#------------------------------------------------------------------------------
#$Date: 2023-11-23 11:33:10 +0200 (Thu, 23 Nov 2023) $
#$Revision: 287753 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/21/61/7216176.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_7216176
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 H18 N2 O6 Pd -2, 2(Na +), H2 O'
_chemical_formula_sum            'C20 H20 N2 Na2 O7 Pd'
_chemical_formula_weight         552.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 124.4800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.4083(6)
_cell_length_b                   22.4457(12)
_cell_length_c                   13.4740(4)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      3.01
_cell_volume                     4090.6(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23741
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.105
_diffrn_reflns_theta_min         1.758
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       prism
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7475
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0286
_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)+(0.0427P)²+13.4385P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.668
_reflns_Friedel_fraction_full    0.723
_reflns_Friedel_fraction_max     0.665
_reflns_number_gt                7363
_reflns_number_total             7475
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ce00669k2.cif
_cod_data_source_block           ff546orang1
_cod_depositor_comments
;
Adding full bibliography for 7216172--7216176.cif.

2023-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H40 N4 Na4 O14 Pd2'
_cod_original_formula_weight         1105.52
_cod_original_formula_moiety         'C40 H40 N4 Na4 O14 Pd2'
_cod_original_formula_units_Z            4
_cod_database_code               7216176
#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   0.865
_shelx_estimated_absorpt_t_max   0.924
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Pd1 Pd -0.00293(3) 0.36662(2) -0.75399(3) 0.01091(11) Uani 1 1 d . .
Pd2 Pd 0.51502(3) 0.38161(2) -0.72944(3) 0.00919(11) Uani 1 1 d . .
N1 N 0.1407(4) 0.3614(2) -0.6099(4) 0.0123(10) Uani 1 1 d . .
O1 O 0.0291(3) 0.28400(19) -0.7843(4) 0.0168(9) Uani 1 1 d . .
O2 O 0.1455(3) 0.21428(19) -0.6991(4) 0.0204(9) Uani 1 1 d . .
O3 O 0.2696(3) 0.29289(19) -0.5213(4) 0.0166(9) Uani 1 1 d . .
C1 C 0.1158(5) 0.2648(3) -0.7015(5) 0.0152(12) Uani 1 1 d . .
C2 C 0.1836(4) 0.3091(3) -0.6005(5) 0.0125(11) Uani 1 1 d . .
C3 C 0.2017(4) 0.4062(3) -0.5218(5) 0.0130(11) Uani 1 1 d . .
C4 C 0.2711(4) 0.4372(3) -0.5317(5) 0.0126(11) Uani 1 1 d . .
C5 C 0.3278(4) 0.4810(3) -0.4458(5) 0.0151(11) Uani 1 1 d . .
H5 H 0.3749 0.5029 -0.4509 0.018 Uiso 1 1 calc R U
C6 C 0.3165(4) 0.4932(3) -0.3537(5) 0.0163(12) Uani 1 1 d . .
H6 H 0.3547 0.5237 -0.2971 0.020 Uiso 1 1 calc R U
C7 C 0.2491(4) 0.4606(3) -0.3440(5) 0.0146(11) Uani 1 1 d . .
H7 H 0.2422 0.4688 -0.2799 0.017 Uiso 1 1 calc R U
C8 C 0.1919(4) 0.4163(3) -0.4269(5) 0.0124(11) Uani 1 1 d . .
C9 C 0.2853(4) 0.4239(3) -0.6306(5) 0.0153(12) Uani 1 1 d . .
H9A H 0.2393 0.3924 -0.6825 0.023 Uiso 1 1 calc R U
H9B H 0.3533 0.4106 -0.5952 0.023 Uiso 1 1 calc R U
H9C H 0.2723 0.4599 -0.6784 0.023 Uiso 1 1 calc R U
C10 C 0.1228(5) 0.3796(3) -0.4135(6) 0.0166(12) Uani 1 1 d . .
H10A H 0.0890 0.3508 -0.4795 0.025 Uiso 1 1 calc R U
H10B H 0.0739 0.4057 -0.4157 0.025 Uiso 1 1 calc R U
H10C H 0.1602 0.3584 -0.3365 0.025 Uiso 1 1 calc R U
N11 N -0.0593(3) 0.4448(2) -0.7426(4) 0.0118(10) Uani 1 1 d . .
O11 O -0.1387(3) 0.3615(2) -0.9101(4) 0.0171(9) Uani 1 1 d . .
O21 O -0.2735(3) 0.4166(2) -1.0308(4) 0.0207(10) Uani 1 1 d . .
O31 O -0.1981(3) 0.5032(2) -0.8561(4) 0.0181(9) Uani 1 1 d . .
C11 C -0.1922(4) 0.4089(3) -0.9363(5) 0.0157(12) Uani 1 1 d . .
C12 C -0.1486(4) 0.4578(3) -0.8391(5) 0.0137(12) Uani 1 1 d . .
C13 C -0.0206(4) 0.4873(3) -0.6477(5) 0.0117(11) Uani 1 1 d . .
C14 C 0.0486(4) 0.5287(3) -0.6321(5) 0.0131(11) Uani 1 1 d . .
C15 C 0.0820(4) 0.5722(3) -0.5443(5) 0.0153(12) Uani 1 1 d . .
H15 H 0.1308 0.5998 -0.5318 0.018 Uiso 1 1 calc R U
C16 C 0.0441(4) 0.5758(3) -0.4735(5) 0.0167(12) Uani 1 1 d . .
H16 H 0.0656 0.6062 -0.4147 0.020 Uiso 1 1 calc R U
C17 C -0.0255(4) 0.5339(3) -0.4913(5) 0.0153(11) Uani 1 1 d . .
H17 H -0.0511 0.5360 -0.4433 0.018 Uiso 1 1 calc R U
C18 C -0.0587(4) 0.4891(3) -0.5773(5) 0.0131(11) Uani 1 1 d . .
C19 C 0.0826(4) 0.5288(3) -0.7150(5) 0.0150(11) Uani 1 1 d . .
H19A H 0.0522 0.4954 -0.7714 0.023 Uiso 1 1 calc R U
H19B H 0.1547 0.5249 -0.6675 0.023 Uiso 1 1 calc R U
H19C H 0.0631 0.5664 -0.7600 0.023 Uiso 1 1 calc R U
C20 C -0.1386(4) 0.4465(3) -0.5988(5) 0.0156(12) Uani 1 1 d . .
H20A H -0.1529 0.4181 -0.6620 0.023 Uiso 1 1 calc R U
H20B H -0.1986 0.4689 -0.6239 0.023 Uiso 1 1 calc R U
H20C H -0.1159 0.4248 -0.5242 0.023 Uiso 1 1 calc R U
N12 N 0.5038(4) 0.3752(2) -0.8862(4) 0.0100(10) Uani 1 1 d . .
O12 O 0.5853(3) 0.45779(18) -0.7167(4) 0.0130(8) Uani 1 1 d . .
O22 O 0.6244(3) 0.51332(18) -0.8208(4) 0.0149(8) Uani 1 1 d . .
O32 O 0.5393(3) 0.43075(18) -1.0018(3) 0.0150(8) Uani 1 1 d . .
C21 C 0.5880(4) 0.4691(3) -0.8094(5) 0.0132(11) Uani 1 1 d . .
C22 C 0.5407(4) 0.4221(3) -0.9091(5) 0.0113(11) Uani 1 1 d . .
C23 C 0.4647(4) 0.3286(2) -0.9728(5) 0.0101(10) Uani 1 1 d . .
C24 C 0.3619(4) 0.3216(3) -1.0497(5) 0.0106(11) Uani 1 1 d . .
C25 C 0.3228(4) 0.2765(3) -1.1352(5) 0.0149(11) Uani 1 1 d . .
H25 H 0.2532 0.2711 -1.1865 0.018 Uiso 1 1 calc R U
C26 C 0.3854(5) 0.2391(3) -1.1458(5) 0.0161(12) Uani 1 1 d . .
H26 H 0.3588 0.2082 -1.2042 0.019 Uiso 1 1 calc R U
C27 C 0.4871(4) 0.2475(3) -1.0703(5) 0.0140(11) Uani 1 1 d . .
H27 H 0.5293 0.2219 -1.0781 0.017 Uiso 1 1 calc R U
C28 C 0.5286(4) 0.2918(3) -0.9844(5) 0.0124(11) Uani 1 1 d . .
C29 C 0.2956(4) 0.3646(3) -1.0432(5) 0.0134(11) Uani 1 1 d . .
H29A H 0.2265 0.3534 -1.1022 0.020 Uiso 1 1 calc R U
H29B H 0.3071 0.4048 -1.0610 0.020 Uiso 1 1 calc R U
H29C H 0.3097 0.3638 -0.9622 0.020 Uiso 1 1 calc R U
C30 C 0.6387(4) 0.3020(3) -0.9094(5) 0.0145(12) Uani 1 1 d . .
H30A H 0.6550 0.3350 -0.8534 0.022 Uiso 1 1 calc R U
H30B H 0.6600 0.3119 -0.9621 0.022 Uiso 1 1 calc R U
H30C H 0.6725 0.2658 -0.8638 0.022 Uiso 1 1 calc R U
N13 N 0.4453(3) 0.3105(2) -0.7156(4) 0.0109(9) Uani 1 1 d . .
O13 O 0.5427(3) 0.40064(19) -0.5669(4) 0.0142(8) Uani 1 1 d . .
O23 O 0.5180(3) 0.3655(2) -0.4314(4) 0.0178(9) Uani 1 1 d . .
O33 O 0.4206(3) 0.26969(18) -0.5763(3) 0.0157(8) Uani 1 1 d . .
C31 C 0.5081(4) 0.3618(3) -0.5292(5) 0.0131(11) Uani 1 1 d . .
C32 C 0.4532(4) 0.3088(3) -0.6115(5) 0.0111(11) Uani 1 1 d . .
C33 C 0.3917(4) 0.2631(2) -0.7994(5) 0.0113(11) Uani 1 1 d . .
C34 C 0.2874(4) 0.2606(3) -0.8635(5) 0.0117(11) Uani 1 1 d . .
C35 C 0.2387(4) 0.2138(3) -0.9445(5) 0.0143(11) Uani 1 1 d . .
H35 H 0.1687 0.2114 -0.9889 0.017 Uiso 1 1 calc R U
C36 C 0.2902(5) 0.1706(3) -0.9616(6) 0.0183(13) Uani 1 1 d . .
H36 H 0.2556 0.1392 -1.0178 0.022 Uiso 1 1 calc R U
C37 C 0.3926(4) 0.1733(3) -0.8964(5) 0.0155(12) Uani 1 1 d . .
H37 H 0.4279 0.1437 -0.9080 0.019 Uiso 1 1 calc R U
C38 C 0.4438(4) 0.2190(3) -0.8146(5) 0.0107(11) Uani 1 1 d . .
C39 C 0.2309(4) 0.3061(3) -0.8448(5) 0.0158(12) Uani 1 1 d . .
H39A H 0.2770 0.3353 -0.7850 0.024 Uiso 1 1 calc R U
H39B H 0.1946 0.2865 -0.8161 0.024 Uiso 1 1 calc R U
H39C H 0.1842 0.3264 -0.9211 0.024 Uiso 1 1 calc R U
C40 C 0.5546(4) 0.2199(3) -0.7400(5) 0.0160(12) Uani 1 1 d . .
H40A H 0.5786 0.2548 -0.6870 0.024 Uiso 1 1 calc R U
H40B H 0.5777 0.2219 -0.7930 0.024 Uiso 1 1 calc R U
H40C H 0.5801 0.1836 -0.6912 0.024 Uiso 1 1 calc R U
Na1 Na 0.32076(18) 0.19958(11) -0.5759(2) 0.0185(5) Uani 1 1 d . .
Na2 Na 0.43530(17) 0.30575(10) -0.3747(2) 0.0179(5) Uani 1 1 d . .
Na3 Na 0.63247(16) 0.39438(10) -0.23547(19) 0.0130(4) Uani 1 1 d . .
Na4 Na 0.63439(16) 0.50741(10) -1.0041(2) 0.0143(5) Uani 1 1 d . .
O1W O 0.4850(3) 0.3851(2) -0.2296(4) 0.0203(9) Uani 1 1 d . .
O2W O 0.2886(4) 0.1228(2) -0.7200(4) 0.0239(10) 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'
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
O11 Pd1 N11 81.19(19) . .
O11 Pd1 O1 89.83(18) . .
N11 Pd1 O1 170.23(18) . .
O11 Pd1 N1 170.21(19) . .
N11 Pd1 N1 108.0(2) . .
O1 Pd1 N1 81.26(19) . .
O12 Pd2 O13 87.80(16) . .
O12 Pd2 N12 81.88(17) . .
O13 Pd2 N12 169.56(18) . .
O12 Pd2 N13 169.50(17) . .
O13 Pd2 N13 81.89(18) . .
N12 Pd2 N13 108.48(18) . .
O12 Pd2 Na4 46.96(12) . 2_565
O13 Pd2 Na4 40.85(12) . 2_565
N12 Pd2 Na4 128.78(13) . 2_565
N13 Pd2 Na4 122.74(13) . 2_565
C2 N1 C3 116.8(5) . .
C2 N1 Pd1 113.8(4) . .
C3 N1 Pd1 129.3(4) . .
C1 O1 Pd1 114.6(4) . .
C1 O1 Na2 103.6(4) . 4_454
Pd1 O1 Na2 134.6(2) . 4_454
C1 O2 Na1 116.7(4) . .
C1 O2 Na3 156.5(4) . 4_454
Na1 O2 Na3 86.38(16) . 4_454
C1 O2 Na2 81.4(4) . 4_454
Na1 O2 Na2 161.61(19) . 4_454
Na3 O2 Na2 75.91(13) 4_454 4_454
C2 O3 Na2 155.7(4) . .
C2 O3 Na1 113.3(4) . .
Na2 O3 Na1 85.84(16) . .
O2 C1 O1 124.0(6) . .
O2 C1 C2 119.7(6) . .
O1 C1 C2 116.3(5) . .
O2 C1 Na2 74.6(3) . 4_454
O1 C1 Na2 51.6(3) . 4_454
C2 C1 Na2 159.4(4) . 4_454
O3 C2 N1 128.0(5) . .
O3 C2 C1 118.0(5) . .
N1 C2 C1 113.9(5) . .
C8 C3 C4 121.8(5) . .
C8 C3 N1 118.8(5) . .
C4 C3 N1 119.4(5) . .
C5 C4 C3 117.8(5) . .
C5 C4 C9 120.6(5) . .
C3 C4 C9 121.6(5) . .
C6 C5 C4 121.2(5) . .
C5 C6 C7 119.9(5) . .
C8 C7 C6 120.7(5) . .
C7 C8 C3 118.5(5) . .
C7 C8 C10 120.7(5) . .
C3 C8 C10 120.8(5) . .
C12 N11 C13 114.5(5) . .
C12 N11 Pd1 114.4(4) . .
C13 N11 Pd1 131.0(4) . .
C11 O11 Pd1 114.5(4) . .
C11 O11 Na1 115.6(4) . 4_454
Pd1 O11 Na1 124.6(2) . 4_454
C11 O21 Na3 143.2(4) . 1_454
C11 O21 Na4 109.4(4) . 1_455
Na3 O21 Na4 106.03(17) 1_454 1_455
C12 O31 Na4 121.9(4) . 1_455
O21 C11 O11 124.7(6) . .
O21 C11 C12 119.4(6) . .
O11 C11 C12 115.9(5) . .
O31 C12 N11 127.3(6) . .
O31 C12 C11 119.2(5) . .
N11 C12 C11 113.5(5) . .
C14 C13 C18 121.2(5) . .
C14 C13 N11 119.7(5) . .
C18 C13 N11 118.9(5) . .
C15 C14 C13 119.7(5) . .
C15 C14 C19 119.9(5) . .
C13 C14 C19 120.3(5) . .
C14 C15 C16 120.5(5) . .
C17 C16 C15 118.7(5) . .
C16 C17 C18 121.8(5) . .
C17 C18 C13 118.1(5) . .
C17 C18 C20 120.3(5) . .
C13 C18 C20 121.5(5) . .
C22 N12 C23 116.3(5) . .
C22 N12 Pd2 113.6(4) . .
C23 N12 Pd2 130.1(4) . .
C21 O12 Pd2 114.4(4) . .
C21 O12 Na4 146.7(4) . 2_565
Pd2 O12 Na4 98.81(16) . 2_565
C21 O22 Na3 123.9(4) . 2_564
C21 O22 Na4 112.6(4) . .
Na3 O22 Na4 120.14(18) 2_564 .
C22 O32 Na4 119.6(4) . .
O22 C21 O12 124.8(5) . .
O22 C21 C22 119.7(5) . .
O12 C21 C22 115.6(5) . .
O32 C22 N12 126.8(5) . .
O32 C22 C21 118.8(5) . .
N12 C22 C21 114.4(5) . .
C24 C23 C28 120.7(5) . .
C24 C23 N12 119.0(5) . .
C28 C23 N12 120.2(5) . .
C25 C24 C23 119.6(5) . .
C25 C24 C29 120.6(5) . .
C23 C24 C29 119.7(5) . .
C24 C25 C26 120.2(5) . .
C27 C26 C25 119.5(5) . .
C28 C27 C26 121.9(5) . .
C27 C28 C23 118.1(5) . .
C27 C28 C30 120.5(5) . .
C23 C28 C30 121.3(5) . .
C32 N13 C33 117.3(5) . .
C32 N13 Pd2 113.2(4) . .
C33 N13 Pd2 129.5(4) . .
C31 O13 Pd2 113.9(4) . .
C31 O13 Na4 140.1(4) . 2_565
Pd2 O13 Na4 105.96(18) . 2_565
C31 O23 Na3 140.5(4) . .
C31 O23 Na2 124.2(4) . .
Na3 O23 Na2 92.01(17) . .
C32 O33 Na1 161.5(4) . .
C32 O33 Na2 110.8(3) . .
Na1 O33 Na2 81.95(14) . .
O23 C31 O13 123.5(5) . .
O23 C31 C32 119.7(5) . .
O13 C31 C32 116.8(5) . .
O33 C32 N13 127.6(5) . .
O33 C32 C31 118.3(5) . .
N13 C32 C31 114.1(5) . .
C38 C33 C34 120.7(5) . .
C38 C33 N13 119.2(5) . .
C34 C33 N13 120.0(5) . .
C35 C34 C33 117.8(5) . .
C35 C34 C39 120.8(5) . .
C33 C34 C39 121.4(5) . .
C36 C35 C34 121.5(5) . .
C37 C36 C35 119.7(5) . .
C38 C37 C36 120.5(5) . .
C37 C38 C33 119.7(5) . .
C37 C38 C40 120.1(5) . .
C33 C38 C40 120.2(5) . .
O33 Na1 O11 125.71(18) . 4
O33 Na1 O2 119.15(18) . .
O11 Na1 O2 108.62(17) 4 .
O33 Na1 O2W 108.72(18) . .
O11 Na1 O2W 99.31(18) 4 .
O2 Na1 O2W 84.88(17) . .
O33 Na1 O3 77.57(16) . .
O11 Na1 O3 99.65(17) 4 .
O2 Na1 O3 67.63(15) . .
O2W Na1 O3 150.43(18) . .
O33 Na1 Na2 54.79(12) . .
O11 Na1 Na2 85.28(14) 4 .
O2 Na1 Na2 111.96(14) . .
O2W Na1 Na2 160.31(16) . .
O3 Na1 Na2 44.33(11) . .
O33 Na1 Na3 147.45(14) . 4_454
O11 Na1 Na3 84.56(13) 4 4_454
O2 Na1 Na3 47.81(12) . 4_454
O2W Na1 Na3 47.94(13) . 4_454
O3 Na1 Na3 112.00(13) . 4_454
Na2 Na1 Na3 151.68(10) . 4_454
O3 Na2 O23 114.64(17) . .
O3 Na2 O1 115.84(17) . 4
O23 Na2 O1 108.91(18) . 4
O3 Na2 O1W 118.65(18) . .
O23 Na2 O1W 81.26(17) . .
O1 Na2 O1W 112.42(17) 4 .
O3 Na2 O33 73.21(15) . .
O23 Na2 O33 65.18(15) . .
O1 Na2 O33 85.73(15) 4 .
O1W Na2 O33 145.83(17) . .
O3 Na2 O2 163.68(17) . 4
O23 Na2 O2 73.25(15) . 4
O1 Na2 O2 48.28(14) 4 4
O1W Na2 O2 75.80(15) . 4
O33 Na2 O2 99.25(15) . 4
O3 Na2 C1 140.53(19) . 4
O23 Na2 C1 93.29(17) . 4
O1 Na2 C1 24.79(16) 4 4
O1W Na2 C1 91.61(17) . 4
O33 Na2 C1 96.37(16) . 4
O2 Na2 C1 24.03(15) 4 4
O3 Na2 Na1 49.83(12) . .
O23 Na2 Na1 108.37(14) . .
O1 Na2 Na1 73.34(12) 4 .
O1W Na2 Na1 167.02(15) . .
O33 Na2 Na1 43.25(10) . .
O2 Na2 Na1 114.84(12) 4 .
C1 Na2 Na1 96.37(14) 4 .
O3 Na2 Na3 149.10(14) . .
O23 Na2 Na3 43.75(11) . .
O1 Na2 Na3 94.36(13) 4 .
O1W Na2 Na3 47.85(12) . .
O33 Na2 Na3 104.48(12) . .
O2 Na2 Na3 46.12(10) 4 .
C1 Na2 Na3 70.05(14) 4 .
Na1 Na2 Na3 144.92(10) . .
O23 Na3 O21 169.08(19) . 1_656
O23 Na3 O22 84.46(16) . 2_565
O21 Na3 O22 102.03(18) 1_656 2_565
O23 Na3 O2 82.65(17) . 4
O21 Na3 O2 92.94(18) 1_656 4
O22 Na3 O2 161.15(17) 2_565 4
O23 Na3 O1W 80.51(16) . .
O21 Na3 O1W 89.09(17) 1_656 .
O22 Na3 O1W 107.81(17) 2_565 .
O2 Na3 O1W 83.56(16) 4 .
O23 Na3 O2W 100.70(18) . 4
O21 Na3 O2W 88.51(17) 1_656 4
O22 Na3 O2W 86.99(17) 2_565 4
O2 Na3 O2W 81.96(16) 4 4
O1W Na3 O2W 165.18(18) . 4
O23 Na3 Na2 44.24(12) . .
O21 Na3 Na2 125.21(14) 1_656 .
O22 Na3 Na2 119.11(13) 2_565 .
O2 Na3 Na2 57.97(12) 4 .
O1W Na3 Na2 46.49(12) . .
O2W Na3 Na2 125.63(14) 4 .
O23 Na3 Na1 114.71(14) . 4
O21 Na3 Na1 67.69(14) 1_656 4
O22 Na3 Na1 130.73(14) 2_565 4
O2 Na3 Na1 45.81(12) 4 4
O1W Na3 Na1 119.54(13) . 4
O2W Na3 Na1 46.43(12) 4 4
Na2 Na3 Na1 103.64(9) . 4
O23 Na3 Na4 135.44(14) . 1_556
O21 Na3 Na4 40.03(13) 1_656 1_556
O22 Na3 Na4 78.15(12) 2_565 1_556
O2 Na3 Na4 120.59(13) 4 1_556
O1W Na3 Na4 66.74(12) . 1_556
O2W Na3 Na4 118.74(13) 4 1_556
Na2 Na3 Na4 113.21(8) . 1_556
Na1 Na3 Na4 107.63(7) 4 1_556
O31 Na4 O32 115.82(17) 1_655 .
O31 Na4 O13 122.68(18) 1_655 2_564
O32 Na4 O13 110.31(16) . 2_564
O31 Na4 O22 82.19(16) 1_655 .
O32 Na4 O22 67.58(15) . .
O13 Na4 O22 85.77(15) 2_564 .
O31 Na4 O12 115.86(16) 1_655 2_564
O32 Na4 O12 116.13(16) . 2_564
O13 Na4 O12 67.41(14) 2_564 2_564
O22 Na4 O12 152.73(16) . 2_564
O31 Na4 O21 66.37(15) 1_655 1_655
O32 Na4 O21 82.68(16) . 1_655
O13 Na4 O21 153.19(16) 2_564 1_655
O22 Na4 O21 121.04(15) . 1_655
O12 Na4 O21 85.87(14) 2_564 1_655
O31 Na4 Pd2 125.44(13) 1_655 2_564
O32 Na4 Pd2 118.73(12) . 2_564
O13 Na4 Pd2 33.18(10) 2_564 2_564
O22 Na4 Pd2 118.86(12) . 2_564
O12 Na4 Pd2 34.23(9) 2_564 2_564
O21 Na4 Pd2 120.04(12) 1_655 2_564
O31 Na4 Na3 97.32(13) 1_655 1_554
O32 Na4 Na3 80.36(12) . 1_554
O13 Na4 Na3 122.79(13) 2_564 1_554
O22 Na4 Na3 143.52(13) . 1_554
O12 Na4 Na3 58.36(10) 2_564 1_554
O21 Na4 Na3 33.95(10) 1_655 1_554
Pd2 Na4 Na3 91.23(6) 2_564 1_554
Na2 O1W Na3 85.66(16) . .
Na1 O2W Na3 85.63(17) . 4_454
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O11 2.023(4) .
Pd1 N11 2.029(5) .
Pd1 O1 2.031(4) .
Pd1 N1 2.039(5) .
Pd2 O12 2.015(4) .
Pd2 O13 2.015(4) .
Pd2 N12 2.019(5) .
Pd2 N13 2.033(5) .
Pd2 Na4 3.539(2) 2_565
N1 C2 1.338(8) .
N1 C3 1.440(7) .
O1 C1 1.287(8) .
O1 Na2 2.406(5) 4_454
O2 C1 1.229(8) .
O2 Na1 2.393(5) .
O2 Na3 2.473(5) 4_454
O2 Na2 2.908(5) 4_454
O3 C2 1.248(7) .
O3 Na2 2.302(5) .
O3 Na1 2.517(5) .
C1 C2 1.537(8) .
C1 Na2 2.983(6) 4_454
C3 C8 1.395(8) .
C3 C4 1.404(8) .
C4 C5 1.397(8) .
C4 C9 1.507(8) .
C5 C6 1.382(9) .
C6 C7 1.393(9) .
C7 C8 1.391(8) .
C8 C10 1.492(8) .
N11 C12 1.329(7) .
N11 C13 1.424(7) .
O11 C11 1.295(8) .
O11 Na1 2.373(5) 4_454
O21 C11 1.228(7) .
O21 Na3 2.327(5) 1_454
O21 Na4 2.680(5) 1_455
O31 C12 1.241(8) .
O31 Na4 2.309(4) 1_455
C11 C12 1.540(8) .
C13 C14 1.388(8) .
C13 C18 1.401(8) .
C14 C15 1.386(8) .
C14 C19 1.505(8) .
C15 C16 1.404(8) .
C16 C17 1.391(9) .
C17 C18 1.392(8) .
C18 C20 1.513(8) .
N12 C22 1.335(7) .
N12 C23 1.420(7) .
O12 C21 1.299(7) .
O12 Na4 2.618(5) 2_565
O22 C21 1.212(7) .
O22 Na3 2.337(5) 2_564
O22 Na4 2.569(5) .
O32 C22 1.252(7) .
O32 Na4 2.334(5) .
C21 C22 1.530(8) .
C23 C24 1.402(7) .
C23 C28 1.411(8) .
C24 C25 1.387(8) .
C24 C29 1.494(8) .
C25 C26 1.397(9) .
C26 C27 1.390(8) .
C27 C28 1.380(8) .
C28 C30 1.506(8) .
N13 C32 1.334(7) .
N13 C33 1.434(7) .
O13 C31 1.292(7) .
O13 Na4 2.408(5) 2_565
O23 C31 1.236(7) .
O23 Na3 2.302(5) .
O23 Na2 2.323(5) .
O33 C32 1.253(7) .
O33 Na1 2.273(5) .
O33 Na2 2.711(5) .
C31 C32 1.524(8) .
C33 C38 1.396(8) .
C33 C34 1.416(7) .
C34 C35 1.395(8) .
C34 C39 1.494(8) .
C35 C36 1.390(9) .
C36 C37 1.388(8) .
C37 C38 1.387(8) .
C38 C40 1.500(7) .
Na1 O11 2.373(5) 4
Na1 O2W 2.420(5) .
Na1 Na2 3.285(3) .
Na1 Na3 3.331(3) 4_454
Na2 O1 2.406(5) 4
Na2 O1W 2.420(5) .
Na2 O2 2.909(5) 4
Na2 C1 2.983(6) 4
Na2 Na3 3.327(3) .
Na3 O21 2.327(5) 1_656
Na3 O22 2.337(5) 2_565
Na3 O2 2.473(5) 4
Na3 O1W 2.474(5) .
Na3 O2W 2.480(5) 4
Na3 Na1 3.331(3) 4
Na3 Na4 4.006(3) 1_556
Na4 O31 2.309(4) 1_655
Na4 O13 2.408(5) 2_564
Na4 O12 2.618(5) 2_564
Na4 O21 2.680(5) 1_655
Na4 Pd2 3.539(2) 2_564
Na4 Na3 4.006(3) 1_554
O2W Na3 2.480(5) 4_454
