
C11 C12 C13 119.4(9) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C14 C13 C12 121.0(9) . . ?
C14 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
C4 C3 C2 118.6(9) . . ?
C4 C3 H3A 120.7 . . ?
C2 C3 H3A 120.7 . . ?
C15 C16 C17 113.3(8) . . ?
C15 C16 C18 110.1(7) . . ?
C17 C16 C18 110.1(7) . . ?
C15 C16 H16A 107.7 . . ?
C17 C16 H16A 107.7 . . ?
C18 C16 H16A 107.7 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C22 C23 119.9(8) . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Cl6 C28 Cl7 110.0(6) . . ?
Cl6 C28 Cl5 111.6(5) . . ?
Cl7 C28 Cl5 109.2(5) . . ?
Cl6 C28 H28A 108.7 . . ?
Cl7 C28 H28A 108.7 . . ?
Cl5 C28 H28A 108.7 . . ?
Cl12 C29 Cl9 111.0(6) . . ?
Cl12 C29 Cl8 111.8(6) . . ?
Cl9 C29 Cl8 109.1(6) . . ?
Cl12 C29 H29A 108.3 . . ?
Cl9 C29 H29A 108.3 . . ?
Cl8 C29 H29A 108.3 . . ?
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 2.244(2) . ?
Pd1 Cl2 2.300(2) . ?
Pd1 Cl1 2.319(2) . ?
Pd1 Cl1 2.403(2) 2_556 ?
Cl1 Pd1 2.403(2) 2_556 ?
P1 C19 1.826(8) . ?
P1 C10 1.827(9) . ?
P1 C1 1.838(8) . ?
Cl5 C28 1.765(9) . ?
Cl6 C28 1.737(10) . ?
Cl7 C28 1.744(11) . ?
Cl12 C29 1.740(11) . ?
Cl8 C29 1.747(11) . ?
Cl9 C29 1.744(11) . ?
C19 C20 1.392(11) . ?
C19 C24 1.426(11) . ?
C20 C21 1.391(12) . ?
C20 H20A 0.9500 . ?
C15 C14 1.394(11) . ?
C15 C10 1.404(12) . ?
C15 C16 1.527(12) . ?
C1 C2 1.388(11) . ?
C1 C6 1.437(11) . ?
C23 C22 1.383(12) . ?
C23 C24 1.398(11) . ?
C23 H23A 0.9500 . ?
C6 C5 1.386(11) . ?
C6 C7 1.535(12) . ?
C7 C8 1.498(12) . ?
C7 C9 1.530(11) . ?
C7 H7A 1.0000 . ?
C24 C25 1.533(12) . ?
C10 C11 1.419(12) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.363(12) . ?
C11 H11A 0.9500 . ?
C27 C25 1.557(12) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C2 C3 1.386(11) . ?
C2 H2A 0.9500 . ?
C26 C25 1.529(12) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 1.0000 . ?
C5 C4 1.381(13) . ?
C5 H5A 0.9500 . ?
C21 C22 1.382(12) . ?
C21 H21A 0.9500 . ?
C4 C3 1.371(13) . ?
C4 H4A 0.9500 . ?
C14 C13 1.367(14) . ?
C14 H14A 0.9500 . ?
C12 C13 1.395(14) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C3 H3A 0.9500 . ?
C16 C17 1.539(12) . ?
C16 C18 1.542(11) . ?
C16 H16A 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C22 H22A 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C28 H28A 1.0000 . ?
C29 H29A 1.0000 . ?
