#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:04:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178547 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/54/4065444.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_4065444
loop_
_publ_author_name
'Herbert, David E.'
'Ozerov, Oleg V.'
_publ_section_title
;
 Binuclear Palladium Complexes Supported by Bridged Pincer Ligands
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6641
_journal_paper_doi               10.1021/om2008056
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C44 H58 Cl2 N4 P2 Pd2'
_chemical_formula_sum            'C44 H58 Cl2 N4 P2 Pd2'
_chemical_formula_weight         988.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 103.707(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.037(11)
_cell_length_b                   13.509(6)
_cell_length_c                   14.442(7)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.41
_cell_volume                     4366(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23962
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0228
_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)+(0.0253P)²+3.1139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0568
_reflns_number_gt                4487
_reflns_number_total             4994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2008056_si_002.cif
_cod_data_source_block           oz316_sad
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4367(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4065444
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
C1 C 0.37988(8) 0.27536(13) 0.27212(12) 0.0143(3) Uani 1 1 d .
C2 C 0.33229(8) 0.31286(13) 0.30757(12) 0.0152(4) Uani 1 1 d .
C3 C 0.31223(8) 0.26260(14) 0.37835(13) 0.0174(4) Uani 1 1 d .
H3 H 0.2803 0.2896 0.4014 0.021 Uiso 1 1 calc R
C4 C 0.33791(8) 0.17392(13) 0.41590(12) 0.0166(4) Uani 1 1 d .
C5 C 0.38443(8) 0.13656(13) 0.37932(13) 0.0175(4) Uani 1 1 d .
H5 H 0.4023 0.0755 0.4033 0.021 Uiso 1 1 calc R
C6 C 0.40541(8) 0.18520(13) 0.30956(13) 0.0161(4) Uani 1 1 d .
H6 H 0.4373 0.1574 0.2868 0.019 Uiso 1 1 calc R
C7 C 0.31716(9) 0.12342(14) 0.49566(14) 0.0218(4) Uani 1 1 d .
H7A H 0.3261 0.1656 0.5525 0.033 Uiso 1 1 calc R
H7B H 0.3379 0.0600 0.5103 0.033 Uiso 1 1 calc R
H7C H 0.2740 0.1119 0.4760 0.033 Uiso 1 1 calc R
C8 C 0.42496(8) 0.29016(13) 0.13694(12) 0.0151(4) Uani 1 1 d .
C9 C 0.46615(8) 0.34059(13) 0.09426(12) 0.0147(4) Uani 1 1 d .
C10 C 0.48954(8) 0.29324(14) 0.02467(12) 0.0167(4) Uani 1 1 d .
H10 H 0.5187 0.3271 0.0000 0.020 Uiso 1 1 calc R
C11 C 0.47214(8) 0.19972(14) -0.00965(13) 0.0189(4) Uani 1 1 d .
C12 C 0.43069(8) 0.15144(14) 0.03135(13) 0.0203(4) Uani 1 1 d .
H12 H 0.4177 0.0869 0.0097 0.024 Uiso 1 1 calc R
C13 C 0.40805(8) 0.19434(14) 0.10223(13) 0.0181(4) Uani 1 1 d .
H13 H 0.3803 0.1582 0.1283 0.022 Uiso 1 1 calc R
C14 C 0.49648(9) 0.15176(15) -0.08726(14) 0.0256(4) Uani 1 1 d .
H14A H 0.4706 0.1679 -0.1496 0.038 Uiso 1 1 calc R
H14B H 0.4977 0.0798 -0.0785 0.038 Uiso 1 1 calc R
H14C H 0.5369 0.1765 -0.0840 0.038 Uiso 1 1 calc R
C15 C 0.23179(8) 0.41887(14) 0.17679(13) 0.0184(4) Uani 1 1 d .
H15 H 0.2171 0.4868 0.1559 0.022 Uiso 1 1 calc R
C16 C 0.23995(9) 0.36364(16) 0.08851(14) 0.0254(4) Uani 1 1 d .
H16A H 0.2589 0.2995 0.1075 0.038 Uiso 1 1 calc R
H16B H 0.2653 0.4028 0.0566 0.038 Uiso 1 1 calc R
H16C H 0.2009 0.3531 0.0447 0.038 Uiso 1 1 calc R
C17 C 0.18489(9) 0.37030(16) 0.22155(14) 0.0260(4) Uani 1 1 d .
H17A H 0.1470 0.3646 0.1736 0.039 Uiso 1 1 calc R
H17B H 0.1790 0.4110 0.2748 0.039 Uiso 1 1 calc R
H17C H 0.1986 0.3042 0.2450 0.039 Uiso 1 1 calc R
C18 C 0.29311(8) 0.50438(14) 0.36211(13) 0.0168(4) Uani 1 1 d .
H18 H 0.2718 0.4605 0.3990 0.020 Uiso 1 1 calc R
C19 C 0.35348(9) 0.53169(17) 0.42778(14) 0.0274(5) Uani 1 1 d .
H19A H 0.3747 0.5774 0.3946 0.041 Uiso 1 1 calc R
H19B H 0.3774 0.4716 0.4453 0.041 Uiso 1 1 calc R
H19C H 0.3470 0.5635 0.4855 0.041 Uiso 1 1 calc R
C20 C 0.25402(10) 0.59550(15) 0.33130(14) 0.0252(4) Uani 1 1 d .
H20A H 0.2493 0.6317 0.3879 0.038 Uiso 1 1 calc R
H20B H 0.2147 0.5747 0.2938 0.038 Uiso 1 1 calc R
H20C H 0.2730 0.6386 0.2925 0.038 Uiso 1 1 calc R
C21 C 0.48828(8) 0.43905(13) 0.12237(12) 0.0142(3) Uani 1 1 d .
H21 H 0.5266 0.4558 0.1135 0.017 Uiso 1 1 calc R
C22 C 0.49287(8) 0.59602(13) 0.19544(12) 0.0161(4) Uani 1 1 d .
H22A H 0.4682 0.6546 0.1707 0.019 Uiso 1 1 calc R
H22B H 0.5304 0.6000 0.1737 0.019 Uiso 1 1 calc R
Cl1 Cl 0.34798(2) 0.64030(3) 0.16777(4) 0.02465(11) Uani 1 1 d .
N1 N 0.40272(7) 0.33358(11) 0.20835(10) 0.0149(3) Uani 1 1 d .
N2 N 0.46052(7) 0.50559(11) 0.15826(10) 0.0137(3) Uani 1 1 d .
P1 P 0.30515(2) 0.43276(3) 0.26003(3) 0.01381(10) Uani 1 1 d .
Pd1 Pd 0.379748(6) 0.477596(10) 0.195632(9) 0.01275(5) Uani 1 1 d .
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'
N N 0.0061 0.0033 '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_3
C6 C1 N1 123.40(16) .
C6 C1 C2 117.57(16) .
N1 C1 C2 118.77(16) .
C3 C2 C1 120.85(17) .
C3 C2 P1 124.66(14) .
C1 C2 P1 114.33(13) .
C4 C3 C2 121.47(17) .
C3 C4 C5 117.27(16) .
C3 C4 C7 120.33(17) .
C5 C4 C7 122.35(17) .
C6 C5 C4 122.42(17) .
C5 C6 C1 120.40(17) .
N1 C8 C13 122.26(16) .
N1 C8 C9 121.48(16) .
C13 C8 C9 116.26(16) .
C10 C9 C8 120.09(17) .
C10 C9 C21 116.78(16) .
C8 C9 C21 123.06(16) .
C11 C10 C9 123.11(17) .
C10 C11 C12 116.35(17) .
C10 C11 C14 122.04(18) .
C12 C11 C14 121.61(18) .
C13 C12 C11 122.24(18) .
C12 C13 C8 121.87(17) .
C16 C15 C17 112.44(17) .
C16 C15 P1 108.67(13) .
C17 C15 P1 113.52(13) .
C20 C18 C19 111.87(17) .
C20 C18 P1 112.39(13) .
C19 C18 P1 109.63(13) .
N2 C21 C9 125.56(17) .
N2 C22 C22 110.09(11) 2_655
C8 N1 C1 120.86(15) .
C8 N1 Pd1 118.46(12) .
C1 N1 Pd1 118.02(11) .
C21 N2 C22 118.29(15) .
C21 N2 Pd1 122.50(13) .
C22 N2 Pd1 117.56(11) .
C2 P1 C15 109.76(9) .
C2 P1 C18 105.70(9) .
C15 P1 C18 106.76(9) .
C2 P1 Pd1 99.81(6) .
C15 P1 Pd1 115.89(7) .
C18 P1 Pd1 118.07(7) .
N1 Pd1 N2 88.14(6) .
N1 Pd1 P1 84.90(5) .
N2 Pd1 P1 168.69(4) .
N1 Pd1 Cl1 174.93(4) .
N2 Pd1 Cl1 92.71(5) .
P1 Pd1 Cl1 95.01(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.404(3) .
C1 N1 1.405(2) .
C1 C2 1.410(2) .
C2 C3 1.394(3) .
C2 P1 1.812(2) .
C3 C4 1.388(3) .
C4 C5 1.397(3) .
C4 C7 1.511(2) .
C5 C6 1.382(3) .
C8 N1 1.386(2) .
C8 C13 1.409(3) .
C8 C9 1.422(2) .
C9 C10 1.402(2) .
C9 C21 1.448(3) .
C10 C11 1.381(3) .
C11 C12 1.398(3) .
C11 C14 1.513(3) .
C12 C13 1.382(3) .
C15 C16 1.527(3) .
C15 C17 1.532(3) .
C15 P1 1.837(2) .
C18 C20 1.528(3) .
C18 C19 1.531(3) .
C18 P1 1.8386(19) .
C21 N2 1.282(2) .
C22 N2 1.465(2) .
C22 C22 1.532(3) 2_655
Cl1 Pd1 2.3213(11) .
N1 Pd1 2.0132(17) .
N2 Pd1 2.0912(17) .
P1 Pd1 2.2233(9) .
