#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:32:26 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179185 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/31/4313135.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_4313135
loop_
_publ_author_name
'Mohammed Fettouhi'
'Bassam El Ali'
'Mohammed Morsy'
'Stéphane Golhen'
'Lahcène Ouahab'
'Boris Le Guennic'
'Jean-Yves Saillard'
'Nathalie Daro'
'Jean-Pascal Sutter'
'Edmond Amouyal'
_publ_section_title
;
 Metal-Dependent Ferro- Versus Antiferromagnetic Interactions in Molecular
 Crystals of Square Planar {M(II) Imino-Nitroxide Radical} Complexes (M =
 Pt, Pd)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1316
_journal_page_last               1321
_journal_paper_doi               10.1021/ic0255813
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C12 H16 Cl2 N3 O Pd'
_chemical_formula_weight         395.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.524(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.900(3)
_cell_length_b                   17.907(9)
_cell_length_c                   10.299(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.61
_cell_measurement_theta_min      9.87
_cell_volume                     1456.9(10)
_computing_cell_refinement       'Nonius CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        MolEN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       θ-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1810
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3393
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.27
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.635
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_refine_diff_density_max         3.084
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1310P)²+2.3278P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1856
_refine_ls_wR_factor_ref         0.2066
_reflns_number_gt                2237
_reflns_number_total             3168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255813-2_s1_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1457.0(10)
_cod_database_code               4313135
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.73687(7) 0.00560(3) 0.42371(5) 0.0454(2) Uani 1 1 d . . .
Cl1 Cl 0.7632(4) 0.02055(14) 0.2066(2) 0.0758(7) Uani 1 1 d . . .
Cl2 Cl 0.7090(4) 0.13372(12) 0.4401(2) 0.0734(7) Uani 1 1 d . . .
N1 N 0.7263(9) -0.0118(3) 0.6194(6) 0.0486(15) Uani 1 1 d . . .
N2 N 0.7592(7) -0.1064(3) 0.4293(5) 0.0423(13) Uani 1 1 d . . .
N3 N 0.7853(8) -0.2082(4) 0.5534(5) 0.0475(14) Uani 1 1 d . . .
O1 O 0.7930(8) -0.2475(3) 0.6554(5) 0.0680(16) Uani 1 1 d . . .
C1 C 0.7057(11) 0.0406(6) 0.7099(9) 0.063(2) Uani 1 1 d . . .
H1 H 0.6881 0.0899 0.6847 0.075 Uiso 1 1 calc R . .
C2 C 0.7099(15) 0.0228(7) 0.8422(9) 0.081(3) Uani 1 1 d . . .
H2 H 0.6905 0.0595 0.9042 0.097 Uiso 1 1 calc R . .
C3 C 0.7424(13) -0.0480(6) 0.8789(8) 0.070(3) Uani 1 1 d . . .
H3 H 0.7512 -0.0600 0.9665 0.084 Uiso 1 1 calc R . .
C4 C 0.7629(10) -0.1029(5) 0.7855(7) 0.0557(19) Uani 1 1 d . . .
H4 H 0.7836 -0.1522 0.8093 0.067 Uiso 1 1 calc R . .
C5 C 0.7517(9) -0.0828(4) 0.6571(6) 0.0420(15) Uani 1 1 d . . .
C6 C 0.7662(8) -0.1329(4) 0.5466(6) 0.0405(15) Uani 1 1 d . . .
C7 C 0.7804(10) -0.2424(4) 0.4206(7) 0.0467(16) Uani 1 1 d . . .
C8 C 0.7863(9) -0.1690(4) 0.3357(7) 0.0453(16) Uani 1 1 d . . .
C9 C 0.6172(11) -0.2853(5) 0.4113(9) 0.060(2) Uani 1 1 d . . .
H9A H 0.6114 -0.3204 0.4816 0.090 Uiso 1 1 calc R . .
H9B H 0.6125 -0.3117 0.3302 0.090 Uiso 1 1 calc R . .
H9C H 0.5235 -0.2513 0.4161 0.090 Uiso 1 1 calc R . .
C10 C 0.9305(11) -0.2937(5) 0.4062(8) 0.062(2) Uani 1 1 d . . .
H10A H 1.0295 -0.2702 0.4423 0.092 Uiso 1 1 calc R . .
H10B H 0.9482 -0.3039 0.3159 0.092 Uiso 1 1 calc R . .
H10C H 0.9092 -0.3396 0.4513 0.092 Uiso 1 1 calc R . .
C11 C 0.6481(16) -0.1662(6) 0.2326(10) 0.092(4) Uani 1 1 d . . .
H11A H 0.5400 -0.1610 0.2735 0.138 Uiso 1 1 calc R . .
H11B H 0.6497 -0.2116 0.1828 0.138 Uiso 1 1 calc R . .
H11C H 0.6670 -0.1244 0.1762 0.138 Uiso 1 1 calc R . .
C12 C 0.9598(13) -0.1548(6) 0.2719(10) 0.081(3) Uani 1 1 d . . .
H12A H 0.9558 -0.1087 0.2244 0.122 Uiso 1 1 calc R . .
H12B H 0.9852 -0.1950 0.2137 0.122 Uiso 1 1 calc R . .
H12C H 1.0459 -0.1518 0.3380 0.122 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'
O O 0.0106 0.0060 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd N1 79.9(2) . . ?
N2 Pd Cl1 97.88(16) . . ?
N1 Pd Cl1 176.5(2) . . ?
N2 Pd Cl2 174.16(17) . . ?
N1 Pd Cl2 94.30(19) . . ?
Cl1 Pd Cl2 87.95(9) . . ?
C1 N1 C5 118.9(7) . . ?
C1 N1 Pd 126.1(6) . . ?
C5 N1 Pd 115.0(5) . . ?
C6 N2 C8 108.8(6) . . ?
C6 N2 Pd 113.1(5) . . ?
C8 N2 Pd 137.8(4) . . ?
O1 N3 C6 126.8(6) . . ?
O1 N3 C7 122.1(6) . . ?
C6 N3 C7 110.9(5) . . ?
N1 C1 C2 121.2(9) . . ?
C3 C2 C1 119.4(9) . . ?
C2 C3 C4 119.8(8) . . ?
C5 C4 C3 118.4(9) . . ?
N1 C5 C4 122.3(7) . . ?
N1 C5 C6 111.7(6) . . ?
C4 C5 C6 126.0(7) . . ?
N2 C6 N3 114.5(6) . . ?
N2 C6 C5 120.0(7) . . ?
N3 C6 C5 125.5(6) . . ?
N3 C7 C9 106.4(6) . . ?
N3 C7 C10 109.0(6) . . ?
C9 C7 C10 110.9(7) . . ?
N3 C7 C8 99.5(5) . . ?
C9 C7 C8 114.8(6) . . ?
C10 C7 C8 115.2(7) . . ?
N2 C8 C11 108.8(7) . . ?
N2 C8 C12 106.5(6) . . ?
C11 C8 C12 109.4(8) . . ?
N2 C8 C7 105.1(5) . . ?
C11 C8 C7 113.0(7) . . ?
C12 C8 C7 113.7(7) . . ?
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
Pd N2 2.015(6) . ?
Pd N1 2.042(7) . ?
Pd Cl1 2.263(2) . ?
Pd Cl2 2.311(2) . ?
N1 C1 1.334(11) . ?
N1 C5 1.344(9) . ?
N2 C6 1.299(8) . ?
N2 C8 1.494(9) . ?
N3 O1 1.265(8) . ?
N3 C6 1.358(10) . ?
N3 C7 1.499(9) . ?
C1 C2 1.400(14) . ?
C2 C3 1.346(16) . ?
C3 C4 1.386(13) . ?
C4 C5 1.373(10) . ?
C5 C6 1.454(9) . ?
C7 C9 1.503(11) . ?
C7 C10 1.509(10) . ?
C7 C8 1.580(10) . ?
C8 C11 1.517(11) . ?
C8 C12 1.546(11) . ?
