#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/38/4323884.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_4323884
loop_
_publ_author_name
'Kazushi Mashima'
'Mitsuhiro Tanaka'
'Kazuhide Tani'
'Hiroshi Nakano'
'Akira Nakamura'
_publ_section_title
;
 Dinuclear Pd(I)-Pd(I) and Pt(II)...Pt(II) Complexes Supported by
 Tridentate Pyphos Ligands (Pyphos = 6-(Diphenylphosphino)-2-pyridonate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5244
_journal_page_last               5248
_journal_paper_doi               10.1021/ic951658u
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C71 H58 Cl6 N4 O4 P4 Pd2'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Sat Jan 13 10:46:08 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 107.65(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   19.794(7)
_cell_length_b                   14.753(7)
_cell_length_c                   25.626(5)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    23.0
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      29.10
_cell_volume                     7131(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_diffrn_ambient_temperature      23.0
_diffrn_measurement_device       AFC5R
_diffrn_measurement_method       'omega scans with profile analysis'
_diffrn_orient_matrix_UB_11      -0.02968
_diffrn_orient_matrix_UB_12      -0.00146
_diffrn_orient_matrix_UB_13      -0.03928
_diffrn_orient_matrix_UB_21      0.04020
_diffrn_orient_matrix_UB_22      -0.02821
_diffrn_orient_matrix_UB_23      -0.01016
_diffrn_orient_matrix_UB_31      -0.01770
_diffrn_orient_matrix_UB_32      -0.06161
_diffrn_orient_matrix_UB_33      0.00558
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  4.39
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11162
_diffrn_reflns_theta_max         30.1130
_diffrn_standards_decay_%        -0.70
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 8.609
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       undefined
_exptl_crystal_F_000             3192.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         -0.65247
_refine_diff_density_min         1.06290
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.239
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         4760
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0577
_refine_ls_shift/esd_max         2.1772
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0804
_cod_data_source_file            ic951658u_1.cif
_cod_data_source_block           Pd2(pyphos)2(pyphosH)2
_cod_original_cell_volume        7131(4)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C71 H58 O4 N4 P4 Pd2 Cl6'
_cod_database_code               4323884
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2+x,1/2+y,   +z'
'   -x,   +y,1/2-z'
1/2-x,1/2+y,1/2-z
'   -x,   -y,   -z'
'1/2-x,1/2-y,   -z'
'   +x,   -y,1/2+z'
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_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_calc_flag
_atom_site_calc_attached_atom
Pd1 0.03233(3) 0.25590(5) 0.71226(3) 0.0298 Uij ? ?
P1 -0.0794(1) 0.2167(2) 0.6626(1) 0.0338 Uij ? ?
P2 0.0952(1) 0.2084(2) 0.6501(1) 0.0365 Uij ? ?
O1 -0.1287(4) 0.4164(5) 0.8002(3) 0.0562 Uij ? ?
O2 0.0861(6) 0.5121(6) 0.5688(4) 0.0929 Uij ? ?
N1 -0.1160(4) 0.3250(5) 0.7314(3) 0.0346 Uij ? ?
N2 0.0860(4) 0.3649(6) 0.5967(3) 0.0483 Uij ? ?
C1 -0.1496(5) 0.3938(7) 0.7490(4) 0.0419 Uij ? ?
C2 -0.2066(6) 0.4374(7) 0.7092(5) 0.0552 Uij ? ?
C3 -0.2280(6) 0.4124(9) 0.6567(5) 0.0603 Uij ? ?
C4 -0.1915(5) 0.3440(8) 0.6404(4) 0.0490 Uij ? ?
C5 -0.1367(5) 0.3031(6) 0.6773(4) 0.0353 Uij ? ?
C6 -0.1201(6) 0.1105(7) 0.6727(4) 0.0426 Uij ? ?
C7 -0.1930(6) 0.1035(8) 0.6608(5) 0.0566 Uij ? ?
C8 -0.2223(7) 0.0214(10) 0.6673(5) 0.0698 Uij ? ?
C9 -0.1790(9) -0.0524(10) 0.6858(6) 0.0823 Uij ? ?
C10 -0.1071(9) -0.0484(9) 0.6967(6) 0.0865 Uij ? ?
C11 -0.0761(6) 0.0354(7) 0.6905(5) 0.0585 Uij ? ?
C12 -0.1026(5) 0.2272(6) 0.5886(4) 0.0424 Uij ? ?
C13 -0.0842(5) 0.3062(7) 0.5673(4) 0.0487 Uij ? ?
C14 -0.1044(7) 0.3176(10) 0.5102(6) 0.0732 Uij ? ?
C15 -0.1376(8) 0.251(1) 0.4741(5) 0.0897 Uij ? ?
C16 -0.1540(8) 0.172(1) 0.4952(5) 0.0999 Uij ? ?
C17 -0.1383(7) 0.1595(9) 0.5531(5) 0.0695 Uij ? ?
C21 0.0811(6) 0.4309(9) 0.5567(5) 0.0639 Uij ? ?
C22 0.0693(7) 0.394(1) 0.5018(6) 0.0755 Uij ? ?
C23 0.0688(8) 0.304(1) 0.4927(5) 0.0801 Uij ? ?
C24 0.0758(6) 0.2409(8) 0.5365(4) 0.0633 Uij ? ?
C25 0.0837(5) 0.2731(7) 0.5875(4) 0.0427 Uij ? ?
C26 0.1929(5) 0.2043(7) 0.6743(4) 0.0426 Uij ? ?
C27 0.2273(6) 0.2043(8) 0.7299(5) 0.0588 Uij ? ?
C28 0.3023(6) 0.1994(9) 0.7484(5) 0.0744 Uij ? ?
C29 0.3392(6) 0.1928(9) 0.7110(6) 0.0672 Uij ? ?
C30 0.3040(7) 0.189(1) 0.6574(5) 0.0760 Uij ? ?
C31 0.2318(6) 0.1949(9) 0.6384(5) 0.0660 Uij ? ?
C32 0.0738(5) 0.0912(7) 0.6295(4) 0.0424 Uij ? ?
C33 0.1064(6) 0.0234(8) 0.6634(5) 0.0636 Uij ? ?
C34 0.0892(8) -0.0665(9) 0.6528(6) 0.0815 Uij ? ?
C35 0.0393(10) -0.0911(9) 0.6087(7) 0.0884 Uij ? ?
C36 0.0041(8) -0.026(1) 0.5746(5) 0.0856 Uij ? ?
C37 0.0201(7) 0.0656(8) 0.5843(5) 0.0662 Uij ? ?
Cl1A 1.0046(7) 0.3084(7) 0.1655(6) 0.0568 Uij ? ?
Cl1B 1.009(1) 0.313(2) 0.159(1) 0.1837 Uij ? ?
Cl2A 0.946(2) 0.484(2) 0.157(2) 0.1264 Uij ? ?
Cl2B 0.960(2) 0.497(3) 0.171(2) 0.1620 Uij ? ?
C101 1.0278(8) 0.4277(10) 0.1669(7) 0.0965 Uij ? ?
Cl3 0.2266(5) 0.4626(6) 0.4703(4) 0.1197 Uij ? ?
Cl4A 0.3285(9) 0.385(1) 0.5499(8) 0.0809 Uij ? ?
Cl4B 0.308(1) 0.328(1) 0.5401(9) 0.1123 Uij ? ?
C102 0.257(2) 0.406(3) 0.535(1) 0.1110 Uij ? ?
H1 -0.2302 0.4870 0.7212 0.0648 Uij ? ?
H2 -0.2682 0.4413 0.6309 0.0702 Uij ? ?
H3 -0.2045 0.3251 0.6024 0.0577 Uij ? ?
H4 -0.2237 0.1563 0.6473 0.0682 Uij ? ?
H5 -0.2739 0.0150 0.6592 0.0859 Uij ? ?
H6 -0.2008 -0.1094 0.6909 0.0932 Uij ? ?
H7 -0.0779 -0.1019 0.7073 0.1006 Uij ? ?
H8 -0.0246 0.0407 0.6986 0.0714 Uij ? ?
H9 -0.0576 0.3530 0.5912 0.0571 Uij ? ?
H10 -0.0938 0.3735 0.4949 0.0870 Uij ? ?
H11 -0.1487 0.2575 0.4347 0.1045 Uij ? ?
H12 -0.1764 0.1226 0.4708 0.1153 Uij ? ?
H13 -0.1534 0.1041 0.5679 0.0841 Uij ? ?
H14 0.0618 0.4341 0.4710 0.0904 Uij ? ?
H15 0.0634 0.2798 0.4562 0.0926 Uij ? ?
H16 0.0750 0.1748 0.5299 0.0733 Uij ? ?
H17 0.2000 0.2081 0.7556 0.0711 Uij ? ?
H18 0.3277 0.2004 0.7879 0.0864 Uij ? ?
H19 0.3902 0.1910 0.7232 0.0802 Uij ? ?
H20 0.3310 0.1832 0.6321 0.0869 Uij ? ?
H21 0.2076 0.1931 0.5993 0.0794 Uij ? ?
H22 0.1441 0.0388 0.6962 0.0738 Uij ? ?
H23 0.1121 -0.1139 0.6774 0.0956 Uij ? ?
H24 0.0263 -0.1527 0.5981 0.1013 Uij ? ?
H25 -0.0356 -0.0408 0.5416 0.0999 Uij ? ?
H26 -0.0066 0.1113 0.5589 0.0777 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 272 0.003 0.002 'International Tables'
H 0 208 0.000 0.000 'International Tables'
O 0 16 0.011 0.006 'International Tables'
N 0 16 0.006 0.003 'International Tables'
P 0 16 0.102 0.094 'International Tables'
Pd 0 8 -0.999 1.007 'International Tables'
Cl 0 24 0.148 0.159 'International Tables'
C 0 12 0.003 0.002 'International Tables'
H 0 24 0.000 0.000 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
