#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:42:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179258 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/78/4317840.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_4317840
loop_
_publ_author_name
'Jin-Kui Tang'
'Yi-Zhi Li'
'Qing-Lun Wang'
'En-Qing Gao'
'Dai-Zheng Liao'
'Zong-Hui Jiang'
'Shi-Ping Yan'
'Peng Cheng'
'Liu-Fang Wang'
'Geng-Lin Wang'
_publ_contact_author
;
  Dai-Zheng Liao
  Department of Chemistry, Nankai University, Tianjin 300071,China
;
_publ_contact_author_email       ' coord@nankai.edu.cn '
_publ_section_title
;
 Synthesis, Crystal Structure, and Magnetic Properties of the First
 Nonanuclear Lanthanide(III)-Copper(II) Complexes of Macrocyclic Oxamide
 [NaLn2Cu6] (Macrocyclic Oxamide =
 1,4,8,11-Tetraazacyclotradecanne-2,3-dione, Ln = Pr, Nd)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2188
_journal_page_last               2192
_journal_paper_doi               10.1021/ic010674q
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C60 H136 Cl7 Cu6 N24 Na Nd2 O50'
_chemical_formula_weight         2934.79
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.195(4)
_cell_angle_beta                 96.602(4)
_cell_angle_gamma                114.109(4)
_cell_formula_units_Z            1
_cell_length_a                   13.892(3)
_cell_length_b                   14.477(3)
_cell_length_c                   16.213(4)
_cell_measurement_temperature    298(2)
_cell_volume                     2891.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0074
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26192
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    2.221
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          1.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.354
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         13098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.354
_refine_ls_R_factor_all          0.0136
_refine_ls_R_factor_gt           0.0130
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+1.2500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                12614
_reflns_number_total             13098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010674q_2.cif
_cod_data_source_block           2
_cod_database_code               4317840
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Nd1 Nd 0.444550(4) 0.215391(3) 0.471015(3) 0.04011(2) Uani 1 1 d . . .
Cu1 Cu 0.820088(10) 0.269867(10) 0.316316(9) 0.05065(4) Uani 1 1 d . . .
Cu2 Cu 0.129379(10) -0.133582(10) 0.212671(8) 0.05023(3) Uani 1 1 d . . .
Cu3 Cu 0.453357(12) 0.216453(11) 0.832605(8) 0.05330(4) Uani 1 1 d . . .
Na1 Na 0.5000 0.0000 0.5000 0.04299(11) Uani 1 2 d S . .
O1 O 0.55861(6) 0.29858(7) 0.36966(5) 0.05435(18) Uani 1 1 d . . .
O2 O 0.58993(6) 0.15834(5) 0.44986(4) 0.04255(13) Uani 1 1 d . . .
O3 O 0.36495(5) 0.02425(5) 0.41442(4) 0.04073(13) Uani 1 1 d . . .
O4 O 0.32859(7) 0.15683(6) 0.32880(5) 0.05507(17) Uani 1 1 d . . .
O5 O 0.46821(6) 0.13235(6) 0.58951(4) 0.04530(14) Uani 1 1 d . . .
O6 O 0.41218(8) 0.29128(6) 0.60772(5) 0.05805(19) Uani 1 1 d . . .
O7 O 0.24430(8) 0.13662(10) 0.48642(8) 0.0829(3) Uani 1 1 d . . .
H7A H 0.2192 0.1804 0.4807 0.080 Uiso 1 1 d R . .
H7B H 0.2091 0.0823 0.4480 0.080 Uiso 1 1 d R . .
O8 O 0.61674(10) 0.36943(9) 0.55347(7) 0.0818(3) Uani 1 1 d . . .
H8B H 0.6114 0.4254 0.5505 0.080 Uiso 1 1 d R . .
H8C H 0.6252 0.3642 0.6051 0.080 Uiso 1 1 d R . .
O9 O 0.39837(12) 0.36085(9) 0.44607(7) 0.0913(4) Uani 1 1 d . . .
H9B H 0.4343 0.4134 0.4860 0.080 Uiso 1 1 d R . .
H9C H 0.4142 0.3759 0.3991 0.080 Uiso 1 1 d R . .
N1 N 0.73789(7) 0.18306(7) 0.38748(6) 0.04722(18) Uani 1 1 d . . .
N2 N 0.70481(7) 0.31428(8) 0.30641(6) 0.0525(2) Uani 1 1 d . . .
N3 N 0.90471(18) 0.3555(2) 0.24252(14) 0.1343(6) Uani 1 1 d . . .
H3B H 0.8731 0.3012 0.1973 0.080 Uiso 1 1 calc R . .
N4 N 0.9383(3) 0.2285(2) 0.33046(17) 0.1577(11) Uani 1 1 d . . .
H4A H 0.9739 0.2783 0.3783 0.080 Uiso 1 1 calc R . .
N5 N 0.23632(6) -0.11227(6) 0.31150(5) 0.04342(16) Uani 1 1 d . . .
N6 N 0.19301(7) 0.01703(6) 0.23422(7) 0.0523(2) Uani 1 1 d . . .
N7 N 0.00688(12) -0.15705(9) 0.12358(9) 0.0801(2) Uani 1 1 d . . .
H7A H -0.0446 -0.1676 0.1559 0.080 Uiso 1 1 calc R . .
N8 N 0.08895(12) -0.28585(9) 0.17021(9) 0.0801(2) Uani 1 1 d . . .
H8A H 0.1336 -0.2851 0.1332 0.080 Uiso 1 1 calc R . .
N9 N 0.47383(7) 0.13697(7) 0.73549(5) 0.04417(17) Uani 1 1 d . . .
N10 N 0.41962(9) 0.28950(9) 0.74987(5) 0.0578(2) Uani 1 1 d . . .
N11 N 0.4891(3) 0.1451(3) 0.91441(17) 0.1625(11) Uani 1 1 d . . .
H11A H 0.4197 0.0980 0.9089 0.080 Uiso 1 1 calc R . .
N12 N 0.4358(3) 0.2979(3) 0.93239(16) 0.1601(11) Uani 1 1 d . . .
H12C H 0.5048 0.3471 0.9413 0.080 Uiso 1 1 calc R . .
C1 C 0.65556(8) 0.19812(7) 0.40287(6) 0.04275(18) Uani 1 1 d . . .
C2 C 0.63856(9) 0.27635(8) 0.35713(7) 0.0504(2) Uani 1 1 d . . .
C11 C 0.69263(13) 0.38823(13) 0.25908(11) 0.0764(4) Uani 1 1 d . . .
H11A H 0.6218 0.3573 0.2232 0.080 Uiso 1 1 calc R . .
H11B H 0.6992 0.4487 0.2983 0.080 Uiso 1 1 calc R . .
C12 C 0.7730(2) 0.4185(3) 0.20779(17) 0.1343(6) Uani 1 1 d . . .
H12A H 0.7303 0.3868 0.1511 0.080 Uiso 1 1 calc R . .
H12B H 0.7914 0.4917 0.2133 0.080 Uiso 1 1 calc R . .
C13 C 0.86209(16) 0.41611(18) 0.19849(15) 0.0980(6) Uani 1 1 d . . .
H13A H 0.9166 0.4872 0.2137 0.080 Uiso 1 1 calc R . .
H13B H 0.8564 0.3927 0.1383 0.080 Uiso 1 1 calc R . .
C14 C 1.00258(18) 0.35462(19) 0.2398(2) 0.1149(8) Uani 1 1 d . . .
H14A H 1.0589 0.4228 0.2662 0.080 Uiso 1 1 calc R . .
H14B H 1.0090 0.3400 0.1810 0.080 Uiso 1 1 calc R . .
C15 C 1.01882(16) 0.27843(16) 0.28259(11) 0.0836(5) Uani 1 1 d . . .
H15A H 1.0217 0.2256 0.2402 0.080 Uiso 1 1 calc R . .
H15B H 1.0881 0.3125 0.3207 0.080 Uiso 1 1 calc R . .
C16 C 0.93785(12) 0.15111(13) 0.37074(10) 0.0711(4) Uani 1 1 d . . .
H16A H 1.0045 0.1791 0.4119 0.080 Uiso 1 1 calc R . .
H16B H 0.9393 0.0971 0.3287 0.080 Uiso 1 1 calc R . .
C17 C 0.8536(2) 0.1042(2) 0.41293(16) 0.1093(7) Uani 1 1 d . . .
H17A H 0.8305 0.0311 0.3905 0.080 Uiso 1 1 calc R . .
H17B H 0.8912 0.1166 0.4705 0.080 Uiso 1 1 calc R . .
C18 C 0.76257(12) 0.10808(14) 0.42480(11) 0.0761(4) Uani 1 1 d . . .
H18A H 0.7649 0.1233 0.4854 0.080 Uiso 1 1 calc R . .
H18B H 0.7041 0.0400 0.4018 0.080 Uiso 1 1 calc R . .
C3 C 0.2945(2) -0.01458(18) 0.34952(16) 0.1034(7) Uani 1 1 d . . .
C4 C 0.27011(8) 0.06040(7) 0.29928(6) 0.0474(2) Uani 1 1 d . . .
C21 C 0.25013(11) -0.19393(9) 0.35015(7) 0.0560(2) Uani 1 1 d . . .
H21A H 0.3248 -0.1691 0.3770 0.080 Uiso 1 1 calc R . .
H21B H 0.2069 -0.2089 0.3937 0.080 Uiso 1 1 calc R . .
C22 C 0.21830(16) -0.28898(10) 0.28654(14) 0.0986(6) Uani 1 1 d . . .
H22A H 0.2712 -0.2739 0.2502 0.080 Uiso 1 1 calc R . .
H22B H 0.2261 -0.3395 0.3167 0.080 Uiso 1 1 calc R . .
C23 C 0.11462(13) -0.33977(9) 0.23159(9) 0.0700(3) Uani 1 1 d . . .
H23A H 0.0606 -0.3552 0.2670 0.080 Uiso 1 1 calc R . .
H23B H 0.1078 -0.4054 0.2008 0.080 Uiso 1 1 calc R . .
C24 C -0.01595(17) -0.33167(13) 0.11604(9) 0.0819(4) Uani 1 1 d . . .
H24A H -0.0705 -0.3572 0.1501 0.080 Uiso 1 1 calc R . .
H24B H -0.0222 -0.3902 0.0746 0.080 Uiso 1 1 calc R . .
C25 C -0.03514(11) -0.25788(12) 0.07187(10) 0.0755(4) Uani 1 1 d . . .
H25A H -0.0025 -0.2544 0.0219 0.080 Uiso 1 1 calc R . .
H25B H -0.1119 -0.2825 0.0530 0.080 Uiso 1 1 calc R . .
C26 C -0.00081(12) -0.07696(14) 0.08904(9) 0.0778(4) Uani 1 1 d . . .
H26A H -0.0762 -0.0974 0.0672 0.080 Uiso 1 1 calc R . .
H26B H 0.0352 -0.0708 0.0409 0.080 Uiso 1 1 calc R . .
C27 C 0.04333(17) 0.02784(14) 0.14520(12) 0.0987(6) Uani 1 1 d . . .
H27A H 0.0013 0.0233 0.1895 0.080 Uiso 1 1 calc R . .
H27B H 0.0311 0.0738 0.1118 0.080 Uiso 1 1 calc R . .
C28 C 0.15933(11) 0.07828(11) 0.18717(9) 0.0654(3) Uani 1 1 d . . .
H28A H 0.2026 0.0958 0.1439 0.080 Uiso 1 1 calc R . .
H28B H 0.1735 0.1424 0.2252 0.080 Uiso 1 1 calc R . .
C5 C 0.45991(7) 0.16786(7) 0.66433(6) 0.04023(17) Uani 1 1 d . . .
C6 C 0.42816(9) 0.25876(9) 0.67444(7) 0.0524(2) Uani 1 1 d . . .
C31 C 0.50224(12) 0.05077(12) 0.73249(8) 0.0636(3) Uani 1 1 d . . .
H31A H 0.4490 -0.0075 0.6900 0.080 Uiso 1 1 calc R . .
H31B H 0.5709 0.0701 0.7146 0.080 Uiso 1 1 calc R . .
C32 C 0.50910(18) 0.01951(14) 0.80931(9) 0.0851(5) Uani 1 1 d . . .
H32A H 0.4427 -0.0426 0.8022 0.080 Uiso 1 1 calc R . .
H32B H 0.5652 -0.0040 0.8090 0.080 Uiso 1 1 calc R . .
C33 C 0.52551(17) 0.06897(14) 0.89261(9) 0.0832(4) Uani 1 1 d . . .
H33A H 0.6024 0.1007 0.9142 0.080 Uiso 1 1 calc R . .
H33B H 0.4934 0.0156 0.9242 0.080 Uiso 1 1 calc R . .
C34 C 0.49692(17) 0.18816(14) 1.00025(9) 0.0841(4) Uani 1 1 d . . .
H34A H 0.5716 0.2205 1.0289 0.080 Uiso 1 1 calc R . .
H34B H 0.4571 0.1338 1.0285 0.080 Uiso 1 1 calc R . .
C35 C 0.4534(2) 0.2658(3) 1.00516(18) 0.1343(6) Uani 1 1 d . . .
H35A H 0.3859 0.2374 1.0248 0.080 Uiso 1 1 calc R . .
H35B H 0.5026 0.3260 1.0479 0.080 Uiso 1 1 calc R . .
C36 C 0.3915(2) 0.37205(15) 0.92064(10) 0.0945(6) Uani 1 1 d . . .
H36A H 0.3166 0.3397 0.9258 0.080 Uiso 1 1 calc R . .
H36B H 0.4277 0.4306 0.9681 0.080 Uiso 1 1 calc R . .
C37 C 0.3949(2) 0.40981(19) 0.85049(15) 0.1076(7) Uani 1 1 d . . .
H37A H 0.4648 0.4689 0.8631 0.080 Uiso 1 1 calc R . .
H37B H 0.3434 0.4390 0.8519 0.080 Uiso 1 1 calc R . .
C38 C 0.38233(17) 0.37083(15) 0.76508(10) 0.0901(5) Uani 1 1 d . . .
H38A H 0.4222 0.4267 0.7382 0.080 Uiso 1 1 calc R . .
H38B H 0.3070 0.3428 0.7390 0.080 Uiso 1 1 calc R . .
Cl1 Cl 0.24629(3) 0.55893(3) 0.06302(2) 0.07877(9) Uani 1 1 d . . .
O11 O 0.1989(3) 0.6263(3) 0.0368(2) 0.2345(11) Uani 1 1 d . . .
O12 O 0.1689(3) 0.4885(3) 0.09624(17) 0.2065(13) Uani 1 1 d . . .
O13 O 0.3348(3) 0.6225(3) 0.12706(18) 0.2136(14) Uani 1 1 d . . .
O14 O 0.27664(15) 0.51925(15) -0.00882(10) 0.1189(5) Uani 1 1 d . . .
Cl2 Cl 0.06047(6) 0.14842(6) 0.64621(5) 0.1215(2) Uani 1 1 d . . .
O21 O -0.0274(3) 0.0525(2) 0.6065(2) 0.2501(18) Uani 1 1 d . . .
O22 O 0.1194(2) 0.1939(2) 0.58441(14) 0.1616(9) Uani 1 1 d . . .
O23 O 0.0216(3) 0.2113(2) 0.69017(19) 0.2049(13) Uani 1 1 d . . .
O24 O 0.1397(3) 0.1286(3) 0.6875(2) 0.2345(11) Uani 1 1 d . . .
Cl3 Cl 0.21566(6) 0.90352(8) 0.94611(8) 0.1562(4) Uani 1 1 d . . .
O31 O 0.2855(2) 0.8698(2) 0.9103(2) 0.1765(10) Uani 1 1 d . . .
O32 O 0.2330(3) 0.9062(4) 1.0264(3) 0.301(3) Uani 1 1 d . . .
O33 O 0.1018(3) 0.8382(4) 0.9159(3) 0.289(2) Uani 1 1 d . . .
O34 O 0.2419(7) 1.0107(5) 0.9499(5) 0.428(5) Uani 1 1 d . . .
O1W O 0.3677(6) 0.4592(4) 0.5736(3) 0.424(3) Uani 1 1 d . . .
H1WA H 0.3711 0.5182 0.5691 0.080 Uiso 1 1 d R . .
H1WB H 0.3025 0.4165 0.5690 0.080 Uiso 1 1 d R . .
O2W O 0.40119(16) 0.33037(15) 0.24945(15) 0.1541(8) Uani 1 1 d . . .
H2WA H 0.3927 0.3758 0.2255 0.080 Uiso 1 1 d R . .
H2WB H 0.4586 0.3268 0.2400 0.080 Uiso 1 1 d R . .
O3W O 0.2442(5) 0.1239(4) 0.8299(4) 0.424(3) Uani 1 1 d . . .
H3WA H 0.2098 0.1217 0.7821 0.080 Uiso 1 1 d R . .
H3WB H 0.2287 0.0627 0.8367 0.080 Uiso 1 1 d R . .
O4W O 0.67067(18) 0.49990(16) 0.71615(11) 0.1438(7) Uani 1 1 d . . .
H4WA H 0.7353 0.5212 0.7413 0.080 Uiso 1 1 d R . .
H4WB H 0.6633 0.5483 0.6962 0.080 Uiso 1 1 d R . .
Cl4 Cl 1.00001(18) 0.49997(16) 0.50000(11) 0.444(3) Uani 1 2 d SR . .
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'
Cl Cl 0.1484 0.1585 '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'
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
O5 Nd1 O4 135.40(3) . . ?
O5 Nd1 O6 65.94(3) . . ?
O4 Nd1 O6 128.29(3) . . ?
O5 Nd1 O3 71.99(3) . . ?
O4 Nd1 O3 65.59(2) . . ?
O6 Nd1 O3 122.19(3) . . ?
O5 Nd1 O1 135.03(3) . . ?
O4 Nd1 O1 72.40(3) . . ?
O6 Nd1 O1 131.30(3) . . ?
O3 Nd1 O1 106.45(3) . . ?
O5 Nd1 O9 138.11(3) . . ?
O4 Nd1 O9 73.68(3) . . ?
O6 Nd1 O9 72.18(3) . . ?
O3 Nd1 O9 136.08(4) . . ?
O1 Nd1 O9 74.75(4) . . ?
O5 Nd1 O2 72.78(2) . . ?
O4 Nd1 O2 103.47(3) . . ?
O6 Nd1 O2 127.76(3) . . ?
O3 Nd1 O2 69.51(2) . . ?
O1 Nd1 O2 65.40(2) . . ?
O9 Nd1 O2 138.52(4) . . ?
O5 Nd1 O8 84.65(4) . . ?
O4 Nd1 O8 138.82(3) . . ?
O6 Nd1 O8 69.71(4) . . ?
O3 Nd1 O8 142.68(3) . . ?
O1 Nd1 O8 70.27(4) . . ?
O9 Nd1 O8 80.27(5) . . ?
O2 Nd1 O8 76.07(4) . . ?
O5 Nd1 O7 83.87(4) . . ?
O4 Nd1 O7 70.69(4) . . ?
O6 Nd1 O7 66.10(4) . . ?
O3 Nd1 O7 71.80(3) . . ?
O1 Nd1 O7 139.78(3) . . ?
O9 Nd1 O7 80.07(5) . . ?
O2 Nd1 O7 139.32(3) . . ?
O8 Nd1 O7 135.25(4) . . ?
O5 Nd1 Na1 43.118(16) . . ?
O4 Nd1 Na1 104.01(2) . . ?
O6 Nd1 Na1 108.94(2) . . ?
O3 Nd1 Na1 41.396(18) . . ?
O1 Nd1 Na1 105.65(2) . . ?
O9 Nd1 Na1 177.48(3) . . ?
O2 Nd1 Na1 42.627(14) . . ?
O8 Nd1 Na1 102.23(3) . . ?
O7 Nd1 Na1 98.27(3) . . ?
N1 Cu1 N2 84.40(3) . . ?
N1 Cu1 N4 95.15(8) . . ?
N2 Cu1 N4 177.89(10) . . ?
N1 Cu1 N3 178.57(8) . . ?
N2 Cu1 N3 96.71(6) . . ?
N4 Cu1 N3 83.78(9) . . ?
N6 Cu2 N5 84.33(4) . . ?
N6 Cu2 N7 96.41(4) . . ?
N5 Cu2 N7 171.98(6) . . ?
N6 Cu2 N8 165.78(6) . . ?
N5 Cu2 N8 96.59(4) . . ?
N7 Cu2 N8 84.66(5) . . ?
N11 Cu3 N9 95.74(7) . . ?
N11 Cu3 N10 179.11(11) . . ?
N9 Cu3 N10 83.98(4) . . ?
N11 Cu3 N12 83.53(11) . . ?
N9 Cu3 N12 178.73(11) . . ?
N10 Cu3 N12 96.73(9) . . ?
O3 Na1 O3 180.00(3) . 2_656 ?
O3 Na1 O2 73.03(3) . . ?
O3 Na1 O2 106.97(3) 2_656 . ?
O3 Na1 O2 106.97(3) . 2_656 ?
O3 Na1 O2 73.03(3) 2_656 2_656 ?
O2 Na1 O2 180.00(2) . 2_656 ?
O3 Na1 O5 74.39(2) . . ?
O3 Na1 O5 105.61(2) 2_656 . ?
O2 Na1 O5 74.48(3) . . ?
O2 Na1 O5 105.52(3) 2_656 . ?
O3 Na1 O5 105.61(2) . 2_656 ?
O3 Na1 O5 74.39(2) 2_656 2_656 ?
O2 Na1 O5 105.52(3) . 2_656 ?
O2 Na1 O5 74.48(3) 2_656 2_656 ?
O5 Na1 O5 180.0 . 2_656 ?
O3 Na1 Nd1 44.152(16) . . ?
O3 Na1 Nd1 135.848(16) 2_656 . ?
O2 Na1 Nd1 44.49(2) . . ?
O2 Na1 Nd1 135.51(2) 2_656 . ?
O5 Na1 Nd1 43.394(18) . . ?
O5 Na1 Nd1 136.606(18) 2_656 . ?
O3 Na1 Nd1 135.848(16) . 2_656 ?
O3 Na1 Nd1 44.152(16) 2_656 2_656 ?
O2 Na1 Nd1 135.51(2) . 2_656 ?
O2 Na1 Nd1 44.49(2) 2_656 2_656 ?
O5 Na1 Nd1 136.606(18) . 2_656 ?
O5 Na1 Nd1 43.394(18) 2_656 2_656 ?
Nd1 Na1 Nd1 180.0 . 2_656 ?
C2 O1 Nd1 118.80(7) . . ?
C1 O2 Na1 142.62(6) . . ?
C1 O2 Nd1 120.44(6) . . ?
Na1 O2 Nd1 92.88(3) . . ?
C3 O3 Na1 143.71(9) . . ?
C3 O3 Nd1 119.40(9) . . ?
Na1 O3 Nd1 94.45(2) . . ?
C4 O4 Nd1 119.95(7) . . ?
C5 O5 Na1 146.28(6) . . ?
C5 O5 Nd1 120.22(6) . . ?
Na1 O5 Nd1 93.49(3) . . ?
C6 O6 Nd1 119.64(7) . . ?
Nd1 O7 H7A 109.1 . . ?
Nd1 O7 H7B 109.0 . . ?
H7A O7 H7B 109.5 . . ?
Nd1 O8 H8B 109.5 . . ?
Nd1 O8 H8C 108.7 . . ?
H8B O8 H8C 109.5 . . ?
Nd1 O9 H9B 109.5 . . ?
Nd1 O9 H9C 108.8 . . ?
H9B O9 H9C 109.5 . . ?
C1 N1 C18 119.58(9) . . ?
C1 N1 Cu1 114.20(6) . . ?
C18 N1 Cu1 126.20(7) . . ?
C2 N2 C11 119.90(10) . . ?
C2 N2 Cu1 111.02(7) . . ?
C11 N2 Cu1 128.73(8) . . ?
C14 N3 C13 125.50(15) . . ?
C14 N3 Cu1 115.12(13) . . ?
C13 N3 Cu1 119.35(12) . . ?
C14 N3 H3B 90.6 . . ?
C13 N3 H3B 90.6 . . ?
Cu1 N3 H3B 90.6 . . ?
C16 N4 C15 123.3(2) . . ?
C16 N4 Cu1 124.54(17) . . ?
C15 N4 Cu1 111.59(16) . . ?
C16 N4 H4A 92.6 . . ?
C15 N4 H4A 92.6 . . ?
Cu1 N4 H4A 92.6 . . ?
C3 N5 C21 118.94(11) . . ?
C3 N5 Cu2 114.37(10) . . ?
C21 N5 Cu2 126.44(7) . . ?
C4 N6 C28 120.47(9) . . ?
C4 N6 Cu2 113.37(7) . . ?
C28 N6 Cu2 126.13(7) . . ?
C26 N7 C25 119.48(13) . . ?
C26 N7 Cu2 122.25(9) . . ?
C25 N7 Cu2 110.88(10) . . ?
C26 N7 H7A 99.1 . . ?
C25 N7 H7A 99.1 . . ?
Cu2 N7 H7A 99.1 . . ?
C24 N8 C23 120.00(13) . . ?
C24 N8 Cu2 108.06(10) . . ?
C23 N8 Cu2 116.41(9) . . ?
C24 N8 H8A 103.3 . . ?
C23 N8 H8A 103.3 . . ?
Cu2 N8 H8A 103.3 . . ?
C5 N9 C31 118.09(8) . . ?
C5 N9 Cu3 113.56(6) . . ?
C31 N9 Cu3 128.35(7) . . ?
C6 N10 C38 118.45(11) . . ?
C6 N10 Cu3 114.43(8) . . ?
C38 N10 Cu3 127.07(9) . . ?
C33 N11 C34 121.1(2) . . ?
C33 N11 Cu3 122.41(15) . . ?
C34 N11 Cu3 115.31(17) . . ?
C33 N11 H11A 93.5 . . ?
C34 N11 H11A 93.5 . . ?
Cu3 N11 H11A 93.5 . . ?
C35 N12 C36 127.1(2) . . ?
C35 N12 Cu3 112.8(2) . . ?
C36 N12 Cu3 119.30(17) . . ?
C35 N12 H12C 92.8 . . ?
C36 N12 H12C 92.8 . . ?
Cu3 N12 H12C 92.8 . . ?
O2 C1 N1 129.61(8) . . ?
O2 C1 C2 117.16(9) . . ?
N1 C1 C2 113.23(8) . . ?
O1 C2 N2 125.35(10) . . ?
O1 C2 C1 118.09(10) . . ?
N2 C2 C1 116.54(9) . . ?
C12 C11 N2 110.18(14) . . ?
C12 C11 H11A 109.6 . . ?
N2 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
N2 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C13 C12 C11 141.40(18) . . ?
C13 C12 H12A 101.7 . . ?
C11 C12 H12A 101.7 . . ?
C13 C12 H12B 101.7 . . ?
C11 C12 H12B 101.7 . . ?
H12A C12 H12B 104.7 . . ?
C12 C13 N3 122.44(15) . . ?
C12 C13 H13A 106.7 . . ?
N3 C13 H13A 106.7 . . ?
C12 C13 H13B 106.7 . . ?
N3 C13 H13B 106.7 . . ?
H13A C13 H13B 106.6 . . ?
N3 C14 C15 113.30(16) . . ?
N3 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
N3 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
N4 C15 C14 115.57(17) . . ?
N4 C15 H15A 108.4 . . ?
C14 C15 H15A 108.4 . . ?
N4 C15 H15B 108.4 . . ?
C14 C15 H15B 108.4 . . ?
H15A C15 H15B 107.4 . . ?
N4 C16 C17 119.16(15) . . ?
N4 C16 H16A 107.5 . . ?
C17 C16 H16A 107.5 . . ?
N4 C16 H16B 107.5 . . ?
C17 C16 H16B 107.5 . . ?
H16A C16 H16B 107.0 . . ?
C18 C17 C16 138.42(16) . . ?
C18 C17 H17A 102.5 . . ?
C16 C17 H17A 102.5 . . ?
C18 C17 H17B 102.5 . . ?
C16 C17 H17B 102.5 . . ?
H17A C17 H17B 104.9 . . ?
C17 C18 N1 116.01(14) . . ?
C17 C18 H18A 108.3 . . ?
N1 C18 H18A 108.3 . . ?
C17 C18 H18B 108.3 . . ?
N1 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
O3 C3 N5 130.42(14) . . ?
O3 C3 C4 117.75(18) . . ?
N5 C3 C4 111.77(17) . . ?
O4 C4 N6 128.45(10) . . ?
O4 C4 C3 115.68(13) . . ?
N6 C4 C3 115.86(13) . . ?
C22 C21 N5 111.44(10) . . ?
C22 C21 H21A 109.3 . . ?
N5 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
N5 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
C23 C22 C21 122.38(18) . . ?
C23 C22 H22A 106.7 . . ?
C21 C22 H22A 106.7 . . ?
C23 C22 H22B 106.7 . . ?
C21 C22 H22B 106.7 . . ?
H22A C22 H22B 106.6 . . ?
C22 C23 N8 117.88(12) . . ?
C22 C23 H23A 107.8 . . ?
N8 C23 H23A 107.8 . . ?
C22 C23 H23B 107.8 . . ?
N8 C23 H23B 107.8 . . ?
H23A C23 H23B 107.2 . . ?
N8 C24 C25 112.05(14) . . ?
N8 C24 H24A 109.2 . . ?
C25 C24 H24A 109.2 . . ?
N8 C24 H24B 109.2 . . ?
C25 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
N7 C25 C24 112.78(13) . . ?
N7 C25 H25A 109.0 . . ?
C24 C25 H25A 109.0 . . ?
N7 C25 H25B 109.0 . . ?
C24 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
N7 C26 C27 118.16(12) . . ?
N7 C26 H26A 107.8 . . ?
C27 C26 H26A 107.8 . . ?
N7 C26 H26B 107.8 . . ?
C27 C26 H26B 107.8 . . ?
H26A C26 H26B 107.1 . . ?
C26 C27 C28 118.81(17) . . ?
C26 C27 H27A 107.6 . . ?
C28 C27 H27A 107.6 . . ?
C26 C27 H27B 107.6 . . ?
C28 C27 H27B 107.6 . . ?
H27A C27 H27B 107.0 . . ?
N6 C28 C27 114.88(12) . . ?
N6 C28 H28A 108.5 . . ?
C27 C28 H28A 108.5 . . ?
N6 C28 H28B 108.5 . . ?
C27 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
O5 C5 N9 129.06(9) . . ?
O5 C5 C6 117.14(8) . . ?
N9 C5 C6 113.80(8) . . ?
O6 C6 N10 128.98(10) . . ?
O6 C6 C5 116.82(9) . . ?
N10 C6 C5 114.18(9) . . ?
C32 C31 N9 114.15(11) . . ?
C32 C31 H31A 108.7 . . ?
N9 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
N9 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C33 C32 C31 132.85(16) . . ?
C33 C32 H32A 104.0 . . ?
C31 C32 H32A 104.0 . . ?
C33 C32 H32B 104.0 . . ?
C31 C32 H32B 104.0 . . ?
H32A C32 H32B 105.5 . . ?
C32 C33 N11 121.55(18) . . ?
C32 C33 H33A 106.9 . . ?
N11 C33 H33A 106.9 . . ?
C32 C33 H33B 106.9 . . ?
N11 C33 H33B 106.9 . . ?
H33A C33 H33B 106.7 . . ?
N11 C34 C35 110.04(18) . . ?
N11 C34 H34A 109.7 . . ?
C35 C34 H34A 109.7 . . ?
N11 C34 H34B 109.7 . . ?
C35 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?
N12 C35 C34 116.8(2) . . ?
N12 C35 H35A 108.1 . . ?
C34 C35 H35A 108.1 . . ?
N12 C35 H35B 108.1 . . ?
C34 C35 H35B 108.1 . . ?
H35A C35 H35B 107.3 . . ?
C37 C36 N12 120.98(15) . . ?
C37 C36 H36A 107.1 . . ?
N12 C36 H36A 107.1 . . ?
C37 C36 H36B 107.1 . . ?
N12 C36 H36B 107.1 . . ?
H36A C36 H36B 106.8 . . ?
C36 C37 C38 135.6(2) . . ?
C36 C37 H37A 103.3 . . ?
C38 C37 H37A 103.3 . . ?
C36 C37 H37B 103.3 . . ?
C38 C37 H37B 103.3 . . ?
H37A C37 H37B 105.2 . . ?
C37 C38 N10 112.47(15) . . ?
C37 C38 H38A 109.1 . . ?
N10 C38 H38A 109.1 . . ?
C37 C38 H38B 109.1 . . ?
N10 C38 H38B 109.1 . . ?
H38A C38 H38B 107.8 . . ?
O12 Cl1 O13 109.93(18) . . ?
O12 Cl1 O14 116.68(15) . . ?
O13 Cl1 O14 112.06(14) . . ?
O12 Cl1 O11 104.7(2) . . ?
O13 Cl1 O11 105.5(2) . . ?
O14 Cl1 O11 107.08(16) . . ?
O24 Cl2 O23 120.1(2) . . ?
O24 Cl2 O21 108.4(3) . . ?
O23 Cl2 O21 108.7(2) . . ?
O24 Cl2 O22 95.8(2) . . ?
O23 Cl2 O22 113.15(18) . . ?
O21 Cl2 O22 110.0(2) . . ?
O32 Cl3 O31 107.6(2) . . ?
O32 Cl3 O34 98.6(4) . . ?
O31 Cl3 O34 114.6(4) . . ?
O32 Cl3 O33 105.8(3) . . ?
O31 Cl3 O33 116.1(2) . . ?
O34 Cl3 O33 112.1(4) . . ?
H1WA O1W H1WB 109.5 . . ?
H2WA O2W H2WB 109.5 . . ?
H3WA O3W H3WB 109.5 . . ?
H4WA O4W H4WB 109.5 . . ?
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
Nd1 O5 2.4659(7) . ?
Nd1 O4 2.4704(9) . ?
Nd1 O6 2.5020(8) . ?
Nd1 O3 2.5030(8) . ?
Nd1 O1 2.5031(8) . ?
Nd1 O9 2.5094(11) . ?
Nd1 O2 2.5140(8) . ?
Nd1 O8 2.5572(12) . ?
Nd1 O7 2.5983(11) . ?
Nd1 Na1 3.5826(7) . ?
Cu1 N1 1.9387(9) . ?
Cu1 N2 1.9533(10) . ?
Cu1 N4 1.965(3) . ?
Cu1 N3 1.9767(14) . ?
Cu2 N6 1.9481(9) . ?
Cu2 N5 1.9511(9) . ?
Cu2 N7 1.9800(13) . ?
Cu2 N8 2.0288(13) . ?
Cu3 N11 1.931(3) . ?
Cu3 N9 1.9333(8) . ?
Cu3 N10 1.9499(10) . ?
Cu3 N12 1.961(2) . ?
Na1 O3 2.3762(7) . ?
Na1 O3 2.3762(7) 2_656 ?
Na1 O2 2.4293(7) . ?
Na1 O2 2.4293(7) 2_656 ?
Na1 O5 2.4532(8) . ?
Na1 O5 2.4532(8) 2_656 ?
Na1 Nd1 3.5826(7) 2_656 ?
O1 C2 1.3053(14) . ?
O2 C1 1.2646(12) . ?
O3 C3 1.235(3) . ?
O4 C4 1.2774(12) . ?
O5 C5 1.2852(11) . ?
O6 C6 1.2714(14) . ?
O7 H7A 0.8500 . ?
O7 H7B 0.8500 . ?
O8 H8B 0.8500 . ?
O8 H8C 0.8501 . ?
O9 H9B 0.8500 . ?
O9 H9C 0.8501 . ?
N1 C1 1.2930(13) . ?
N1 C18 1.4510(16) . ?
N2 C2 1.3095(15) . ?
N2 C11 1.4547(14) . ?
N3 C14 1.371(3) . ?
N3 C13 1.461(2) . ?
N3 H3B 0.9100 . ?
N4 C16 1.373(3) . ?
N4 C15 1.441(3) . ?
N4 H4A 0.9100 . ?
N5 C3 1.318(3) . ?
N5 C21 1.4820(13) . ?
N6 C4 1.2868(14) . ?
N6 C28 1.4271(15) . ?
N7 C26 1.394(2) . ?
N7 C25 1.4202(19) . ?
N7 H7A 0.9100 . ?
N8 C24 1.444(2) . ?
N8 C23 1.4472(18) . ?
N8 H8A 0.9100 . ?
N9 C5 1.3172(12) . ?
N9 C31 1.4509(14) . ?
N10 C6 1.2762(14) . ?
N10 C38 1.4698(17) . ?
N11 C33 1.408(3) . ?
N11 C34 1.414(3) . ?
N11 H11A 0.9100 . ?
N12 C35 1.360(3) . ?
N12 C36 1.463(3) . ?
N12 H12C 0.9100 . ?
C1 C2 1.5185(14) . ?
C11 C12 1.431(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.278(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.461(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.402(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.323(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C3 C4 1.564(2) . ?
C21 C22 1.465(2) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.436(2) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.460(2) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.492(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.496(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C5 C6 1.5435(14) . ?
C31 C32 1.3907(19) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.382(2) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.475(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.328(3) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.381(3) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
Cl1 O12 1.371(3) . ?
Cl1 O13 1.395(3) . ?
Cl1 O14 1.4087(15) . ?
Cl1 O11 1.465(4) . ?
Cl2 O24 1.373(4) . ?
Cl2 O23 1.390(2) . ?
Cl2 O21 1.418(3) . ?
Cl2 O22 1.430(2) . ?
Cl3 O32 1.288(5) . ?
Cl3 O31 1.398(2) . ?
Cl3 O34 1.432(5) . ?
Cl3 O33 1.451(4) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
O4W H4WA 0.8499 . ?
O4W H4WB 0.8500 . ?
