#------------------------------------------------------------------------------
#$Date: 2017-07-11 14:26:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198632 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/90/4339057.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_4339057
loop_
_publ_author_name
'Nuricumbo-Escobar, Juan José'
'Campos-Alvarado, Carlos'
'Ríos-Moreno, Gustavo'
'Morales-Morales, David'
'Walsh, Patrick J.'
'Parra-Hake, Miguel'
_publ_section_title
;
 Binuclear palladium(I) and palladium(II) complexes of
 ortho-functionalized 1,3-bis(aryl)triazenido ligands.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6182
_journal_page_last               6189
_journal_paper_doi               10.1021/ic700516p
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C30 H28 N6 O4 Pd2'
_chemical_formula_weight         749.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.579(6)
_cell_angle_beta                 80.885(6)
_cell_angle_gamma                74.607(6)
_cell_formula_units_Z            1
_cell_length_a                   6.6288(5)
_cell_length_b                   10.2631(10)
_cell_length_c                   11.0246(11)
_cell_measurement_temperature    143(1)
_cell_volume                     713.51(12)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Rigaku Mercury CCD Area Detector'
_diffrn_measurement_method       'phi rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8129
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             374
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0172P)²+0.5506P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                2994
_reflns_number_total             3063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700516p-file002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        713.51(11)
_cod_database_code               4339057
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_method 'symmetry-related measurements'
#END Tags that were not found in dictionaries
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
Pd1 Pd 0.335293(19) 0.582498(12) 0.487966(11) 0.01402(5) Uani 1 1 d .
N1 N 0.3575(2) 0.48986(15) 0.32840(13) 0.0159(3) Uani 1 1 d .
N2 N 0.5034(2) 0.38759(15) 0.28469(13) 0.0159(3) Uani 1 1 d .
N3 N 0.6492(2) 0.33184(15) 0.35534(13) 0.0158(3) Uani 1 1 d .
C1 C 0.2189(3) 0.54866(17) 0.24003(15) 0.0153(3) Uani 1 1 d .
C2 C 0.3008(3) 0.58342(18) 0.12129(16) 0.0185(4) Uani 1 1 d .
H2 H 0.4461 0.5693 0.0991 0.025 Uiso 1 1 calc R
C3 C 0.1658(3) 0.63900(18) 0.03661(16) 0.0210(4) Uani 1 1 d .
H3 H 0.2217 0.6612 -0.0427 0.028 Uiso 1 1 calc R
C4 C -0.0525(3) 0.66232(18) 0.06774(17) 0.0209(4) Uani 1 1 d .
C5 C -0.1309(3) 0.62550(19) 0.18619(18) 0.0221(4) Uani 1 1 d .
H5 H -0.2761 0.6389 0.2083 0.029 Uiso 1 1 calc R
C6 C 0.0025(3) 0.56921(19) 0.27204(17) 0.0200(4) Uani 1 1 d .
H6 H -0.0531 0.5453 0.3509 0.027 Uiso 1 1 calc R
C7 C -0.1978(4) 0.7251(2) -0.02584(19) 0.0287(5) Uani 1 1 d .
H7A H -0.1933 0.6588 -0.0837 0.043 Uiso 1 1 calc R
H7B H -0.1526 0.7999 -0.0685 0.043 Uiso 1 1 calc R
H7C H -0.3398 0.7566 0.0153 0.043 Uiso 1 1 calc R
C8 C 0.7769(3) 0.20731(18) 0.30969(16) 0.0175(4) Uani 1 1 d .
C9 C 0.7059(3) 0.14209(19) 0.22231(17) 0.0230(4) Uani 1 1 d .
H9 H 0.5734 0.1803 0.1990 0.031 Uiso 1 1 calc R
C10 C 0.8284(4) 0.0236(2) 0.17119(19) 0.0289(5) Uani 1 1 d .
H10 H 0.7797 -0.0152 0.1119 0.038 Uiso 1 1 calc R
C11 C 1.0234(4) -0.0386(2) 0.2069(2) 0.0318(5) Uani 1 1 d .
H11 H 1.1059 -0.1186 0.1721 0.042 Uiso 1 1 calc R
C12 C 1.0927(3) 0.0200(2) 0.29463(19) 0.0270(4) Uani 1 1 d .
H12 H 1.2228 -0.0222 0.3195 0.036 Uiso 1 1 calc R
C13 C 0.9729(3) 0.14212(18) 0.34823(17) 0.0196(4) Uani 1 1 d .
C14 C 1.0611(3) 0.19181(18) 0.44481(16) 0.0193(4) Uani 1 1 d .
C15 C 1.3564(3) 0.1678(2) 0.54666(19) 0.0274(4) Uani 1 1 d .
H15A H 1.3434 0.2634 0.5410 0.041 Uiso 1 1 calc R
H15B H 1.5032 0.1201 0.5401 0.041 Uiso 1 1 calc R
H15C H 1.2835 0.1445 0.6243 0.041 Uiso 1 1 calc R
O1 O 0.9686(2) 0.27502(13) 0.52108(12) 0.0216(3) Uani 1 1 d .
O2 O 1.2646(2) 0.13054(14) 0.44775(13) 0.0266(3) 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'
O O 0.0106 0.0060 '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
N3 Pd1 N1 173.25(6) 2_666 .
N3 Pd1 O1 88.55(5) 2_666 2_666
N1 Pd1 O1 97.56(5) . 2_666
N3 Pd1 Pd1 89.39(4) 2_666 2_666
N1 Pd1 Pd1 84.68(4) . 2_666
O1 Pd1 Pd1 175.95(4) 2_666 2_666
N2 N1 C1 111.08(14) . .
N2 N1 Pd1 127.70(12) . .
C1 N1 Pd1 120.62(11) . .
N1 N2 N3 116.05(14) . .
N2 N3 C8 111.19(14) . .
N2 N3 Pd1 121.68(11) . 2_666
C8 N3 Pd1 127.05(12) . 2_666
C6 C1 C2 119.68(17) . .
C6 C1 N1 119.95(16) . .
C2 C1 N1 120.37(16) . .
C3 C2 C1 119.86(17) . .
C2 C3 C4 121.25(17) . .
C5 C4 C3 117.97(17) . .
C5 C4 C7 121.61(18) . .
C3 C4 C7 120.41(18) . .
C6 C5 C4 121.45(18) . .
C1 C6 C5 119.77(17) . .
N3 C8 C13 123.15(16) . .
N3 C8 C9 119.33(17) . .
C13 C8 C9 117.52(17) . .
C10 C9 C8 121.54(19) . .
C9 C10 C11 120.80(19) . .
C12 C11 C10 118.83(19) . .
C11 C12 C13 122.1(2) . .
C12 C13 C8 119.14(17) . .
C12 C13 C14 116.81(17) . .
C8 C13 C14 124.04(16) . .
O1 C14 O2 119.20(17) . .
O1 C14 C13 127.75(17) . .
O2 C14 C13 112.99(16) . .
C14 O1 Pd1 125.66(12) . 2_666
C14 O2 C15 115.61(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N3 2.0264(15) 2_666
Pd1 N1 2.0302(14) .
Pd1 O1 2.1641(13) 2_666
Pd1 Pd1 2.4202(3) 2_666
N1 N2 1.289(2) .
N1 C1 1.434(2) .
N2 N3 1.321(2) .
N3 C8 1.412(2) .
N3 Pd1 2.0264(15) 2_666
C1 C6 1.384(3) .
C1 C2 1.393(2) .
C2 C3 1.382(3) .
C3 C4 1.393(3) .
C4 C5 1.390(3) .
C4 C7 1.513(3) .
C5 C6 1.386(3) .
C8 C13 1.409(3) .
C8 C9 1.417(3) .
C9 C10 1.376(3) .
C10 C11 1.384(3) .
C11 C12 1.373(3) .
C12 C13 1.410(3) .
C13 C14 1.475(3) .
C14 O1 1.217(2) .
C14 O2 1.333(2) .
C15 O2 1.451(2) .
O1 Pd1 2.1641(13) 2_666
