#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:10:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179955 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/50/7025074.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_7025074
loop_
_publ_author_name
'Coleman, Dennis'
'Edwards, Peter G.'
'Kariuki, Benson M.'
'Newman, Paul D.'
_publ_section_title
;
 Coordination chemistry of cis,cis and trans,trans
 1,1'-[1,2-phenylenebis(methylene)]bis(2,2,3,4,4-pentamethylphosphetane).
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3842
_journal_page_last               3850
_journal_paper_doi               10.1039/b924982f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C25 H42 Cl4 P2 Pd'
_chemical_formula_sum            'C25 H42 Cl4 P2 Pd'
_chemical_formula_weight         652.73
_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                109.6672(8)
_cell_angle_beta                 93.1967(8)
_cell_angle_gamma                95.8861(10)
_cell_formula_units_Z            2
_cell_length_a                   8.78660(10)
_cell_length_b                   10.8661(2)
_cell_length_c                   15.9424(3)
_cell_measurement_reflns_used    5559
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.98
_cell_volume                     1419.13(4)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXs-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD 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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26820
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  0.7609
_exptl_absorpt_correction_T_min  0.7229
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Denzo/Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0348
_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)+(0.0390P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                5559
_reflns_number_total             6456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b924982f.txt
_cod_data_source_block           compound11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7025074
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_occupancy
Pd(1) pd -0.0008(1) 0.4473(1) 0.1914(1) 0.015(1) 1
P(1) p 0.2188(1) 0.3589(1) 0.1610(1) 0.014(1) 1
P(2) p 0.1254(1) 0.6381(1) 0.2898(1) 0.017(1) 1
Cl(1) cl -0.2288(1) 0.5193(1) 0.2545(1) 0.027(1) 1
Cl(2) cl -0.1523(1) 0.2721(1) 0.0774(1) 0.027(1) 1
C(1) c 0.2897(3) 0.3460(3) 0.0503(2) 0.018(1) 1
C(2) c 0.2050(3) 0.4165(3) -0.0025(2) 0.024(1) 1
C(3) c 0.4639(3) 0.3815(3) 0.0546(2) 0.022(1) 1
C(4) c 0.2340(3) 0.1941(3) 0.0195(2) 0.020(1) 1
C(5) c 0.3254(4) 0.1035(3) -0.0486(2) 0.031(1) 1
C(6) c 0.2290(3) 0.1757(3) 0.1128(2) 0.019(1) 1
C(7) c 0.0962(3) 0.0775(3) 0.1185(2) 0.025(1) 1
C(8) c 0.3779(3) 0.1358(3) 0.1449(2) 0.025(1) 1
C(9) c 0.2976(3) 0.7563(3) 0.2836(2) 0.025(1) 1
C(10) c 0.4504(3) 0.7661(3) 0.3378(2) 0.034(1) 1
C(11) c 0.3278(4) 0.7428(3) 0.1873(2) 0.033(1) 1
C(12) c 0.2036(4) 0.8710(3) 0.3270(2) 0.039(1) 1
C(13) c 0.2629(6) 0.9730(5) 0.4151(3) 0.039(1) 0.65
C(13') c 0.2327(10) 1.0029(7) 0.3206(7) 0.037(2) 0.35
C(14) c 0.0382(3) 0.7955(3) 0.3136(2) 0.024(1) 1
C(15) c -0.0562(4) 0.8368(3) 0.3937(2) 0.031(1) 1
C(16) c -0.0560(4) 0.8018(3) 0.2317(2) 0.031(1) 1
C(17) c 0.3678(3) 0.4402(3) 0.2541(2) 0.016(1) 1
C(18) c 0.1557(3) 0.6154(3) 0.3971(2) 0.023(1) 1
C(19) c 0.3360(3) 0.4298(3) 0.3445(2) 0.018(1) 1
C(20) c 0.4130(3) 0.3388(3) 0.3695(2) 0.023(1) 1
C(21) c 0.4005(4) 0.3216(3) 0.4507(2) 0.029(1) 1
C(22) c 0.3093(4) 0.3956(3) 0.5107(2) 0.030(1) 1
C(23) c 0.2326(3) 0.4863(3) 0.4879(2) 0.026(1) 1
C(24) c 0.2438(3) 0.5061(3) 0.4058(2) 0.018(1) 1
Cl(3) cl -0.3289(1) 0.0833(1) 0.3169(1) 0.047(1) 1
Cl(4) cl -0.0287(1) 0.2382(1) 0.3495(1) 0.059(1) 1
C(25) c -0.2054(4) 0.1936(4) 0.2841(2) 0.039(1) 1
H(2A) h 0.2326 0.5120 0.0260 0.036 1
H(2B) h 0.0939 0.3940 -0.0035 0.036 1
H(2C h 0.2342 0.3888 -0.0639 0.036 1
H(3A h 0.4916 0.4765 0.0857 0.033 1
H(3B h 0.4954 0.3575 -0.0063 0.033 1
H(3C h 0.5163 0.3332 0.0871 0.033 1
H(4) h 0.1255 0.1793 -0.0080 0.024 1
H(5A h 0.3131 0.1194 -0.1054 0.046 1
H(5B h 0.2873 0.0114 -0.0580 0.046 1
H(5C h 0.4344 0.1216 -0.0261 0.046 1
H(7A h 0.0911 0.0834 0.1810 0.037 1
H(7B h 0.1128 -0.0120 0.0823 0.037 1
H(7C) h -0.0005 0.0981 0.0960 0.037 1
H(8A h 0.4655 0.1981 0.1431 0.038 1
H(8B h 0.3909 0.0469 0.1057 0.038 1
H(8C h 0.3725 0.1368 0.2064 0.038 1
H(10A h 0.5062 0.8548 0.3528 0.051 1
H(10B h 0.5123 0.7010 0.3024 0.051 1
H(10C h 0.4305 0.7490 0.3930 0.051 1
H(11A h 0.3953 0.8205 0.1875 0.049 1
H(11B h 0.2301 0.7356 0.1521 0.049 1
H(11C h 0.3771 0.6636 0.1607 0.049 1
H(13A h 0.3654 1.0141 0.4108 0.058 0.65
H(13B h 0.2692 0.9315 0.4609 0.058 0.65
H(13C h 0.1932 1.0403 0.4316 0.058 0.65
H(13D h 0.1732 1.0629 0.3625 0.056 0.35
H(13E h 0.2019 0.9982 0.2595 0.056 0.35
H(13F h 0.3425 1.0356 0.3356 0.056 0.35
H(15A h 0.0024 0.8329 0.4467 0.046 1
H(15B) h -0.1526 0.7769 0.3811 0.046 1
H(15C) h -0.0790 0.9270 0.4048 0.046 1
H(16A) h -0.0752 0.8928 0.2422 0.046 1
H(16B) h -0.1542 0.7450 0.2214 0.046 1
H(16C h 0.0013 0.7717 0.1790 0.046 1
H(17A h 0.4644 0.4030 0.2372 0.019 1
H(17B h 0.3855 0.5349 0.2614 0.019 1
H(18A h 0.2093 0.6996 0.4399 0.027 1
H(18B h 0.0531 0.6019 0.4177 0.027 1
H(20 h 0.4762 0.2871 0.3289 0.028 1
H(21 h 0.4546 0.2591 0.4654 0.035 1
H(22 h 0.2994 0.3844 0.5668 0.036 1
H(23 h 0.1699 0.5371 0.5293 0.031 1
H(25A) h -0.1882 0.1519 0.2204 0.047 1
H(25B) h -0.2547 0.2737 0.2899 0.047 1
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'
Pd Pd -0.9988 1.0072 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
P(1) Pd(1) P(2) 92.36(2)
P(1) Pd(1) Cl(2) 93.79(2)
P(2) Pd(1) Cl(2) 170.03(3)
P(1) Pd(1) Cl(1) 165.17(3)
P(2) Pd(1) Cl(1) 86.67(2)
Cl(2) Pd(1) Cl(1) 89.37(2)
C(17) P(1) C(1) 112.14(12)
C(17) P(1) C(6) 111.20(12)
C(1) P(1) C(6) 79.64(12)
C(17) P(1) Pd(1) 110.00(9)
C(1) P(1) Pd(1) 116.79(9)
C(6) P(1) Pd(1) 123.95(9)
C(18) P(2) C(14) 105.79(13)
C(18) P(2) C(9) 106.21(13)
C(14) P(2) C(9) 78.85(13)
C(18) P(2) Pd(1) 107.62(10)
C(14) P(2) Pd(1) 120.19(9)
C(9) P(2) Pd(1) 133.51(10)
C(2) C(1) C(3) 110.7(2)
C(2) C(1) C(4) 113.5(2)
C(3) C(1) C(4) 114.4(2)
C(2) C(1) P(1) 115.47(19)
C(3) C(1) P(1) 113.86(18)
C(4) C(1) P(1) 87.18(15)
C(5) C(4) C(6) 117.1(2)
C(5) C(4) C(1) 116.7(2)
C(6) C(4) C(1) 100.2(2)
C(7) C(6) C(8) 107.4(2)
C(7) C(6) C(4) 114.9(2)
C(8) C(6) C(4) 113.5(2)
C(7) C(6) P(1) 120.27(19)
C(8) C(6) P(1) 113.18(19)
C(4) C(6) P(1) 86.56(16)
C(10) C(9) C(11) 109.2(3)
C(10) C(9) C(12) 113.3(3)
C(11) C(9) C(12) 112.6(3)
C(10) C(9) P(2) 119.8(2)
C(11) C(9) P(2) 112.9(2)
C(12) C(9) P(2) 87.63(19)
C(13') C(12) C(13) 68.1(5)
C(13') C(12) C(9) 124.4(5)
C(13) C(12) C(9) 119.7(3)
C(13') C(12) C(14) 122.2(4)
C(13) C(12) C(14) 120.2(3)
C(9) C(12) C(14) 101.3(2)
C(15) C(14) C(16) 108.5(2)
C(15) C(14) C(12) 115.9(3)
C(16) C(14) C(12) 112.0(3)
C(15) C(14) P(2) 118.1(2)
C(16) C(14) P(2) 112.7(2)
C(12) C(14) P(2) 88.69(18)
C(19) C(17) P(1) 116.82(18)
C(24) C(18) P(2) 120.64(19)
C(20) C(19) C(24) 117.8(2)
C(20) C(19) C(17) 115.7(2)
C(24) C(19) C(17) 126.4(2)
C(21) C(20) C(19) 122.5(3)
C(20) C(21) C(22) 119.7(3)
C(21) C(22) C(23) 119.0(3)
C(22) C(23) C(24) 122.5(3)
C(23) C(24) C(19) 118.5(3)
C(23) C(24) C(18) 113.3(2)
C(19) C(24) C(18) 128.1(2)
Cl(4) C(25) Cl(3) 111.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd(1) P(1) 2.2474(7)
Pd(1) P(2) 2.2650(7)
Pd(1) Cl(2) 2.3628(7)
Pd(1) Cl(1) 2.3781(7)
P(1) C(17) 1.833(3)
P(1) C(1) 1.870(3)
P(1) C(6) 1.891(3)
P(2) C(18) 1.817(3)
P(2) C(14) 1.876(3)
P(2) C(9) 1.912(3)
C(1) C(2) 1.527(4)
C(1) C(3) 1.531(4)
C(1) C(4) 1.572(4)
C(4) C(5) 1.527(4)
C(4) C(6) 1.568(4)
C(6) C(7) 1.526(4)
C(6) C(8) 1.534(4)
C(9) C(10) 1.530(4)
C(9) C(11) 1.533(4)
C(9) C(12) 1.553(4)
C(12) C(13') 1.468(5)
C(12) C(13) 1.491(4)
C(12) C(14) 1.560(4)
C(14) C(15) 1.526(4)
C(14) C(16) 1.533(4)
C(17) C(19) 1.521(4)
C(18) C(24) 1.522(4)
C(19) C(20) 1.403(4)
C(19) C(24) 1.407(4)
C(20) C(21) 1.377(4)
C(21) C(22) 1.380(5)
C(22) C(23) 1.380(4)
C(23) C(24) 1.403(4)
Cl(3) C(25) 1.762(3)
Cl(4) C(25) 1.749(4)
