#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:40:12 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178910 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/39/4113980.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_4113980
loop_
_publ_author_name
'Diran Herebian'
'Eberhard Bothe'
'Frank Neese'
'Thomas Weyhermüller'
'Karl Wieghardt'
_publ_section_title
;
 Molecular and Electronic Structures of
 Bis-(o-diiminobenzosemiquinonato)metal(II) Complexes (Ni, Pd, Pt), Their
 Monocations and -Anions, and of Dimeric Dications Containing Weak
 Metal-Metal Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9116
_journal_page_last               9128
_journal_paper_doi               10.1021/ja030123u
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C24 H20 N4 Pd'
_chemical_formula_weight         470.84
_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
_cell_angle_alpha                73.74(1)
_cell_angle_beta                 75.84(1)
_cell_angle_gamma                63.36(1)
_cell_formula_units_Z            2
_cell_length_a                   9.5312(6)
_cell_length_b                   10.2585(6)
_cell_length_c                   11.7914(6)
_cell_measurement_reflns_used    14050
_cell_measurement_temperature    100(2)
_cell_volume                     979.73(14)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method       '129 images at 1.0 deg. in ω and 40 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11863
_diffrn_reflns_theta_max         33.15
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   'gaussian, face-indexed'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       'opaque needle'
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.707
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.009
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         7344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_obs          0.0331
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+0.7518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0807
_refine_ls_wR_factor_obs         0.0714
_reflns_number_observed          5509
_reflns_number_total             7391
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja030123u_3.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.7518P] 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^)+(0.0000P)^2^+0.7518P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        979.73(10)
_cod_database_code               4113980
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.5000 0.5000 0.0000 0.01235(5) Uani 1 d S
N1 N 0.3497(2) 0.7093(2) -0.0262(2) 0.0157(3) Uani 1 d .
H1 H 0.3223(30) 0.7686(29) -0.0919(23) 0.016(6) Uiso 1 d .
N2 N 0.4377(2) 0.5317(2) 0.16683(14) 0.0132(3) Uani 1 d .
C1 C 0.2798(2) 0.7697(2) 0.0709(2) 0.0142(3) Uani 1 d .
C2 C 0.3276(2) 0.6693(2) 0.1811(2) 0.0130(3) Uani 1 d .
C3 C 0.2643(2) 0.7233(2) 0.2894(2) 0.0146(4) Uani 1 d .
H3 H 0.2970(2) 0.6614(2) 0.3611(2) 0.018 Uiso 1 calc R
C4 C 0.1542(2) 0.8678(2) 0.2874(2) 0.0161(4) Uani 1 d .
H4 H 0.1110(2) 0.9018(2) 0.3587(2) 0.019 Uiso 1 calc R
C5 C 0.1053(2) 0.9656(2) 0.1794(2) 0.0166(4) Uani 1 d .
H5 H 0.0299(2) 1.0623(2) 0.1808(2) 0.020 Uiso 1 calc R
C6 C 0.1683(2) 0.9190(2) 0.0728(2) 0.0162(4) Uani 1 d .
H6 H 0.1382(2) 0.9848(2) 0.0019(2) 0.019 Uiso 1 calc R
C7 C 0.4950(2) 0.4198(2) 0.2681(2) 0.0135(3) Uani 1 d .
C8 C 0.3923(2) 0.3708(2) 0.3573(2) 0.0163(4) Uani 1 d .
H8 H 0.2850(2) 0.4109(2) 0.3508(2) 0.020 Uiso 1 calc R
C9 C 0.4509(3) 0.2621(2) 0.4555(2) 0.0194(4) Uani 1 d .
H9 H 0.3824(3) 0.2298(2) 0.5147(2) 0.023 Uiso 1 calc R
C10 C 0.6113(3) 0.2014(2) 0.4659(2) 0.0190(4) Uani 1 d .
H10 H 0.6497(3) 0.1302(2) 0.5326(2) 0.023 Uiso 1 calc R
C11 C 0.7139(2) 0.2477(2) 0.3760(2) 0.0188(4) Uani 1 d .
H11 H 0.8214(2) 0.2061(2) 0.3822(2) 0.023 Uiso 1 calc R
C12 C 0.6567(2) 0.3556(2) 0.2771(2) 0.0167(4) Uani 1 d .
H12 H 0.7262(2) 0.3852(2) 0.2167(2) 0.020 Uiso 1 calc R
Pd2 Pd 0.0000 0.5000 0.0000 0.01094(5) Uani 1 d S
N3 N 0.1201(2) 0.3144(2) 0.10321(15) 0.0140(3) Uani 1 d .
H3A H 0.1862(36) 0.2297(35) 0.0827(27) 0.034(8) Uiso 1 d .
N4 N -0.0855(2) 0.5602(2) 0.15741(14) 0.0120(3) Uani 1 d .
C13 C 0.0926(2) 0.3144(2) 0.2203(2) 0.0129(3) Uani 1 d .
C14 C -0.0239(2) 0.4536(2) 0.2516(2) 0.0121(3) Uani 1 d .
C15 C -0.0689(2) 0.4634(2) 0.3740(2) 0.0141(3) Uani 1 d .
H15 H -0.1458(2) 0.5514(2) 0.3962(2) 0.017 Uiso 1 calc R
C16 C 0.0012(2) 0.3430(2) 0.4595(2) 0.0150(4) Uani 1 d .
H16 H -0.0283(2) 0.3507(2) 0.5394(2) 0.018 Uiso 1 calc R
C17 C 0.1180(2) 0.2067(2) 0.4283(2) 0.0164(4) Uani 1 d .
H17 H 0.1644(2) 0.1267(2) 0.4877(2) 0.020 Uiso 1 calc R
C18 C 0.1624(2) 0.1927(2) 0.3113(2) 0.0140(3) Uani 1 d .
H18 H 0.2385(2) 0.1031(2) 0.2915(2) 0.017 Uiso 1 calc R
C19 C -0.1963(2) 0.7056(2) 0.1754(2) 0.0121(3) Uani 1 d .
C20 C -0.3458(2) 0.7658(2) 0.1400(2) 0.0157(4) Uani 1 d .
H20 H -0.3729(2) 0.7115(2) 0.1044(2) 0.019 Uiso 1 calc R
C21 C -0.4547(2) 0.9073(2) 0.1580(2) 0.0189(4) Uani 1 d .
H21 H -0.5542(2) 0.9474(2) 0.1340(2) 0.023 Uiso 1 calc R
C22 C -0.4154(3) 0.9887(2) 0.2116(2) 0.0201(4) Uani 1 d .
H22 H -0.4889(3) 1.0823(2) 0.2248(2) 0.024 Uiso 1 calc R
C23 C -0.2655(2) 0.9294(2) 0.2453(2) 0.0163(4) Uani 1 d .
H23 H -0.2387(2) 0.9840(2) 0.2807(2) 0.020 Uiso 1 calc R
C24 C -0.1552(2) 0.7886(2) 0.2266(2) 0.0144(4) Uani 1 d .
H24 H -0.0545(2) 0.7502(2) 0.2482(2) 0.017 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'
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
N1 Pd1 N1 179.998(1) . 2_665
N1 Pd1 N2 80.07(7) . .
N1 Pd1 N2 99.93(7) 2_665 .
N1 Pd1 N2 99.94(7) . 2_665
N1 Pd1 N2 80.07(7) 2_665 2_665
N2 Pd1 N2 180.0 . 2_665
C1 N1 Pd1 116.61(13) . .
C2 N2 C7 120.2(2) . .
C2 N2 Pd1 115.25(13) . .
C7 N2 Pd1 124.49(13) . .
N1 C1 C6 126.1(2) . .
N1 C1 C2 114.2(2) . .
C6 C1 C2 119.6(2) . .
N2 C2 C3 127.2(2) . .
N2 C2 C1 113.8(2) . .
C3 C2 C1 118.9(2) . .
C4 C3 C2 119.5(2) . .
C3 C4 C5 121.5(2) . .
C6 C5 C4 120.5(2) . .
C5 C6 C1 119.8(2) . .
C12 C7 C8 119.5(2) . .
C12 C7 N2 119.4(2) . .
C8 C7 N2 121.0(2) . .
C9 C8 C7 119.9(2) . .
C8 C9 C10 120.5(2) . .
C11 C10 C9 119.6(2) . .
C10 C11 C12 120.4(2) . .
C11 C12 C7 120.0(2) . .
N3 Pd2 N3 180.0 . 2_565
N3 Pd2 N4 99.77(7) . 2_565
N3 Pd2 N4 80.23(7) 2_565 2_565
N3 Pd2 N4 80.23(7) . .
N3 Pd2 N4 99.77(7) 2_565 .
N4 Pd2 N4 180.0 2_565 .
C13 N3 Pd2 116.57(13) . .
C14 N4 C19 119.8(2) . .
C14 N4 Pd2 115.06(12) . .
C19 N4 Pd2 125.03(12) . .
N3 C13 C18 126.4(2) . .
N3 C13 C14 114.0(2) . .
C18 C13 C14 119.6(2) . .
N4 C14 C15 127.0(2) . .
N4 C14 C13 114.1(2) . .
C15 C14 C13 118.7(2) . .
C16 C15 C14 119.9(2) . .
C15 C16 C17 121.3(2) . .
C18 C17 C16 120.3(2) . .
C17 C18 C13 120.2(2) . .
C20 C19 C24 119.8(2) . .
C20 C19 N4 119.8(2) . .
C24 C19 N4 120.5(2) . .
C21 C20 C19 120.0(2) . .
C22 C21 C20 120.4(2) . .
C21 C22 C23 119.6(2) . .
C22 C23 C24 120.5(2) . .
C23 C24 C19 119.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 1.961(2) .
Pd1 N1 1.961(2) 2_665
Pd1 N2 1.985(2) .
Pd1 N2 1.985(2) 2_665
N1 C1 1.338(3) .
N2 C2 1.357(3) .
N2 C7 1.426(3) .
C1 C6 1.422(3) .
C1 C2 1.441(3) .
C2 C3 1.421(3) .
C3 C4 1.377(3) .
C4 C5 1.414(3) .
C5 C6 1.371(3) .
C7 C12 1.397(3) .
C7 C8 1.399(3) .
C8 C9 1.390(3) .
C9 C10 1.391(3) .
C10 C11 1.390(3) .
C11 C12 1.390(3) .
Pd2 N3 1.961(2) .
Pd2 N3 1.961(2) 2_565
Pd2 N4 1.985(2) 2_565
Pd2 N4 1.985(2) .
N3 C13 1.341(2) .
N4 C14 1.355(2) .
N4 C19 1.428(2) .
C13 C18 1.416(3) .
C13 C14 1.443(3) .
C14 C15 1.420(3) .
C15 C16 1.371(3) .
C16 C17 1.421(3) .
C17 C18 1.369(3) .
C19 C20 1.394(3) .
C19 C24 1.396(3) .
C20 C21 1.394(3) .
C21 C22 1.388(3) .
C22 C23 1.390(3) .
C23 C24 1.394(3) .
