#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:25:00 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180504 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/73/7217350.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_7217350
loop_
_publ_author_name
'Fortea-Pérez, Francisco R.'
'Marino, Nadia'
'Armentano, Donatella'
'De Munno, Giovanni'
'Julve, Miguel'
'Stiriba, Salah-Eddine'
_publ_section_title
;
 Solid-state cis--trans isomerism in bis(oxamato)palladate(ii) complexes:
 synthesis, structural studies and catalytic activity
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              6971
_journal_paper_doi               10.1039/C4CE00669K
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C20 H22 N2 Na2 O8 Pd'
_chemical_formula_sum            'C20 H22 N2 Na2 O8 Pd'
_chemical_formula_weight         570.77
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.888(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.889(2)
_cell_length_b                   14.4316(18)
_cell_length_c                   13.6143(19)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      3.29
_cell_volume                     2435.6(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25193
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.100
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.332
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2298
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0164
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0383P)²+1.7111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2208
_reflns_number_total             2298
_reflns_threshold_expression     'I > 2σ(I)'
_cod_duplicate_entry             7216172
_cod_data_source_file            c4ce00669k2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2435.7(6)
_cod_database_code               7217350
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.877
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.2500 0.2500 0.2500 0.01444(10) Uani 1 2 d S . P
N1 N 0.17753(11) 0.35562(10) 0.30274(11) 0.0171(3) Uani 1 1 d . . .
O1 O 0.38329(9) 0.32351(9) 0.31583(10) 0.0199(3) Uani 1 1 d . . .
O2 O 0.43487(9) 0.44611(8) 0.41714(9) 0.0179(3) Uani 1 1 d . . .
O3 O 0.22157(10) 0.49546(8) 0.38858(9) 0.0177(3) Uani 1 1 d . . .
C1 C 0.36403(13) 0.39691(12) 0.36296(13) 0.0157(3) Uani 1 1 d . . .
C2 C 0.24413(13) 0.42135(12) 0.35113(12) 0.0154(3) Uani 1 1 d . . .
C3 C 0.06310(13) 0.36231(12) 0.28860(14) 0.0192(4) Uani 1 1 d . . .
C4 C 0.01556(15) 0.30267(13) 0.34627(15) 0.0238(4) Uani 1 1 d . . .
C5 C -0.09675(16) 0.30589(16) 0.32888(18) 0.0316(5) Uani 1 1 d . . .
H5 H -0.1305 0.2666 0.3669 0.038 Uiso 1 1 calc R U .
C6 C -0.15945(16) 0.36609(16) 0.25653(18) 0.0353(5) Uani 1 1 d . . .
H6 H -0.2355 0.3675 0.2455 0.042 Uiso 1 1 calc R U .
C7 C -0.11139(16) 0.42385(15) 0.20072(17) 0.0334(5) Uani 1 1 d . . .
H7 H -0.1551 0.4644 0.1514 0.040 Uiso 1 1 calc R U .
C8 C 0.00109(15) 0.42362(14) 0.21564(15) 0.0254(4) Uani 1 1 d . . .
C9 C 0.0829(2) 0.23695(15) 0.42397(19) 0.0293(5) Uani 1 1 d . . .
H9A H 0.1161 0.1908 0.3893 0.044 Uiso 1 1 calc R U .
H9B H 0.0370 0.2056 0.4603 0.044 Uiso 1 1 calc R U .
H9C H 0.1395 0.2717 0.4728 0.044 Uiso 1 1 calc R U .
C10 C 0.05367(18) 0.48715(16) 0.15550(17) 0.0352(5) Uani 1 1 d . . .
H10A H -0.0018 0.5245 0.1085 0.053 Uiso 1 1 calc R U .
H10B H 0.0923 0.4501 0.1164 0.053 Uiso 1 1 calc R U .
H10C H 0.1047 0.5281 0.2025 0.053 Uiso 1 1 calc R U .
Na1 Na 0.38012(5) 0.55977(5) 0.51436(5) 0.01683(16) Uani 1 1 d . . .
O1W O 0.39373(11) 0.70828(10) 0.58547(11) 0.0276(3) Uani 1 1 d D . .
H1W1 H 0.363(2) 0.7492(14) 0.611(2) 0.041 Uiso 1 1 d D U .
H1W2 H 0.4581(9) 0.7094(19) 0.6194(18) 0.041 Uiso 1 1 d D U .
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'
Na Na 0.0362 0.0249 '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
O1 Pd1 O1 180.0 . 7
O1 Pd1 N1 82.25(5) . .
O1 Pd1 N1 97.75(5) 7 .
O1 Pd1 N1 97.75(5) . 7
O1 Pd1 N1 82.25(5) 7 7
N1 Pd1 N1 180.0 . 7
C2 N1 C3 121.27(14) . .
C2 N1 Pd1 114.63(11) . .
C3 N1 Pd1 124.09(11) . .
C1 O1 Pd1 113.31(10) . .
C1 O2 Na1 137.31(11) . 5_666
C1 O2 Na1 117.09(11) . .
Na1 O2 Na1 103.63(5) 5_666 .
C2 O3 Na1 144.27(11) . 2_556
C2 O3 Na1 111.36(10) . .
Na1 O3 Na1 86.75(5) 2_556 .
O2 C1 O1 123.83(15) . .
O2 C1 C2 119.10(15) . .
O1 C1 C2 117.06(14) . .
O2 C1 Na1 42.19(8) . .
O1 C1 Na1 164.24(12) . .
C2 C1 Na1 77.27(9) . .
O3 C2 N1 128.44(15) . .
O3 C2 C1 119.20(14) . .
N1 C2 C1 112.33(14) . .
C8 C3 C4 121.82(17) . .
C8 C3 N1 120.09(17) . .
C4 C3 N1 118.03(16) . .
C5 C4 C3 118.1(2) . .
C5 C4 C9 120.6(2) . .
C3 C4 C9 121.29(17) . .
C6 C5 C4 120.8(2) . .
C6 C5 H5 119.6 . .
C4 C5 H5 119.6 . .
C7 C6 C5 120.24(18) . .
C7 C6 H6 119.9 . .
C5 C6 H6 119.9 . .
C6 C7 C8 121.2(2) . .
C6 C7 H7 119.4 . .
C8 C7 H7 119.4 . .
C3 C8 C7 117.88(19) . .
C3 C8 C10 120.90(17) . .
C7 C8 C10 121.22(19) . .
C4 C9 H9A 109.5 . .
C4 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C4 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O3 Na1 O2 116.18(5) 2_556 5_666
O3 Na1 O2 110.55(5) 2_556 .
O2 Na1 O2 76.37(5) 5_666 .
O3 Na1 O1W 97.02(5) 2_556 .
O2 Na1 O1W 85.09(5) 5_666 .
O2 Na1 O1W 151.45(6) . .
O3 Na1 O3 75.64(6) 2_556 .
O2 Na1 O3 146.64(5) 5_666 .
O2 Na1 O3 70.30(4) . .
O1W Na1 O3 126.00(5) . .
O3 Na1 C1 97.56(5) 2_556 .
O2 Na1 C1 96.57(5) 5_666 .
O2 Na1 C1 20.72(4) . .
O1W Na1 C1 162.81(6) . .
O3 Na1 C1 50.11(4) . .
O3 Na1 Na1 48.72(4) 2_556 2_556
O2 Na1 Na1 163.63(5) 5_666 2_556
O2 Na1 Na1 113.06(4) . 2_556
O1W Na1 Na1 90.45(4) . 2_556
O3 Na1 Na1 44.54(3) . 2_556
C1 Na1 Na1 92.34(4) . 2_556
O3 Na1 Na1 120.24(5) 2_556 5_666
O2 Na1 Na1 38.41(3) 5_666 5_666
O2 Na1 Na1 37.96(3) . 5_666
O1W Na1 Na1 120.49(5) . 5_666
O3 Na1 Na1 108.25(4) . 5_666
C1 Na1 Na1 58.30(4) . 5_666
Na1 Na1 Na1 149.06(3) 2_556 5_666
O3 Na1 H1W2 102.2(6) 2_556 .
O2 Na1 H1W2 67.2(3) 5_666 .
O2 Na1 H1W2 139.0(4) . .
O1W Na1 H1W2 18.0(3) . .
O3 Na1 H1W2 143.9(3) . .
C1 Na1 H1W2 158.5(5) . .
Na1 Na1 H1W2 106.9(4) 2_556 .
Na1 Na1 H1W2 103.7(4) 5_666 .
Na1 O1W H1W1 146.0(19) . .
Na1 O1W H1W2 101.4(19) . .
H1W1 O1W H1W2 106(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O1 2.0093(12) .
Pd1 O1 2.0094(12) 7
Pd1 N1 2.0196(14) .
Pd1 N1 2.0196(14) 7
N1 C2 1.327(2) .
N1 C3 1.438(2) .
O1 C1 1.297(2) .
O2 C1 1.230(2) .
O2 Na1 2.3121(14) 5_666
O2 Na1 2.3349(13) .
O3 C2 1.253(2) .
O3 Na1 2.2965(14) 2_556
O3 Na1 2.4605(14) .
C1 C2 1.550(2) .
C1 Na1 3.0954(18) .
C3 C8 1.405(3) .
C3 C4 1.413(3) .
C4 C5 1.402(3) .
C4 C9 1.507(3) .
C5 C6 1.394(3) .
C5 H5 0.9500 .
C6 C7 1.383(4) .
C6 H6 0.9500 .
C7 C8 1.408(3) .
C7 H7 0.9500 .
C8 C10 1.508(3) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
Na1 O3 2.2964(14) 2_556
Na1 O2 2.3121(14) 5_666
Na1 O1W 2.3385(15) .
Na1 Na1 3.2689(14) 2_556
Na1 Na1 3.6526(14) 5_666
Na1 H1W2 2.63(2) .
O1W H1W1 0.834(10) .
O1W H1W2 0.831(10) .
