#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:52:01 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179132 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/94/4309466.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_4309466
loop_
_publ_author_name
'John F. Berry'
'F. Albert Cotton'
'Sergey A. Ibragimov'
'Carlos A. Murillo'
'Xiaoping Wang'
_publ_contact_author_address
;
Department of Chemistry and
Laboratory for Molecular Structure and Bonding
P.O. Box. 30012
Texas A&M University
College Station
TX 77842-3012
U.S.A.
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         979-845-9351
_publ_contact_author_name        'Dr. F. Albert Cotton'
_publ_contact_author_phone       979-845-3646
_publ_section_title
;
Searching for Precursors to Metal-Metal Bonded Dipalladium Species: A
Study of Pd24+ Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6129
_journal_page_last               6137
_journal_paper_doi               10.1021/ic050876c
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C38 H30 N4 Pd'
_chemical_formula_sum            'C38 H30 N4 Pd'
_chemical_formula_weight         649.06
_chemical_name_common            Pd(dpb)2
_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                105.079(9)
_cell_angle_beta                 112.883(8)
_cell_angle_gamma                96.779(9)
_cell_formula_units_Z            2
_cell_length_a                   11.584(6)
_cell_length_b                   11.651(6)
_cell_length_c                   13.222(7)
_cell_measurement_reflns_used    4240
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.0295
_cell_measurement_theta_min      2.6385
_cell_volume                     1538.5(14)
_computing_cell_refinement       SMART
_computing_data_collection       SAINT
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  'Shelxl-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  SMART
_diffrn_measurement_method       ω-scan
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8264
_diffrn_reflns_theta_full        25.18
_diffrn_reflns_theta_max         25.18
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.9628
_exptl_absorpt_correction_T_min  0.8871
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0509
_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)+(0.0857P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                4635
_reflns_number_total             5409
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic050876csi20050727_104043_4.cif
_cod_data_source_block           cmpd4
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1538.5(13)
_cod_database_code               4309466
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.69862(3) 0.97452(2) 0.98896(2) 0.03524(15) Uani 1 1 d . . .
N3 N 0.6031(4) 1.1066(3) 0.9530(3) 0.0437(8) Uani 1 1 d . . .
N2 N 0.7927(3) 0.8415(3) 1.0264(3) 0.0404(8) Uani 1 1 d . . .
N4 N 0.7578(3) 1.1366(3) 1.1222(3) 0.0423(8) Uani 1 1 d . . .
N1 N 0.6512(4) 0.8181(3) 0.8530(3) 0.0444(8) Uani 1 1 d . . .
C10 C 0.5701(4) 0.7726(4) 0.7316(3) 0.0411(9) Uani 1 1 d . . .
C40 C 0.8447(4) 1.1865(4) 1.2411(3) 0.0408(9) Uani 1 1 d . . .
C41 C 0.9645(4) 1.1607(4) 1.2768(4) 0.0465(10) Uani 1 1 d . . .
H41A H 0.9859 1.1109 1.2217 0.056 Uiso 1 1 calc R . .
C42 C 1.0528(5) 1.2069(5) 1.3920(4) 0.0662(14) Uani 1 1 d . . .
H42A H 1.1344 1.1890 1.4152 0.079 Uiso 1 1 calc R . .
C43 C 1.0216(6) 1.2802(6) 1.4744(4) 0.0752(17) Uani 1 1 d . . .
H43A H 1.0816 1.3109 1.5534 0.090 Uiso 1 1 calc R . .
C44 C 0.9045(6) 1.3072(6) 1.4405(4) 0.0746(16) Uani 1 1 d . . .
H44A H 0.8846 1.3586 1.4959 0.090 Uiso 1 1 calc R . .
C45 C 0.8132(5) 1.2590(5) 1.3238(4) 0.0567(12) Uani 1 1 d . . .
H45A H 0.7310 1.2754 1.3012 0.068 Uiso 1 1 calc R . .
C50 C 0.7880(4) 0.6654(4) 0.8669(4) 0.0415(10) Uani 1 1 d . . .
C5 C 0.7422(4) 0.7734(4) 0.9132(4) 0.0407(9) Uani 1 1 d . . .
C6 C 0.6799(4) 1.1902(4) 1.0580(3) 0.0391(9) Uani 1 1 d . . .
C52 C 0.8482(5) 0.4769(5) 0.8777(6) 0.0664(15) Uani 1 1 d . . .
H52A H 0.8581 0.4162 0.9132 0.080 Uiso 1 1 calc R . .
C15 C 0.5049(4) 0.6498(4) 0.6738(4) 0.0502(11) Uani 1 1 d . . .
H15A H 0.5158 0.5940 0.7149 0.060 Uiso 1 1 calc R . .
C22 C 1.1437(5) 0.8729(5) 1.1746(6) 0.0719(16) Uani 1 1 d . . .
H22A H 1.2160 0.8787 1.1585 0.086 Uiso 1 1 calc R . .
C20 C 0.9169(4) 0.8495(3) 1.1109(3) 0.0384(9) Uani 1 1 d . . .
C11 C 0.5531(5) 0.8529(5) 0.6703(4) 0.0547(12) Uani 1 1 d . . .
H11A H 0.5972 0.9361 0.7089 0.066 Uiso 1 1 calc R . .
C31 C 0.5635(5) 1.2241(4) 0.8191(4) 0.0498(11) Uani 1 1 d . . .
H31A H 0.6432 1.2815 0.8682 0.060 Uiso 1 1 calc R . .
C30 C 0.5246(4) 1.1289(4) 0.8514(3) 0.0399(9) Uani 1 1 d . . .
C35 C 0.4081(4) 1.0448(5) 0.7779(4) 0.0599(13) Uani 1 1 d . . .
H35A H 0.3815 0.9783 0.7983 0.072 Uiso 1 1 calc R . .
C34 C 0.3300(5) 1.0590(8) 0.6732(5) 0.083(2) Uani 1 1 d . . .
H34A H 0.2487 1.0040 0.6245 0.099 Uiso 1 1 calc R . .
C33 C 0.3702(8) 1.1514(8) 0.6412(5) 0.092(3) Uani 1 1 d . . .
H33A H 0.3192 1.1581 0.5687 0.111 Uiso 1 1 calc R . .
C32 C 0.4851(8) 1.2348(6) 0.7146(5) 0.080(2) Uani 1 1 d . . .
H32A H 0.5112 1.3007 0.6934 0.096 Uiso 1 1 calc R . .
C21 C 1.0236(4) 0.8590(4) 1.0898(4) 0.0537(11) Uani 1 1 d . . .
H21A H 1.0140 0.8558 1.0150 0.064 Uiso 1 1 calc R . .
C24 C 1.0540(6) 0.8682(5) 1.3079(5) 0.0672(16) Uani 1 1 d . . .
H24A H 1.0649 0.8701 1.3826 0.081 Uiso 1 1 calc R . .
C51 C 0.8055(4) 0.5770(4) 0.9201(4) 0.0505(11) Uani 1 1 d . . .
H51A H 0.7885 0.5846 0.9852 0.061 Uiso 1 1 calc R . .
C55 C 0.8137(4) 0.6539(4) 0.7710(4) 0.0504(11) Uani 1 1 d . . .
H55A H 0.7994 0.7123 0.7330 0.061 Uiso 1 1 calc R . .
C62 C 0.7901(5) 1.5331(4) 1.1817(4) 0.0533(11) Uani 1 1 d . . .
H62A H 0.8678 1.5937 1.2146 0.064 Uiso 1 1 calc R . .
C61 C 0.7904(4) 1.4115(4) 1.1444(4) 0.0456(10) Uani 1 1 d . . .
H61A H 0.8682 1.3894 1.1525 0.055 Uiso 1 1 calc R . .
C60 C 0.6761(4) 1.3212(4) 1.0949(3) 0.0391(9) Uani 1 1 d . . .
C65 C 0.5621(4) 1.3546(4) 1.0833(4) 0.0462(10) Uani 1 1 d . . .
H65A H 0.4839 1.2943 1.0492 0.055 Uiso 1 1 calc R . .
C64 C 0.5640(5) 1.4772(5) 1.1222(4) 0.0532(12) Uani 1 1 d . . .
H64A H 0.4865 1.4995 1.1150 0.064 Uiso 1 1 calc R . .
C63 C 0.6764(5) 1.5674(4) 1.1712(5) 0.0577(12) Uani 1 1 d . . .
H63A H 0.6763 1.6505 1.1971 0.069 Uiso 1 1 calc R . .
C54 C 0.8603(4) 0.5562(5) 0.7314(5) 0.0624(14) Uani 1 1 d . . .
H54A H 0.8814 0.5506 0.6687 0.075 Uiso 1 1 calc R . .
C25 C 0.9313(4) 0.8548(4) 1.2211(4) 0.0488(11) Uani 1 1 d . . .
H25A H 0.8591 0.8495 1.2373 0.059 Uiso 1 1 calc R . .
C13 C 0.4080(5) 0.6899(6) 0.4961(4) 0.0685(16) Uani 1 1 d . . .
H13A H 0.3531 0.6618 0.4158 0.082 Uiso 1 1 calc R . .
C14 C 0.4241(5) 0.6097(5) 0.5559(4) 0.0617(14) Uani 1 1 d . . .
H14A H 0.3801 0.5265 0.5169 0.074 Uiso 1 1 calc R . .
C23 C 1.1578(5) 0.8785(5) 1.2834(6) 0.0753(17) Uani 1 1 d . . .
H23A H 1.2407 0.8896 1.3425 0.090 Uiso 1 1 calc R . .
C53 C 0.8762(5) 0.4663(5) 0.7838(5) 0.0714(18) Uani 1 1 d . . .
H53A H 0.9057 0.3989 0.7555 0.086 Uiso 1 1 calc R . .
C12 C 0.4716(6) 0.8124(5) 0.5521(4) 0.0713(16) Uani 1 1 d . . .
H12A H 0.4597 0.8678 0.5105 0.086 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 0.0033 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'
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
N1 Pd1 N4 175.36(14) . . ?
N1 Pd1 N3 116.52(14) . . ?
N4 Pd1 N3 63.79(14) . . ?
N1 Pd1 N2 63.76(14) . . ?
N4 Pd1 N2 116.01(14) . . ?
N3 Pd1 N2 179.08(13) . . ?
N1 Pd1 C5 31.58(14) . . ?
N4 Pd1 C5 147.37(14) . . ?
N3 Pd1 C5 147.77(14) . . ?
N2 Pd1 C5 32.62(13) . . ?
N1 Pd1 C6 148.11(14) . . ?
N4 Pd1 C6 31.64(13) . . ?
N3 Pd1 C6 32.29(13) . . ?
N2 Pd1 C6 147.56(13) . . ?
C5 Pd1 C6 171.52(13) . . ?
C6 N3 C30 127.2(4) . . ?
C6 N3 Pd1 93.0(3) . . ?
C30 N3 Pd1 135.8(3) . . ?
C5 N2 C20 125.0(4) . . ?
C5 N2 Pd1 91.9(3) . . ?
C20 N2 Pd1 131.4(3) . . ?
C6 N4 C40 127.8(4) . . ?
C6 N4 Pd1 94.1(2) . . ?
C40 N4 Pd1 138.2(3) . . ?
C5 N1 C10 128.1(4) . . ?
C5 N1 Pd1 93.7(3) . . ?
C10 N1 Pd1 137.4(3) . . ?
C11 C10 C15 119.3(4) . . ?
C11 C10 N1 118.9(4) . . ?
C15 C10 N1 121.8(4) . . ?
C41 C40 C45 119.2(4) . . ?
C41 C40 N4 118.4(4) . . ?
C45 C40 N4 122.4(4) . . ?
C42 C41 C40 120.7(5) . . ?
C41 C42 C43 120.1(5) . . ?
C44 C43 C42 119.9(5) . . ?
C43 C44 C45 120.4(5) . . ?
C40 C45 C44 119.7(5) . . ?
C51 C50 C55 119.7(4) . . ?
C51 C50 C5 120.0(4) . . ?
C55 C50 C5 120.3(4) . . ?
N1 C5 N2 109.1(4) . . ?
N1 C5 C50 127.0(4) . . ?
N2 C5 C50 123.8(4) . . ?
N1 C5 Pd1 54.7(2) . . ?
N2 C5 Pd1 55.5(2) . . ?
C50 C5 Pd1 170.0(3) . . ?
N4 C6 N3 108.6(4) . . ?
N4 C6 C60 126.2(4) . . ?
N3 C6 C60 125.1(4) . . ?
N4 C6 Pd1 54.3(2) . . ?
N3 C6 Pd1 54.7(2) . . ?
C60 C6 Pd1 175.3(3) . . ?
C53 C52 C51 120.3(5) . . ?
C14 C15 C10 120.0(5) . . ?
C21 C22 C23 119.2(6) . . ?
C21 C20 C25 119.2(4) . . ?
C21 C20 N2 122.6(4) . . ?
C25 C20 N2 118.1(4) . . ?
C10 C11 C12 120.6(5) . . ?
C32 C31 C30 119.6(6) . . ?
C31 C30 C35 119.5(4) . . ?
C31 C30 N3 123.1(4) . . ?
C35 C30 N3 117.2(4) . . ?
C30 C35 C34 119.5(6) . . ?
C33 C34 C35 120.5(6) . . ?
C34 C33 C32 119.6(5) . . ?
C33 C32 C31 121.2(6) . . ?
C22 C21 C20 121.5(5) . . ?
C23 C24 C25 119.4(5) . . ?
C50 C51 C52 120.2(5) . . ?
C54 C55 C50 119.9(5) . . ?
C61 C62 C63 120.7(4) . . ?
C62 C61 C60 120.1(4) . . ?
C65 C60 C61 119.5(4) . . ?
C65 C60 C6 121.6(4) . . ?
C61 C60 C6 118.9(4) . . ?
C64 C65 C60 119.4(4) . . ?
C63 C64 C65 121.6(4) . . ?
C64 C63 C62 118.6(4) . . ?
C55 C54 C53 120.4(5) . . ?
C20 C25 C24 119.4(5) . . ?
C14 C13 C12 120.6(5) . . ?
C13 C14 C15 120.3(5) . . ?
C24 C23 C22 121.3(5) . . ?
C52 C53 C54 119.4(5) . . ?
C13 C12 C11 119.3(5) . . ?
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 N1 2.037(3) . ?
Pd1 N4 2.041(3) . ?
Pd1 N3 2.048(4) . ?
Pd1 N2 2.053(4) . ?
Pd1 C5 2.491(4) . ?
Pd1 C6 2.507(4) . ?
N3 C6 1.341(5) . ?
N3 C30 1.410(5) . ?
N2 C5 1.344(5) . ?
N2 C20 1.410(5) . ?
N4 C6 1.318(5) . ?
N4 C40 1.407(5) . ?
N1 C5 1.307(6) . ?
N1 C10 1.416(5) . ?
C10 C11 1.374(6) . ?
C10 C15 1.388(6) . ?
C40 C41 1.379(6) . ?
C40 C45 1.395(6) . ?
C41 C42 1.374(6) . ?
C42 C43 1.394(8) . ?
C43 C44 1.357(9) . ?
C44 C45 1.398(7) . ?
C50 C51 1.384(7) . ?
C50 C55 1.388(6) . ?
C50 C5 1.499(6) . ?
C6 C60 1.488(6) . ?
C52 C53 1.380(9) . ?
C52 C51 1.389(7) . ?
C15 C14 1.381(7) . ?
C22 C21 1.363(8) . ?
C22 C23 1.366(9) . ?
C20 C21 1.368(6) . ?
C20 C25 1.385(6) . ?
C11 C12 1.386(7) . ?
C31 C32 1.375(8) . ?
C31 C30 1.375(6) . ?
C30 C35 1.378(6) . ?
C35 C34 1.394(8) . ?
C34 C33 1.352(11) . ?
C33 C32 1.362(11) . ?
C24 C23 1.361(9) . ?
C24 C25 1.396(7) . ?
C55 C54 1.384(7) . ?
C62 C61 1.375(6) . ?
C62 C63 1.387(7) . ?
C61 C60 1.389(6) . ?
C60 C65 1.383(6) . ?
C65 C64 1.381(7) . ?
C64 C63 1.373(7) . ?
C54 C53 1.391(8) . ?
C13 C14 1.359(8) . ?
C13 C12 1.381(8) . ?
