#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:29:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179330 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/27/4322774.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_4322774
loop_
_publ_author_name
'Victor I. Ovcharenko'
'Sergei V. Fokin'
'Vladimir A. Reznikov'
'Vladimir N. Ikorskii'
'Galina V. Romanenko'
'Renad Z. Sagdeev'
_publ_section_title
;
 Nonclassical Packing of Metal Dioximates. Superexchange through a
 Diamagnetic Metal Cation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2104
_journal_page_last               2105
_journal_paper_doi               10.1021/ic971523j
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C16 H26 N6 O6 Pd'
_chemical_formula_weight         504.83
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.91(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.079(2)
_cell_length_b                   11.329(2)
_cell_length_c                   12.078(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1039.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.836
_diffrn_measured_fraction_theta_max 0.836
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2173
_diffrn_reflns_theta_full        27.05
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.938
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             516
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.203
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0299P)²+1.0499P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                1521
_reflns_number_total             2014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic971523j_2.cif
_cod_data_source_block           f75n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+1.0499P] 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^)+(0.0299P)^2^+1.0499P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322774
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.0000 0.5000 0.0000 0.02650(14) Uani 1 d S . .
N3 N -0.1790(4) 0.4003(3) 0.0350(3) 0.0285(7) Uani 1 d . . .
O31 O -0.3483(3) 0.4299(3) 0.0053(3) 0.0389(7) Uani 1 d . . .
C4 C -0.1115(5) 0.3060(3) 0.0934(3) 0.0289(8) Uani 1 d . . .
C3 C -0.1914(5) 0.2084(3) 0.1432(4) 0.0312(8) Uani 1 d . . .
C31 C -0.3442(7) 0.1463(5) 0.0502(5) 0.0464(11) Uani 1 d . . .
H311 H -0.447(6) 0.191(4) 0.029(4) 0.050(14) Uiso 1 d . . .
H312 H -0.320(5) 0.129(4) -0.018(4) 0.033(12) Uiso 1 d . . .
H313 H -0.369(7) 0.072(5) 0.080(5) 0.072(17) Uiso 1 d . . .
C32 C -0.2413(8) 0.2472(5) 0.2481(5) 0.0485(12) Uani 1 d . . .
H321 H -0.270(7) 0.175(5) 0.288(5) 0.077(18) Uiso 1 d . . .
H322 H -0.143(7) 0.271(5) 0.306(5) 0.060(16) Uiso 1 d . . .
H323 H -0.329(6) 0.296(4) 0.227(4) 0.033(12) Uiso 1 d . . .
N2 N -0.0344(5) 0.1271(3) 0.1834(3) 0.0405(8) Uani 1 d . . .
O21 O -0.0453(4) 0.0262(3) 0.2252(4) 0.0623(10) Uani 1 d . . .
C2 C 0.1378(5) 0.1758(4) 0.1847(4) 0.0356(9) Uani 1 d . . .
C21 C 0.2185(9) 0.0913(5) 0.1204(7) 0.0603(16) Uani 1 d . . .
H211 H 0.325(7) 0.112(4) 0.121(4) 0.055(15) Uiso 1 d . . .
H212 H 0.137(7) 0.085(5) 0.043(5) 0.052(16) Uiso 1 d . . .
H213 H 0.235(8) 0.014(6) 0.160(6) 0.10(2) Uiso 1 d . . .
C22 C 0.2598(8) 0.1982(7) 0.3111(5) 0.0644(17) Uani 1 d . . .
H221 H 0.269(8) 0.129(6) 0.351(6) 0.09(2) Uiso 1 d . . .
H222 H 0.205(9) 0.238(7) 0.357(7) 0.11(3) Uiso 1 d . . .
H223 H 0.377(8) 0.240(5) 0.318(5) 0.077(17) Uiso 1 d . . .
C1 C 0.0761(5) 0.2885(3) 0.1188(3) 0.0297(8) Uani 1 d . . .
N1 N 0.1580(4) 0.3704(3) 0.0836(3) 0.0282(7) Uani 1 d . . .
O11 O 0.3318(3) 0.3665(3) 0.1039(3) 0.0396(7) Uani 1 d . . .
H11 H 0.363(13) 0.445(8) 0.080(9) 0.18(4) Uiso 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
_geom_angle_publ_flag
N1 Pd N1 180.0 3_565 . ?
N1 Pd N3 81.93(12) 3_565 3_565 ?
N1 Pd N3 98.07(12) . 3_565 ?
N1 Pd N3 98.07(12) 3_565 . ?
N1 Pd N3 81.93(12) . . ?
N3 Pd N3 180.0 3_565 . ?
C4 N3 O31 123.9(3) . . ?
C4 N3 Pd 112.5(2) . . ?
O31 N3 Pd 123.6(2) . . ?
N3 C4 C1 116.3(3) . . ?
N3 C4 C3 131.8(3) . . ?
C1 C4 C3 111.9(3) . . ?
C4 C3 N2 98.6(3) . . ?
C4 C3 C32 113.1(4) . . ?
N2 C3 C32 109.9(3) . . ?
C4 C3 C31 113.2(4) . . ?
N2 C3 C31 109.6(4) . . ?
C32 C3 C31 111.6(4) . . ?
C3 C31 H311 112(3) . . ?
C3 C31 H312 113(3) . . ?
H311 C31 H312 108(4) . . ?
C3 C31 H313 110(3) . . ?
H311 C31 H313 107(4) . . ?
H312 C31 H313 106(4) . . ?
C3 C32 H321 109(3) . . ?
C3 C32 H322 109(3) . . ?
H321 C32 H322 99(4) . . ?
C3 C32 H323 111(3) . . ?
H321 C32 H323 111(4) . . ?
H322 C32 H323 117(4) . . ?
O21 N2 C2 121.4(3) . . ?
O21 N2 C3 121.0(3) . . ?
C2 N2 C3 117.2(3) . . ?
N2 C2 C1 99.7(3) . . ?
N2 C2 C21 109.0(4) . . ?
C1 C2 C21 112.9(4) . . ?
N2 C2 C22 110.7(4) . . ?
C1 C2 C22 111.9(4) . . ?
C21 C2 C22 111.9(5) . . ?
C2 C21 H211 115(3) . . ?
C2 C21 H212 106(3) . . ?
H211 C21 H212 112(5) . . ?
C2 C21 H213 109(4) . . ?
H211 C21 H213 105(5) . . ?
H212 C21 H213 110(5) . . ?
C2 C22 H221 107(4) . . ?
C2 C22 H222 113(4) . . ?
H221 C22 H222 94(6) . . ?
C2 C22 H223 114(3) . . ?
H221 C22 H223 116(5) . . ?
H222 C22 H223 110(6) . . ?
N1 C1 C4 116.5(3) . . ?
N1 C1 C2 132.2(3) . . ?
C4 C1 C2 111.3(3) . . ?
C1 N1 O11 122.5(3) . . ?
C1 N1 Pd 112.7(2) . . ?
O11 N1 Pd 124.7(2) . . ?
N1 O11 H11 106(6) . . ?
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 N1 1.982(3) 3_565 ?
Pd N1 1.982(3) . ?
Pd N3 1.990(3) 3_565 ?
Pd N3 1.990(3) . ?
N3 C4 1.295(5) . ?
N3 O31 1.333(4) . ?
C4 C1 1.454(5) . ?
C4 C3 1.504(5) . ?
C3 N2 1.507(5) . ?
C3 C32 1.520(6) . ?
C3 C31 1.528(6) . ?
C31 H311 0.93(5) . ?
C31 H312 0.93(4) . ?
C31 H313 0.96(6) . ?
C32 H321 1.02(6) . ?
C32 H322 0.90(5) . ?
C32 H323 0.87(4) . ?
N2 O21 1.266(4) . ?
N2 C2 1.492(5) . ?
C2 C1 1.497(5) . ?
C2 C21 1.513(7) . ?
C2 C22 1.530(7) . ?
C21 H211 0.89(5) . ?
C21 H212 0.94(5) . ?
C21 H213 0.98(7) . ?
C22 H221 0.91(7) . ?
C22 H222 0.93(7) . ?
C22 H223 1.04(6) . ?
C1 N1 1.292(5) . ?
N1 O11 1.342(4) . ?
O11 H11 0.99(9) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H11 O31 0.99(9) 1.74(10) 2.683(4) 159(9) 3_565
