#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/76/4317620.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_4317620
loop_
_publ_author_name
'Matthew D. Hall'
'Timothy W. Failes'
'David E. Hibbs'
'Trevor W. Hambley'
_publ_contact_author_address
;
    Centre for Heavy Metals Research
    School of Chemistry
    The University of Sydney
    N.S.W. 2006
    Australia
;
_publ_contact_author_email       ' t.hambley@chem.usyd.edu.au'
_publ_contact_author_fax         ' 61-2-9351-3329'
_publ_contact_author_name        ' Trevor W. Hambley'
_publ_contact_author_phone       ' 61-2-9351-2830'
_publ_section_title
;
 Structural Investigations of Palladium(II) and Platinum(II) Complexes of
 Salicylhydroxamic Acid
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1223
_journal_page_last               1228
_journal_paper_doi               10.1021/ic010760q
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C26 H40 N6 O10 Pd'
_chemical_formula_weight         703.04
_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'
_audit_creation_date             19101-06-14
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                99.213(3)
_cell_angle_beta                 90.669(3)
_cell_angle_gamma                109.767(3)
_cell_formula_units_Z            1
_cell_length_a                   7.066(1)
_cell_length_b                   9.842(2)
_cell_length_c                   12.385(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    273.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     798.1(2)
_computing_cell_refinement       'd*TREK (MSC, 1996-1998)'
_computing_data_collection       'd*TREK (MSC, 1996-1998)'
_computing_data_reduction        'd*TREK (MSC, 1996-1998)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      273.2
_diffrn_detector_area_resol_mean 11.76
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03676
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8552
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_description       unknown
_exptl_crystal_F_000             364.00
_exptl_crystal_size_max          0.00
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.249
_refine_ls_goodness_of_fit_ref   1.374
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2910
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.0120
_refine_ls_shift/su_mean         0.0430
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0354
_refine_ls_wR_factor_ref         0.0344
_reflns_number_gt                2910
_reflns_number_total             3698
_reflns_threshold_expression     I>2.50σ(I)
_cod_data_source_file            ic010760q_1.cif
_cod_data_source_block           mh2_in_P-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C26 H40 N6 O10 Pd '
_cod_database_code               4317620
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -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_occupancy
_atom_site_refinement_flags
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Pd(1) 0.0000 0.0000 0.0000 0.0375(1) 0.500 S Uani d ?
O(1) 0.1391(4) 0.2860(3) -0.0671(2) 0.0520(9) 1.000 . Uani d ?
O(2) 0.2018(4) 0.4513(3) 0.1214(2) 0.0594(9) 1.000 . Uani d ?
O(3) -0.0290(4) -0.0036(3) 0.1575(2) 0.0475(8) 1.000 . Uani d ?
O(4) 0.3126(4) 0.6207(3) -0.0192(2) 0.067(1) 1.000 . Uani d ?
O(5) 0.2943(4) 0.2831(3) -0.2912(2) 0.072(1) 1.000 . Uani d ?
N(1) 0.0990(4) 0.2171(3) 0.0246(2) 0.0370(9) 1.000 . Uani d ?
N(2) 0.3756(5) 0.7098(4) -0.1761(2) 0.050(1) 1.000 . Uani d ?
N(3) 0.5800(5) 0.2306(4) -0.3123(3) 0.057(1) 1.000 . Uani d ?
C(1) 0.1349(5) 0.3080(4) 0.1165(3) 0.037(1) 1.000 . Uani d ?
C(2) 0.1026(5) 0.2602(4) 0.2228(3) 0.037(1) 1.000 . Uani d ?
C(3) 0.0243(5) 0.1114(4) 0.2367(3) 0.038(1) 1.000 . Uani d ?
C(4) 0.0025(6) 0.0829(5) 0.3454(3) 0.047(1) 1.000 . Uani d ?
C(5) 0.0563(6) 0.1922(5) 0.4348(3) 0.053(1) 1.000 . Uani d ?
C(6) 0.1333(7) 0.3366(5) 0.4206(3) 0.057(1) 1.000 . Uani d ?
C(7) 0.1546(6) 0.3693(5) 0.3162(3) 0.048(1) 1.000 . Uani d ?
C(8) 0.3142(6) 0.6024(4) -0.1198(3) 0.054(1) 1.000 . Uani d ?
C(9) 0.3703(7) 0.6815(5) -0.2950(3) 0.077(2) 1.000 . Uani d ?
C(10) 0.4459(6) 0.8603(5) -0.1227(4) 0.067(2) 1.000 . Uani d ?
C(11) 0.4405(7) 0.2637(4) -0.2547(3) 0.057(1) 1.000 . Uani d ?
C(12) 0.5659(8) 0.2177(6) -0.4304(4) 0.094(2) 1.000 . Uani d ?
C(13) 0.7521(8) 0.2120(6) -0.2615(4) 0.089(2) 1.000 . Uani d ?
H(1) -0.064(5) -0.012(4) 0.350(3) 0.05(1) 1.000 . Uiso d ?
H(2) 0.036(5) 0.161(4) 0.501(3) 0.06(1) 1.000 . Uiso d ?
H(3) 0.174(5) 0.413(4) 0.479(3) 0.07(1) 1.000 . Uiso d ?
H(4) 0.206(4) 0.467(3) 0.306(2) 0.034(9) 1.000 . Uiso d ?
H(5) 0.2683 0.5047 -0.1590 0.065 1.000 . Uiso c ?
H(6) 0.2356 0.6290 -0.3241 0.092 1.000 . Uiso c ?
H(7) 0.4187 0.7721 -0.3210 0.092 1.000 . Uiso c ?
H(8) 0.4531 0.6252 -0.3176 0.092 1.000 . Uiso c ?
H(9) 0.5592 0.8780 -0.0735 0.081 1.000 . Uiso c ?
H(10) 0.4836 0.9222 -0.1761 0.081 1.000 . Uiso c ?
H(11) 0.3414 0.8805 -0.0830 0.081 1.000 . Uiso c ?
H(12) 0.4568 0.2732 -0.1772 0.069 1.000 . Uiso c ?
H(13) 0.4454 0.1407 -0.4602 0.113 1.000 . Uiso c ?
H(14) 0.5642 0.3073 -0.4491 0.113 1.000 . Uiso c ?
H(15) 0.6788 0.1968 -0.4594 0.113 1.000 . Uiso c ?
H(16) 0.7075 0.1348 -0.2203 0.106 1.000 . Uiso c ?
H(17) 0.8341 0.1886 -0.3165 0.106 1.000 . Uiso c ?
H(18) 0.8281 0.3003 -0.2140 0.106 1.000 . Uiso c ?
H(19) 0.121(5) 0.203(4) -0.118(3) 0.06(1) 1.000 . Uiso d ?
H(20) 0.233(6) 0.491(4) 0.066(3) 0.07(1) 1.000 . Uiso d ?
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 26 0.002 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H 0 40 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N 0 6 0.004 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O 0 10 0.008 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Pd 0 1 -1.177 1.007
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(3) Pd(1) O(3) 180.00 . . 2 yes
O(3) Pd(1) N(1) 92.2(1) . . . yes
O(3) Pd(1) N(1) 87.8(1) . . 2 yes
O(3) Pd(1) N(1) 87.8(1) 2 . . yes
O(3) Pd(1) N(1) 92.2(1) 2 . 2 yes
N(1) Pd(1) N(1) 180.00 . . 2 yes
N(1) O(1) H(19) 97(2) . . . no
C(1) O(2) H(20) 123(3) . . . no
Pd(1) O(3) C(3) 126.1(2) . . . yes
Pd(1) N(1) O(1) 118.0(2) . . . yes
Pd(1) N(1) C(1) 128.6(2) . . . yes
O(1) N(1) C(1) 113.4(3) . . . yes
C(8) N(2) C(9) 121.5(4) . . . yes
C(8) N(2) C(10) 121.3(3) . . . yes
C(9) N(2) C(10) 117.2(3) . . . yes
C(11) N(3) C(12) 119.6(4) . . . yes
C(11) N(3) C(13) 122.3(4) . . . yes
C(12) N(3) C(13) 118.1(4) . . . yes
O(2) C(1) N(1) 122.4(3) . . . yes
O(2) C(1) C(2) 114.8(3) . . . yes
N(1) C(1) C(2) 122.8(3) . . . yes
C(1) C(2) C(3) 124.3(3) . . . yes
C(1) C(2) C(7) 117.2(3) . . . yes
C(3) C(2) C(7) 118.5(3) . . . yes
O(3) C(3) C(2) 125.9(3) . . . yes
O(3) C(3) C(4) 116.6(3) . . . yes
C(2) C(3) C(4) 117.5(3) . . . yes
C(3) C(4) C(5) 122.4(4) . . . yes
C(3) C(4) H(1) 114(2) . . . no
C(5) C(4) H(1) 123(2) . . . no
C(4) C(5) C(6) 119.7(4) . . . yes
C(4) C(5) H(2) 115(2) . . . no
C(6) C(5) H(2) 125(2) . . . no
C(5) C(6) C(7) 119.8(4) . . . yes
C(5) C(6) H(3) 122(2) . . . no
C(7) C(6) H(3) 118(2) . . . no
C(2) C(7) C(6) 122.0(4) . . . yes
C(2) C(7) H(4) 118(2) . . . no
C(6) C(7) H(4) 120(2) . . . no
O(4) C(8) N(2) 124.0(4) . . . yes
O(4) C(8) H(5) 118.0 . . . no
N(2) C(8) H(5) 118.0 . . . no
N(2) C(9) H(6) 109.5 . . . no
N(2) C(9) H(7) 109.5 . . . no
N(2) C(9) H(8) 109.5 . . . no
H(6) C(9) H(7) 109.4 . . . no
H(6) C(9) H(8) 109.5 . . . no
H(7) C(9) H(8) 109.5 . . . no
N(2) C(10) H(9) 109.5 . . . no
N(2) C(10) H(10) 109.5 . . . no
N(2) C(10) H(11) 109.5 . . . no
H(9) C(10) H(10) 109.5 . . . no
H(9) C(10) H(11) 109.4 . . . no
H(10) C(10) H(11) 109.4 . . . no
O(5) C(11) N(3) 126.1(4) . . . yes
O(5) C(11) H(12) 117.0 . . . no
N(3) C(11) H(12) 117.0 . . . no
N(3) C(12) H(13) 109.5 . . . no
N(3) C(12) H(14) 109.5 . . . no
N(3) C(12) H(15) 109.5 . . . no
H(13) C(12) H(14) 109.5 . . . no
H(13) C(12) H(15) 109.5 . . . no
H(14) C(12) H(15) 109.5 . . . no
N(3) C(13) H(16) 109.5 . . . no
N(3) C(13) H(17) 109.5 . . . no
N(3) C(13) H(18) 109.5 . . . no
H(16) C(13) H(17) 109.5 . . . no
H(16) C(13) H(18) 109.5 . . . no
H(17) C(13) H(18) 109.4 . . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd(1) O(3) 1.968(2) . . yes
Pd(1) O(3) 1.968(2) . 2 yes
Pd(1) N(1) 1.981(3) . . yes
Pd(1) N(1) 1.981(3) . 2 yes
O(1) N(1) 1.398(3) . . yes
O(1) H(19) 0.92(4) . . no
O(2) C(1) 1.319(4) . . yes
O(2) H(20) 0.83(4) . . no
O(3) C(3) 1.316(4) . . yes
O(4) C(8) 1.230(4) . . yes
O(5) C(11) 1.208(4) . . yes
N(1) C(1) 1.294(4) . . yes
N(2) C(8) 1.313(4) . . yes
N(2) C(9) 1.451(5) . . yes
N(2) C(10) 1.435(5) . . yes
N(3) C(11) 1.321(5) . . yes
N(3) C(12) 1.446(5) . . yes
N(3) C(13) 1.442(5) . . yes
C(1) C(2) 1.463(4) . . yes
C(2) C(3) 1.419(4) . . yes
C(2) C(7) 1.397(5) . . yes
C(3) C(4) 1.418(4) . . yes
C(4) C(5) 1.364(5) . . yes
C(4) H(1) 0.90(3) . . no
C(5) C(6) 1.381(5) . . yes
C(5) H(2) 0.91(3) . . no
C(6) C(7) 1.379(5) . . yes
C(6) H(3) 0.92(4) . . no
C(7) H(4) 0.94(3) . . no
C(8) H(5) 0.95 . . no
C(9) H(6) 0.95 . . no
C(9) H(7) 0.95 . . no
C(9) H(8) 0.95 . . no
C(10) H(9) 0.95 . . no
C(10) H(10) 0.95 . . no
C(10) H(11) 0.95 . . no
C(11) H(12) 0.95 . . no
C(12) H(13) 0.95 . . no
C(12) H(14) 0.95 . . no
C(12) H(15) 0.95 . . no
C(13) H(16) 0.95 . . no
C(13) H(17) 0.95 . . no
C(13) H(18) 0.95 . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O(1) O(5) 2.995(4) . . no
O(1) O(4) 3.055(4) . . no
O(1) C(8) 3.118(5) . . no
O(1) C(11) 3.201(5) . . no
O(1) C(13) 3.426(6) . 1_455 no
O(2) O(4) 2.550(4) . . no
O(2) C(11) 3.256(5) . 2_665 no
O(2) C(13) 3.393(6) . 2_665 no
O(2) N(3) 3.471(4) . 2_665 no
O(2) C(8) 3.502(5) . 2_565 no
O(2) C(8) 3.527(5) . . no
O(3) O(5) 3.445(4) . 2 no
O(3) C(11) 3.534(4) . 2 no
O(5) C(4) 3.451(5) . 2 no
O(5) C(8) 3.459(5) . . no
N(2) C(2) 3.539(4) . 2_565 no
N(2) C(1) 3.596(4) . 2_665 no
C(1) C(8) 3.569(5) . 2_565 no
C(7) C(9) 3.565(6) . 2_665 no
C(7) C(9) 3.572(6) . 2_565 no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd(1) O(3) C(3) C(2) . . . . 3.6(5) no
Pd(1) O(3) C(3) C(4) . . . . -175.8(2) no
Pd(1) O(3) C(3) C(2) . 2 2 2 -3.6(5) no
Pd(1) O(3) C(3) C(4) . 2 2 2 175.8(2) no
Pd(1) N(1) C(1) O(2) . . . . 179.7(2) no
Pd(1) N(1) C(1) C(2) . . . . -1.0(5) no
Pd(1) N(1) C(1) O(2) . 2 2 2 -179.7(2) no
Pd(1) N(1) C(1) C(2) . 2 2 2 1.0(5) no
O(1) N(1) Pd(1) O(3) . . . . -177.2(2) no
O(1) N(1) Pd(1) O(3) . . . 2 2.8(2) no
O(1) N(1) Pd(1) N(1) . . . 2 2.8(2) no
O(1) N(1) C(1) O(2) . . . . 0.3(5) no
O(1) N(1) C(1) C(2) . . . . 179.7(3) no
O(2) C(1) C(2) C(3) . . . . 177.5(3) no
O(2) C(1) C(2) C(7) . . . . -3.0(5) no
O(3) Pd(1) O(3) C(3) . . 2 2 -3.0(5) no
O(3) Pd(1) N(1) C(1) . . . . 3.4(3) no
O(3) Pd(1) N(1) C(1) . . 2 2 176.6(3) no
O(3) C(3) C(2) C(1) . . . . 0.4(5) no
O(3) C(3) C(2) C(7) . . . . -179.0(3) no
O(3) C(3) C(4) C(5) . . . . 178.6(4) no
O(4) C(8) N(2) C(9) . . . . -178.8(4) no
O(4) C(8) N(2) C(10) . . . . -0.4(6) no
O(5) C(11) N(3) C(12) . . . . 1.3(7) no
O(5) C(11) N(3) C(13) . . . . 178.8(4) no
N(1) Pd(1) O(3) C(3) . . . . -4.7(3) no
N(1) Pd(1) O(3) C(3) . . 2 2 -175.3(3) no
N(1) Pd(1) N(1) C(1) . . 2 2 -175.3(3) no
N(1) C(1) C(2) C(3) . . . . -1.8(5) no
N(1) C(1) C(2) C(7) . . . . 177.6(3) no
C(1) C(2) C(3) C(4) . . . . 179.8(3) no
C(1) C(2) C(7) C(6) . . . . -179.0(3) no
C(2) C(3) C(4) C(5) . . . . -0.9(5) no
C(2) C(7) C(6) C(5) . . . . -0.8(6) no
C(3) C(2) C(7) C(6) . . . . 0.4(6) no
C(3) C(4) C(5) C(6) . . . . 0.6(6) no
C(4) C(3) C(2) C(7) . . . . 0.4(5) no
C(4) C(5) C(6) C(7) . . . . 0.2(7) no
