#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:05:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179825 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/21/7012150.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_7012150
loop_
_publ_author_name
'Sub Kim, Jang'
'Sen, Ayusman'
'Guzei, Ilia A.'
'Liable-Sands, Louise M.'
'Rheingold, Arnold L.'
_publ_section_title
;
 Synthesis and reactivity of bimetallic palladium(ii) methyl complexes
 with new functional phosphine ligands
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4726
_journal_paper_doi               10.1039/b208060p
_journal_year                    2002
_chemical_formula_sum            'C26 H40 Cl2 O2 P2 Pd2'
_chemical_formula_weight         730.22
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 108.695(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.078(2)
_cell_length_b                   11.830(2)
_cell_length_c                   11.619(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1442.4(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6514
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.565
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.587
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.380
_refine_ls_goodness_of_fit_obs   1.478
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.421
_refine_ls_restrained_S_obs      1.478
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_obs          0.0339
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0884
_refine_ls_wR_factor_obs         0.0846
_reflns_number_observed          2821
_reflns_number_total             3309
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b208060p.txt
_cod_data_source_block           sen05
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012150
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd1 Pd 0.53816(2) -0.44418(2) 0.88930(2) 0.02369(9) Uani 1 d . .
Cl1 Cl 0.70884(8) -0.42255(9) 0.82331(9) 0.0478(3) Uani 1 d . .
P1 P 0.41227(7) -0.36087(7) 0.72796(7) 0.0245(2) Uani 1 d . .
O1 O 0.3817(2) -0.4656(2) 0.9408(2) 0.0313(5) Uani 1 d . .
C2 C 0.2716(3) -0.4200(3) 0.8717(3) 0.0254(6) Uani 1 d . .
C3 C 0.1635(3) -0.4218(3) 0.9078(3) 0.0305(7) Uani 1 d . .
H3A H 0.1669(3) -0.4554(3) 0.9812(3) 0.037 Uiso 1 calc R .
C4 C 0.0507(3) -0.3740(3) 0.8350(3) 0.0302(7) Uani 1 d . .
H4A H -0.0207(3) -0.3764(3) 0.8606(3) 0.036 Uiso 1 calc R .
C5 C 0.0412(3) -0.3223(3) 0.7242(3) 0.0287(7) Uani 1 d . .
C6 C 0.1492(3) -0.3191(3) 0.6899(3) 0.0300(7) Uani 1 d . .
H6A H 0.1459(3) -0.2836(3) 0.6175(3) 0.036 Uiso 1 calc R .
C7 C 0.2645(3) -0.3683(3) 0.7617(3) 0.0257(6) Uani 1 d . .
C8 C -0.0831(3) -0.2716(3) 0.6464(3) 0.0413(8) Uani 1 d . .
H8A H -0.1468(3) -0.2821(3) 0.6853(3) 0.062 Uiso 1 calc R .
H8B H -0.1099(3) -0.3081(3) 0.5685(3) 0.062 Uiso 1 calc R .
H8C H -0.0717(3) -0.1922(3) 0.6359(3) 0.062 Uiso 1 calc R .
C9 C 0.4373(3) -0.2112(3) 0.7057(3) 0.0311(7) Uani 1 d . .
H9A H 0.3604(3) -0.1831(3) 0.6438(3) 0.037 Uiso 1 calc R .
C10 C 0.4492(4) -0.1480(3) 0.8230(3) 0.0442(9) Uani 1 d . .
H10A H 0.3771(4) -0.1651(3) 0.8487(3) 0.066 Uiso 1 calc R .
H10B H 0.4520(4) -0.0682(3) 0.8094(3) 0.066 Uiso 1 calc R .
H10C H 0.5260(4) -0.1709(3) 0.8848(3) 0.066 Uiso 1 calc R .
C11 C 0.5496(4) -0.1872(3) 0.6601(4) 0.0494(10) Uani 1 d . .
H11A H 0.5388(4) -0.2284(3) 0.5863(4) 0.074 Uiso 1 calc R .
H11B H 0.6273(4) -0.2105(3) 0.7204(4) 0.074 Uiso 1 calc R .
H11C H 0.5534(4) -0.1078(3) 0.6449(4) 0.074 Uiso 1 calc R .
C12 C 0.4017(3) -0.4375(3) 0.5893(3) 0.0326(7) Uani 1 d . .
H12A H 0.4858(3) -0.4327(3) 0.5786(3) 0.039 Uiso 1 calc R .
C13 C 0.3763(5) -0.5622(3) 0.6045(4) 0.0598(13) Uani 1 d . .
H13A H 0.4377(5) -0.5904(3) 0.6773(4) 0.090 Uiso 1 calc R .
H13B H 0.3830(5) -0.6037(3) 0.5358(4) 0.090 Uiso 1 calc R .
H13C H 0.2921(5) -0.5712(3) 0.6098(4) 0.090 Uiso 1 calc R .
C14 C 0.3074(4) -0.3900(5) 0.4762(3) 0.0701(15) Uani 1 d . .
H14A H 0.3255(4) -0.3115(5) 0.4688(3) 0.105 Uiso 1 calc R .
H14B H 0.2228(4) -0.3978(5) 0.4807(3) 0.105 Uiso 1 calc R .
H14C H 0.3136(4) -0.4304(5) 0.4066(3) 0.105 Uiso 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'
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'
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'
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
O1 Pd1 O1 78.96(9) . 3_647 ?
O1 Pd1 P1 86.47(6) . . ?
O1 Pd1 P1 165.39(6) 3_647 . ?
O1 Pd1 Cl1 177.54(7) . . ?
O1 Pd1 Cl1 102.75(6) 3_647 . ?
P1 Pd1 Cl1 91.78(3) . . ?
O1 Pd1 Pd1 41.12(6) . 3_647 ?
O1 Pd1 Pd1 37.84(6) 3_647 3_647 ?
P1 Pd1 Pd1 127.58(3) . 3_647 ?
Cl1 Pd1 Pd1 140.56(3) . 3_647 ?
C7 P1 C12 111.27(15) . . ?
C7 P1 C9 105.56(14) . . ?
C12 P1 C9 109.13(15) . . ?
C7 P1 Pd1 99.56(10) . . ?
C12 P1 Pd1 112.21(11) . . ?
C9 P1 Pd1 118.46(11) . . ?
C2 O1 Pd1 118.3(2) . . ?
C2 O1 Pd1 140.5(2) . 3_647 ?
Pd1 O1 Pd1 101.04(9) . 3_647 ?
O1 C2 C3 121.3(3) . . ?
O1 C2 C7 119.9(3) . . ?
C3 C2 C7 118.8(3) . . ?
C4 C3 C2 120.4(3) . . ?
C3 C4 C5 121.9(3) . . ?
C6 C5 C4 117.5(3) . . ?
C6 C5 C8 121.8(3) . . ?
C4 C5 C8 120.7(3) . . ?
C5 C6 C7 121.6(3) . . ?
C2 C7 C6 119.9(3) . . ?
C2 C7 P1 115.5(2) . . ?
C6 C7 P1 124.4(2) . . ?
C10 C9 C11 111.9(3) . . ?
C10 C9 P1 108.8(2) . . ?
C11 C9 P1 114.0(2) . . ?
C14 C12 C13 111.2(4) . . ?
C14 C12 P1 114.7(3) . . ?
C13 C12 P1 110.0(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 O1 2.022(2) . ?
Pd1 O1 2.168(2) 3_647 ?
Pd1 P1 2.1805(8) . ?
Pd1 Cl1 2.2711(9) . ?
Pd1 Pd1 3.2357(6) 3_647 ?
P1 C7 1.804(3) . ?
P1 C12 1.819(3) . ?
P1 C9 1.824(3) . ?
O1 C2 1.340(4) . ?
O1 Pd1 2.168(2) 3_647 ?
C2 C3 1.391(4) . ?
C2 C7 1.396(4) . ?
C3 C4 1.385(4) . ?
C4 C5 1.399(4) . ?
C5 C6 1.378(4) . ?
C5 C8 1.509(4) . ?
C6 C7 1.408(4) . ?
C9 C10 1.522(5) . ?
C9 C11 1.527(4) . ?
C12 C14 1.502(5) . ?
C12 C13 1.523(5) . ?
