#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180128 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/26/7102654.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_7102654
loop_
_publ_author_name
'Christmann, Ute'
'Vilar, Ramón'
'White, Andrew J P'
'Williams, David J'
_publ_section_title
;
 Synthesis of two novel dinuclear palladium(I) complexes and studies of
 their catalytic activity in amination reactions.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1294
_journal_page_last               1295
_journal_paper_doi               10.1039/b402283a
_journal_year                    2004
_chemical_formula_sum            'C20 H27 Cl2 P Pd2'
_chemical_formula_weight         582.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.823(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.276(2)
_cell_length_b                   15.907(9)
_cell_length_c                   15.125(4)
_cell_measurement_reflns_used    72
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      11.15
_cell_volume                     2176.1(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1297
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3444
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         4.09
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.282
_exptl_absorpt_correction_T_max  0.5885
_exptl_absorpt_correction_T_min  0.1199
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Very dark brown'
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.00035(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0590
_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)+(0.1034P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                2556
_reflns_number_total             3225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402283a.txt
_cod_data_source_block           Compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7102654
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.59803(6) 0.66649(4) 0.38804(4) 0.0319(3) Uani 1 1 d .
Pd2 Pd 0.44175(7) 0.54309(4) 0.31655(5) 0.0390(3) Uani 1 1 d .
Cl1 Cl 0.6995(3) 0.56352(18) 0.3091(2) 0.0555(7) Uani 1 1 d .
Cl2 Cl 0.3307(3) 0.41836(16) 0.24985(19) 0.0488(6) Uani 1 1 d .
P P 0.7485(2) 0.77321(14) 0.45373(15) 0.0288(5) Uani 1 1 d .
C1 C 0.4432(9) 0.7142(6) 0.4610(6) 0.0293(18) Uani 1 1 d .
C2 C 0.3587(8) 0.7257(6) 0.3703(6) 0.0335(19) Uani 1 1 d .
H2A H 0.3620 0.7767 0.3408 0.040 Uiso 1 1 calc R
C3 C 0.2715(11) 0.6601(7) 0.3263(7) 0.045(2) Uani 1 1 d .
H3A H 0.2204 0.6676 0.2666 0.054 Uiso 1 1 calc R
C4 C 0.2584(9) 0.5845(6) 0.3685(8) 0.045(2) Uani 1 1 d .
H4A H 0.1960 0.5426 0.3389 0.054 Uiso 1 1 calc R
C5 C 0.3426(11) 0.5720(7) 0.4583(9) 0.049(3) Uani 1 1 d .
H5A H 0.3363 0.5206 0.4866 0.059 Uiso 1 1 calc R
C6 C 0.4343(10) 0.6343(6) 0.5053(7) 0.042(2) Uani 1 1 d .
H6A H 0.4887 0.6248 0.5639 0.051 Uiso 1 1 calc R
C7 C 0.4971(9) 0.7897(6) 0.5203(6) 0.0329(19) Uani 1 1 d .
C8 C 0.4071(10) 0.8226(7) 0.5719(8) 0.048(3) Uani 1 1 d .
H8A H 0.3182 0.7962 0.5733 0.058 Uiso 1 1 calc R
C9 C 0.4471(13) 0.8947(8) 0.6219(9) 0.056(3) Uani 1 1 d .
H9A H 0.3858 0.9156 0.6578 0.067 Uiso 1 1 calc R
C10 C 0.5748(11) 0.9358(7) 0.6196(8) 0.047(2) Uani 1 1 d .
H10A H 0.5982 0.9860 0.6510 0.057 Uiso 1 1 calc R
C11 C 0.6696(10) 0.9021(7) 0.5702(7) 0.043(2) Uani 1 1 d .
H11A H 0.7589 0.9289 0.5707 0.051 Uiso 1 1 calc R
C12 C 0.6338(9) 0.8284(6) 0.5194(6) 0.0306(18) Uani 1 1 d .
C13 C 0.9135(10) 0.7349(8) 0.5376(8) 0.047(3) Uani 1 1 d .
C14 C 0.8532(16) 0.6677(10) 0.5926(11) 0.081(5) Uani 1 1 d .
H14A H 0.9331 0.6443 0.6372 0.122 Uiso 1 1 calc R
H14B H 0.8061 0.6240 0.5527 0.122 Uiso 1 1 calc R
H14C H 0.7825 0.6928 0.6224 0.122 Uiso 1 1 calc R
C15 C 0.9917(13) 0.7987(10) 0.6058(8) 0.063(3) Uani 1 1 d .
H15A H 1.0754 0.7727 0.6450 0.095 Uiso 1 1 calc R
H15B H 0.9248 0.8188 0.6412 0.095 Uiso 1 1 calc R
H15C H 1.0245 0.8449 0.5745 0.095 Uiso 1 1 calc R
C16 C 1.0211(15) 0.6934(12) 0.4897(12) 0.085(5) Uani 1 1 d .
H16A H 1.1055 0.6740 0.5338 0.127 Uiso 1 1 calc R
H16B H 1.0523 0.7333 0.4501 0.127 Uiso 1 1 calc R
H16C H 0.9739 0.6466 0.4549 0.127 Uiso 1 1 calc R
C17 C 0.7959(11) 0.8481(7) 0.3690(7) 0.044(2) Uani 1 1 d .
C18 C 0.9003(16) 0.9203(10) 0.4068(10) 0.072(4) Uani 1 1 d .
H18A H 0.9173 0.9543 0.3576 0.108 Uiso 1 1 calc R
H18B H 0.9926 0.8978 0.4399 0.108 Uiso 1 1 calc R
H18C H 0.8565 0.9540 0.4464 0.108 Uiso 1 1 calc R
C19 C 0.8562(15) 0.7995(9) 0.2969(9) 0.064(3) Uani 1 1 d .
H19A H 0.8806 0.8383 0.2539 0.096 Uiso 1 1 calc R
H19B H 0.7825 0.7608 0.2662 0.096 Uiso 1 1 calc R
H19C H 0.9433 0.7689 0.3258 0.096 Uiso 1 1 calc R
C20 C 0.6465(15) 0.8844(9) 0.3198(9) 0.063(3) Uani 1 1 d .
H20A H 0.6615 0.9237 0.2745 0.094 Uiso 1 1 calc R
H20B H 0.6010 0.9126 0.3627 0.094 Uiso 1 1 calc R
H20C H 0.5835 0.8397 0.2915 0.094 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 0.0181 0.0091 '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 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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
C1 Pd1 P 85.8(2)
C1 Pd1 Cl1 154.7(2)
P Pd1 Cl1 117.78(8)
C1 Pd1 C2 36.6(3)
P Pd1 C2 102.7(2)
Cl1 Pd1 C2 133.7(2)
C1 Pd1 Pd2 96.3(2)
P Pd1 Pd2 177.19(6)
Cl1 Pd1 Pd2 59.86(7)
C2 Pd1 Pd2 80.0(2)
C1 Pd1 C6 33.4(3)
P Pd1 C6 103.9(2)
Cl1 Pd1 C6 124.4(2)
C2 Pd1 C6 59.2(3)
Pd2 Pd1 C6 77.0(2)
C4 Pd2 Cl2 96.3(3)
C4 Pd2 Cl1 147.9(3)
Cl2 Pd2 Cl1 115.58(9)
C4 Pd2 C3 33.9(4)
Cl2 Pd2 C3 115.9(3)
Cl1 Pd2 C3 123.3(3)
C4 Pd2 Pd1 91.8(2)
Cl2 Pd2 Pd1 171.33(7)
Cl1 Pd2 Pd1 56.17(6)
C3 Pd2 Pd1 72.7(2)
C4 Pd2 C5 33.8(4)
Cl2 Pd2 C5 107.8(2)
Cl1 Pd2 C5 123.6(2)
C3 Pd2 C5 57.3(4)
Pd1 Pd2 C5 77.3(2)
Pd1 Cl1 Pd2 63.96(6)
C12 P C13 106.0(4)
C12 P C17 108.6(5)
C13 P C17 113.1(5)
C12 P Pd1 102.7(3)
C13 P Pd1 112.6(4)
C17 P Pd1 112.9(3)
C2 C1 C6 118.7(8)
C2 C1 C7 120.3(8)
C6 C1 C7 117.9(8)
C2 C1 Pd1 80.7(5)
C6 C1 Pd1 92.3(6)
C7 C1 Pd1 114.6(6)
C3 C2 C1 119.8(9)
C3 C2 Pd1 100.7(7)
C1 C2 Pd1 62.7(4)
C4 C3 C2 122.2(10)
C4 C3 Pd2 59.5(6)
C2 C3 Pd2 106.3(6)
C3 C4 C5 118.5(9)
C3 C4 Pd2 86.5(6)
C5 C4 Pd2 89.7(6)
C6 C5 C4 122.1(10)
C6 C5 Pd2 105.3(7)
C4 C5 Pd2 56.5(6)
C5 C6 C1 118.6(9)
C5 C6 Pd1 100.0(7)
C1 C6 Pd1 54.3(5)
C8 C7 C12 120.1(9)
C8 C7 C1 118.5(8)
C12 C7 C1 121.3(8)
C7 C8 C9 120.5(10)
C10 C9 C8 121.0(10)
C9 C10 C11 119.4(10)
C10 C11 C12 121.3(9)
C11 C12 C7 117.7(8)
C11 C12 P 127.1(7)
C7 C12 P 115.2(7)
C16 C13 C15 110.6(10)
C16 C13 C14 108.3(13)
C15 C13 C14 105.9(11)
C16 C13 P 110.4(9)
C15 C13 P 116.3(9)
C14 C13 P 104.7(7)
C18 C17 C20 109.2(11)
C18 C17 C19 110.0(10)
C20 C17 C19 106.1(10)
C18 C17 P 116.6(8)
C20 C17 P 104.3(7)
C19 C17 P 110.0(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 C1 2.136(8)
Pd1 P 2.281(2)
Pd1 Cl1 2.344(3)
Pd1 C2 2.371(8)
Pd1 Pd2 2.5354(13)
Pd1 C6 2.628(11)
Pd2 C4 2.130(10)
Pd2 Cl2 2.357(3)
Pd2 Cl1 2.440(2)
Pd2 C3 2.466(10)
Pd2 C5 2.555(12)
P C12 1.832(9)
P C13 1.860(10)
P C17 1.873(11)
C1 C2 1.433(12)
C1 C6 1.447(14)
C1 C7 1.515(12)
C2 C3 1.395(14)
C3 C4 1.379(16)
C4 C5 1.423(17)
C5 C6 1.394(16)
C7 C8 1.368(14)
C7 C12 1.412(12)
C8 C9 1.379(16)
C9 C10 1.360(17)
C10 C11 1.382(16)
C11 C12 1.400(14)
C13 C16 1.508(17)
C13 C15 1.512(16)
C13 C14 1.536(18)
C17 C18 1.528(15)
C17 C20 1.533(16)
C17 C19 1.540(17)
