# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_6339
_database_code_depnum_ccdc_archive 'CCDC 1411162'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
{Tb(OAc)(H2O)[15-MCCu(N)glyha-5](H2O)4}?2NO3?4H2O
_chemical_name_common            metallacrown
_chemical_melting_point          ?
_chemical_formula_moiety         
{Tb(OAc)(H2O)[15-MCCu(N)glyha-5](H2O)4}?2NO3?4H2O
_chemical_formula_sum            'C12 H41 Cu5 N12 O27 Tb'
_chemical_formula_weight         1262.19

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'
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'
Tb Tb -0.1723 4.1537 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5766(9)
_cell_length_b                   12.3448(8)
_cell_length_c                   16.1597(12)
_cell_angle_alpha                101.337(6)
_cell_angle_beta                 107.519(7)
_cell_angle_gamma                106.783(7)
_cell_volume                     1831.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2938
_cell_measurement_theta_min      3.3340
_cell_measurement_theta_max      27.4170

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_F_000             1246
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    4.869
_shelx_estimated_absorpt_T_min   0.234
_shelx_estimated_absorpt_T_max   0.510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.29259
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11881
_diffrn_reflns_av_unetI/netI     0.1358
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.605
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_full        25.020
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6468
_reflns_number_gt                5045
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0600P)²+39.2675P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6468
_refine_ls_number_parameters     515
_refine_ls_number_restraints     1422
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0803
_refine_ls_wR_factor_ref         0.2055
_refine_ls_wR_factor_gt          0.1772
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.006
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.22251(7) 0.86925(5) 0.20445(4) 0.0098(2) Uani 1 1 d . U . . .
Cu1 Cu -0.09949(19) 0.62832(13) -0.00155(10) 0.0119(4) Uani 1 1 d . U . . .
Cu2 Cu 0.19212(19) 0.98243(14) -0.00679(11) 0.0134(4) Uani 1 1 d . U . . .
Cu3 Cu 0.4296(2) 1.21016(14) 0.29484(11) 0.0159(4) Uani 1 1 d . U . . .
Cu4 Cu 0.2855(2) 0.97234(14) 0.45863(10) 0.0142(4) Uani 1 1 d . U . . .
Cu5 Cu 0.1090(2) 0.58651(14) 0.27791(11) 0.0155(4) Uani 1 1 d . U . . .
O1 O -0.1498(11) 0.6743(8) -0.1135(6) 0.0147(16) Uani 1 1 d . U . . .
O2 O 0.0569(11) 0.7795(8) 0.0477(6) 0.0152(14) Uani 1 1 d . U . . .
O3 O 0.3158(11) 1.1483(8) 0.0239(6) 0.0151(16) Uani 1 1 d . U . . .
O4 O 0.2570(11) 1.0140(8) 0.1233(6) 0.0175(14) Uani 1 1 d . U . . .
O5 O 0.4670(11) 1.2831(8) 0.4230(6) 0.0218(17) Uani 1 1 d . U . . .
O6 O 0.3188(11) 1.0647(8) 0.3098(6) 0.0171(14) Uani 1 1 d . U . . .
O7 O 0.2521(11) 0.8470(8) 0.5126(6) 0.0196(18) Uani 1 1 d . U . . .
O8 O 0.2534(11) 0.8472(8) 0.3531(6) 0.0160(15) Uani 1 1 d . U . . .
O9 O -0.0517(11) 0.4517(8) 0.1828(7) 0.0201(17) Uani 1 1 d . U . . .
O10 O 0.1130(11) 0.6571(8) 0.1791(6) 0.0169(14) Uani 1 1 d . U . . .
O11 O 0.3748(11) 0.8210(8) 0.1233(6) 0.0192(16) Uani 1 1 d . U . . .
O12 O 0.4725(13) 0.8925(10) 0.2697(7) 0.0330(18) Uani 1 1 d . U . . .
O13 O 0.2811(12) 0.5096(9) 0.2747(7) 0.0252(15) Uani 1 1 d . U . . .
H13B H 0.2588 0.4720 0.2192 0.030 Uiso 1 1 d R U . . .
H13C H 0.2721 0.4579 0.3026 0.030 Uiso 1 1 d R U . . .
O14 O 0.6399(11) 1.1727(8) 0.3132(6) 0.0188(12) Uani 1 1 d . U . . .
H14B H 0.6162 1.0976 0.2979 0.023 Uiso 1 1 d R U . . .
H14C H 0.6904 1.1995 0.3701 0.023 Uiso 1 1 d R U . . .
O15 O 0.3752(11) 0.9115(8) -0.0212(6) 0.0172(12) Uani 1 1 d . U . . .
H15B H 0.3434 0.8627 -0.0745 0.021 Uiso 1 1 d R U . . .
H15C H 0.3915 0.8734 0.0167 0.021 Uiso 1 1 d R U . . .
O16 O -0.0015(11) 0.8685(8) 0.2124(6) 0.0155(11) Uani 1 1 d . U . . .
H16B H -0.0117 0.8400 0.2548 0.019 Uiso 1 1 d R U . . .
H16C H -0.0675 0.8201 0.1627 0.019 Uiso 1 1 d R U . . .
O17 O -0.2298(11) 0.7107(8) 0.0665(6) 0.0139(12) Uani 1 1 d . U . . .
H17B H -0.2438 0.6797 0.1071 0.017 Uiso 1 1 d R U . . .
H17C H -0.3103 0.6992 0.0268 0.017 Uiso 1 1 d R U . . .
O18 O 0.0219(11) 0.9232(8) 0.3901(6) 0.0178(16) Uani 1 1 d . U . . .
H18C H -0.0189 0.8900 0.4214 0.021 Uiso 1 1 d R U . . .
H18D H -0.0005 0.9832 0.3854 0.021 Uiso 1 1 d R U . . .
O19 O 0.7720(12) 0.2411(9) 0.1954(7) 0.024(2) Uani 1 1 d . . . . .
H19C H 0.8232 0.3125 0.2038 0.028 Uiso 1 1 d R U . . .
H19D H 0.7421 0.2392 0.2386 0.028 Uiso 1 1 d R U . . .
O20 O 0.3776(16) 0.4905(12) 0.4486(9) 0.053(2) Uani 1 1 d . U . . .
H20C H 0.2985 0.4506 0.4502 0.064 Uiso 1 1 d R U . . .
H20D H 0.4148 0.5569 0.4907 0.064 Uiso 1 1 d R U . . .
O21 O 0.2014(14) 0.4678(10) 0.6247(8) 0.0379(18) Uani 1 1 d . U . . .
H21C H 0.2152 0.4324 0.6648 0.045 Uiso 1 1 d R U . . .
H21D H 0.1671 0.4166 0.5721 0.045 Uiso 1 1 d R U . . .
O22 O -0.0338(16) 0.1207(11) 0.3653(9) 0.048(2) Uani 1 1 d . U . . .
O23 O 0.0855(15) 0.3151(11) 0.4281(9) 0.0461(17) Uani 1 1 d . U . . .
O24 O 0.1003(15) 0.2027(11) 0.5084(8) 0.0406(19) Uani 1 1 d . U . . .
O25 O 0.2595(14) 0.3786(11) 0.7759(8) 0.0392(19) Uani 1 1 d . U . . .
O26 O 0.4494(14) 0.3826(11) 0.7543(8) 0.0386(19) Uani 1 1 d . U . . .
O27 O 0.4478(14) 0.4171(10) 0.8901(8) 0.037(2) Uani 1 1 d . U . . .
C1 C -0.0481(16) 0.8293(12) -0.1759(9) 0.016(2) Uani 1 1 d . U . . .
H1A H -0.0575 0.7720 -0.2301 0.019 Uiso 1 1 calc R U . . .
H1B H -0.1286 0.8545 -0.1915 0.019 Uiso 1 1 calc R U . . .
C2 C -0.0480(15) 0.7706(11) -0.0989(8) 0.011(2) Uani 1 1 d . U . . .
C3 C 0.4722(16) 1.3198(12) 0.1572(9) 0.016(2) Uani 1 1 d . U . . .
H3A H 0.4291 1.3700 0.1296 0.020 Uiso 1 1 calc R U . . .
H3B H 0.5619 1.3317 0.1491 0.020 Uiso 1 1 calc R U . . .
C4 C 0.3758(16) 1.1937(12) 0.1129(9) 0.0151(18) Uani 1 1 d . U . . .
C5 C 0.4309(17) 1.2265(12) 0.5514(9) 0.020(2) Uani 1 1 d . U . . .
H5A H 0.3997 1.2909 0.5688 0.024 Uiso 1 1 calc R U . . .
H5B H 0.5312 1.2509 0.5891 0.024 Uiso 1 1 calc R U . . .
C6 C 0.4109(16) 1.2000(12) 0.4519(9) 0.017(2) Uani 1 1 d . U . . .
C7 C 0.165(2) 0.6326(14) 0.4693(11) 0.033(2) Uani 1 1 d . U . . .
H7A H 0.2481 0.6199 0.5058 0.039 Uiso 1 1 calc R U . . .
H7B H 0.1055 0.6355 0.5041 0.039 Uiso 1 1 calc R U . . .
C8 C 0.2139(17) 0.7488(13) 0.4516(10) 0.021(2) Uani 1 1 d . U . . .
C9 C -0.2231(16) 0.4120(12) 0.0324(9) 0.017(2) Uani 1 1 d . U . . .
H9A H -0.2245 0.3319 0.0138 0.021 Uiso 1 1 calc R U . . .
H9B H -0.3033 0.4078 0.0507 0.021 Uiso 1 1 calc R U . . .
C10 C -0.0877(15) 0.4874(11) 0.1119(9) 0.0133(19) Uani 1 1 d . U . . .
C11 C 0.6304(17) 0.8907(13) 0.1921(10) 0.0221(17) Uani 1 1 d . U . . .
H11A H 0.6712 0.8400 0.2193 0.033 Uiso 1 1 calc R U . . .
H11B H 0.6904 0.9724 0.2253 0.033 Uiso 1 1 calc R U . . .
H11C H 0.6227 0.8745 0.1298 0.033 Uiso 1 1 calc R U . . .
C12 C 0.4873(17) 0.8678(12) 0.1948(9) 0.0189(18) Uani 1 1 d . U . . .
N1 N 0.0866(13) 0.9332(10) -0.1445(7) 0.0146(18) Uani 1 1 d . U . . .
H1C H 0.0674 0.9939 -0.1596 0.018 Uiso 1 1 calc R U . . .
H1D H 0.1422 0.9152 -0.1723 0.018 Uiso 1 1 calc R U . . .
N2 N 0.0568(13) 0.8341(10) -0.0214(7) 0.0151(16) Uani 1 1 d . U . . .
N3 N 0.4989(14) 1.3528(10) 0.2574(8) 0.0180(19) Uani 1 1 d . U . . .
H3C H 0.4548 1.4016 0.2697 0.022 Uiso 1 1 calc R U . . .
H3D H 0.5921 1.3913 0.2897 0.022 Uiso 1 1 calc R U . . .
N4 N 0.3542(13) 1.1325(10) 0.1673(7) 0.0155(16) Uani 1 1 d . U . . .
N5 N 0.3440(14) 1.1153(10) 0.5660(8) 0.019(2) Uani 1 1 d . U . . .
H5C H 0.2666 1.1236 0.5729 0.023 Uiso 1 1 calc R U . . .
H5D H 0.3958 1.1053 0.6165 0.023 Uiso 1 1 calc R U . . .
N6 N 0.3356(13) 1.0916(10) 0.4018(7) 0.0155(17) Uani 1 1 d . U . . .
N7 N 0.0848(16) 0.5315(11) 0.3840(8) 0.0277(18) Uani 1 1 d . U . . .
H7D H -0.0077 0.5159 0.3752 0.033 Uiso 1 1 d R U . . .
H7C H 0.0978 0.4631 0.3862 0.033 Uiso 1 1 d R U . . .
N8 N 0.2098(14) 0.7396(10) 0.3700(8) 0.0186(16) Uani 1 1 d . U . . .
N9 N -0.2399(13) 0.4587(9) -0.0461(7) 0.0141(18) Uani 1 1 d . U . . .
H9C H -0.3286 0.4563 -0.0700 0.017 Uiso 1 1 calc R U . . .
H9D H -0.2230 0.4146 -0.0891 0.017 Uiso 1 1 calc R U . . .
N10 N -0.0148(13) 0.5825(10) 0.1030(7) 0.0152(16) Uani 1 1 d . U . . .
N11 N 0.0420(19) 0.2104(14) 0.4296(11) 0.043(2) Uani 1 1 d . U . . .
N12 N 0.3843(17) 0.3920(13) 0.8054(10) 0.033(2) Uani 1 1 d . U . . .


_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
Tb1 O6 2.383(9) . ?
Tb1 O8 2.406(9) . ?
Tb1 O16 2.409(10) . ?
Tb1 O2 2.412(9) . ?
Tb1 O4 2.425(9) . ?
Tb1 O10 2.431(9) . ?
Tb1 O12 2.439(12) . ?
Tb1 O11 2.488(10) . ?
Cu1 O2 1.922(9) . ?
Cu1 N10 1.931(11) . ?
Cu1 O1 1.969(9) . ?
Cu1 N9 2.018(11) . ?
Cu1 O17 2.330(10) . ?
Cu2 N2 1.889(11) . ?
Cu2 O4 1.922(9) . ?
Cu2 O3 1.953(9) . ?
Cu2 N1 2.036(11) . ?
Cu2 O15 2.396(11) . ?
Cu3 N4 1.897(11) . ?
Cu3 O6 1.944(9) . ?
Cu3 O5 1.955(10) . ?
Cu3 N3 1.986(11) . ?
Cu3 O14 2.345(11) . ?
Cu4 N6 1.914(11) . ?
Cu4 O7 1.918(9) . ?
Cu4 O8 1.929(9) . ?
Cu4 N5 2.007(11) . ?
Cu5 N8 1.923(12) . ?
Cu5 O9 1.952(10) . ?
Cu5 O10 1.969(9) . ?
Cu5 N7 2.021(12) . ?
Cu5 O13 2.291(12) . ?
O1 C2 1.275(16) . ?
O2 N2 1.413(13) . ?
O3 C4 1.309(16) . ?
O4 N4 1.409(14) . ?
O5 C6 1.275(16) . ?
O6 N6 1.402(14) . ?
O7 C8 1.269(17) . ?
O8 N8 1.384(14) . ?
O9 C10 1.297(16) . ?
O10 N10 1.423(15) . ?
O11 C12 1.265(17) . ?
O12 C12 1.256(17) . ?
O13 H13B 0.8501 . ?
O13 H13C 0.8502 . ?
O14 H14B 0.8500 . ?
O14 H14C 0.8500 . ?
O15 H15B 0.8500 . ?
O15 H15C 0.8499 . ?
O16 H16B 0.8501 . ?
O16 H16C 0.8499 . ?
O17 H17B 0.8500 . ?
O17 H17C 0.8500 . ?
O18 H18C 0.8499 . ?
O18 H18D 0.8500 . ?
O19 H19C 0.8500 . ?
O19 H19D 0.8500 . ?
O20 H20C 0.8501 . ?
O20 H20D 0.8501 . ?
O21 H21C 0.8496 . ?
O21 H21D 0.8504 . ?
O22 N11 1.218(19) . ?
O23 N11 1.247(18) . ?
O24 N11 1.272(19) . ?
O25 N12 1.209(19) . ?
O26 N12 1.233(18) . ?
O27 N12 1.258(18) . ?
C1 N1 1.478(17) . ?
C1 C2 1.558(17) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.300(17) . ?
C3 C4 1.477(18) . ?
C3 N3 1.506(16) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.294(17) . ?
C5 C6 1.512(18) . ?
C5 N5 1.521(18) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N6 1.285(17) . ?
C7 N7 1.48(2) . ?
C7 C8 1.49(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N8 1.288(18) . ?
C9 N9 1.478(16) . ?
C9 C10 1.491(19) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N10 1.267(17) . ?
C11 C12 1.47(2) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N5 H5C 0.8900 . ?
N5 H5D 0.8900 . ?
N7 H7D 0.9000 . ?
N7 H7C 0.9000 . ?
N9 H9C 0.8900 . ?
N9 H9D 0.8900 . ?

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
O6 Tb1 O8 73.1(3) . . ?
O6 Tb1 O16 84.4(3) . . ?
O8 Tb1 O16 79.4(3) . . ?
O6 Tb1 O2 133.8(3) . . ?
O8 Tb1 O2 140.6(3) . . ?
O16 Tb1 O2 76.5(3) . . ?
O6 Tb1 O4 70.7(3) . . ?
O8 Tb1 O4 143.8(3) . . ?
O16 Tb1 O4 98.1(3) . . ?
O2 Tb1 O4 70.9(3) . . ?
O6 Tb1 O10 146.5(3) . . ?
O8 Tb1 O10 74.1(3) . . ?
O16 Tb1 O10 82.7(3) . . ?
O2 Tb1 O10 72.3(3) . . ?
O4 Tb1 O10 141.9(3) . . ?
O6 Tb1 O12 80.3(4) . . ?
O8 Tb1 O12 76.1(4) . . ?
O16 Tb1 O12 154.1(3) . . ?
O2 Tb1 O12 128.8(3) . . ?
O4 Tb1 O12 96.5(4) . . ?
O10 Tb1 O12 98.6(4) . . ?
O6 Tb1 O11 115.8(3) . . ?
O8 Tb1 O11 121.2(3) . . ?
O16 Tb1 O11 153.6(3) . . ?
O2 Tb1 O11 77.2(3) . . ?
O4 Tb1 O11 75.0(3) . . ?
O10 Tb1 O11 87.5(3) . . ?
O12 Tb1 O11 51.8(3) . . ?
O2 Cu1 N10 90.4(4) . . ?
O2 Cu1 O1 84.6(4) . . ?
N10 Cu1 O1 167.8(5) . . ?
O2 Cu1 N9 170.9(5) . . ?
N10 Cu1 N9 82.6(5) . . ?
O1 Cu1 N9 101.0(4) . . ?
O2 Cu1 O17 90.4(4) . . ?
N10 Cu1 O17 93.2(4) . . ?
O1 Cu1 O17 97.9(4) . . ?
N9 Cu1 O17 95.9(4) . . ?
N2 Cu2 O4 89.1(4) . . ?
N2 Cu2 O3 168.9(5) . . ?
O4 Cu2 O3 84.3(4) . . ?
N2 Cu2 N1 82.1(4) . . ?
O4 Cu2 N1 169.2(5) . . ?
O3 Cu2 N1 103.4(4) . . ?
N2 Cu2 O15 96.8(4) . . ?
O4 Cu2 O15 94.3(4) . . ?
O3 Cu2 O15 92.5(4) . . ?
N1 Cu2 O15 92.9(4) . . ?
N4 Cu3 O6 88.9(4) . . ?
N4 Cu3 O5 168.4(5) . . ?
O6 Cu3 O5 85.2(4) . . ?
N4 Cu3 N3 82.5(5) . . ?
O6 Cu3 N3 166.5(5) . . ?
O5 Cu3 N3 101.3(4) . . ?
N4 Cu3 O14 91.4(5) . . ?
O6 Cu3 O14 98.1(4) . . ?
O5 Cu3 O14 99.2(4) . . ?
N3 Cu3 O14 92.6(5) . . ?
N6 Cu4 O7 173.3(5) . . ?
N6 Cu4 O8 91.8(4) . . ?
O7 Cu4 O8 84.3(4) . . ?
N6 Cu4 N5 82.4(5) . . ?
O7 Cu4 N5 101.0(4) . . ?
O8 Cu4 N5 171.9(5) . . ?
N8 Cu5 O9 158.5(5) . . ?
N8 Cu5 O10 92.2(4) . . ?
O9 Cu5 O10 85.2(4) . . ?
N8 Cu5 N7 83.1(5) . . ?
O9 Cu5 N7 96.0(5) . . ?
O10 Cu5 N7 169.8(5) . . ?
N8 Cu5 O13 104.9(5) . . ?
O9 Cu5 O13 96.6(4) . . ?
O10 Cu5 O13 96.7(4) . . ?
N7 Cu5 O13 93.2(5) . . ?
C2 O1 Cu1 106.2(8) . . ?
N2 O2 Cu1 109.5(7) . . ?
N2 O2 Tb1 124.4(7) . . ?
Cu1 O2 Tb1 126.0(4) . . ?
C4 O3 Cu2 108.5(8) . . ?
N4 O4 Cu2 109.6(7) . . ?
N4 O4 Tb1 122.3(7) . . ?
Cu2 O4 Tb1 127.0(4) . . ?
C6 O5 Cu3 107.0(8) . . ?
N6 O6 Cu3 106.6(7) . . ?
N6 O6 Tb1 125.2(7) . . ?
Cu3 O6 Tb1 126.5(4) . . ?
C8 O7 Cu4 108.3(8) . . ?
N8 O8 Cu4 108.3(7) . . ?
N8 O8 Tb1 124.9(7) . . ?
Cu4 O8 Tb1 124.3(4) . . ?
C10 O9 Cu5 106.1(8) . . ?
N10 O10 Cu5 105.4(7) . . ?
N10 O10 Tb1 122.3(7) . . ?
Cu5 O10 Tb1 123.7(4) . . ?
C12 O11 Tb1 93.4(9) . . ?
C12 O12 Tb1 95.9(10) . . ?
Cu5 O13 H13B 106.5 . . ?
Cu5 O13 H13C 106.4 . . ?
H13B O13 H13C 106.6 . . ?
Cu3 O14 H14B 106.9 . . ?
Cu3 O14 H14C 106.5 . . ?
H14B O14 H14C 106.7 . . ?
Cu2 O15 H15B 108.1 . . ?
Cu2 O15 H15C 108.6 . . ?
H15B O15 H15C 107.5 . . ?
Tb1 O16 H16B 107.2 . . ?
Tb1 O16 H16C 107.4 . . ?
H16B O16 H16C 107.0 . . ?
Cu1 O17 H17B 110.7 . . ?
Cu1 O17 H17C 110.4 . . ?
H17B O17 H17C 108.8 . . ?
H18C O18 H18D 108.6 . . ?
H19C O19 H19D 108.8 . . ?
H20C O20 H20D 108.7 . . ?
H21C O21 H21D 108.7 . . ?
N1 C1 C2 109.6(11) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
O1 C2 N2 126.4(11) . . ?
O1 C2 C1 120.3(11) . . ?
N2 C2 C1 113.1(11) . . ?
C4 C3 N3 109.0(11) . . ?
C4 C3 H3A 109.9 . . ?
N3 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
N3 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N4 C4 O3 122.8(12) . . ?
N4 C4 C3 116.0(12) . . ?
O3 C4 C3 121.2(11) . . ?
C6 C5 N5 109.2(11) . . ?
C6 C5 H5A 109.8 . . ?
N5 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
N5 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
O5 C6 N6 124.6(12) . . ?
O5 C6 C5 119.9(12) . . ?
N6 C6 C5 115.6(12) . . ?
N7 C7 C8 112.3(13) . . ?
N7 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N7 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
O7 C8 N8 124.2(13) . . ?
O7 C8 C7 121.5(13) . . ?
N8 C8 C7 114.3(13) . . ?
N9 C9 C10 112.3(11) . . ?
N9 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
N9 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
N10 C10 O9 125.2(13) . . ?
N10 C10 C9 115.4(12) . . ?
O9 C10 C9 119.4(11) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O12 C12 O11 117.1(15) . . ?
O12 C12 C11 120.6(13) . . ?
O11 C12 C11 122.2(13) . . ?
C1 N1 Cu2 111.2(8) . . ?
C1 N1 H1C 109.4 . . ?
Cu2 N1 H1C 109.4 . . ?
C1 N1 H1D 109.4 . . ?
Cu2 N1 H1D 109.4 . . ?
H1C N1 H1D 108.0 . . ?
C2 N2 O2 112.6(10) . . ?
C2 N2 Cu2 122.1(9) . . ?
O2 N2 Cu2 125.3(8) . . ?
C3 N3 Cu3 111.6(8) . . ?
C3 N3 H3C 109.3 . . ?
Cu3 N3 H3C 109.3 . . ?
C3 N3 H3D 109.3 . . ?
Cu3 N3 H3D 109.3 . . ?
H3C N3 H3D 108.0 . . ?
C4 N4 O4 114.8(11) . . ?
C4 N4 Cu3 119.6(9) . . ?
O4 N4 Cu3 125.0(8) . . ?
C5 N5 Cu4 110.0(8) . . ?
C5 N5 H5C 109.7 . . ?
Cu4 N5 H5C 109.7 . . ?
C5 N5 H5D 109.7 . . ?
Cu4 N5 H5D 109.7 . . ?
H5C N5 H5D 108.2 . . ?
C6 N6 O6 116.4(11) . . ?
C6 N6 Cu4 119.3(9) . . ?
O6 N6 Cu4 123.2(8) . . ?
C7 N7 Cu5 109.3(9) . . ?
C7 N7 H7D 104.9 . . ?
Cu5 N7 H7D 105.1 . . ?
C7 N7 H7C 115.6 . . ?
Cu5 N7 H7C 115.5 . . ?
H7D N7 H7C 105.3 . . ?
C8 N8 O8 114.4(11) . . ?
C8 N8 Cu5 119.0(10) . . ?
O8 N8 Cu5 125.1(8) . . ?
C9 N9 Cu1 108.3(8) . . ?
C9 N9 H9C 110.0 . . ?
Cu1 N9 H9C 110.0 . . ?
C9 N9 H9D 110.0 . . ?
Cu1 N9 H9D 110.0 . . ?
H9C N9 H9D 108.4 . . ?
C10 N10 O10 116.2(11) . . ?
C10 N10 Cu1 118.2(10) . . ?
O10 N10 Cu1 124.7(8) . . ?
O22 N11 O23 127.8(16) . . ?
O22 N11 O24 120.1(15) . . ?
O23 N11 O24 111.6(15) . . ?
O25 N12 O26 121.4(15) . . ?
O25 N12 O27 118.5(15) . . ?
O26 N12 O27 120.1(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C2 N2 -9.1(17) . . . . ?
Cu1 O1 C2 C1 176.6(10) . . . . ?
N1 C1 C2 O1 -175.1(12) . . . . ?
N1 C1 C2 N2 9.8(17) . . . . ?
Cu2 O3 C4 N4 1.4(18) . . . . ?
Cu2 O3 C4 C3 -178.0(12) . . . . ?
N3 C3 C4 N4 -11.5(19) . . . . ?
N3 C3 C4 O3 167.9(13) . . . . ?
Cu3 O5 C6 N6 -4.7(19) . . . . ?
Cu3 O5 C6 C5 175.5(12) . . . . ?
N5 C5 C6 O5 175.5(14) . . . . ?
N5 C5 C6 N6 -4.4(19) . . . . ?
Cu4 O7 C8 N8 5(2) . . . . ?
Cu4 O7 C8 C7 -173.7(13) . . . . ?
N7 C7 C8 O7 162.0(15) . . . . ?
N7 C7 C8 N8 -16(2) . . . . ?
Cu5 O9 C10 N10 11.7(18) . . . . ?
Cu5 O9 C10 C9 -169.6(11) . . . . ?
N9 C9 C10 N10 5.2(19) . . . . ?
N9 C9 C10 O9 -173.6(12) . . . . ?
Tb1 O12 C12 O11 -13.7(14) . . . . ?
Tb1 O12 C12 C11 167.7(12) . . . . ?
Tb1 O11 C12 O12 13.3(14) . . . . ?
Tb1 O11 C12 C11 -168.1(13) . . . . ?
C2 C1 N1 Cu2 -14.5(14) . . . . ?
O1 C2 N2 O2 6(2) . . . . ?
C1 C2 N2 O2 -179.3(11) . . . . ?
O1 C2 N2 Cu2 -174.5(11) . . . . ?
C1 C2 N2 Cu2 0.2(17) . . . . ?
Cu1 O2 N2 C2 0.8(14) . . . . ?
Tb1 O2 N2 C2 -176.3(9) . . . . ?
Cu1 O2 N2 Cu2 -178.7(7) . . . . ?
Tb1 O2 N2 Cu2 4.2(15) . . . . ?
O4 Cu2 N2 C2 166.8(12) . . . . ?
O3 Cu2 N2 C2 114(2) . . . . ?
N1 Cu2 N2 C2 -7.0(12) . . . . ?
O15 Cu2 N2 C2 -99.0(12) . . . . ?
O4 Cu2 N2 O2 -13.8(11) . . . . ?
O3 Cu2 N2 O2 -67(3) . . . . ?
N1 Cu2 N2 O2 172.4(11) . . . . ?
O15 Cu2 N2 O2 80.5(11) . . . . ?
C4 C3 N3 Cu3 11.6(15) . . . . ?
O3 C4 N4 O4 -2(2) . . . . ?
C3 C4 N4 O4 177.3(12) . . . . ?
O3 C4 N4 Cu3 -173.3(11) . . . . ?
C3 C4 N4 Cu3 6.1(19) . . . . ?
Cu2 O4 N4 C4 1.6(15) . . . . ?
Tb1 O4 N4 C4 170.3(10) . . . . ?
Cu2 O4 N4 Cu3 172.3(7) . . . . ?
Tb1 O4 N4 Cu3 -19.1(14) . . . . ?
O6 Cu3 N4 C4 170.4(12) . . . . ?
O5 Cu3 N4 C4 111(2) . . . . ?
N3 Cu3 N4 C4 0.9(12) . . . . ?
O14 Cu3 N4 C4 -91.6(12) . . . . ?
O6 Cu3 N4 O4 0.1(11) . . . . ?
O5 Cu3 N4 O4 -59(3) . . . . ?
N3 Cu3 N4 O4 -169.4(11) . . . . ?
O14 Cu3 N4 O4 98.2(11) . . . . ?
C6 C5 N5 Cu4 15.6(15) . . . . ?
O5 C6 N6 O6 2(2) . . . . ?
C5 C6 N6 O6 -178.5(12) . . . . ?
O5 C6 N6 Cu4 169.7(12) . . . . ?
C5 C6 N6 Cu4 -10.4(19) . . . . ?
Cu3 O6 N6 C6 2.4(15) . . . . ?
Tb1 O6 N6 C6 168.7(10) . . . . ?
Cu3 O6 N6 Cu4 -165.2(7) . . . . ?
Tb1 O6 N6 Cu4 1.1(15) . . . . ?
C8 C7 N7 Cu5 12.3(18) . . . . ?
O7 C8 N8 O8 1(2) . . . . ?
C7 C8 N8 O8 179.4(13) . . . . ?
O7 C8 N8 Cu5 -165.7(13) . . . . ?
C7 C8 N8 Cu5 13(2) . . . . ?
Cu4 O8 N8 C8 -6.0(15) . . . . ?
Tb1 O8 N8 C8 -168.4(11) . . . . ?
Cu4 O8 N8 Cu5 159.7(7) . . . . ?
Tb1 O8 N8 Cu5 -2.7(16) . . . . ?
C10 C9 N9 Cu1 -15.3(15) . . . . ?
O9 C10 N10 O10 -3(2) . . . . ?
C9 C10 N10 O10 178.4(12) . . . . ?
O9 C10 N10 Cu1 -172.4(11) . . . . ?
C9 C10 N10 Cu1 8.9(17) . . . . ?
Cu5 O10 N10 C10 -7.7(14) . . . . ?
Tb1 O10 N10 C10 -156.5(10) . . . . ?
Cu5 O10 N10 Cu1 161.1(7) . . . . ?
Tb1 O10 N10 Cu1 12.2(14) . . . . ?

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
O13 H13B O1 0.85 1.98 2.747(13) 150.2 2_565
O13 H13C O20 0.85 2.18 2.768(17) 126.1 .
O14 H14B O12 0.85 2.42 3.218(15) 157.6 .
O15 H15C O11 0.85 1.99 2.780(13) 153.6 .
O16 H16B O18 0.85 2.10 2.734(13) 131.2 .
O16 H16C O17 0.85 1.85 2.690(13) 170.2 .
O17 H17B O25 0.85 2.19 3.031(14) 172.7 2_566
O17 H17B O27 0.85 2.16 2.757(15) 126.8 2_566
O17 H17B N12 0.85 2.45 3.231(16) 153.4 2_566
O17 H17C O3 0.85 2.20 2.666(13) 114.0 2_575
O18 H18C O24 0.85 1.97 2.810(15) 172.1 2_566
O19 H19C O9 0.85 2.00 2.813(14) 159.6 1_655
O20 H20C O23 0.85 2.26 3.10(2) 167.6 .
O20 H20D O5 0.85 1.96 2.799(16) 167.6 2_676
O21 H21C O25 0.85 2.01 2.846(16) 169.5 .
O21 H21D O23 0.85 2.18 3.019(17) 169.0 .
O21 H21D O24 0.85 2.44 3.120(17) 137.6 .
C1 H1B N4 0.97 2.57 3.44(2) 149.1 2_575
C5 H5B N8 0.97 2.58 3.49(2) 157.0 2_676
C9 H9A O11 0.97 2.35 3.039(16) 127.9 2_565
N1 H1C O16 0.89 2.23 3.121(15) 173.6 2_575
N1 H1D O19 0.89 2.37 3.073(16) 136.0 2_665
N3 H3C O13 0.89 2.57 3.448(17) 167.6 1_565
N3 H3D O21 0.89 2.18 3.039(17) 162.0 2_676
N5 H5C O24 0.89 2.33 3.038(19) 136.7 1_565
N5 H5D O12 0.89 1.93 2.816(17) 171.5 2_676
N7 H7D O21 0.90 2.12 2.99(2) 163.4 2_566
N7 H7C O23 0.90 2.05 2.900(18) 156.0 .
N9 H9C O27 0.89 2.13 3.000(18) 165.3 1_454
N9 H9D O10 0.89 2.32 3.179(15) 163.2 2_565
N9 H9D N10 0.89 2.58 3.234(17) 130.6 2_565

_refine_diff_density_max         2.616
_refine_diff_density_min         -3.678
_refine_diff_density_rms         0.324


_exptl_crystal_preparation       'Magnetic properties,DNA interaction'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_6327
_database_code_depnum_ccdc_archive 'CCDC 1423973'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
{La(OAc)(H2O)2[15-MCCu(N)glyha-5](H2O)4}?2NO3?5H2O
_chemical_name_common            metallacrown
_chemical_melting_point          ?
_chemical_formula_moiety         
{La(OAc)(H2O)2[15-MCCu(N)glyha-5](H2O)4}?2NO3?5H2O
_chemical_formula_sum            'C12 H45 Cu5 La N12 O29'
_chemical_formula_weight         1278.21

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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4509(5)
_cell_length_b                   12.5437(6)
_cell_length_c                   16.3152(8)
_cell_angle_alpha                71.343(4)
_cell_angle_beta                 76.532(4)
_cell_angle_gamma                76.328(4)
_cell_volume                     1940.05(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2800
_cell_measurement_theta_min      2.6197
_cell_measurement_theta_max      28.7514

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_F_000             1270
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    3.881
_shelx_estimated_absorpt_T_min   0.293
_shelx_estimated_absorpt_T_max   0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75616
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12812
_diffrn_reflns_av_unetI/netI     0.1279
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.620
_diffrn_reflns_theta_max         25.014
_diffrn_reflns_theta_full        25.014
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6850
_reflns_number_gt                4717
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0752P)²+17.6157P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6850
_refine_ls_number_parameters     533
_refine_ls_number_restraints     1508
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.1979
_refine_ls_wR_factor_gt          0.1575
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      0.988
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.55408(6) 0.66021(5) 0.70315(4) 0.0109(2) Uani 1 1 d . U . . .
Cu1 Cu 0.40756(14) 0.88376(11) 0.49572(9) 0.0159(4) Uani 1 1 d . U . . .
Cu2 Cu 0.68507(15) 0.53770(12) 0.49726(9) 0.0167(4) Uani 1 1 d . U . . .
Cu4 Cu 0.35053(15) 0.53916(12) 0.94054(9) 0.0165(4) Uani 1 1 d . U . . .
Cu3 Cu 0.67989(16) 0.32906(12) 0.78665(10) 0.0215(4) Uani 1 1 d . U . . .
Cu5 Cu 0.29655(17) 0.91321(12) 0.77430(10) 0.0249(4) Uani 1 1 d . U . . .
O1 O 0.4648(8) 0.8383(7) 0.3879(5) 0.0202(18) Uani 1 1 d . U . . .
O2 O 0.5281(8) 0.7471(6) 0.5436(5) 0.0182(17) Uani 1 1 d . U . . .
O3 O 0.7688(8) 0.3761(7) 0.5253(5) 0.0181(17) Uani 1 1 d . U . . .
O4 O 0.6507(8) 0.5125(6) 0.6224(5) 0.0161(16) Uani 1 1 d . U . . .
O5 O 0.5905(8) 0.2516(7) 0.9030(6) 0.0222(19) Uani 1 1 d . U . . .
O6 O 0.5558(8) 0.4619(6) 0.8069(5) 0.0186(17) Uani 1 1 d . U . . .
O7 O 0.2428(8) 0.6560(6) 0.9927(6) 0.0223(19) Uani 1 1 d . U . . .
O8 O 0.4100(8) 0.6683(6) 0.8460(5) 0.0186(17) Uani 1 1 d . U . . .
O9 O 0.2349(9) 1.0429(7) 0.6808(5) 0.027(2) Uani 1 1 d . U . . .
O10 O 0.4124(9) 0.8561(6) 0.6799(5) 0.0230(18) Uani 1 1 d . U . . .
O11 O 0.2258(9) 0.7802(7) 0.5568(6) 0.026(2) Uani 1 1 d . U . . .
H11B H 0.1610 0.8220 0.5804 0.032 Uiso 1 1 d R U . . .
H11C H 0.2005 0.7685 0.5150 0.032 Uiso 1 1 d R U . . .
O12 O 0.3295(8) 0.6224(6) 0.6955(5) 0.0196(19) Uani 1 1 d . U . . .
H12E H 0.2728 0.6436 0.7365 0.024 Uiso 1 1 d R U . . .
H12F H 0.3071 0.6662 0.6473 0.024 Uiso 1 1 d R U . . .
O13 O 0.1802(9) 0.5457(8) 0.8592(6) 0.031(2) Uani 1 1 d . U . . .
H13B H 0.2062 0.4863 0.8412 0.037 Uiso 1 1 d R U . . .
H13C H 0.1121 0.5326 0.8987 0.037 Uiso 1 1 d R U . . .
O14 O 0.8585(9) 0.3595(7) 0.8380(6) 0.030(2) Uani 1 1 d . U . . .
H14B H 0.9274 0.3086 0.8324 0.036 Uiso 1 1 d R U . . .
H14C H 0.8785 0.4251 0.8106 0.036 Uiso 1 1 d R U . . .
O15 O 0.6339(9) 0.7987(8) 0.7577(6) 0.031(2) Uani 1 1 d D U . . .
H15B H 0.5790 0.8545 0.7716 0.037 Uiso 1 1 d DR U . . .
H15C H 0.7125 0.8065 0.7692 0.037 Uiso 1 1 d DR U . . .
O16 O 0.0990(8) 0.4046(7) 0.5215(5) 0.022(2) Uani 1 1 d . U . . .
H16C H 0.0993 0.3549 0.5711 0.026 Uiso 1 1 d R U . . .
H16D H 0.1312 0.3710 0.4815 0.026 Uiso 1 1 d R U . . .
O17 O 0.0903(9) 0.2568(8) 0.6883(6) 0.034(2) Uani 1 1 d . U . . .
H17C H 0.1351 0.1913 0.6862 0.040 Uiso 1 1 d R U . . .
H17D H 0.1146 0.2764 0.7268 0.040 Uiso 1 1 d R U . . .
O18 O 0.5603(15) 0.0370(11) 0.9161(8) 0.074(4) Uani 1 1 d . U . . .
H18C H 0.5563 0.1065 0.9135 0.089 Uiso 1 1 d R U . . .
H18D H 0.6421 0.0071 0.9059 0.089 Uiso 1 1 d R U . . .
O19 O 0.9452(12) 0.6797(12) 0.9012(11) 0.082(4) Uani 1 1 d . U . . .
H19C H 0.9227 0.6998 0.9484 0.099 Uiso 1 1 d R U . . .
H19D H 0.9734 0.7346 0.8597 0.099 Uiso 1 1 d R U . . .
O20 O 0.4798(9) 1.0024(7) 0.7782(6) 0.028(2) Uani 1 1 d . U . . .
H20C H 0.4988 1.0525 0.7300 0.034 Uiso 1 1 d R U . . .
H20D H 0.5065 1.0169 0.8182 0.034 Uiso 1 1 d R U . . .
O21 O 0.8675(14) 0.9661(12) 0.8769(11) 0.091(4) Uani 1 1 d . U . . .
H21C H 0.8523 0.9405 0.8384 0.109 Uiso 1 1 d R U . . .
H21D H 0.8398 0.9244 0.9276 0.109 Uiso 1 1 d R U . . .
O22 O 0.7981(8) 0.6887(7) 0.6203(5) 0.0201(18) Uani 1 1 d . U . . .
O23 O 0.7790(8) 0.5832(7) 0.7580(5) 0.0187(18) Uani 1 1 d . U . . .
O24 O 0.8443(11) 0.9227(10) 0.7225(8) 0.055(3) Uani 1 1 d . U . . .
O25 O 0.9823(11) 0.9187(9) 0.6032(7) 0.045(3) Uani 1 1 d . U . . .
O26 O 1.0532(13) 0.8363(11) 0.7269(8) 0.063(3) Uani 1 1 d . U . . .
O28 O 0.169(2) 0.3231(17) 0.8186(12) 0.146(7) Uani 1 1 d D U . . .
O29 O 0.131(2) 0.3105(16) 0.9544(12) 0.151(7) Uani 1 1 d D U . . .
O30 O 0.220(3) 0.1524(16) 0.9186(15) 0.209(9) Uani 1 1 d D U . . .
C1 C 0.5942(12) 0.6785(10) 0.3362(8) 0.019(2) Uani 1 1 d . U . . .
H1A H 0.6364 0.7290 0.2836 0.023 Uiso 1 1 calc R U . . .
H1B H 0.5203 0.6575 0.3218 0.023 Uiso 1 1 calc R U . . .
C2 C 0.5436(12) 0.7382(10) 0.4056(8) 0.019(2) Uani 1 1 d . U . . .
C3 C 0.8167(13) 0.2167(10) 0.6540(8) 0.020(3) Uani 1 1 d . U . . .
H3A H 0.7630 0.1673 0.6478 0.024 Uiso 1 1 calc R U . . .
H3B H 0.9082 0.1949 0.6270 0.024 Uiso 1 1 calc R U . . .
C4 C 0.7646(12) 0.3397(9) 0.6086(8) 0.017(2) Uani 1 1 d . U . . .
C5 C 0.4129(12) 0.2944(10) 1.0201(8) 0.017(2) Uani 1 1 d . U . . .
H5A H 0.4678 0.2550 1.0650 0.021 Uiso 1 1 calc R U . . .
H5B H 0.3579 0.2425 1.0191 0.021 Uiso 1 1 calc R U . . .
C6 C 0.4998(12) 0.3269(10) 0.9335(8) 0.018(2) Uani 1 1 d . U . . .
C7 C 0.1642(15) 0.8618(11) 0.9557(9) 0.030(3) Uani 1 1 d . U . . .
H7A H 0.0736 0.8487 0.9808 0.036 Uiso 1 1 calc R U . . .
H7B H 0.1989 0.8822 0.9978 0.036 Uiso 1 1 calc R U . . .
C8 C 0.2507(13) 0.7545(10) 0.9360(8) 0.023(3) Uani 1 1 d . U . . .
C9 C 0.2330(14) 1.0878(10) 0.5271(8) 0.023(3) Uani 1 1 d . U . . .
H9A H 0.2526 1.1642 0.5129 0.028 Uiso 1 1 calc R U . . .
H9B H 0.1369 1.0938 0.5358 0.028 Uiso 1 1 calc R U . . .
C10 C 0.2816(13) 1.0173(10) 0.6081(8) 0.020(2) Uani 1 1 d . U . . .
C11 C 0.8513(12) 0.6233(10) 0.6840(8) 0.016(2) Uani 1 1 d . U . . .
C12 C 0.9983(13) 0.5864(12) 0.6752(9) 0.035(4) Uani 1 1 d . U . . .
H12A H 1.0406 0.6317 0.6207 0.052 Uiso 1 1 calc R U . . .
H12B H 1.0208 0.5073 0.6762 0.052 Uiso 1 1 calc R U . . .
H12C H 1.0285 0.5963 0.7231 0.052 Uiso 1 1 calc R U . . .
N1 N 0.6938(10) 0.5728(8) 0.3677(6) 0.020(2) Uani 1 1 d . U . . .
H1C H 0.7758 0.5837 0.3400 0.023 Uiso 1 1 calc R U . . .
H1D H 0.6761 0.5141 0.3556 0.023 Uiso 1 1 calc R U . . .
N2 N 0.5795(10) 0.6888(8) 0.4803(6) 0.016(2) Uani 1 1 d . U . . .
N3 N 0.8111(12) 0.2031(9) 0.7471(7) 0.033(3) Uani 1 1 d . U . . .
H3C H 0.8918 0.2031 0.7563 0.040 Uiso 1 1 calc R U . . .
H3D H 0.7876 0.1362 0.7787 0.040 Uiso 1 1 calc R U . . .
N4 N 0.7107(10) 0.4022(8) 0.6619(7) 0.018(2) Uani 1 1 d . U . . .
N5 N 0.3254(11) 0.3978(8) 1.0418(7) 0.023(2) Uani 1 1 d . U . . .
H5C H 0.3452 0.4058 1.0894 0.027 Uiso 1 1 calc R U . . .
H5D H 0.2403 0.3891 1.0535 0.027 Uiso 1 1 calc R U . . .
N6 N 0.4760(10) 0.4325(8) 0.8891(7) 0.018(2) Uani 1 1 d . U . . .
N7 N 0.1644(11) 0.9563(8) 0.8725(7) 0.027(2) Uani 1 1 d . U . . .
H7C H 0.1831 1.0173 0.8808 0.032 Uiso 1 1 calc R U . . .
H7D H 0.0832 0.9752 0.8582 0.032 Uiso 1 1 calc R U . . .
N8 N 0.3305(10) 0.7692(8) 0.8606(6) 0.018(2) Uani 1 1 d . U . . .
N9 N 0.2970(11) 1.0379(8) 0.4523(7) 0.021(2) Uani 1 1 d . U . . .
H9C H 0.3486 1.0843 0.4127 0.026 Uiso 1 1 calc R U . . .
H9D H 0.2341 1.0314 0.4266 0.026 Uiso 1 1 calc R U . . .
N10 N 0.3729(10) 0.9273(8) 0.5998(6) 0.016(2) Uani 1 1 d . U . . .
N11 N 0.9629(13) 0.8964(12) 0.6821(11) 0.049(3) Uani 1 1 d . U . . .
N12 N 0.160(3) 0.2612(17) 0.8946(12) 0.122(7) Uani 1 1 d D U . . .


_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
La1 O8 2.480(8) . ?
La1 O4 2.500(7) . ?
La1 O10 2.514(8) . ?
La1 O6 2.521(7) . ?
La1 O2 2.533(8) . ?
La1 O12 2.539(8) . ?
La1 O15 2.554(9) . ?
La1 O23 2.572(8) . ?
La1 O22 2.641(8) . ?
Cu1 N10 1.878(10) . ?
Cu1 O2 1.927(8) . ?
Cu1 O1 1.941(8) . ?
Cu1 N9 2.006(9) . ?
Cu1 O11 2.397(9) . ?
Cu2 O4 1.922(8) . ?
Cu2 N2 1.925(9) . ?
Cu2 O3 1.959(8) . ?
Cu2 N1 2.000(10) . ?
Cu4 N6 1.895(10) . ?
Cu4 O7 1.926(8) . ?
Cu4 O8 1.955(8) . ?
Cu4 N5 2.021(10) . ?
Cu4 O13 2.428(10) . ?
Cu3 O6 1.923(8) . ?
Cu3 N4 1.930(10) . ?
Cu3 O5 1.960(8) . ?
Cu3 N3 2.002(10) . ?
Cu3 O14 2.367(10) . ?
Cu5 N8 1.917(9) . ?
Cu5 O9 1.940(8) . ?
Cu5 O10 1.943(8) . ?
Cu5 N7 1.984(10) . ?
Cu5 O20 2.458(9) . ?
O1 C2 1.314(13) . ?
O2 N2 1.389(12) . ?
O3 C4 1.282(14) . ?
O4 N4 1.389(12) . ?
O5 C6 1.302(14) . ?
O6 N6 1.391(12) . ?
O7 C8 1.292(14) . ?
O8 N8 1.397(11) . ?
O9 C10 1.284(15) . ?
O10 N10 1.417(12) . ?
O11 H11B 0.8499 . ?
O11 H11C 0.8500 . ?
O12 H12E 0.8503 . ?
O12 H12F 0.8497 . ?
O13 H13B 0.8500 . ?
O13 H13C 0.8501 . ?
O14 H14B 0.8500 . ?
O14 H14C 0.8499 . ?
O15 H15B 0.8500 . ?
O15 H15C 0.9177 . ?
O16 H16C 0.8499 . ?
O16 H16D 0.8500 . ?
O17 H17C 0.8501 . ?
O17 H17D 0.8499 . ?
O18 H18C 0.8500 . ?
O18 H18D 0.8500 . ?
O19 H19C 0.8499 . ?
O19 H19D 0.8500 . ?
O20 H20C 0.8500 . ?
O20 H20D 0.8500 . ?
O21 H21C 0.8500 . ?
O21 H21D 0.8500 . ?
O22 C11 1.253(14) . ?
O23 C11 1.284(14) . ?
O24 N11 1.283(16) . ?
O25 N11 1.205(17) . ?
O26 N11 1.276(17) . ?
O28 N12 1.230(16) . ?
O29 N12 1.259(17) . ?
O30 N12 1.330(17) . ?
C1 C2 1.483(17) . ?
C1 N1 1.505(14) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.277(15) . ?
C3 N3 1.462(16) . ?
C3 C4 1.511(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.300(15) . ?
C5 C6 1.482(16) . ?
C5 N5 1.492(14) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N6 1.287(15) . ?
C7 N7 1.489(15) . ?
C7 C8 1.516(16) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N8 1.301(15) . ?
C9 C10 1.462(17) . ?
C9 N9 1.495(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N10 1.316(15) . ?
C11 C12 1.482(17) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N5 H5C 0.8900 . ?
N5 H5D 0.8900 . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
N9 H9C 0.8900 . ?
N9 H9D 0.8900 . ?

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
O8 La1 O4 136.7(2) . . ?
O8 La1 O10 72.9(3) . . ?
O4 La1 O10 139.2(3) . . ?
O8 La1 O6 69.7(2) . . ?
O4 La1 O6 69.2(2) . . ?
O10 La1 O6 140.0(3) . . ?
O8 La1 O2 135.1(3) . . ?
O4 La1 O2 70.9(2) . . ?
O10 La1 O2 69.1(3) . . ?
O6 La1 O2 133.8(3) . . ?
O8 La1 O12 74.2(3) . . ?
O4 La1 O12 85.0(3) . . ?
O10 La1 O12 77.6(3) . . ?
O6 La1 O12 79.0(3) . . ?
O2 La1 O12 75.1(3) . . ?
O8 La1 O15 72.9(3) . . ?
O4 La1 O15 138.8(3) . . ?
O10 La1 O15 65.3(3) . . ?
O6 La1 O15 115.0(3) . . ?
O2 La1 O15 110.3(3) . . ?
O12 La1 O15 136.0(3) . . ?
O8 La1 O23 97.9(3) . . ?
O4 La1 O23 80.2(3) . . ?
O10 La1 O23 130.4(3) . . ?
O6 La1 O23 69.5(3) . . ?
O2 La1 O23 124.8(3) . . ?
O12 La1 O23 148.2(2) . . ?
O15 La1 O23 65.4(3) . . ?
O8 La1 O22 138.9(3) . . ?
O4 La1 O22 70.4(3) . . ?
O10 La1 O22 106.6(3) . . ?
O6 La1 O22 110.8(2) . . ?
O2 La1 O22 76.0(3) . . ?
O12 La1 O22 146.9(3) . . ?
O15 La1 O22 70.2(3) . . ?
O23 La1 O22 50.0(2) . . ?
N10 Cu1 O2 91.9(4) . . ?
N10 Cu1 O1 173.5(4) . . ?
O2 Cu1 O1 84.5(3) . . ?
N10 Cu1 N9 82.6(4) . . ?
O2 Cu1 N9 171.6(4) . . ?
O1 Cu1 N9 100.4(4) . . ?
N10 Cu1 O11 87.8(4) . . ?
O2 Cu1 O11 89.1(3) . . ?
O1 Cu1 O11 97.5(3) . . ?
N9 Cu1 O11 97.0(4) . . ?
O4 Cu2 N2 91.3(4) . . ?
O4 Cu2 O3 84.3(3) . . ?
N2 Cu2 O3 171.6(4) . . ?
O4 Cu2 N1 172.1(4) . . ?
N2 Cu2 N1 83.1(4) . . ?
O3 Cu2 N1 100.6(4) . . ?
N6 Cu4 O7 172.5(4) . . ?
N6 Cu4 O8 91.8(4) . . ?
O7 Cu4 O8 84.0(3) . . ?
N6 Cu4 N5 82.5(4) . . ?
O7 Cu4 N5 100.5(4) . . ?
O8 Cu4 N5 169.2(4) . . ?
N6 Cu4 O13 93.2(4) . . ?
O7 Cu4 O13 93.0(4) . . ?
O8 Cu4 O13 88.5(3) . . ?
N5 Cu4 O13 101.0(4) . . ?
O6 Cu3 N4 91.0(4) . . ?
O6 Cu3 O5 83.7(3) . . ?
N4 Cu3 O5 160.0(4) . . ?
O6 Cu3 N3 171.7(4) . . ?
N4 Cu3 N3 80.7(4) . . ?
O5 Cu3 N3 104.0(4) . . ?
O6 Cu3 O14 96.5(3) . . ?
N4 Cu3 O14 104.5(4) . . ?
O5 Cu3 O14 95.2(3) . . ?
N3 Cu3 O14 86.0(4) . . ?
N8 Cu5 O9 167.3(5) . . ?
N8 Cu5 O10 92.9(4) . . ?
O9 Cu5 O10 85.0(3) . . ?
N8 Cu5 N7 83.6(4) . . ?
O9 Cu5 N7 97.0(4) . . ?
O10 Cu5 N7 172.6(4) . . ?
N8 Cu5 O20 100.7(4) . . ?
O9 Cu5 O20 91.8(4) . . ?
O10 Cu5 O20 87.8(3) . . ?
N7 Cu5 O20 99.2(4) . . ?
C2 O1 Cu1 107.5(7) . . ?
N2 O2 Cu1 108.9(6) . . ?
N2 O2 La1 123.1(6) . . ?
Cu1 O2 La1 126.8(4) . . ?
C4 O3 Cu2 107.6(7) . . ?
N4 O4 Cu2 109.1(6) . . ?
N4 O4 La1 123.2(6) . . ?
Cu2 O4 La1 126.7(3) . . ?
C6 O5 Cu3 108.6(7) . . ?
N6 O6 Cu3 109.7(6) . . ?
N6 O6 La1 126.2(6) . . ?
Cu3 O6 La1 124.0(4) . . ?
C8 O7 Cu4 108.6(7) . . ?
N8 O8 Cu4 108.4(6) . . ?
N8 O8 La1 122.9(6) . . ?
Cu4 O8 La1 126.6(4) . . ?
C10 O9 Cu5 107.6(7) . . ?
N10 O10 Cu5 107.7(6) . . ?
N10 O10 La1 126.1(6) . . ?
Cu5 O10 La1 123.8(4) . . ?
Cu1 O11 H11B 108.3 . . ?
Cu1 O11 H11C 108.2 . . ?
H11B O11 H11C 107.5 . . ?
La1 O12 H12E 107.3 . . ?
La1 O12 H12F 107.3 . . ?
H12E O12 H12F 106.9 . . ?
Cu4 O13 H13B 104.3 . . ?
Cu4 O13 H13C 103.8 . . ?
H13B O13 H13C 105.5 . . ?
Cu3 O14 H14B 111.1 . . ?
Cu3 O14 H14C 111.1 . . ?
H14B O14 H14C 109.2 . . ?
La1 O15 H15B 120.2 . . ?
La1 O15 H15C 137.2 . . ?
H15B O15 H15C 102.5 . . ?
H16C O16 H16D 108.6 . . ?
H17C O17 H17D 108.4 . . ?
H18C O18 H18D 108.1 . . ?
H19C O19 H19D 108.8 . . ?
Cu5 O20 H20C 111.1 . . ?
Cu5 O20 H20D 134.7 . . ?
H20C O20 H20D 108.5 . . ?
H21C O21 H21D 108.8 . . ?
C11 O22 La1 93.3(7) . . ?
C11 O23 La1 95.7(7) . . ?
C2 C1 N1 109.9(10) . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N1 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 O1 123.2(11) . . ?
N2 C2 C1 117.5(10) . . ?
O1 C2 C1 119.2(11) . . ?
N3 C3 C4 109.8(9) . . ?
N3 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N3 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 N4 123.9(10) . . ?
O3 C4 C3 122.2(10) . . ?
N4 C4 C3 113.9(11) . . ?
C6 C5 N5 110.5(9) . . ?
C6 C5 H5A 109.5 . . ?
N5 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
N5 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N6 C6 O5 122.3(11) . . ?
N6 C6 C5 115.9(10) . . ?
O5 C6 C5 121.7(10) . . ?
N7 C7 C8 108.8(10) . . ?
N7 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
N7 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O7 C8 N8 123.9(11) . . ?
O7 C8 C7 120.1(11) . . ?
N8 C8 C7 116.0(10) . . ?
C10 C9 N9 111.2(10) . . ?
C10 C9 H9A 109.4 . . ?
N9 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
N9 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
O9 C10 N10 124.1(11) . . ?
O9 C10 C9 121.0(11) . . ?
N10 C10 C9 114.8(11) . . ?
O22 C11 O23 120.5(11) . . ?
O22 C11 C12 121.3(11) . . ?
O23 C11 C12 118.2(11) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 N1 Cu2 110.0(7) . . ?
C1 N1 H1C 109.7 . . ?
Cu2 N1 H1C 109.7 . . ?
C1 N1 H1D 109.7 . . ?
Cu2 N1 H1D 109.7 . . ?
H1C N1 H1D 108.2 . . ?
C2 N2 O2 115.5(9) . . ?
C2 N2 Cu2 117.7(8) . . ?
O2 N2 Cu2 126.6(7) . . ?
C3 N3 Cu3 111.3(7) . . ?
C3 N3 H3C 109.4 . . ?
Cu3 N3 H3C 109.4 . . ?
C3 N3 H3D 109.4 . . ?
Cu3 N3 H3D 109.4 . . ?
H3C N3 H3D 108.0 . . ?
C4 N4 O4 114.8(10) . . ?
C4 N4 Cu3 119.0(8) . . ?
O4 N4 Cu3 124.2(7) . . ?
C5 N5 Cu4 110.6(7) . . ?
C5 N5 H5C 109.5 . . ?
Cu4 N5 H5C 109.5 . . ?
C5 N5 H5D 109.5 . . ?
Cu4 N5 H5D 109.5 . . ?
H5C N5 H5D 108.1 . . ?
C6 N6 O6 115.7(9) . . ?
C6 N6 Cu4 120.0(8) . . ?
O6 N6 Cu4 124.1(7) . . ?
C7 N7 Cu5 112.2(8) . . ?
C7 N7 H7C 109.2 . . ?
Cu5 N7 H7C 109.2 . . ?
C7 N7 H7D 109.2 . . ?
Cu5 N7 H7D 109.2 . . ?
H7C N7 H7D 107.9 . . ?
C8 N8 O8 114.0(9) . . ?
C8 N8 Cu5 117.3(8) . . ?
O8 N8 Cu5 126.8(7) . . ?
C9 N9 Cu1 110.2(7) . . ?
C9 N9 H9C 109.6 . . ?
Cu1 N9 H9C 109.6 . . ?
C9 N9 H9D 109.6 . . ?
Cu1 N9 H9D 109.6 . . ?
H9C N9 H9D 108.1 . . ?
C10 N10 O10 114.0(10) . . ?
C10 N10 Cu1 119.6(8) . . ?
O10 N10 Cu1 124.6(7) . . ?
O25 N11 O26 121.7(14) . . ?
O25 N11 O24 118.9(15) . . ?
O26 N11 O24 118.9(15) . . ?
O28 N12 O29 116.6(16) . . ?
O28 N12 O30 125.0(16) . . ?
O29 N12 O30 114.7(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C2 N2 -4.6(14) . . . . ?
Cu1 O1 C2 C1 175.4(9) . . . . ?
N1 C1 C2 N2 -6.3(16) . . . . ?
N1 C1 C2 O1 173.7(10) . . . . ?
Cu2 O3 C4 N4 1.3(15) . . . . ?
Cu2 O3 C4 C3 178.0(10) . . . . ?
N3 C3 C4 O3 174.3(12) . . . . ?
N3 C3 C4 N4 -8.6(16) . . . . ?
Cu3 O5 C6 N6 2.1(15) . . . . ?
Cu3 O5 C6 C5 178.9(9) . . . . ?
N5 C5 C6 N6 -7.2(16) . . . . ?
N5 C5 C6 O5 175.8(11) . . . . ?
Cu4 O7 C8 N8 -6.7(17) . . . . ?
Cu4 O7 C8 C7 173.5(11) . . . . ?
N7 C7 C8 O7 -164.5(12) . . . . ?
N7 C7 C8 N8 15.7(18) . . . . ?
Cu5 O9 C10 N10 -10.7(16) . . . . ?
Cu5 O9 C10 C9 168.3(10) . . . . ?
N9 C9 C10 O9 -177.2(11) . . . . ?
N9 C9 C10 N10 1.8(16) . . . . ?
La1 O22 C11 O23 -7.1(11) . . . . ?
La1 O22 C11 C12 170.4(11) . . . . ?
La1 O23 C11 O22 7.3(11) . . . . ?
La1 O23 C11 C12 -170.2(10) . . . . ?
C2 C1 N1 Cu2 13.0(12) . . . . ?
O1 C2 N2 O2 0.9(17) . . . . ?
C1 C2 N2 O2 -179.1(10) . . . . ?
O1 C2 N2 Cu2 175.8(9) . . . . ?
C1 C2 N2 Cu2 -4.2(15) . . . . ?
Cu1 O2 N2 C2 3.3(12) . . . . ?
La1 O2 N2 C2 171.3(8) . . . . ?
Cu1 O2 N2 Cu2 -171.0(5) . . . . ?
La1 O2 N2 Cu2 -3.0(12) . . . . ?
C4 C3 N3 Cu3 21.2(13) . . . . ?
O3 C4 N4 O4 2.9(18) . . . . ?
C3 C4 N4 O4 -174.1(10) . . . . ?
O3 C4 N4 Cu3 167.8(9) . . . . ?
C3 C4 N4 Cu3 -9.2(15) . . . . ?
Cu2 O4 N4 C4 -5.5(12) . . . . ?
La1 O4 N4 C4 -174.8(8) . . . . ?
Cu2 O4 N4 Cu3 -169.4(6) . . . . ?
La1 O4 N4 Cu3 21.2(12) . . . . ?
C6 C5 N5 Cu4 4.3(13) . . . . ?
O5 C6 N6 O6 -1.6(18) . . . . ?
C5 C6 N6 O6 -178.5(10) . . . . ?
O5 C6 N6 Cu4 -176.0(9) . . . . ?
C5 C6 N6 Cu4 7.1(16) . . . . ?
Cu3 O6 N6 C6 0.1(12) . . . . ?
La1 O6 N6 C6 -175.6(8) . . . . ?
Cu3 O6 N6 Cu4 174.3(6) . . . . ?
La1 O6 N6 Cu4 -1.4(13) . . . . ?
O8 Cu4 N6 C6 167.2(10) . . . . ?
N5 Cu4 N6 C6 -3.5(10) . . . . ?
O13 Cu4 N6 C6 -104.2(10) . . . . ?
O8 Cu4 N6 O6 -6.7(9) . . . . ?
N5 Cu4 N6 O6 -177.5(9) . . . . ?
O13 Cu4 N6 O6 81.9(9) . . . . ?
C8 C7 N7 Cu5 -8.9(15) . . . . ?
O7 C8 N8 O8 -0.9(19) . . . . ?
C7 C8 N8 O8 178.9(11) . . . . ?
O7 C8 N8 Cu5 164.6(11) . . . . ?
C7 C8 N8 Cu5 -15.7(16) . . . . ?
Cu4 O8 N8 C8 7.8(13) . . . . ?
La1 O8 N8 C8 172.6(9) . . . . ?
Cu4 O8 N8 Cu5 -156.0(6) . . . . ?
La1 O8 N8 Cu5 8.8(13) . . . . ?
C10 C9 N9 Cu1 6.9(13) . . . . ?
O9 C10 N10 O10 2.8(18) . . . . ?
C9 C10 N10 O10 -176.2(10) . . . . ?
O9 C10 N10 Cu1 167.9(10) . . . . ?
C9 C10 N10 Cu1 -11.1(15) . . . . ?
Cu5 O10 N10 C10 6.7(12) . . . . ?
La1 O10 N10 C10 169.5(8) . . . . ?
Cu5 O10 N10 Cu1 -157.5(6) . . . . ?
La1 O10 N10 Cu1 5.3(12) . . . . ?
O2 Cu1 N10 C10 -174.2(9) . . . . ?
N9 Cu1 N10 C10 12.1(9) . . . . ?
O11 Cu1 N10 C10 -85.2(9) . . . . ?
O2 Cu1 N10 O10 -10.8(9) . . . . ?
N9 Cu1 N10 O10 175.5(9) . . . . ?
O11 Cu1 N10 O10 78.2(8) . . . . ?

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
N9 H9D O25 0.89 2.32 3.131(16) 151.1 2_676
N9 H9D O24 0.89 2.59 3.358(17) 144.5 2_676
N7 H7D O21 0.89 2.23 3.061(19) 155.5 1_455
N7 H7C O30 0.89 2.12 3.00(3) 172.4 1_565
N5 H5D O19 0.89 2.18 3.051(17) 164.5 2_667
N5 H5C O23 0.89 2.56 3.261(13) 136.7 2_667
N3 H3D O21 0.89 2.33 3.066(18) 140.5 1_545
N3 H3C O17 0.89 2.26 3.017(16) 143.0 1_655
N1 H1D O12 0.89 2.15 3.023(13) 167.6 2_666
N1 H1C O28 0.89 2.47 3.05(2) 123.9 2_666
N1 H1C O17 0.89 2.57 3.250(15) 133.7 2_666
C9 H9A O22 0.97 2.43 3.061(14) 122.1 2_676
C9 H9A O2 0.97 2.63 3.380(16) 134.5 2_676
C5 H5A N8 0.97 2.58 3.470(17) 152.5 2_667
C5 H5A O8 0.97 2.65 3.372(16) 131.8 2_667
C3 H3A O1 0.97 2.60 3.435(16) 144.2 2_666
C1 H1B N4 0.97 2.62 3.555(17) 160.8 2_666
C1 H1A O28 0.97 2.42 3.10(2) 127.1 2_666
O21 H21D O30 0.85 2.37 3.20(3) 163.8 2_667
O21 H21C O24 0.85 2.00 2.82(2) 161.6 .
O20 H20D O18 0.85 1.92 2.764(17) 174.5 1_565
O20 H20C O1 0.85 1.99 2.832(12) 174.5 2_676
O19 H19D O26 0.85 2.22 3.03(2) 161.0 .
O19 H19C N12 0.85 2.67 3.51(2) 172.9 2_667
O19 H19C O29 0.85 1.53 2.34(2) 157.8 2_667
O18 H18D O21 0.85 2.26 3.09(2) 167.3 1_545
O18 H18C O5 0.85 1.88 2.719(15) 166.9 .
O17 H17D O28 0.85 2.00 2.85(2) 179.1 .
O17 H17C O9 0.85 1.93 2.775(12) 179.4 1_545
O16 H16D O22 0.85 1.96 2.803(12) 173.3 2_666
O16 H16C O17 0.85 1.91 2.755(12) 173.6 .
O15 H15C O24 0.92 2.09 2.835(14) 138.1 .
O15 H15B O20 0.85 1.92 2.754(12) 165.9 .
O14 H14C O23 0.85 2.03 2.707(11) 136.6 .
O14 H14B O28 0.85 2.52 3.12(2) 127.9 1_655
O13 H13C O19 0.85 2.22 2.707(15) 116.0 1_455
O13 H13B O29 0.85 2.54 2.97(2) 112.4 .
O13 H13B O28 0.85 2.33 3.10(2) 152.2 .
O12 H12F O11 0.85 1.90 2.734(12) 166.9 .
O12 H12E O13 0.85 2.13 2.760(12) 130.5 .
O11 H11C O3 0.85 2.05 2.689(12) 131.1 2_666
O11 H11B N11 0.85 2.53 3.354(16) 164.6 1_455
O11 H11B O26 0.85 2.44 3.126(15) 138.6 1_455
O11 H11B O25 0.85 2.00 2.815(13) 161.0 1_455

_refine_diff_density_max         4.065
_refine_diff_density_min         -2.154
_refine_diff_density_rms         0.257


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method water
_exptl_crystal_preparation       'Magnetic properties,DNA interaction'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_6330
_database_code_depnum_ccdc_archive 'CCDC 1423974'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'{Pr(NO3)(H2O)2[15-MCCu(N)glyha-5] (H2O)}?2NO3?8H2O'
_chemical_name_common            metallacrown
_chemical_melting_point          ?
_chemical_formula_moiety         
'{Pr(NO3)(H2O)2[15-MCCu(N)glyha-5] (H2O)}?2NO3?8H2O'
_chemical_formula_sum            'C10 H42 Cu5 N13 O30 Pr'
_chemical_formula_weight         1283.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -2.4164 10.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7585(9)
_cell_length_b                   11.4924(7)
_cell_length_c                   16.8500(10)
_cell_angle_alpha                72.440(5)
_cell_angle_beta                 87.722(6)
_cell_angle_gamma                73.844(6)
_cell_volume                     1905.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3608
_cell_measurement_theta_min      4.2790
_cell_measurement_theta_max      71.7120

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.236
_exptl_crystal_F_000             1274
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    13.733
_shelx_estimated_absorpt_T_min   0.204
_shelx_estimated_absorpt_T_max   0.290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.20475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11839
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.202
_diffrn_reflns_theta_max         67.245
_diffrn_reflns_theta_full        67.245
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6831
_reflns_number_gt                5453
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1304P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6831
_refine_ls_number_parameters     532
_refine_ls_number_restraints     1374
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0784
_refine_ls_wR_factor_ref         0.2204
_refine_ls_wR_factor_gt          0.1958
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      0.931
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.42376(15) 0.64824(14) 0.49267(9) 0.0166(3) Uani 1 1 d . U . . .
Cu2 Cu 0.36750(16) 0.59404(15) 0.23817(9) 0.0185(4) Uani 1 1 d . U . . .
Cu3 Cu 0.61042(15) 0.81181(15) 0.05320(9) 0.0180(4) Uani 1 1 d . U . . .
Cu4 Cu 0.77796(16) 1.03443(15) 0.18558(9) 0.0188(4) Uani 1 1 d . U . . .
Cu5 Cu 0.70498(15) 0.89214(14) 0.46498(9) 0.0172(4) Uani 1 1 d . U . . .
Pr1 Pr 0.54497(5) 0.82049(5) 0.28304(3) 0.0152(2) Uani 1 1 d . U . . .
O1 O 0.2661(7) 0.5279(7) 0.3300(5) 0.0201(15) Uani 1 1 d . U . . .
O2 O 0.4564(7) 0.6315(7) 0.3223(4) 0.0188(14) Uani 1 1 d . U . . .
O3 O 0.5112(7) 0.7184(7) 0.0150(5) 0.0202(15) Uani 1 1 d . U . . .
O4 O 0.5260(7) 0.7640(7) 0.1561(4) 0.0181(14) Uani 1 1 d . U . . .
O5 O 0.7974(8) 1.0650(7) 0.0658(5) 0.0197(15) Uani 1 1 d . U . . .
O6 O 0.6812(7) 0.9190(7) 0.1761(4) 0.0190(14) Uani 1 1 d . U . . .
O7 O 0.7848(8) 1.0299(7) 0.4256(5) 0.0202(15) Uani 1 1 d . U . . .
O8 O 0.6825(8) 0.9115(7) 0.3477(5) 0.0202(15) Uani 1 1 d . U . . .
O9 O 0.4579(7) 0.7024(7) 0.5864(5) 0.0209(15) Uani 1 1 d . U . . .
O10 O 0.5550(7) 0.7246(7) 0.4400(4) 0.0179(14) Uani 1 1 d . U . . .
O11 O 0.4384(8) 1.0492(7) 0.2227(5) 0.0220(16) Uani 1 1 d . U . . .
H11C H 0.4771 1.1053 0.2000 0.026 Uiso 1 1 d R U . . .
H11D H 0.3583 1.0862 0.2237 0.026 Uiso 1 1 d R U . . .
O12 O 0.7368(7) 0.6364(7) 0.3035(5) 0.0198(15) Uani 1 1 d . U . . .
H12B H 0.8064 0.6572 0.3043 0.024 Uiso 1 1 d R U . . .
H12C H 0.7392 0.6002 0.2660 0.024 Uiso 1 1 d R U . . .
O13 O 0.9129(8) 0.7467(7) 0.4868(5) 0.0243(17) Uani 1 1 d . U . . .
H13B H 0.9150 0.6922 0.5342 0.029 Uiso 1 1 d R U . . .
H13C H 0.9664 0.7873 0.4903 0.029 Uiso 1 1 d R U . . .
O14 O 0.9522(9) 0.6857(8) 0.9721(5) 0.033(2) Uani 1 1 d . . . . .
H14C H 0.9265 0.6703 0.9302 0.040 Uiso 1 1 d R U . . .
H14D H 0.9038 0.6624 1.0112 0.040 Uiso 1 1 d R U . . .
O15 O 0.9007(10) 0.6198(9) 0.6497(6) 0.038(2) Uani 1 1 d . U . . .
H15C H 0.9155 0.6265 0.6971 0.046 Uiso 1 1 d R U . . .
H15D H 0.8491 0.5739 0.6555 0.046 Uiso 1 1 d R U . . .
O16 O 0.9960(8) 0.8630(8) 0.1984(5) 0.0305(18) Uani 1 1 d . U . . .
H16C H 0.9837 0.8016 0.2381 0.037 Uiso 1 1 d R U . . .
H16D H 1.0189 0.8368 0.1565 0.037 Uiso 1 1 d R U . . .
O17 O 0.9496(8) 0.6795(8) 0.3371(6) 0.0316(19) Uani 1 1 d . U . . .
H17C H 1.0059 0.6085 0.3428 0.038 Uiso 1 1 d R U . . .
H17D H 0.9418 0.6932 0.3841 0.038 Uiso 1 1 d R U . . .
O18 O 0.8869(9) 0.1591(8) 0.5031(5) 0.0284(18) Uani 1 1 d . . . . .
H18C H 0.8783 0.1358 0.5554 0.034 Uiso 1 1 d R U . . .
H18D H 0.8532 0.1164 0.4815 0.034 Uiso 1 1 d R U . . .
O19 O 0.0717(8) 0.8013(8) 0.0539(5) 0.0276(18) Uani 1 1 d . U . . .
H19C H 0.0335 0.7647 0.0299 0.033 Uiso 1 1 d R U . . .
H19D H 0.1130 0.8435 0.0178 0.033 Uiso 1 1 d R U . . .
O20 O 0.4309(7) 0.7804(7) 0.8481(5) 0.0192(15) Uani 1 1 d . . . . .
H20C H 0.4593 0.7504 0.8986 0.023 Uiso 1 1 d R U . . .
H20D H 0.4454 0.7198 0.8269 0.023 Uiso 1 1 d R U . . .
O21 O 0.5374(8) 0.3921(7) 0.2430(4) 0.0198(15) Uani 1 1 d . U . . .
H21C H 0.5364 0.3625 0.2956 0.024 Uiso 1 1 d R U . . .
H21D H 0.6038 0.4193 0.2313 0.024 Uiso 1 1 d R U . . .
O22 O 0.2817(8) 0.8779(8) 0.2358(5) 0.0262(16) Uani 1 1 d . U . . .
O23 O 0.3290(7) 0.8942(7) 0.3558(5) 0.0216(15) Uani 1 1 d . U . . .
O24 O 0.1326(8) 0.9075(8) 0.3230(6) 0.0301(19) Uani 1 1 d . U . . .
O25 O 0.2460(8) 0.5233(8) 0.7895(5) 0.0301(19) Uani 1 1 d . U . . .
O26 O 0.1881(9) 0.3892(8) 0.8940(6) 0.037(2) Uani 1 1 d . U . . .
O27 O 0.1986(10) 0.5693(9) 0.9054(6) 0.039(2) Uani 1 1 d . U . . .
O28 O 0.2566(10) 0.3119(9) 0.1724(8) 0.048(3) Uani 1 1 d . U . . .
O29 O 0.0521(9) 0.3598(10) 0.1928(7) 0.046(3) Uani 1 1 d . U . . .
O30 O 0.1699(9) 0.1637(8) 0.2293(7) 0.042(2) Uani 1 1 d . U . . .
C1 C 0.2283(11) 0.5298(10) 0.4748(7) 0.019(2) Uani 1 1 d . U . . .
H1A H 0.1367 0.5731 0.4632 0.023 Uiso 1 1 calc R U . . .
H1B H 0.2378 0.4394 0.4977 0.023 Uiso 1 1 calc R U . . .
C2 C 0.2989(10) 0.5545(10) 0.3947(6) 0.0157(19) Uani 1 1 d . U . . .
C3 C 0.3630(11) 0.5886(11) 0.0708(6) 0.0179(19) Uani 1 1 d . U . . .
H3A H 0.3102 0.6263 0.0192 0.021 Uiso 1 1 calc R U . . .
H3B H 0.4185 0.5063 0.0702 0.021 Uiso 1 1 calc R U . . .
C4 C 0.4461(11) 0.6738(11) 0.0769(7) 0.020(2) Uani 1 1 d . U . . .
C5 C 0.7489(10) 0.9832(10) -0.0440(6) 0.018(2) Uani 1 1 d . U . . .
H5A H 0.8378 0.9669 -0.0607 0.021 Uiso 1 1 calc R U . . .
H5B H 0.6996 1.0645 -0.0809 0.021 Uiso 1 1 calc R U . . .
C6 C 0.7445(11) 0.9882(10) 0.0430(7) 0.019(2) Uani 1 1 d . U . . .
C7 C 0.8649(11) 1.1463(10) 0.2977(7) 0.021(2) Uani 1 1 d . U . . .
H7A H 0.8197 1.2297 0.3020 0.025 Uiso 1 1 calc R U . . .
H7B H 0.9519 1.1230 0.3220 0.025 Uiso 1 1 calc R U . . .
C8 C 0.7959(11) 1.0517(10) 0.3458(7) 0.022(2) Uani 1 1 d . U . . .
C9 C 0.5849(11) 0.8254(11) 0.6235(7) 0.020(2) Uani 1 1 d . U . . .
H9A H 0.5131 0.8934 0.6312 0.025 Uiso 1 1 calc R U . . .
H9B H 0.6123 0.7627 0.6774 0.025 Uiso 1 1 calc R U . . .
C10 C 0.5420(10) 0.7646(10) 0.5648(6) 0.0171(19) Uani 1 1 d . U . . .
N1 N 0.2795(9) 0.5745(9) 0.5366(5) 0.0189(18) Uani 1 1 d . U . . .
H1D H 0.3075 0.5097 0.5826 0.023 Uiso 1 1 calc R U . . .
H1C H 0.2161 0.6330 0.5500 0.023 Uiso 1 1 calc R U . . .
N2 N 0.3939(9) 0.6054(9) 0.3963(5) 0.0196(17) Uani 1 1 d . U . . .
N3 N 0.2795(9) 0.5723(9) 0.1416(6) 0.0220(18) Uani 1 1 d . U . . .
H3C H 0.2672 0.4953 0.1556 0.026 Uiso 1 1 calc R U . . .
H3D H 0.2027 0.6299 0.1282 0.026 Uiso 1 1 calc R U . . .
N4 N 0.4480(9) 0.6904(8) 0.1487(6) 0.0189(17) Uani 1 1 d . U . . .
N5 N 0.6942(9) 0.8816(9) -0.0512(6) 0.0225(19) Uani 1 1 d . U . . .
H5C H 0.7571 0.8194 -0.0613 0.027 Uiso 1 1 calc R U . . .
H5D H 0.6360 0.9128 -0.0939 0.027 Uiso 1 1 calc R U . . .
N6 N 0.6861(9) 0.9142(9) 0.0950(6) 0.0208(17) Uani 1 1 d . U . . .
N7 N 0.8721(9) 1.1525(9) 0.2085(6) 0.0216(18) Uani 1 1 d . U . . .
H7C H 0.9547 1.1297 0.1958 0.026 Uiso 1 1 calc R U . . .
H7D H 0.8361 1.2318 0.1769 0.026 Uiso 1 1 calc R U . . .
N8 N 0.7475(9) 0.9981(8) 0.3023(6) 0.0181(16) Uani 1 1 d . U . . .
N9 N 0.6946(9) 0.8773(9) 0.5874(6) 0.0207(18) Uani 1 1 d . U . . .
H9C H 0.7686 0.8262 0.6143 0.025 Uiso 1 1 calc R U . . .
H9D H 0.6832 0.9535 0.5940 0.025 Uiso 1 1 calc R U . . .
N10 N 0.5959(9) 0.7821(8) 0.4921(5) 0.0168(16) Uani 1 1 d . U . . .
N11 N 0.2460(10) 0.8956(9) 0.3038(6) 0.0229(18) Uani 1 1 d . U . . .
N12 N 0.2101(10) 0.4952(9) 0.8652(6) 0.024(2) Uani 1 1 d . U . . .
N13 N 0.1598(10) 0.2800(10) 0.1988(6) 0.028(2) Uani 1 1 d . U . . .


_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
Cu1 N2 1.897(9) . ?
Cu1 O10 1.916(7) . ?
Cu1 O9 1.944(8) . ?
Cu1 N1 1.984(9) . ?
Cu2 N4 1.916(9) . ?
Cu2 O1 1.944(8) . ?
Cu2 O2 1.953(7) . ?
Cu2 N3 2.027(9) . ?
Cu3 N6 1.903(9) . ?
Cu3 O4 1.926(7) . ?
Cu3 O3 1.953(7) . ?
Cu3 N5 1.994(9) . ?
Cu4 N8 1.918(9) . ?
Cu4 O6 1.944(8) . ?
Cu4 O5 1.954(7) . ?
Cu4 N7 2.032(9) . ?
Cu5 N10 1.903(9) . ?
Cu5 O8 1.938(7) . ?
Cu5 O7 1.940(8) . ?
Cu5 N9 2.019(9) . ?
Cu5 O13 2.355(8) . ?
Pr1 O4 2.446(7) . ?
Pr1 O12 2.458(7) . ?
Pr1 O11 2.462(8) . ?
Pr1 O8 2.479(7) . ?
Pr1 O6 2.482(7) . ?
Pr1 O2 2.510(7) . ?
Pr1 O10 2.534(7) . ?
Pr1 O23 2.632(8) . ?
Pr1 O22 2.813(8) . ?
O1 C2 1.304(13) . ?
O2 N2 1.384(11) . ?
O3 C4 1.288(13) . ?
O4 N4 1.379(11) . ?
O5 C6 1.324(13) . ?
O6 N6 1.383(12) . ?
O7 C8 1.299(14) . ?
O8 N8 1.396(11) . ?
O9 C10 1.280(13) . ?
O10 N10 1.394(11) . ?
O22 N11 1.250(13) . ?
O23 N11 1.270(12) . ?
O24 N11 1.230(13) . ?
O25 N12 1.289(13) . ?
O26 N12 1.253(13) . ?
O27 N12 1.218(13) . ?
O28 N13 1.223(14) . ?
O29 N13 1.246(14) . ?
O30 N13 1.254(13) . ?
C1 N1 1.475(14) . ?
C1 C2 1.512(14) . ?
C2 N2 1.315(14) . ?
C3 N3 1.463(13) . ?
C3 C4 1.524(15) . ?
C4 N4 1.283(15) . ?
C5 C6 1.482(14) . ?
C5 N5 1.483(13) . ?
C6 N6 1.300(15) . ?
C7 N7 1.482(14) . ?
C7 C8 1.504(15) . ?
C8 N8 1.292(14) . ?
C9 N9 1.494(14) . ?
C9 C10 1.521(14) . ?
C10 N10 1.318(14) . ?

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
N2 Cu1 O10 91.5(4) . . ?
N2 Cu1 O9 176.0(4) . . ?
O10 Cu1 O9 85.0(3) . . ?
N2 Cu1 N1 83.9(4) . . ?
O10 Cu1 N1 174.6(3) . . ?
O9 Cu1 N1 99.5(3) . . ?
N4 Cu2 O1 169.0(4) . . ?
N4 Cu2 O2 92.5(3) . . ?
O1 Cu2 O2 84.5(3) . . ?
N4 Cu2 N3 81.5(4) . . ?
O1 Cu2 N3 101.0(3) . . ?
O2 Cu2 N3 173.6(4) . . ?
N6 Cu3 O4 90.9(4) . . ?
N6 Cu3 O3 172.5(4) . . ?
O4 Cu3 O3 84.3(3) . . ?
N6 Cu3 N5 83.5(4) . . ?
O4 Cu3 N5 173.1(4) . . ?
O3 Cu3 N5 100.8(4) . . ?
N8 Cu4 O6 90.4(3) . . ?
N8 Cu4 O5 175.2(3) . . ?
O6 Cu4 O5 85.0(3) . . ?
N8 Cu4 N7 83.4(4) . . ?
O6 Cu4 N7 173.6(4) . . ?
O5 Cu4 N7 101.3(3) . . ?
N10 Cu5 O8 90.3(3) . . ?
N10 Cu5 O7 168.4(4) . . ?
O8 Cu5 O7 84.6(3) . . ?
N10 Cu5 N9 82.9(4) . . ?
O8 Cu5 N9 170.0(4) . . ?
O7 Cu5 N9 100.8(3) . . ?
N10 Cu5 O13 102.0(3) . . ?
O8 Cu5 O13 96.9(3) . . ?
O7 Cu5 O13 89.0(3) . . ?
N9 Cu5 O13 91.7(3) . . ?
O4 Pr1 O12 79.6(2) . . ?
O4 Pr1 O11 96.0(3) . . ?
O12 Pr1 O11 150.6(3) . . ?
O4 Pr1 O8 140.2(2) . . ?
O12 Pr1 O8 85.6(2) . . ?
O11 Pr1 O8 79.3(2) . . ?
O4 Pr1 O6 70.7(2) . . ?
O12 Pr1 O6 81.2(2) . . ?
O11 Pr1 O6 70.1(2) . . ?
O8 Pr1 O6 70.6(2) . . ?
O4 Pr1 O2 72.6(2) . . ?
O12 Pr1 O2 75.3(2) . . ?
O11 Pr1 O2 131.5(2) . . ?
O8 Pr1 O2 138.2(2) . . ?
O6 Pr1 O2 139.3(2) . . ?
O4 Pr1 O10 140.2(2) . . ?
O12 Pr1 O10 79.1(2) . . ?
O11 Pr1 O10 118.4(2) . . ?
O8 Pr1 O10 70.5(2) . . ?
O6 Pr1 O10 137.3(2) . . ?
O2 Pr1 O10 69.6(2) . . ?
O4 Pr1 O23 117.0(2) . . ?
O12 Pr1 O23 139.8(2) . . ?
O11 Pr1 O23 68.0(2) . . ?
O8 Pr1 O23 98.0(2) . . ?
O6 Pr1 O23 137.9(2) . . ?
O2 Pr1 O23 75.8(2) . . ?
O10 Pr1 O23 64.9(2) . . ?
O4 Pr1 O22 70.4(2) . . ?
O12 Pr1 O22 136.3(2) . . ?
O11 Pr1 O22 65.9(2) . . ?
O8 Pr1 O22 137.3(2) . . ?
O6 Pr1 O22 116.1(2) . . ?
O2 Pr1 O22 65.9(2) . . ?
O10 Pr1 O22 104.3(2) . . ?
O23 Pr1 O22 47.0(2) . . ?
C2 O1 Cu2 107.7(6) . . ?
N2 O2 Cu2 108.9(6) . . ?
N2 O2 Pr1 118.6(6) . . ?
Cu2 O2 Pr1 120.3(3) . . ?
C4 O3 Cu3 106.8(6) . . ?
N4 O4 Cu3 109.3(6) . . ?
N4 O4 Pr1 122.8(6) . . ?
Cu3 O4 Pr1 127.9(3) . . ?
C6 O5 Cu4 107.5(6) . . ?
N6 O6 Cu4 108.2(6) . . ?
N6 O6 Pr1 124.7(6) . . ?
Cu4 O6 Pr1 126.6(3) . . ?
C8 O7 Cu5 107.6(7) . . ?
N8 O8 Cu5 108.3(6) . . ?
N8 O8 Pr1 123.8(6) . . ?
Cu5 O8 Pr1 127.6(4) . . ?
C10 O9 Cu1 107.7(7) . . ?
N10 O10 Cu1 109.2(6) . . ?
N10 O10 Pr1 120.9(5) . . ?
Cu1 O10 Pr1 120.0(3) . . ?
N11 O22 Pr1 92.3(6) . . ?
N11 O23 Pr1 100.5(6) . . ?
N1 C1 C2 111.2(9) . . ?
O1 C2 N2 123.7(10) . . ?
O1 C2 C1 121.9(9) . . ?
N2 C2 C1 114.4(9) . . ?
N3 C3 C4 110.3(8) . . ?
N4 C4 O3 125.0(10) . . ?
N4 C4 C3 113.8(9) . . ?
O3 C4 C3 121.1(9) . . ?
C6 C5 N5 110.4(9) . . ?
N6 C6 O5 122.2(10) . . ?
N6 C6 C5 116.7(10) . . ?
O5 C6 C5 121.1(10) . . ?
N7 C7 C8 112.0(9) . . ?
N8 C8 O7 123.7(10) . . ?
N8 C8 C7 115.7(10) . . ?
O7 C8 C7 120.6(10) . . ?
N9 C9 C10 109.3(8) . . ?
O9 C10 N10 123.9(10) . . ?
O9 C10 C9 120.7(9) . . ?
N10 C10 C9 115.4(9) . . ?
C1 N1 Cu1 111.5(6) . . ?
C2 N2 O2 114.6(8) . . ?
C2 N2 Cu1 119.0(7) . . ?
O2 N2 Cu1 126.2(7) . . ?
C3 N3 Cu2 108.0(6) . . ?
C4 N4 O4 114.6(9) . . ?
C4 N4 Cu2 118.8(8) . . ?
O4 N4 Cu2 125.9(7) . . ?
C5 N5 Cu3 110.8(7) . . ?
C6 N6 O6 116.9(9) . . ?
C6 N6 Cu3 117.8(8) . . ?
O6 N6 Cu3 125.2(7) . . ?
C7 N7 Cu4 109.8(6) . . ?
C8 N8 O8 115.0(9) . . ?
C8 N8 Cu4 119.0(7) . . ?
O8 N8 Cu4 125.9(6) . . ?
C9 N9 Cu5 110.6(7) . . ?
C10 N10 O10 114.0(8) . . ?
C10 N10 Cu5 118.7(7) . . ?
O10 N10 Cu5 127.0(6) . . ?
O24 N11 O22 120.9(9) . . ?
O24 N11 O23 119.3(10) . . ?
O22 N11 O23 119.6(10) . . ?
O27 N12 O26 122.9(11) . . ?
O27 N12 O25 120.7(10) . . ?
O26 N12 O25 116.4(10) . . ?
O28 N13 O29 121.5(11) . . ?
O28 N13 O30 118.3(10) . . ?
O29 N13 O30 120.2(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu2 O1 C2 N2 -6.3(13) . . . . ?
Cu2 O1 C2 C1 173.1(8) . . . . ?
N1 C1 C2 O1 -176.9(9) . . . . ?
N1 C1 C2 N2 2.6(13) . . . . ?
Cu3 O3 C4 N4 0.5(14) . . . . ?
Cu3 O3 C4 C3 -176.4(8) . . . . ?
N3 C3 C4 N4 14.3(14) . . . . ?
N3 C3 C4 O3 -168.4(10) . . . . ?
Cu4 O5 C6 N6 3.4(12) . . . . ?
Cu4 O5 C6 C5 -176.9(8) . . . . ?
N5 C5 C6 N6 -5.6(14) . . . . ?
N5 C5 C6 O5 174.7(9) . . . . ?
Cu5 O7 C8 N8 7.0(13) . . . . ?
Cu5 O7 C8 C7 -174.8(8) . . . . ?
N7 C7 C8 N8 -4.3(14) . . . . ?
N7 C7 C8 O7 177.3(10) . . . . ?
Cu1 O9 C10 N10 -2.1(13) . . . . ?
Cu1 O9 C10 C9 177.1(8) . . . . ?
N9 C9 C10 O9 173.0(9) . . . . ?
N9 C9 C10 N10 -7.8(13) . . . . ?
C2 C1 N1 Cu1 -0.9(11) . . . . ?
O1 C2 N2 O2 1.2(15) . . . . ?
C1 C2 N2 O2 -178.3(8) . . . . ?
O1 C2 N2 Cu1 176.3(8) . . . . ?
C1 C2 N2 Cu1 -3.2(13) . . . . ?
Cu2 O2 N2 C2 4.6(10) . . . . ?
Pr1 O2 N2 C2 147.2(7) . . . . ?
Cu2 O2 N2 Cu1 -170.0(5) . . . . ?
Pr1 O2 N2 Cu1 -27.4(10) . . . . ?
O10 Cu1 N2 C2 -174.9(8) . . . . ?
N1 Cu1 N2 C2 2.2(8) . . . . ?
O10 Cu1 N2 O2 -0.5(8) . . . . ?
N1 Cu1 N2 O2 176.6(9) . . . . ?
C4 C3 N3 Cu2 -26.9(11) . . . . ?
O3 C4 N4 O4 1.0(16) . . . . ?
C3 C4 N4 O4 178.1(9) . . . . ?
O3 C4 N4 Cu2 -169.8(9) . . . . ?
C3 C4 N4 Cu2 7.3(13) . . . . ?
Cu3 O4 N4 C4 -1.9(11) . . . . ?
Pr1 O4 N4 C4 177.7(7) . . . . ?
Cu3 O4 N4 Cu2 168.2(5) . . . . ?
Pr1 O4 N4 Cu2 -12.3(11) . . . . ?
C6 C5 N5 Cu3 9.4(11) . . . . ?
O5 C6 N6 O6 0.0(15) . . . . ?
C5 C6 N6 O6 -179.7(9) . . . . ?
O5 C6 N6 Cu3 178.4(8) . . . . ?
C5 C6 N6 Cu3 -1.3(13) . . . . ?
Cu4 O6 N6 C6 -3.4(11) . . . . ?
Pr1 O6 N6 C6 168.5(7) . . . . ?
Cu4 O6 N6 Cu3 178.3(5) . . . . ?
Pr1 O6 N6 Cu3 -9.7(11) . . . . ?
C8 C7 N7 Cu4 2.4(11) . . . . ?
O7 C8 N8 O8 -1.0(16) . . . . ?
C7 C8 N8 O8 -179.3(9) . . . . ?
O7 C8 N8 Cu4 -177.5(8) . . . . ?
C7 C8 N8 Cu4 4.3(13) . . . . ?
Cu5 O8 N8 C8 -5.6(11) . . . . ?
Pr1 O8 N8 C8 168.6(7) . . . . ?
Cu5 O8 N8 Cu4 170.6(5) . . . . ?
Pr1 O8 N8 Cu4 -15.2(11) . . . . ?
C10 C9 N9 Cu5 16.6(11) . . . . ?
O9 C10 N10 O10 -1.1(15) . . . . ?
C9 C10 N10 O10 179.7(8) . . . . ?
O9 C10 N10 Cu5 173.3(8) . . . . ?
C9 C10 N10 Cu5 -5.9(13) . . . . ?
Cu1 O10 N10 C10 3.7(10) . . . . ?
Pr1 O10 N10 C10 149.3(7) . . . . ?
Cu1 O10 N10 Cu5 -170.1(5) . . . . ?
Pr1 O10 N10 Cu5 -24.5(10) . . . . ?
Pr1 O22 N11 O24 -169.5(9) . . . . ?
Pr1 O22 N11 O23 6.5(9) . . . . ?
Pr1 O23 N11 O24 169.0(8) . . . . ?
Pr1 O23 N11 O22 -7.1(10) . . . . ?

_refine_diff_density_max         5.460
_refine_diff_density_min         -2.627
_refine_diff_density_rms         0.284


_exptl_crystal_preparation       'Magnetic properties,DNA interaction'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_140720f
_database_code_depnum_ccdc_archive 'CCDC 1423975'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
{Nd(NO3)(H2O)2[15-MCCu(N)glyha-5](H2O)2}?2NO3?7H2O
_chemical_name_common            metallacrown
_chemical_melting_point          ?
_chemical_formula_moiety         
{Nd(NO3)(H2O)2[15-MCCu(N)glyha-5](H2O)2}?2NO3?7H2O
_chemical_formula_sum            'C10 H42 Cu5 N13 Nd O30'
_chemical_formula_weight         1286.50

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7503(8)
_cell_length_b                   11.5848(11)
_cell_length_c                   16.9532(14)
_cell_angle_alpha                72.7020(10)
_cell_angle_beta                 87.426(2)
_cell_angle_gamma                74.9780(10)
_cell_volume                     1945.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3879
_cell_measurement_theta_min      2.357
_cell_measurement_theta_max      28.139

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_F_000             1276
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.360
_exptl_absorpt_coefficient_mu    4.108
_shelx_estimated_absorpt_T_min   0.259
_shelx_estimated_absorpt_T_max   0.319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2593
_exptl_absorpt_correction_T_max  0.3194
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9754
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.357
_diffrn_reflns_theta_max         25.017
_diffrn_reflns_theta_full        25.017
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             6709
_reflns_number_gt                5027
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0723P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6709
_refine_ls_number_parameters     532
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1318
_refine_ls_wR_factor_gt          0.1179
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.028
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O28 O 0.8030(8) 0.1150(7) 0.1107(6) 0.083(3) Uani 1 1 d . . . . .
Nd1 Nd 0.53633(4) 0.32525(3) 0.28213(2) 0.02035(13) Uani 1 1 d . . . . .
Cu1 Cu 0.60377(9) 0.31293(8) 0.05425(5) 0.0265(2) Uani 1 1 d . . . . .
Cu2 Cu 0.35859(9) 0.09710(9) 0.23988(6) 0.0278(2) Uani 1 1 d . . . . .
Cu3 Cu 0.41869(8) 0.14934(8) 0.49252(5) 0.0241(2) Uani 1 1 d . . . . .
Cu4 Cu 0.70031(9) 0.39618(8) 0.46141(5) 0.0266(2) Uani 1 1 d . . . . .
Cu5 Cu 0.77145(9) 0.53788(9) 0.18387(6) 0.0299(2) Uani 1 1 d . . . . .
O1 O 0.5064(5) 0.2170(5) 0.0181(3) 0.0329(13) Uani 1 1 d . . . . .
O2 O 0.5177(5) 0.2689(5) 0.1562(3) 0.0264(12) Uani 1 1 d . . . . .
O3 O 0.2607(5) 0.0286(5) 0.3324(3) 0.0334(13) Uani 1 1 d . . . . .
O4 O 0.4466(5) 0.1377(5) 0.3208(3) 0.0299(12) Uani 1 1 d . . . . .
O5 O 0.4591(5) 0.1982(5) 0.5855(3) 0.0280(12) Uani 1 1 d . . . . .
O6 O 0.5460(5) 0.2329(5) 0.4368(3) 0.0285(12) Uani 1 1 d . . . . .
O7 O 0.7836(5) 0.5317(5) 0.4217(3) 0.0319(13) Uani 1 1 d . . . . .
O8 O 0.6757(5) 0.4153(5) 0.3455(3) 0.0276(12) Uani 1 1 d . . . . .
O9 O 0.7951(5) 0.5630(5) 0.0651(3) 0.0298(12) Uani 1 1 d . . . . .
O10 O 0.6728(5) 0.4234(5) 0.1750(3) 0.0266(12) Uani 1 1 d . . . . .
O11 O 0.7275(5) 0.1489(5) 0.2995(4) 0.0394(14) Uani 1 1 d . . . . .
H11B H 0.7964 0.1717 0.3000 0.047 Uiso 1 1 d R U . . .
H11C H 0.7306 0.1126 0.2624 0.047 Uiso 1 1 d R U . . .
O12 O 0.9068(6) 0.2515(6) 0.4845(5) 0.064(2) Uani 1 1 d . . . . .
H12B H 0.9064 0.1955 0.5302 0.077 Uiso 1 1 d R U . . .
H12C H 0.9626 0.2893 0.4895 0.077 Uiso 1 1 d R U . . .
O13 O 0.4347(5) 0.5523(5) 0.2227(3) 0.0352(13) Uani 1 1 d . . . . .
H13B H 0.4863 0.5978 0.2202 0.042 Uiso 1 1 d R U . . .
H13C H 0.3662 0.5780 0.2464 0.042 Uiso 1 1 d R U . . .
O14 O 0.5669(5) 0.7234(5) 0.1492(3) 0.0345(13) Uani 1 1 d . . . . .
H14C H 0.5407 0.7527 0.0988 0.041 Uiso 1 1 d R U . . .
H14D H 0.5516 0.7830 0.1706 0.041 Uiso 1 1 d R U . . .
O15 O 0.0374(12) 0.9022(10) 0.3574(7) 0.149(4) Uani 1 1 d . U . . .
H15D H 0.0360 0.8858 0.3118 0.178 Uiso 1 1 d R U . . .
H15C H 0.0913 0.9457 0.3536 0.178 Uiso 1 1 d R U . . .
O16 O 0.5326(5) 0.8955(5) 0.2435(3) 0.0386(14) Uani 1 1 d . . . . .
H16C H 0.5326 0.8656 0.2958 0.046 Uiso 1 1 d R U . . .
H16D H 0.5995 0.9223 0.2311 0.046 Uiso 1 1 d R U . . .
O17 O 0.9978(7) 0.3593(8) 0.1957(4) 0.074(2) Uani 1 1 d . . . . .
H17C H 0.9445 0.4212 0.1635 0.089 Uiso 1 1 d R U . . .
H17D H 1.0290 0.3847 0.2306 0.089 Uiso 1 1 d R U . . .
O18 O 0.9479(7) 0.1847(7) 0.3341(5) 0.079(3) Uani 1 1 d . . . . .
H18C H 1.0266 0.1460 0.3333 0.094 Uiso 1 1 d R U . . .
H18D H 0.9362 0.2049 0.3786 0.094 Uiso 1 1 d R U . . .
O19 O 0.8813(6) 0.6651(6) 0.5008(4) 0.0537(18) Uani 1 1 d . . . . .
H19C H 0.8496 0.6210 0.4793 0.064 Uiso 1 1 d R U . . .
H19D H 0.8772 0.6383 0.5530 0.064 Uiso 1 1 d R U . . .
O20 O 0.0682(7) 0.3001(7) 0.0520(4) 0.0628(19) Uani 1 1 d . . . . .
H20C H 0.1104 0.3423 0.0166 0.075 Uiso 1 1 d R U . . .
H20D H 0.0312 0.2627 0.0279 0.075 Uiso 1 1 d R U . . .
O21 O 0.9502(8) 0.1808(8) 0.9722(5) 0.080(2) Uani 1 1 d . . . . .
H21C H 1.0208 0.1326 0.9641 0.096 Uiso 1 1 d R U . . .
H21D H 0.9149 0.1426 1.0143 0.096 Uiso 1 1 d R U . . .
O22 O 0.3216(5) 0.3959(5) 0.3546(3) 0.0342(13) Uani 1 1 d . . . . .
O23 O 0.2749(6) 0.3808(6) 0.2369(4) 0.0439(15) Uani 1 1 d . . . . .
O24 O 0.9410(8) 0.1400(9) 0.8011(6) 0.104(3) Uani 1 1 d . . . . .
O25 O 0.7423(7) 0.1929(7) 0.8240(6) 0.093(3) Uani 1 1 d . . . . .
O26 O 0.8328(8) 0.3309(8) 0.7671(6) 0.098(3) Uani 1 1 d . . . . .
O27 O 0.7510(8) -0.0191(8) 0.2097(5) 0.077(2) Uani 1 1 d . . . . .
O29 O 0.7945(10) -0.0581(9) 0.0939(6) 0.105(3) Uani 1 1 d . . . . .
O30 O 0.1237(6) 0.4115(7) 0.3235(4) 0.062(2) Uani 1 1 d . . . . .
C1 C 0.3558(8) 0.0891(8) 0.0723(5) 0.0328(19) Uani 1 1 d . . . . .
H1A H 0.3012 0.1278 0.0225 0.039 Uiso 1 1 calc R U . . .
H1B H 0.4098 0.0095 0.0689 0.039 Uiso 1 1 calc R U . . .
C2 C 0.4380(7) 0.1720(7) 0.0793(5) 0.0281(17) Uani 1 1 d . . . . .
C3 C 0.2269(7) 0.0232(8) 0.4765(4) 0.0305(18) Uani 1 1 d . . . . .
H3A H 0.1360 0.0652 0.4663 0.037 Uiso 1 1 calc R U . . .
H3B H 0.2352 -0.0661 0.4973 0.037 Uiso 1 1 calc R U . . .
C4 C 0.2957(7) 0.0512(7) 0.3970(4) 0.0233(16) Uani 1 1 d . . . . .
C5 C 0.5879(8) 0.3197(8) 0.6217(5) 0.035(2) Uani 1 1 d . . . . .
H5A H 0.5164 0.3798 0.6360 0.041 Uiso 1 1 calc R U . . .
H5B H 0.6225 0.2539 0.6720 0.041 Uiso 1 1 calc R U . . .
C6 C 0.5413(7) 0.2647(7) 0.5620(5) 0.0267(17) Uani 1 1 d . . . . .
C7 C 0.8623(8) 0.6487(7) 0.2951(5) 0.0304(18) Uani 1 1 d . . . . .
H7A H 0.8186 0.7308 0.2997 0.036 Uiso 1 1 calc R U . . .
H7B H 0.9489 0.6262 0.3186 0.036 Uiso 1 1 calc R U . . .
C8 C 0.7914(7) 0.5547(7) 0.3427(5) 0.0262(17) Uani 1 1 d . . . . .
C9 C 0.7504(8) 0.4792(8) -0.0422(5) 0.0325(19) Uani 1 1 d . . . . .
H9A H 0.7060 0.5589 -0.0803 0.039 Uiso 1 1 calc R U . . .
H9B H 0.8401 0.4604 -0.0569 0.039 Uiso 1 1 calc R U . . .
C10 C 0.7416(7) 0.4883(7) 0.0438(4) 0.0248(16) Uani 1 1 d . . . . .
N1 N 0.2751(6) 0.0689(6) 0.1459(4) 0.0336(16) Uani 1 1 d . . . . .
H1C H 0.2661 -0.0088 0.1605 0.040 Uiso 1 1 calc R U . . .
H1D H 0.1972 0.1216 0.1339 0.040 Uiso 1 1 calc R U . . .
N2 N 0.4393(6) 0.1928(6) 0.1500(4) 0.0270(14) Uani 1 1 d . . . . .
N3 N 0.2801(6) 0.0649(6) 0.5400(4) 0.0324(15) Uani 1 1 d . . . . .
H3C H 0.3121 -0.0009 0.5832 0.039 Uiso 1 1 calc R U . . .
H3D H 0.2172 0.1178 0.5573 0.039 Uiso 1 1 calc R U . . .
N4 N 0.3867(6) 0.1059(6) 0.3966(4) 0.0262(14) Uani 1 1 d . . . . .
N5 N 0.6895(8) 0.3825(7) 0.5832(4) 0.047(2) Uani 1 1 d . . . . .
H5C H 0.7653 0.3390 0.6086 0.056 Uiso 1 1 calc R U . . .
H5D H 0.6718 0.4586 0.5894 0.056 Uiso 1 1 calc R U . . .
N6 N 0.5887(6) 0.2860(6) 0.4907(4) 0.0276(15) Uani 1 1 d . . . . .
N7 N 0.8686(6) 0.6534(6) 0.2065(4) 0.0321(15) Uani 1 1 d . . . . .
H7C H 0.9505 0.6307 0.1934 0.039 Uiso 1 1 calc R U . . .
H7D H 0.8345 0.7314 0.1753 0.039 Uiso 1 1 calc R U . . .
N8 N 0.7409(6) 0.5024(6) 0.2987(4) 0.0302(15) Uani 1 1 d . . . . .
N9 N 0.6920(7) 0.3802(6) -0.0497(4) 0.0358(16) Uani 1 1 d . . . . .
H9C H 0.7531 0.3183 -0.0597 0.043 Uiso 1 1 calc R U . . .
H9D H 0.6351 0.4114 -0.0921 0.043 Uiso 1 1 calc R U . . .
N10 N 0.6777(6) 0.4178(6) 0.0942(4) 0.0280(14) Uani 1 1 d . . . . .
N11 N 0.2389(7) 0.3959(6) 0.3038(5) 0.0393(17) Uani 1 1 d . . . . .
N12 N 0.7833(8) 0.0111(8) 0.1356(6) 0.053(2) Uani 1 1 d . . . . .
N13 N 0.8402(7) 0.2211(8) 0.7951(6) 0.053(2) Uani 1 1 d . . . . .


_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
O28 N12 1.221(10) . ?
O28 Cu1 2.664(8) . ?
Nd1 O2 2.441(4) . ?
Nd1 O11 2.450(5) . ?
Nd1 O8 2.472(5) . ?
Nd1 O10 2.477(5) . ?
Nd1 O13 2.482(5) . ?
Nd1 O4 2.502(5) . ?
Nd1 O6 2.516(5) . ?
Nd1 O22 2.622(5) . ?
Nd1 O23 2.804(6) . ?
Cu1 N10 1.899(6) . ?
Cu1 O2 1.918(5) . ?
Cu1 O1 1.942(5) . ?
Cu1 N9 2.008(6) . ?
Cu2 N2 1.918(6) . ?
Cu2 O4 1.932(5) . ?
Cu2 O3 1.934(5) . ?
Cu2 N1 2.010(6) . ?
Cu3 N4 1.909(6) . ?
Cu3 O5 1.926(5) . ?
Cu3 O6 1.931(5) . ?
Cu3 N3 2.001(6) . ?
Cu4 N6 1.918(6) . ?
Cu4 O8 1.933(5) . ?
Cu4 O7 1.940(5) . ?
Cu4 N5 2.023(7) . ?
Cu4 O12 2.377(6) . ?
Cu5 N8 1.898(6) . ?
Cu5 O10 1.941(5) . ?
Cu5 O9 1.961(5) . ?
Cu5 N7 2.024(6) . ?
Cu5 O14 2.591(5) . ?
O1 C2 1.303(9) . ?
O2 N2 1.395(7) . ?
O3 C4 1.291(8) . ?
O4 N4 1.403(7) . ?
O5 C6 1.294(9) . ?
O6 N6 1.395(7) . ?
O7 C8 1.289(9) . ?
O8 N8 1.406(7) . ?
O9 C10 1.294(8) . ?
O10 N10 1.389(7) . ?
O22 N11 1.265(8) . ?
O23 N11 1.228(8) . ?
O24 N13 1.222(10) . ?
O25 N13 1.220(11) . ?
O26 N13 1.201(10) . ?
O27 N12 1.259(11) . ?
O29 N12 1.198(10) . ?
O30 N11 1.250(9) . ?
C1 N1 1.484(10) . ?
C1 C2 1.495(10) . ?
C2 N2 1.293(9) . ?
C3 N3 1.493(9) . ?
C3 C4 1.498(10) . ?
C4 N4 1.295(9) . ?
C5 N5 1.488(10) . ?
C5 C6 1.509(10) . ?
C6 N6 1.269(10) . ?
C7 N7 1.485(10) . ?
C7 C8 1.507(10) . ?
C8 N8 1.302(9) . ?
C9 N9 1.481(9) . ?
C9 C10 1.491(10) . ?
C10 N10 1.301(9) . ?

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
N12 O28 Cu1 118.8(7) . . ?
O2 Nd1 O11 79.50(18) . . ?
O2 Nd1 O8 139.78(16) . . ?
O11 Nd1 O8 84.46(18) . . ?
O2 Nd1 O10 70.30(15) . . ?
O11 Nd1 O10 80.14(18) . . ?
O8 Nd1 O10 70.74(15) . . ?
O2 Nd1 O13 96.26(17) . . ?
O11 Nd1 O13 148.80(18) . . ?
O8 Nd1 O13 79.12(17) . . ?
O10 Nd1 O13 69.47(17) . . ?
O2 Nd1 O4 72.61(16) . . ?
O11 Nd1 O4 76.20(18) . . ?
O8 Nd1 O4 138.10(16) . . ?
O10 Nd1 O4 138.86(15) . . ?
O13 Nd1 O4 132.41(18) . . ?
O2 Nd1 O6 140.60(16) . . ?
O11 Nd1 O6 79.68(18) . . ?
O8 Nd1 O6 70.04(15) . . ?
O10 Nd1 O6 137.19(16) . . ?
O13 Nd1 O6 118.26(17) . . ?
O4 Nd1 O6 70.13(15) . . ?
O2 Nd1 O22 116.87(16) . . ?
O11 Nd1 O22 140.95(18) . . ?
O8 Nd1 O22 98.68(16) . . ?
O10 Nd1 O22 137.81(17) . . ?
O13 Nd1 O22 68.41(17) . . ?
O4 Nd1 O22 75.94(17) . . ?
O6 Nd1 O22 65.38(17) . . ?
O2 Nd1 O23 70.90(16) . . ?
O11 Nd1 O23 137.57(18) . . ?
O8 Nd1 O23 137.29(17) . . ?
O10 Nd1 O23 115.67(17) . . ?
O13 Nd1 O23 66.19(17) . . ?
O4 Nd1 O23 66.47(17) . . ?
O6 Nd1 O23 104.65(17) . . ?
O22 Nd1 O23 46.45(16) . . ?
N10 Cu1 O2 90.4(2) . . ?
N10 Cu1 O1 172.4(3) . . ?
O2 Cu1 O1 84.7(2) . . ?
N10 Cu1 N9 83.2(3) . . ?
O2 Cu1 N9 172.6(2) . . ?
O1 Cu1 N9 101.3(2) . . ?
N10 Cu1 O28 92.8(3) . . ?
O2 Cu1 O28 91.0(2) . . ?
O1 Cu1 O28 93.1(2) . . ?
N9 Cu1 O28 93.0(3) . . ?
N2 Cu2 O4 92.2(2) . . ?
N2 Cu2 O3 170.0(3) . . ?
O4 Cu2 O3 84.5(2) . . ?
N2 Cu2 N1 81.4(3) . . ?
O4 Cu2 N1 173.5(2) . . ?
O3 Cu2 N1 101.7(2) . . ?
N4 Cu3 O5 176.4(2) . . ?
N4 Cu3 O6 91.5(2) . . ?
O5 Cu3 O6 84.8(2) . . ?
N4 Cu3 N3 83.6(3) . . ?
O5 Cu3 N3 100.1(2) . . ?
O6 Cu3 N3 174.7(2) . . ?
N6 Cu4 O8 90.7(2) . . ?
N6 Cu4 O7 169.0(3) . . ?
O8 Cu4 O7 84.7(2) . . ?
N6 Cu4 N5 82.1(3) . . ?
O8 Cu4 N5 169.2(3) . . ?
O7 Cu4 N5 100.9(2) . . ?
N6 Cu4 O12 101.5(2) . . ?
O8 Cu4 O12 98.5(2) . . ?
O7 Cu4 O12 89.1(2) . . ?
N5 Cu4 O12 90.8(3) . . ?
N8 Cu5 O10 90.2(2) . . ?
N8 Cu5 O9 174.8(2) . . ?
O10 Cu5 O9 84.7(2) . . ?
N8 Cu5 N7 83.4(3) . . ?
O10 Cu5 N7 173.5(2) . . ?
O9 Cu5 N7 101.8(2) . . ?
N8 Cu5 O14 91.4(2) . . ?
O10 Cu5 O14 91.0(2) . . ?
O9 Cu5 O14 89.08(19) . . ?
N7 Cu5 O14 88.7(2) . . ?
C2 O1 Cu1 108.2(4) . . ?
N2 O2 Cu1 109.1(4) . . ?
N2 O2 Nd1 122.3(4) . . ?
Cu1 O2 Nd1 128.7(2) . . ?
C4 O3 Cu2 108.8(4) . . ?
N4 O4 Cu2 108.4(4) . . ?
N4 O4 Nd1 119.8(4) . . ?
Cu2 O4 Nd1 121.3(2) . . ?
C6 O5 Cu3 107.7(5) . . ?
N6 O6 Cu3 107.8(4) . . ?
N6 O6 Nd1 123.2(4) . . ?
Cu3 O6 Nd1 121.1(2) . . ?
C8 O7 Cu4 107.6(4) . . ?
N8 O8 Cu4 108.8(4) . . ?
N8 O8 Nd1 122.9(4) . . ?
Cu4 O8 Nd1 128.1(2) . . ?
C10 O9 Cu5 107.5(4) . . ?
N10 O10 Cu5 108.2(4) . . ?
N10 O10 Nd1 124.7(4) . . ?
Cu5 O10 Nd1 126.6(2) . . ?
N11 O22 Nd1 101.1(4) . . ?
N11 O23 Nd1 93.1(5) . . ?
N1 C1 C2 108.9(6) . . ?
N2 C2 O1 122.7(7) . . ?
N2 C2 C1 115.9(7) . . ?
O1 C2 C1 121.4(6) . . ?
N3 C3 C4 111.5(6) . . ?
O3 C4 N4 122.9(7) . . ?
O3 C4 C3 121.7(6) . . ?
N4 C4 C3 115.2(6) . . ?
N5 C5 C6 109.6(6) . . ?
N6 C6 O5 124.0(7) . . ?
N6 C6 C5 116.4(7) . . ?
O5 C6 C5 119.6(7) . . ?
N7 C7 C8 110.9(6) . . ?
O7 C8 N8 124.6(7) . . ?
O7 C8 C7 119.8(6) . . ?
N8 C8 C7 115.6(7) . . ?
N9 C9 C10 110.6(6) . . ?
O9 C10 N10 123.4(7) . . ?
O9 C10 C9 120.6(6) . . ?
N10 C10 C9 116.0(6) . . ?
C1 N1 Cu2 109.7(4) . . ?
C2 N2 O2 115.4(6) . . ?
C2 N2 Cu2 117.8(5) . . ?
O2 N2 Cu2 126.0(4) . . ?
C3 N3 Cu3 110.4(5) . . ?
C4 N4 O4 115.1(6) . . ?
C4 N4 Cu3 119.2(5) . . ?
O4 N4 Cu3 125.4(4) . . ?
C5 N5 Cu4 110.9(5) . . ?
C6 N6 O6 115.6(6) . . ?
C6 N6 Cu4 119.6(5) . . ?
O6 N6 Cu4 124.6(4) . . ?
C7 N7 Cu5 110.6(4) . . ?
C8 N8 O8 113.7(6) . . ?
C8 N8 Cu5 119.3(5) . . ?
O8 N8 Cu5 126.7(4) . . ?
C9 N9 Cu1 110.9(4) . . ?
C10 N10 O10 116.0(6) . . ?
C10 N10 Cu1 118.8(5) . . ?
O10 N10 Cu1 125.1(4) . . ?
O23 N11 O30 122.5(8) . . ?
O23 N11 O22 118.8(7) . . ?
O30 N11 O22 118.7(7) . . ?
O29 N12 O28 123.5(10) . . ?
O29 N12 O27 121.8(10) . . ?
O28 N12 O27 114.6(9) . . ?
O26 N13 O25 116.4(8) . . ?
O26 N13 O24 123.2(10) . . ?
O25 N13 O24 120.1(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C2 N2 0.5(9) . . . . ?
Cu1 O1 C2 C1 -177.6(6) . . . . ?
N1 C1 C2 N2 10.4(10) . . . . ?
N1 C1 C2 O1 -171.4(7) . . . . ?
Cu2 O3 C4 N4 -3.0(9) . . . . ?
Cu2 O3 C4 C3 172.8(6) . . . . ?
N3 C3 C4 O3 -176.4(6) . . . . ?
N3 C3 C4 N4 -0.3(10) . . . . ?
Cu3 O5 C6 N6 -3.2(9) . . . . ?
Cu3 O5 C6 C5 178.2(6) . . . . ?
N5 C5 C6 N6 -3.6(10) . . . . ?
N5 C5 C6 O5 175.1(7) . . . . ?
Cu4 O7 C8 N8 5.7(9) . . . . ?
Cu4 O7 C8 C7 -174.8(6) . . . . ?
N7 C7 C8 O7 175.5(7) . . . . ?
N7 C7 C8 N8 -4.9(10) . . . . ?
Cu5 O9 C10 N10 4.1(9) . . . . ?
Cu5 O9 C10 C9 -176.1(6) . . . . ?
N9 C9 C10 O9 175.1(6) . . . . ?
N9 C9 C10 N10 -5.1(10) . . . . ?
C2 C1 N1 Cu2 -23.3(8) . . . . ?
O1 C2 N2 O2 1.0(11) . . . . ?
C1 C2 N2 O2 179.2(6) . . . . ?
O1 C2 N2 Cu2 -169.2(6) . . . . ?
C1 C2 N2 Cu2 9.0(9) . . . . ?
Cu1 O2 N2 C2 -2.0(7) . . . . ?
Nd1 O2 N2 C2 179.3(5) . . . . ?
Cu1 O2 N2 Cu2 167.2(3) . . . . ?
Nd1 O2 N2 Cu2 -11.4(7) . . . . ?
C4 C3 N3 Cu3 2.4(8) . . . . ?
O3 C4 N4 O4 -0.9(10) . . . . ?
C3 C4 N4 O4 -176.9(6) . . . . ?
O3 C4 N4 Cu3 173.8(5) . . . . ?
C3 C4 N4 Cu3 -2.2(9) . . . . ?
Cu2 O4 N4 C4 4.3(7) . . . . ?
Nd1 O4 N4 C4 149.5(5) . . . . ?
Cu2 O4 N4 Cu3 -170.1(3) . . . . ?
Nd1 O4 N4 Cu3 -24.9(7) . . . . ?
C6 C5 N5 Cu4 10.3(9) . . . . ?
O5 C6 N6 O6 0.3(11) . . . . ?
C5 C6 N6 O6 179.1(6) . . . . ?
O5 C6 N6 Cu4 175.6(5) . . . . ?
C5 C6 N6 Cu4 -5.7(9) . . . . ?
Cu3 O6 N6 C6 2.7(7) . . . . ?
Nd1 O6 N6 C6 151.9(5) . . . . ?
Cu3 O6 N6 Cu4 -172.3(3) . . . . ?
Nd1 O6 N6 Cu4 -23.1(7) . . . . ?
C8 C7 N7 Cu5 2.9(8) . . . . ?
O7 C8 N8 O8 -0.5(11) . . . . ?
C7 C8 N8 O8 180.0(6) . . . . ?
O7 C8 N8 Cu5 -175.6(6) . . . . ?
C7 C8 N8 Cu5 4.8(9) . . . . ?
Cu4 O8 N8 C8 -5.1(7) . . . . ?
Nd1 O8 N8 C8 169.0(5) . . . . ?
Cu4 O8 N8 Cu5 169.7(4) . . . . ?
Nd1 O8 N8 Cu5 -16.3(8) . . . . ?
O10 Cu5 N8 C8 178.0(6) . . . . ?
N7 Cu5 N8 C8 -2.5(6) . . . . ?
O14 Cu5 N8 C8 -91.0(6) . . . . ?
O10 Cu5 N8 O8 3.6(6) . . . . ?
N7 Cu5 N8 O8 -176.9(6) . . . . ?
O14 Cu5 N8 O8 94.6(6) . . . . ?
C10 C9 N9 Cu1 7.4(8) . . . . ?
O9 C10 N10 O10 -2.1(11) . . . . ?
C9 C10 N10 O10 178.2(6) . . . . ?
O9 C10 N10 Cu1 179.8(5) . . . . ?
C9 C10 N10 Cu1 0.0(9) . . . . ?
Cu5 O10 N10 C10 -1.3(7) . . . . ?
Nd1 O10 N10 C10 171.3(5) . . . . ?
Cu5 O10 N10 Cu1 176.8(3) . . . . ?
Nd1 O10 N10 Cu1 -10.7(8) . . . . ?
O2 Cu1 N10 C10 -172.7(6) . . . . ?
N9 Cu1 N10 C10 3.6(6) . . . . ?
O28 Cu1 N10 C10 96.2(6) . . . . ?
O2 Cu1 N10 O10 9.3(6) . . . . ?
N9 Cu1 N10 O10 -174.4(6) . . . . ?
O28 Cu1 N10 O10 -81.7(6) . . . . ?
Nd1 O23 N11 O30 -172.3(7) . . . . ?
Nd1 O23 N11 O22 7.7(7) . . . . ?
Nd1 O22 N11 O23 -8.4(7) . . . . ?
Nd1 O22 N11 O30 171.6(6) . . . . ?
Cu1 O28 N12 O29 96.1(10) . . . . ?
Cu1 O28 N12 O27 -84.7(10) . . . . ?

_refine_diff_density_max         1.161
_refine_diff_density_min         -3.140
_refine_diff_density_rms         0.203


_exptl_crystal_preparation       'Magnetic properties,DNA interaction'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_140610j
_database_code_depnum_ccdc_archive 'CCDC 1423976'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'{Sm(NO3)(H2O)2[15-MCCu(N)glyha-5] (H2O)2}?2NO3?6H2O'
_chemical_name_common            metallacrown
_chemical_melting_point          ?
_chemical_formula_moiety         
'{Sm(NO3)(H2O)2[15-MCCu(N)glyha-5] (H2O)2}?2NO3?6H2O'
_chemical_formula_sum            'C10 H42 Cu5 N13 O30 Sm'
_chemical_formula_weight         1292.61

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7100(8)
_cell_length_b                   11.5449(9)
_cell_length_c                   16.8941(13)
_cell_angle_alpha                72.927(2)
_cell_angle_beta                 87.173(2)
_cell_angle_gamma                74.987(3)
_cell_volume                     1927.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4075
_cell_measurement_theta_min      2.369
_cell_measurement_theta_max      28.052

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.320
_exptl_absorpt_coefficient_mu    4.323
_shelx_estimated_absorpt_T_min   0.258
_shelx_estimated_absorpt_T_max   0.338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2579
_exptl_absorpt_correction_T_max  0.3384
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9835
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.308
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_full        25.020
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             6685
_reflns_number_gt                5211
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0556P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6685
_refine_ls_number_parameters     532
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.1049
_refine_ls_wR_factor_gt          0.0985
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.988
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.53462(3) 0.82667(3) 0.28183(2) 0.02380(11) Uani 1 1 d . . . . .
Cu1 Cu 0.60340(8) 0.81336(7) 0.05457(4) 0.02971(19) Uani 1 1 d . . . . .
Cu2 Cu 0.77074(8) 1.03857(7) 0.18417(4) 0.0333(2) Uani 1 1 d . . . . .
Cu3 Cu 0.69753(8) 0.89773(7) 0.46119(4) 0.0302(2) Uani 1 1 d . . . . .
Cu4 Cu 0.41609(8) 0.65053(7) 0.49231(4) 0.02754(19) Uani 1 1 d . . . . .
Cu5 Cu 0.35610(8) 0.59893(7) 0.23963(4) 0.0313(2) Uani 1 1 d . . . . .
O1 O 0.7966(4) 1.0629(4) 0.0661(3) 0.0360(11) Uani 1 1 d . . . . .
O2 O 0.6715(4) 0.9240(4) 0.1757(2) 0.0313(10) Uani 1 1 d . . . . .
O3 O 0.7810(5) 1.0337(4) 0.4221(2) 0.0365(11) Uani 1 1 d . . . . .
O4 O 0.6726(4) 0.9164(4) 0.3449(2) 0.0287(10) Uani 1 1 d . . . . .
O5 O 0.4575(4) 0.6973(4) 0.5860(2) 0.0314(10) Uani 1 1 d . . . . .
O6 O 0.5423(4) 0.7356(4) 0.4361(2) 0.0312(10) Uani 1 1 d . . . . .
O7 O 0.2598(4) 0.5274(4) 0.3330(3) 0.0378(11) Uani 1 1 d . . . . .
O8 O 0.4426(4) 0.6423(4) 0.3203(2) 0.0356(11) Uani 1 1 d . . . . .
O9 O 0.5059(4) 0.7185(4) 0.0177(2) 0.0356(11) Uani 1 1 d . . . . .
O10 O 0.5162(4) 0.7707(4) 0.1568(2) 0.0313(10) Uani 1 1 d . . . . .
O11 O 0.3210(4) 0.8973(4) 0.3526(3) 0.0393(11) Uani 1 1 d . . . . .
O12 O 0.1216(5) 0.9141(6) 0.3232(3) 0.0629(16) Uani 1 1 d . . . . .
O13 O 0.2715(5) 0.8835(5) 0.2346(3) 0.0497(13) Uani 1 1 d . . . . .
O14 O 0.4351(4) 1.0513(4) 0.2232(3) 0.0363(11) Uani 1 1 d . . . . .
H14B H 0.4873 1.0966 0.2203 0.044 Uiso 1 1 d R U . . .
H14C H 0.3666 1.0777 0.2472 0.044 Uiso 1 1 d R U . . .
O15 O 0.9081(5) 0.7533(5) 0.4841(4) 0.0673(17) Uani 1 1 d . . . . .
H15B H 0.9408 0.7922 0.5097 0.081 Uiso 1 1 d R U . . .
H15C H 0.8636 0.7333 0.4818 0.081 Uiso 1 1 d R U . . .
O16 O 0.7228(4) 0.6532(4) 0.2996(3) 0.0404(11) Uani 1 1 d . . . . .
H16B H 0.7886 0.6827 0.2949 0.049 Uiso 1 1 d DR U . . .
H16C H 0.7260 0.6090 0.2698 0.049 Uiso 1 1 d R U . . .
O17 O 0.2508(6) 0.5156(6) 0.7903(4) 0.0767(18) Uani 1 1 d . . . . .
O18 O 0.2044(8) 0.5579(7) 0.9039(5) 0.103(3) Uani 1 1 d . . . . .
O19 O 0.1961(7) 0.3839(6) 0.8895(5) 0.085(2) Uani 1 1 d . . . . .
O20 O 0.8325(6) 0.8300(6) 0.7644(5) 0.102(3) Uani 1 1 d . . . . .
O21 O 0.7428(6) 0.6934(6) 0.8250(5) 0.094(2) Uani 1 1 d . . . . .
O22 O 0.9394(7) 0.6384(7) 0.7985(5) 0.104(3) Uani 1 1 d . . . . .
O23 O 0.9962(6) 0.8582(5) 0.1959(3) 0.0793(19) Uani 1 1 d . . . . .
H23C H 1.0279 0.8838 0.2307 0.095 Uiso 1 1 d DR U . . .
H23D H 0.9435 0.9203 0.1635 0.095 Uiso 1 1 d R U . . .
O24 O 0.9469(5) 0.6833(5) 0.3363(4) 0.0750(18) Uani 1 1 d . . . . .
H24D H 0.9842 0.7014 0.2927 0.090 Uiso 1 1 d DR U . . .
H24C H 0.9653 0.7182 0.3704 0.090 Uiso 1 1 d DR U . . .
O25 O 0.8776(6) 1.1675(5) 0.5007(3) 0.0621(16) Uani 1 1 d . . . . .
H25C H 0.8465 1.1227 0.4792 0.075 Uiso 1 1 d R U . . .
H25D H 0.8756 1.1393 0.5531 0.075 Uiso 1 1 d R U . . .
O26 O 0.9733(11) 0.5899(8) 0.6424(5) 0.161(4) Uani 1 1 d . . . . .
H26D H 0.9723 0.6085 0.6875 0.193 Uiso 1 1 d R U . . .
H26C H 0.9091 0.6395 0.6120 0.193 Uiso 1 1 d R U . . .
O27 O 0.9515(7) 0.6797(6) 0.9717(4) 0.083(2) Uani 1 1 d . . . . .
H27C H 0.9369 0.6624 0.9282 0.100 Uiso 1 1 d R U . . .
H27D H 0.8995 0.6551 1.0086 0.100 Uiso 1 1 d R U . . .
O28 O 0.0670(6) 0.8000(5) 0.0516(3) 0.0634(15) Uani 1 1 d . . . . .
H28C H 0.1082 0.8429 0.0162 0.076 Uiso 1 1 d R U . . .
H28D H 0.0293 0.7624 0.0281 0.076 Uiso 1 1 d R U . . .
O29 O 0.5661(5) 1.2230(4) 0.1495(3) 0.0382(11) Uani 1 1 d . . . . .
H29C H 0.5393 1.2521 0.0993 0.046 Uiso 1 1 d R U . . .
H29D H 0.5499 1.2828 0.1713 0.046 Uiso 1 1 d R U . . .
O30 O 0.5318(5) 1.3970(4) 0.2429(3) 0.0410(12) Uani 1 1 d . . . . .
H30C H 0.5320 1.3670 0.2952 0.049 Uiso 1 1 d R U . . .
H30D H 0.5982 1.4251 0.2301 0.049 Uiso 1 1 d R U . . .
C1 C 0.7513(7) 0.9791(6) -0.0417(4) 0.0343(15) Uani 1 1 d . . . . .
H1A H 0.7070 1.0592 -0.0793 0.041 Uiso 1 1 calc R U . . .
H1B H 0.8411 0.9599 -0.0571 0.041 Uiso 1 1 calc R U . . .
C2 C 0.7438(6) 0.9879(5) 0.0456(4) 0.0278(14) Uani 1 1 d . . . . .
C3 C 0.8607(7) 1.1501(6) 0.2955(4) 0.0350(16) Uani 1 1 d . . . . .
H3A H 0.8163 1.2326 0.2998 0.042 Uiso 1 1 calc R U . . .
H3B H 0.9472 1.1282 0.3194 0.042 Uiso 1 1 calc R U . . .
C4 C 0.7891(6) 1.0560(5) 0.3435(4) 0.0267(14) Uani 1 1 d . . . . .
C5 C 0.5887(7) 0.8179(6) 0.6220(4) 0.0396(17) Uani 1 1 d . . . . .
H5A H 0.5167 0.8758 0.6385 0.047 Uiso 1 1 calc R U . . .
H5B H 0.6259 0.7514 0.6713 0.047 Uiso 1 1 calc R U . . .
C6 C 0.5409(6) 0.7633(5) 0.5628(4) 0.0278(14) Uani 1 1 d . . . . .
C7 C 0.2283(6) 0.5201(6) 0.4766(4) 0.0331(15) Uani 1 1 d . . . . .
H7A H 0.1367 0.5609 0.4680 0.040 Uiso 1 1 calc R U . . .
H7B H 0.2381 0.4303 0.4960 0.040 Uiso 1 1 calc R U . . .
C8 C 0.2947(6) 0.5518(5) 0.3959(4) 0.0292(14) Uani 1 1 d . . . . .
C9 C 0.3550(7) 0.5902(6) 0.0723(4) 0.0382(17) Uani 1 1 d . . . . .
H9A H 0.3011 0.6289 0.0222 0.046 Uiso 1 1 calc R U . . .
H9B H 0.4089 0.5101 0.0690 0.046 Uiso 1 1 calc R U . . .
C10 C 0.4384(7) 0.6729(5) 0.0794(4) 0.0302(15) Uani 1 1 d . . . . .
N1 N 0.6918(6) 0.8811(5) -0.0494(3) 0.0419(15) Uani 1 1 d . . . . .
H1C H 0.7525 0.8190 -0.0601 0.050 Uiso 1 1 calc R U . . .
H1D H 0.6345 0.9130 -0.0916 0.050 Uiso 1 1 calc R U . . .
N2 N 0.6781(5) 0.9177(5) 0.0947(3) 0.0303(12) Uani 1 1 d . . . . .
N3 N 0.8690(6) 1.1535(5) 0.2077(3) 0.0370(13) Uani 1 1 d . . . . .
H3C H 0.9515 1.1297 0.1952 0.044 Uiso 1 1 calc R U . . .
H3D H 0.8362 1.2315 0.1761 0.044 Uiso 1 1 calc R U . . .
N4 N 0.7378(5) 1.0039(5) 0.3001(3) 0.0318(12) Uani 1 1 d . . . . .
N5 N 0.6872(7) 0.8845(6) 0.5834(3) 0.0522(18) Uani 1 1 d . . . . .
H5C H 0.7639 0.8433 0.6082 0.063 Uiso 1 1 calc R U . . .
H5D H 0.6667 0.9609 0.5898 0.063 Uiso 1 1 calc R U . . .
N6 N 0.5864(5) 0.7886(5) 0.4898(3) 0.0279(12) Uani 1 1 d . . . . .
N7 N 0.2814(5) 0.5601(5) 0.5408(3) 0.0342(13) Uani 1 1 d . . . . .
H7C H 0.3161 0.4932 0.5827 0.041 Uiso 1 1 calc R U . . .
H7D H 0.2179 0.6103 0.5603 0.041 Uiso 1 1 calc R U . . .
N8 N 0.3850(5) 0.6084(4) 0.3957(3) 0.0277(12) Uani 1 1 d . . . . .
N9 N 0.2729(5) 0.5707(5) 0.1454(3) 0.0352(13) Uani 1 1 d . . . . .
H9C H 0.2633 0.4929 0.1598 0.042 Uiso 1 1 calc R U . . .
H9D H 0.1950 0.6238 0.1333 0.042 Uiso 1 1 calc R U . . .
N10 N 0.4377(5) 0.6935(4) 0.1505(3) 0.0313(12) Uani 1 1 d . . . . .
N11 N 0.2370(6) 0.8990(5) 0.3025(4) 0.0398(14) Uani 1 1 d . . . . .
N12 N 0.2148(7) 0.4870(6) 0.8653(5) 0.0542(17) Uani 1 1 d . . . . .
N13 N 0.8387(7) 0.7207(6) 0.7946(4) 0.0516(17) Uani 1 1 d . . . . .


_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
Sm1 O16 2.404(4) . ?
Sm1 O10 2.414(4) . ?
Sm1 O4 2.447(4) . ?
Sm1 O14 2.451(4) . ?
Sm1 O2 2.457(4) . ?
Sm1 O8 2.477(4) . ?
Sm1 O6 2.505(4) . ?
Sm1 O11 2.581(5) . ?
Sm1 O13 2.822(5) . ?
Cu1 N2 1.894(5) . ?
Cu1 O10 1.918(4) . ?
Cu1 O9 1.932(4) . ?
Cu1 N1 2.002(6) . ?
Cu2 N4 1.914(5) . ?
Cu2 O2 1.938(4) . ?
Cu2 O1 1.947(4) . ?
Cu2 N3 2.025(5) . ?
Cu2 O29 2.580(4) . ?
Cu2 H23D 2.0777 . ?
Cu3 N6 1.898(5) . ?
Cu3 O4 1.936(4) . ?
Cu3 O3 1.939(4) . ?
Cu3 N5 2.024(5) . ?
Cu3 O15 2.403(5) . ?
Cu4 N8 1.901(5) . ?
Cu4 O5 1.921(4) . ?
Cu4 O6 1.926(4) . ?
Cu4 N7 2.001(5) . ?
Cu5 N10 1.903(5) . ?
Cu5 O8 1.932(4) . ?
Cu5 O7 1.936(4) . ?
Cu5 N9 2.008(5) . ?
O1 C2 1.280(7) . ?
O2 N2 1.389(6) . ?
O3 C4 1.279(7) . ?
O4 N4 1.395(6) . ?
O5 C6 1.294(7) . ?
O6 N6 1.391(6) . ?
O7 C8 1.272(7) . ?
O8 N8 1.382(6) . ?
O9 C10 1.299(8) . ?
O10 N10 1.401(6) . ?
O11 N11 1.258(7) . ?
O12 N11 1.250(7) . ?
O13 N11 1.236(7) . ?
O14 H14B 0.8500 . ?
O14 H14C 0.8500 . ?
O15 H15B 0.8500 . ?
O15 H15C 0.5874 . ?
O16 H16B 0.8500 . ?
O16 H16C 0.8097 . ?
O17 N12 1.278(9) . ?
O18 N12 1.170(8) . ?
O19 N12 1.205(8) . ?
O20 N13 1.199(8) . ?
O21 N13 1.199(9) . ?
O22 N13 1.229(8) . ?
O23 H23C 0.8499 . ?
O23 H23D 0.8501 . ?
O24 H24D 0.8178 . ?
O24 H24C 0.8501 . ?
O25 H25C 0.8500 . ?
O25 H25D 0.8501 . ?
O26 H26C 0.8500 . ?
O26 H26D 0.8499 . ?
O26 H26C 0.8500 . ?
O27 H27C 0.8469 . ?
O27 H27D 0.8501 . ?
O28 H28C 0.8429 . ?
O28 H28D 0.8475 . ?
O29 H29C 0.8500 . ?
O29 H29D 0.8498 . ?
O30 H30C 0.8494 . ?
O30 H30D 0.8492 . ?
C1 N1 1.474(8) . ?
C1 C2 1.504(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.297(8) . ?
C3 N3 1.471(8) . ?
C3 C4 1.509(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.294(7) . ?
C5 N5 1.479(9) . ?
C5 C6 1.499(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N6 1.284(8) . ?
C7 N7 1.483(7) . ?
C7 C8 1.498(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N8 1.300(8) . ?
C9 N9 1.478(8) . ?
C9 C10 1.498(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N10 1.291(7) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N5 H5C 0.8900 . ?
N5 H5D 0.8900 . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
N9 H9C 0.8900 . ?
N9 H9D 0.8900 . ?

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
O16 Sm1 O10 80.09(15) . . ?
O16 Sm1 O4 84.24(14) . . ?
O10 Sm1 O4 139.96(14) . . ?
O16 Sm1 O14 148.76(15) . . ?
O10 Sm1 O14 96.11(14) . . ?
O4 Sm1 O14 78.99(14) . . ?
O16 Sm1 O2 80.37(15) . . ?
O10 Sm1 O2 70.54(13) . . ?
O4 Sm1 O2 70.62(13) . . ?
O14 Sm1 O2 69.28(14) . . ?
O16 Sm1 O8 76.88(15) . . ?
O10 Sm1 O8 72.84(13) . . ?
O4 Sm1 O8 138.21(13) . . ?
O14 Sm1 O8 131.96(15) . . ?
O2 Sm1 O8 139.51(13) . . ?
O16 Sm1 O6 79.47(14) . . ?
O10 Sm1 O6 140.69(13) . . ?
O4 Sm1 O6 70.08(13) . . ?
O14 Sm1 O6 118.19(14) . . ?
O2 Sm1 O6 137.18(14) . . ?
O8 Sm1 O6 70.01(13) . . ?
O16 Sm1 O11 140.94(15) . . ?
O10 Sm1 O11 116.33(14) . . ?
O4 Sm1 O11 98.91(14) . . ?
O14 Sm1 O11 68.38(15) . . ?
O2 Sm1 O11 137.58(14) . . ?
O8 Sm1 O11 75.26(15) . . ?
O6 Sm1 O11 65.57(14) . . ?
O16 Sm1 O13 137.75(14) . . ?
O10 Sm1 O13 70.24(14) . . ?
O4 Sm1 O13 137.40(14) . . ?
O14 Sm1 O13 66.10(14) . . ?
O2 Sm1 O13 115.19(14) . . ?
O8 Sm1 O13 66.19(15) . . ?
O6 Sm1 O13 105.07(14) . . ?
O11 Sm1 O13 46.58(13) . . ?
N2 Cu1 O10 90.22(19) . . ?
N2 Cu1 O9 172.6(2) . . ?
O10 Cu1 O9 85.18(17) . . ?
N2 Cu1 N1 83.0(2) . . ?
O10 Cu1 N1 172.0(2) . . ?
O9 Cu1 N1 101.12(19) . . ?
N4 Cu2 O2 89.81(19) . . ?
N4 Cu2 O1 175.05(19) . . ?
O2 Cu2 O1 85.26(17) . . ?
N4 Cu2 N3 83.2(2) . . ?
O2 Cu2 N3 173.04(19) . . ?
O1 Cu2 N3 101.7(2) . . ?
N4 Cu2 O29 91.18(19) . . ?
O2 Cu2 O29 90.64(16) . . ?
O1 Cu2 O29 89.27(16) . . ?
N3 Cu2 O29 89.33(19) . . ?
N4 Cu2 H23D 110.9 . . ?
O2 Cu2 H23D 92.4 . . ?
O1 Cu2 H23D 69.1 . . ?
N3 Cu2 H23D 90.2 . . ?
O29 Cu2 H23D 157.7 . . ?
N6 Cu3 O4 90.23(18) . . ?
N6 Cu3 O3 168.9(2) . . ?
O4 Cu3 O3 85.24(16) . . ?
N6 Cu3 N5 82.6(2) . . ?
O4 Cu3 N5 169.3(2) . . ?
O3 Cu3 N5 100.4(2) . . ?
N6 Cu3 O15 102.2(2) . . ?
O4 Cu3 O15 98.86(19) . . ?
O3 Cu3 O15 88.54(19) . . ?
N5 Cu3 O15 90.5(2) . . ?
N8 Cu4 O5 176.0(2) . . ?
N8 Cu4 O6 90.95(19) . . ?
O5 Cu4 O6 85.05(17) . . ?
N8 Cu4 N7 83.8(2) . . ?
O5 Cu4 N7 100.2(2) . . ?
O6 Cu4 N7 174.74(19) . . ?
N10 Cu5 O8 91.78(19) . . ?
N10 Cu5 O7 171.1(2) . . ?
O8 Cu5 O7 84.57(17) . . ?
N10 Cu5 N9 81.5(2) . . ?
O8 Cu5 N9 173.0(2) . . ?
O7 Cu5 N9 101.8(2) . . ?
C2 O1 Cu2 106.7(4) . . ?
N2 O2 Cu2 107.7(3) . . ?
N2 O2 Sm1 124.9(3) . . ?
Cu2 O2 Sm1 127.03(17) . . ?
C4 O3 Cu3 107.1(4) . . ?
N4 O4 Cu3 107.2(3) . . ?
N4 O4 Sm1 124.1(3) . . ?
Cu3 O4 Sm1 128.37(19) . . ?
C6 O5 Cu4 107.6(4) . . ?
N6 O6 Cu4 108.3(3) . . ?
N6 O6 Sm1 123.0(3) . . ?
Cu4 O6 Sm1 121.62(18) . . ?
C8 O7 Cu5 107.8(4) . . ?
N8 O8 Cu5 108.4(3) . . ?
N8 O8 Sm1 120.9(3) . . ?
Cu5 O8 Sm1 121.83(19) . . ?
C10 O9 Cu1 107.6(3) . . ?
N10 O10 Cu1 108.7(3) . . ?
N10 O10 Sm1 122.4(3) . . ?
Cu1 O10 Sm1 128.9(2) . . ?
N11 O11 Sm1 102.6(4) . . ?
N11 O13 Sm1 91.4(4) . . ?
Sm1 O14 H14B 113.3 . . ?
Sm1 O14 H14C 113.4 . . ?
H14B O14 H14C 110.7 . . ?
Cu3 O15 H15B 96.0 . . ?
Cu3 O15 H15C 62.4 . . ?
H15B O15 H15C 144.9 . . ?
Sm1 O16 H16B 107.3 . . ?
Sm1 O16 H16C 116.2 . . ?
H16B O16 H16C 111.8 . . ?
H23C O23 H23D 108.6 . . ?
H24D O24 H24C 111.6 . . ?
H25C O25 H25D 108.5 . . ?
H26C O26 H26D 108.6 . . ?
H26C O26 H26C 0.0 . . ?
H26D O26 H26C 108.6 . . ?
H27C O27 H27D 109.0 . . ?
H28C O28 H28D 109.3 . . ?
Cu2 O29 H29C 117.2 . . ?
Cu2 O29 H29D 123.9 . . ?
H29C O29 H29D 108.7 . . ?
H30C O30 H30D 108.4 . . ?
N1 C1 C2 110.8(5) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
O1 C2 N2 124.8(5) . . ?
O1 C2 C1 120.4(5) . . ?
N2 C2 C1 114.7(5) . . ?
N3 C3 C4 111.3(5) . . ?
N3 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
N3 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O3 C4 N4 124.4(6) . . ?
O3 C4 C3 119.8(5) . . ?
N4 C4 C3 115.8(5) . . ?
N5 C5 C6 110.8(5) . . ?
N5 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N5 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N6 C6 O5 124.1(5) . . ?
N6 C6 C5 115.6(6) . . ?
O5 C6 C5 120.3(5) . . ?
N7 C7 C8 112.1(5) . . ?
N7 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N7 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
O7 C8 N8 124.2(6) . . ?
O7 C8 C7 120.9(6) . . ?
N8 C8 C7 114.8(5) . . ?
N9 C9 C10 109.4(5) . . ?
N9 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
N9 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
N10 C10 O9 123.8(6) . . ?
N10 C10 C9 115.0(6) . . ?
O9 C10 C9 121.2(5) . . ?
C1 N1 Cu1 111.1(4) . . ?
C1 N1 H1C 109.4 . . ?
Cu1 N1 H1C 109.4 . . ?
C1 N1 H1D 109.4 . . ?
Cu1 N1 H1D 109.4 . . ?
H1C N1 H1D 108.0 . . ?
C2 N2 O2 115.3(5) . . ?
C2 N2 Cu1 119.8(4) . . ?
O2 N2 Cu1 124.8(4) . . ?
C3 N3 Cu2 110.7(4) . . ?
C3 N3 H3C 109.5 . . ?
Cu2 N3 H3C 109.5 . . ?
C3 N3 H3D 109.5 . . ?
Cu2 N3 H3D 109.5 . . ?
H3C N3 H3D 108.1 . . ?
C4 N4 O4 115.5(5) . . ?
C4 N4 Cu2 118.7(4) . . ?
O4 N4 Cu2 125.5(3) . . ?
C5 N5 Cu3 110.3(4) . . ?
C5 N5 H5C 109.6 . . ?
Cu3 N5 H5C 109.6 . . ?
C5 N5 H5D 109.6 . . ?
Cu3 N5 H5D 109.6 . . ?
H5C N5 H5D 108.1 . . ?
C6 N6 O6 114.8(5) . . ?
C6 N6 Cu3 119.8(4) . . ?
O6 N6 Cu3 125.4(3) . . ?
C7 N7 Cu4 110.0(4) . . ?
C7 N7 H7C 109.7 . . ?
Cu4 N7 H7C 109.7 . . ?
C7 N7 H7D 109.7 . . ?
Cu4 N7 H7D 109.7 . . ?
H7C N7 H7D 108.2 . . ?
C8 N8 O8 114.8(5) . . ?
C8 N8 Cu4 119.1(4) . . ?
O8 N8 Cu4 125.8(4) . . ?
C9 N9 Cu5 109.3(4) . . ?
C9 N9 H9C 109.8 . . ?
Cu5 N9 H9C 109.8 . . ?
C9 N9 H9D 109.8 . . ?
Cu5 N9 H9D 109.8 . . ?
H9C N9 H9D 108.3 . . ?
C10 N10 O10 114.7(5) . . ?
C10 N10 Cu5 118.5(4) . . ?
O10 N10 Cu5 126.1(4) . . ?
O13 N11 O12 121.9(6) . . ?
O13 N11 O11 118.9(6) . . ?
O12 N11 O11 119.2(6) . . ?
O18 N12 O19 126.2(9) . . ?
O18 N12 O17 120.0(8) . . ?
O19 N12 O17 113.9(7) . . ?
O20 N13 O21 117.4(7) . . ?
O20 N13 O22 122.6(8) . . ?
O21 N13 O22 119.9(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu2 O1 C2 N2 4.6(8) . . . . ?
Cu2 O1 C2 C1 -177.4(5) . . . . ?
N1 C1 C2 O1 176.1(6) . . . . ?
N1 C1 C2 N2 -5.7(8) . . . . ?
Cu3 O3 C4 N4 6.3(7) . . . . ?
Cu3 O3 C4 C3 -174.6(5) . . . . ?
N3 C3 C4 O3 174.8(6) . . . . ?
N3 C3 C4 N4 -6.0(8) . . . . ?
Cu4 O5 C6 N6 -1.0(7) . . . . ?
Cu4 O5 C6 C5 177.8(5) . . . . ?
N5 C5 C6 N6 -3.6(9) . . . . ?
N5 C5 C6 O5 177.5(6) . . . . ?
Cu5 O7 C8 N8 -3.7(8) . . . . ?
Cu5 O7 C8 C7 173.8(5) . . . . ?
N7 C7 C8 O7 -178.2(5) . . . . ?
N7 C7 C8 N8 -0.5(8) . . . . ?
Cu1 O9 C10 N10 1.8(8) . . . . ?
Cu1 O9 C10 C9 -177.8(5) . . . . ?
N9 C9 C10 N10 10.2(8) . . . . ?
N9 C9 C10 O9 -170.1(6) . . . . ?
C2 C1 N1 Cu1 7.5(7) . . . . ?
O1 C2 N2 O2 -2.6(9) . . . . ?
C1 C2 N2 O2 179.4(5) . . . . ?
O1 C2 N2 Cu1 179.0(5) . . . . ?
C1 C2 N2 Cu1 1.0(7) . . . . ?
Cu2 O2 N2 C2 -1.1(6) . . . . ?
Sm1 O2 N2 C2 171.8(4) . . . . ?
Cu2 O2 N2 Cu1 177.2(3) . . . . ?
Sm1 O2 N2 Cu1 -9.8(6) . . . . ?
O10 Cu1 N2 C2 -173.0(5) . . . . ?
N1 Cu1 N2 C2 2.8(5) . . . . ?
O10 Cu1 N2 O2 8.8(5) . . . . ?
N1 Cu1 N2 O2 -175.5(5) . . . . ?
C4 C3 N3 Cu2 3.7(7) . . . . ?
O3 C4 N4 O4 -1.3(9) . . . . ?
C3 C4 N4 O4 179.6(5) . . . . ?
O3 C4 N4 Cu2 -175.2(5) . . . . ?
C3 C4 N4 Cu2 5.6(7) . . . . ?
Cu3 O4 N4 C4 -4.5(6) . . . . ?
Sm1 O4 N4 C4 169.3(4) . . . . ?
Cu3 O4 N4 Cu2 169.0(3) . . . . ?
Sm1 O4 N4 Cu2 -17.2(6) . . . . ?
C6 C5 N5 Cu3 8.6(7) . . . . ?
O5 C6 N6 O6 -2.1(9) . . . . ?
C5 C6 N6 O6 179.1(5) . . . . ?
O5 C6 N6 Cu3 174.9(4) . . . . ?
C5 C6 N6 Cu3 -4.0(8) . . . . ?
Cu4 O6 N6 C6 3.9(6) . . . . ?
Sm1 O6 N6 C6 154.7(4) . . . . ?
Cu4 O6 N6 Cu3 -172.8(3) . . . . ?
Sm1 O6 N6 Cu3 -22.1(6) . . . . ?
O4 Cu3 N6 C6 -164.7(5) . . . . ?
O3 Cu3 N6 C6 -98.9(10) . . . . ?
N5 Cu3 N6 C6 7.3(5) . . . . ?
O15 Cu3 N6 C6 96.1(5) . . . . ?
O4 Cu3 N6 O6 11.9(4) . . . . ?
O3 Cu3 N6 O6 77.7(11) . . . . ?
N5 Cu3 N6 O6 -176.1(5) . . . . ?
O15 Cu3 N6 O6 -87.3(5) . . . . ?
C8 C7 N7 Cu4 3.2(6) . . . . ?
O7 C8 N8 O8 0.2(9) . . . . ?
C7 C8 N8 O8 -177.4(5) . . . . ?
O7 C8 N8 Cu4 174.8(5) . . . . ?
C7 C8 N8 Cu4 -2.9(7) . . . . ?
Cu5 O8 N8 C8 3.4(6) . . . . ?
Sm1 O8 N8 C8 151.2(4) . . . . ?
Cu5 O8 N8 Cu4 -170.8(3) . . . . ?
Sm1 O8 N8 Cu4 -23.0(6) . . . . ?
C10 C9 N9 Cu5 -23.4(6) . . . . ?
O9 C10 N10 O10 0.2(9) . . . . ?
C9 C10 N10 O10 179.8(5) . . . . ?
O9 C10 N10 Cu5 -170.1(5) . . . . ?
C9 C10 N10 Cu5 9.5(7) . . . . ?
Cu1 O10 N10 C10 -2.1(6) . . . . ?
Sm1 O10 N10 C10 179.9(4) . . . . ?
Cu1 O10 N10 Cu5 167.3(3) . . . . ?
Sm1 O10 N10 Cu5 -10.7(6) . . . . ?
Sm1 O13 N11 O12 -171.6(6) . . . . ?
Sm1 O13 N11 O11 7.1(5) . . . . ?
Sm1 O11 N11 O13 -7.9(6) . . . . ?
Sm1 O11 N11 O12 170.8(5) . . . . ?

_refine_diff_density_max         0.946
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.196


_exptl_crystal_preparation       'Magnetic properties,DNA interaction'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_6326
_database_code_depnum_ccdc_archive 'CCDC 1423977'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'{Gd(OAc)(H2O)[15-MCCu(N)glyha-5] (H2O)3}?2NO3?5H2O'
_chemical_name_common            metallacrown
_chemical_melting_point          ?
_chemical_formula_moiety         
'{Gd(OAc)(H2O)[15-MCCu(N)glyha-5] (H2O)3}?2NO3?5H2O'
_chemical_formula_sum            'C12 H41 Cu5 Gd N12 O27'
_chemical_formula_weight         1260.52

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'
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'
Gd Gd -0.1653 3.9035 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5669(8)
_cell_length_b                   12.3139(9)
_cell_length_c                   16.1763(10)
_cell_angle_alpha                101.321(6)
_cell_angle_beta                 107.610(6)
_cell_angle_gamma                106.655(7)
_cell_volume                     1827.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3185
_cell_measurement_theta_min      2.9930
_cell_measurement_theta_max      27.4630
_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.291
_exptl_crystal_F_000             1244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    4.758
_shelx_estimated_absorpt_T_min   0.240
_shelx_estimated_absorpt_T_max   0.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2398
_exptl_absorpt_correction_T_max  0.5165
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11689
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.509
_diffrn_reflns_theta_max         25.017
_diffrn_reflns_theta_full        25.017
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6459
_reflns_number_gt                5055
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0719P)²+26.4100P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6459
_refine_ls_number_parameters     515
_refine_ls_number_restraints     1422
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0759
_refine_ls_wR_factor_ref         0.2053
_refine_ls_wR_factor_gt          0.1741
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.020
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.77650(6) 0.63151(5) 0.29528(4) 0.0100(2) Uani 1 1 d . U . . .
Cu1 Cu 0.71362(17) 0.52764(14) 0.04103(10) 0.0140(4) Uani 1 1 d . U . . .
Cu2 Cu 0.89224(17) 0.91412(14) 0.22176(11) 0.0165(4) Uani 1 1 d . U . . .
Cu3 Cu 1.09919(16) 0.87280(14) 0.50147(10) 0.0122(4) Uani 1 1 d . U . . .
Cu4 Cu 0.80853(16) 0.51822(14) 0.50657(10) 0.0133(4) Uani 1 1 d . U . . .
Cu5 Cu 0.57061(17) 0.28978(14) 0.20494(11) 0.0160(4) Uani 1 1 d . U . . .
O1 O 0.7469(10) 0.6531(8) -0.0139(6) 0.0190(17) Uani 1 1 d . U . . .
O2 O 0.7464(10) 0.6544(8) 0.1474(6) 0.0156(14) Uani 1 1 d . U . . .
O3 O 1.0520(10) 1.0474(8) 0.3159(6) 0.0177(16) Uani 1 1 d . U . . .
O4 O 0.8889(10) 0.8447(8) 0.3221(6) 0.0179(14) Uani 1 1 d . U . . .
O5 O 1.1491(9) 0.8280(8) 0.6140(6) 0.0147(15) Uani 1 1 d . U . . .
O6 O 0.9422(9) 0.7218(8) 0.4518(6) 0.0162(14) Uani 1 1 d . U . . .
O7 O 0.6857(9) 0.3525(8) 0.4758(6) 0.0144(16) Uani 1 1 d . U . . .
O8 O 0.7462(10) 0.4855(8) 0.3760(6) 0.0176(14) Uani 1 1 d . U . . .
O9 O 0.5337(10) 0.2162(8) 0.0775(6) 0.0195(16) Uani 1 1 d . U . . .
O10 O 0.6806(10) 0.4351(8) 0.1894(6) 0.0172(14) Uani 1 1 d . U . . .
O11 O 1.0022(9) 0.6314(8) 0.2874(6) 0.0166(11) Uani 1 1 d . U . . .
H11B H 1.0682 0.6799 0.3371 0.020 Uiso 1 1 d R U . . .
H11C H 1.0123 0.6601 0.2451 0.020 Uiso 1 1 d R U . . .
O12 O 1.2306(9) 0.7899(8) 0.4339(6) 0.0153(12) Uani 1 1 d . U . . .
H12E H 1.2703 0.7531 0.4661 0.018 Uiso 1 1 d R U . . .
H12F H 1.2945 0.8435 0.4270 0.018 Uiso 1 1 d R U . . .
O13 O 0.3592(9) 0.3284(8) 0.1877(6) 0.0187(12) Uani 1 1 d . U . . .
H13B H 0.3257 0.3258 0.1322 0.022 Uiso 1 1 d R U . . .
H13C H 0.3874 0.4011 0.2188 0.022 Uiso 1 1 d R U . . .
O14 O 0.7185(10) 0.9917(8) 0.2257(6) 0.0199(15) Uani 1 1 d . U . . .
H14B H 0.7466 1.0429 0.2775 0.024 Uiso 1 1 d R U . . .
H14C H 0.6424 0.9361 0.2182 0.024 Uiso 1 1 d R U . . .
O15 O 0.6236(10) 0.5879(8) 0.5213(6) 0.0191(16) Uani 1 1 d . U . . .
H15B H 0.6052 0.6240 0.4821 0.023 Uiso 1 1 d R U . . .
H15C H 0.6566 0.6388 0.5738 0.023 Uiso 1 1 d R U . . .
O16 O 0.378(2) 0.988(2) 0.9497(16) 0.147(10) Uani 1 1 d . . . . .
H16C H 0.4052 0.9291 0.9446 0.177 Uiso 1 1 d R U . . .
H16D H 0.3483 0.9967 0.8973 0.177 Uiso 1 1 d R U . . .
O17 O 0.7685(10) 0.7395(9) 0.6951(6) 0.0217(19) Uani 1 1 d . U . . .
H17C H 0.8206 0.8110 0.7041 0.026 Uiso 1 1 d R U . . .
H17D H 0.7396 0.7372 0.7386 0.026 Uiso 1 1 d R U . . .
O18 O 0.7983(11) 0.0317(10) 0.8747(8) 0.034(2) Uani 1 1 d . U . . .
H18C H 0.7855 0.0675 0.8347 0.041 Uiso 1 1 d R U . . .
H18D H 0.8341 0.0830 0.9272 0.041 Uiso 1 1 d R U . . .
O19 O 0.9765(10) 0.5746(9) 0.1090(6) 0.0232(15) Uani 1 1 d . U . . .
H19C H 1.0170 0.6079 0.0776 0.028 Uiso 1 1 d R U . . .
H19D H 0.9994 0.5148 0.1140 0.028 Uiso 1 1 d R U . . .
O20 O 0.6221(10) 0.6774(8) 0.3778(6) 0.0199(16) Uani 1 1 d . U . . .
O21 O 0.5266(11) 0.6064(10) 0.2327(7) 0.0331(17) Uani 1 1 d . U . . .
O22 O 0.9032(12) 0.3001(10) -0.0084(7) 0.0323(15) Uani 1 1 d . U . . .
O23 O 0.9280(15) 0.1917(12) 0.0769(9) 0.052(2) Uani 1 1 d . U . . .
O24 O 1.0343(13) 0.3777(10) 0.1342(8) 0.0393(17) Uani 1 1 d . U . . .
O25 O 0.5515(11) 0.0835(11) 0.6092(8) 0.036(2) Uani 1 1 d . U . . .
O26 O 0.5481(12) 0.1167(11) 0.7442(8) 0.0364(19) Uani 1 1 d . U . . .
O27 O 0.7421(12) 0.1198(11) 0.7245(8) 0.0384(19) Uani 1 1 d . U . . .
C1 C 0.8368(16) 0.8680(13) 0.0300(10) 0.024(2) Uani 1 1 d . U . . .
H1A H 0.7550 0.8813 -0.0073 0.029 Uiso 1 1 calc R U . . .
H1B H 0.8981 0.8644 -0.0037 0.029 Uiso 1 1 calc R U . . .
C2 C 0.7875(14) 0.7540(12) 0.0484(9) 0.018(2) Uani 1 1 d . U . . .
C3 C 1.2256(14) 1.0876(12) 0.4670(9) 0.019(2) Uani 1 1 d . U . . .
H3A H 1.3052 1.0878 0.4488 0.022 Uiso 1 1 calc R U . . .
H3B H 1.2306 1.1691 0.4849 0.022 Uiso 1 1 calc R U . . .
C4 C 1.0881(13) 1.0132(12) 0.3879(9) 0.0132(18) Uani 1 1 d . U . . .
C5 C 1.0484(14) 0.6722(12) 0.6751(9) 0.018(2) Uani 1 1 d . U . . .
H5A H 1.1285 0.6461 0.6890 0.021 Uiso 1 1 calc R U . . .
H5B H 1.0602 0.7298 0.7300 0.021 Uiso 1 1 calc R U . . .
C6 C 1.0454(13) 0.7305(12) 0.5991(9) 0.013(2) Uani 1 1 d . U . . .
C7 C 0.5265(14) 0.1798(12) 0.3418(9) 0.016(2) Uani 1 1 d . U . . .
H7A H 0.5675 0.1284 0.3696 0.020 Uiso 1 1 calc R U . . .
H7B H 0.4367 0.1696 0.3495 0.020 Uiso 1 1 calc R U . . .
C8 C 0.6280(14) 0.3089(12) 0.3886(9) 0.0147(18) Uani 1 1 d . U . . .
C9 C 0.5733(15) 0.2770(13) -0.0485(9) 0.020(2) Uani 1 1 d . U . . .
H9A H 0.4728 0.2513 -0.0866 0.023 Uiso 1 1 calc R U . . .
H9B H 0.6054 0.2127 -0.0654 0.023 Uiso 1 1 calc R U . . .
C10 C 0.5901(15) 0.3006(13) 0.0478(9) 0.020(2) Uani 1 1 d . U . . .
C11 C 0.5137(15) 0.6348(13) 0.3063(10) 0.0207(19) Uani 1 1 d . U . . .
C12 C 0.3662(15) 0.6088(13) 0.3062(10) 0.0225(19) Uani 1 1 d . U . . .
H12A H 0.3223 0.6548 0.2744 0.034 Uiso 1 1 calc R U . . .
H12B H 0.3716 0.6296 0.3679 0.034 Uiso 1 1 calc R U . . .
H12C H 0.3101 0.5255 0.2762 0.034 Uiso 1 1 calc R U . . .
N1 N 0.9177(12) 0.9700(10) 0.1175(8) 0.0196(19) Uani 1 1 d . U . . .
H1C H 0.8854 1.0289 0.1137 0.023 Uiso 1 1 calc R U . . .
H1D H 1.0101 0.9977 0.1269 0.023 Uiso 1 1 calc R U . . .
N2 N 0.7923(12) 0.7618(10) 0.1295(8) 0.0165(15) Uani 1 1 d . U . . .
N3 N 1.2372(12) 1.0410(10) 0.5454(8) 0.0172(18) Uani 1 1 d . U . . .
H3C H 1.2178 1.0855 0.5867 0.021 Uiso 1 1 calc R U . . .
H3D H 1.3258 1.0438 0.5715 0.021 Uiso 1 1 calc R U . . .
N4 N 1.0150(11) 0.9182(10) 0.3967(7) 0.0136(15) Uani 1 1 d . U . . .
N5 N 0.9121(11) 0.5681(10) 0.6447(7) 0.0147(18) Uani 1 1 d . U . . .
H5C H 0.8565 0.5874 0.6720 0.018 Uiso 1 1 calc R U . . .
H5D H 0.9308 0.5075 0.6607 0.018 Uiso 1 1 calc R U . . .
N6 N 0.9426(11) 0.6688(10) 0.5203(7) 0.0140(16) Uani 1 1 d . U . . .
N7 N 0.5001(12) 0.1454(10) 0.2417(7) 0.0179(18) Uani 1 1 d . U . . .
H7C H 0.4069 0.1068 0.2093 0.021 Uiso 1 1 calc R U . . .
H7D H 0.5447 0.0965 0.2300 0.021 Uiso 1 1 calc R U . . .
N8 N 0.6474(11) 0.3679(10) 0.3326(7) 0.0134(16) Uani 1 1 d . U . . .
N9 N 0.6558(13) 0.3843(10) -0.0662(8) 0.0204(18) Uani 1 1 d . U . . .
H9C H 0.6022 0.3930 -0.1168 0.024 Uiso 1 1 calc R U . . .
H9D H 0.7331 0.3760 -0.0735 0.024 Uiso 1 1 calc R U . . .
N10 N 0.6629(12) 0.4098(10) 0.0969(7) 0.0170(17) Uani 1 1 d . U . . .
N11 N 0.9554(16) 0.2911(13) 0.0701(10) 0.039(2) Uani 1 1 d . U . . .
N12 N 0.6163(14) 0.1103(13) 0.6963(9) 0.031(2) Uani 1 1 d . U . . .


_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
Gd1 O10 2.393(9) . ?
Gd1 O2 2.400(9) . ?
Gd1 O6 2.410(9) . ?
Gd1 O21 2.426(10) . ?
Gd1 O8 2.425(9) . ?
Gd1 O11 2.427(9) . ?
Gd1 O4 2.438(9) . ?
Gd1 O20 2.512(10) . ?
Cu1 N10 1.890(12) . ?
Cu1 O1 1.928(10) . ?
Cu1 O2 1.947(9) . ?
Cu1 N9 2.009(11) . ?
Cu2 N2 1.916(11) . ?
Cu2 O3 1.933(9) . ?
Cu2 O4 1.982(9) . ?
Cu2 N1 2.003(11) . ?
Cu2 O14 2.311(10) . ?
Cu3 O6 1.922(9) . ?
Cu3 N4 1.929(11) . ?
Cu3 O5 1.968(9) . ?
Cu3 N3 1.996(11) . ?
Cu3 O12 2.336(9) . ?
Cu4 N6 1.907(11) . ?
Cu4 O8 1.932(9) . ?
Cu4 O7 1.947(9) . ?
Cu4 N5 2.041(11) . ?
Cu5 N8 1.899(11) . ?
Cu5 O10 1.944(9) . ?
Cu5 O9 1.949(9) . ?
Cu5 N7 1.999(11) . ?
Cu5 O13 2.362(9) . ?
O1 C2 1.297(17) . ?
O2 N2 1.391(14) . ?
O3 C4 1.303(16) . ?
O4 N4 1.399(13) . ?
O5 C6 1.294(16) . ?
O6 N6 1.392(14) . ?
O7 C8 1.282(16) . ?
O8 N8 1.404(14) . ?
O9 C10 1.297(17) . ?
O10 N10 1.408(14) . ?
O11 H11B 0.8500 . ?
O11 H11C 0.8502 . ?
O12 H12E 0.8500 . ?
O12 H12F 0.8499 . ?
O13 H13B 0.8501 . ?
O13 H13C 0.8500 . ?
O14 H14B 0.8500 . ?
O14 H14C 0.8500 . ?
O15 H15B 0.8500 . ?
O15 H15C 0.8501 . ?
O16 H16C 0.8500 . ?
O16 H16D 0.8500 . ?
O17 H17C 0.8499 . ?
O17 H17D 0.8500 . ?
O18 H18C 0.8501 . ?
O18 H18D 0.8501 . ?
O19 H19C 0.8499 . ?
O19 H19D 0.8500 . ?
O20 C11 1.240(16) . ?
O21 C11 1.233(17) . ?
O22 N11 1.263(17) . ?
O23 N11 1.210(18) . ?
O24 N11 1.200(17) . ?
O25 N12 1.291(17) . ?
O26 N12 1.213(16) . ?
O27 N12 1.230(16) . ?
C1 C2 1.472(19) . ?
C1 N1 1.506(18) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.281(18) . ?
C3 N3 1.478(18) . ?
C3 C4 1.497(18) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.265(17) . ?
C5 N5 1.491(17) . ?
C5 C6 1.536(19) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N6 1.300(16) . ?
C7 N7 1.506(17) . ?
C7 C8 1.520(18) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N8 1.295(17) . ?
C9 C10 1.473(19) . ?
C9 N9 1.492(18) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N10 1.284(18) . ?
C11 C12 1.50(2) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N5 H5C 0.8900 . ?
N5 H5D 0.8900 . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
N9 H9C 0.8900 . ?
N9 H9D 0.8900 . ?

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
O10 Gd1 O2 73.2(3) . . ?
O10 Gd1 O6 134.0(3) . . ?
O2 Gd1 O6 140.3(3) . . ?
O10 Gd1 O21 80.3(3) . . ?
O2 Gd1 O21 77.5(3) . . ?
O6 Gd1 O21 128.0(3) . . ?
O10 Gd1 O8 70.5(3) . . ?
O2 Gd1 O8 143.7(3) . . ?
O6 Gd1 O8 70.9(3) . . ?
O21 Gd1 O8 96.3(4) . . ?
O10 Gd1 O11 84.1(3) . . ?
O2 Gd1 O11 79.4(3) . . ?
O6 Gd1 O11 76.5(3) . . ?
O21 Gd1 O11 155.1(3) . . ?
O8 Gd1 O11 96.8(3) . . ?
O10 Gd1 O4 146.6(3) . . ?
O2 Gd1 O4 74.3(3) . . ?
O6 Gd1 O4 71.5(3) . . ?
O21 Gd1 O4 100.1(4) . . ?
O8 Gd1 O4 141.5(3) . . ?
O11 Gd1 O4 82.4(3) . . ?
O10 Gd1 O20 115.4(3) . . ?
O2 Gd1 O20 121.9(3) . . ?
O6 Gd1 O20 77.1(3) . . ?
O21 Gd1 O20 51.1(3) . . ?
O8 Gd1 O20 75.2(3) . . ?
O11 Gd1 O20 153.6(3) . . ?
O4 Gd1 O20 88.5(3) . . ?
N10 Cu1 O1 173.1(5) . . ?
N10 Cu1 O2 91.8(4) . . ?
O1 Cu1 O2 84.6(4) . . ?
N10 Cu1 N9 82.4(5) . . ?
O1 Cu1 N9 100.6(4) . . ?
O2 Cu1 N9 172.1(4) . . ?
N2 Cu2 O3 158.2(4) . . ?
N2 Cu2 O4 93.2(4) . . ?
O3 Cu2 O4 84.6(4) . . ?
N2 Cu2 N1 83.1(5) . . ?
O3 Cu2 N1 95.5(4) . . ?
O4 Cu2 N1 170.3(5) . . ?
N2 Cu2 O14 105.1(4) . . ?
O3 Cu2 O14 96.8(4) . . ?
O4 Cu2 O14 96.0(4) . . ?
N1 Cu2 O14 93.6(4) . . ?
O6 Cu3 N4 90.1(4) . . ?
O6 Cu3 O5 85.0(4) . . ?
N4 Cu3 O5 167.7(4) . . ?
O6 Cu3 N3 170.4(4) . . ?
N4 Cu3 N3 82.5(5) . . ?
O5 Cu3 N3 100.9(4) . . ?
O6 Cu3 O12 90.6(4) . . ?
N4 Cu3 O12 93.0(4) . . ?
O5 Cu3 O12 98.3(3) . . ?
N3 Cu3 O12 96.0(4) . . ?
N6 Cu4 O8 88.5(4) . . ?
N6 Cu4 O7 169.1(4) . . ?
O8 Cu4 O7 84.2(4) . . ?
N6 Cu4 N5 82.8(4) . . ?
O8 Cu4 N5 169.1(4) . . ?
O7 Cu4 N5 103.4(4) . . ?
N8 Cu5 O10 89.0(4) . . ?
N8 Cu5 O9 167.9(4) . . ?
O10 Cu5 O9 85.2(4) . . ?
N8 Cu5 N7 83.0(5) . . ?
O10 Cu5 N7 167.0(4) . . ?
O9 Cu5 N7 100.7(4) . . ?
N8 Cu5 O13 91.3(4) . . ?
O10 Cu5 O13 98.0(4) . . ?
O9 Cu5 O13 99.9(4) . . ?
N7 Cu5 O13 92.4(4) . . ?
C2 O1 Cu1 108.2(8) . . ?
N2 O2 Cu1 107.3(7) . . ?
N2 O2 Gd1 125.8(7) . . ?
Cu1 O2 Gd1 124.0(4) . . ?
C4 O3 Cu2 106.9(8) . . ?
N4 O4 Cu2 105.7(7) . . ?
N4 O4 Gd1 123.1(7) . . ?
Cu2 O4 Gd1 122.7(4) . . ?
C6 O5 Cu3 106.0(8) . . ?
N6 O6 Cu3 108.9(7) . . ?
N6 O6 Gd1 124.7(7) . . ?
Cu3 O6 Gd1 126.4(4) . . ?
C8 O7 Cu4 107.9(8) . . ?
N8 O8 Cu4 109.3(7) . . ?
N8 O8 Gd1 122.3(7) . . ?
Cu4 O8 Gd1 126.5(4) . . ?
C10 O9 Cu5 107.0(8) . . ?
N10 O10 Cu5 107.5(7) . . ?
N10 O10 Gd1 124.6(7) . . ?
Cu5 O10 Gd1 126.1(4) . . ?
Gd1 O11 H11B 107.3 . . ?
Gd1 O11 H11C 107.1 . . ?
H11B O11 H11C 106.9 . . ?
Cu3 O12 H12E 110.8 . . ?
Cu3 O12 H12F 111.0 . . ?
H12E O12 H12F 109.0 . . ?
Cu5 O13 H13B 104.4 . . ?
Cu5 O13 H13C 105.0 . . ?
H13B O13 H13C 105.8 . . ?
Cu2 O14 H14B 109.5 . . ?
Cu2 O14 H14C 109.5 . . ?
H14B O14 H14C 108.2 . . ?
H15B O15 H15C 107.4 . . ?
H16C O16 H16D 108.3 . . ?
H17C O17 H17D 108.8 . . ?
H18C O18 H18D 108.6 . . ?
H19C O19 H19D 108.6 . . ?
C11 O20 Gd1 92.3(9) . . ?
C11 O21 Gd1 96.7(8) . . ?
C2 C1 N1 111.0(11) . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
N1 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 O1 123.1(13) . . ?
N2 C2 C1 115.8(13) . . ?
O1 C2 C1 121.0(13) . . ?
N3 C3 C4 111.0(11) . . ?
N3 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
N3 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N4 C4 O3 124.5(12) . . ?
N4 C4 C3 115.6(12) . . ?
O3 C4 C3 119.8(12) . . ?
N5 C5 C6 109.5(10) . . ?
N5 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N5 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
O5 C6 N6 124.7(12) . . ?
O5 C6 C5 119.6(11) . . ?
N6 C6 C5 115.3(12) . . ?
N7 C7 C8 110.0(11) . . ?
N7 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
N7 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
O7 C8 N8 124.9(12) . . ?
O7 C8 C7 121.4(12) . . ?
N8 C8 C7 113.8(11) . . ?
C10 C9 N9 112.2(12) . . ?
C10 C9 H9A 109.2 . . ?
N9 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
N9 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
N10 C10 O9 124.7(13) . . ?
N10 C10 C9 114.1(13) . . ?
O9 C10 C9 121.2(12) . . ?
O21 C11 O20 119.1(13) . . ?
O21 C11 C12 118.4(12) . . ?
O20 C11 C12 122.5(13) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 N1 Cu2 109.6(8) . . ?
C1 N1 H1C 109.7 . . ?
Cu2 N1 H1C 109.7 . . ?
C1 N1 H1D 109.7 . . ?
Cu2 N1 H1D 109.7 . . ?
H1C N1 H1D 108.2 . . ?
C2 N2 O2 116.1(11) . . ?
C2 N2 Cu2 118.8(10) . . ?
O2 N2 Cu2 124.0(8) . . ?
C3 N3 Cu3 109.1(8) . . ?
C3 N3 H3C 109.9 . . ?
Cu3 N3 H3C 109.9 . . ?
C3 N3 H3D 109.9 . . ?
Cu3 N3 H3D 109.9 . . ?
H3C N3 H3D 108.3 . . ?
C4 N4 O4 116.6(11) . . ?
C4 N4 Cu3 118.0(9) . . ?
O4 N4 Cu3 124.6(8) . . ?
C5 N5 Cu4 110.1(8) . . ?
C5 N5 H5C 109.6 . . ?
Cu4 N5 H5C 109.6 . . ?
C5 N5 H5D 109.6 . . ?
Cu4 N5 H5D 109.6 . . ?
H5C N5 H5D 108.1 . . ?
C6 N6 O6 114.7(10) . . ?
C6 N6 Cu4 119.7(9) . . ?
O6 N6 Cu4 125.6(8) . . ?
C7 N7 Cu5 110.7(8) . . ?
C7 N7 H7C 109.5 . . ?
Cu5 N7 H7C 109.5 . . ?
C7 N7 H7D 109.5 . . ?
Cu5 N7 H7D 109.5 . . ?
H7C N7 H7D 108.1 . . ?
C8 N8 O8 113.6(10) . . ?
C8 N8 Cu5 120.9(9) . . ?
O8 N8 Cu5 124.8(8) . . ?
C9 N9 Cu1 108.3(8) . . ?
C9 N9 H9C 110.0 . . ?
Cu1 N9 H9C 110.0 . . ?
C9 N9 H9D 110.0 . . ?
Cu1 N9 H9D 110.0 . . ?
H9C N9 H9D 108.4 . . ?
C10 N10 O10 115.4(11) . . ?
C10 N10 Cu1 120.0(10) . . ?
O10 N10 Cu1 124.0(8) . . ?
O24 N11 O23 121.6(15) . . ?
O24 N11 O22 120.9(14) . . ?
O23 N11 O22 117.3(14) . . ?
O26 N12 O27 124.1(14) . . ?
O26 N12 O25 118.7(13) . . ?
O27 N12 O25 117.0(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C2 N2 -4.5(16) . . . . ?
Cu1 O1 C2 C1 173.0(11) . . . . ?
N1 C1 C2 N2 14.6(18) . . . . ?
N1 C1 C2 O1 -163.1(12) . . . . ?
Cu2 O3 C4 N4 -10.8(16) . . . . ?
Cu2 O3 C4 C3 168.3(10) . . . . ?
N3 C3 C4 N4 -7.9(17) . . . . ?
N3 C3 C4 O3 172.9(11) . . . . ?
Cu3 O5 C6 N6 9.2(15) . . . . ?
Cu3 O5 C6 C5 -178.4(10) . . . . ?
N5 C5 C6 O5 174.8(11) . . . . ?
N5 C5 C6 N6 -12.0(16) . . . . ?
Cu4 O7 C8 N8 -1.5(16) . . . . ?
Cu4 O7 C8 C7 179.3(10) . . . . ?
N7 C7 C8 O7 -167.9(12) . . . . ?
N7 C7 C8 N8 12.9(16) . . . . ?
Cu5 O9 C10 N10 3.6(17) . . . . ?
Cu5 O9 C10 C9 -175.8(11) . . . . ?
N9 C9 C10 N10 4.9(18) . . . . ?
N9 C9 C10 O9 -175.6(12) . . . . ?
Gd1 O21 C11 O20 9.2(15) . . . . ?
Gd1 O21 C11 C12 -166.9(12) . . . . ?
Gd1 O20 C11 O21 -8.8(15) . . . . ?
Gd1 O20 C11 C12 167.1(13) . . . . ?
C2 C1 N1 Cu2 -11.2(15) . . . . ?
O1 C2 N2 O2 -2.2(19) . . . . ?
C1 C2 N2 O2 -179.8(11) . . . . ?
O1 C2 N2 Cu2 166.5(10) . . . . ?
C1 C2 N2 Cu2 -11.1(17) . . . . ?
Cu1 O2 N2 C2 7.4(13) . . . . ?
Gd1 O2 N2 C2 168.8(9) . . . . ?
Cu1 O2 N2 Cu2 -160.6(6) . . . . ?
Gd1 O2 N2 Cu2 0.8(13) . . . . ?
C4 C3 N3 Cu3 18.1(13) . . . . ?
O3 C4 N4 O4 1.8(19) . . . . ?
C3 C4 N4 O4 -177.4(11) . . . . ?
O3 C4 N4 Cu3 171.7(10) . . . . ?
C3 C4 N4 Cu3 -7.5(16) . . . . ?
Cu2 O4 N4 C4 8.1(13) . . . . ?
Gd1 O4 N4 C4 156.4(9) . . . . ?
Cu2 O4 N4 Cu3 -161.1(6) . . . . ?
Gd1 O4 N4 Cu3 -12.7(13) . . . . ?
C6 C5 N5 Cu4 16.6(13) . . . . ?
O5 C6 N6 O6 -6.4(18) . . . . ?
C5 C6 N6 O6 -179.2(10) . . . . ?
O5 C6 N6 Cu4 173.5(10) . . . . ?
C5 C6 N6 Cu4 0.7(16) . . . . ?
Cu3 O6 N6 C6 -0.4(13) . . . . ?
Gd1 O6 N6 C6 176.9(9) . . . . ?
Cu3 O6 N6 Cu4 179.8(6) . . . . ?
Gd1 O6 N6 Cu4 -3.0(13) . . . . ?
C8 C7 N7 Cu5 -13.0(13) . . . . ?
O7 C8 N8 O8 3.5(18) . . . . ?
C7 C8 N8 O8 -177.3(10) . . . . ?
O7 C8 N8 Cu5 173.9(10) . . . . ?
C7 C8 N8 Cu5 -6.8(15) . . . . ?
Cu4 O8 N8 C8 -3.5(12) . . . . ?
Gd1 O8 N8 C8 -168.6(8) . . . . ?
Cu4 O8 N8 Cu5 -173.5(6) . . . . ?
Gd1 O8 N8 Cu5 21.4(12) . . . . ?
O10 Cu5 N8 C8 -170.5(10) . . . . ?
O9 Cu5 N8 C8 -110(2) . . . . ?
N7 Cu5 N8 C8 -0.7(10) . . . . ?
O13 Cu5 N8 C8 91.5(10) . . . . ?
O10 Cu5 N8 O8 -1.2(9) . . . . ?
O9 Cu5 N8 O8 60(2) . . . . ?
N7 Cu5 N8 O8 168.6(10) . . . . ?
O13 Cu5 N8 O8 -99.2(9) . . . . ?
C10 C9 N9 Cu1 -14.9(14) . . . . ?
O9 C10 N10 O10 0(2) . . . . ?
C9 C10 N10 O10 179.9(11) . . . . ?
O9 C10 N10 Cu1 -170.3(10) . . . . ?
C9 C10 N10 Cu1 9.1(17) . . . . ?
Cu5 O10 N10 C10 -4.3(13) . . . . ?
Gd1 O10 N10 C10 -169.8(9) . . . . ?
Cu5 O10 N10 Cu1 166.0(6) . . . . ?
Gd1 O10 N10 Cu1 0.5(13) . . . . ?
O2 Cu1 N10 C10 160.1(11) . . . . ?
N9 Cu1 N10 C10 -14.6(11) . . . . ?
O2 Cu1 N10 O10 -9.9(10) . . . . ?
N9 Cu1 N10 O10 175.5(10) . . . . ?

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
N9 H9D O22 0.89 2.33 3.039(17) 136.9 .
N9 H9C O21 0.89 1.96 2.845(16) 173.8 2_665
N7 H7D O14 0.89 2.54 3.413(15) 167.5 1_545
N7 H7C O18 0.89 2.15 3.016(16) 162.6 2_656
N5 H5D O11 0.89 2.24 3.129(14) 174.1 2_766
N5 H5C O17 0.89 2.33 3.054(15) 138.1 .
N3 H3D O25 0.89 2.15 3.014(16) 162.8 1_665
N3 H3C N4 0.89 2.54 3.214(16) 132.7 2_776
N3 H3C O4 0.89 2.29 3.159(15) 164.3 2_776
N1 H1D O18 0.89 2.16 2.972(16) 150.8 2_766
N1 H1C O23 0.89 2.17 2.911(18) 140.9 1_565
N1 H1C O16 0.89 2.59 3.21(3) 127.6 2_676
C9 H9A N2 0.97 2.62 3.536(18) 157.0 2_665
C5 H5A N8 0.97 2.54 3.423(18) 150.9 2_766
C5 H5A O8 0.97 2.62 3.470(17) 145.8 2_766
C3 H3B O20 0.97 2.35 3.050(16) 128.9 2_776
C1 H1B O23 0.97 2.64 3.59(2) 164.6 2_765
C1 H1A O16 0.97 2.63 3.31(3) 126.7 2_676
O19 H19D N11 0.85 2.57 3.353(18) 153.6 .
O19 H19D O24 0.85 1.90 2.740(15) 172.2 .
O19 H19C O22 0.85 1.94 2.785(15) 171.9 2_765
O18 H18D O23 0.85 2.27 3.109(17) 169.8 1_556
O18 H18D O22 0.85 2.47 3.147(16) 137.4 1_556
O18 H18C N12 0.85 2.66 3.430(17) 151.4 .
O18 H18C O27 0.85 1.98 2.820(16) 169.0 .
O17 H17D O13 0.85 1.95 2.764(14) 159.3 2_666
O17 H17C O3 0.85 2.02 2.837(13) 159.8 2_776
O16 H16D O14 0.85 1.95 2.80(3) 176.6 2_676
O16 H16C O9 0.85 2.07 2.92(2) 176.0 2_666
O15 H15C O17 0.85 1.89 2.726(13) 165.9 .
O15 H15B O20 0.85 1.97 2.756(13) 154.2 .
O14 H14C O26 0.85 2.23 2.981(15) 146.7 2_666
O14 H14B O5 0.85 1.89 2.716(13) 165.4 2_776
O13 H13C O21 0.85 2.46 3.186(15) 143.8 .
O13 H13B O1 0.85 1.93 2.775(13) 170.6 2_665
O12 H12F N12 0.85 2.54 3.241(16) 140.0 2_766
O12 H12F O27 0.85 2.52 3.045(14) 121.3 2_766
O12 H12F O25 0.85 1.94 2.750(14) 160.0 2_766
O12 H12E O7 0.85 1.83 2.665(12) 166.8 2_766
O11 H11C O19 0.85 2.11 2.741(13) 130.6 .
O11 H11B O12 0.85 1.86 2.697(12) 170.4 .

_refine_diff_density_max         2.790
_refine_diff_density_min         -3.309
_refine_diff_density_rms         0.328


_exptl_crystal_preparation       'Magnetic properties,DNA interaction'
