# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_publ_contact_author_name 'Hegen Zheng'
_publ_contact_author_email ZHENGHG@NJU.EDU.CN
_publ_section_title
;
Unprecedented NaI-CuII-LnIII heterometallic
coordination polymers based on 3,5-pyrazoledicarboxylate with both
infinite cationic and anionic chains
;
loop_
_publ_author_name
'Hegen Zheng.'
'Zijian Guo.'
'Zheng Hu.'
'Zhao-Rui Pan.'
'Ying-Zhong Shen.'
;
You Song
;
'Yan Wang.'
# Attachment '4.cif'
data_251029bm
_database_code_depnum_ccdc_archive 'CCDC 602777'
_audit_update_record
;
2008-06-30 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C10 H12 Cu N4 Nd O13), 2(H8 Na O4), 3(H2 O)'
_chemical_formula_sum 'C20 H46 Cu2 N8 Na2 Nd2 O37'
_chemical_formula_weight 1452.19
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_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'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 24.542(10)
_cell_length_b 13.429(10)
_cell_length_c 13.701(10)
_cell_angle_alpha 90.00
_cell_angle_beta 92.42(10)
_cell_angle_gamma 90.00
_cell_volume 4512(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description block
_exptl_crystal_colour purple
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.138
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2872
_exptl_absorpt_coefficient_mu 3.335
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.40
_exptl_absorpt_correction_T_max 0.60
_exptl_absorpt_process_details 'SADABS(Bruker, 2000)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 13184
_diffrn_reflns_av_R_equivalents 0.0518
_diffrn_reflns_av_sigmaI/netI 0.0552
_diffrn_reflns_limit_h_min -31
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 1.66
_diffrn_reflns_theta_max 27.00
_reflns_number_total 4901
_reflns_number_gt 4025
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker, 2000)'
_computing_cell_refinement 'SAINT (Bruker, 2000)'
_computing_data_reduction 'SAINT (Bruker, 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F^2^, conventional
R-factors R are based on F, with F set to zero for negative
F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for
calculating R-factors(gt) etc. and is not relevant to the choice
of reflections for refinement. R-factors based on F^2^ are
statistically about twice as large as those based on F, and R-- factors based
on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment geom
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4901
_refine_ls_number_parameters 325
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0423
_refine_ls_R_factor_gt 0.0314
_refine_ls_wR_factor_ref 0.0732
_refine_ls_wR_factor_gt 0.0676
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_restrained_S_all 1.024
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
Na1 Na 0.50653(7) 0.52104(15) 0.62401(14) 0.0428(5) Uani 1 1 d . . .
Nd1 Nd 0.105091(8) 0.556271(15) 0.893393(15) 0.01813(7) Uani 1 1 d . . .
Cu1 Cu 0.285661(18) 0.63002(4) 0.93014(4) 0.02207(12) Uani 1 1 d . . .
C1 C 0.31762(16) 0.7042(3) 0.7532(3) 0.0233(9) Uani 1 1 d . . .
C2 C 0.25758(15) 0.6925(3) 0.7431(3) 0.0210(9) Uani 1 1 d . . .
C3 C 0.21655(15) 0.7124(3) 0.6721(3) 0.0220(9) Uani 1 1 d . . .
H3 H 0.2199 0.7384 0.6097 0.026 Uiso 1 1 d R . .
C4 C 0.16939(15) 0.6849(3) 0.7166(3) 0.0198(8) Uani 1 1 d . . .
C5 C 0.11040(16) 0.6900(3) 0.6858(3) 0.0221(9) Uani 1 1 d . . .
N1 N 0.18089(12) 0.6500(2) 0.8082(2) 0.0205(7) Uani 1 1 d . . .
N2 N 0.23493(13) 0.6557(2) 0.8228(2) 0.0213(7) Uani 1 1 d . . .
O1 O 0.33905(10) 0.6762(2) 0.8358(2) 0.0269(7) Uani 1 1 d . . .
O2 O 0.34458(11) 0.7377(2) 0.6858(2) 0.0322(7) Uani 1 1 d . . .
O3 O 0.07695(11) 0.6591(2) 0.7465(2) 0.0257(6) Uani 1 1 d . . .
O4 O 0.09600(11) 0.7228(2) 0.6031(2) 0.0292(7) Uani 1 1 d . . .
C6 C 0.31593(16) 0.5950(3) 1.1254(3) 0.0229(9) Uani 1 1 d . . .
C7 C 0.25564(15) 0.5875(3) 1.1175(3) 0.0206(8) Uani 1 1 d . . .
C8 C 0.21512(16) 0.5638(3) 1.1798(3) 0.0214(9) Uani 1 1 d . . .
H8 H 0.2189 0.5465 1.2455 0.026 Uiso 1 1 d R . .
C9 C 0.16799(15) 0.5711(3) 1.1220(3) 0.0188(8) Uani 1 1 d . . .
C10 C 0.11036(16) 0.5540(3) 1.1457(3) 0.0201(8) Uani 1 1 d . . .
N3 N 0.17887(12) 0.5969(2) 1.0296(2) 0.0199(7) Uani 1 1 d . . .
N4 N 0.23303(12) 0.6073(2) 1.0280(2) 0.0211(7) Uani 1 1 d . . .
O5 O 0.33832(10) 0.6202(2) 1.0449(2) 0.0242(6) Uani 1 1 d . . .
O6 O 0.34128(11) 0.5764(2) 1.2029(2) 0.0338(8) Uani 1 1 d . . .
O7 O 0.07653(11) 0.5502(2) 1.0716(2) 0.0261(7) Uani 1 1 d . . .
O8 O 0.09755(11) 0.5441(2) 1.2328(2) 0.0255(6) Uani 1 1 d . . .
O9 O 0.29181(12) 0.4616(2) 0.8883(2) 0.0316(7) Uani 1 1 d . . .
H9A H 0.3124 0.4223 0.9354 0.038 Uiso 1 1 d R . .
H9B H 0.3129 0.4614 0.8310 0.038 Uiso 1 1 d R . .
O10 O 0.17774(12) 0.4234(2) 0.9102(2) 0.0311(7) Uani 1 1 d . . .
H10A H 0.2164 0.4344 0.9097 0.037 Uiso 1 1 d R . .
H10B H 0.1692 0.3675 0.8687 0.037 Uiso 1 1 d R . .
O11 O 0.06573(13) 0.3874(2) 0.9314(2) 0.0386(8) Uani 1 1 d . . .
H11A H 0.0279 0.3721 0.9184 0.046 Uiso 1 1 d R . .
H11B H 0.0706 0.3550 0.9936 0.046 Uiso 1 1 d R . .
O12 O 0.00636(11) 0.5676(2) 0.8753(2) 0.0293(7) Uani 1 1 d . . .
H12A H -0.0162 0.6128 0.8373 0.035 Uiso 1 1 d R . .
H12B H -0.0184 0.5189 0.8992 0.035 Uiso 1 1 d R . .
O13 O 0.08418(11) 0.7309(2) 0.9449(2) 0.0274(7) Uani 1 1 d . . .
H13A H 0.1129 0.7523 0.9883 0.033 Uiso 1 1 d R . .
H13B H 0.0834 0.7867 0.9029 0.033 Uiso 1 1 d R . .
O14 O 0.43310(12) 0.5013(2) 0.5025(2) 0.0411(8) Uani 1 1 d . . .
H14A H 0.4080 0.4520 0.5241 0.049 Uiso 1 1 d R . .
H14B H 0.4106 0.5588 0.5119 0.049 Uiso 1 1 d R . .
O15 O 0.43335(13) 0.5409(3) 0.7346(3) 0.0485(9) Uani 1 1 d . . .
H15A H 0.4057 0.4911 0.7241 0.058 Uiso 1 1 d R . .
H15B H 0.4096 0.5967 0.7428 0.058 Uiso 1 1 d R . .
O16 O 0.50182(12) 0.3399(2) 0.6486(2) 0.0388(8) Uani 1 1 d . A .
H16A H 0.5030 0.3115 0.5856 0.047 Uiso 1 1 d R . .
H16B H 0.5358 0.3126 0.6720 0.047 Uiso 1 1 d R . .
O17 O 0.5474(3) 0.7012(4) 0.6225(4) 0.0496(14) Uani 0.662(7) 1 d P A 1
H17A H 0.5862 0.6977 0.6347 0.060 Uiso 0.662(7) 1 d PR A 1
H17B H 0.5314 0.7402 0.6726 0.060 Uiso 0.662(7) 1 d PR A 1
O17' O 0.5111(5) 0.6962(9) 0.5995(9) 0.0496(14) Uani 0.338(7) 1 d P A 2
H17C H 0.5483 0.7129 0.5885 0.060 Uiso 0.338(7) 1 d PR A 2
H17D H 0.5044 0.7230 0.6617 0.060 Uiso 0.338(7) 1 d PR A 2
O18 O 0.14453(12) 0.8511(2) 0.4893(2) 0.0370(8) Uani 1 1 d . . .
H18A H 0.1319 0.7997 0.5316 0.044 Uiso 1 1 d R . .
H18B H 0.1486 0.8264 0.4243 0.044 Uiso 1 1 d R . .
O19 O 0.0000 0.3412(4) 0.7500 0.0581(15) Uani 1 2 d S . .
H19A H 0.0342 0.3095 0.7664 0.070 Uiso 0.50 1 d PR . .
H19B H -0.0049 0.4079 0.7731 0.070 Uiso 0.50 1 d PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Na1 0.0362(11) 0.0534(12) 0.0388(12) 0.0020(10) 0.0004(9) 0.0017(9)
Nd1 0.01471(12) 0.02318(12) 0.01646(12) 0.00113(9) 0.00023(8) -0.00185(8)
Cu1 0.0146(2) 0.0322(3) 0.0194(3) 0.0039(2) 0.00075(19) -0.0020(2)
C1 0.021(2) 0.021(2) 0.028(2) -0.0045(18) 0.0041(17) -0.0003(17)
C2 0.023(2) 0.021(2) 0.019(2) -0.0004(17) 0.0051(16) 0.0000(16)
C3 0.022(2) 0.027(2) 0.017(2) 0.0041(17) 0.0035(16) -0.0016(17)
C4 0.020(2) 0.022(2) 0.018(2) 0.0010(16) -0.0014(16) -0.0027(16)
C5 0.019(2) 0.021(2) 0.027(2) 0.0000(17) -0.0004(17) 0.0005(16)
N1 0.0156(16) 0.0268(18) 0.0190(18) 0.0031(14) -0.0001(13) 0.0018(14)
N2 0.0180(17) 0.0260(18) 0.0202(18) 0.0026(15) 0.0042(13) -0.0012(14)
O1 0.0167(14) 0.0378(17) 0.0262(16) 0.0071(14) 0.0018(12) -0.0015(12)
O2 0.0258(16) 0.0430(19) 0.0287(17) 0.0010(14) 0.0093(13) -0.0092(14)
O3 0.0188(15) 0.0347(17) 0.0236(16) 0.0089(13) -0.0006(12) -0.0004(12)
O4 0.0251(16) 0.0397(18) 0.0222(16) 0.0084(14) -0.0053(12) -0.0018(13)
C6 0.017(2) 0.026(2) 0.026(2) -0.0009(18) 0.0011(17) -0.0011(17)
C7 0.018(2) 0.025(2) 0.019(2) 0.0017(17) -0.0024(16) -0.0017(16)
C8 0.021(2) 0.027(2) 0.016(2) 0.0024(17) -0.0010(16) -0.0011(17)
C9 0.016(2) 0.023(2) 0.017(2) -0.0013(16) 0.0009(15) -0.0005(16)
C10 0.020(2) 0.022(2) 0.018(2) 0.0037(17) 0.0016(16) -0.0022(16)
N3 0.0129(16) 0.0292(18) 0.0177(18) 0.0012(14) 0.0027(13) -0.0029(14)
N4 0.0126(16) 0.0313(19) 0.0196(18) -0.0001(15) 0.0007(13) -0.0014(14)
O5 0.0156(14) 0.0336(16) 0.0234(16) 0.0024(13) -0.0005(12) -0.0041(12)
O6 0.0211(16) 0.056(2) 0.0236(17) 0.0084(15) -0.0052(13) 0.0012(14)
O7 0.0189(15) 0.0389(17) 0.0204(16) 0.0027(13) -0.0023(12) -0.0078(12)
O8 0.0241(15) 0.0354(17) 0.0173(15) 0.0043(12) 0.0047(12) -0.0026(12)
O9 0.0309(17) 0.0334(17) 0.0301(18) -0.0011(14) -0.0028(13) 0.0052(13)
O10 0.0318(17) 0.0301(16) 0.0312(18) -0.0054(14) -0.0033(13) 0.0065(13)
O11 0.043(2) 0.0378(19) 0.0343(19) 0.0121(15) -0.0092(15) -0.0153(15)
O12 0.0142(14) 0.0396(18) 0.0339(18) 0.0131(14) -0.0013(12) -0.0031(12)
O13 0.0263(16) 0.0243(15) 0.0312(17) -0.0002(13) -0.0034(13) -0.0038(12)
O14 0.0271(17) 0.043(2) 0.053(2) 0.0056(17) 0.0054(15) -0.0029(15)
O15 0.0249(18) 0.060(2) 0.060(2) -0.0101(19) -0.0028(16) 0.0013(16)
O16 0.0328(18) 0.0419(19) 0.041(2) -0.0009(16) -0.0063(15) 0.0052(15)
O17 0.049(4) 0.052(3) 0.048(3) 0.009(2) 0.005(3) 0.010(3)
O17' 0.049(4) 0.052(3) 0.048(3) 0.009(2) 0.005(3) 0.010(3)
O18 0.053(2) 0.0337(18) 0.0241(17) 0.0008(14) 0.0030(15) -0.0110(15)
O19 0.047(3) 0.067(4) 0.060(4) 0.000 0.008(3) 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Na1 O14 2.346(4) 5_666 ?
Na1 O17' 2.379(11) . ?
Na1 O15 2.400(4) 2_656 ?
Na1 O15 2.413(4) . ?
Na1 O14 2.416(3) . ?
Na1 O16 2.460(4) . ?
Na1 O17 2.620(6) . ?
Na1 Na1 3.446(4) 5_666 ?
Na1 Na1 3.481(4) 2_656 ?
Nd1 O12 2.430(3) . ?
Nd1 O13 2.509(3) . ?
Nd1 O3 2.514(3) . ?
Nd1 O10 2.526(3) . ?
Nd1 O11 2.527(3) . ?
Nd1 N1 2.567(3) . ?
Nd1 O7 2.570(3) . ?
Nd1 O8 2.581(3) 6_565 ?
Nd1 N3 2.602(3) . ?
Cu1 N2 1.918(3) . ?
Cu1 N4 1.924(3) . ?
Cu1 O1 1.979(3) . ?
Cu1 O5 1.997(3) . ?
Cu1 O9 2.339(3) . ?
C1 O2 1.242(5) . ?
C1 O1 1.284(5) . ?
C1 C2 1.482(5) . ?
C2 N2 1.340(5) . ?
C2 C3 1.396(5) . ?
C3 C4 1.381(5) . ?
C3 H3 0.9300 . ?
C4 N1 1.358(5) . ?
C4 C5 1.493(5) . ?
C5 O4 1.253(5) . ?
C5 O3 1.263(5) . ?
N1 N2 1.335(4) . ?
C6 O6 1.234(5) . ?
C6 O5 1.297(5) . ?
C6 C7 1.483(5) . ?
C7 N4 1.352(5) . ?
C7 C8 1.375(5) . ?
C8 C9 1.377(5) . ?
C8 H8 0.9300 . ?
C9 N3 1.351(5) . ?
C9 C10 1.482(5) . ?
C10 O8 1.254(5) . ?
C10 O7 1.285(4) . ?
N3 N4 1.338(4) . ?
O8 Nd1 2.581(3) 6_566 ?
O9 H9A 0.9600 . ?
O9 H9B 0.9599 . ?
O10 H10A 0.9598 . ?
O10 H10B 0.9600 . ?
O11 H11A 0.9600 . ?
O11 H11B 0.9598 . ?
O12 H12A 0.9601 . ?
O12 H12B 0.9601 . ?
O13 H13A 0.9476 . ?
O13 H13B 0.9444 . ?
O14 Na1 2.346(4) 5_666 ?
O14 H14A 0.9598 . ?
O14 H14B 0.9600 . ?
O15 Na1 2.400(4) 2_656 ?
O15 H15A 0.9598 . ?
O15 H15B 0.9599 . ?
O16 H16A 0.9451 . ?
O16 H16B 0.9527 . ?
O17 H17A 0.9601 . ?
O17 H17B 0.9600 . ?
O17 H17C 0.4921 . ?
O17 H17D 1.2399 . ?
O17' H17B 1.2477 . ?
O17' H17C 0.9569 . ?
O17' H17D 0.9457 . ?
O18 H18A 0.9600 . ?
O18 H18B 0.9599 . ?
O19 H19A 0.9602 . ?
O19 H19B 0.9601 . ?
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
O14 Na1 O17' 89.3(3) 5_666 . ?
O14 Na1 O15 102.98(13) 5_666 2_656 ?
O17' Na1 O15 88.4(3) . 2_656 ?
O14 Na1 O15 171.07(13) 5_666 . ?
O17' Na1 O15 91.2(3) . . ?
O15 Na1 O15 85.95(13) 2_656 . ?
O14 Na1 O14 87.29(12) 5_666 . ?
O17' Na1 O14 92.8(3) . . ?
O15 Na1 O14 169.67(15) 2_656 . ?
O15 Na1 O14 83.78(12) . . ?
O14 Na1 O16 90.54(13) 5_666 . ?
O17' Na1 O16 179.8(3) . . ?
O15 Na1 O16 91.73(12) 2_656 . ?
O15 Na1 O16 89.02(13) . . ?
O14 Na1 O16 87.03(12) . . ?
O14 Na1 O17 81.85(16) 5_666 . ?
O17' Na1 O17 20.9(3) . . ?
O15 Na1 O17 71.40(16) 2_656 . ?
O15 Na1 O17 101.45(17) . . ?
O14 Na1 O17 111.75(17) . . ?
O16 Na1 O17 159.19(17) . . ?
O14 Na1 Na1 44.44(8) 5_666 5_666 ?
O17' Na1 Na1 91.5(3) . 5_666 ?
O15 Na1 Na1 147.41(13) 2_656 5_666 ?
O15 Na1 Na1 126.63(12) . 5_666 ?
O14 Na1 Na1 42.85(9) . 5_666 ?
O16 Na1 Na1 88.29(11) . 5_666 ?
O17 Na1 Na1 99.39(15) . 5_666 ?
O14 Na1 Na1 145.09(12) 5_666 2_656 ?
O17' Na1 Na1 98.4(3) . 2_656 ?
O15 Na1 Na1 43.82(9) 2_656 2_656 ?
O15 Na1 Na1 43.54(9) . 2_656 ?
O14 Na1 Na1 125.90(12) . 2_656 ?
O16 Na1 Na1 81.79(9) . 2_656 ?
O17 Na1 Na1 93.40(13) . 2_656 ?
Na1 Na1 Na1 165.79(10) 5_666 2_656 ?
O12 Nd1 O13 75.85(9) . . ?
O12 Nd1 O3 69.20(9) . . ?
O13 Nd1 O3 70.08(9) . . ?
O12 Nd1 O10 138.62(10) . . ?
O13 Nd1 O10 141.87(9) . . ?
O3 Nd1 O10 129.05(9) . . ?
O12 Nd1 O11 71.87(10) . . ?
O13 Nd1 O11 134.11(10) . . ?
O3 Nd1 O11 124.29(9) . . ?
O10 Nd1 O11 67.80(10) . . ?
O12 Nd1 N1 131.42(9) . . ?
O13 Nd1 N1 80.25(10) . . ?
O3 Nd1 N1 63.03(9) . . ?
O10 Nd1 N1 82.26(10) . . ?
O11 Nd1 N1 145.50(11) . . ?
O12 Nd1 O7 77.78(9) . . ?
O13 Nd1 O7 72.25(9) . . ?
O3 Nd1 O7 134.56(9) . . ?
O10 Nd1 O7 96.35(9) . . ?
O11 Nd1 O7 69.73(10) . . ?
N1 Nd1 O7 132.82(9) . . ?
O12 Nd1 O8 84.85(9) . 6_565 ?
O13 Nd1 O8 136.09(9) . 6_565 ?
O3 Nd1 O8 66.23(9) . 6_565 ?
O10 Nd1 O8 74.55(9) . 6_565 ?
O11 Nd1 O8 72.11(10) . 6_565 ?
N1 Nd1 O8 84.01(9) . 6_565 ?
O7 Nd1 O8 141.33(9) . 6_565 ?
O12 Nd1 N3 136.11(10) . . ?
O13 Nd1 N3 75.31(9) . . ?
O3 Nd1 N3 128.18(10) . . ?
O10 Nd1 N3 67.40(10) . . ?
O11 Nd1 N3 107.51(10) . . ?
N1 Nd1 N3 74.19(10) . . ?
O7 Nd1 N3 62.28(9) . . ?
O8 Nd1 N3 138.04(9) 6_565 . ?
N2 Cu1 N4 97.45(13) . . ?
N2 Cu1 O1 82.46(12) . . ?
N4 Cu1 O1 170.77(13) . . ?
N2 Cu1 O5 173.35(13) . . ?
N4 Cu1 O5 82.66(12) . . ?
O1 Cu1 O5 96.36(11) . . ?
N2 Cu1 O9 91.87(12) . . ?
N4 Cu1 O9 93.98(13) . . ?
O1 Cu1 O9 95.25(12) . . ?
O5 Cu1 O9 94.76(11) . . ?
O2 C1 O1 123.4(4) . . ?
O2 C1 C2 121.8(4) . . ?
O1 C1 C2 114.8(4) . . ?
N2 C2 C3 109.0(3) . . ?
N2 C2 C1 114.1(3) . . ?
C3 C2 C1 136.9(4) . . ?
C4 C3 C2 103.6(3) . . ?
C4 C3 H3 127.9 . . ?
C2 C3 H3 128.5 . . ?
N1 C4 C3 110.8(3) . . ?
N1 C4 C5 116.0(3) . . ?
C3 C4 C5 133.1(4) . . ?
O4 C5 O3 123.0(4) . . ?
O4 C5 C4 120.4(4) . . ?
O3 C5 C4 116.6(3) . . ?
N2 N1 C4 106.5(3) . . ?
N2 N1 Nd1 134.0(2) . . ?
C4 N1 Nd1 117.6(2) . . ?
N1 N2 C2 110.1(3) . . ?
N1 N2 Cu1 135.5(3) . . ?
C2 N2 Cu1 114.4(3) . . ?
C1 O1 Cu1 114.2(2) . . ?
C5 O3 Nd1 122.9(2) . . ?
O6 C6 O5 124.6(4) . . ?
O6 C6 C7 121.0(4) . . ?
O5 C6 C7 114.4(3) . . ?
N4 C7 C8 109.2(3) . . ?
N4 C7 C6 115.0(4) . . ?
C8 C7 C6 135.8(4) . . ?
C7 C8 C9 103.8(3) . . ?
C7 C8 H8 127.9 . . ?
C9 C8 H8 128.3 . . ?
N3 C9 C8 111.3(3) . . ?
N3 C9 C10 118.3(3) . . ?
C8 C9 C10 130.5(4) . . ?
O8 C10 O7 124.6(4) . . ?
O8 C10 C9 120.3(3) . . ?
O7 C10 C9 115.1(3) . . ?
N4 N3 C9 106.2(3) . . ?
N4 N3 Nd1 132.2(2) . . ?
C9 N3 Nd1 117.3(2) . . ?
N3 N4 C7 109.5(3) . . ?
N3 N4 Cu1 136.4(3) . . ?
C7 N4 Cu1 113.7(3) . . ?
C6 O5 Cu1 113.8(2) . . ?
C10 O7 Nd1 123.8(2) . . ?
C10 O8 Nd1 148.7(3) . 6_566 ?
Cu1 O9 H9A 113.9 . . ?
Cu1 O9 H9B 104.3 . . ?
H9A O9 H9B 105.1 . . ?
Nd1 O10 H10A 125.8 . . ?
Nd1 O10 H10B 111.3 . . ?
H10A O10 H10B 107.9 . . ?
Nd1 O11 H11A 121.9 . . ?
Nd1 O11 H11B 123.8 . . ?
H11A O11 H11B 98.7 . . ?
Nd1 O12 H12A 130.2 . . ?
Nd1 O12 H12B 124.5 . . ?
H12A O12 H12B 104.8 . . ?
Nd1 O13 H13A 107.7 . . ?
Nd1 O13 H13B 124.6 . . ?
H13A O13 H13B 97.9 . . ?
Na1 O14 Na1 92.71(12) 5_666 . ?
Na1 O14 H14A 124.9 5_666 . ?
Na1 O14 H14A 109.4 . . ?
Na1 O14 H14B 125.9 5_666 . ?
Na1 O14 H14B 103.6 . . ?
H14A O14 H14B 97.7 . . ?
Na1 O15 Na1 92.64(13) 2_656 . ?
Na1 O15 H15A 116.8 2_656 . ?
Na1 O15 H15A 111.7 . . ?
Na1 O15 H15B 110.4 2_656 . ?
Na1 O15 H15B 129.2 . . ?
H15A O15 H15B 97.6 . . ?
Na1 O16 H16A 105.7 . . ?
Na1 O16 H16B 112.4 . . ?
H16A O16 H16B 95.3 . . ?
Na1 O17 H17A 109.3 . . ?
Na1 O17 H17B 109.2 . . ?
H17A O17 H17B 109.5 . . ?
Na1 O17 H17C 109.5 . . ?
H17A O17 H17C 95.8 . . ?
H17B O17 H17C 122.4 . . ?
Na1 O17 H17D 83.1 . . ?
H17A O17 H17D 142.3 . . ?
H17C O17 H17D 113.9 . . ?
Na1 O17' H17B 112.0 . . ?
Na1 O17' H17C 107.7 . . ?
H17B O17' H17C 70.4 . . ?
Na1 O17' H17D 103.7 . . ?
H17C O17' H17D 104.8 . . ?
H18A O18 H18B 111.2 . . ?
H19A O19 H19B 117.3 . . ?
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
O9 H9A O18 0.96 1.73 2.689(4) 173.4 4_546
O9 H9B O6 0.96 1.98 2.907(4) 161.6 6_565
O10 H10A O9 0.96 1.92 2.874(4) 171.4 .
O10 H10B O2 0.96 1.92 2.862(4) 166.1 4_546
O11 H11A O19 0.96 2.42 2.971(3) 116.5 .
O11 H11B O4 0.96 1.91 2.851(4) 165.8 6_566
O12 H12A O3 0.96 1.94 2.861(4) 158.9 2_556
O12 H12B O7 0.96 1.76 2.700(4) 165.2 5_567
O13 H13A O5 0.95 2.15 2.758(4) 121.0 7_567
O13 H13B O16 0.94 2.29 2.830(4) 115.4 4_556
O14 H14A O5 0.96 2.00 2.920(4) 160.6 6_565
O14 H14B O18 0.96 1.82 2.755(4) 165.2 7_566
O15 H15A O6 0.96 1.83 2.774(4) 165.4 6_565
O15 H15B O1 0.96 2.44 3.294(4) 148.4 .
O16 H16B O4 0.95 2.16 2.885(4) 132.4 3_545
O17 H17A O1 0.96 1.88 2.840(7) 173.5 2_656
O17 H17B O19 0.96 1.91 2.849(7) 166.8 3
O18 H18A O4 0.96 1.70 2.640(4) 167.0 .
O18 H18B O2 0.96 1.75 2.702(4) 170.8 7_566
O19 H19B O12 0.96 2.57 3.491(6) 161.2 .
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 27.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 0.892
_refine_diff_density_min -0.981
_refine_diff_density_rms 0.170
# Attachment '1.cif'
data_51007bm
_database_code_depnum_ccdc_archive 'CCDC 602778'
_audit_update_record
;
2008-06-30 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C10 H12 Cu La N4 O13), 2(H8 Na O4), 3(H2 O)'
_chemical_formula_sum 'C20 H46 Cu2 La2 N8 Na2 O37'
_chemical_formula_weight 1441.53
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_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'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 24.569(5)
_cell_length_b 13.414(3)
_cell_length_c 13.795(3)
_cell_angle_alpha 90.00
_cell_angle_beta 92.440(10)
_cell_angle_gamma 90.00
_cell_volume 4542.3(17)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description block
_exptl_crystal_colour purple
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.108
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2848
_exptl_absorpt_coefficient_mu 2.907
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.40
_exptl_absorpt_correction_T_max 0.64
_exptl_absorpt_process_details 'SADABS(Bruker, 2000)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type ?
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 12883
_diffrn_reflns_av_R_equivalents 0.0365
_diffrn_reflns_av_sigmaI/netI 0.0483
_diffrn_reflns_limit_h_min -31
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 1.73
_diffrn_reflns_theta_max 27.00
_reflns_number_total 4938
_reflns_number_gt 4264
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker, 2000)'
_computing_cell_refinement 'SAINT (Bruker, 2000)'
_computing_data_reduction 'SAINT (Bruker, 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment geom
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4938
_refine_ls_number_parameters 325
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0431
_refine_ls_R_factor_gt 0.0345
_refine_ls_wR_factor_ref 0.0816
_refine_ls_wR_factor_gt 0.0783
_refine_ls_goodness_of_fit_ref 1.023
_refine_ls_restrained_S_all 1.023
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
Na1 Na 0.50712(7) 0.02127(15) 0.62437(14) 0.0435(5) Uani 1 1 d . . .
Cu1 Cu 0.213836(18) 0.63045(4) 0.56890(3) 0.02454(13) Uani 1 1 d . . .
La1 La 0.395211(8) 0.555417(17) 0.606788(16) 0.01980(8) Uani 1 1 d . . .
C1 C 0.18368(15) 0.5930(3) 0.3751(3) 0.0254(9) Uani 1 1 d . . .
C2 C 0.24340(15) 0.5874(3) 0.3825(3) 0.0222(8) Uani 1 1 d . . .
C3 C 0.28382(15) 0.5640(3) 0.3206(3) 0.0245(9) Uani 1 1 d . . .
H3 H 0.2801 0.5468 0.2553 0.029 Uiso 1 1 d R . .
C4 C 0.33118(15) 0.5719(3) 0.3776(3) 0.0212(8) Uani 1 1 d . . .
C5 C 0.38868(15) 0.5554(3) 0.3538(3) 0.0211(8) Uani 1 1 d . . .
N1 N 0.26611(12) 0.6072(3) 0.4711(2) 0.0229(7) Uani 1 1 d . . .
N2 N 0.32000(12) 0.5970(3) 0.4695(2) 0.0225(7) Uani 1 1 d . . .
O1 O 0.16112(10) 0.6187(2) 0.45483(19) 0.0258(6) Uani 1 1 d . . .
O2 O 0.15818(11) 0.5753(2) 0.2976(2) 0.0375(8) Uani 1 1 d . . .
O3 O 0.42280(11) 0.5520(2) 0.4260(2) 0.0278(7) Uani 1 1 d . . .
O4 O 0.40102(11) 0.5457(2) 0.2672(2) 0.0277(7) Uani 1 1 d . . .
C6 C 0.18067(16) 0.7026(3) 0.7452(3) 0.0264(9) Uani 1 1 d . . .
C7 C 0.24106(15) 0.6930(3) 0.7553(3) 0.0225(8) Uani 1 1 d . . .
C8 C 0.28143(15) 0.7130(3) 0.8265(3) 0.0247(9) Uani 1 1 d . . .
H8 H 0.2774 0.7380 0.8886 0.030 Uiso 1 1 d R . .
C9 C 0.32887(15) 0.6869(3) 0.7826(3) 0.0224(8) Uani 1 1 d . . .
C10 C 0.38757(15) 0.6914(3) 0.8147(3) 0.0243(9) Uani 1 1 d . . .
N3 N 0.26403(12) 0.6576(2) 0.6761(2) 0.0233(7) Uani 1 1 d . . .
N4 N 0.31826(12) 0.6530(2) 0.6914(2) 0.0226(7) Uani 1 1 d . . .
O5 O 0.16002(10) 0.6757(2) 0.6617(2) 0.0296(7) Uani 1 1 d . . .
O6 O 0.15335(11) 0.7345(2) 0.8115(2) 0.0345(7) Uani 1 1 d . . .
O7 O 0.42128(10) 0.6609(2) 0.7557(2) 0.0279(6) Uani 1 1 d . . .
O8 O 0.40107(11) 0.7246(2) 0.8971(2) 0.0335(7) Uani 1 1 d . . .
O9 O 0.20773(12) 0.4622(2) 0.6131(2) 0.0336(7) Uani 1 1 d . . .
H9A H 0.2107 0.4212 0.5586 0.040 Uiso 1 1 d R . .
H9B H 0.1735 0.4461 0.6342 0.040 Uiso 1 1 d R . .
O10 O 0.32086(12) 0.4195(2) 0.5918(2) 0.0350(7) Uani 1 1 d . . .
H10A H 0.3299 0.3526 0.5893 0.042 Uiso 1 1 d R . .
H10B H 0.2913 0.4407 0.5534 0.042 Uiso 1 1 d R . .
O11 O 0.43598(13) 0.3840(2) 0.5647(2) 0.0430(8) Uani 1 1 d . . .
H11A H 0.4713 0.3694 0.5937 0.052 Uiso 1 1 d R . .
H11B H 0.4148 0.3344 0.5954 0.052 Uiso 1 1 d R . .
O12 O 0.49601(11) 0.5676(2) 0.6280(2) 0.0341(7) Uani 1 1 d . . .
H12B H 0.5167 0.5230 0.5924 0.041 Uiso 1 1 d R . .
H12A H 0.5086 0.6321 0.6282 0.041 Uiso 1 1 d R . .
O13 O 0.41712(11) 0.7352(2) 0.5546(2) 0.0311(7) Uani 1 1 d . . .
H13A H 0.4326 0.7547 0.6169 0.037 Uiso 1 1 d R . .
H13B H 0.3869 0.7804 0.5565 0.037 Uiso 1 1 d R . .
O14 O 0.56629(12) -0.0031(3) 0.4968(2) 0.0434(8) Uani 1 1 d . . .
H14A H 0.5879 -0.0610 0.4851 0.052 Uiso 1 1 d R . .
H14B H 0.5928 0.0449 0.4781 0.052 Uiso 1 1 d R . .
O15 O 0.56614(13) 0.0419(3) 0.7664(3) 0.0500(9) Uani 1 1 d . . .
H15A H 0.5892 0.0992 0.7607 0.060 Uiso 1 1 d R . .
H15B H 0.5945 -0.0073 0.7680 0.060 Uiso 1 1 d R . .
O16 O 0.50333(12) -0.1597(2) 0.6490(2) 0.0441(8) Uani 1 1 d . A .
H16A H 0.5339 -0.1740 0.6911 0.053 Uiso 1 1 d R . .
H16B H 0.5176 -0.1903 0.5931 0.053 Uiso 1 1 d R . .
O17 O 0.5468(3) 0.1996(4) 0.6223(4) 0.0507(14) Uani 0.676(7) 1 d P A 1
H17A H 0.5573 0.2199 0.6859 0.061 Uiso 0.676(7) 1 d PR A 1
H17B H 0.5767 0.2134 0.5824 0.061 Uiso 0.676(7) 1 d PR A 1
O17' O 0.5111(5) 0.1985(9) 0.6013(9) 0.0507(14) Uani 0.324(7) 1 d P A 2
H17C H 0.5366 0.2134 0.5526 0.061 Uiso 0.324(7) 1 d PR A 2
H17D H 0.5228 0.2297 0.6613 0.061 Uiso 0.324(7) 1 d PR A 2
O18 O 0.14611(13) 0.6484(2) 0.9878(2) 0.0423(8) Uani 1 1 d . . .
H18A H 0.1316 0.6967 1.0311 0.051 Uiso 1 1 d R . .
H18B H 0.1550 0.6793 0.9278 0.051 Uiso 1 1 d R . .
O19 O 0.5000 0.3378(4) 0.7500 0.0640(15) Uani 1 2 d S . .
H19A H 0.4661 0.3719 0.7588 0.077 Uiso 0.50 1 d PR . .
H19B H 0.5358 0.3660 0.7416 0.077 Uiso 0.50 1 d PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Na1 0.0372(10) 0.0525(12) 0.0407(11) 0.0042(9) 0.0012(9) 0.0009(9)
Cu1 0.0171(2) 0.0357(3) 0.0209(3) -0.0040(2) 0.00054(19) 0.0015(2)
La1 0.01634(12) 0.02611(14) 0.01691(13) -0.00105(9) 0.00031(8) 0.00172(9)
C1 0.021(2) 0.029(2) 0.026(2) 0.0055(18) -0.0025(17) -0.0014(17)
C2 0.0204(19) 0.028(2) 0.018(2) 0.0014(16) 0.0007(16) 0.0007(16)
C3 0.0208(19) 0.033(2) 0.019(2) -0.0010(17) -0.0015(16) -0.0005(17)
C4 0.0218(19) 0.022(2) 0.020(2) 0.0016(15) 0.0008(16) 0.0031(15)
C5 0.0205(19) 0.019(2) 0.024(2) -0.0005(16) 0.0011(16) 0.0018(15)
N1 0.0156(15) 0.035(2) 0.0183(18) 0.0001(14) 0.0019(13) 0.0024(14)
N2 0.0155(15) 0.0315(19) 0.0205(18) 0.0006(14) 0.0008(13) 0.0004(14)
O1 0.0143(13) 0.0386(17) 0.0245(16) -0.0013(12) 0.0000(11) 0.0028(12)
O2 0.0251(16) 0.058(2) 0.0283(18) -0.0069(15) -0.0039(13) -0.0012(14)
O3 0.0201(14) 0.0436(18) 0.0196(15) -0.0033(12) -0.0007(11) 0.0069(12)
O4 0.0242(14) 0.0392(18) 0.0198(15) -0.0017(12) 0.0026(12) 0.0048(12)
C6 0.025(2) 0.028(2) 0.026(2) 0.0019(17) 0.0046(18) 0.0015(17)
C7 0.0209(19) 0.027(2) 0.020(2) -0.0006(16) 0.0050(16) 0.0012(16)
C8 0.026(2) 0.028(2) 0.021(2) -0.0043(16) 0.0035(17) 0.0014(17)
C9 0.0225(19) 0.026(2) 0.018(2) -0.0039(16) 0.0006(16) 0.0010(16)
C10 0.022(2) 0.025(2) 0.025(2) -0.0030(17) -0.0010(17) -0.0008(16)
N3 0.0163(15) 0.0300(19) 0.0235(18) -0.0066(14) 0.0001(13) 0.0005(14)
N4 0.0160(15) 0.0287(19) 0.0228(18) -0.0017(14) -0.0012(13) 0.0014(14)
O5 0.0182(13) 0.0403(18) 0.0301(17) -0.0083(13) 0.0000(12) 0.0027(12)
O6 0.0288(15) 0.048(2) 0.0277(17) -0.0001(14) 0.0097(13) 0.0098(14)
O7 0.0220(14) 0.0355(17) 0.0260(16) -0.0075(13) -0.0011(12) 0.0023(12)
O8 0.0270(15) 0.049(2) 0.0245(16) -0.0132(14) -0.0048(12) 0.0033(14)
O9 0.0338(16) 0.0347(18) 0.0324(18) 0.0026(13) 0.0006(14) -0.0052(13)
O10 0.0348(16) 0.0332(17) 0.0365(19) 0.0045(14) -0.0035(14) -0.0042(13)
O11 0.0453(19) 0.040(2) 0.043(2) -0.0041(15) -0.0089(16) 0.0114(15)
O12 0.0201(14) 0.0410(19) 0.0411(19) -0.0095(14) -0.0004(13) 0.0035(13)
O13 0.0288(15) 0.0323(17) 0.0317(17) 0.0013(13) -0.0029(13) 0.0043(13)
O14 0.0315(17) 0.047(2) 0.052(2) 0.0053(17) 0.0056(15) -0.0021(15)
O15 0.0291(17) 0.061(2) 0.060(2) 0.0060(18) -0.0029(16) 0.0010(16)
O16 0.0368(18) 0.044(2) 0.051(2) -0.0001(16) -0.0074(16) 0.0048(15)
O17 0.057(4) 0.057(3) 0.039(3) 0.008(2) 0.008(3) 0.004(3)
O17' 0.057(4) 0.057(3) 0.039(3) 0.008(2) 0.008(3) 0.004(3)
O18 0.059(2) 0.0379(19) 0.0302(18) 0.0008(14) 0.0063(16) 0.0134(16)
O19 0.042(3) 0.080(4) 0.071(4) 0.000 0.008(3) 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Na1 O14 2.353(4) . ?
Na1 O17' 2.401(12) . ?
Na1 O15 2.403(4) . ?
Na1 O15 2.412(4) 2_656 ?
Na1 O14 2.418(4) 5_656 ?
Na1 O16 2.454(4) . ?
Na1 O17 2.584(6) . ?
Na1 Na1 3.481(4) 5_656 ?
Na1 Na1 3.498(4) 2_656 ?
Cu1 N3 1.920(3) . ?
Cu1 N1 1.928(3) . ?
Cu1 O5 1.975(3) . ?
Cu1 O1 2.001(3) . ?
Cu1 O9 2.344(3) . ?
La1 O12 2.487(3) . ?
La1 O7 2.553(3) . ?
La1 O13 2.581(3) . ?
La1 O10 2.583(3) . ?
La1 O11 2.584(3) . ?
La1 O4 2.595(3) 6_566 ?
La1 O3 2.612(3) . ?
La1 N4 2.615(3) . ?
La1 N2 2.649(3) . ?
C1 O2 1.239(5) . ?
C1 O1 1.299(5) . ?
C1 C2 1.468(5) . ?
C2 N1 1.348(5) . ?
C2 C3 1.374(5) . ?
C3 C4 1.381(5) . ?
C3 H3 0.9301 . ?
C4 N2 1.351(5) . ?
C4 C5 1.481(5) . ?
C5 O4 1.251(5) . ?
C5 O3 1.276(4) . ?
N1 N2 1.332(4) . ?
O4 La1 2.595(3) 6_565 ?
C6 O6 1.234(5) . ?
C6 O5 1.290(5) . ?
C6 C7 1.490(5) . ?
C7 N3 1.339(5) . ?
C7 C8 1.391(5) . ?
C8 C9 1.381(5) . ?
C8 H8 0.9301 . ?
C9 N4 1.353(5) . ?
C9 C10 1.492(5) . ?
C10 O8 1.252(5) . ?
C10 O7 1.255(5) . ?
N3 N4 1.341(4) . ?
O9 H9A 0.9368 . ?
O9 H9B 0.9280 . ?
O10 H10A 0.9254 . ?
O10 H10B 0.9254 . ?
O11 H11A 0.9597 . ?
O11 H11B 0.9554 . ?
O12 H12B 0.9374 . ?
O12 H12A 0.9197 . ?
O13 H13A 0.9619 . ?
O13 H13B 0.9588 . ?
O14 Na1 2.418(4) 5_656 ?
O14 H14A 0.9591 . ?
O14 H14B 0.9589 . ?
O15 Na1 2.412(4) 2_656 ?
O15 H15A 0.9590 . ?
O15 H15B 0.9593 . ?
O16 H16A 0.9495 . ?
O16 H16B 0.9536 . ?
O17 H17A 0.9435 . ?
O17 H17B 0.9559 . ?
O17 H17C 1.0010 . ?
O17 H17D 0.9089 . ?
O17' H17C 0.9600 . ?
O17' H17D 0.9600 . ?
O18 H18A 0.9597 . ?
O18 H18B 0.9594 . ?
O19 H19A 0.9629 . ?
O19 H19B 0.9697 . ?
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
O14 Na1 O17' 90.5(3) . . ?
O14 Na1 O15 104.79(13) . . ?
O17' Na1 O15 88.1(3) . . ?
O14 Na1 O15 169.91(13) . 2_656 ?
O17' Na1 O15 90.3(3) . 2_656 ?
O15 Na1 O15 85.29(13) . 2_656 ?
O14 Na1 O14 86.29(12) . 5_656 ?
O17' Na1 O14 92.4(3) . 5_656 ?
O15 Na1 O14 168.90(14) . 5_656 ?
O15 Na1 O14 83.62(12) 2_656 5_656 ?
O14 Na1 O16 89.68(14) . . ?
O17' Na1 O16 179.6(4) . . ?
O15 Na1 O16 91.51(12) . . ?
O15 Na1 O16 89.63(13) 2_656 . ?
O14 Na1 O16 87.95(12) 5_656 . ?
O14 Na1 O17 82.83(16) . . ?
O17' Na1 O17 20.7(3) . . ?
O15 Na1 O17 71.79(16) . . ?
O15 Na1 O17 101.07(17) 2_656 . ?
O14 Na1 O17 110.87(17) 5_656 . ?
O16 Na1 O17 159.11(17) . . ?
O14 Na1 Na1 43.88(8) . 5_656 ?
O17' Na1 Na1 92.0(3) . 5_656 ?
O15 Na1 Na1 148.67(13) . 5_656 ?
O15 Na1 Na1 126.03(12) 2_656 5_656 ?
O14 Na1 Na1 42.41(9) 5_656 5_656 ?
O16 Na1 Na1 88.36(11) . 5_656 ?
O17 Na1 Na1 99.39(15) . 5_656 ?
O14 Na1 Na1 146.32(12) . 2_656 ?
O17' Na1 Na1 97.9(3) . 2_656 ?
O15 Na1 Na1 43.50(9) . 2_656 ?
O15 Na1 Na1 43.31(9) 2_656 2_656 ?
O14 Na1 Na1 125.56(12) 5_656 2_656 ?
O16 Na1 Na1 81.77(9) . 2_656 ?
O17 Na1 Na1 93.70(13) . 2_656 ?
Na1 Na1 Na1 165.11(10) 5_656 2_656 ?
N3 Cu1 N1 98.32(13) . . ?
N3 Cu1 O5 82.42(12) . . ?
N1 Cu1 O5 171.13(14) . . ?
N3 Cu1 O1 173.57(13) . . ?
N1 Cu1 O1 82.24(12) . . ?
O5 Cu1 O1 96.04(11) . . ?
N3 Cu1 O9 91.60(12) . . ?
N1 Cu1 O9 94.50(13) . . ?
O5 Cu1 O9 94.32(12) . . ?
O1 Cu1 O9 94.75(11) . . ?
O12 La1 O7 69.78(9) . . ?
O12 La1 O13 75.70(9) . . ?
O7 La1 O13 70.03(9) . . ?
O12 La1 O10 138.86(10) . . ?
O7 La1 O10 127.44(9) . . ?
O13 La1 O10 142.43(9) . . ?
O12 La1 O11 72.02(10) . . ?
O7 La1 O11 125.97(9) . . ?
O13 La1 O11 132.96(10) . . ?
O10 La1 O11 68.50(10) . . ?
O12 La1 O4 85.15(9) . 6_566 ?
O7 La1 O4 66.46(9) . 6_566 ?
O13 La1 O4 136.24(9) . 6_566 ?
O10 La1 O4 73.28(9) . 6_566 ?
O11 La1 O4 73.66(10) . 6_566 ?
O12 La1 O3 79.40(9) . . ?
O7 La1 O3 135.34(9) . . ?
O13 La1 O3 71.59(9) . . ?
O10 La1 O3 97.04(9) . . ?
O11 La1 O3 69.58(9) . . ?
O4 La1 O3 142.95(9) 6_566 . ?
O12 La1 N4 130.53(10) . . ?
O7 La1 N4 61.64(9) . . ?
O13 La1 N4 79.63(10) . . ?
O10 La1 N4 82.35(10) . . ?
O11 La1 N4 147.17(11) . . ?
O4 La1 N4 84.01(9) 6_566 . ?
O3 La1 N4 131.05(9) . . ?
O12 La1 N2 137.00(10) . . ?
O7 La1 N2 127.01(9) . . ?
O13 La1 N2 75.57(9) . . ?
O10 La1 N2 67.80(10) . . ?
O11 La1 N2 106.99(10) . . ?
O4 La1 N2 137.02(9) 6_566 . ?
O3 La1 N2 61.48(9) . . ?
N4 La1 N2 73.62(10) . . ?
O2 C1 O1 124.3(4) . . ?
O2 C1 C2 121.1(4) . . ?
O1 C1 C2 114.6(3) . . ?
N1 C2 C3 109.1(3) . . ?
N1 C2 C1 115.3(3) . . ?
C3 C2 C1 135.7(4) . . ?
C2 C3 C4 104.0(3) . . ?
C2 C3 H3 128.0 . . ?
C4 C3 H3 128.0 . . ?
N2 C4 C3 110.7(3) . . ?
N2 C4 C5 118.7(3) . . ?
C3 C4 C5 130.6(4) . . ?
O4 C5 O3 124.3(3) . . ?
O4 C5 C4 120.0(3) . . ?
O3 C5 C4 115.7(3) . . ?
N2 N1 C2 109.8(3) . . ?
N2 N1 Cu1 136.1(3) . . ?
C2 N1 Cu1 113.8(2) . . ?
N1 N2 C4 106.4(3) . . ?
N1 N2 La1 132.3(2) . . ?
C4 N2 La1 117.0(2) . . ?
C1 O1 Cu1 113.7(2) . . ?
C5 O3 La1 123.8(2) . . ?
C5 O4 La1 149.5(3) . 6_565 ?
O6 C6 O5 123.6(4) . . ?
O6 C6 C7 122.1(4) . . ?
O5 C6 C7 114.3(4) . . ?
N3 C7 C8 109.4(3) . . ?
N3 C7 C6 114.0(3) . . ?
C8 C7 C6 136.6(4) . . ?
C9 C8 C7 103.4(3) . . ?
C9 C8 H8 128.4 . . ?
C7 C8 H8 128.2 . . ?
N4 C9 C8 111.1(3) . . ?
N4 C9 C10 115.8(3) . . ?
C8 C9 C10 133.1(4) . . ?
O8 C10 O7 123.3(4) . . ?
O8 C10 C9 120.0(4) . . ?
O7 C10 C9 116.7(3) . . ?
C7 N3 N4 109.8(3) . . ?
C7 N3 Cu1 114.6(2) . . ?
N4 N3 Cu1 135.5(3) . . ?
N3 N4 C9 106.4(3) . . ?
N3 N4 La1 133.2(2) . . ?
C9 N4 La1 118.0(2) . . ?
C6 O5 Cu1 114.6(2) . . ?
C10 O7 La1 123.6(2) . . ?
Cu1 O9 H9A 110.3 . . ?
Cu1 O9 H9B 112.0 . . ?
H9A O9 H9B 102.5 . . ?
La1 O10 H10A 121.2 . . ?
La1 O10 H10B 111.3 . . ?
H10A O10 H10B 117.4 . . ?
La1 O11 H11A 116.1 . . ?
La1 O11 H11B 107.2 . . ?
H11A O11 H11B 100.1 . . ?
La1 O12 H12B 117.1 . . ?
La1 O12 H12A 113.3 . . ?
H12B O12 H12A 114.3 . . ?
La1 O13 H13A 94.8 . . ?
La1 O13 H13B 114.3 . . ?
H13A O13 H13B 94.7 . . ?
Na1 O14 Na1 93.71(12) . 5_656 ?
Na1 O14 H14A 127.1 . . ?
Na1 O14 H14A 101.8 5_656 . ?
Na1 O14 H14B 123.8 . . ?
Na1 O14 H14B 112.2 5_656 . ?
H14A O14 H14B 96.3 . . ?
Na1 O15 Na1 93.19(13) . 2_656 ?
Na1 O15 H15A 111.3 . . ?
Na1 O15 H15A 127.0 2_656 . ?
Na1 O15 H15B 110.6 . . ?
Na1 O15 H15B 117.8 2_656 . ?
H15A O15 H15B 97.1 . . ?
Na1 O16 H16A 104.5 . . ?
Na1 O16 H16B 107.2 . . ?
H16A O16 H16B 95.6 . . ?
Na1 O17 H17A 110.2 . . ?
Na1 O17 H17B 119.0 . . ?
H17A O17 H17B 107.0 . . ?
Na1 O17 H17C 95.9 . . ?
H17A O17 H17C 152.6 . . ?
H17B O17 H17C 65.0 . . ?
Na1 O17 H17D 98.6 . . ?
H17A O17 H17D 58.8 . . ?
H17B O17 H17D 142.2 . . ?
H17C O17 H17D 110.2 . . ?
Na1 O17' H17C 109.3 . . ?
Na1 O17' H17D 109.2 . . ?
H17C O17' H17D 109.5 . . ?
H18A O18 H18B 110.5 . . ?
H19A O19 H19B 128.7 . . ?
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
O9 H9A O18 0.94 2.05 2.695(4) 124.4 6_565
O9 H9B O2 0.93 2.32 2.911(4) 121.3 6_566
O10 H10A O6 0.93 2.12 2.875(4) 137.8 4_546
O10 H10B O9 0.93 2.26 2.865(4) 122.2 .
O11 H11A O19 0.96 2.28 3.008(3) 132.0 .
O11 H11B O6 0.96 2.53 3.475(4) 167.8 4_546
O12 H12B O3 0.94 1.82 2.690(4) 152.8 5_666
O12 H12A O8 0.92 2.58 3.320(4) 138.1 2_656
O13 H13A O7 0.96 2.32 2.946(4) 122.3 .
O13 H13B O1 0.96 1.80 2.744(4) 168.1 7_566
O14 H14A O18 0.96 1.85 2.772(5) 160.9 8
O14 H14B O1 0.96 1.99 2.924(4) 165.1 3_545
O15 H15A O5 0.96 2.48 3.303(4) 143.8 3_545
O15 H15B O2 0.96 1.84 2.773(4) 162.7 8_556
O16 H16A O7 0.95 2.57 3.278(4) 131.8 2_646
O16 H16B O8 0.95 2.30 2.908(4) 121.0 2_646
O17 H17B O13 0.96 2.02 2.773(6) 133.9 5_666
O17 H17A O19 0.94 2.32 2.833(7) 113.8 .
O18 H18A O8 0.96 1.68 2.632(4) 173.1 7_567
O18 H18B O6 0.96 1.77 2.704(4) 165.4 .
O19 H19A O4 0.96 1.95 2.909(4) 173.0 6_566
O19 H19B O4 0.97 1.96 2.909(4) 165.5 5_666
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 27.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 0.728
_refine_diff_density_min -0.652
_refine_diff_density_rms 0.111
# Attachment '2.cif'
data_51031dm
_database_code_depnum_ccdc_archive 'CCDC 602779'
_audit_update_record
;
2008-06-30 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C10 H12 Cu N4 O13 Sm), 2(H8 Na O4), 3(H2 O)'
_chemical_formula_sum 'C20 H46 Cu2 N8 Na2 O37 Sm2'
_chemical_formula_weight 1464.41
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_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'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 24.441(7)
_cell_length_b 13.388(3)
_cell_length_c 13.608(3)
_cell_angle_alpha 90.00
_cell_angle_beta 92.480(10)
_cell_angle_gamma 90.00
_cell_volume 4448.6(19)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description block
_exptl_crystal_colour purple
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.186
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2888
_exptl_absorpt_coefficient_mu 3.687
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.30
_exptl_absorpt_correction_T_max 0.57
_exptl_absorpt_process_details 'SADABS(Bruker, 2000)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 12624
_diffrn_reflns_av_R_equivalents 0.0374
_diffrn_reflns_av_sigmaI/netI 0.0456
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 1.73
_diffrn_reflns_theta_max 27.00
_reflns_number_total 4833
_reflns_number_gt 4260
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker, 2000)'
_computing_cell_refinement 'SAINT (Bruker, 2000)'
_computing_data_reduction 'SAINT (Bruker, 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment geom
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4833
_refine_ls_number_parameters 325
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0374
_refine_ls_R_factor_gt 0.0308
_refine_ls_wR_factor_ref 0.0711
_refine_ls_wR_factor_gt 0.0685
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_restrained_S_all 1.039
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
Na1 Na 0.49377(7) 0.47889(15) 0.87614(13) 0.0434(5) Uani 1 1 d . . .
Cu1 Cu 0.285362(18) 0.62985(4) 0.42946(3) 0.02324(12) Uani 1 1 d . . .
Sm1 Sm 0.105215(7) 0.556753(14) 0.393508(14) 0.01886(7) Uani 1 1 d . . .
C1 C 0.31578(16) 0.5953(3) 0.6262(3) 0.0242(8) Uani 1 1 d . . .
C2 C 0.25564(15) 0.5883(3) 0.6178(3) 0.0209(8) Uani 1 1 d . . .
C3 C 0.21493(16) 0.5641(3) 0.6802(3) 0.0228(8) Uani 1 1 d . . .
H3 H 0.2186 0.5471 0.7464 0.027 Uiso 1 1 d R . .
C4 C 0.16744(15) 0.5706(3) 0.6221(3) 0.0195(8) Uani 1 1 d . . .
C5 C 0.11002(15) 0.5525(3) 0.6448(3) 0.0202(8) Uani 1 1 d . . .
C6 C 0.31680(16) 0.7051(3) 0.2515(3) 0.0244(9) Uani 1 1 d . . .
C7 C 0.25683(15) 0.6924(3) 0.2419(3) 0.0218(8) Uani 1 1 d . . .
C8 C 0.21544(15) 0.7127(3) 0.1708(3) 0.0247(9) Uani 1 1 d . . .
H8 H 0.2188 0.7391 0.1082 0.030 Uiso 1 1 d R . .
C9 C 0.16837(15) 0.6841(3) 0.2157(3) 0.0212(8) Uani 1 1 d . . .
C10 C 0.10934(15) 0.6887(3) 0.1861(3) 0.0216(8) Uani 1 1 d . . .
N1 N 0.23278(12) 0.6073(2) 0.5277(2) 0.0231(7) Uani 1 1 d . . .
N2 N 0.17855(12) 0.5961(2) 0.5292(2) 0.0214(7) Uani 1 1 d . . .
N3 N 0.23410(12) 0.6547(2) 0.3217(2) 0.0213(7) Uani 1 1 d . . .
N4 N 0.17999(12) 0.6481(2) 0.3072(2) 0.0220(7) Uani 1 1 d . . .
O1 O 0.33820(10) 0.6209(2) 0.54484(19) 0.0248(6) Uani 1 1 d . . .
O2 O 0.34096(11) 0.5774(2) 0.7037(2) 0.0354(7) Uani 1 1 d . . .
O3 O 0.07637(11) 0.5488(2) 0.57116(19) 0.0260(6) Uani 1 1 d . . .
O4 O 0.09706(11) 0.54336(19) 0.73251(19) 0.0254(6) Uani 1 1 d . . .
O5 O 0.33855(10) 0.6772(2) 0.3350(2) 0.0281(6) Uani 1 1 d . . .
O6 O 0.34361(11) 0.7394(2) 0.1843(2) 0.0330(7) Uani 1 1 d . . .
O7 O 0.07589(10) 0.6580(2) 0.24727(19) 0.0262(6) Uani 1 1 d . . .
O8 O 0.09478(11) 0.7220(2) 0.10289(19) 0.0294(7) Uani 1 1 d . . .
O9 O 0.29187(11) 0.4616(2) 0.3888(2) 0.0307(7) Uani 1 1 d . . .
H9A H 0.3102 0.4570 0.3279 0.037 Uiso 1 1 d R . .
H9B H 0.3099 0.4229 0.4400 0.037 Uiso 1 1 d R . .
O10 O 0.17677(12) 0.4260(2) 0.4092(2) 0.0318(7) Uani 1 1 d . . .
H10A H 0.2152 0.4413 0.4142 0.038 Uiso 1 1 d R . .
H10B H 0.1687 0.3646 0.3752 0.038 Uiso 1 1 d R . .
O11 O 0.06561(12) 0.3897(2) 0.4304(2) 0.0367(7) Uani 1 1 d . . .
H11A H 0.0708 0.3657 0.4972 0.044 Uiso 1 1 d R . .
H11B H 0.0881 0.3461 0.3931 0.044 Uiso 1 1 d R . .
O12 O 0.00745(11) 0.5672(2) 0.3757(2) 0.0301(7) Uani 1 1 d . . .
H12B H -0.0053 0.6354 0.3772 0.036 Uiso 1 1 d R . .
H12A H -0.0147 0.5194 0.4126 0.036 Uiso 1 1 d R . .
O13 O 0.08475(10) 0.72984(19) 0.44444(19) 0.0274(6) Uani 1 1 d . . .
H13A H 0.0882 0.7369 0.5140 0.033 Uiso 1 1 d R . .
H13B H 0.1156 0.7610 0.4181 0.033 Uiso 1 1 d R . .
O14 O 0.56670(13) 0.4593(3) 0.7640(3) 0.0502(9) Uani 1 1 d . . .
H14A H 0.5914 0.5150 0.7679 0.060 Uiso 1 1 d R . .
H14B H 0.5931 0.4113 0.7885 0.060 Uiso 1 1 d R . .
O15 O 0.43328(12) 0.5007(2) 1.0027(2) 0.0409(8) Uani 1 1 d . . .
H15A H 0.4076 0.4462 1.0011 0.049 Uiso 1 1 d R . .
H15B H 0.4105 0.5596 1.0116 0.049 Uiso 1 1 d R . .
O16 O 0.49837(12) 0.6600(2) 0.8515(2) 0.0396(8) Uani 1 1 d . A .
H16A H 0.5247 0.6950 0.8916 0.048 Uiso 1 1 d R . .
H16B H 0.4679 0.6870 0.8829 0.048 Uiso 1 1 d R . .
O17 O 0.4519(3) 0.2983(4) 0.8783(4) 0.0473(13) Uani 0.657(7) 1 d P A 1
H17A H 0.4234 0.3085 0.8292 0.057 Uiso 0.657(7) 1 d PR A 1
H17B H 0.4730 0.2553 0.8381 0.057 Uiso 0.657(7) 1 d PR A 1
O17' O 0.4873(5) 0.3026(8) 0.8990(8) 0.0473(13) Uani 0.343(7) 1 d P A 2
H17C H 0.4689 0.2732 0.8423 0.057 Uiso 0.343(7) 1 d PR A 2
H17D H 0.5236 0.2755 0.9067 0.057 Uiso 0.343(7) 1 d PR A 2
O18 O 0.35619(12) 0.3507(2) 0.5104(2) 0.0382(8) Uani 1 1 d . . .
H18A H 0.3541 0.3249 0.5769 0.046 Uiso 1 1 d R . .
H18B H 0.3699 0.3040 0.4638 0.046 Uiso 1 1 d R . .
O19 O 0.0000 0.6563(4) 0.7500 0.0528(13) Uani 1 2 d S . .
H19A H -0.0150 0.7090 0.7093 0.063 Uiso 0.50 1 d PR . .
H19B H 0.0311 0.6128 0.7463 0.063 Uiso 0.50 1 d PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Na1 0.0368(10) 0.0535(12) 0.0400(11) 0.0022(9) 0.0025(8) 0.0017(9)
Cu1 0.0160(2) 0.0339(3) 0.0199(2) 0.0040(2) 0.00194(19) -0.0021(2)
Sm1 0.01575(11) 0.02354(11) 0.01736(11) 0.00131(8) 0.00165(7) -0.00197(8)
C1 0.020(2) 0.028(2) 0.025(2) -0.0042(17) 0.0007(16) -0.0007(16)
C2 0.019(2) 0.027(2) 0.0163(19) 0.0007(16) 0.0028(15) -0.0021(16)
C3 0.023(2) 0.033(2) 0.0123(18) 0.0032(16) 0.0015(15) 0.0002(16)
C4 0.021(2) 0.023(2) 0.0156(19) -0.0020(15) 0.0049(15) -0.0023(15)
C5 0.021(2) 0.0177(19) 0.022(2) 0.0015(15) 0.0012(15) -0.0012(15)
C6 0.022(2) 0.024(2) 0.028(2) -0.0024(17) 0.0046(17) 0.0000(16)
C7 0.024(2) 0.022(2) 0.019(2) 0.0014(16) 0.0043(16) -0.0005(16)
C8 0.025(2) 0.029(2) 0.020(2) 0.0055(17) -0.0001(16) -0.0006(17)
C9 0.025(2) 0.0201(19) 0.0189(19) 0.0003(15) 0.0016(15) -0.0020(16)
C10 0.024(2) 0.0174(19) 0.023(2) -0.0001(16) 0.0004(16) -0.0004(15)
N1 0.0161(17) 0.0353(19) 0.0183(17) 0.0018(14) 0.0040(13) -0.0028(14)
N2 0.0169(16) 0.0300(18) 0.0174(16) -0.0020(14) 0.0024(13) -0.0025(14)
N3 0.0155(16) 0.0276(18) 0.0207(16) 0.0049(14) 0.0008(13) -0.0013(13)
N4 0.0184(16) 0.0282(18) 0.0196(16) 0.0036(14) 0.0018(13) -0.0005(13)
O1 0.0157(13) 0.0388(16) 0.0199(14) 0.0008(12) -0.0002(11) -0.0037(12)
O2 0.0229(16) 0.056(2) 0.0272(16) 0.0049(14) -0.0022(13) 0.0002(14)
O3 0.0198(14) 0.0380(17) 0.0200(14) 0.0040(12) -0.0007(11) -0.0062(12)
O4 0.0226(15) 0.0336(16) 0.0204(15) 0.0030(12) 0.0038(11) -0.0023(12)
O5 0.0182(14) 0.0377(16) 0.0285(16) 0.0075(13) 0.0026(12) -0.0019(12)
O6 0.0286(16) 0.0429(18) 0.0286(16) 0.0030(14) 0.0125(13) -0.0065(13)
O7 0.0212(14) 0.0327(16) 0.0249(15) 0.0062(12) 0.0034(11) -0.0028(12)
O8 0.0259(15) 0.0401(17) 0.0217(15) 0.0085(13) -0.0030(12) -0.0031(13)
O9 0.0319(16) 0.0340(16) 0.0259(16) -0.0013(13) -0.0022(13) 0.0072(13)
O10 0.0330(17) 0.0317(16) 0.0304(17) -0.0058(13) -0.0022(13) 0.0059(13)
O11 0.0455(19) 0.0373(18) 0.0271(16) 0.0060(13) -0.0009(14) -0.0092(15)
O12 0.0179(14) 0.0379(17) 0.0348(17) 0.0107(13) 0.0031(12) -0.0031(12)
O13 0.0256(15) 0.0301(15) 0.0269(15) -0.0039(12) 0.0044(12) -0.0041(12)
O14 0.0279(18) 0.063(2) 0.059(2) -0.0042(18) -0.0034(16) -0.0004(16)
O15 0.0313(17) 0.0407(19) 0.051(2) 0.0030(16) 0.0043(15) -0.0035(15)
O16 0.0328(17) 0.0386(18) 0.0472(19) 0.0007(15) -0.0021(15) 0.0019(14)
O17 0.047(4) 0.053(3) 0.042(3) 0.005(2) 0.008(3) 0.014(3)
O17' 0.047(4) 0.053(3) 0.042(3) 0.005(2) 0.008(3) 0.014(3)
O18 0.053(2) 0.0362(18) 0.0256(16) -0.0001(13) 0.0032(14) 0.0119(15)
O19 0.042(3) 0.063(3) 0.054(3) 0.000 0.009(2) 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Na1 O15 2.336(4) . ?
Na1 O14 2.377(4) 2_656 ?
Na1 O17' 2.387(11) . ?
Na1 O15 2.391(3) 5_667 ?
Na1 O14 2.410(4) . ?
Na1 O16 2.451(4) . ?
Na1 O17 2.626(6) . ?
Na1 Na1 3.419(4) 5_667 ?
Na1 Na1 3.460(4) 2_656 ?
Cu1 N3 1.916(3) . ?
Cu1 N1 1.918(3) . ?
Cu1 O5 1.972(3) . ?
Cu1 O1 1.993(2) . ?
Cu1 O9 2.327(3) . ?
Sm1 O12 2.395(3) . ?
Sm1 O13 2.476(3) . ?
Sm1 O10 2.477(3) . ?
Sm1 O7 2.487(3) . ?
Sm1 O11 2.496(3) . ?
Sm1 N4 2.530(3) . ?
Sm1 O3 2.550(3) . ?
Sm1 O4 2.569(3) 6_565 ?
Sm1 N2 2.571(3) . ?
C1 O2 1.222(5) . ?
C1 O1 1.302(5) . ?
C1 C2 1.472(5) . ?
C2 N1 1.349(4) . ?
C2 C3 1.375(5) . ?
C3 C4 1.379(5) . ?
C3 H3 0.9299 . ?
C4 N2 1.349(5) . ?
C4 C5 1.470(5) . ?
C5 O4 1.253(4) . ?
C5 O3 1.270(4) . ?
C6 O6 1.236(4) . ?
C6 O5 1.289(4) . ?
C6 C7 1.476(5) . ?
C7 N3 1.340(4) . ?
C7 C8 1.396(5) . ?
C8 C9 1.380(5) . ?
C8 H8 0.9300 . ?
C9 N4 1.353(5) . ?
C9 C10 1.482(5) . ?
C10 O8 1.254(4) . ?
C10 O7 1.261(4) . ?
N1 N2 1.335(4) . ?
N3 N4 1.332(4) . ?
O4 Sm1 2.569(3) 6_566 ?
O9 H9A 0.9599 . ?
O9 H9B 0.9598 . ?
O10 H10A 0.9600 . ?
O10 H10B 0.9599 . ?
O11 H11A 0.9681 . ?
O11 H11B 0.9621 . ?
O12 H12B 0.9659 . ?
O12 H12A 0.9890 . ?
O13 H13A 0.9512 . ?
O13 H13B 0.9463 . ?
O14 Na1 2.377(4) 2_656 ?
O14 H14A 0.9600 . ?
O14 H14B 0.9599 . ?
O15 Na1 2.391(3) 5_667 ?
O15 H15A 0.9618 . ?
O15 H15B 0.9746 . ?
O16 H16A 0.9493 . ?
O16 H16B 0.9463 . ?
O17 H17A 0.9535 . ?
O17 H17B 0.9600 . ?
O17 H17C 0.7366 . ?
O17' H17B 1.0883 . ?
O17' H17C 0.9600 . ?
O17' H17D 0.9600 . ?
O18 H18A 0.9723 . ?
O18 H18B 0.9611 . ?
O19 H19A 0.9605 . ?
O19 H19B 0.9602 . ?
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
O15 Na1 O14 102.37(13) . 2_656 ?
O15 Na1 O17' 88.9(3) . . ?
O14 Na1 O17' 87.3(3) 2_656 . ?
O15 Na1 O15 87.37(12) . 5_667 ?
O14 Na1 O15 170.17(14) 2_656 5_667 ?
O17' Na1 O15 94.3(3) . 5_667 ?
O15 Na1 O14 171.57(14) . . ?
O14 Na1 O14 86.06(13) 2_656 . ?
O17' Na1 O14 91.7(3) . . ?
O15 Na1 O14 84.20(13) 5_667 . ?
O15 Na1 O16 90.64(13) . . ?
O14 Na1 O16 91.74(12) 2_656 . ?
O17' Na1 O16 178.8(3) . . ?
O15 Na1 O16 86.80(12) 5_667 . ?
O14 Na1 O16 88.96(13) . . ?
O15 Na1 O17 81.23(15) . . ?
O14 Na1 O17 71.22(16) 2_656 . ?
O17' Na1 O17 20.0(3) . . ?
O15 Na1 O17 112.12(17) 5_667 . ?
O14 Na1 O17 101.89(16) . . ?
O16 Na1 O17 158.83(17) . . ?
O15 Na1 Na1 44.32(8) . 5_667 ?
O14 Na1 Na1 146.67(13) 2_656 5_667 ?
O17' Na1 Na1 92.2(3) . 5_667 ?
O15 Na1 Na1 43.05(8) 5_667 5_667 ?
O14 Na1 Na1 127.25(12) . 5_667 ?
O16 Na1 Na1 88.20(11) . 5_667 ?
O17 Na1 Na1 99.16(14) . 5_667 ?
O15 Na1 Na1 144.81(12) . 2_656 ?
O14 Na1 Na1 44.11(9) 2_656 2_656 ?
O17' Na1 Na1 97.9(3) . 2_656 ?
O15 Na1 Na1 126.09(12) 5_667 2_656 ?
O14 Na1 Na1 43.33(9) . 2_656 ?
O16 Na1 Na1 81.82(8) . 2_656 ?
O17 Na1 Na1 93.57(12) . 2_656 ?
Na1 Na1 Na1 166.06(10) 5_667 2_656 ?
N3 Cu1 N1 97.20(13) . . ?
N3 Cu1 O5 82.71(12) . . ?
N1 Cu1 O5 170.23(13) . . ?
N3 Cu1 O1 173.33(13) . . ?
N1 Cu1 O1 82.65(12) . . ?
O5 Cu1 O1 96.31(11) . . ?
N3 Cu1 O9 92.02(12) . . ?
N1 Cu1 O9 93.91(12) . . ?
O5 Cu1 O9 95.86(11) . . ?
O1 Cu1 O9 94.64(10) . . ?
O12 Sm1 O13 76.18(9) . . ?
O12 Sm1 O10 138.36(9) . . ?
O13 Sm1 O10 141.97(9) . . ?
O12 Sm1 O7 68.64(9) . . ?
O13 Sm1 O7 70.08(9) . . ?
O10 Sm1 O7 129.17(9) . . ?
O12 Sm1 O11 71.25(10) . . ?
O13 Sm1 O11 134.22(10) . . ?
O10 Sm1 O11 68.18(10) . . ?
O7 Sm1 O11 123.23(9) . . ?
O12 Sm1 N4 131.49(10) . . ?
O13 Sm1 N4 80.56(10) . . ?
O10 Sm1 N4 81.95(10) . . ?
O7 Sm1 N4 63.52(9) . . ?
O11 Sm1 N4 145.15(10) . . ?
O12 Sm1 O3 77.45(9) . . ?
O13 Sm1 O3 72.91(9) . . ?
O10 Sm1 O3 96.44(9) . . ?
O7 Sm1 O3 134.38(9) . . ?
O11 Sm1 O3 69.30(9) . . ?
N4 Sm1 O3 134.03(9) . . ?
O12 Sm1 O4 84.48(9) . 6_565 ?
O13 Sm1 O4 135.88(9) . 6_565 ?
O10 Sm1 O4 74.52(9) . 6_565 ?
O7 Sm1 O4 65.97(9) . 6_565 ?
O11 Sm1 O4 71.79(9) . 6_565 ?
N4 Sm1 O4 83.54(9) . 6_565 ?
O3 Sm1 O4 140.59(8) . 6_565 ?
O12 Sm1 N2 136.22(10) . . ?
O13 Sm1 N2 75.54(9) . . ?
O10 Sm1 N2 67.38(10) . . ?
O7 Sm1 N2 129.08(9) . . ?
O11 Sm1 N2 107.68(10) . . ?
N4 Sm1 N2 74.86(10) . . ?
O3 Sm1 N2 62.65(9) . . ?
O4 Sm1 N2 138.17(9) 6_565 . ?
O2 C1 O1 124.8(4) . . ?
O2 C1 C2 121.2(4) . . ?
O1 C1 C2 114.0(3) . . ?
N1 C2 C3 108.9(3) . . ?
N1 C2 C1 115.6(3) . . ?
C3 C2 C1 135.6(4) . . ?
C2 C3 C4 104.2(3) . . ?
C2 C3 H3 127.9 . . ?
C4 C3 H3 128.0 . . ?
N2 C4 C3 110.8(3) . . ?
N2 C4 C5 118.2(3) . . ?
C3 C4 C5 131.0(3) . . ?
O4 C5 O3 124.5(3) . . ?
O4 C5 C4 119.9(3) . . ?
O3 C5 C4 115.6(3) . . ?
O6 C6 O5 123.2(4) . . ?
O6 C6 C7 122.3(4) . . ?
O5 C6 C7 114.5(3) . . ?
N3 C7 C8 108.8(3) . . ?
N3 C7 C6 114.6(3) . . ?
C8 C7 C6 136.6(4) . . ?
C9 C8 C7 103.4(3) . . ?
C9 C8 H8 128.4 . . ?
C7 C8 H8 128.2 . . ?
N4 C9 C8 111.1(3) . . ?
N4 C9 C10 115.4(3) . . ?
C8 C9 C10 133.5(4) . . ?
O8 C10 O7 123.1(4) . . ?
O8 C10 C9 119.7(4) . . ?
O7 C10 C9 117.2(3) . . ?
N2 N1 C2 109.8(3) . . ?
N2 N1 Cu1 136.3(2) . . ?
C2 N1 Cu1 113.5(2) . . ?
N1 N2 C4 106.4(3) . . ?
N1 N2 Sm1 132.4(2) . . ?
C4 N2 Sm1 117.3(2) . . ?
N4 N3 C7 110.4(3) . . ?
N4 N3 Cu1 135.6(2) . . ?
C7 N3 Cu1 113.9(2) . . ?
N3 N4 C9 106.3(3) . . ?
N3 N4 Sm1 134.1(2) . . ?
C9 N4 Sm1 118.1(2) . . ?
C1 O1 Cu1 113.8(2) . . ?
C5 O3 Sm1 123.4(2) . . ?
C5 O4 Sm1 148.1(2) . 6_566 ?
C6 O5 Cu1 114.2(2) . . ?
C10 O7 Sm1 122.2(2) . . ?
Cu1 O9 H9A 107.9 . . ?
Cu1 O9 H9B 112.5 . . ?
H9A O9 H9B 112.1 . . ?
Sm1 O10 H10A 122.7 . . ?
Sm1 O10 H10B 115.7 . . ?
H10A O10 H10B 113.4 . . ?
Sm1 O11 H11A 116.8 . . ?
Sm1 O11 H11B 101.6 . . ?
H11A O11 H11B 103.8 . . ?
Sm1 O12 H12B 111.9 . . ?
Sm1 O12 H12A 118.5 . . ?
H12B O12 H12A 114.6 . . ?
Sm1 O13 H13A 111.1 . . ?
Sm1 O13 H13B 97.6 . . ?
H13A O13 H13B 107.2 . . ?
Na1 O14 Na1 92.56(13) 2_656 . ?
Na1 O14 H14A 109.0 2_656 . ?
Na1 O14 H14A 111.1 . . ?
Na1 O14 H14B 137.6 2_656 . ?
Na1 O14 H14B 111.0 . . ?
H14A O14 H14B 95.1 . . ?
Na1 O15 Na1 92.63(12) . 5_667 ?
Na1 O15 H15A 108.7 . . ?
Na1 O15 H15A 124.6 5_667 . ?
Na1 O15 H15B 125.1 . . ?
Na1 O15 H15B 103.6 5_667 . ?
H15A O15 H15B 104.0 . . ?
Na1 O16 H16A 116.3 . . ?
Na1 O16 H16B 105.9 . . ?
H16A O16 H16B 94.5 . . ?
Na1 O17 H17A 97.7 . . ?
Na1 O17 H17B 109.1 . . ?
H17A O17 H17B 94.6 . . ?
Na1 O17 H17C 100.5 . . ?
H17A O17 H17C 90.8 . . ?
Na1 O17' H17B 119.8 . . ?
Na1 O17' H17C 109.4 . . ?
Na1 O17' H17D 108.7 . . ?
H17B O17' H17D 97.4 . . ?
H17C O17' H17D 109.5 . . ?
H18A O18 H18B 114.7 . . ?
H19A O19 H19B 134.3 . . ?
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
O9 H9A O2 0.96 1.94 2.884(4) 169.1 6_565
O9 H9B O18 0.96 1.74 2.681(4) 164.7 .
O10 H10A O9 0.96 1.94 2.878(4) 165.1 .
O10 H10B O6 0.96 1.88 2.838(4) 175.7 4_545
O11 H11A O8 0.97 1.93 2.848(4) 158.0 6_566
O11 H11B O6 0.96 2.47 3.422(4) 171.7 4_545
O12 H12B O8 0.97 2.50 3.269(4) 136.4 2
O12 H12A O3 0.99 1.78 2.694(4) 151.4 5_566
O13 H13A O17 0.95 1.98 2.765(6) 138.8 4_556
O13 H13B O1 0.95 1.99 2.745(4) 134.8 7_566
O14 H14A O2 0.96 1.88 2.775(4) 154.6 2_656
O14 H14B O6 0.96 2.56 3.499(4) 166.0 5_666
O15 H15A O1 0.96 2.03 2.915(4) 151.7 6_566
O15 H15B O18 0.97 1.79 2.745(4) 165.4 6_566
O16 H16A O13 0.95 1.90 2.828(4) 167.0 8_566
O16 H16B O8 0.95 1.97 2.861(4) 155.4 7_566
O17 H17A O5 0.95 2.09 2.826(7) 133.1 6_566
O17 H17B O19 0.96 1.92 2.868(6) 167.5 3_545
O18 H18A O6 0.97 1.73 2.686(4) 169.1 6_566
O18 H18B O8 0.96 1.69 2.634(4) 168.5 4_545
O19 H19A O17 0.96 2.32 2.868(6) 115.5 4_556
O19 H19B O4 0.96 1.88 2.832(4) 172.1 .
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 27.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 0.828
_refine_diff_density_min -0.712
_refine_diff_density_rms 0.111
# Attachment '3.cif'
data_51103am
_database_code_depnum_ccdc_archive 'CCDC 602780'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C10 H12 Cu N4 O13 Pr), 2(H8 Na O4), 3(H2 O)'
_chemical_formula_sum 'C20 H46 Cu2 N8 Na2 O37 Pr2'
_chemical_formula_weight 1445.53
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_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'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 24.485(5)
_cell_length_b 13.390(3)
_cell_length_c 13.691(3)
_cell_angle_alpha 90.00
_cell_angle_beta 92.430(10)
_cell_angle_gamma 90.00
_cell_volume 4484.6(17)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description block
_exptl_crystal_colour purple
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.141
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2864
_exptl_absorpt_coefficient_mu 3.212
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.40
_exptl_absorpt_correction_T_max 0.61
_exptl_absorpt_process_details 'SADABS(Bruker, 2000)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 11917
_diffrn_reflns_av_R_equivalents 0.0517
_diffrn_reflns_av_sigmaI/netI 0.0767
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 1.73
_diffrn_reflns_theta_max 26.00
_reflns_number_total 4387
_reflns_number_gt 3437
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker, 2000)'
_computing_cell_refinement 'SAINT (Bruker, 2000)'
_computing_data_reduction 'SAINT (Bruker, 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment geom
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4387
_refine_ls_number_parameters 325
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0578
_refine_ls_R_factor_gt 0.0400
_refine_ls_wR_factor_ref 0.0725
_refine_ls_wR_factor_gt 0.0684
_refine_ls_goodness_of_fit_ref 0.936
_refine_ls_restrained_S_all 0.936
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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
Na1 Na 0.50662(9) 0.52079(18) 0.12427(17) 0.0439(6) Uani 1 1 d . . .
Cu1 Cu 0.21419(3) 0.13013(5) 0.06956(5) 0.02541(17) Uani 1 1 d . . .
Pr1 Pr 0.394994(12) 0.05609(2) 0.10665(2) 0.02132(9) Uani 1 1 d . . .
C1 C 0.1838(2) 0.0938(4) -0.1257(4) 0.0259(13) Uani 1 1 d . . .
C2 C 0.2440(2) 0.0871(4) -0.1178(4) 0.0205(12) Uani 1 1 d . . .
C3 C 0.2845(2) 0.0637(4) -0.1799(4) 0.0222(12) Uani 1 1 d . . .
H3A H 0.2806 0.0457 -0.2477 0.027 Uiso 1 1 d R . .
C4 C 0.3320(2) 0.0713(3) -0.1223(4) 0.0193(12) Uani 1 1 d . . .
C5 C 0.3896(2) 0.0540(4) -0.1458(4) 0.0242(12) Uani 1 1 d . . .
N1 N 0.26676(16) 0.1075(3) -0.0287(3) 0.0232(10) Uani 1 1 d . . .
N2 N 0.32086(16) 0.0965(3) -0.0298(3) 0.0212(10) Uani 1 1 d . . .
O1 O 0.16156(13) 0.1198(3) -0.0452(3) 0.0256(9) Uani 1 1 d . . .
O2 O 0.15877(15) 0.0760(3) -0.2031(3) 0.0365(10) Uani 1 1 d . . .
O3 O 0.42304(14) 0.0507(3) -0.0724(3) 0.0281(9) Uani 1 1 d . . .
O4 O 0.40210(13) 0.0446(3) -0.2328(3) 0.0282(9) Uani 1 1 d . . .
C6 C 0.1817(2) 0.2035(4) 0.2470(4) 0.0248(13) Uani 1 1 d . . .
C7 C 0.2418(2) 0.1928(4) 0.2565(4) 0.0224(12) Uani 1 1 d . . .
C8 C 0.2827(2) 0.2130(4) 0.3273(4) 0.0259(13) Uani 1 1 d . . .
H8A H 0.2788 0.2399 0.3916 0.031 Uiso 1 1 d R . .
C9 C 0.3301(2) 0.1853(4) 0.2832(4) 0.0222(12) Uani 1 1 d . . .
C10 C 0.3889(2) 0.1898(4) 0.3140(4) 0.0253(13) Uani 1 1 d . . .
N3 N 0.26506(17) 0.1560(3) 0.1774(3) 0.0229(10) Uani 1 1 d . . .
N4 N 0.31912(16) 0.1505(3) 0.1918(3) 0.0229(10) Uani 1 1 d . . .
O5 O 0.16079(14) 0.1763(3) 0.1632(3) 0.0286(9) Uani 1 1 d . . .
O6 O 0.15469(15) 0.2363(3) 0.3137(3) 0.0336(10) Uani 1 1 d . . .
O7 O 0.42234(14) 0.1597(3) 0.2536(3) 0.0289(9) Uani 1 1 d . . .
O8 O 0.40299(14) 0.2233(3) 0.3974(3) 0.0327(10) Uani 1 1 d . . .
O9 O 0.20780(14) -0.0384(2) 0.1120(3) 0.0327(10) Uani 1 1 d . . .
H9A H 0.1890 -0.0551 0.1694 0.039 Uiso 1 1 d R . .
H9B H 0.1951 -0.0732 0.0547 0.039 Uiso 1 1 d R . .
O10 O 0.32204(15) -0.0780(3) 0.0898(3) 0.0344(10) Uani 1 1 d . . .
H10A H 0.3306 -0.1346 0.1307 0.041 Uiso 1 1 d R . .
H10B H 0.2835 -0.0666 0.0930 0.041 Uiso 1 1 d R . .
O11 O 0.43495(16) -0.1134(3) 0.0667(3) 0.0417(11) Uani 1 1 d . . .
H11B H 0.4731 -0.1239 0.0824 0.050 Uiso 1 1 d R . .
H11A H 0.4077 -0.1566 0.0923 0.050 Uiso 1 1 d R . .
O12 O 0.49402(13) 0.0681(3) 0.1255(3) 0.0323(10) Uani 1 1 d . . .
H12A H 0.5198 0.0217 0.1005 0.039 Uiso 1 1 d R . .
H12B H 0.5162 0.1113 0.1668 0.039 Uiso 1 1 d R . .
O13 O 0.41605(14) 0.2320(2) 0.0545(3) 0.0310(9) Uani 1 1 d . . .
H13B H 0.3888 0.2726 0.0249 0.037 Uiso 1 1 d R . .
H13A H 0.4228 0.2759 0.1076 0.037 Uiso 1 1 d R . .
O14 O 0.56639(15) 0.4985(3) -0.0022(3) 0.0431(11) Uani 1 1 d . . .
H14A H 0.5907 0.4429 -0.0086 0.052 Uiso 1 1 d R . .
H14B H 0.5895 0.5497 -0.0271 0.052 Uiso 1 1 d R . .
O15 O 0.43355(15) 0.5405(3) 0.2341(3) 0.0499(12) Uani 1 1 d . . .
H15B H 0.4127 0.5965 0.2554 0.060 Uiso 1 1 d R . .
H15A H 0.4058 0.4898 0.2325 0.060 Uiso 1 1 d R . .
O16 O 0.50186(15) 0.3395(3) 0.1484(3) 0.0412(11) Uani 1 1 d . A .
H16B H 0.5247 0.3235 0.0974 0.049 Uiso 1 1 d R . .
H16A H 0.5281 0.3225 0.1977 0.049 Uiso 1 1 d R . .
O17 O 0.5489(4) 0.7008(5) 0.1234(5) 0.051(2) Uani 0.676(10) 1 d P A 1
H17B H 0.5325 0.7349 0.1746 0.062 Uiso 0.676(10) 1 d PR A 1
H17A H 0.5324 0.7239 0.0639 0.062 Uiso 0.676(10) 1 d PR A 1
O17' O 0.5128(8) 0.6951(12) 0.1029(12) 0.051(2) Uani 0.324(10) 1 d P A 2
H17D H 0.4967 0.7275 0.1565 0.062 Uiso 0.324(10) 1 d PR A 2
H17C H 0.4850 0.7129 0.0554 0.062 Uiso 0.324(10) 1 d PR A 2
O18 O 0.35492(16) 0.3516(3) 0.5108(3) 0.0401(11) Uani 1 1 d . . .
H18A H 0.3659 0.2972 0.4704 0.048 Uiso 1 1 d R . .
H18B H 0.3476 0.3220 0.5727 0.048 Uiso 1 1 d R . .
O19 O 0.5000 0.1613(5) 0.7500 0.0616(19) Uani 1 2 d S . .
H19A H 0.5370 0.1375 0.7523 0.074 Uiso 0.50 1 d PR . .
H19B H 0.4730 0.1112 0.7617 0.074 Uiso 0.50 1 d PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Na1 0.0368(15) 0.0512(16) 0.0435(16) 0.0034(13) -0.0008(12) 0.0009(12)
Cu1 0.0187(4) 0.0356(4) 0.0220(4) -0.0039(3) 0.0016(3) 0.0016(3)
Pr1 0.01870(16) 0.02614(17) 0.01913(17) -0.00116(15) 0.00080(11) 0.00205(14)
C1 0.025(3) 0.027(3) 0.026(3) 0.009(3) 0.001(3) 0.002(3)
C2 0.022(3) 0.022(3) 0.017(3) 0.001(2) -0.002(2) -0.003(2)
C3 0.023(3) 0.025(3) 0.019(3) -0.001(2) -0.002(2) -0.004(2)
C4 0.019(3) 0.021(3) 0.018(3) 0.003(2) 0.000(2) -0.004(2)
C5 0.028(3) 0.013(3) 0.031(3) 0.001(3) 0.002(3) 0.002(2)
N1 0.015(2) 0.034(3) 0.021(3) -0.001(2) -0.0009(19) 0.001(2)
N2 0.016(2) 0.029(3) 0.020(3) 0.001(2) 0.0043(19) 0.0005(19)
O1 0.017(2) 0.035(2) 0.024(2) 0.0007(18) -0.0007(16) 0.0033(17)
O2 0.024(2) 0.060(3) 0.026(2) -0.005(2) -0.0074(18) 0.0002(19)
O3 0.023(2) 0.039(2) 0.023(2) -0.0037(18) -0.0006(16) 0.0069(18)
O4 0.023(2) 0.038(2) 0.024(2) -0.0053(18) 0.0026(16) 0.0061(18)
C6 0.028(3) 0.023(3) 0.024(3) 0.006(3) 0.003(3) 0.002(2)
C7 0.021(3) 0.024(3) 0.023(3) -0.001(2) 0.003(2) 0.002(2)
C8 0.034(4) 0.024(3) 0.020(3) -0.003(2) -0.001(3) 0.002(3)
C9 0.023(3) 0.022(3) 0.021(3) -0.001(2) 0.003(2) -0.001(2)
C10 0.027(3) 0.019(3) 0.030(4) 0.002(3) -0.001(3) -0.004(2)
N3 0.020(3) 0.025(3) 0.024(3) -0.003(2) 0.002(2) 0.001(2)
N4 0.018(2) 0.029(3) 0.022(3) -0.003(2) 0.0012(19) -0.001(2)
O5 0.018(2) 0.041(2) 0.027(2) -0.0058(19) 0.0021(17) 0.0012(17)
O6 0.032(2) 0.041(2) 0.028(2) 0.0000(19) 0.0121(18) 0.0092(19)
O7 0.021(2) 0.036(2) 0.029(2) -0.0071(19) 0.0027(17) 0.0020(18)
O8 0.030(2) 0.044(2) 0.024(2) -0.0126(19) -0.0037(18) 0.0008(19)
O9 0.036(2) 0.035(2) 0.027(2) 0.0041(18) 0.0004(18) -0.0078(18)
O10 0.034(2) 0.035(2) 0.033(2) 0.0074(19) -0.0030(19) -0.0033(18)
O11 0.039(3) 0.040(2) 0.046(3) -0.003(2) -0.004(2) 0.006(2)
O12 0.017(2) 0.044(2) 0.036(2) -0.014(2) -0.0031(17) 0.0057(18)
O13 0.031(2) 0.027(2) 0.035(2) 0.0022(18) -0.0035(18) 0.0081(17)
O14 0.033(2) 0.039(2) 0.057(3) 0.008(2) 0.007(2) -0.002(2)
O15 0.030(2) 0.058(3) 0.062(3) -0.013(2) 0.001(2) -0.002(2)
O16 0.038(3) 0.045(3) 0.040(3) 0.003(2) -0.005(2) 0.007(2)
O17 0.059(6) 0.053(4) 0.042(4) 0.008(3) 0.007(4) 0.003(5)
O17' 0.059(6) 0.053(4) 0.042(4) 0.008(3) 0.007(4) 0.003(5)
O18 0.058(3) 0.032(2) 0.030(2) -0.0028(19) 0.004(2) 0.010(2)
O19 0.043(4) 0.080(5) 0.063(5) 0.000 0.010(3) 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Na1 O14 2.333(5) . ?
Na1 O17' 2.357(16) . ?
Na1 O15 2.395(4) 2_655 ?
Na1 O15 2.400(5) . ?
Na1 O14 2.409(4) 5_665 ?
Na1 O16 2.453(4) . ?
Na1 O17 2.623(8) . ?
Na1 Na1 3.450(5) 5_665 ?
Na1 Na1 3.472(5) 2_655 ?
Cu1 N3 1.922(4) . ?
Cu1 N1 1.925(4) . ?
Cu1 O5 1.969(4) . ?
Cu1 O1 1.994(3) . ?
Cu1 O9 2.337(3) . ?
Pr1 O12 2.433(3) . ?
Pr1 O7 2.511(3) . ?
Pr1 O13 2.521(3) . ?
Pr1 O10 2.537(3) . ?
Pr1 O11 2.540(4) . ?
Pr1 N4 2.567(4) . ?
Pr1 O3 2.575(4) . ?
Pr1 O4 2.578(3) 6_556 ?
Pr1 N2 2.606(4) . ?
C1 O2 1.225(6) . ?
C1 O1 1.298(6) . ?
C1 C2 1.475(7) . ?
C2 N1 1.348(6) . ?
C2 C3 1.370(7) . ?
C3 C4 1.382(6) . ?
C3 H3A 0.9599 . ?
C4 N2 1.349(6) . ?
C4 C5 1.478(7) . ?
C5 O4 1.248(6) . ?
C5 O3 1.270(6) . ?
N1 N2 1.333(5) . ?
O4 Pr1 2.578(3) 6 ?
C6 O6 1.230(6) . ?
C6 O5 1.289(6) . ?
C6 C7 1.479(7) . ?
C7 N3 1.339(6) . ?
C7 C8 1.390(6) . ?
C8 C9 1.383(7) . ?
C8 H8A 0.9595 . ?
C9 N4 1.352(6) . ?
C9 C10 1.484(7) . ?
C10 O7 1.254(6) . ?
C10 O8 1.261(6) . ?
N3 N4 1.332(5) . ?
O9 H9A 0.9540 . ?
O9 H9B 0.9539 . ?
O10 H10A 0.9599 . ?
O10 H10B 0.9598 . ?
O11 H11B 0.9603 . ?
O11 H11A 0.9600 . ?
O12 H12A 0.9587 . ?
O12 H12B 0.9601 . ?
O13 H13B 0.9400 . ?
O13 H13A 0.9447 . ?
O14 Na1 2.409(4) 5_665 ?
O14 H14A 0.9600 . ?
O14 H14B 0.9598 . ?
O15 Na1 2.395(4) 2_655 ?
O15 H15B 0.9598 . ?
O15 H15A 0.9599 . ?
O16 H16B 0.9382 . ?
O16 H16A 0.9404 . ?
O17 H17B 0.9421 . ?
O17 H17A 0.9470 . ?
O17' H17A 0.8279 . ?
O17' H17D 0.9529 . ?
O17' H17C 0.9522 . ?
O18 H18A 0.9600 . ?
O18 H18B 0.9598 . ?
O19 H19A 0.9599 . ?
O19 H19B 0.9600 . ?
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
O14 Na1 O17' 89.3(4) . . ?
O14 Na1 O15 103.51(16) . 2_655 ?
O17' Na1 O15 87.2(5) . 2_655 ?
O14 Na1 O15 170.66(16) . . ?
O17' Na1 O15 91.3(4) . . ?
O15 Na1 O15 85.83(16) 2_655 . ?
O14 Na1 O14 86.66(15) . 5_665 ?
O17' Na1 O14 94.0(5) . 5_665 ?
O15 Na1 O14 169.78(18) 2_655 5_665 ?
O15 Na1 O14 84.00(15) . 5_665 ?
O14 Na1 O16 90.48(16) . . ?
O17' Na1 O16 178.9(5) . . ?
O15 Na1 O16 91.76(15) 2_655 . ?
O15 Na1 O16 89.05(16) . . ?
O14 Na1 O16 87.08(14) 5_665 . ?
O14 Na1 O17 81.6(2) . . ?
O17' Na1 O17 20.4(4) . . ?
O15 Na1 O17 71.0(2) 2_655 . ?
O15 Na1 O17 102.0(2) . . ?
O14 Na1 O17 112.1(2) 5_665 . ?
O16 Na1 O17 158.5(2) . . ?
O14 Na1 Na1 44.19(10) . 5_665 ?
O17' Na1 Na1 92.4(4) . 5_665 ?
O15 Na1 Na1 147.69(17) 2_655 5_665 ?
O15 Na1 Na1 126.47(14) . 5_665 ?
O14 Na1 Na1 42.47(11) 5_665 5_665 ?
O16 Na1 Na1 88.29(13) . 5_665 ?
O17 Na1 Na1 99.45(19) . 5_665 ?
O14 Na1 Na1 145.47(14) . 2_655 ?
O17' Na1 Na1 97.6(4) . 2_655 ?
O15 Na1 Na1 43.67(11) 2_655 2_655 ?
O15 Na1 Na1 43.55(11) . 2_655 ?
O14 Na1 Na1 126.17(15) 5_665 2_655 ?
O16 Na1 Na1 81.92(11) . 2_655 ?
O17 Na1 Na1 93.34(17) . 2_655 ?
Na1 Na1 Na1 165.78(12) 5_665 2_655 ?
N3 Cu1 N1 97.71(18) . . ?
N3 Cu1 O5 82.52(16) . . ?
N1 Cu1 O5 170.62(16) . . ?
N3 Cu1 O1 173.57(16) . . ?
N1 Cu1 O1 82.38(16) . . ?
O5 Cu1 O1 96.33(14) . . ?
N3 Cu1 O9 91.78(15) . . ?
N1 Cu1 O9 94.32(16) . . ?
O5 Cu1 O9 95.05(14) . . ?
O1 Cu1 O9 94.63(13) . . ?
O12 Pr1 O7 69.38(11) . . ?
O12 Pr1 O13 75.70(11) . . ?
O7 Pr1 O13 70.14(12) . . ?
O12 Pr1 O10 138.72(12) . . ?
O7 Pr1 O10 128.82(12) . . ?
O13 Pr1 O10 141.93(11) . . ?
O12 Pr1 O11 71.99(12) . . ?
O7 Pr1 O11 125.01(11) . . ?
O13 Pr1 O11 133.51(13) . . ?
O10 Pr1 O11 67.92(12) . . ?
O12 Pr1 N4 131.03(12) . . ?
O7 Pr1 N4 62.47(12) . . ?
O13 Pr1 N4 80.19(12) . . ?
O10 Pr1 N4 82.50(12) . . ?
O11 Pr1 N4 146.12(13) . . ?
O12 Pr1 O3 78.33(11) . . ?
O7 Pr1 O3 134.87(11) . . ?
O13 Pr1 O3 71.96(11) . . ?
O10 Pr1 O3 96.23(11) . . ?
O11 Pr1 O3 69.47(12) . . ?
N4 Pr1 O3 132.35(12) . . ?
O12 Pr1 O4 85.04(11) . 6_556 ?
O7 Pr1 O4 66.39(11) . 6_556 ?
O13 Pr1 O4 136.29(11) . 6_556 ?
O10 Pr1 O4 74.31(11) . 6_556 ?
O11 Pr1 O4 72.77(12) . 6_556 ?
N4 Pr1 O4 83.91(12) . 6_556 ?
O3 Pr1 O4 141.82(11) . 6_556 ?
O12 Pr1 N2 136.29(13) . . ?
O7 Pr1 N2 127.87(12) . . ?
O13 Pr1 N2 75.37(12) . . ?
O10 Pr1 N2 67.37(12) . . ?
O11 Pr1 N2 107.11(12) . . ?
N4 Pr1 N2 74.22(13) . . ?
O3 Pr1 N2 61.90(12) . . ?
O4 Pr1 N2 137.71(12) 6_556 . ?
O2 C1 O1 125.1(5) . . ?
O2 C1 C2 120.9(5) . . ?
O1 C1 C2 114.0(5) . . ?
N1 C2 C3 109.0(4) . . ?
N1 C2 C1 115.4(5) . . ?
C3 C2 C1 135.6(5) . . ?
C2 C3 C4 104.0(5) . . ?
C2 C3 H3A 127.8 . . ?
C4 C3 H3A 128.1 . . ?
N2 C4 C3 110.8(5) . . ?
N2 C4 C5 118.4(4) . . ?
C3 C4 C5 130.7(5) . . ?
O4 C5 O3 125.1(5) . . ?
O4 C5 C4 119.9(5) . . ?
O3 C5 C4 115.0(5) . . ?
N2 N1 C2 109.9(4) . . ?
N2 N1 Cu1 136.1(3) . . ?
C2 N1 Cu1 113.6(3) . . ?
N1 N2 C4 106.2(4) . . ?
N1 N2 Pr1 132.5(3) . . ?
C4 N2 Pr1 117.3(3) . . ?
C1 O1 Cu1 114.1(3) . . ?
C5 O3 Pr1 124.3(3) . . ?
C5 O4 Pr1 148.8(3) . 6 ?
O6 C6 O5 123.8(5) . . ?
O6 C6 C7 122.2(5) . . ?
O5 C6 C7 114.0(5) . . ?
N3 C7 C8 108.5(5) . . ?
N3 C7 C6 114.9(5) . . ?
C8 C7 C6 136.6(5) . . ?
C9 C8 C7 103.7(5) . . ?
C9 C8 H8A 128.2 . . ?
C7 C8 H8A 128.2 . . ?
N4 C9 C8 111.0(5) . . ?
N4 C9 C10 115.5(5) . . ?
C8 C9 C10 133.5(5) . . ?
O7 C10 O8 123.4(5) . . ?
O7 C10 C9 116.8(5) . . ?
O8 C10 C9 119.7(5) . . ?
N4 N3 C7 110.8(4) . . ?
N4 N3 Cu1 135.3(3) . . ?
C7 N3 Cu1 113.8(3) . . ?
N3 N4 C9 106.0(4) . . ?
N3 N4 Pr1 133.9(3) . . ?
C9 N4 Pr1 118.1(3) . . ?
C6 O5 Cu1 114.8(3) . . ?
C10 O7 Pr1 123.1(3) . . ?
Cu1 O9 H9A 118.1 . . ?
Cu1 O9 H9B 106.9 . . ?
H9A O9 H9B 114.3 . . ?
Pr1 O10 H10A 111.7 . . ?
Pr1 O10 H10B 125.0 . . ?
H10A O10 H10B 106.8 . . ?
Pr1 O11 H11B 117.6 . . ?
Pr1 O11 H11A 100.4 . . ?
H11B O11 H11A 121.0 . . ?
Pr1 O12 H12A 125.9 . . ?
Pr1 O12 H12B 129.7 . . ?
H12A O12 H12B 103.7 . . ?
Pr1 O13 H13B 120.9 . . ?
Pr1 O13 H13A 113.2 . . ?
H13B O13 H13A 93.9 . . ?
Na1 O14 Na1 93.34(15) . 5_665 ?
Na1 O14 H14A 125.3 . . ?
Na1 O14 H14A 107.4 5_665 . ?
Na1 O14 H14B 124.7 . . ?
Na1 O14 H14B 105.2 5_665 . ?
H14A O14 H14B 98.3 . . ?
Na1 O15 Na1 92.79(15) 2_655 . ?
Na1 O15 H15B 98.9 2_655 . ?
Na1 O15 H15B 134.2 . . ?
Na1 O15 H15A 110.5 2_655 . ?
Na1 O15 H15A 117.0 . . ?
H15B O15 H15A 100.0 . . ?
Na1 O16 H16B 95.3 . . ?
Na1 O16 H16A 107.5 . . ?
H16B O16 H16A 93.9 . . ?
Na1 O17 H17B 105.1 . . ?
Na1 O17 H17A 98.6 . . ?
H17B O17 H17A 107.5 . . ?
Na1 O17 H17D 82.5 . . ?
H17A O17 H17D 80.4 . . ?
Na1 O17' H17B 111.4 . . ?
Na1 O17' H17A 125.8 . . ?
H17B O17' H17A 95.6 . . ?
Na1 O17' H17D 109.0 . . ?
H17B O17' H17D 48.1 . . ?
H17A O17' H17D 123.6 . . ?
Na1 O17' H17C 106.6 . . ?
H17B O17' H17C 134.2 . . ?
H17A O17' H17C 81.8 . . ?
H17D O17' H17C 96.0 . . ?
H18A O18 H18B 105.1 . . ?
H19A O19 H19B 114.7 . . ?
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
O9 H9A O2 0.95 1.94 2.891(5) 171.3 6_556
O9 H9B O18 0.95 1.79 2.671(5) 151.3 4_545
O10 H10A O6 0.96 1.92 2.862(5) 167.5 4_545
O10 H10B O9 0.96 1.92 2.876(5) 174.4 .
O11 H11B O19 0.96 2.41 2.984(4) 117.8 5_656
O11 H11A O6 0.96 2.49 3.443(6) 170.2 4_545
O12 H12A O3 0.96 1.76 2.703(5) 167.7 5_655
O12 H12B O7 0.96 1.93 2.855(5) 160.3 2_655
O13 H13B O1 0.94 1.92 2.748(5) 145.0 7
O13 H13A O16 0.94 2.17 2.813(5) 124.6 .
O14 H14A O18 0.96 1.81 2.759(5) 170.4 2_655
O14 H14B O1 0.96 2.02 2.920(5) 154.7 3
O15 H15B O5 0.96 2.41 3.301(5) 154.9 4
O15 H15A O2 0.96 1.84 2.764(5) 160.9 7
O16 H16B O8 0.94 2.22 2.892(5) 127.9 2_655
O16 H16A O7 0.94 2.57 3.291(5) 133.8 2_655
O17 H17B O19 0.94 1.92 2.833(8) 161.9 5_666
O17 H17A O13 0.95 2.18 2.766(8) 119.2 5_665
O18 H18A O8 0.96 1.70 2.627(5) 162.1 .
O18 H18B O6 0.96 1.74 2.695(5) 170.9 7_556
O19 H19A O4 0.96 1.97 2.880(5) 157.6 2_655
O19 H19B O4 0.96 1.96 2.880(5) 160.6 1_556
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 0.775
_refine_diff_density_min -0.634
_refine_diff_density_rms 0.124