# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_Dy2Co2
_audit_block_doi                 10.5517/cc14ht5m
_database_code_depnum_ccdc_archive 'CCDC 1057880'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H74 Co2 Dy2 N4 O24'
_chemical_formula_sum            'C78 H74 Co2 Dy2 N4 O24'
_chemical_formula_weight         1894.27

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.102(5)
_cell_length_b                   16.905(3)
_cell_length_c                   22.710(6)
_cell_angle_alpha                90
_cell_angle_beta                 120.960(11)
_cell_angle_gamma                90
_cell_volume                     7935(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2513
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      20.88

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_F_000             3792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.350
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22112
_diffrn_reflns_av_unetI/netI     0.1800
_diffrn_reflns_av_R_equivalents  0.1638
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.971
_diffrn_reflns_theta_max         25.110
_diffrn_reflns_theta_full        25.110
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7059
_reflns_number_gt                2841
_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.

 The command 'isor' was also used to restrain the C and O atom 
 with NPD and ADP problems. The restraint command lead to restraint number 278, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the h11a-o11 distance to
 be in the reasonable range

 The compounds show large solvent accessible void and the sovlents cannot be determined.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1137P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7059
_refine_ls_number_parameters     440
_refine_ls_number_restraints     278
_refine_ls_R_factor_all          0.2031
_refine_ls_R_factor_gt           0.0742
_refine_ls_wR_factor_ref         0.2495
_refine_ls_wR_factor_gt          0.1789
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_restrained_S_all      0.966
_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
C1 C 0.2234(9) 0.5213(12) 0.2942(10) 0.108(7) Uani 1 1 d . U . . .
H1A H 0.2394 0.5085 0.3415 0.162 Uiso 1 1 calc R U . . .
H1B H 0.1836 0.4935 0.2656 0.162 Uiso 1 1 calc R U . . .
H1C H 0.2159 0.5772 0.2875 0.162 Uiso 1 1 calc R U . . .
C2 C 0.3305(4) 0.5322(7) 0.3129(6) 0.074(5) Uani 1 1 d G U . . .
C3 C 0.3505(6) 0.5803(8) 0.3700(6) 0.112(7) Uani 1 1 d G U . . .
H3 H 0.3235 0.5884 0.3875 0.134 Uiso 1 1 calc R U . . .
C4 C 0.4110(7) 0.6163(7) 0.4010(6) 0.160(9) Uani 1 1 d G U . . .
H4 H 0.4244 0.6485 0.4392 0.192 Uiso 1 1 calc R U . . .
C5 C 0.4513(5) 0.6042(7) 0.3749(6) 0.114(7) Uani 1 1 d G U . . .
H5 H 0.4917 0.6283 0.3957 0.137 Uiso 1 1 calc R U . . .
C6 C 0.4313(5) 0.5561(7) 0.3178(6) 0.070(4) Uani 1 1 d G U . . .
C7 C 0.3708(5) 0.5201(6) 0.2868(5) 0.064(4) Uani 1 1 d G U . . .
C8 C 0.4772(7) 0.5456(9) 0.2949(8) 0.065(4) Uani 1 1 d . U . . .
H8 H 0.5093 0.5836 0.3072 0.078 Uiso 1 1 calc R U . . .
C9 C 0.1478(9) 0.2708(11) 0.0447(10) 0.104(6) Uani 1 1 d . U . . .
H9A H 0.1464 0.2426 0.0073 0.156 Uiso 1 1 calc R U . . .
H9B H 0.1216 0.3176 0.0275 0.156 Uiso 1 1 calc R U . . .
H9C H 0.1315 0.2377 0.0668 0.156 Uiso 1 1 calc R U . . .
C10 C 0.2598(4) 0.2454(6) 0.0963(5) 0.072(4) Uani 1 1 d G U . . .
C11 C 0.2464(4) 0.1793(7) 0.0546(5) 0.091(5) Uani 1 1 d G U . . .
H11 H 0.2037 0.1650 0.0239 0.109 Uiso 1 1 calc R U . . .
C12 C 0.2968(7) 0.1348(6) 0.0587(6) 0.105(6) Uani 1 1 d G U . . .
H12 H 0.2878 0.0906 0.0308 0.126 Uiso 1 1 calc R U . . .
C13 C 0.3605(5) 0.1562(7) 0.1045(6) 0.114(7) Uani 1 1 d G U . . .
H13 H 0.3942 0.1264 0.1073 0.137 Uiso 1 1 calc R U . . .
C14 C 0.3740(4) 0.2222(7) 0.1462(5) 0.069(4) Uani 1 1 d G U . . .
C15 C 0.3236(5) 0.2668(5) 0.1421(5) 0.060(4) Uani 1 1 d G U . . .
C16 C 0.4421(7) 0.2417(9) 0.1909(7) 0.061(4) Uani 1 1 d . U . . .
H16 H 0.4715 0.2046 0.1929 0.073 Uiso 1 1 calc R U . . .
C17 C 0.1532(7) 0.5149(11) 0.0729(8) 0.066(4) Uani 1 1 d . U . . .
C18 C 0.1039(6) 0.5706(8) 0.0209(6) 0.077(5) Uani 1 1 d G U . . .
C19 C 0.0449(7) 0.5406(6) -0.0304(7) 0.124(7) Uani 1 1 d G U . . .
H19 H 0.0365 0.4867 -0.0323 0.148 Uiso 1 1 calc R U . . .
C20 C -0.0017(5) 0.5912(9) -0.0789(6) 0.119(7) Uani 1 1 d G U . . .
H20 H -0.0411 0.5712 -0.1132 0.143 Uiso 1 1 calc R U . . .
C21 C 0.0108(6) 0.6719(9) -0.0761(7) 0.125(8) Uani 1 1 d G U . . .
H21 H -0.0203 0.7057 -0.1085 0.150 Uiso 1 1 calc R U . . .
C22 C 0.0698(8) 0.7018(6) -0.0248(8) 0.145(9) Uani 1 1 d G U . . .
H22 H 0.0782 0.7558 -0.0229 0.174 Uiso 1 1 calc R U . . .
C23 C 0.1164(6) 0.6512(8) 0.0237(6) 0.109(7) Uani 1 1 d G U . . .
H23 H 0.1559 0.6713 0.0580 0.131 Uiso 1 1 calc R U . . .
C24 C 0.1998(9) 0.3242(10) 0.2317(9) 0.073(5) Uani 1 1 d . U . . .
C25 C 0.1728(6) 0.2794(7) 0.2670(5) 0.072(4) Uani 1 1 d G U . . .
C26 C 0.1187(6) 0.3072(6) 0.2674(6) 0.104(6) Uani 1 1 d G U . . .
H26 H 0.0977 0.3526 0.2429 0.125 Uiso 1 1 calc R U . . .
C27 C 0.0962(5) 0.2672(8) 0.3045(7) 0.111(7) Uani 1 1 d G U . . .
H27 H 0.0600 0.2858 0.3048 0.134 Uiso 1 1 calc R U . . .
C28 C 0.1277(6) 0.1994(8) 0.3411(6) 0.101(6) Uani 1 1 d G U . . .
H28 H 0.1126 0.1726 0.3659 0.122 Uiso 1 1 calc R U . . .
C29 C 0.1818(6) 0.1716(6) 0.3407(6) 0.096(6) Uani 1 1 d G U . . .
H29 H 0.2028 0.1262 0.3652 0.115 Uiso 1 1 calc R U . . .
C30 C 0.2043(5) 0.2116(7) 0.3036(6) 0.081(5) Uani 1 1 d G U . . .
H30 H 0.2405 0.1930 0.3033 0.097 Uiso 1 1 calc R U . . .
C31 C 0.3307(7) 0.4703(8) 0.0874(7) 0.049(3) Uani 1 1 d . U . . .
C32 C 0.3248(5) 0.5247(6) 0.0334(5) 0.060(4) Uani 1 1 d G U . . .
C33 C 0.3747(4) 0.5302(6) 0.0197(6) 0.088(5) Uani 1 1 d G U . . .
H33 H 0.4109 0.4979 0.0429 0.106 Uiso 1 1 calc R U . . .
C34 C 0.3704(5) 0.5841(8) -0.0287(6) 0.107(6) Uani 1 1 d G U . . .
H34 H 0.4038 0.5879 -0.0378 0.128 Uiso 1 1 calc R U . . .
C35 C 0.3163(6) 0.6325(7) -0.0634(6) 0.107(6) Uani 1 1 d G U . . .
H35 H 0.3135 0.6685 -0.0958 0.129 Uiso 1 1 calc R U . . .
C36 C 0.2664(5) 0.6269(6) -0.0497(6) 0.096(6) Uani 1 1 d G U . . .
H36 H 0.2302 0.6592 -0.0730 0.116 Uiso 1 1 calc R U . . .
C37 C 0.2707(5) 0.5730(7) -0.0014(6) 0.075(5) Uani 1 1 d G U . . .
H37 H 0.2374 0.5693 0.0078 0.090 Uiso 1 1 calc R U . . .
C38 C 0.4961(9) 0.3627(11) 0.3944(9) 0.097(6) Uani 1 1 d . U . . .
H38A H 0.5093 0.3103 0.4128 0.146 Uiso 1 1 calc R U . . .
H38B H 0.4866 0.3929 0.4239 0.146 Uiso 1 1 calc R U . . .
H38C H 0.5303 0.3879 0.3915 0.146 Uiso 1 1 calc R U . . .
C39 C 0.3871(14) 0.1775(14) 0.3232(14) 0.165(10) Uani 1 1 d . U . . .
H39A H 0.4320 0.1796 0.3367 0.247 Uiso 1 1 calc R U . . .
H39B H 0.3614 0.1666 0.2749 0.247 Uiso 1 1 calc R U . . .
H39C H 0.3808 0.1364 0.3483 0.247 Uiso 1 1 calc R U . . .
Co1 Co 0.41106(8) 0.39800(11) 0.22396(9) 0.0531(6) Uani 1 1 d . . . . .
Dy1 Dy 0.24900(3) 0.41574(5) 0.16478(4) 0.0678(3) Uani 1 1 d . . . . .
N1 N 0.4658(5) 0.3022(6) 0.2269(5) 0.055(3) Uani 1 1 d . . . . .
N2 N 0.4758(5) 0.4882(7) 0.2595(6) 0.058(3) Uani 1 1 d . . . . .
O1 O 0.2700(5) 0.4982(6) 0.2763(6) 0.079(3) Uani 1 1 d . U . . .
O2 O 0.3502(4) 0.4693(6) 0.2355(4) 0.058(2) Uani 1 1 d . . . . .
O3 O 0.2141(5) 0.2931(7) 0.0939(6) 0.090(3) Uani 1 1 d . U . . .
O4 O 0.3325(4) 0.3282(6) 0.1819(4) 0.059(3) Uani 1 1 d . . . . .
O5 O 0.1507(5) 0.4440(7) 0.0595(5) 0.079(3) Uani 1 1 d . U . . .
O6 O 0.1971(5) 0.5446(7) 0.1302(6) 0.078(3) Uani 1 1 d . U . . .
O7 O 0.2559(5) 0.3142(6) 0.2443(6) 0.081(3) Uani 1 1 d . U . . .
O8 O 0.1652(5) 0.3772(7) 0.1883(6) 0.088(3) Uani 1 1 d . U . . .
O9 O 0.2801(4) 0.4618(6) 0.0888(4) 0.064(3) Uani 1 1 d . . . . .
O10 O 0.3837(4) 0.4397(5) 0.1258(5) 0.059(3) Uani 1 1 d . . . . .
O11 O 0.4394(5) 0.3580(7) 0.3272(5) 0.083(3) Uani 1 1 d D . . . .
H11A H 0.4156 0.3229 0.3266 0.125 Uiso 1 1 calc DR U . . .
O12 O 0.3684(7) 0.2506(9) 0.3372(7) 0.118(4) Uani 1 1 d . U . . .
H12A H 0.3291 0.2557 0.3128 0.177 Uiso 1 1 calc R 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
C1 O1 1.431(17) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.378(13) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.458(17) . ?
C7 O2 1.321(11) . ?
C8 N2 1.249(16) . ?
C8 H8 0.9300 . ?
C9 O3 1.452(19) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.346(14) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C16 1.455(15) . ?
C15 O4 1.319(11) . ?
C16 N1 1.248(16) . ?
C16 H16 0.9300 . ?
C17 O5 1.230(17) . ?
C17 O6 1.284(18) . ?
C17 C18 1.500(18) . ?
C17 Dy1 2.746(16) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O7 1.242(18) . ?
C24 O8 1.274(18) . ?
C24 C25 1.474(17) . ?
C24 Dy1 2.823(16) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O10 1.229(15) . ?
C31 O9 1.247(15) . ?
C31 C32 1.480(15) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 O11 1.434(18) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 O12 1.41(2) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
Co1 O4 2.008(9) . ?
Co1 O2 2.017(9) . ?
Co1 N2 2.029(12) . ?
Co1 N1 2.069(11) . ?
Co1 O10 2.095(9) . ?
Co1 O11 2.185(10) . ?
Co1 Dy1 3.428(2) . ?
Dy1 O2 2.307(9) . ?
Dy1 O9 2.339(9) . ?
Dy1 O4 2.363(9) . ?
Dy1 O5 2.393(10) . ?
Dy1 O8 2.429(10) . ?
Dy1 O6 2.433(11) . ?
Dy1 O7 2.433(10) . ?
Dy1 O3 2.490(12) . ?
Dy1 O1 2.701(11) . ?
N1 N1 1.43(2) 2_655 ?
N2 N2 1.44(2) 2_655 ?
O11 H11A 0.8200 . ?
O12 H12A 0.8200 . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.0(9) . . ?
O1 C2 C7 115.9(9) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C8 123.8(10) . . ?
C5 C6 C8 116.2(10) . . ?
O2 C7 C6 123.5(9) . . ?
O2 C7 C2 116.3(9) . . ?
C6 C7 C2 120.0 . . ?
N2 C8 C6 123.4(13) . . ?
N2 C8 H8 118.3 . . ?
C6 C8 H8 118.3 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 123.8(9) . . ?
O3 C10 C15 116.2(9) . . ?
C11 C10 C15 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 C16 123.8(10) . . ?
C13 C14 C16 116.1(10) . . ?
O4 C15 C14 123.5(9) . . ?
O4 C15 C10 116.4(9) . . ?
C14 C15 C10 120.0 . . ?
N1 C16 C14 127.9(14) . . ?
N1 C16 H16 116.1 . . ?
C14 C16 H16 116.1 . . ?
O5 C17 O6 122.8(15) . . ?
O5 C17 C18 120.0(15) . . ?
O6 C17 C18 117.3(15) . . ?
O5 C17 Dy1 60.5(8) . . ?
O6 C17 Dy1 62.4(8) . . ?
C18 C17 Dy1 176.1(10) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 119.0(12) . . ?
C23 C18 C17 121.0(12) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O7 C24 O8 118.3(15) . . ?
O7 C24 C25 122.6(16) . . ?
O8 C24 C25 119.1(15) . . ?
O7 C24 Dy1 59.2(8) . . ?
O8 C24 Dy1 59.1(8) . . ?
C25 C24 Dy1 177.6(12) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 120.5(11) . . ?
C30 C25 C24 119.4(11) . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 120.0 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O10 C31 O9 127.3(13) . . ?
O10 C31 C32 118.2(12) . . ?
O9 C31 C32 114.5(12) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 120.1(9) . . ?
C37 C32 C31 119.9(9) . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C37 120.0 . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O11 C38 H38A 109.5 . . ?
O11 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O11 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O12 C39 H39A 109.5 . . ?
O12 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O12 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O4 Co1 O2 80.9(4) . . ?
O4 Co1 N2 167.3(4) . . ?
O2 Co1 N2 87.7(4) . . ?
O4 Co1 N1 89.1(4) . . ?
O2 Co1 N1 163.4(4) . . ?
N2 Co1 N1 103.2(4) . . ?
O4 Co1 O10 89.3(4) . . ?
O2 Co1 O10 94.9(4) . . ?
N2 Co1 O10 85.8(4) . . ?
N1 Co1 O10 98.3(4) . . ?
O4 Co1 O11 91.5(4) . . ?
O2 Co1 O11 83.8(4) . . ?
N2 Co1 O11 93.1(4) . . ?
N1 Co1 O11 83.2(4) . . ?
O10 Co1 O11 178.3(4) . . ?
O4 Co1 Dy1 42.2(3) . . ?
O2 Co1 Dy1 40.6(3) . . ?
N2 Co1 Dy1 125.3(3) . . ?
N1 Co1 Dy1 131.3(3) . . ?
O10 Co1 Dy1 83.2(2) . . ?
O11 Co1 Dy1 96.4(3) . . ?
O2 Dy1 O9 76.0(3) . . ?
O2 Dy1 O4 68.0(3) . . ?
O9 Dy1 O4 76.2(3) . . ?
O2 Dy1 O5 140.0(4) . . ?
O9 Dy1 O5 74.0(3) . . ?
O4 Dy1 O5 127.6(4) . . ?
O2 Dy1 O8 130.8(4) . . ?
O9 Dy1 O8 150.4(4) . . ?
O4 Dy1 O8 121.9(4) . . ?
O5 Dy1 O8 76.5(4) . . ?
O2 Dy1 O6 93.3(3) . . ?
O9 Dy1 O6 76.7(3) . . ?
O4 Dy1 O6 150.1(3) . . ?
O5 Dy1 O6 54.4(4) . . ?
O8 Dy1 O6 88.0(4) . . ?
O2 Dy1 O7 96.7(3) . . ?
O9 Dy1 O7 148.9(4) . . ?
O4 Dy1 O7 73.0(3) . . ?
O5 Dy1 O7 122.5(4) . . ?
O8 Dy1 O7 52.8(4) . . ?
O6 Dy1 O7 134.3(4) . . ?
O2 Dy1 O3 131.4(4) . . ?
O9 Dy1 O3 86.0(3) . . ?
O4 Dy1 O3 64.0(3) . . ?
O5 Dy1 O3 71.9(4) . . ?
O8 Dy1 O3 82.8(4) . . ?
O6 Dy1 O3 126.2(4) . . ?
O7 Dy1 O3 76.3(4) . . ?
O2 Dy1 O1 61.6(3) . . ?
O9 Dy1 O1 122.9(3) . . ?
O4 Dy1 O1 115.8(3) . . ?
O5 Dy1 O1 116.5(4) . . ?
O8 Dy1 O1 73.0(4) . . ?
O6 Dy1 O1 70.0(3) . . ?
O7 Dy1 O1 76.1(4) . . ?
O3 Dy1 O1 150.9(3) . . ?
O2 Dy1 C17 117.6(4) . . ?
O9 Dy1 C17 72.5(4) . . ?
O4 Dy1 C17 145.0(4) . . ?
O5 Dy1 C17 26.6(4) . . ?
O8 Dy1 C17 82.1(4) . . ?
O6 Dy1 C17 27.9(4) . . ?
O7 Dy1 C17 134.8(4) . . ?
O3 Dy1 C17 98.3(5) . . ?
O1 Dy1 C17 94.4(4) . . ?
O2 Dy1 C24 115.3(4) . . ?
O9 Dy1 C24 164.2(4) . . ?
O4 Dy1 C24 97.2(4) . . ?
O5 Dy1 C24 100.0(4) . . ?
O8 Dy1 C24 26.8(4) . . ?
O6 Dy1 C24 112.1(4) . . ?
O7 Dy1 C24 26.0(4) . . ?
O3 Dy1 C24 78.2(4) . . ?
O1 Dy1 C24 72.9(4) . . ?
C17 Dy1 C24 108.8(5) . . ?
O2 Dy1 Co1 34.7(2) . . ?
O9 Dy1 Co1 65.5(2) . . ?
O4 Dy1 Co1 34.8(2) . . ?
O5 Dy1 Co1 138.7(3) . . ?
O8 Dy1 Co1 143.0(3) . . ?
O6 Dy1 Co1 119.8(2) . . ?
O7 Dy1 Co1 91.0(3) . . ?
O3 Dy1 Co1 96.8(3) . . ?
O1 Dy1 Co1 92.9(2) . . ?
C17 Dy1 Co1 134.0(3) . . ?
C24 Dy1 Co1 116.8(4) . . ?
C16 N1 N1 116.6(10) . 2_655 ?
C16 N1 Co1 123.4(10) . . ?
N1 N1 Co1 120.0(5) 2_655 . ?
C8 N2 N2 115.8(10) . 2_655 ?
C8 N2 Co1 126.9(10) . . ?
N2 N2 Co1 117.3(6) 2_655 . ?
C2 O1 C1 117.2(12) . . ?
C2 O1 Dy1 114.2(8) . . ?
C1 O1 Dy1 127.7(10) . . ?
C7 O2 Co1 122.3(7) . . ?
C7 O2 Dy1 130.7(7) . . ?
Co1 O2 Dy1 104.7(4) . . ?
C10 O3 C9 115.5(12) . . ?
C10 O3 Dy1 118.4(8) . . ?
C9 O3 Dy1 125.8(11) . . ?
C15 O4 Co1 124.6(7) . . ?
C15 O4 Dy1 123.8(7) . . ?
Co1 O4 Dy1 103.0(4) . . ?
C17 O5 Dy1 92.9(10) . . ?
C17 O6 Dy1 89.7(10) . . ?
C24 O7 Dy1 94.8(10) . . ?
C24 O8 Dy1 94.1(10) . . ?
C31 O9 Dy1 138.4(9) . . ?
C31 O10 Co1 122.7(9) . . ?
C38 O11 Co1 136.5(10) . . ?
C38 O11 H11A 109.5 . . ?
Co1 O11 H11A 112.1 . . ?
C39 O12 H12A 109.5 . . ?

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
O1 C2 C3 C4 -175.7(12) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C8 -178.8(11) . . . . ?
C5 C6 C7 O2 -175.1(11) . . . . ?
C8 C6 C7 O2 3.7(13) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C8 C6 C7 C2 178.7(12) . . . . ?
O1 C2 C7 O2 -8.5(11) . . . . ?
C3 C2 C7 O2 175.4(10) . . . . ?
O1 C2 C7 C6 176.1(11) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C7 C6 C8 N2 -21(2) . . . . ?
C5 C6 C8 N2 157.7(12) . . . . ?
O3 C10 C11 C12 177.8(11) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C16 -178.0(10) . . . . ?
C13 C14 C15 O4 177.0(10) . . . . ?
C16 C14 C15 O4 -5.1(12) . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C16 C14 C15 C10 177.8(11) . . . . ?
O3 C10 C15 O4 4.8(10) . . . . ?
C11 C10 C15 O4 -177.2(9) . . . . ?
O3 C10 C15 C14 -177.9(10) . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C15 C14 C16 N1 -6.6(19) . . . . ?
C13 C14 C16 N1 171.3(12) . . . . ?
O5 C17 C18 C19 21.9(18) . . . . ?
O6 C17 C18 C19 -158.7(11) . . . . ?
O5 C17 C18 C23 -158.5(12) . . . . ?
O6 C17 C18 C23 20.9(17) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 179.6(12) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C17 C18 C23 C22 -179.6(12) . . . . ?
O7 C24 C25 C26 160.6(13) . . . . ?
O8 C24 C25 C26 -16.9(19) . . . . ?
O7 C24 C25 C30 -15(2) . . . . ?
O8 C24 C25 C30 167.2(12) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 -175.9(12) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 175.9(12) . . . . ?
O10 C31 C32 C33 10.5(16) . . . . ?
O9 C31 C32 C33 -170.6(9) . . . . ?
O10 C31 C32 C37 -166.4(10) . . . . ?
O9 C31 C32 C37 12.6(15) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C34 -176.8(10) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C31 C32 C37 C36 176.8(10) . . . . ?
C14 C16 N1 N1 172.0(13) . . . 2_655 ?
C14 C16 N1 Co1 -6(2) . . . . ?
C6 C8 N2 N2 179.0(12) . . . 2_655 ?
C6 C8 N2 Co1 1(2) . . . . ?
C3 C2 O1 C1 7.0(16) . . . . ?
C7 C2 O1 C1 -168.8(11) . . . . ?
C3 C2 O1 Dy1 176.8(6) . . . . ?
C7 C2 O1 Dy1 0.9(10) . . . . ?
C6 C7 O2 Co1 30.2(12) . . . . ?
C2 C7 O2 Co1 -145.1(6) . . . . ?
C6 C7 O2 Dy1 -169.7(6) . . . . ?
C2 C7 O2 Dy1 15.0(12) . . . . ?
C11 C10 O3 C9 0.8(16) . . . . ?
C15 C10 O3 C9 178.7(10) . . . . ?
C11 C10 O3 Dy1 -173.9(5) . . . . ?
C15 C10 O3 Dy1 4.0(11) . . . . ?
C14 C15 O4 Co1 28.2(12) . . . . ?
C10 C15 O4 Co1 -154.6(6) . . . . ?
C14 C15 O4 Dy1 170.4(5) . . . . ?
C10 C15 O4 Dy1 -12.4(10) . . . . ?
O6 C17 O5 Dy1 -3.9(16) . . . . ?
C18 C17 O5 Dy1 175.5(12) . . . . ?
O5 C17 O6 Dy1 3.9(16) . . . . ?
C18 C17 O6 Dy1 -175.6(11) . . . . ?
O8 C24 O7 Dy1 -0.6(17) . . . . ?
C25 C24 O7 Dy1 -178.1(13) . . . . ?
O7 C24 O8 Dy1 0.6(17) . . . . ?
C25 C24 O8 Dy1 178.2(12) . . . . ?
O10 C31 O9 Dy1 16(2) . . . . ?
C32 C31 O9 Dy1 -162.6(9) . . . . ?
O9 C31 O10 Co1 -22(2) . . . . ?
C32 C31 O10 Co1 156.3(8) . . . . ?

_refine_diff_density_max         0.981
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.143

####################################################################### 
# 
# 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_Dy2Cu2
_audit_block_doi                 10.5517/cc14ht6n
_database_code_depnum_ccdc_archive 'CCDC 1057881'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C76 H70 Cu2 Dy2 N4 O26'
_chemical_formula_sum            'C76 H70 Cu2 Dy2 N4 O26'
_chemical_formula_weight         1915.44

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.592(6)
_cell_length_b                   16.697(4)
_cell_length_c                   23.137(8)
_cell_angle_alpha                90
_cell_angle_beta                 119.867(4)
_cell_angle_gamma                90
_cell_volume                     7904(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5551
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      23.97

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_F_000             3840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.482
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_T_max  0.594
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            21852
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.574
_diffrn_reflns_theta_max         25.045
_diffrn_reflns_theta_full        25.045
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6930
_reflns_number_gt                4240
_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.

 The command 'isor' was also used to restrain the all O and C atom with NPD and ADP
 problems. The restraint command lead to restraint number 304, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the O5-O12, O11-H11a, O11-C38 and H13-H16c distance to
 be in the reasonable range.

 In the final refinement, the compounds show large solvent accessible void 
 and the sovlents cannot be determined.
;

_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.1280P)²+112.7976P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6930
_refine_ls_number_parameters     443
_refine_ls_number_restraints     304
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0777
_refine_ls_wR_factor_ref         0.2580
_refine_ls_wR_factor_gt          0.2114
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.073
_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
C1 C 0.2834(4) 0.4757(9) 0.7119(5) 0.117(4) Uani 1 1 d . U . . .
H1A H 0.2900 0.4190 0.7184 0.176 Uiso 1 1 calc R U . . .
H1B H 0.3236 0.5030 0.7406 0.176 Uiso 1 1 calc R U . . .
H1C H 0.2694 0.4886 0.6663 0.176 Uiso 1 1 calc R U . . .
C2 C 0.1733(2) 0.4692(3) 0.6907(2) 0.081(3) Uani 1 1 d G U . . .
C3 C 0.1552(3) 0.4177(4) 0.6371(3) 0.123(4) Uani 1 1 d G U . . .
H3 H 0.1851 0.4045 0.6235 0.147 Uiso 1 1 calc R U . . .
C4 C 0.0924(3) 0.3861(5) 0.6037(4) 0.152(4) Uani 1 1 d G U . . .
H4 H 0.0803 0.3517 0.5678 0.182 Uiso 1 1 calc R U . . .
C5 C 0.0477(3) 0.4058(5) 0.6239(4) 0.116(4) Uani 1 1 d G U . . .
H5 H 0.0057 0.3846 0.6016 0.140 Uiso 1 1 calc R U . . .
C6 C 0.0658(2) 0.4572(4) 0.6776(3) 0.076(3) Uani 1 1 d G U . . .
C7 C 0.1286(3) 0.4889(3) 0.7110(3) 0.061(2) Uani 1 1 d G U . . .
C8 C 0.0198(4) 0.4696(5) 0.6997(4) 0.067(2) Uani 1 1 d . U . . .
H8 H -0.0161 0.4356 0.6831 0.080 Uiso 1 1 calc R U . . .
C9 C 0.0571(4) 0.7603(5) 0.8087(4) 0.070(2) Uani 1 1 d . U . . .
H9 H 0.0270 0.7987 0.8052 0.084 Uiso 1 1 calc R U . . .
C10 C 0.1261(2) 0.7781(3) 0.85521(19) 0.074(3) Uani 1 1 d G U . . .
C11 C 0.1390(3) 0.8453(3) 0.8954(3) 0.108(4) Uani 1 1 d G U . . .
H11 H 0.1047 0.8761 0.8922 0.130 Uiso 1 1 calc R U . . .
C12 C 0.2033(3) 0.8663(4) 0.9405(3) 0.111(4) Uani 1 1 d G U . . .
H12 H 0.2119 0.9112 0.9674 0.133 Uiso 1 1 calc R U . . .
C13 C 0.2545(2) 0.8202(4) 0.9454(3) 0.106(3) Uani 1 1 d G U . . .
H13 H 0.2975 0.8342 0.9755 0.128 Uiso 1 1 calc DR U . . .
C14 C 0.2415(2) 0.7530(4) 0.9052(3) 0.081(3) Uani 1 1 d G U . . .
C15 C 0.1773(2) 0.7320(3) 0.8601(2) 0.069(2) Uani 1 1 d G U . . .
C16 C 0.3536(5) 0.7255(6) 0.9538(6) 0.137(5) Uani 1 1 d . U . . .
H16A H 0.3607 0.7796 0.9449 0.206 Uiso 1 1 calc R U . . .
H16B H 0.3829 0.6904 0.9485 0.206 Uiso 1 1 calc R U . . .
H16C H 0.3615 0.7217 0.9987 0.206 Uiso 1 1 calc DR U . . .
C17 C 0.1693(3) 0.5227(5) 0.9151(4) 0.058(2) Uani 1 1 d . U . . .
C18 C 0.1772(4) 0.4692(5) 0.9709(4) 0.067(2) Uani 1 1 d . U . . .
C19 C 0.1300(5) 0.4666(7) 0.9888(5) 0.097(3) Uani 1 1 d . U . . .
H19 H 0.0931 0.4986 0.9661 0.116 Uiso 1 1 calc R U . . .
C20 C 0.1356(7) 0.4176(8) 1.0396(7) 0.130(4) Uani 1 1 d . U . . .
H20 H 0.1036 0.4165 1.0517 0.156 Uiso 1 1 calc R U . . .
C21 C 0.1919(6) 0.3695(8) 1.0721(6) 0.124(4) Uani 1 1 d . U . . .
H21 H 0.1966 0.3351 1.1058 0.148 Uiso 1 1 calc R U . . .
C22 C 0.2396(5) 0.3721(7) 1.0553(5) 0.103(4) Uani 1 1 d . U . . .
H22 H 0.2769 0.3406 1.0776 0.124 Uiso 1 1 calc R U . . .
C23 C 0.2311(4) 0.4236(5) 1.0036(4) 0.068(2) Uani 1 1 d . U . . .
H23 H 0.2633 0.4261 0.9916 0.082 Uiso 1 1 calc R U . . .
C24 C 0.3475(5) 0.4768(8) 0.9248(5) 0.097(3) Uani 1 1 d . U . . .
C25 C 0.3939(3) 0.4158(5) 0.9757(3) 0.091(3) Uani 1 1 d G U . . .
C26 C 0.3800(4) 0.3345(5) 0.9731(4) 0.139(4) Uani 1 1 d G U . . .
H26 H 0.3407 0.3146 0.9389 0.167 Uiso 1 1 calc R U . . .
C27 C 0.4247(5) 0.2831(5) 1.0217(5) 0.174(5) Uani 1 1 d G U . . .
H27 H 0.4153 0.2288 1.0200 0.208 Uiso 1 1 calc R U . . .
C28 C 0.4833(5) 0.3129(7) 1.0728(4) 0.150(5) Uani 1 1 d G U . . .
H28 H 0.5132 0.2785 1.1053 0.180 Uiso 1 1 calc R U . . .
C29 C 0.4973(3) 0.3941(7) 1.0754(3) 0.139(5) Uani 1 1 d G U . . .
H29 H 0.5365 0.4141 1.1096 0.167 Uiso 1 1 calc R U . . .
C30 C 0.4526(3) 0.4456(5) 1.0268(3) 0.142(4) Uani 1 1 d G U . . .
H30 H 0.4619 0.4999 1.0286 0.171 Uiso 1 1 calc R U . . .
C31 C 0.3055(5) 0.6729(6) 0.7724(4) 0.085(3) Uani 1 1 d . U . . .
C32 C 0.3327(2) 0.7188(3) 0.7355(2) 0.081(3) Uani 1 1 d G U . . .
C33 C 0.3025(3) 0.7884(4) 0.7009(3) 0.093(3) Uani 1 1 d G U . . .
H33 H 0.2667 0.8089 0.7025 0.112 Uiso 1 1 calc R U . . .
C34 C 0.3259(4) 0.8274(4) 0.6639(4) 0.114(4) Uani 1 1 d G U . . .
H34 H 0.3058 0.8740 0.6408 0.137 Uiso 1 1 calc R U . . .
C35 C 0.3795(4) 0.7968(5) 0.6616(4) 0.117(4) Uani 1 1 d G U . . .
H35 H 0.3952 0.8229 0.6368 0.141 Uiso 1 1 calc R U . . .
C36 C 0.4097(3) 0.7271(5) 0.6962(4) 0.117(4) Uani 1 1 d G U . . .
H36 H 0.4456 0.7066 0.6946 0.141 Uiso 1 1 calc R U . . .
C37 C 0.3863(3) 0.6881(4) 0.7332(3) 0.110(4) Uani 1 1 d G U . . .
H37 H 0.4065 0.6416 0.7563 0.132 Uiso 1 1 calc R U . . .
C38 C 0.9485(7) 0.3362(11) 0.3487(6) 0.164(6) Uani 1 1 d D U . . .
H38A H 0.9232 0.2915 0.3493 0.246 Uiso 1 1 calc R U . . .
H38B H 0.9592 0.3286 0.3141 0.246 Uiso 1 1 calc R U . . .
H38C H 0.9237 0.3846 0.3405 0.246 Uiso 1 1 calc R U . . .
Cu1 Cu 0.09181(4) 0.60495(6) 0.78098(4) 0.0550(3) Uani 1 1 d . . . . .
Dy1 Dy 0.25410(2) 0.58123(3) 0.83693(2) 0.07504(15) Uani 1 1 d . . . . .
N1 N 0.0334(3) 0.6966(4) 0.7717(3) 0.0533(17) Uani 1 1 d . . . . .
N2 N 0.0246(2) 0.5237(4) 0.7405(3) 0.0505(16) Uani 1 1 d . . . . .
O1 O 0.2879(3) 0.7029(4) 0.9085(3) 0.094(2) Uani 1 1 d . U . . .
O2 O 0.1688(2) 0.6699(4) 0.8214(2) 0.0675(16) Uani 1 1 d . U . . .
O3 O 0.2339(2) 0.5007(4) 0.7277(3) 0.0793(18) Uani 1 1 d . U . . .
O4 O 0.1491(2) 0.5372(3) 0.7620(2) 0.0594(14) Uani 1 1 d . U . . .
O5 O 0.2486(3) 0.6858(4) 0.7604(3) 0.088(2) Uani 1 1 d D U . . .
O6 O 0.3399(3) 0.6194(5) 0.8145(3) 0.094(2) Uani 1 1 d . U . . .
O7 O 0.3503(3) 0.5470(5) 0.9375(3) 0.102(2) Uani 1 1 d . U . . .
O8 O 0.3045(3) 0.4490(5) 0.8674(3) 0.098(2) Uani 1 1 d . U . . .
O9 O 0.2183(2) 0.5313(4) 0.9078(2) 0.0715(17) Uani 1 1 d . U . . .
O10 O 0.1161(2) 0.5561(4) 0.8806(2) 0.0683(16) Uani 1 1 d . U . . .
O11 O 1.0095(7) 0.3420(10) 0.4139(5) 0.245(7) Uani 1 1 d D U . . .
H11A H 1.0408 0.3467 0.4079 0.368 Uiso 1 1 calc DR U . . .
O12 O 0.1416(6) 0.7916(8) 0.6832(6) 0.228(6) 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
C1 O3 1.447(12) . ?
C2 O3 1.355(7) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C6 C8 1.426(10) . ?
C7 O4 1.307(7) . ?
C8 N2 1.271(10) . ?
C9 N1 1.304(10) . ?
C9 C10 1.467(9) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 O1 1.349(9) . ?
C14 C15 1.3900 . ?
C15 O2 1.318(7) . ?
C16 O1 1.422(11) . ?
C17 O10 1.234(9) . ?
C17 O9 1.256(10) . ?
C17 C18 1.503(12) . ?
C18 C23 1.347(11) . ?
C18 C19 1.367(14) . ?
C19 C20 1.383(17) . ?
C20 C21 1.406(18) . ?
C21 C22 1.361(19) . ?
C22 C23 1.405(15) . ?
C24 O7 1.203(14) . ?
C24 O8 1.290(12) . ?
C24 C25 1.529(12) . ?
C24 Dy1 2.751(11) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C31 O5 1.246(12) . ?
C31 O6 1.272(11) . ?
C31 C32 1.508(12) . ?
C31 Dy1 2.800(10) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C38 O11 1.480(13) . ?
Cu1 O2 1.912(5) . ?
Cu1 N2 1.937(6) . ?
Cu1 O4 1.973(6) . ?
Cu1 N1 1.998(6) . ?
Cu1 O10 2.235(5) . ?
Cu1 Dy1 3.3995(13) . ?
Dy1 O4 2.325(4) . ?
Dy1 O9 2.342(6) . ?
Dy1 O7 2.373(6) . ?
Dy1 O2 2.378(6) . ?
Dy1 O6 2.411(7) . ?
Dy1 O8 2.440(8) . ?
Dy1 O5 2.445(6) . ?
Dy1 O1 2.489(7) . ?
Dy1 O3 2.688(6) . ?
N1 N1 1.383(11) 2_556 ?
N2 N2 1.431(12) 2_556 ?

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
O3 C2 C3 124.3(4) . . ?
O3 C2 C7 115.7(4) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C8 122.5(5) . . ?
C5 C6 C8 117.3(5) . . ?
O4 C7 C6 123.3(4) . . ?
O4 C7 C2 116.7(4) . . ?
C6 C7 C2 120.0 . . ?
N2 C8 C6 124.6(7) . . ?
N1 C9 C10 127.2(8) . . ?
C11 C10 C15 120.0 . . ?
C11 C10 C9 116.7(5) . . ?
C15 C10 C9 123.3(5) . . ?
C10 C11 C12 120.0 . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C14 120.0 . . ?
O1 C14 C15 115.9(5) . . ?
O1 C14 C13 124.0(5) . . ?
C15 C14 C13 120.0 . . ?
O2 C15 C14 116.7(4) . . ?
O2 C15 C10 123.2(4) . . ?
C14 C15 C10 120.0 . . ?
O10 C17 O9 124.7(8) . . ?
O10 C17 C18 118.4(7) . . ?
O9 C17 C18 117.0(7) . . ?
C23 C18 C19 119.8(9) . . ?
C23 C18 C17 119.8(8) . . ?
C19 C18 C17 120.5(8) . . ?
C18 C19 C20 121.8(11) . . ?
C19 C20 C21 117.3(14) . . ?
C22 C21 C20 121.5(13) . . ?
C21 C22 C23 118.4(11) . . ?
C18 C23 C22 121.2(10) . . ?
O7 C24 O8 121.4(10) . . ?
O7 C24 C25 122.0(8) . . ?
O8 C24 C25 116.6(10) . . ?
O7 C24 Dy1 59.2(5) . . ?
O8 C24 Dy1 62.5(6) . . ?
C25 C24 Dy1 173.8(7) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 123.6(6) . . ?
C30 C25 C24 116.4(6) . . ?
C25 C26 C27 120.0 . . ?
C28 C27 C26 120.0 . . ?
C29 C28 C27 120.0 . . ?
C28 C29 C30 120.0 . . ?
C29 C30 C25 120.0 . . ?
O5 C31 O6 119.9(9) . . ?
O5 C31 C32 120.0(8) . . ?
O6 C31 C32 120.1(9) . . ?
O5 C31 Dy1 60.7(5) . . ?
O6 C31 Dy1 59.2(5) . . ?
C32 C31 Dy1 177.2(7) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 120.7(5) . . ?
C37 C32 C31 119.2(5) . . ?
C34 C33 C32 120.0 . . ?
C33 C34 C35 120.0 . . ?
C36 C35 C34 120.0 . . ?
C37 C36 C35 120.0 . . ?
C36 C37 C32 120.0 . . ?
O2 Cu1 N2 169.4(3) . . ?
O2 Cu1 O4 81.1(2) . . ?
N2 Cu1 O4 88.7(2) . . ?
O2 Cu1 N1 93.1(2) . . ?
N2 Cu1 N1 97.4(2) . . ?
O4 Cu1 N1 158.1(2) . . ?
O2 Cu1 O10 90.5(2) . . ?
N2 Cu1 O10 88.3(2) . . ?
O4 Cu1 O10 99.7(2) . . ?
N1 Cu1 O10 101.5(2) . . ?
O2 Cu1 Dy1 42.66(18) . . ?
N2 Cu1 Dy1 126.72(17) . . ?
O4 Cu1 Dy1 41.51(13) . . ?
N1 Cu1 Dy1 135.74(17) . . ?
O10 Cu1 Dy1 84.43(14) . . ?
O4 Dy1 O9 77.73(18) . . ?
O4 Dy1 O7 143.0(2) . . ?
O9 Dy1 O7 74.4(2) . . ?
O4 Dy1 O2 64.97(18) . . ?
O9 Dy1 O2 75.7(2) . . ?
O7 Dy1 O2 128.5(2) . . ?
O4 Dy1 O6 128.3(2) . . ?
O9 Dy1 O6 151.54(18) . . ?
O7 Dy1 O6 77.2(2) . . ?
O2 Dy1 O6 122.8(2) . . ?
O4 Dy1 O8 96.6(2) . . ?
O9 Dy1 O8 76.6(2) . . ?
O7 Dy1 O8 53.7(3) . . ?
O2 Dy1 O8 149.5(2) . . ?
O6 Dy1 O8 87.8(3) . . ?
O4 Dy1 O5 91.91(19) . . ?
O9 Dy1 O5 148.8(2) . . ?
O7 Dy1 O5 124.2(2) . . ?
O2 Dy1 O5 73.2(2) . . ?
O6 Dy1 O5 53.3(2) . . ?
O8 Dy1 O5 134.3(2) . . ?
O4 Dy1 O1 128.6(2) . . ?
O9 Dy1 O1 86.1(2) . . ?
O7 Dy1 O1 73.2(3) . . ?
O2 Dy1 O1 63.83(19) . . ?
O6 Dy1 O1 84.4(3) . . ?
O8 Dy1 O1 126.7(2) . . ?
O5 Dy1 O1 77.5(2) . . ?
O4 Dy1 O3 61.08(18) . . ?
O9 Dy1 O3 121.6(2) . . ?
O7 Dy1 O3 115.9(2) . . ?
O2 Dy1 O3 115.43(17) . . ?
O6 Dy1 O3 72.8(2) . . ?
O8 Dy1 O3 69.6(2) . . ?
O5 Dy1 O3 75.8(2) . . ?
O1 Dy1 O3 151.9(2) . . ?
O4 Dy1 C24 121.0(3) . . ?
O9 Dy1 C24 72.1(3) . . ?
O7 Dy1 C24 25.8(3) . . ?
O2 Dy1 C24 144.4(3) . . ?
O6 Dy1 C24 82.9(3) . . ?
O8 Dy1 C24 28.0(3) . . ?
O5 Dy1 C24 136.2(3) . . ?
O1 Dy1 C24 98.8(3) . . ?
O3 Dy1 C24 94.5(3) . . ?
O4 Dy1 C31 111.0(2) . . ?
O9 Dy1 C31 166.2(3) . . ?
O7 Dy1 C31 101.4(3) . . ?
O2 Dy1 C31 97.9(3) . . ?
O6 Dy1 C31 26.9(2) . . ?
O8 Dy1 C31 111.8(3) . . ?
O5 Dy1 C31 26.4(2) . . ?
O1 Dy1 C31 80.1(3) . . ?
O3 Dy1 C31 72.1(3) . . ?
C24 Dy1 C31 109.9(3) . . ?
O4 Dy1 Cu1 34.23(14) . . ?
O9 Dy1 Cu1 64.98(13) . . ?
O7 Dy1 Cu1 138.4(2) . . ?
O2 Dy1 Cu1 33.03(13) . . ?
O6 Dy1 Cu1 142.56(15) . . ?
O8 Dy1 Cu1 120.66(17) . . ?
O5 Dy1 Cu1 89.88(14) . . ?
O1 Dy1 Cu1 94.90(15) . . ?
O3 Dy1 Cu1 93.54(11) . . ?
C24 Dy1 Cu1 133.7(2) . . ?
C31 Dy1 Cu1 116.0(2) . . ?
C9 N1 N1 116.0(6) . 2_556 ?
C9 N1 Cu1 120.4(5) . . ?
N1 N1 Cu1 123.6(3) 2_556 . ?
C8 N2 N2 116.3(5) . 2_556 ?
C8 N2 Cu1 127.3(6) . . ?
N2 N2 Cu1 116.5(4) 2_556 . ?
C14 O1 C16 115.6(8) . . ?
C14 O1 Dy1 119.1(4) . . ?
C16 O1 Dy1 125.3(7) . . ?
C15 O2 Cu1 124.4(5) . . ?
C15 O2 Dy1 123.8(4) . . ?
Cu1 O2 Dy1 104.3(3) . . ?
C2 O3 C1 117.3(7) . . ?
C2 O3 Dy1 115.2(4) . . ?
C1 O3 Dy1 126.5(5) . . ?
C7 O4 Cu1 124.6(4) . . ?
C7 O4 Dy1 130.2(4) . . ?
Cu1 O4 Dy1 104.3(2) . . ?
C31 O5 Dy1 93.0(6) . . ?
C31 O6 Dy1 93.8(6) . . ?
C24 O7 Dy1 94.9(6) . . ?
C24 O8 Dy1 89.6(7) . . ?
C17 O9 Dy1 144.3(5) . . ?
C17 O10 Cu1 119.2(6) . . ?

_refine_diff_density_max         2.292
_refine_diff_density_min         -2.569
_refine_diff_density_rms         0.169


# start Validation Reply Form
_vrf_PLAT973_x                   
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_Dy2Ni2
_audit_block_doi                 10.5517/cc14ht7p
_database_code_depnum_ccdc_archive 'CCDC 1057882'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H76 Dy2 N4 Ni2 O25'
_chemical_formula_sum            'C78 H76 Dy2 N4 Ni2 O25'
_chemical_formula_weight         1911.84

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.030(5)
_cell_length_b                   16.831(3)
_cell_length_c                   22.733(5)
_cell_angle_alpha                90
_cell_angle_beta                 121.087(3)
_cell_angle_gamma                90
_cell_volume                     7874(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5286
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      23.09

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_F_000             3840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.427
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            21981
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.563
_diffrn_reflns_theta_max         25.271
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             7041
_reflns_number_gt                3988
_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.

 The command 'isor' was also used to restrain the all O and C atom with NPD and ADP
 problems. The restraint command lead to restraint number 314, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the O11-H11A and C38-O12 distance to
 be in the reasonable range

 The H-atoms on water cannot be determined.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.0756P)²+30.7282P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7041
_refine_ls_number_parameters     447
_refine_ls_number_restraints     314
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0557
_refine_ls_wR_factor_ref         0.1739
_refine_ls_wR_factor_gt          0.1357
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.023
_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
C1 C 0.2751(6) 0.4739(8) 0.2059(7) 0.109(4) Uani 1 1 d . U . . .
H1A H 0.2611 0.4887 0.1595 0.164 Uiso 1 1 calc R U . . .
H1B H 0.2798 0.4172 0.2105 0.164 Uiso 1 1 calc R U . . .
H1C H 0.3161 0.4987 0.2366 0.164 Uiso 1 1 calc R U . . .
C2 C 0.1681(3) 0.4646(4) 0.1869(4) 0.075(3) Uani 1 1 d G U . . .
C3 C 0.1478(4) 0.4163(5) 0.1298(4) 0.111(4) Uani 1 1 d G U . . .
H3 H 0.1754 0.4066 0.1133 0.133 Uiso 1 1 calc R U . . .
C4 C 0.0862(4) 0.3824(5) 0.0974(3) 0.128(5) Uani 1 1 d G U . . .
H4 H 0.0726 0.3501 0.0591 0.154 Uiso 1 1 calc R U . . .
C5 C 0.0450(3) 0.3969(4) 0.1221(4) 0.104(4) Uani 1 1 d G U . . .
H5 H 0.0037 0.3742 0.1003 0.125 Uiso 1 1 calc R U . . .
C6 C 0.0653(3) 0.4452(4) 0.1792(3) 0.070(3) Uani 1 1 d G U . . .
C7 C 0.1269(3) 0.4791(4) 0.2116(3) 0.057(2) Uani 1 1 d G U . . .
C8 C 0.0208(4) 0.4563(6) 0.2029(5) 0.066(2) Uani 1 1 d . U . . .
H8 H -0.0119 0.4188 0.1901 0.079 Uiso 1 1 calc R U . . .
C9 C 0.0583(5) 0.7569(5) 0.3090(4) 0.062(2) Uani 1 1 d . U . . .
H9 H 0.0290 0.7948 0.3068 0.074 Uiso 1 1 calc R U . . .
C10 C 0.1260(3) 0.7746(4) 0.3533(3) 0.071(3) Uani 1 1 d G U . . .
C11 C 0.1392(4) 0.8403(4) 0.3956(4) 0.097(4) Uani 1 1 d G U . . .
H11 H 0.1053 0.8696 0.3931 0.116 Uiso 1 1 calc R U . . .
C12 C 0.2032(4) 0.8622(4) 0.4415(3) 0.111(4) Uani 1 1 d G U . . .
H12 H 0.2121 0.9062 0.4698 0.133 Uiso 1 1 calc R U . . .
C13 C 0.2540(3) 0.8184(5) 0.4452(3) 0.094(3) Uani 1 1 d G U . . .
H13 H 0.2968 0.8330 0.4759 0.112 Uiso 1 1 calc R U . . .
C14 C 0.2407(3) 0.7527(4) 0.4029(3) 0.078(3) Uani 1 1 d G U . . .
C15 C 0.1767(3) 0.7308(3) 0.3570(3) 0.064(3) Uani 1 1 d G U . . .
C16 C 0.3530(6) 0.7241(8) 0.4507(7) 0.128(5) Uani 1 1 d . U . . .
H16A H 0.3636 0.7706 0.4338 0.192 Uiso 1 1 calc R U . . .
H16B H 0.3802 0.6808 0.4532 0.192 Uiso 1 1 calc R U . . .
H16C H 0.3602 0.7347 0.4956 0.192 Uiso 1 1 calc R U . . .
C17 C 0.1683(5) 0.5286(5) 0.4107(4) 0.055(2) Uani 1 1 d . U . . .
C18 C 0.1745(3) 0.4760(3) 0.4658(3) 0.059(2) Uani 1 1 d G U . . .
C19 C 0.1238(3) 0.4707(4) 0.4784(3) 0.086(3) Uani 1 1 d G U . . .
H19 H 0.0871 0.5022 0.4538 0.104 Uiso 1 1 calc R U . . .
C20 C 0.1282(3) 0.4183(5) 0.5279(4) 0.104(4) Uani 1 1 d G U . . .
H20 H 0.0943 0.4148 0.5364 0.124 Uiso 1 1 calc R U . . .
C21 C 0.1831(4) 0.3712(4) 0.5647(3) 0.104(4) Uani 1 1 d G U . . .
H21 H 0.1860 0.3361 0.5978 0.125 Uiso 1 1 calc R U . . .
C22 C 0.2338(3) 0.3764(4) 0.5521(3) 0.096(4) Uani 1 1 d G U . . .
H22 H 0.2705 0.3449 0.5767 0.115 Uiso 1 1 calc R U . . .
C23 C 0.2294(3) 0.4288(4) 0.5026(3) 0.069(3) Uani 1 1 d G U . . .
H23 H 0.2633 0.4324 0.4941 0.083 Uiso 1 1 calc R U . . .
C24 C 0.3457(5) 0.4794(8) 0.4249(6) 0.077(3) Uani 1 1 d . U . . .
C25 C 0.3933(4) 0.4250(5) 0.4779(4) 0.083(3) Uani 1 1 d G U . . .
C26 C 0.3817(4) 0.3438(6) 0.4748(4) 0.124(5) Uani 1 1 d G U . . .
H26 H 0.3423 0.3232 0.4403 0.149 Uiso 1 1 calc R U . . .
C27 C 0.4288(6) 0.2934(4) 0.5234(5) 0.149(6) Uani 1 1 d G U . . .
H27 H 0.4211 0.2390 0.5213 0.179 Uiso 1 1 calc R U . . .
C28 C 0.4877(5) 0.3242(6) 0.5750(5) 0.140(5) Uani 1 1 d G U . . .
H28 H 0.5193 0.2904 0.6075 0.168 Uiso 1 1 calc R U . . .
C29 C 0.4993(4) 0.4054(7) 0.5781(4) 0.133(5) Uani 1 1 d G U . . .
H29 H 0.5387 0.4260 0.6127 0.159 Uiso 1 1 calc R U . . .
C30 C 0.4521(5) 0.4558(5) 0.5295(5) 0.132(5) Uani 1 1 d G U . . .
H30 H 0.4599 0.5102 0.5316 0.158 Uiso 1 1 calc R U . . .
C31 C 0.3019(6) 0.6696(6) 0.2676(5) 0.072(3) Uani 1 1 d . U . . .
C32 C 0.3284(3) 0.7155(4) 0.2316(3) 0.073(3) Uani 1 1 d G U . . .
C33 C 0.2994(3) 0.7859(4) 0.1976(4) 0.077(3) Uani 1 1 d G U . . .
H33 H 0.2641 0.8063 0.1990 0.093 Uiso 1 1 calc R U . . .
C34 C 0.3232(4) 0.8259(4) 0.1616(4) 0.099(4) Uani 1 1 d G U . . .
H34 H 0.3038 0.8731 0.1389 0.119 Uiso 1 1 calc R U . . .
C35 C 0.3760(4) 0.7955(5) 0.1596(4) 0.104(4) Uani 1 1 d G U . . .
H35 H 0.3919 0.8222 0.1356 0.125 Uiso 1 1 calc R U . . .
C36 C 0.4050(3) 0.7250(5) 0.1936(4) 0.106(4) Uani 1 1 d G U . . .
H36 H 0.4403 0.7046 0.1923 0.127 Uiso 1 1 calc R U . . .
C37 C 0.3812(3) 0.6850(4) 0.2296(4) 0.097(4) Uani 1 1 d G U . . .
H37 H 0.4006 0.6379 0.2523 0.117 Uiso 1 1 calc R U . . .
C38 C 0.1116(12) 0.8286(9) 0.1792(13) 0.249(12) Uani 1 1 d D U . . .
H38A H 0.1484 0.8590 0.2121 0.374 Uiso 1 1 calc R U . . .
H38B H 0.0838 0.8181 0.1970 0.374 Uiso 1 1 calc R U . . .
H38C H 0.0880 0.8580 0.1371 0.374 Uiso 1 1 calc R U . . .
C39 C 0.0076(6) 0.6387(7) 0.1079(5) 0.099(4) Uani 1 1 d . U . . .
H39A H 0.0169 0.6081 0.0784 0.148 Uiso 1 1 calc R U . . .
H39B H -0.0048 0.6916 0.0900 0.148 Uiso 1 1 calc R U . . .
H39C H -0.0273 0.6142 0.1102 0.148 Uiso 1 1 calc R U . . .
Dy1 Dy 0.25055(2) 0.58117(3) 0.33334(2) 0.0680(2) Uani 1 1 d . . . . .
N1 N 0.0339(3) 0.6943(4) 0.2722(3) 0.0519(17) Uani 1 1 d . . . . .
N2 N 0.0231(3) 0.5138(4) 0.2401(3) 0.0495(16) Uani 1 1 d . . . . .
Ni Ni 0.08904(5) 0.60156(6) 0.27454(5) 0.0505(3) Uani 1 1 d . . . . .
O1 O 0.2865(3) 0.7038(4) 0.4052(3) 0.084(2) Uani 1 1 d . U . . .
O2 O 0.1673(3) 0.6711(4) 0.3157(3) 0.0629(16) Uani 1 1 d . U . . .
O3 O 0.1498(3) 0.5269(3) 0.2658(3) 0.0550(14) Uani 1 1 d . U . . .
O4 O 0.2274(3) 0.4996(4) 0.2225(3) 0.0783(19) Uani 1 1 d . U . . .
O5 O 0.2451(3) 0.6838(4) 0.2547(3) 0.084(2) Uani 1 1 d . U . . .
O6 O 0.3355(3) 0.6178(5) 0.3103(4) 0.093(2) Uani 1 1 d . U . . .
O7 O 0.3008(3) 0.4510(5) 0.3677(4) 0.092(2) Uani 1 1 d . U . . .
O8 O 0.3484(3) 0.5514(6) 0.4377(4) 0.091(2) Uani 1 1 d . U . . .
O9 O 0.2197(3) 0.5395(4) 0.4095(3) 0.0683(17) Uani 1 1 d . U . . .
O10 O 0.1145(3) 0.5604(3) 0.3705(3) 0.0570(15) Uani 1 1 d . U . . .
O11 O 0.0630(3) 0.6420(4) 0.1738(3) 0.0730(18) Uani 1 1 d D U . . .
H11A H 0.0816 0.6845 0.1789 0.109 Uiso 1 1 calc DR U . . .
O12 O 0.1332(5) 0.7555(7) 0.1664(6) 0.147(4) Uani 1 1 d D U . . .
H12A H 0.1711 0.7476 0.1966 0.220 Uiso 1 1 calc R U . . .
O13 O 0.0000 0.967(2) 0.2500 0.47(3) Uani 1 2 d S TU P . .


_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
C1 O4 1.446(11) . ?
C2 O4 1.357(8) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C6 C8 1.437(10) . ?
C7 O3 1.328(7) . ?
C8 N2 1.267(10) . ?
C9 N1 1.285(10) . ?
C9 C10 1.434(10) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 O1 1.353(9) . ?
C14 C15 1.3900 . ?
C15 O2 1.311(7) . ?
C16 O1 1.427(12) . ?
C17 O10 1.254(10) . ?
C17 O9 1.264(10) . ?
C17 C18 1.477(9) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C24 O8 1.241(12) . ?
C24 O7 1.279(13) . ?
C24 C25 1.474(12) . ?
C24 Dy1 2.754(11) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C31 O6 1.243(12) . ?
C31 O5 1.262(12) . ?
C31 C32 1.486(10) . ?
C31 Dy1 2.807(10) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C38 O12 1.422(9) . ?
C39 O11 1.400(11) . ?
Dy1 O3 2.283(5) . ?
Dy1 O9 2.316(6) . ?
Dy1 O2 2.372(6) . ?
Dy1 O8 2.376(7) . ?
Dy1 O7 2.427(8) . ?
Dy1 O6 2.433(6) . ?
Dy1 O5 2.440(6) . ?
Dy1 O1 2.494(7) . ?
Dy1 O4 2.664(6) . ?
Dy1 Ni 3.4074(13) . ?
N1 N1 1.404(13) 2 ?
N1 Ni 2.030(7) . ?
N2 N2 1.397(12) 2 ?
N2 Ni 2.006(6) . ?
Ni O2 1.992(6) . ?
Ni O3 2.013(5) . ?
Ni O10 2.058(5) . ?
Ni O11 2.149(6) . ?

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
O4 C2 C3 124.4(5) . . ?
O4 C2 C7 115.6(5) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C8 117.1(6) . . ?
C7 C6 C8 122.9(6) . . ?
O3 C7 C6 124.0(5) . . ?
O3 C7 C2 116.0(5) . . ?
C6 C7 C2 120.0 . . ?
N2 C8 C6 124.4(8) . . ?
N1 C9 C10 126.7(8) . . ?
C11 C10 C15 120.0 . . ?
C11 C10 C9 115.0(6) . . ?
C15 C10 C9 125.0(6) . . ?
C12 C11 C10 120.0 . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
O1 C14 C13 124.4(6) . . ?
O1 C14 C15 115.5(6) . . ?
C13 C14 C15 120.0 . . ?
O2 C15 C14 117.1(6) . . ?
O2 C15 C10 122.8(6) . . ?
C14 C15 C10 120.0 . . ?
O10 C17 O9 125.1(8) . . ?
O10 C17 C18 119.2(7) . . ?
O9 C17 C18 115.7(8) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 119.9(6) . . ?
C23 C18 C17 120.1(6) . . ?
C18 C19 C20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C22 C21 C20 120.0 . . ?
C21 C22 C23 120.0 . . ?
C22 C23 C18 120.0 . . ?
O8 C24 O7 121.1(11) . . ?
O8 C24 C25 119.4(11) . . ?
O7 C24 C25 119.4(11) . . ?
O8 C24 Dy1 59.4(6) . . ?
O7 C24 Dy1 61.8(6) . . ?
C25 C24 Dy1 174.2(7) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 121.2(9) . . ?
C30 C25 C24 118.7(8) . . ?
C27 C26 C25 120.0 . . ?
C26 C27 C28 120.0 . . ?
C29 C28 C27 120.0 . . ?
C28 C29 C30 120.0 . . ?
C29 C30 C25 120.0 . . ?
O6 C31 O5 120.1(9) . . ?
O6 C31 C32 120.3(10) . . ?
O5 C31 C32 119.6(9) . . ?
O6 C31 Dy1 59.9(5) . . ?
O5 C31 Dy1 60.2(5) . . ?
C32 C31 Dy1 178.9(7) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 121.0(7) . . ?
C37 C32 C31 119.0(7) . . ?
C34 C33 C32 120.0 . . ?
C33 C34 C35 120.0 . . ?
C36 C35 C34 120.0 . . ?
C35 C36 C37 120.0 . . ?
C36 C37 C32 120.0 . . ?
O3 Dy1 O9 75.20(19) . . ?
O3 Dy1 O2 68.5(2) . . ?
O9 Dy1 O2 75.7(2) . . ?
O3 Dy1 O8 138.2(2) . . ?
O9 Dy1 O8 73.9(2) . . ?
O2 Dy1 O8 128.1(3) . . ?
O3 Dy1 O7 91.9(2) . . ?
O9 Dy1 O7 77.5(2) . . ?
O2 Dy1 O7 150.0(2) . . ?
O8 Dy1 O7 54.4(3) . . ?
O3 Dy1 O6 132.2(2) . . ?
O9 Dy1 O6 149.9(2) . . ?
O2 Dy1 O6 122.0(2) . . ?
O8 Dy1 O6 76.2(2) . . ?
O7 Dy1 O6 88.0(3) . . ?
O3 Dy1 O5 98.8(2) . . ?
O9 Dy1 O5 147.7(2) . . ?
O2 Dy1 O5 72.7(2) . . ?
O8 Dy1 O5 122.1(2) . . ?
O7 Dy1 O5 134.8(2) . . ?
O6 Dy1 O5 52.9(2) . . ?
O3 Dy1 O1 131.3(2) . . ?
O9 Dy1 O1 84.1(2) . . ?
O2 Dy1 O1 63.8(2) . . ?
O8 Dy1 O1 72.0(3) . . ?
O7 Dy1 O1 126.1(2) . . ?
O6 Dy1 O1 83.4(3) . . ?
O5 Dy1 O1 76.3(2) . . ?
O3 Dy1 O4 61.73(19) . . ?
O9 Dy1 O4 124.0(2) . . ?
O2 Dy1 O4 115.04(19) . . ?
O8 Dy1 O4 116.8(3) . . ?
O7 Dy1 O4 70.5(2) . . ?
O6 Dy1 O4 73.5(2) . . ?
O5 Dy1 O4 76.5(2) . . ?
O1 Dy1 O4 151.5(2) . . ?
O3 Dy1 C24 116.0(3) . . ?
O9 Dy1 C24 73.0(3) . . ?
O2 Dy1 C24 145.5(3) . . ?
O8 Dy1 C24 26.7(3) . . ?
O7 Dy1 C24 27.7(3) . . ?
O6 Dy1 C24 81.9(3) . . ?
O5 Dy1 C24 134.7(3) . . ?
O1 Dy1 C24 98.5(3) . . ?
O4 Dy1 C24 94.6(3) . . ?
O3 Dy1 C31 117.3(3) . . ?
O9 Dy1 C31 163.2(3) . . ?
O2 Dy1 C31 97.8(3) . . ?
O8 Dy1 C31 99.4(3) . . ?
O7 Dy1 C31 111.6(3) . . ?
O6 Dy1 C31 26.2(3) . . ?
O5 Dy1 C31 26.7(3) . . ?
O1 Dy1 C31 79.1(3) . . ?
O4 Dy1 C31 72.8(3) . . ?
C24 Dy1 C31 108.1(3) . . ?
O3 Dy1 Ni 34.85(14) . . ?
O9 Dy1 Ni 65.46(15) . . ?
O2 Dy1 Ni 34.83(14) . . ?
O8 Dy1 Ni 138.78(17) . . ?
O7 Dy1 Ni 119.56(17) . . ?
O6 Dy1 Ni 143.31(17) . . ?
O5 Dy1 Ni 91.25(16) . . ?
O1 Dy1 Ni 96.47(17) . . ?
O4 Dy1 Ni 92.39(13) . . ?
C24 Dy1 Ni 133.8(2) . . ?
C31 Dy1 Ni 117.6(2) . . ?
C9 N1 N1 116.0(6) . 2 ?
C9 N1 Ni 122.8(6) . . ?
N1 N1 Ni 121.2(3) 2 . ?
C8 N2 N2 116.6(6) . 2 ?
C8 N2 Ni 125.2(6) . . ?
N2 N2 Ni 118.2(4) 2 . ?
O2 Ni N2 168.6(3) . . ?
O2 Ni O3 81.7(2) . . ?
N2 Ni O3 88.2(2) . . ?
O2 Ni N1 90.3(3) . . ?
N2 Ni N1 100.5(3) . . ?
O3 Ni N1 167.0(2) . . ?
O2 Ni O10 90.5(2) . . ?
N2 Ni O10 84.8(2) . . ?
O3 Ni O10 93.5(2) . . ?
N1 Ni O10 96.8(2) . . ?
O2 Ni O11 89.9(2) . . ?
N2 Ni O11 94.6(3) . . ?
O3 Ni O11 85.4(2) . . ?
N1 Ni O11 84.4(3) . . ?
O10 Ni O11 178.7(3) . . ?
O2 Ni Dy1 42.84(19) . . ?
N2 Ni Dy1 126.11(18) . . ?
O3 Ni Dy1 40.39(16) . . ?
N1 Ni Dy1 133.14(19) . . ?
O10 Ni Dy1 84.01(17) . . ?
O11 Ni Dy1 95.49(19) . . ?
C14 O1 C16 117.9(9) . . ?
C14 O1 Dy1 118.5(5) . . ?
C16 O1 Dy1 123.5(8) . . ?
C15 O2 Ni 123.9(5) . . ?
C15 O2 Dy1 123.3(5) . . ?
Ni O2 Dy1 102.3(3) . . ?
C7 O3 Ni 119.6(4) . . ?
C7 O3 Dy1 130.9(4) . . ?
Ni O3 Dy1 104.8(2) . . ?
C2 O4 C1 116.4(8) . . ?
C2 O4 Dy1 115.4(4) . . ?
C1 O4 Dy1 126.5(7) . . ?
C31 O5 Dy1 93.1(6) . . ?
C31 O6 Dy1 93.9(6) . . ?
C24 O7 Dy1 90.5(7) . . ?
C24 O8 Dy1 93.9(7) . . ?
C17 O9 Dy1 139.0(5) . . ?
C17 O10 Ni 123.1(5) . . ?
C39 O11 Ni 136.1(6) . . ?

_refine_diff_density_max         1.088
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.119

####################################################################### 
# 
# 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_Dy2Zn2
_audit_block_doi                 10.5517/cc14ht8q
_database_code_depnum_ccdc_archive 'CCDC 1057883'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C76 H70 Dy2 N4 O24 Zn2'
_chemical_formula_sum            'C76 H70 Dy2 N4 O24 Zn2'
_chemical_formula_weight         1879.10

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'
Dy Dy -0.1892 4.4098 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.874(3)
_cell_length_b                   16.890(3)
_cell_length_c                   22.915(4)
_cell_angle_alpha                90
_cell_angle_beta                 120.515(12)
_cell_angle_gamma                90
_cell_volume                     7960(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5863
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      24.70

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_F_000             3752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.527
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18502
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.569
_diffrn_reflns_theta_max         25.095
_diffrn_reflns_theta_full        25.095
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             6961
_reflns_number_gt                4061
_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.

 The command 'isor' was also used to restrain the all C and O atom with NPD and ADP
 problems. The restraint command lead to restraint number 302, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the H12A-O12 and H9A-H11 distance to
 be in the reasonable range

 The H-atoms on water cannot be determined.

 The omit command has been used to omit the bad equivalents.
 
 The high Ueq as Compared to Neighbors for O12 were abtained because of the disorder of solvent molecule.
 
 In the final refinement, the compounds show large solvent accessible void 
 and the sovlents cannot be determined. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.1393P)²+21.5339P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6961
_refine_ls_number_parameters     430
_refine_ls_number_restraints     302
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0776
_refine_ls_wR_factor_ref         0.2611
_refine_ls_wR_factor_gt          0.2172
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.109
_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
C1 C 0.7180(7) -0.0223(12) 0.2877(8) 0.119(6) Uani 1 1 d . U . . .
H1A H 0.7148 -0.0790 0.2859 0.178 Uiso 1 1 calc R U . . .
H1B H 0.6770 0.0001 0.2547 0.178 Uiso 1 1 calc R U . . .
H1C H 0.7292 -0.0044 0.3320 0.178 Uiso 1 1 calc R U . . .
C2 C 0.8273(3) -0.0288(6) 0.3108(5) 0.083(4) Uani 1 1 d G U . . .
C3 C 0.8458(5) -0.0768(7) 0.3670(5) 0.127(6) Uani 1 1 d G U . . .
H3 H 0.8170 -0.0859 0.3824 0.152 Uiso 1 1 calc R U . . .
C4 C 0.9072(5) -0.1112(7) 0.4002(5) 0.146(7) Uani 1 1 d G U . . .
H4 H 0.9195 -0.1433 0.4378 0.175 Uiso 1 1 calc R U . . .
C5 C 0.9501(4) -0.0976(6) 0.3771(5) 0.123(6) Uani 1 1 d G U . . .
H5 H 0.9912 -0.1206 0.3993 0.148 Uiso 1 1 calc R U . . .
C6 C 0.9317(3) -0.0496(6) 0.3210(5) 0.078(3) Uani 1 1 d G U . . .
C7 C 0.8703(3) -0.0153(5) 0.2878(3) 0.061(3) Uani 1 1 d G U . . .
C8 C 0.9790(5) -0.0408(8) 0.2987(6) 0.070(3) Uani 1 1 d . U . . .
H8 H 1.0138 -0.0759 0.3155 0.084 Uiso 1 1 calc R U . . .
C9 C 0.6459(7) 0.2264(11) 0.0431(8) 0.149(8) Uani 1 1 d . U . . .
H9A H 0.6438 0.2507 0.0041 0.223 Uiso 1 1 calc DR U . . .
H9B H 0.6307 0.2631 0.0639 0.223 Uiso 1 1 calc R U . . .
H9C H 0.6192 0.1798 0.0294 0.223 Uiso 1 1 calc R U . . .
C10 C 0.7579(3) 0.2550(5) 0.0951(4) 0.084(4) Uani 1 1 d G U . . .
C11 C 0.7450(4) 0.3220(6) 0.0551(4) 0.104(5) Uani 1 1 d G U . . .
H11 H 0.7023 0.3364 0.0246 0.125 Uiso 1 1 calc DR U . . .
C12 C 0.7960(6) 0.3675(5) 0.0606(5) 0.129(6) Uani 1 1 d G U . . .
H12 H 0.7874 0.4123 0.0338 0.155 Uiso 1 1 calc R U . . .
C13 C 0.8599(5) 0.3459(6) 0.1061(5) 0.113(5) Uani 1 1 d G U . . .
H13 H 0.8940 0.3763 0.1098 0.136 Uiso 1 1 calc R U . . .
C14 C 0.8728(3) 0.2788(6) 0.1462(4) 0.081(4) Uani 1 1 d G U . . .
C15 C 0.8218(4) 0.2334(4) 0.1406(3) 0.064(3) Uani 1 1 d G U . . .
C16 C 0.9411(6) 0.2593(8) 0.1907(6) 0.074(3) Uani 1 1 d . U . . .
H16 H 0.9705 0.2965 0.1923 0.089 Uiso 1 1 calc R U . . .
C17 C 0.6532(6) -0.0163(11) 0.0722(7) 0.080(4) Uani 1 1 d . U . . .
C18 C 0.6059(4) -0.0757(7) 0.0219(5) 0.082(4) Uani 1 1 d G U . . .
C19 C 0.5476(5) -0.0444(6) -0.0291(6) 0.122(5) Uani 1 1 d G U . . .
H19 H 0.5402 0.0098 -0.0312 0.147 Uiso 1 1 calc R U . . .
C20 C 0.5002(4) -0.0943(8) -0.0770(5) 0.128(6) Uani 1 1 d G U . . .
H20 H 0.4611 -0.0734 -0.1111 0.153 Uiso 1 1 calc R U . . .
C21 C 0.5111(6) -0.1754(8) -0.0739(6) 0.128(6) Uani 1 1 d G U . . .
H21 H 0.4794 -0.2088 -0.1059 0.154 Uiso 1 1 calc R U . . .
C22 C 0.5694(7) -0.2067(6) -0.0229(7) 0.157(8) Uani 1 1 d G U . . .
H22 H 0.5768 -0.2610 -0.0208 0.188 Uiso 1 1 calc R U . . .
C23 C 0.6168(5) -0.1569(7) 0.0250(5) 0.131(6) Uani 1 1 d G U . . .
H23 H 0.6559 -0.1778 0.0591 0.157 Uiso 1 1 calc R U . . .
C24 C 0.6964(7) 0.1720(9) 0.2274(6) 0.083(4) Uani 1 1 d . U . . .
C25 C 0.6702(4) 0.2200(6) 0.2654(4) 0.080(4) Uani 1 1 d G U . . .
C26 C 0.7010(4) 0.2887(6) 0.3006(5) 0.097(4) Uani 1 1 d G U . . .
H26 H 0.7369 0.3080 0.2994 0.116 Uiso 1 1 calc R U . . .
C27 C 0.6782(5) 0.3284(5) 0.3375(5) 0.116(5) Uani 1 1 d G U . . .
H27 H 0.6988 0.3743 0.3611 0.139 Uiso 1 1 calc R U . . .
C28 C 0.6245(5) 0.2995(7) 0.3393(5) 0.112(5) Uani 1 1 d G U . . .
H28 H 0.6093 0.3260 0.3640 0.134 Uiso 1 1 calc R U . . .
C29 C 0.5937(4) 0.2309(7) 0.3041(5) 0.112(5) Uani 1 1 d G U . . .
H29 H 0.5578 0.2115 0.3052 0.135 Uiso 1 1 calc R U . . .
C30 C 0.6166(4) 0.1911(6) 0.2671(5) 0.111(5) Uani 1 1 d G U . . .
H30 H 0.5959 0.1452 0.2436 0.133 Uiso 1 1 calc R U . . .
C31 C 0.8306(5) 0.0240(7) 0.0848(5) 0.059(3) Uani 1 1 d . U . . .
C32 C 0.8235(4) -0.0300(5) 0.0302(4) 0.067(3) Uani 1 1 d G U . . .
C33 C 0.7689(3) -0.0781(5) -0.0030(4) 0.068(3) Uani 1 1 d G U . . .
H33 H 0.7368 -0.0758 0.0086 0.081 Uiso 1 1 calc R U . . .
C34 C 0.7623(4) -0.1296(5) -0.0534(5) 0.111(5) Uani 1 1 d G U . . .
H34 H 0.7257 -0.1618 -0.0756 0.134 Uiso 1 1 calc R U . . .
C35 C 0.8102(6) -0.1329(6) -0.0707(5) 0.122(6) Uani 1 1 d G U . . .
H35 H 0.8058 -0.1674 -0.1044 0.147 Uiso 1 1 calc R U . . .
C36 C 0.8649(5) -0.0848(7) -0.0375(6) 0.138(7) Uani 1 1 d G U . . .
H36 H 0.8970 -0.0871 -0.0490 0.166 Uiso 1 1 calc R U . . .
C37 C 0.8715(4) -0.0334(6) 0.0130(5) 0.100(4) Uani 1 1 d G U . . .
H37 H 0.9081 -0.0012 0.0352 0.120 Uiso 1 1 calc R U . . .
C38 C 1.0020(11) 0.1525(15) 0.4051(9) 0.160(8) Uani 1 1 d . U . . .
H38A H 1.0414 0.1496 0.4036 0.240 Uiso 1 1 calc R U . . .
H38B H 0.9989 0.1070 0.4285 0.240 Uiso 1 1 calc R U . . .
H38C H 1.0022 0.1997 0.4285 0.240 Uiso 1 1 calc R U . . .
Dy1 Dy 0.74704(2) 0.08346(4) 0.16379(2) 0.0734(3) Uani 1 1 d . . . . .
N1 N 0.9750(4) 0.0123(5) 0.2576(4) 0.053(2) Uani 1 1 d . . . . .
N2 N 0.9664(4) 0.1977(5) 0.2283(4) 0.055(2) Uani 1 1 d . . . . .
O1 O 0.7673(4) 0.0021(6) 0.2733(4) 0.082(2) Uani 1 1 d . U . . .
O2 O 0.8505(3) 0.0337(5) 0.2373(3) 0.0609(19) Uani 1 1 d . U . . .
O3 O 0.7120(4) 0.2050(6) 0.0907(4) 0.091(3) Uani 1 1 d . U . . .
O4 O 0.8300(3) 0.1705(5) 0.1781(3) 0.066(2) Uani 1 1 d . U . . .
O5 O 0.6514(4) 0.0516(8) 0.0614(5) 0.098(3) Uani 1 1 d . U . . .
O6 O 0.6973(4) -0.0476(7) 0.1320(4) 0.092(3) Uani 1 1 d . U . . .
O7 O 0.6616(4) 0.1211(7) 0.1843(4) 0.097(3) Uani 1 1 d . U . . .
O8 O 0.7524(4) 0.1873(6) 0.2409(4) 0.086(3) Uani 1 1 d . U . . .
O9 O 0.7818(3) 0.0323(5) 0.0909(3) 0.068(2) Uani 1 1 d . U . . .
O10 O 0.8839(4) 0.0565(5) 0.1208(4) 0.067(2) Uani 1 1 d . U . . .
O12 O 0.9442(9) 0.1540(12) 0.3336(9) 0.204(7) Uani 1 1 d D U . . .
H12A H 0.9162 0.1235 0.3307 0.306 Uiso 1 1 calc DR U . . .
Zn1 Zn 0.90808(6) 0.09940(8) 0.21371(7) 0.0623(4) Uani 1 1 d . . . . .
O11 O 0.8710(10) 0.2776(13) 0.3267(8) 0.245(9) 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
C1 O1 1.434(15) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.347(10) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.466(13) . ?
C7 O2 1.301(9) . ?
C8 N1 1.268(14) . ?
C8 H8 0.9300 . ?
C9 O3 1.436(15) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.345(13) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C16 1.455(13) . ?
C15 O4 1.317(10) . ?
C16 N2 1.289(14) . ?
C16 H16 0.9300 . ?
C17 O5 1.169(17) . ?
C17 O6 1.341(16) . ?
C17 C18 1.512(16) . ?
C17 Dy1 2.737(14) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O8 1.238(16) . ?
C24 O7 1.254(16) . ?
C24 C25 1.536(13) . ?
C24 Dy1 2.759(12) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O10 1.239(12) . ?
C31 O9 1.248(12) . ?
C31 C32 1.487(12) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 O12 1.51(2) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
Dy1 O2 2.327(7) . ?
Dy1 O4 2.352(8) . ?
Dy1 O5 2.360(9) . ?
Dy1 O9 2.373(7) . ?
Dy1 O7 2.401(8) . ?
Dy1 O6 2.442(10) . ?
Dy1 O8 2.445(8) . ?
Dy1 O3 2.509(10) . ?
Dy1 O1 2.681(8) . ?
Dy1 Zn1 3.4200(14) . ?
N1 N1 1.405(16) 2_755 ?
N1 Zn1 2.023(8) . ?
N2 N2 1.392(16) 2_755 ?
N2 Zn1 2.083(9) . ?
O2 Zn1 2.042(7) . ?
O4 Zn1 2.010(7) . ?
O10 Zn1 2.036(8) . ?
O12 H12A 0.8200 . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.4(7) . . ?
O1 C2 C7 116.4(7) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C8 123.6(7) . . ?
C5 C6 C8 116.4(7) . . ?
O2 C7 C6 123.9(6) . . ?
O2 C7 C2 116.0(6) . . ?
C6 C7 C2 120.0 . . ?
N1 C8 C6 123.3(10) . . ?
N1 C8 H8 118.4 . . ?
C6 C8 H8 118.4 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 124.3(7) . . ?
O3 C10 C15 115.6(7) . . ?
C11 C10 C15 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 C16 123.8(8) . . ?
C13 C14 C16 116.2(8) . . ?
O4 C15 C14 123.6(7) . . ?
O4 C15 C10 116.4(7) . . ?
C14 C15 C10 120.0 . . ?
N2 C16 C14 129.1(11) . . ?
N2 C16 H16 115.4 . . ?
C14 C16 H16 115.4 . . ?
O5 C17 O6 121.8(14) . . ?
O5 C17 C18 123.8(14) . . ?
O6 C17 C18 114.4(14) . . ?
O5 C17 Dy1 59.1(8) . . ?
O6 C17 Dy1 63.0(7) . . ?
C18 C17 Dy1 175.2(9) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 115.5(10) . . ?
C23 C18 C17 124.5(10) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O8 C24 O7 122.7(11) . . ?
O8 C24 C25 116.6(12) . . ?
O7 C24 C25 120.7(12) . . ?
O8 C24 Dy1 62.4(6) . . ?
O7 C24 Dy1 60.4(6) . . ?
C25 C24 Dy1 177.9(8) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 121.4(9) . . ?
C30 C25 C24 118.5(9) . . ?
C25 C26 C27 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O10 C31 O9 125.2(10) . . ?
O10 C31 C32 118.0(9) . . ?
O9 C31 C32 116.7(9) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 119.5(7) . . ?
C37 C32 C31 120.5(7) . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.0 . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O12 C38 H38A 109.5 . . ?
O12 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O12 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O2 Dy1 O4 67.4(2) . . ?
O2 Dy1 O5 140.6(3) . . ?
O4 Dy1 O5 127.0(4) . . ?
O2 Dy1 O9 75.9(2) . . ?
O4 Dy1 O9 75.8(3) . . ?
O5 Dy1 O9 74.0(3) . . ?
O2 Dy1 O7 130.5(3) . . ?
O4 Dy1 O7 123.1(3) . . ?
O5 Dy1 O7 76.5(3) . . ?
O9 Dy1 O7 150.5(3) . . ?
O2 Dy1 O6 93.8(3) . . ?
O4 Dy1 O6 148.9(3) . . ?
O5 Dy1 O6 54.4(4) . . ?
O9 Dy1 O6 75.6(3) . . ?
O7 Dy1 O6 88.0(3) . . ?
O2 Dy1 O8 95.1(3) . . ?
O4 Dy1 O8 73.7(3) . . ?
O5 Dy1 O8 123.5(3) . . ?
O9 Dy1 O8 149.3(3) . . ?
O7 Dy1 O8 53.6(3) . . ?
O6 Dy1 O8 134.8(3) . . ?
O2 Dy1 O3 130.5(3) . . ?
O4 Dy1 O3 63.5(3) . . ?
O5 Dy1 O3 72.3(4) . . ?
O9 Dy1 O3 86.8(3) . . ?
O7 Dy1 O3 83.5(3) . . ?
O6 Dy1 O3 126.5(3) . . ?
O8 Dy1 O3 76.9(3) . . ?
O2 Dy1 O1 61.1(2) . . ?
O4 Dy1 O1 116.8(2) . . ?
O5 Dy1 O1 115.9(4) . . ?
O9 Dy1 O1 120.7(3) . . ?
O7 Dy1 O1 73.7(3) . . ?
O6 Dy1 O1 69.1(3) . . ?
O8 Dy1 O1 76.9(3) . . ?
O3 Dy1 O1 152.3(3) . . ?
O2 Dy1 C17 119.2(4) . . ?
O4 Dy1 C17 142.7(3) . . ?
O5 Dy1 C17 25.2(4) . . ?
O9 Dy1 C17 71.3(3) . . ?
O7 Dy1 C17 82.4(3) . . ?
O6 Dy1 C17 29.3(4) . . ?
O8 Dy1 C17 135.9(3) . . ?
O3 Dy1 C17 97.3(4) . . ?
O1 Dy1 C17 95.2(4) . . ?
O2 Dy1 C24 113.7(3) . . ?
O4 Dy1 C24 98.7(4) . . ?
O5 Dy1 C24 100.8(4) . . ?
O9 Dy1 C24 166.6(4) . . ?
O7 Dy1 C24 27.0(4) . . ?
O6 Dy1 C24 111.8(4) . . ?
O8 Dy1 C24 26.7(4) . . ?
O3 Dy1 C24 79.8(4) . . ?
O1 Dy1 C24 72.7(3) . . ?
C17 Dy1 C24 109.3(4) . . ?
O2 Dy1 Zn1 35.59(18) . . ?
O4 Dy1 Zn1 34.93(17) . . ?
O5 Dy1 Zn1 134.9(2) . . ?
O9 Dy1 Zn1 61.87(18) . . ?
O7 Dy1 Zn1 146.8(2) . . ?
O6 Dy1 Zn1 117.7(2) . . ?
O8 Dy1 Zn1 93.7(2) . . ?
O3 Dy1 Zn1 95.5(2) . . ?
O1 Dy1 Zn1 95.13(16) . . ?
C17 Dy1 Zn1 130.4(3) . . ?
C24 Dy1 Zn1 120.0(3) . . ?
C8 N1 N1 115.5(8) . 2_755 ?
C8 N1 Zn1 128.9(8) . . ?
N1 N1 Zn1 115.6(5) 2_755 . ?
C16 N2 N2 117.2(8) . 2_755 ?
C16 N2 Zn1 119.2(8) . . ?
N2 N2 Zn1 123.2(3) 2_755 . ?
C2 O1 C1 118.2(10) . . ?
C2 O1 Dy1 115.1(5) . . ?
C1 O1 Dy1 125.7(8) . . ?
C7 O2 Zn1 126.2(5) . . ?
C7 O2 Dy1 130.3(5) . . ?
Zn1 O2 Dy1 102.8(3) . . ?
C10 O3 C9 115.9(12) . . ?
C10 O3 Dy1 118.7(6) . . ?
C9 O3 Dy1 125.3(12) . . ?
C15 O4 Zn1 123.1(6) . . ?
C15 O4 Dy1 125.3(6) . . ?
Zn1 O4 Dy1 103.0(3) . . ?
C17 O5 Dy1 95.8(9) . . ?
C17 O6 Dy1 87.7(9) . . ?
C24 O7 Dy1 92.6(8) . . ?
C24 O8 Dy1 90.9(8) . . ?
C31 O9 Dy1 143.0(7) . . ?
C31 O10 Zn1 120.2(7) . . ?
C38 O12 H12A 109.5 . . ?
O4 Zn1 N1 166.3(3) . . ?
O4 Zn1 O10 94.4(3) . . ?
N1 Zn1 O10 89.7(3) . . ?
O4 Zn1 O2 79.7(3) . . ?
N1 Zn1 O2 86.6(3) . . ?
O10 Zn1 O2 102.2(3) . . ?
O4 Zn1 N2 89.8(3) . . ?
N1 Zn1 N2 101.8(3) . . ?
O10 Zn1 N2 105.2(3) . . ?
O2 Zn1 N2 151.2(3) . . ?
O4 Zn1 Dy1 42.1(2) . . ?
N1 Zn1 Dy1 125.3(2) . . ?
O10 Zn1 Dy1 87.0(2) . . ?
O2 Zn1 Dy1 41.56(19) . . ?
N2 Zn1 Dy1 131.6(2) . . ?

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
O1 C2 C3 C4 175.3(11) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C8 -177.9(10) . . . . ?
C5 C6 C7 O2 176.1(9) . . . . ?
C8 C6 C7 O2 -6.2(12) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C8 C6 C7 C2 177.7(11) . . . . ?
O1 C2 C7 O2 8.0(10) . . . . ?
C3 C2 C7 O2 -176.4(9) . . . . ?
O1 C2 C7 C6 -175.6(10) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C7 C6 C8 N1 16.8(16) . . . . ?
C5 C6 C8 N1 -165.5(9) . . . . ?
O3 C10 C11 C12 -176.2(9) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C16 178.0(9) . . . . ?
C13 C14 C15 O4 -177.9(8) . . . . ?
C16 C14 C15 O4 4.2(10) . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C16 C14 C15 C10 -177.9(9) . . . . ?
O3 C10 C15 O4 -5.5(8) . . . . ?
C11 C10 C15 O4 178.1(7) . . . . ?
O3 C10 C15 C14 176.5(8) . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C15 C14 C16 N2 4.6(16) . . . . ?
C13 C14 C16 N2 -173.3(10) . . . . ?
O5 C17 C18 C19 -20.4(16) . . . . ?
O6 C17 C18 C19 158.0(9) . . . . ?
O5 C17 C18 C23 161.1(11) . . . . ?
O6 C17 C18 C23 -20.4(14) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 -178.5(9) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C17 C18 C23 C22 178.4(10) . . . . ?
O8 C24 C25 C26 14.5(15) . . . . ?
O7 C24 C25 C26 -164.3(11) . . . . ?
O8 C24 C25 C30 -162.0(10) . . . . ?
O7 C24 C25 C30 19.2(16) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 -176.4(9) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 176.5(9) . . . . ?
O10 C31 C32 C33 168.6(8) . . . . ?
O9 C31 C32 C33 -10.8(13) . . . . ?
O10 C31 C32 C37 -10.5(13) . . . . ?
O9 C31 C32 C37 170.0(8) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C34 -179.1(8) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C31 C32 C37 C36 179.1(8) . . . . ?
C6 C8 N1 N1 179.5(10) . . . 2_755 ?
C6 C8 N1 Zn1 1.9(17) . . . . ?
C14 C16 N2 N2 -173.3(11) . . . 2_755 ?
C14 C16 N2 Zn1 13.5(16) . . . . ?
C3 C2 O1 C1 -6.7(14) . . . . ?
C7 C2 O1 C1 168.7(10) . . . . ?
C3 C2 O1 Dy1 -176.0(5) . . . . ?
C7 C2 O1 Dy1 -0.5(10) . . . . ?
C6 C7 O2 Zn1 -21.2(11) . . . . ?
C2 C7 O2 Zn1 155.0(6) . . . . ?
C6 C7 O2 Dy1 169.5(6) . . . . ?
C2 C7 O2 Dy1 -14.3(10) . . . . ?
C11 C10 O3 C9 -2.9(13) . . . . ?
C15 C10 O3 C9 -179.2(9) . . . . ?
C11 C10 O3 Dy1 176.7(4) . . . . ?
C15 C10 O3 Dy1 0.4(9) . . . . ?
C14 C15 O4 Zn1 -31.0(9) . . . . ?
C10 C15 O4 Zn1 151.1(5) . . . . ?
C14 C15 O4 Dy1 -173.2(5) . . . . ?
C10 C15 O4 Dy1 8.8(8) . . . . ?
O6 C17 O5 Dy1 6.3(13) . . . . ?
C18 C17 O5 Dy1 -175.4(10) . . . . ?
O5 C17 O6 Dy1 -6.1(13) . . . . ?
C18 C17 O6 Dy1 175.5(8) . . . . ?
O8 C24 O7 Dy1 3.4(15) . . . . ?
C25 C24 O7 Dy1 -177.9(10) . . . . ?
O7 C24 O8 Dy1 -3.4(15) . . . . ?
C25 C24 O8 Dy1 177.9(10) . . . . ?
O10 C31 O9 Dy1 -11(2) . . . . ?
C32 C31 O9 Dy1 168.0(8) . . . . ?
O9 C31 O10 Zn1 20.3(15) . . . . ?
C32 C31 O10 Zn1 -159.1(7) . . . . ?

_refine_diff_density_max         1.268
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.160

####################################################################### 
# 
# 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_Gd2Co2
_audit_block_doi                 10.5517/cc14ht9r
_database_code_depnum_ccdc_archive 'CCDC 1057884'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H74 Co2 Gd2 N4 O25'
_chemical_formula_sum            'C78 H74 Co2 Gd2 N4 O25'
_chemical_formula_weight         1899.77

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'
Co Co 0.3494 0.9721 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.175(4)
_cell_length_b                   16.937(3)
_cell_length_c                   22.730(5)
_cell_angle_alpha                90
_cell_angle_beta                 121.179(3)
_cell_angle_gamma                90
_cell_volume                     7963(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3750
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      21.19

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_F_000             3808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.133
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22620
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.554
_diffrn_reflns_theta_max         25.171
_diffrn_reflns_theta_full        25.171
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7113
_reflns_number_gt                4032
_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.

 The command 'isor' was also used to restrain the C and O atom with NPD and ADP
 problems. The restraint command lead to restraint number 249, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the H1A-H3, H9A-H11 and H11a-O11 distance to
 be in the reasonable range.

 The H-atoms on water cannot be determined.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.0712P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7113
_refine_ls_number_parameters     447
_refine_ls_number_restraints     249
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1582
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.033
_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
C1 C 0.3509(4) 0.2285(6) 0.4528(6) 0.117(4) Uani 1 1 d . U . . .
H1A H 0.3578 0.2815 0.4431 0.176 Uiso 1 1 calc DR U . . .
H1B H 0.3788 0.1932 0.4470 0.176 Uiso 1 1 calc R U . . .
H1C H 0.3604 0.2254 0.4993 0.176 Uiso 1 1 calc R U . . .
C2 C 0.2397(2) 0.2555(4) 0.4040(3) 0.069(3) Uani 1 1 d G . . . .
C3 C 0.2529(3) 0.3215(4) 0.4456(3) 0.086(3) Uani 1 1 d G . . . .
H3 H 0.2955 0.3363 0.4762 0.104 Uiso 1 1 calc DR U . . .
C4 C 0.2024(4) 0.3655(3) 0.4414(3) 0.103(4) Uani 1 1 d G . . . .
H4 H 0.2113 0.4097 0.4692 0.124 Uiso 1 1 calc R U . . .
C5 C 0.1388(3) 0.3435(3) 0.3957(3) 0.095(3) Uani 1 1 d G U . . .
H5 H 0.1050 0.3730 0.3929 0.115 Uiso 1 1 calc R U . . .
C6 C 0.1255(2) 0.2775(3) 0.3541(3) 0.061(2) Uani 1 1 d G U . . .
C7 C 0.1760(3) 0.2335(3) 0.3583(2) 0.052(2) Uani 1 1 d G U . . .
C8 C 0.0583(4) 0.2600(5) 0.3095(4) 0.058(2) Uani 1 1 d . . . . .
H8 H 0.0291 0.2977 0.3070 0.069 Uiso 1 1 calc R U . . .
C9 C 0.2741(5) -0.0209(7) 0.2061(5) 0.102(4) Uani 1 1 d . U . . .
H9A H 0.2756 -0.0774 0.2041 0.153 Uiso 1 1 calc DR U . . .
H9B H 0.3159 -0.0013 0.2401 0.153 Uiso 1 1 calc R U . . .
H9C H 0.2620 0.0008 0.1620 0.153 Uiso 1 1 calc R U . . .
C10 C 0.1689(2) -0.0331(4) 0.1873(3) 0.069(2) Uani 1 1 d G U . . .
C11 C 0.1492(3) -0.0819(4) 0.1307(3) 0.107(4) Uani 1 1 d G U . . .
H11 H 0.1766 -0.0909 0.1140 0.128 Uiso 1 1 calc DR U . . .
C12 C 0.0886(3) -0.1173(4) 0.0990(3) 0.129(5) Uani 1 1 d G U . . .
H12 H 0.0755 -0.1500 0.0611 0.155 Uiso 1 1 calc R U . . .
C13 C 0.0477(3) -0.1039(4) 0.1239(3) 0.097(3) Uani 1 1 d G U . . .
H13 H 0.0071 -0.1276 0.1027 0.116 Uiso 1 1 calc R U . . .
C14 C 0.0673(2) -0.0551(4) 0.1805(3) 0.067(3) Uani 1 1 d G . . . .
C15 C 0.1279(2) -0.0197(3) 0.2122(2) 0.058(2) Uani 1 1 d G . . . .
C16 C 0.0214(4) -0.0454(5) 0.2031(4) 0.062(2) Uani 1 1 d . U . . .
H16 H -0.0112 -0.0827 0.1891 0.074 Uiso 1 1 calc R U . . .
C17 C 0.3012(5) 0.1743(6) 0.2689(5) 0.071(3) Uani 1 1 d . U . . .
C18 C 0.3266(3) 0.2213(4) 0.2319(3) 0.067(2) Uani 1 1 d G U . . .
C19 C 0.3803(3) 0.1937(4) 0.2310(3) 0.095(3) Uani 1 1 d G U . . .
H19 H 0.4013 0.1481 0.2550 0.114 Uiso 1 1 calc R U . . .
C20 C 0.4027(3) 0.2343(5) 0.1942(4) 0.104(4) Uani 1 1 d G U . . .
H20 H 0.4386 0.2159 0.1936 0.125 Uiso 1 1 calc R U . . .
C21 C 0.3714(3) 0.3025(4) 0.1584(3) 0.099(4) Uani 1 1 d G U . . .
H21 H 0.3863 0.3297 0.1338 0.119 Uiso 1 1 calc R U . . .
C22 C 0.3177(3) 0.3301(3) 0.1593(3) 0.085(3) Uani 1 1 d G U . . .
H22 H 0.2967 0.3757 0.1353 0.102 Uiso 1 1 calc R U . . .
C23 C 0.2953(3) 0.2895(4) 0.1960(3) 0.074(3) Uani 1 1 d G U . . .
H23 H 0.2593 0.3079 0.1966 0.089 Uiso 1 1 calc R U . . .
C24 C 0.3480(4) -0.0164(6) 0.4283(5) 0.064(2) Uani 1 1 d . U . . .
C25 C 0.3972(3) -0.0692(4) 0.4804(3) 0.071(3) Uani 1 1 d G U . . .
C26 C 0.4552(4) -0.0373(4) 0.5322(4) 0.110(4) Uani 1 1 d G U . . .
H26 H 0.4621 0.0169 0.5342 0.132 Uiso 1 1 calc R U . . .
C27 C 0.5028(3) -0.0866(5) 0.5812(3) 0.123(4) Uani 1 1 d G U . . .
H27 H 0.5416 -0.0653 0.6159 0.148 Uiso 1 1 calc R U . . .
C28 C 0.4925(4) -0.1676(5) 0.5783(4) 0.121(4) Uani 1 1 d G U . . .
H28 H 0.5244 -0.2005 0.6110 0.146 Uiso 1 1 calc R U . . .
C29 C 0.4346(4) -0.1994(3) 0.5264(4) 0.140(5) Uani 1 1 d G U . . .
H29 H 0.4277 -0.2536 0.5245 0.168 Uiso 1 1 calc R U . . .
C30 C 0.3869(3) -0.1502(4) 0.4775(4) 0.104(4) Uani 1 1 d G U . . .
H30 H 0.3481 -0.1714 0.4428 0.124 Uiso 1 1 calc R U . . .
C31 C 0.1689(4) 0.0281(4) 0.4122(4) 0.0463(19) Uani 1 1 d . . . . .
C32 C 0.1751(3) -0.0261(3) 0.4671(2) 0.052(2) Uani 1 1 d G U . . .
C33 C 0.2295(2) -0.0736(3) 0.5029(3) 0.065(2) Uani 1 1 d G U . . .
H33 H 0.2631 -0.0695 0.4945 0.078 Uiso 1 1 calc R U . . .
C34 C 0.2335(3) -0.1273(3) 0.5512(3) 0.088(3) Uani 1 1 d G U . . .
H34 H 0.2699 -0.1591 0.5752 0.105 Uiso 1 1 calc R U . . .
C35 C 0.1832(3) -0.1335(4) 0.5638(3) 0.097(3) Uani 1 1 d G U . . .
H35 H 0.1859 -0.1694 0.5961 0.116 Uiso 1 1 calc R U . . .
C36 C 0.1288(3) -0.0860(4) 0.5279(3) 0.097(3) Uani 1 1 d G U . . .
H36 H 0.0951 -0.0901 0.5363 0.117 Uiso 1 1 calc R U . . .
C37 C 0.1247(2) -0.0323(3) 0.4796(3) 0.077(3) Uani 1 1 d G U . . .
H37 H 0.0883 -0.0005 0.4557 0.092 Uiso 1 1 calc R U . . .
C38 C 0.0046(4) 0.1363(7) 0.1060(4) 0.088(3) Uani 1 1 d . U . . .
H38A H -0.0296 0.1114 0.1089 0.133 Uiso 1 1 calc R U . . .
H38B H 0.0141 0.1057 0.0768 0.133 Uiso 1 1 calc R U . . .
H38C H -0.0085 0.1884 0.0874 0.133 Uiso 1 1 calc R U . . .
C39 C 0.1147(7) 0.3227(8) 0.1778(7) 0.148(6) Uani 1 1 d . . . . .
H39A H 0.0897 0.3150 0.1992 0.221 Uiso 1 1 calc R U . . .
H39B H 0.0900 0.3530 0.1365 0.221 Uiso 1 1 calc R U . . .
H39C H 0.1538 0.3505 0.2088 0.221 Uiso 1 1 calc R U . . .
Co1 Co 0.08871(5) 0.10189(6) 0.27600(5) 0.0447(3) Uani 1 1 d . . . . .
Gd1 Gd 0.25094(2) 0.08401(3) 0.33486(2) 0.05694(18) Uani 1 1 d . . . . .
N1 N 0.0338(3) 0.1973(3) 0.2723(3) 0.0464(15) Uani 1 1 d . . . . .
N2 N 0.0234(3) 0.0110(4) 0.2406(3) 0.0487(16) Uani 1 1 d . . . . .
O1 O 0.2854(3) 0.2067(4) 0.4069(3) 0.0728(18) Uani 1 1 d . U . . .
O2 O 0.1670(2) 0.1734(3) 0.3178(2) 0.0508(13) Uani 1 1 d . . . . .
O3 O 0.2279(3) 0.0016(4) 0.2237(3) 0.0713(17) Uani 1 1 d . . . . .
O4 O 0.1494(2) 0.0293(3) 0.2655(2) 0.0495(13) Uani 1 1 d . . . . .
O5 O 0.3358(3) 0.1227(4) 0.3116(3) 0.0813(19) Uani 1 1 d . U . . .
O6 O 0.2445(3) 0.1875(4) 0.2550(3) 0.0738(18) Uani 1 1 d . U . . .
O7 O 0.3500(3) 0.0557(4) 0.4411(3) 0.0726(17) Uani 1 1 d . U . . .
O8 O 0.3042(3) -0.0438(4) 0.3709(3) 0.0728(17) Uani 1 1 d . U . . .
O9 O 0.2194(2) 0.0386(3) 0.4111(2) 0.0568(14) Uani 1 1 d . U . . .
O10 O 0.1154(3) 0.0602(3) 0.3734(3) 0.0524(13) Uani 1 1 d . U . . .
O11 O 0.0600(3) 0.1411(4) 0.1719(3) 0.0673(16) Uani 1 1 d D U . . .
H11A H 0.0830 0.1774 0.1731 0.101 Uiso 1 1 calc DR U . . .
O12 O 0.1301(4) 0.2486(5) 0.1616(4) 0.101(2) Uani 1 1 d . U . . .
H12A H 0.1676 0.2373 0.1903 0.152 Uiso 1 1 calc R U . . .
O13 O 0.0000 0.4718(19) 0.2500 0.419(17) Uani 1 2 d S TU P . .


_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
C1 O1 1.423(10) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.354(8) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.433(8) . ?
C7 O2 1.314(6) . ?
C8 N1 1.294(9) . ?
C8 H8 0.9300 . ?
C9 O3 1.421(10) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.357(7) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C16 1.452(9) . ?
C15 O4 1.332(6) . ?
C16 N2 1.265(9) . ?
C16 H16 0.9300 . ?
C17 O5 1.251(10) . ?
C17 O6 1.256(11) . ?
C17 C18 1.502(10) . ?
C17 Gd1 2.818(9) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O7 1.250(10) . ?
C24 O8 1.268(10) . ?
C24 C25 1.470(10) . ?
C24 Gd1 2.783(9) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O9 1.246(9) . ?
C31 O10 1.251(9) . ?
C31 C32 1.493(8) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 O11 1.403(9) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 O12 1.412(13) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
Co1 O4 2.022(5) . ?
Co1 O2 2.022(5) . ?
Co1 N2 2.049(6) . ?
Co1 N1 2.065(6) . ?
Co1 O10 2.082(5) . ?
Co1 O11 2.195(5) . ?
Co1 Gd1 3.4395(12) . ?
Gd1 O4 2.315(5) . ?
Gd1 O9 2.354(5) . ?
Gd1 O2 2.396(5) . ?
Gd1 O7 2.410(5) . ?
Gd1 O8 2.434(6) . ?
Gd1 O5 2.457(6) . ?
Gd1 O6 2.469(5) . ?
Gd1 O1 2.507(6) . ?
Gd1 O3 2.680(6) . ?
N1 N1 1.409(11) 2 ?
N2 N2 1.401(11) 2 ?
O11 H11A 0.8200 . ?
O12 H12A 0.8200 . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.3(5) . . ?
O1 C2 C7 115.6(5) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C8 124.9(5) . . ?
C5 C6 C8 115.1(5) . . ?
O2 C7 C6 123.2(4) . . ?
O2 C7 C2 116.7(4) . . ?
C6 C7 C2 120.0 . . ?
N1 C8 C6 126.8(7) . . ?
N1 C8 H8 116.6 . . ?
C6 C8 H8 116.6 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 124.7(5) . . ?
O3 C10 C15 115.2(5) . . ?
C11 C10 C15 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 C16 124.1(5) . . ?
C13 C14 C16 115.9(5) . . ?
O4 C15 C14 123.4(4) . . ?
O4 C15 C10 116.6(4) . . ?
C14 C15 C10 120.0 . . ?
N2 C16 C14 123.7(7) . . ?
N2 C16 H16 118.1 . . ?
C14 C16 H16 118.1 . . ?
O5 C17 O6 121.6(8) . . ?
O5 C17 C18 120.1(9) . . ?
O6 C17 C18 118.2(9) . . ?
O5 C17 Gd1 60.5(5) . . ?
O6 C17 Gd1 61.1(5) . . ?
C18 C17 Gd1 178.4(6) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 119.1(6) . . ?
C23 C18 C17 120.8(6) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O7 C24 O8 120.6(9) . . ?
O7 C24 C25 119.3(8) . . ?
O8 C24 C25 120.1(9) . . ?
O7 C24 Gd1 59.8(5) . . ?
O8 C24 Gd1 60.9(5) . . ?
C25 C24 Gd1 176.2(6) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 119.2(7) . . ?
C30 C25 C24 120.8(7) . . ?
C25 C26 C27 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O9 C31 O10 126.1(7) . . ?
O9 C31 C32 115.5(7) . . ?
O10 C31 C32 118.3(7) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 120.0(5) . . ?
C37 C32 C31 119.9(5) . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C37 120.0 . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O11 C38 H38A 109.5 . . ?
O11 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O11 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O12 C39 H39A 109.5 . . ?
O12 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O12 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O4 Co1 O2 81.9(2) . . ?
O4 Co1 N2 87.5(2) . . ?
O2 Co1 N2 168.0(2) . . ?
O4 Co1 N1 164.1(2) . . ?
O2 Co1 N1 88.6(2) . . ?
N2 Co1 N1 102.9(2) . . ?
O4 Co1 O10 94.3(2) . . ?
O2 Co1 O10 90.3(2) . . ?
N2 Co1 O10 85.1(2) . . ?
N1 Co1 O10 98.5(2) . . ?
O4 Co1 O11 84.3(2) . . ?
O2 Co1 O11 91.2(2) . . ?
N2 Co1 O11 93.1(2) . . ?
N1 Co1 O11 83.2(2) . . ?
O10 Co1 O11 177.7(2) . . ?
O4 Co1 Gd1 40.61(13) . . ?
O2 Co1 Gd1 42.97(15) . . ?
N2 Co1 Gd1 125.35(17) . . ?
N1 Co1 Gd1 131.61(16) . . ?
O10 Co1 Gd1 83.86(15) . . ?
O11 Co1 Gd1 96.10(16) . . ?
O4 Gd1 O9 74.78(17) . . ?
O4 Gd1 O2 68.43(17) . . ?
O9 Gd1 O2 75.87(18) . . ?
O4 Gd1 O7 139.1(2) . . ?
O9 Gd1 O7 74.35(19) . . ?
O2 Gd1 O7 127.4(2) . . ?
O4 Gd1 O8 93.59(19) . . ?
O9 Gd1 O8 77.2(2) . . ?
O2 Gd1 O8 150.73(18) . . ?
O7 Gd1 O8 53.7(2) . . ?
O4 Gd1 O5 131.99(19) . . ?
O9 Gd1 O5 150.42(19) . . ?
O2 Gd1 O5 121.9(2) . . ?
O7 Gd1 O5 76.2(2) . . ?
O8 Gd1 O5 87.4(2) . . ?
O4 Gd1 O6 98.19(18) . . ?
O9 Gd1 O6 148.4(2) . . ?
O2 Gd1 O6 72.96(18) . . ?
O7 Gd1 O6 122.0(2) . . ?
O8 Gd1 O6 134.4(2) . . ?
O5 Gd1 O6 52.75(19) . . ?
O4 Gd1 O1 130.78(19) . . ?
O9 Gd1 O1 85.08(19) . . ?
O2 Gd1 O1 63.20(18) . . ?
O7 Gd1 O1 71.9(2) . . ?
O8 Gd1 O1 125.4(2) . . ?
O5 Gd1 O1 83.6(2) . . ?
O6 Gd1 O1 76.4(2) . . ?
O4 Gd1 O3 61.29(17) . . ?
O9 Gd1 O3 122.34(19) . . ?
O2 Gd1 O3 115.50(16) . . ?
O7 Gd1 O3 117.0(2) . . ?
O8 Gd1 O3 70.71(19) . . ?
O5 Gd1 O3 74.1(2) . . ?
O6 Gd1 O3 76.9(2) . . ?
O1 Gd1 O3 152.19(19) . . ?
O4 Gd1 C24 116.9(2) . . ?
O9 Gd1 C24 72.9(2) . . ?
O2 Gd1 C24 144.9(2) . . ?
O7 Gd1 C24 26.6(2) . . ?
O8 Gd1 C24 27.1(2) . . ?
O5 Gd1 C24 81.9(2) . . ?
O6 Gd1 C24 134.6(2) . . ?
O1 Gd1 C24 98.3(3) . . ?
O3 Gd1 C24 94.8(2) . . ?
O4 Gd1 C17 116.9(2) . . ?
O9 Gd1 C17 164.0(2) . . ?
O2 Gd1 C17 97.7(3) . . ?
O7 Gd1 C17 99.3(3) . . ?
O8 Gd1 C17 111.3(3) . . ?
O5 Gd1 C17 26.3(2) . . ?
O6 Gd1 C17 26.5(2) . . ?
O1 Gd1 C17 79.0(2) . . ?
O3 Gd1 C17 73.6(2) . . ?
C24 Gd1 C17 108.2(3) . . ?
O4 Gd1 Co1 34.64(13) . . ?
O9 Gd1 Co1 64.94(12) . . ?
O2 Gd1 Co1 35.11(11) . . ?
O7 Gd1 Co1 138.49(15) . . ?
O8 Gd1 Co1 120.48(15) . . ?
O5 Gd1 Co1 143.48(15) . . ?
O6 Gd1 Co1 91.52(13) . . ?
O1 Gd1 Co1 96.14(14) . . ?
O3 Gd1 Co1 92.31(12) . . ?
C24 Gd1 Co1 133.76(18) . . ?
C17 Gd1 Co1 117.6(2) . . ?
C8 N1 N1 116.0(5) . 2 ?
C8 N1 Co1 123.3(5) . . ?
N1 N1 Co1 120.7(3) 2 . ?
C16 N2 N2 116.9(6) . 2 ?
C16 N2 Co1 125.7(5) . . ?
N2 N2 Co1 117.4(4) 2 . ?
C2 O1 C1 116.7(7) . . ?
C2 O1 Gd1 119.2(4) . . ?
C1 O1 Gd1 124.1(6) . . ?
C7 O2 Co1 124.6(4) . . ?
C7 O2 Gd1 123.9(4) . . ?
Co1 O2 Gd1 101.9(2) . . ?
C10 O3 C9 116.3(7) . . ?
C10 O3 Gd1 116.1(4) . . ?
C9 O3 Gd1 126.6(6) . . ?
C15 O4 Co1 121.4(4) . . ?
C15 O4 Gd1 130.2(4) . . ?
Co1 O4 Gd1 104.7(2) . . ?
C17 O5 Gd1 93.2(5) . . ?
C17 O6 Gd1 92.5(6) . . ?
C24 O7 Gd1 93.5(5) . . ?
C24 O8 Gd1 92.0(6) . . ?
C31 O9 Gd1 139.0(5) . . ?
C31 O10 Co1 122.4(5) . . ?
C38 O11 Co1 136.7(5) . . ?
C38 O11 H11A 109.5 . . ?
Co1 O11 H11A 111.2 . . ?
C39 O12 H12A 109.5 . . ?

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
O1 C2 C3 C4 -176.4(6) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C8 179.4(6) . . . . ?
C5 C6 C7 O2 -175.8(6) . . . . ?
C8 C6 C7 O2 4.8(7) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C8 C6 C7 C2 -179.4(6) . . . . ?
O1 C2 C7 O2 -7.2(6) . . . . ?
C3 C2 C7 O2 176.1(5) . . . . ?
O1 C2 C7 C6 176.7(6) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C7 C6 C8 N1 8.2(11) . . . . ?
C5 C6 C8 N1 -171.2(7) . . . . ?
O3 C10 C11 C12 177.1(7) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C16 -179.4(7) . . . . ?
C13 C14 C15 O4 178.2(6) . . . . ?
C16 C14 C15 O4 -2.4(8) . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C16 C14 C15 C10 179.4(7) . . . . ?
O3 C10 C15 O4 4.3(6) . . . . ?
C11 C10 C15 O4 -178.3(6) . . . . ?
O3 C10 C15 C14 -177.4(6) . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C15 C14 C16 N2 19.9(11) . . . . ?
C13 C14 C16 N2 -160.7(7) . . . . ?
O5 C17 C18 C19 17.2(11) . . . . ?
O6 C17 C18 C19 -161.8(7) . . . . ?
O5 C17 C18 C23 -166.0(7) . . . . ?
O6 C17 C18 C23 15.0(11) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 176.9(6) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C17 C18 C23 C22 -176.8(6) . . . . ?
O7 C24 C25 C26 -20.1(10) . . . . ?
O8 C24 C25 C26 159.5(6) . . . . ?
O7 C24 C25 C30 161.2(7) . . . . ?
O8 C24 C25 C30 -19.2(10) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 -178.8(7) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 178.7(7) . . . . ?
O9 C31 C32 C33 -13.7(8) . . . . ?
O10 C31 C32 C33 168.4(5) . . . . ?
O9 C31 C32 C37 170.0(5) . . . . ?
O10 C31 C32 C37 -7.9(8) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C34 -176.3(5) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C31 C32 C37 C36 176.3(5) . . . . ?
C6 C8 N1 N1 -174.2(7) . . . 2 ?
C6 C8 N1 Co1 5.5(11) . . . . ?
C14 C16 N2 N2 -178.4(7) . . . 2 ?
C14 C16 N2 Co1 1.6(12) . . . . ?
C3 C2 O1 C1 -4.2(9) . . . . ?
C7 C2 O1 C1 179.3(6) . . . . ?
C3 C2 O1 Gd1 174.5(3) . . . . ?
C7 C2 O1 Gd1 -2.0(6) . . . . ?
C6 C7 O2 Co1 -29.9(6) . . . . ?
C2 C7 O2 Co1 154.1(3) . . . . ?
C6 C7 O2 Gd1 -169.9(3) . . . . ?
C2 C7 O2 Gd1 14.2(6) . . . . ?
C11 C10 O3 C9 -6.7(9) . . . . ?
C15 C10 O3 C9 170.5(6) . . . . ?
C11 C10 O3 Gd1 -176.1(3) . . . . ?
C15 C10 O3 Gd1 1.2(6) . . . . ?
C14 C15 O4 Co1 -32.9(7) . . . . ?
C10 C15 O4 Co1 145.4(4) . . . . ?
C14 C15 O4 Gd1 172.0(3) . . . . ?
C10 C15 O4 Gd1 -9.7(7) . . . . ?
O6 C17 O5 Gd1 0.7(10) . . . . ?
C18 C17 O5 Gd1 -178.3(7) . . . . ?
O5 C17 O6 Gd1 -0.7(10) . . . . ?
C18 C17 O6 Gd1 178.3(7) . . . . ?
O8 C24 O7 Gd1 4.6(8) . . . . ?
C25 C24 O7 Gd1 -175.8(6) . . . . ?
O7 C24 O8 Gd1 -4.6(8) . . . . ?
C25 C24 O8 Gd1 175.8(7) . . . . ?
O10 C31 O9 Gd1 -20.8(13) . . . . ?
C32 C31 O9 Gd1 161.5(5) . . . . ?
O9 C31 O10 Co1 25.2(11) . . . . ?
C32 C31 O10 Co1 -157.1(4) . . . . ?

_refine_diff_density_max         0.958
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.112

####################################################################### 
# 
# 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_Gd2Cu2
_audit_block_doi                 10.5517/cc14htbs
_database_code_depnum_ccdc_archive 'CCDC 1057885'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H66 Cu2 Gd2 N4 O24'
_chemical_formula_sum            'C74 H66 Cu2 Gd2 N4 O24'
_chemical_formula_weight         1836.88

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.668(18)
_cell_length_b                   16.575(13)
_cell_length_c                   23.13(2)
_cell_angle_alpha                90
_cell_angle_beta                 119.671(14)
_cell_angle_gamma                90
_cell_volume                     7885(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4644
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      23.46

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_F_000             3664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.268
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            22086
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.588
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6938
_reflns_number_gt                3644
_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.

 The command 'isor' was also used to restrain the C, O AND Gd atom with 
 NPD and ADP problems. The restraint command lead to restraint number 224,
 but cannot be completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the C25-C24 and C9-O3 distance to
 be in the reasonable range

 The compounds show large solvent accessible void and the sovlents cannot be 
 determined because the diffractions were collected at room temperature.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.1543P)²+99.4973P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00027(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6938
_refine_ls_number_parameters     445
_refine_ls_number_restraints     224
_refine_ls_R_factor_all          0.1573
_refine_ls_R_factor_gt           0.0833
_refine_ls_wR_factor_ref         0.2959
_refine_ls_wR_factor_gt          0.2256
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.043
_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
C1 C 0.2814(9) 0.4745(14) 0.7130(11) 0.116(7) Uani 1 1 d . U . . .
H1A H 0.2901 0.4181 0.7225 0.174 Uiso 1 1 calc R U . . .
H1B H 0.3206 0.5048 0.7389 0.174 Uiso 1 1 calc R U . . .
H1C H 0.2658 0.4838 0.6665 0.174 Uiso 1 1 calc R U . . .
C2 C 0.1727(4) 0.4694(7) 0.6912(6) 0.081(4) Uani 1 1 d G U . . .
C3 C 0.1552(6) 0.4166(9) 0.6383(7) 0.129(7) Uani 1 1 d G U . . .
H3 H 0.1851 0.4030 0.6250 0.155 Uiso 1 1 calc R U . . .
C4 C 0.0929(7) 0.3841(8) 0.6054(6) 0.145(8) Uani 1 1 d G U . . .
H4 H 0.0811 0.3487 0.5700 0.174 Uiso 1 1 calc R U . . .
C5 C 0.0481(5) 0.4044(8) 0.6254(6) 0.122(7) Uani 1 1 d G U . . .
H5 H 0.0065 0.3826 0.6034 0.147 Uiso 1 1 calc R U . . .
C6 C 0.0657(4) 0.4572(7) 0.6783(6) 0.084(5) Uani 1 1 d G . . . .
C7 C 0.1280(5) 0.4897(6) 0.7112(5) 0.060(3) Uani 1 1 d G . . . .
C8 C 0.0191(6) 0.4701(9) 0.7006(8) 0.070(4) Uani 1 1 d . . . . .
H8 H -0.0171 0.4364 0.6840 0.085 Uiso 1 1 calc R U . . .
C9 C 0.3516(7) 0.7276(13) 0.9549(9) 0.136(8) Uani 1 1 d D U . . .
H9A H 0.3678 0.7623 0.9332 0.204 Uiso 1 1 calc R U . . .
H9B H 0.3777 0.6797 0.9700 0.204 Uiso 1 1 calc R U . . .
H9C H 0.3535 0.7553 0.9923 0.204 Uiso 1 1 calc R U . . .
C10 C 0.2425(10) 0.7552(11) 0.9061(8) 0.084(5) Uani 1 1 d . U . . .
C11 C 0.2513(12) 0.8244(13) 0.9454(10) 0.114(6) Uani 1 1 d . U . . .
H11 H 0.2933 0.8394 0.9768 0.137 Uiso 1 1 calc R U . . .
C12 C 0.2026(12) 0.8680(13) 0.9393(10) 0.114(6) Uani 1 1 d . U . . .
H12 H 0.2115 0.9143 0.9650 0.137 Uiso 1 1 calc R U . . .
C13 C 0.1388(12) 0.8481(13) 0.8964(10) 0.122(8) Uani 1 1 d . . . . .
H13 H 0.1054 0.8798 0.8940 0.146 Uiso 1 1 calc R U . . .
C14 C 0.1246(10) 0.7784(10) 0.8556(7) 0.084(5) Uani 1 1 d . . . . .
C15 C 0.1755(8) 0.7345(11) 0.8600(7) 0.074(4) Uani 1 1 d . . . . .
C16 C 0.0567(8) 0.7622(9) 0.8095(7) 0.075(4) Uani 1 1 d . . . . .
H16 H 0.0269 0.8012 0.8060 0.090 Uiso 1 1 calc R U . . .
C17 C 0.1700(7) 0.5227(9) 0.9152(6) 0.059(3) Uani 1 1 d . . . . .
C18 C 0.1767(7) 0.4686(9) 0.9705(7) 0.063(4) Uani 1 1 d . . . . .
C19 C 0.1292(9) 0.4645(11) 0.9880(9) 0.091(5) Uani 1 1 d . U . . .
H19 H 0.0912 0.4938 0.9634 0.109 Uiso 1 1 calc R U . . .
C20 C 0.1357(13) 0.4178(15) 1.0415(13) 0.134(8) Uani 1 1 d . U . . .
H20 H 0.1056 0.4194 1.0561 0.161 Uiso 1 1 calc R U . . .
C21 C 0.1906(13) 0.3689(15) 1.0711(13) 0.133(8) Uani 1 1 d . U . . .
H21 H 0.1952 0.3333 1.1042 0.160 Uiso 1 1 calc R U . . .
C22 C 0.2366(11) 0.3704(13) 1.0545(11) 0.113(6) Uani 1 1 d . U . . .
H22 H 0.2732 0.3377 1.0768 0.136 Uiso 1 1 calc R U . . .
C23 C 0.2300(8) 0.4219(9) 1.0028(8) 0.075(4) Uani 1 1 d . . . . .
H23 H 0.2624 0.4235 0.9911 0.090 Uiso 1 1 calc R U . . .
C24 C 0.3504(9) 0.4783(13) 0.9282(9) 0.096(5) Uani 1 1 d D U . . .
C25 C 0.3969(7) 0.4199(10) 0.9782(7) 0.102(6) Uani 1 1 d DG U . . .
C26 C 0.4552(9) 0.4496(9) 1.0295(9) 0.166(10) Uani 1 1 d G U . . .
H26 H 0.4646 0.5044 1.0314 0.200 Uiso 1 1 calc R U . . .
C27 C 0.4995(7) 0.3975(13) 1.0778(7) 0.145(9) Uani 1 1 d G U . . .
H27 H 0.5385 0.4174 1.1120 0.174 Uiso 1 1 calc R U . . .
C28 C 0.4854(9) 0.3157(12) 1.0748(8) 0.177(11) Uani 1 1 d G U . . .
H28 H 0.5150 0.2809 1.1072 0.213 Uiso 1 1 calc R U . . .
C29 C 0.4271(10) 0.2860(8) 1.0236(10) 0.184(12) Uani 1 1 d G U . . .
H29 H 0.4177 0.2313 1.0217 0.221 Uiso 1 1 calc R U . . .
C30 C 0.3829(7) 0.3381(11) 0.9753(8) 0.147(9) Uani 1 1 d G U . . .
H30 H 0.3438 0.3182 0.9411 0.176 Uiso 1 1 calc R U . . .
C31 C 0.3067(10) 0.6730(11) 0.7733(9) 0.090(5) Uani 1 1 d . U . . .
C32 C 0.3315(6) 0.7221(7) 0.7350(5) 0.085(5) Uani 1 1 d G U . . .
C33 C 0.2998(5) 0.7906(8) 0.6987(6) 0.097(5) Uani 1 1 d G U . . .
H33 H 0.2636 0.8103 0.6998 0.116 Uiso 1 1 calc R U . . .
C34 C 0.3224(7) 0.8297(7) 0.6610(6) 0.126(7) Uani 1 1 d G U . . .
H34 H 0.3013 0.8755 0.6367 0.151 Uiso 1 1 calc R U . . .
C35 C 0.3767(7) 0.8002(9) 0.6594(6) 0.113(6) Uani 1 1 d G U . . .
H35 H 0.3918 0.8263 0.6341 0.136 Uiso 1 1 calc R U . . .
C36 C 0.4083(6) 0.7317(9) 0.6957(7) 0.129(7) Uani 1 1 d G U . . .
H36 H 0.4446 0.7120 0.6947 0.155 Uiso 1 1 calc R U . . .
C37 C 0.3857(6) 0.6926(7) 0.7335(6) 0.109(6) Uani 1 1 d G U . . .
H37 H 0.4069 0.6468 0.7577 0.131 Uiso 1 1 calc R U . . .
Cu1 Cu 0.09172(8) 0.60600(10) 0.78155(8) 0.0560(5) Uani 1 1 d . . . . .
Gd1 Gd 0.25432(3) 0.58264(6) 0.83743(3) 0.0775(4) Uani 1 1 d . U . . .
N1 N 0.0246(4) 0.5244(6) 0.7413(5) 0.049(2) Uani 1 1 d . . . . .
N2 N 0.0335(5) 0.6983(6) 0.7725(5) 0.058(3) Uani 1 1 d . . . . .
O1 O 0.2332(5) 0.4998(7) 0.7293(5) 0.086(3) Uani 1 1 d . U . . .
O2 O 0.1484(4) 0.5383(6) 0.7623(4) 0.062(2) Uani 1 1 d . . . . .
O3 O 0.2860(5) 0.7063(8) 0.9094(5) 0.097(4) Uani 1 1 d D U . . .
O4 O 0.1678(4) 0.6721(6) 0.8218(4) 0.071(3) Uani 1 1 d . . . . .
O5 O 0.1158(5) 0.5570(6) 0.8808(4) 0.068(3) Uani 1 1 d . . . . .
O6 O 0.2184(5) 0.5312(6) 0.9085(4) 0.070(3) Uani 1 1 d . U . . .
O7 O 0.3067(6) 0.4492(8) 0.8701(6) 0.098(4) Uani 1 1 d . U . . .
O8 O 0.3511(6) 0.5494(9) 0.9395(6) 0.103(4) Uani 1 1 d . U . . .
O9 O 0.2492(6) 0.6892(8) 0.7601(5) 0.093(3) Uani 1 1 d . U . . .
O10 O 0.3401(6) 0.6194(8) 0.8138(6) 0.100(4) Uani 1 1 d . U . . .
O11 O 0.1360(13) 0.7856(16) 0.6766(11) 0.238(11) Uani 1 1 d . U . . .
O12 O 0.0204(17) 0.3366(19) 0.1192(17) 0.302(14) 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
C1 O1 1.430(18) . ?
C2 O1 1.353(13) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C6 C8 1.447(16) . ?
C7 O2 1.309(11) . ?
C8 N1 1.262(16) . ?
C9 O3 1.423(9) . ?
C10 O3 1.28(2) . ?
C10 C11 1.41(3) . ?
C10 C15 1.45(2) . ?
C11 C12 1.31(3) . ?
C12 C13 1.37(3) . ?
C13 C14 1.42(2) . ?
C14 C15 1.37(2) . ?
C14 C16 1.45(2) . ?
C15 O4 1.313(18) . ?
C16 N2 1.300(17) . ?
C17 O6 1.237(16) . ?
C17 O5 1.261(16) . ?
C17 C18 1.505(18) . ?
C18 C23 1.35(2) . ?
C18 C19 1.37(2) . ?
C19 C20 1.40(3) . ?
C20 C21 1.39(3) . ?
C21 C22 1.32(3) . ?
C22 C23 1.41(2) . ?
C24 O8 1.21(2) . ?
C24 O7 1.32(2) . ?
C24 C25 1.492(10) . ?
C24 Gd1 2.801(14) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C31 O10 1.25(2) . ?
C31 O9 1.27(2) . ?
C31 C32 1.519(18) . ?
C31 Gd1 2.792(17) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
Cu1 O4 1.911(9) . ?
Cu1 N1 1.937(10) . ?
Cu1 O2 1.962(9) . ?
Cu1 N2 1.999(11) . ?
Cu1 O5 2.227(9) . ?
Cu1 Gd1 3.421(3) . ?
Gd1 O6 2.353(9) . ?
Gd1 O2 2.353(8) . ?
Gd1 O8 2.402(12) . ?
Gd1 O4 2.406(11) . ?
Gd1 O10 2.428(11) . ?
Gd1 O7 2.465(13) . ?
Gd1 O9 2.474(10) . ?
Gd1 O3 2.509(13) . ?
Gd1 O1 2.674(11) . ?
N1 N1 1.408(18) 2_556 ?
N2 N2 1.40(2) 2_556 ?

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
O1 C2 C3 124.5(9) . . ?
O1 C2 C7 115.3(9) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C8 122.4(9) . . ?
C5 C6 C8 117.3(9) . . ?
O2 C7 C6 123.4(8) . . ?
O2 C7 C2 116.6(8) . . ?
C6 C7 C2 120.0 . . ?
N1 C8 C6 123.8(12) . . ?
O3 C10 C11 128.0(18) . . ?
O3 C10 C15 116.6(16) . . ?
C11 C10 C15 115(2) . . ?
C12 C11 C10 123(2) . . ?
C11 C12 C13 123(2) . . ?
C12 C13 C14 119(2) . . ?
C15 C14 C13 118.2(18) . . ?
C15 C14 C16 124.8(14) . . ?
C13 C14 C16 117(2) . . ?
O4 C15 C14 123.1(14) . . ?
O4 C15 C10 114.8(18) . . ?
C14 C15 C10 122.1(17) . . ?
N2 C16 C14 126.1(15) . . ?
O6 C17 O5 125.7(13) . . ?
O6 C17 C18 117.4(13) . . ?
O5 C17 C18 116.9(13) . . ?
C23 C18 C19 119.1(14) . . ?
C23 C18 C17 119.4(13) . . ?
C19 C18 C17 121.5(14) . . ?
C18 C19 C20 122.7(19) . . ?
C21 C20 C19 115(2) . . ?
C22 C21 C20 123(2) . . ?
C21 C22 C23 120(2) . . ?
C18 C23 C22 119.8(17) . . ?
O8 C24 O7 119.9(14) . . ?
O8 C24 C25 122.7(19) . . ?
O7 C24 C25 117.3(18) . . ?
O8 C24 Gd1 58.5(8) . . ?
O7 C24 Gd1 61.6(8) . . ?
C25 C24 Gd1 174.5(12) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 118.1(16) . . ?
C30 C25 C24 121.9(16) . . ?
C25 C26 C27 120.0 . . ?
C28 C27 C26 120.0 . . ?
C27 C28 C29 120.0 . . ?
C30 C29 C28 120.0 . . ?
C29 C30 C25 120.0 . . ?
O10 C31 O9 122.6(16) . . ?
O10 C31 C32 122.3(18) . . ?
O9 C31 C32 115.1(16) . . ?
O10 C31 Gd1 60.2(9) . . ?
O9 C31 Gd1 62.4(8) . . ?
C32 C31 Gd1 176.9(13) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 122.8(12) . . ?
C37 C32 C31 117.1(12) . . ?
C32 C33 C34 120.0 . . ?
C33 C34 C35 120.0 . . ?
C36 C35 C34 120.0 . . ?
C35 C36 C37 120.0 . . ?
C36 C37 C32 120.0 . . ?
O4 Cu1 N1 170.1(4) . . ?
O4 Cu1 O2 81.6(4) . . ?
N1 Cu1 O2 88.9(4) . . ?
O4 Cu1 N2 92.6(4) . . ?
N1 Cu1 N2 97.2(4) . . ?
O2 Cu1 N2 158.0(4) . . ?
O4 Cu1 O5 90.5(4) . . ?
N1 Cu1 O5 88.4(4) . . ?
O2 Cu1 O5 99.8(4) . . ?
N2 Cu1 O5 101.5(4) . . ?
O4 Cu1 Gd1 43.0(3) . . ?
N1 Cu1 Gd1 127.1(3) . . ?
O2 Cu1 Gd1 41.7(3) . . ?
N2 Cu1 Gd1 135.6(3) . . ?
O5 Cu1 Gd1 84.4(3) . . ?
O6 Gd1 O2 77.4(3) . . ?
O6 Gd1 O8 74.3(4) . . ?
O2 Gd1 O8 143.5(4) . . ?
O6 Gd1 O4 75.7(3) . . ?
O2 Gd1 O4 64.2(3) . . ?
O8 Gd1 O4 128.0(4) . . ?
O6 Gd1 O10 151.7(4) . . ?
O2 Gd1 O10 128.1(4) . . ?
O8 Gd1 O10 77.4(4) . . ?
O4 Gd1 O10 123.8(4) . . ?
O6 Gd1 O7 76.2(4) . . ?
O2 Gd1 O7 97.9(4) . . ?
O8 Gd1 O7 53.3(5) . . ?
O4 Gd1 O7 149.4(4) . . ?
O10 Gd1 O7 86.8(4) . . ?
O6 Gd1 O9 149.1(4) . . ?
O2 Gd1 O9 92.1(4) . . ?
O8 Gd1 O9 123.8(4) . . ?
O4 Gd1 O9 73.6(4) . . ?
O10 Gd1 O9 53.5(4) . . ?
O7 Gd1 O9 134.4(4) . . ?
O6 Gd1 O3 85.7(4) . . ?
O2 Gd1 O3 127.2(4) . . ?
O8 Gd1 O3 73.1(5) . . ?
O4 Gd1 O3 63.2(4) . . ?
O10 Gd1 O3 86.3(4) . . ?
O7 Gd1 O3 126.1(4) . . ?
O9 Gd1 O3 77.8(4) . . ?
O6 Gd1 O1 120.2(4) . . ?
O2 Gd1 O1 60.7(3) . . ?
O8 Gd1 O1 116.6(4) . . ?
O4 Gd1 O1 115.1(3) . . ?
O10 Gd1 O1 73.1(4) . . ?
O7 Gd1 O1 70.1(4) . . ?
O9 Gd1 O1 76.7(4) . . ?
O3 Gd1 O1 153.6(4) . . ?
O6 Gd1 C31 167.0(5) . . ?
O2 Gd1 C31 111.5(5) . . ?
O8 Gd1 C31 100.8(5) . . ?
O4 Gd1 C31 99.1(5) . . ?
O10 Gd1 C31 26.5(5) . . ?
O7 Gd1 C31 110.8(5) . . ?
O9 Gd1 C31 27.0(5) . . ?
O3 Gd1 C31 81.3(5) . . ?
O1 Gd1 C31 72.8(5) . . ?
O6 Gd1 C24 72.1(4) . . ?
O2 Gd1 C24 122.3(5) . . ?
O8 Gd1 C24 25.3(5) . . ?
O4 Gd1 C24 143.9(4) . . ?
O10 Gd1 C24 82.2(5) . . ?
O7 Gd1 C24 28.0(5) . . ?
O9 Gd1 C24 135.6(5) . . ?
O3 Gd1 C24 98.1(6) . . ?
O1 Gd1 C24 95.2(5) . . ?
C31 Gd1 C24 108.7(6) . . ?
O6 Gd1 Cu1 65.0(2) . . ?
O2 Gd1 Cu1 33.7(2) . . ?
O8 Gd1 Cu1 138.1(3) . . ?
O4 Gd1 Cu1 32.8(2) . . ?
O10 Gd1 Cu1 142.8(3) . . ?
O7 Gd1 Cu1 121.2(3) . . ?
O9 Gd1 Cu1 90.1(3) . . ?
O3 Gd1 Cu1 94.0(3) . . ?
O1 Gd1 Cu1 92.9(2) . . ?
C31 Gd1 Cu1 116.8(5) . . ?
C24 Gd1 Cu1 134.2(4) . . ?
C8 N1 N1 114.7(10) . 2_556 ?
C8 N1 Cu1 127.9(9) . . ?
N1 N1 Cu1 117.4(7) 2_556 . ?
C16 N2 N2 116.3(10) . 2_556 ?
C16 N2 Cu1 120.7(10) . . ?
N2 N2 Cu1 123.1(5) 2_556 . ?
C2 O1 C1 116.3(13) . . ?
C2 O1 Gd1 116.6(7) . . ?
C1 O1 Gd1 126.4(11) . . ?
C7 O2 Cu1 124.7(7) . . ?
C7 O2 Gd1 129.9(7) . . ?
Cu1 O2 Gd1 104.6(4) . . ?
C10 O3 C9 115.8(17) . . ?
C10 O3 Gd1 120.6(9) . . ?
C9 O3 Gd1 123.6(14) . . ?
C15 O4 Cu1 124.2(10) . . ?
C15 O4 Gd1 124.1(10) . . ?
Cu1 O4 Gd1 104.3(5) . . ?
C17 O5 Cu1 118.5(8) . . ?
C17 O6 Gd1 143.7(9) . . ?
C24 O7 Gd1 90.3(10) . . ?
C24 O8 Gd1 96.2(10) . . ?
C31 O9 Gd1 90.7(10) . . ?
C31 O10 Gd1 93.3(11) . . ?

_refine_diff_density_max         1.509
_refine_diff_density_min         -1.844
_refine_diff_density_rms         0.165


# start Validation Reply Form
_vrf_PLAT973_x                   
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_Gd2Ni2
_audit_block_doi                 10.5517/cc14htct
_database_code_depnum_ccdc_archive 'CCDC 1057886'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H78 Gd2 N4 Ni2 O26'
_chemical_formula_sum            'C78 H78 Gd2 N4 Ni2 O26'
_chemical_formula_weight         1919.36

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'
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'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.011(8)
_cell_length_b                   16.677(6)
_cell_length_c                   22.589(10)
_cell_angle_alpha                90
_cell_angle_beta                 121.27(2)
_cell_angle_gamma                90
_cell_volume                     7731(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3081
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      21.20

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_F_000             3864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.256
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_T_max  0.623
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22209
_diffrn_reflns_av_unetI/netI     0.1852
_diffrn_reflns_av_R_equivalents  0.1594
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.573
_diffrn_reflns_theta_max         25.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7141
_reflns_number_gt                3013
_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.

 The command 'isor' was also used to restrain the C and O atom with NPD and ADP
 problems. The restraint command lead to restraint number 195, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the H11a-H12a, H11a-O11 and H12a-O12 distance to
 be in the reasonable range.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SAINT'
_computing_publication_material  'Bruker SAINT'
_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)+(0.1041P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7141
_refine_ls_number_parameters     451
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.2001
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.2539
_refine_ls_wR_factor_gt          0.1943
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      1.022
_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
C1 C 0.3504(8) 0.2265(11) 0.4496(10) 0.126(7) Uani 1 1 d . U . A 1
H1A H 0.3589 0.2778 0.4367 0.190 Uiso 1 1 calc R U . A 1
H1B H 0.3778 0.1867 0.4468 0.190 Uiso 1 1 calc R U . A 1
H1C H 0.3592 0.2290 0.4961 0.190 Uiso 1 1 calc R U . A 1
C2 C 0.2388(4) 0.2539(6) 0.4017(5) 0.076(4) Uani 1 1 d G U . A 1
C3 C 0.2526(4) 0.3199(7) 0.4448(5) 0.086(5) Uani 1 1 d G U . A 1
H3 H 0.2956 0.3349 0.4753 0.103 Uiso 1 1 calc R U . A 1
C4 C 0.2021(6) 0.3634(6) 0.4424(5) 0.101(6) Uani 1 1 d G U . A 1
H4 H 0.2113 0.4075 0.4713 0.122 Uiso 1 1 calc R U . A 1
C5 C 0.1378(5) 0.3409(6) 0.3969(6) 0.100(6) Uani 1 1 d G U . A 1
H5 H 0.1040 0.3701 0.3953 0.120 Uiso 1 1 calc R U . A 1
C6 C 0.1240(4) 0.2750(6) 0.3539(5) 0.066(4) Uani 1 1 d G . . A 1
C7 C 0.1745(5) 0.2315(5) 0.3563(4) 0.058(4) Uani 1 1 d G . . A 1
C8 C 0.0578(7) 0.2574(9) 0.3096(7) 0.067(4) Uani 1 1 d . U . A 1
H8 H 0.0280 0.2951 0.3068 0.080 Uiso 1 1 calc R U . A 1
C9 C 0.2737(8) -0.0253(12) 0.2069(9) 0.105(6) Uani 1 1 d . U . A 1
H9A H 0.2783 -0.0825 0.2106 0.157 Uiso 1 1 calc R U . A 1
H9B H 0.3149 -0.0006 0.2383 0.157 Uiso 1 1 calc R U . A 1
H9C H 0.2596 -0.0092 0.1603 0.157 Uiso 1 1 calc R U . A 1
C10 C 0.1675(4) -0.0345(6) 0.1870(5) 0.071(4) Uani 1 1 d G U . A 1
C11 C 0.1471(5) -0.0836(7) 0.1296(6) 0.111(6) Uani 1 1 d G U . A 1
H11 H 0.1746 -0.0930 0.1128 0.133 Uiso 1 1 calc R U . A 1
C12 C 0.0857(6) -0.1185(6) 0.0974(5) 0.134(7) Uani 1 1 d G U . A 1
H12 H 0.0720 -0.1514 0.0590 0.161 Uiso 1 1 calc R U . A 1
C13 C 0.0446(4) -0.1044(6) 0.1225(5) 0.094(5) Uani 1 1 d G U . A 1
H13 H 0.0034 -0.1278 0.1009 0.112 Uiso 1 1 calc R U . A 1
C14 C 0.0649(4) -0.0553(6) 0.1798(5) 0.070(4) Uani 1 1 d G . . A 1
C15 C 0.1264(4) -0.0203(5) 0.2121(4) 0.058(4) Uani 1 1 d G . . A 1
C16 C 0.0208(7) -0.0441(9) 0.2024(7) 0.066(4) Uani 1 1 d . . . A 1
H16 H -0.0118 -0.0823 0.1891 0.079 Uiso 1 1 calc R U . A 1
C17 C 0.3018(8) 0.1706(10) 0.2682(7) 0.073(4) Uani 1 1 d . . . A 1
C18 C 0.3263(5) 0.2184(7) 0.2311(5) 0.073(4) Uani 1 1 d G . . A 1
C19 C 0.3802(5) 0.1891(6) 0.2306(6) 0.101(6) Uani 1 1 d G U . A 1
H19 H 0.4004 0.1422 0.2543 0.121 Uiso 1 1 calc R U . A 1
C20 C 0.4040(5) 0.2299(8) 0.1946(6) 0.112(6) Uani 1 1 d G U . A 1
H20 H 0.4401 0.2103 0.1943 0.134 Uiso 1 1 calc R U . A 1
C21 C 0.3739(6) 0.3001(8) 0.1592(6) 0.110(6) Uani 1 1 d G . . A 1
H21 H 0.3899 0.3274 0.1352 0.132 Uiso 1 1 calc R U . A 1
C22 C 0.3200(6) 0.3294(6) 0.1597(6) 0.105(6) Uani 1 1 d G U . A 1
H22 H 0.2998 0.3764 0.1360 0.126 Uiso 1 1 calc R U . A 1
C23 C 0.2962(5) 0.2886(7) 0.1956(6) 0.080(5) Uani 1 1 d G U . A 1
H23 H 0.2601 0.3082 0.1960 0.096 Uiso 1 1 calc R U . A 1
C24 C 0.3487(8) -0.0153(13) 0.4275(9) 0.074(5) Uani 1 1 d . . . A 1
C25 C 0.3963(5) -0.0700(8) 0.4808(6) 0.084(5) Uani 1 1 d G . . A 1
C26 C 0.3850(5) -0.1521(8) 0.4771(6) 0.116(7) Uani 1 1 d G U . A 1
H26 H 0.3455 -0.1729 0.4422 0.140 Uiso 1 1 calc R U . A 1
C27 C 0.4328(7) -0.2031(6) 0.5255(8) 0.135(8) Uani 1 1 d G U . A 1
H27 H 0.4252 -0.2580 0.5231 0.162 Uiso 1 1 calc R U . A 1
C28 C 0.4918(6) -0.1719(8) 0.5776(7) 0.149(9) Uani 1 1 d G U . A 1
H28 H 0.5238 -0.2060 0.6100 0.179 Uiso 1 1 calc R U . A 1
C29 C 0.5031(5) -0.0898(9) 0.5813(6) 0.123(7) Uani 1 1 d G U . A 1
H29 H 0.5425 -0.0689 0.6162 0.148 Uiso 1 1 calc R U . A 1
C30 C 0.4553(6) -0.0388(6) 0.5329(7) 0.111(6) Uani 1 1 d G U . A 1
H30 H 0.4628 0.0161 0.5353 0.134 Uiso 1 1 calc R U . A 1
C31 C 0.1678(7) 0.0290(8) 0.4106(7) 0.054(3) Uani 1 1 d . U . A 1
C32 C 0.1736(5) -0.0246(5) 0.4649(4) 0.058(4) Uani 1 1 d G . . A 1
C33 C 0.2291(4) -0.0716(6) 0.5019(5) 0.073(4) Uani 1 1 d G U . A 1
H33 H 0.2631 -0.0672 0.4935 0.088 Uiso 1 1 calc R U . A 1
C34 C 0.2339(5) -0.1252(6) 0.5514(5) 0.096(5) Uani 1 1 d G U . A 1
H34 H 0.2710 -0.1567 0.5762 0.115 Uiso 1 1 calc R U . A 1
C35 C 0.1831(6) -0.1319(6) 0.5639(5) 0.108(6) Uani 1 1 d G U . A 1
H35 H 0.1863 -0.1678 0.5970 0.129 Uiso 1 1 calc R U . A 1
C36 C 0.1276(5) -0.0849(7) 0.5269(6) 0.100(6) Uani 1 1 d G U . A 1
H36 H 0.0937 -0.0893 0.5352 0.120 Uiso 1 1 calc R U . A 1
C37 C 0.1229(4) -0.0312(6) 0.4773(5) 0.084(5) Uani 1 1 d G U . A 1
H37 H 0.0858 0.0002 0.4526 0.101 Uiso 1 1 calc R U . A 1
C38 C 0.0051(8) 0.1376(11) 0.1077(8) 0.102(6) Uani 1 1 d . U . A 1
H38A H 0.0100 0.0957 0.0816 0.153 Uiso 1 1 calc R U . A 1
H38B H 0.0024 0.1884 0.0863 0.153 Uiso 1 1 calc R U . A 1
H38C H -0.0339 0.1288 0.1087 0.153 Uiso 1 1 calc R U . A 1
C39 C 0.1138(13) 0.3194(16) 0.1780(13) 0.170(10) Uani 1 1 d . U . B 1
H39A H 0.1409 0.3279 0.2270 0.254 Uiso 1 1 calc R U . B 1
H39B H 0.0700 0.3087 0.1663 0.254 Uiso 1 1 calc R U . B 1
H39C H 0.1144 0.3666 0.1539 0.254 Uiso 1 1 calc R U . B 1
Gd2 Gd 0.25037(3) 0.08272(5) 0.33381(4) 0.0672(3) Uani 1 1 d . . . A 1
N1 N 0.0220(4) 0.0132(6) 0.2391(5) 0.052(3) Uani 1 1 d . . . A 1
N2 N 0.0347(5) 0.1945(6) 0.2727(5) 0.053(3) Uani 1 1 d . . . A 1
Ni1 Ni 0.08865(7) 0.10155(10) 0.27508(8) 0.0518(5) Uani 1 1 d . . . A 1
O1 O 0.2848(4) 0.2060(7) 0.4044(5) 0.083(3) Uani 1 1 d . . . A 1
O2 O 0.1665(4) 0.1728(5) 0.3164(4) 0.058(2) Uani 1 1 d . . . A 1
O3 O 0.2267(4) -0.0005(7) 0.2238(5) 0.085(3) Uani 1 1 d . . . A 1
O4 O 0.1480(4) 0.0266(5) 0.2660(4) 0.056(2) Uani 1 1 d . . . A 1
O5 O 0.3037(5) -0.0459(7) 0.3712(6) 0.085(3) Uani 1 1 d . . . A 1
O6 O 0.3494(5) 0.0546(8) 0.4400(5) 0.081(3) Uani 1 1 d . . . A 1
O7 O 0.3345(5) 0.1197(7) 0.3097(6) 0.087(3) Uani 1 1 d . U . A 1
O8 O 0.2444(5) 0.1883(7) 0.2535(5) 0.088(3) Uani 1 1 d . U . A 1
O9 O 0.2191(4) 0.0384(6) 0.4099(4) 0.062(2) Uani 1 1 d . . . A 1
O10 O 0.1143(4) 0.0610(5) 0.3709(4) 0.058(2) Uani 1 1 d . . . A 1
O11 O 0.0607(4) 0.1376(6) 0.1776(4) 0.080(3) Uani 1 1 d D . . A 1
H11A H 0.0838(5) 0.1700(7) 0.1813(4) 0.120 Uiso 1 1 calc DR U . A 1
O12 O 0.1362(6) 0.2575(9) 0.1596(6) 0.129(5) Uani 1 1 d D U . B 1
H12A H 0.1067(7) 0.2425(9) 0.1173(8) 0.194 Uiso 1 1 calc DR U . B 1
O13 O 0.041(2) 0.479(2) 0.273(3) 0.51(3) Uani 1 1 d . U . C 1


_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
C1 O1 1.403(17) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.339(13) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.400(15) . ?
C7 O2 1.276(10) . ?
C8 N2 1.273(15) . ?
C8 H8 0.9300 . ?
C9 O3 1.428(16) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.343(11) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C16 1.406(14) . ?
C15 O4 1.307(10) . ?
C16 N1 1.257(14) . ?
C16 H16 0.9300 . ?
C17 O7 1.205(16) . ?
C17 O8 1.274(17) . ?
C17 C18 1.482(16) . ?
C17 Gd2 2.788(15) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O6 1.198(18) . ?
C24 O5 1.272(19) . ?
C24 C25 1.470(18) . ?
C24 Gd2 2.745(17) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O10 1.241(15) . ?
C31 O9 1.251(14) . ?
C31 C32 1.464(14) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 O11 1.445(16) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 O12 1.33(2) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
Gd2 O4 2.314(8) . ?
Gd2 O9 2.325(8) . ?
Gd2 O2 2.375(9) . ?
Gd2 O6 2.389(10) . ?
Gd2 O5 2.415(11) . ?
Gd2 O7 2.429(10) . ?
Gd2 O1 2.467(11) . ?
Gd2 O8 2.478(10) . ?
Gd2 O3 2.638(10) . ?
Gd2 Ni1 3.404(2) . ?
N1 N1 1.375(19) 2 ?
N1 Ni1 2.011(10) . ?
N2 N2 1.433(19) 2 ?
N2 Ni1 2.003(11) . ?
Ni1 O4 1.984(9) . ?
Ni1 O2 1.991(8) . ?
Ni1 O11 2.031(8) . ?
Ni1 O10 2.035(8) . ?
O11 H11A 0.748(10) . ?
O12 H12A 0.881(10) . ?
O13 O13 1.69(8) 2 ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.3(9) . . ?
O1 C2 C7 116.5(9) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C8 115.8(9) . . ?
C7 C6 C8 124.2(10) . . ?
O2 C7 C6 124.4(8) . . ?
O2 C7 C2 115.5(8) . . ?
C6 C7 C2 120.0 . . ?
N2 C8 C6 126.0(13) . . ?
N2 C8 H8 117.0 . . ?
C6 C8 H8 117.0 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 124.9(8) . . ?
O3 C10 C15 115.1(8) . . ?
C11 C10 C15 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C16 116.7(9) . . ?
C15 C14 C16 123.3(9) . . ?
O4 C15 C14 122.7(7) . . ?
O4 C15 C10 117.3(7) . . ?
C14 C15 C10 120.0 . . ?
N1 C16 C14 125.2(13) . . ?
N1 C16 H16 117.4 . . ?
C14 C16 H16 117.4 . . ?
O7 C17 O8 123.1(14) . . ?
O7 C17 C18 122.0(14) . . ?
O8 C17 C18 114.9(14) . . ?
O7 C17 Gd2 60.4(8) . . ?
O8 C17 Gd2 62.7(8) . . ?
C18 C17 Gd2 177.5(11) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 117.4(11) . . ?
C23 C18 C17 122.6(11) . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O6 C24 O5 121.9(16) . . ?
O6 C24 C25 120.0(16) . . ?
O5 C24 C25 117.7(18) . . ?
O6 C24 Gd2 60.3(9) . . ?
O5 C24 Gd2 61.6(8) . . ?
C25 C24 Gd2 173.2(10) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 121.2(12) . . ?
C30 C25 C24 118.6(12) . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 120.0 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O10 C31 O9 126.5(12) . . ?
O10 C31 C32 118.7(11) . . ?
O9 C31 C32 114.8(12) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 119.6(8) . . ?
C37 C32 C31 120.3(8) . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C37 120.0 . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O11 C38 H38A 109.5 . . ?
O11 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O11 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O12 C39 H39A 109.5 . . ?
O12 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O12 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O4 Gd2 O9 73.8(3) . . ?
O4 Gd2 O2 68.2(3) . . ?
O9 Gd2 O2 75.7(3) . . ?
O4 Gd2 O6 138.3(4) . . ?
O9 Gd2 O6 74.3(3) . . ?
O2 Gd2 O6 127.3(4) . . ?
O4 Gd2 O5 93.5(4) . . ?
O9 Gd2 O5 77.0(3) . . ?
O2 Gd2 O5 150.4(3) . . ?
O6 Gd2 O5 53.4(4) . . ?
O4 Gd2 O7 132.5(3) . . ?
O9 Gd2 O7 150.7(3) . . ?
O2 Gd2 O7 122.3(3) . . ?
O6 Gd2 O7 76.4(4) . . ?
O5 Gd2 O7 87.2(4) . . ?
O4 Gd2 O1 130.5(3) . . ?
O9 Gd2 O1 85.1(3) . . ?
O2 Gd2 O1 63.3(3) . . ?
O6 Gd2 O1 71.9(4) . . ?
O5 Gd2 O1 125.1(4) . . ?
O7 Gd2 O1 84.0(4) . . ?
O4 Gd2 O8 99.5(3) . . ?
O9 Gd2 O8 148.1(4) . . ?
O2 Gd2 O8 73.0(3) . . ?
O6 Gd2 O8 121.6(4) . . ?
O5 Gd2 O8 134.9(3) . . ?
O7 Gd2 O8 52.7(3) . . ?
O1 Gd2 O8 75.7(3) . . ?
O4 Gd2 O3 61.8(3) . . ?
O9 Gd2 O3 122.3(3) . . ?
O2 Gd2 O3 115.3(3) . . ?
O6 Gd2 O3 117.3(4) . . ?
O5 Gd2 O3 71.2(4) . . ?
O7 Gd2 O3 73.7(3) . . ?
O1 Gd2 O3 152.1(3) . . ?
O8 Gd2 O3 77.4(4) . . ?
O4 Gd2 C24 117.6(5) . . ?
O9 Gd2 C24 73.7(4) . . ?
O2 Gd2 C24 145.1(4) . . ?
O6 Gd2 C24 25.8(4) . . ?
O5 Gd2 C24 27.6(4) . . ?
O7 Gd2 C24 80.9(4) . . ?
O1 Gd2 C24 97.6(5) . . ?
O8 Gd2 C24 133.4(4) . . ?
O3 Gd2 C24 95.3(5) . . ?
O4 Gd2 C17 118.2(4) . . ?
O9 Gd2 C17 164.3(4) . . ?
O2 Gd2 C17 98.7(4) . . ?
O6 Gd2 C17 98.8(4) . . ?
O5 Gd2 C17 110.6(4) . . ?
O7 Gd2 C17 25.5(4) . . ?
O1 Gd2 C17 79.2(4) . . ?
O8 Gd2 C17 27.2(4) . . ?
O3 Gd2 C17 73.4(4) . . ?
C24 Gd2 C17 106.4(5) . . ?
O4 Gd2 Ni1 34.4(2) . . ?
O9 Gd2 Ni1 65.0(2) . . ?
O2 Gd2 Ni1 34.88(19) . . ?
O6 Gd2 Ni1 138.5(3) . . ?
O5 Gd2 Ni1 120.6(3) . . ?
O7 Gd2 Ni1 143.3(3) . . ?
O1 Gd2 Ni1 96.1(2) . . ?
O8 Gd2 Ni1 91.6(2) . . ?
O3 Gd2 Ni1 92.1(2) . . ?
C24 Gd2 Ni1 134.9(4) . . ?
C17 Gd2 Ni1 118.3(3) . . ?
C16 N1 N1 118.5(9) . 2 ?
C16 N1 Ni1 124.3(9) . . ?
N1 N1 Ni1 117.0(6) 2 . ?
C8 N2 N2 114.7(9) . 2 ?
C8 N2 Ni1 124.3(9) . . ?
N2 N2 Ni1 121.0(5) 2 . ?
O4 Ni1 O2 82.8(4) . . ?
O4 Ni1 N2 166.8(4) . . ?
O2 Ni1 N2 89.3(4) . . ?
O4 Ni1 N1 87.8(4) . . ?
O2 Ni1 N1 169.5(4) . . ?
N2 Ni1 N1 100.8(4) . . ?
O4 Ni1 O11 85.7(4) . . ?
O2 Ni1 O11 91.9(3) . . ?
N2 Ni1 O11 84.1(4) . . ?
N1 Ni1 O11 91.9(4) . . ?
O4 Ni1 O10 93.7(3) . . ?
O2 Ni1 O10 90.5(3) . . ?
N2 Ni1 O10 96.9(4) . . ?
N1 Ni1 O10 85.6(4) . . ?
O11 Ni1 O10 177.5(4) . . ?
O4 Ni1 Gd2 41.2(2) . . ?
O2 Ni1 Gd2 43.0(3) . . ?
N2 Ni1 Gd2 132.3(3) . . ?
N1 Ni1 Gd2 126.7(3) . . ?
O11 Ni1 Gd2 96.8(3) . . ?
O10 Ni1 Gd2 84.3(2) . . ?
C2 O1 C1 118.4(13) . . ?
C2 O1 Gd2 118.5(7) . . ?
C1 O1 Gd2 123.1(11) . . ?
C7 O2 Ni1 123.3(7) . . ?
C7 O2 Gd2 124.4(7) . . ?
Ni1 O2 Gd2 102.1(4) . . ?
C10 O3 C9 116.3(11) . . ?
C10 O3 Gd2 116.5(7) . . ?
C9 O3 Gd2 126.2(9) . . ?
C15 O4 Ni1 120.9(6) . . ?
C15 O4 Gd2 129.1(6) . . ?
Ni1 O4 Gd2 104.5(4) . . ?
C24 O5 Gd2 90.8(11) . . ?
C24 O6 Gd2 93.9(10) . . ?
C17 O7 Gd2 94.1(10) . . ?
C17 O8 Gd2 90.1(9) . . ?
C31 O9 Gd2 138.4(8) . . ?
C31 O10 Ni1 122.6(8) . . ?
C38 O11 Ni1 141.5(9) . . ?
C38 O11 H11A 109.5 . . ?
Ni1 O11 H11A 106.5 . . ?
C39 O12 H12A 109.5 . . ?

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
O1 C2 C3 C4 -175.3(10) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C8 -179.6(10) . . . . ?
C5 C6 C7 O2 -176.3(9) . . . . ?
C8 C6 C7 O2 3.2(12) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C8 C6 C7 C2 179.6(11) . . . . ?
O1 C2 C7 O2 -7.8(9) . . . . ?
C3 C2 C7 O2 176.6(9) . . . . ?
O1 C2 C7 C6 175.6(9) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C5 C6 C8 N2 -170.4(11) . . . . ?
C7 C6 C8 N2 10.1(19) . . . . ?
O3 C10 C11 C12 177.1(12) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C16 -179.7(11) . . . . ?
C13 C14 C15 O4 179.7(10) . . . . ?
C16 C14 C15 O4 -0.7(13) . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C16 C14 C15 C10 179.6(12) . . . . ?
O3 C10 C15 O4 3.0(11) . . . . ?
C11 C10 C15 O4 -179.7(10) . . . . ?
O3 C10 C15 C14 -177.3(11) . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C13 C14 C16 N1 -159.0(12) . . . . ?
C15 C14 C16 N1 21(2) . . . . ?
O7 C17 C18 C19 17.2(19) . . . . ?
O8 C17 C18 C19 -163.7(11) . . . . ?
O7 C17 C18 C23 -165.0(13) . . . . ?
O8 C17 C18 C23 14.2(18) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 177.9(11) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C17 C18 C23 C22 -177.7(11) . . . . ?
O6 C24 C25 C26 159.1(13) . . . . ?
O5 C24 C25 C26 -14.1(18) . . . . ?
O6 C24 C25 C30 -25.3(19) . . . . ?
O5 C24 C25 C30 161.5(11) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 175.5(12) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 -175.6(12) . . . . ?
O10 C31 C32 C33 168.9(10) . . . . ?
O9 C31 C32 C33 -11.8(14) . . . . ?
O10 C31 C32 C37 -8.3(16) . . . . ?
O9 C31 C32 C37 171.0(9) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C34 -177.2(10) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C31 C32 C37 C36 177.2(10) . . . . ?
C14 C16 N1 N1 -175.8(12) . . . 2 ?
C14 C16 N1 Ni1 -1(2) . . . . ?
C6 C8 N2 N2 -174.8(12) . . . 2 ?
C6 C8 N2 Ni1 4.6(19) . . . . ?
C3 C2 O1 C1 -4.7(15) . . . . ?
C7 C2 O1 C1 179.9(11) . . . . ?
C3 C2 O1 Gd2 172.6(5) . . . . ?
C7 C2 O1 Gd2 -2.8(10) . . . . ?
C6 C7 O2 Ni1 -28.7(11) . . . . ?
C2 C7 O2 Ni1 154.8(5) . . . . ?
C6 C7 O2 Gd2 -167.5(5) . . . . ?
C2 C7 O2 Gd2 16.0(9) . . . . ?
C11 C10 O3 C9 -7.9(16) . . . . ?
C15 C10 O3 C9 169.3(11) . . . . ?
C11 C10 O3 Gd2 -176.7(5) . . . . ?
C15 C10 O3 Gd2 0.5(11) . . . . ?
C14 C15 O4 Ni1 -36.1(11) . . . . ?
C10 C15 O4 Ni1 143.6(6) . . . . ?
C14 C15 O4 Gd2 174.3(5) . . . . ?
C10 C15 O4 Gd2 -6.1(12) . . . . ?
O6 C24 O5 Gd2 -0.7(17) . . . . ?
C25 C24 O5 Gd2 172.4(11) . . . . ?
O5 C24 O6 Gd2 0.7(17) . . . . ?
C25 C24 O6 Gd2 -172.2(12) . . . . ?
O8 C17 O7 Gd2 1.8(18) . . . . ?
C18 C17 O7 Gd2 -179.2(12) . . . . ?
O7 C17 O8 Gd2 -1.8(17) . . . . ?
C18 C17 O8 Gd2 179.1(11) . . . . ?
O10 C31 O9 Gd2 -19(2) . . . . ?
C32 C31 O9 Gd2 161.6(8) . . . . ?
O9 C31 O10 Ni1 23.9(19) . . . . ?
C32 C31 O10 Ni1 -156.9(8) . . . . ?

_refine_diff_density_max         1.181
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.148


# start Validation Reply Form
_vrf_PLAT973_x                   
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_Gd2Zn2
_audit_block_doi                 10.5517/cc14htdv
_database_code_depnum_ccdc_archive 'CCDC 1057887'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C76 H70 Gd2 N4 O24 Zn2'
_chemical_formula_sum            'C76 H70 Gd2 N4 O24 Zn2'
_chemical_formula_weight         1868.60

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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.749(3)
_cell_length_b                   16.590(2)
_cell_length_c                   22.922(3)
_cell_angle_alpha                90
_cell_angle_beta                 120.225(12)
_cell_angle_gamma                90
_cell_volume                     7803.4(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5015
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      24.01

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_F_000             3736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.363
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22020
_diffrn_reflns_av_unetI/netI     0.0896
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.588
_diffrn_reflns_theta_max         25.261
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7031
_reflns_number_gt                3728
_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.

 The command 'isor' was also used to restrain the O11 and all C atom with NPD and ADP
 problems. The restraint command lead to restraint number 236, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the O7-O12, H1C-H3 distance to
 be in the reasonable range.

 The H-atoms on water cannot be determined.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.1237P)²+62.7310P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7031
_refine_ls_number_parameters     430
_refine_ls_number_restraints     236
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0734
_refine_ls_wR_factor_ref         0.2495
_refine_ls_wR_factor_gt          0.1942
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.027
_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
C1 C 0.6488(9) 0.2691(11) 0.5408(9) 0.150(8) Uani 1 1 d . U . . .
H1A H 0.6403 0.2852 0.4969 0.225 Uiso 1 1 calc R U . . .
H1B H 0.6186 0.2956 0.5507 0.225 Uiso 1 1 calc R U . . .
H1C H 0.6437 0.2117 0.5415 0.225 Uiso 1 1 calc DR U . . .
C2 C 0.7592(4) 0.2438(6) 0.5939(5) 0.090(4) Uani 1 1 d G U . . .
C3 C 0.7472(4) 0.1759(7) 0.5538(5) 0.111(5) Uani 1 1 d G U . . .
H3 H 0.7045 0.1612 0.5228 0.133 Uiso 1 1 calc DR U . . .
C4 C 0.7989(6) 0.1299(6) 0.5600(5) 0.124(6) Uani 1 1 d G U . . .
H4 H 0.7908 0.0845 0.5332 0.149 Uiso 1 1 calc R U . . .
C5 C 0.8626(5) 0.1519(6) 0.6064(6) 0.118(6) Uani 1 1 d G U . . .
H5 H 0.8972 0.1211 0.6106 0.142 Uiso 1 1 calc R U . . .
C6 C 0.8746(4) 0.2198(6) 0.6465(4) 0.080(4) Uani 1 1 d G U . . .
C7 C 0.8229(5) 0.2658(5) 0.6403(4) 0.072(3) Uani 1 1 d G U . . .
C8 C 0.9425(7) 0.2391(8) 0.6917(7) 0.077(4) Uani 1 1 d . U . . .
H8 H 0.9725 0.2010 0.6944 0.092 Uiso 1 1 calc R U . . .
C9 C 0.7181(8) 0.5233(12) 0.7871(10) 0.118(6) Uani 1 1 d . U . . .
H9A H 0.7330 0.5141 0.8340 0.177 Uiso 1 1 calc R U . . .
H9B H 0.6791 0.4927 0.7600 0.177 Uiso 1 1 calc R U . . .
H9C H 0.7091 0.5796 0.7771 0.177 Uiso 1 1 calc R U . . .
C10 C 0.8260(4) 0.5324(6) 0.8083(5) 0.087(4) Uani 1 1 d G U . . .
C11 C 0.8444(6) 0.5810(8) 0.8644(6) 0.135(7) Uani 1 1 d G U . . .
H11 H 0.8149 0.5920 0.8788 0.162 Uiso 1 1 calc R U . . .
C12 C 0.9069(6) 0.6133(8) 0.8991(5) 0.160(8) Uani 1 1 d G U . . .
H12 H 0.9192 0.6458 0.9367 0.192 Uiso 1 1 calc R U . . .
C13 C 0.9510(4) 0.5969(7) 0.8776(6) 0.131(7) Uani 1 1 d G U . . .
H13 H 0.9928 0.6184 0.9008 0.157 Uiso 1 1 calc R U . . .
C14 C 0.9326(4) 0.5482(6) 0.8215(5) 0.074(4) Uani 1 1 d G U . . .
C15 C 0.8701(4) 0.5160(5) 0.7868(4) 0.062(3) Uani 1 1 d G U . . .
C16 C 0.9790(6) 0.5410(8) 0.8002(7) 0.067(3) Uani 1 1 d . U . . .
H16 H 1.0144 0.5760 0.8184 0.081 Uiso 1 1 calc R U . . .
C17 C 0.8315(6) 0.4758(7) 0.5846(6) 0.059(3) Uani 1 1 d . U . . .
C18 C 0.8248(4) 0.5288(5) 0.5301(4) 0.068(3) Uani 1 1 d G U . . .
C19 C 0.8734(4) 0.5312(6) 0.5133(6) 0.103(5) Uani 1 1 d G U . . .
H19 H 0.9102 0.4989 0.5363 0.123 Uiso 1 1 calc R U . . .
C20 C 0.8671(5) 0.5820(8) 0.4621(6) 0.140(7) Uani 1 1 d G U . . .
H20 H 0.8996 0.5836 0.4508 0.168 Uiso 1 1 calc R U . . .
C21 C 0.8122(6) 0.6303(7) 0.4277(5) 0.134(7) Uani 1 1 d G U . . .
H21 H 0.8079 0.6643 0.3934 0.161 Uiso 1 1 calc R U . . .
C22 C 0.7636(5) 0.6279(6) 0.4445(5) 0.111(5) Uani 1 1 d G U . . .
H22 H 0.7268 0.6603 0.4215 0.133 Uiso 1 1 calc R U . . .
C23 C 0.7699(4) 0.5772(6) 0.4957(5) 0.077(4) Uani 1 1 d G U . . .
H23 H 0.7374 0.5756 0.5070 0.092 Uiso 1 1 calc R U . . .
C24 C 0.6532(8) 0.5219(12) 0.5742(10) 0.093(5) Uani 1 1 d . U . . .
C25 C 0.6046(5) 0.5774(8) 0.5211(6) 0.097(5) Uani 1 1 d G U . . .
C26 C 0.6169(6) 0.6596(9) 0.5240(6) 0.137(7) Uani 1 1 d G U . . .
H26 H 0.6562 0.6802 0.5581 0.164 Uiso 1 1 calc R U . . .
C27 C 0.5704(8) 0.7110(6) 0.4761(8) 0.175(9) Uani 1 1 d G U . . .
H27 H 0.5786 0.7661 0.4781 0.210 Uiso 1 1 calc R U . . .
C28 C 0.5116(7) 0.6802(9) 0.4252(7) 0.165(9) Uani 1 1 d G U . . .
H28 H 0.4805 0.7146 0.3932 0.198 Uiso 1 1 calc R U . . .
C29 C 0.4993(5) 0.5979(10) 0.4223(6) 0.136(7) Uani 1 1 d G U . . .
H29 H 0.4600 0.5773 0.3882 0.163 Uiso 1 1 calc R U . . .
C30 C 0.5458(6) 0.5465(7) 0.4702(7) 0.137(7) Uani 1 1 d G U . . .
H30 H 0.5376 0.4915 0.4682 0.165 Uiso 1 1 calc R U . . .
C31 C 0.6951(8) 0.3257(10) 0.7287(8) 0.085(4) Uani 1 1 d . U . . .
C32 C 0.6694(5) 0.2793(7) 0.7660(5) 0.088(4) Uani 1 1 d G U . . .
C33 C 0.6155(5) 0.3091(6) 0.7674(6) 0.126(6) Uani 1 1 d G U . . .
H33 H 0.5945 0.3552 0.7430 0.151 Uiso 1 1 calc R U . . .
C34 C 0.5928(5) 0.2702(8) 0.8053(6) 0.126(6) Uani 1 1 d G U . . .
H34 H 0.5567 0.2902 0.8062 0.151 Uiso 1 1 calc R U . . .
C35 C 0.6241(6) 0.2013(8) 0.8418(6) 0.117(6) Uani 1 1 d G U . . .
H35 H 0.6090 0.1752 0.8671 0.141 Uiso 1 1 calc R U . . .
C36 C 0.6781(6) 0.1714(6) 0.8404(5) 0.118(6) Uani 1 1 d G U . . .
H36 H 0.6991 0.1253 0.8648 0.141 Uiso 1 1 calc R U . . .
C37 C 0.7008(5) 0.2104(7) 0.8025(6) 0.101(5) Uani 1 1 d G U . . .
H37 H 0.7369 0.1904 0.8016 0.121 Uiso 1 1 calc R U . . .
C38 C 0.9960(13) 0.3465(16) 0.9015(12) 0.177(10) Uani 1 1 d . U . . .
H38A H 1.0362 0.3546 0.9018 0.265 Uiso 1 1 calc R U . . .
H38B H 0.9976 0.2958 0.9225 0.265 Uiso 1 1 calc R U . . .
H38C H 0.9900 0.3893 0.9261 0.265 Uiso 1 1 calc R U . . .
Gd1 Gd 0.74648(3) 0.41667(5) 0.66384(3) 0.0747(3) Uani 1 1 d . . . . .
N4 N 0.9748(4) 0.4890(5) 0.7575(5) 0.052(2) Uani 1 1 d . . . . .
N5 N 0.9662(4) 0.3013(5) 0.7281(4) 0.058(2) Uani 1 1 d . . . . .
O1 O 0.7135(5) 0.2908(7) 0.5900(5) 0.110(4) Uani 1 1 d . . . . .
O2 O 0.8304(4) 0.3282(5) 0.6777(4) 0.067(2) Uani 1 1 d . . . . .
O3 O 0.8505(3) 0.4671(5) 0.7373(4) 0.0586(19) Uani 1 1 d . . . . .
O4 O 0.7670(4) 0.4987(6) 0.7726(4) 0.087(3) Uani 1 1 d . . . . .
O5 O 0.8849(4) 0.4434(5) 0.6205(4) 0.068(2) Uani 1 1 d . . . . .
O6 O 0.7831(4) 0.4684(5) 0.5915(4) 0.070(2) Uani 1 1 d . . . . .
O7 O 0.7512(4) 0.3110(7) 0.7401(5) 0.096(3) Uani 1 1 d D . . . .
O8 O 0.6610(4) 0.3777(8) 0.6859(5) 0.113(4) Uani 1 1 d . . . . .
O9 O 0.6948(4) 0.5492(8) 0.6305(5) 0.102(3) Uani 1 1 d . . . . .
O10 O 0.6498(4) 0.4498(9) 0.5600(5) 0.108(4) Uani 1 1 d . . . . .
O11 O 0.9437(10) 0.3461(12) 0.8344(11) 0.212(8) Uani 1 1 d . U . . .
H11A H 0.9164 0.3131 0.8307 0.319 Uiso 1 1 calc R U . . .
O12 O 0.8675(8) 0.2178(14) 0.8237(9) 0.277(12) Uani 1 1 d D . . . .
Zn1 Zn 0.90781(6) 0.40050(8) 0.71284(7) 0.0623(4) 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
C1 O1 1.421(17) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.302(14) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.448(15) . ?
C7 O2 1.298(10) . ?
C8 N5 1.267(15) . ?
C8 H8 0.9300 . ?
C9 O4 1.420(16) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O4 1.338(11) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C16 1.418(14) . ?
C15 O3 1.278(10) . ?
C16 N4 1.270(14) . ?
C16 H16 0.9300 . ?
C17 O5 1.235(13) . ?
C17 O6 1.243(13) . ?
C17 C18 1.468(14) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O10 1.231(19) . ?
C24 O9 1.25(2) . ?
C24 C25 1.50(2) . ?
C24 Gd1 2.756(18) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O7 1.247(17) . ?
C31 O8 1.249(17) . ?
C31 C32 1.491(15) . ?
C31 Gd1 2.793(13) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 O11 1.41(3) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
Gd1 O3 2.334(7) . ?
Gd1 O2 2.364(9) . ?
Gd1 O6 2.386(8) . ?
Gd1 O10 2.395(9) . ?
Gd1 O8 2.415(9) . ?
Gd1 O7 2.438(9) . ?
Gd1 O9 2.445(12) . ?
Gd1 O1 2.550(12) . ?
Gd1 O4 2.662(9) . ?
Gd1 Zn1 3.4177(15) . ?
N4 N4 1.400(16) 2_756 ?
N4 Zn1 2.024(9) . ?
N5 N5 1.403(18) 2_756 ?
N5 Zn1 2.064(9) . ?
O2 Zn1 1.995(7) . ?
O3 Zn1 2.038(8) . ?
O5 Zn1 2.030(8) . ?
O11 H11A 0.8200 . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.6(9) . . ?
O1 C2 C7 116.3(9) . . ?
C3 C2 C7 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C8 124.1(9) . . ?
C5 C6 C8 115.9(9) . . ?
O2 C7 C6 123.3(8) . . ?
O2 C7 C2 116.7(8) . . ?
C6 C7 C2 120.0 . . ?
N5 C8 C6 128.0(12) . . ?
N5 C8 H8 116.0 . . ?
C6 C8 H8 116.0 . . ?
O4 C9 H9A 109.5 . . ?
O4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O4 C10 C11 123.5(8) . . ?
O4 C10 C15 116.5(8) . . ?
C11 C10 C15 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 C16 124.2(8) . . ?
C13 C14 C16 115.6(8) . . ?
O3 C15 C14 123.9(7) . . ?
O3 C15 C10 115.9(7) . . ?
C14 C15 C10 120.0 . . ?
N4 C16 C14 123.3(11) . . ?
N4 C16 H16 118.3 . . ?
C14 C16 H16 118.3 . . ?
O5 C17 O6 125.2(11) . . ?
O5 C17 C18 117.6(10) . . ?
O6 C17 C18 117.2(11) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 120.3(8) . . ?
C23 C18 C17 119.7(8) . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O10 C24 O9 122.5(17) . . ?
O10 C24 C25 117.4(17) . . ?
O9 C24 C25 120.1(18) . . ?
O10 C24 Gd1 60.2(9) . . ?
O9 C24 Gd1 62.5(9) . . ?
C25 C24 Gd1 174.9(11) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 120.4(13) . . ?
C30 C25 C24 119.6(13) . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O7 C31 O8 120.2(12) . . ?
O7 C31 C32 118.7(14) . . ?
O8 C31 C32 121.1(14) . . ?
O7 C31 Gd1 60.7(7) . . ?
O8 C31 Gd1 59.6(7) . . ?
C32 C31 Gd1 177.5(10) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 118.5(11) . . ?
C37 C32 C31 121.4(11) . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O11 C38 H38A 109.5 . . ?
O11 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O11 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O3 Gd1 O2 67.1(3) . . ?
O3 Gd1 O6 75.4(3) . . ?
O2 Gd1 O6 74.9(3) . . ?
O3 Gd1 O10 140.5(3) . . ?
O2 Gd1 O10 126.7(4) . . ?
O6 Gd1 O10 74.3(3) . . ?
O3 Gd1 O8 129.9(3) . . ?
O2 Gd1 O8 123.1(4) . . ?
O6 Gd1 O8 151.8(3) . . ?
O10 Gd1 O8 77.5(3) . . ?
O3 Gd1 O7 95.2(3) . . ?
O2 Gd1 O7 74.1(3) . . ?
O6 Gd1 O7 148.8(3) . . ?
O10 Gd1 O7 123.6(3) . . ?
O8 Gd1 O7 53.0(3) . . ?
O3 Gd1 O9 94.9(3) . . ?
O2 Gd1 O9 149.0(3) . . ?
O6 Gd1 O9 76.2(3) . . ?
O10 Gd1 O9 53.4(4) . . ?
O8 Gd1 O9 87.9(4) . . ?
O7 Gd1 O9 134.8(3) . . ?
O3 Gd1 O1 129.2(3) . . ?
O2 Gd1 O1 62.4(3) . . ?
O6 Gd1 O1 86.0(3) . . ?
O10 Gd1 O1 73.0(4) . . ?
O8 Gd1 O1 84.9(4) . . ?
O7 Gd1 O1 77.0(3) . . ?
O9 Gd1 O1 126.2(3) . . ?
O3 Gd1 O4 60.9(3) . . ?
O2 Gd1 O4 116.6(3) . . ?
O6 Gd1 O4 120.5(3) . . ?
O10 Gd1 O4 116.4(4) . . ?
O8 Gd1 O4 73.6(4) . . ?
O7 Gd1 O4 77.0(3) . . ?
O9 Gd1 O4 70.1(3) . . ?
O1 Gd1 O4 153.0(3) . . ?
O3 Gd1 C24 118.2(5) . . ?
O2 Gd1 C24 143.1(4) . . ?
O6 Gd1 C24 72.0(4) . . ?
O10 Gd1 C24 26.5(4) . . ?
O8 Gd1 C24 83.2(4) . . ?
O7 Gd1 C24 136.1(4) . . ?
O9 Gd1 C24 27.0(5) . . ?
O1 Gd1 C24 99.2(5) . . ?
O4 Gd1 C24 94.2(5) . . ?
O3 Gd1 C31 113.4(4) . . ?
O2 Gd1 C31 99.1(4) . . ?
O6 Gd1 C31 166.9(4) . . ?
O10 Gd1 C31 101.3(4) . . ?
O8 Gd1 C31 26.5(4) . . ?
O7 Gd1 C31 26.5(4) . . ?
O9 Gd1 C31 111.5(5) . . ?
O1 Gd1 C31 80.8(4) . . ?
O4 Gd1 C31 72.6(4) . . ?
C24 Gd1 C31 109.7(5) . . ?
O3 Gd1 Zn1 35.58(19) . . ?
O2 Gd1 Zn1 34.67(18) . . ?
O6 Gd1 Zn1 61.06(19) . . ?
O10 Gd1 Zn1 134.4(3) . . ?
O8 Gd1 Zn1 146.3(3) . . ?
O7 Gd1 Zn1 93.9(2) . . ?
O9 Gd1 Zn1 118.5(2) . . ?
O1 Gd1 Zn1 94.2(2) . . ?
O4 Gd1 Zn1 94.94(17) . . ?
C24 Gd1 Zn1 129.9(3) . . ?
C31 Gd1 Zn1 120.0(4) . . ?
C16 N4 N4 116.3(9) . 2_756 ?
C16 N4 Zn1 128.2(8) . . ?
N4 N4 Zn1 115.3(6) 2_756 . ?
C8 N5 N5 116.1(9) . 2_756 ?
C8 N5 Zn1 120.1(9) . . ?
N5 N5 Zn1 123.4(4) 2_756 . ?
C2 O1 C1 115.7(14) . . ?
C2 O1 Gd1 118.6(7) . . ?
C1 O1 Gd1 125.7(12) . . ?
C7 O2 Zn1 122.6(7) . . ?
C7 O2 Gd1 125.5(6) . . ?
Zn1 O2 Gd1 102.9(3) . . ?
C15 O3 Zn1 126.4(6) . . ?
C15 O3 Gd1 130.4(6) . . ?
Zn1 O3 Gd1 102.6(3) . . ?
C10 O4 C9 117.8(11) . . ?
C10 O4 Gd1 115.3(6) . . ?
C9 O4 Gd1 125.5(9) . . ?
C17 O5 Zn1 119.7(8) . . ?
C17 O6 Gd1 144.0(8) . . ?
C31 O7 Gd1 92.9(9) . . ?
C31 O8 Gd1 93.9(8) . . ?
C24 O9 Gd1 90.5(11) . . ?
C24 O10 Gd1 93.3(11) . . ?
C38 O11 H11A 109.5 . . ?
O2 Zn1 N4 166.2(3) . . ?
O2 Zn1 O5 94.6(3) . . ?
N4 Zn1 O5 90.1(4) . . ?
O2 Zn1 O3 80.2(3) . . ?
N4 Zn1 O3 86.1(3) . . ?
O5 Zn1 O3 103.3(3) . . ?
O2 Zn1 N5 89.6(3) . . ?
N4 Zn1 N5 101.7(3) . . ?
O5 Zn1 N5 105.1(4) . . ?
O3 Zn1 N5 150.5(3) . . ?
O2 Zn1 Gd1 42.4(3) . . ?
N4 Zn1 Gd1 125.1(2) . . ?
O5 Zn1 Gd1 87.8(2) . . ?
O3 Zn1 Gd1 41.8(2) . . ?
N5 Zn1 Gd1 131.6(2) . . ?

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
O1 C2 C3 C4 178.5(11) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C8 -178.2(10) . . . . ?
C5 C6 C7 O2 177.5(9) . . . . ?
C8 C6 C7 O2 -4.5(12) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C8 C6 C7 C2 178.0(10) . . . . ?
O1 C2 C7 O2 3.8(10) . . . . ?
C3 C2 C7 O2 -177.6(9) . . . . ?
O1 C2 C7 C6 -178.6(10) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C7 C6 C8 N5 -5.8(18) . . . . ?
C5 C6 C8 N5 172.3(11) . . . . ?
O4 C10 C11 C12 179.5(12) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C16 174.7(11) . . . . ?
C13 C14 C15 O3 -175.8(10) . . . . ?
C16 C14 C15 O3 10.0(13) . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C16 C14 C15 C10 -174.2(12) . . . . ?
O4 C10 C15 O3 -3.5(11) . . . . ?
C11 C10 C15 O3 176.1(10) . . . . ?
O4 C10 C15 C14 -179.6(11) . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C15 C14 C16 N4 -17.7(18) . . . . ?
C13 C14 C16 N4 167.8(10) . . . . ?
O5 C17 C18 C19 10.4(14) . . . . ?
O6 C17 C18 C19 -170.9(9) . . . . ?
O5 C17 C18 C23 -169.1(9) . . . . ?
O6 C17 C18 C23 9.5(14) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 -179.5(10) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C17 C18 C23 C22 179.5(10) . . . . ?
O10 C24 C25 C26 -159.7(12) . . . . ?
O9 C24 C25 C26 21.1(18) . . . . ?
O10 C24 C25 C30 22.9(18) . . . . ?
O9 C24 C25 C30 -156.4(12) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 -177.4(12) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 177.4(12) . . . . ?
O7 C31 C32 C33 163.0(11) . . . . ?
O8 C31 C32 C33 -18.0(18) . . . . ?
O7 C31 C32 C37 -12.8(18) . . . . ?
O8 C31 C32 C37 166.1(12) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C34 -175.9(11) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C31 C32 C37 C36 175.8(11) . . . . ?
C14 C16 N4 N4 -179.1(11) . . . 2_756 ?
C14 C16 N4 Zn1 -4.0(18) . . . . ?
C6 C8 N5 N5 174.5(12) . . . 2_756 ?
C6 C8 N5 Zn1 -12.7(18) . . . . ?
C3 C2 O1 C1 -0.6(15) . . . . ?
C7 C2 O1 C1 178.0(10) . . . . ?
C3 C2 O1 Gd1 -176.7(5) . . . . ?
C7 C2 O1 Gd1 1.8(10) . . . . ?
C6 C7 O2 Zn1 32.4(10) . . . . ?
C2 C7 O2 Zn1 -150.0(5) . . . . ?
C6 C7 O2 Gd1 173.9(5) . . . . ?
C2 C7 O2 Gd1 -8.5(9) . . . . ?
C14 C15 O3 Zn1 18.1(12) . . . . ?
C10 C15 O3 Zn1 -157.8(6) . . . . ?
C14 C15 O3 Gd1 -172.1(6) . . . . ?
C10 C15 O3 Gd1 11.9(11) . . . . ?
C11 C10 O4 C9 9.2(16) . . . . ?
C15 C10 O4 C9 -171.2(11) . . . . ?
C11 C10 O4 Gd1 176.4(5) . . . . ?
C15 C10 O4 Gd1 -4.1(11) . . . . ?
O6 C17 O5 Zn1 -18.4(17) . . . . ?
C18 C17 O5 Zn1 160.1(7) . . . . ?
O5 C17 O6 Gd1 9(2) . . . . ?
C18 C17 O6 Gd1 -169.8(9) . . . . ?
O8 C31 O7 Gd1 3.8(16) . . . . ?
C32 C31 O7 Gd1 -177.2(11) . . . . ?
O7 C31 O8 Gd1 -3.9(16) . . . . ?
C32 C31 O8 Gd1 177.2(12) . . . . ?
O10 C24 O9 Gd1 5.8(16) . . . . ?
C25 C24 O9 Gd1 -175.0(12) . . . . ?
O9 C24 O10 Gd1 -6.0(16) . . . . ?
C25 C24 O10 Gd1 174.8(11) . . . . ?

_refine_diff_density_max         1.218
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.144

####################################################################### 
# 
# 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_Tb2Co2
_audit_block_doi                 10.5517/cc14htfw
_database_code_depnum_ccdc_archive 'CCDC 1057888'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H74 Co2 N4 O24 Tb2'
_chemical_formula_sum            'C78 H74 Co2 N4 O24 Tb2'
_chemical_formula_weight         1887.11

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'
Co Co 0.3494 0.9721 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.168(3)
_cell_length_b                   16.9669(16)
_cell_length_c                   22.816(3)
_cell_angle_alpha                90
_cell_angle_beta                 121.013(2)
_cell_angle_gamma                90
_cell_volume                     8018.3(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5159
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      24.32

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_F_000             3784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.226
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_T_max  0.627
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            24249
_diffrn_reflns_av_unetI/netI     0.0816
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.551
_diffrn_reflns_theta_max         26.016
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7881
_reflns_number_gt                4406
_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.
 
 The command 'isor' was also used to restrain the C atom with NPD and ADP
 problems. The restraint command lead to restraint number 73, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the O11-H11a distance to
 be in the reasonable range

 The omit command has been used to omit the bad equivalents.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.0930P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7881
_refine_ls_number_parameters     445
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1791
_refine_ls_wR_factor_gt          0.1447
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      1.010
_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
C1 C 0.2759(5) 0.5204(7) 0.7058(6) 0.102(4) Uani 1 1 d . . . . .
H1A H 0.2593 0.5099 0.6582 0.153 Uiso 1 1 calc R U . . .
H1B H 0.3147 0.4905 0.7329 0.153 Uiso 1 1 calc R U . . .
H1C H 0.2853 0.5756 0.7146 0.153 Uiso 1 1 calc R U . . .
C2 C 0.1691(2) 0.5327(4) 0.6873(3) 0.079(3) Uani 1 1 d G . . . .
C3 C 0.1498(3) 0.5815(5) 0.6311(4) 0.123(4) Uani 1 1 d G U . . .
H3 H 0.1773 0.5902 0.6145 0.148 Uiso 1 1 calc R U . . .
C4 C 0.0894(4) 0.6172(5) 0.5996(3) 0.149(5) Uani 1 1 d G U . . .
H4 H 0.0765 0.6499 0.5620 0.179 Uiso 1 1 calc R U . . .
C5 C 0.0484(3) 0.6042(4) 0.6244(4) 0.113(4) Uani 1 1 d G U . . .
H5 H 0.0080 0.6281 0.6034 0.136 Uiso 1 1 calc R U . . .
C6 C 0.0676(3) 0.5554(4) 0.6806(3) 0.076(3) Uani 1 1 d G . . . .
C7 C 0.1280(3) 0.5196(4) 0.7121(3) 0.061(2) Uani 1 1 d G . . . .
C8 C 0.0227(4) 0.5458(5) 0.7046(5) 0.065(2) Uani 1 1 d . . . . .
H8 H -0.0088 0.5843 0.6927 0.078 Uiso 1 1 calc R U . . .
C9 C 0.3532(5) 0.2734(7) 0.9554(6) 0.134(6) Uani 1 1 d . U . . .
H9A H 0.3655 0.2940 0.9997 0.202 Uiso 1 1 calc R U . . .
H9B H 0.3797 0.2966 0.9400 0.202 Uiso 1 1 calc R U . . .
H9C H 0.3587 0.2173 0.9582 0.202 Uiso 1 1 calc R U . . .
C10 C 0.2403(2) 0.2437(4) 0.9050(3) 0.076(3) Uani 1 1 d G U . . .
C11 C 0.2530(3) 0.1775(4) 0.9460(3) 0.097(4) Uani 1 1 d G U . . .
H11 H 0.2954 0.1629 0.9769 0.117 Uiso 1 1 calc R U . . .
C12 C 0.2023(4) 0.1332(3) 0.9408(3) 0.109(4) Uani 1 1 d G U . . .
H12 H 0.2108 0.0890 0.9682 0.130 Uiso 1 1 calc R U . . .
C13 C 0.1389(3) 0.1550(4) 0.8946(3) 0.097(4) Uani 1 1 d G U . . .
H13 H 0.1049 0.1254 0.8911 0.117 Uiso 1 1 calc R U . . .
C14 C 0.1262(2) 0.2211(4) 0.8536(3) 0.062(2) Uani 1 1 d G U . . .
C15 C 0.1769(3) 0.2655(3) 0.8588(3) 0.061(2) Uani 1 1 d G U . . .
C16 C 0.0590(4) 0.2394(5) 0.8089(4) 0.060(2) Uani 1 1 d . . . . .
H16 H 0.0301 0.2013 0.8063 0.071 Uiso 1 1 calc R U . . .
C17 C 0.1692(4) 0.4716(5) 0.9128(4) 0.0490(18) Uani 1 1 d . . . . .
C18 C 0.1748(3) 0.5255(3) 0.9668(3) 0.057(2) Uani 1 1 d G . . . .
C19 C 0.1247(2) 0.5309(4) 0.9797(3) 0.087(3) Uani 1 1 d G . . . .
H19 H 0.0884 0.4991 0.9559 0.105 Uiso 1 1 calc R U . . .
C20 C 0.1288(3) 0.5839(5) 1.0283(4) 0.127(5) Uani 1 1 d G . . . .
H20 H 0.0952 0.5875 1.0369 0.152 Uiso 1 1 calc R U . . .
C21 C 0.1830(4) 0.6314(4) 1.0639(3) 0.110(4) Uani 1 1 d G . . . .
H21 H 0.1858 0.6668 1.0964 0.132 Uiso 1 1 calc R U . . .
C22 C 0.2332(3) 0.6260(4) 1.0510(3) 0.094(3) Uani 1 1 d G . . . .
H22 H 0.2694 0.6578 1.0749 0.113 Uiso 1 1 calc R U . . .
C23 C 0.2290(2) 0.5730(4) 1.0024(3) 0.071(3) Uani 1 1 d G . . . .
H23 H 0.2626 0.5694 0.9938 0.085 Uiso 1 1 calc R U . . .
C24 C 0.3473(4) 0.5163(8) 0.9280(4) 0.075(3) Uani 1 1 d . . . . .
C25 C 0.3949(3) 0.5715(5) 0.9799(3) 0.091(3) Uani 1 1 d G . . . .
C26 C 0.3853(3) 0.6525(5) 0.9775(4) 0.112(4) Uani 1 1 d G . . . .
H26 H 0.3467 0.6742 0.9434 0.134 Uiso 1 1 calc R U . . .
C27 C 0.4336(5) 0.7010(4) 1.0259(4) 0.152(6) Uani 1 1 d G . . . .
H27 H 0.4271 0.7552 1.0243 0.182 Uiso 1 1 calc R U . . .
C28 C 0.4914(4) 0.6686(6) 1.0769(4) 0.139(6) Uani 1 1 d G . . . .
H28 H 0.5236 0.7010 1.1093 0.166 Uiso 1 1 calc R U . . .
C29 C 0.5009(3) 0.5876(6) 1.0793(4) 0.131(5) Uani 1 1 d G U . . .
H29 H 0.5396 0.5658 1.1134 0.157 Uiso 1 1 calc R U . . .
C30 C 0.4527(4) 0.5390(4) 1.0308(4) 0.112(4) Uani 1 1 d G U . . .
H30 H 0.4591 0.4848 1.0325 0.134 Uiso 1 1 calc R U . . .
C31 C 0.3019(5) 0.3277(6) 0.7687(4) 0.071(3) Uani 1 1 d . . . . .
C32 C 0.3280(3) 0.2812(4) 0.7324(3) 0.066(2) Uani 1 1 d G . . . .
C33 C 0.3808(3) 0.3105(4) 0.7305(3) 0.094(3) Uani 1 1 d G . . . .
H33 H 0.4012 0.3563 0.7543 0.113 Uiso 1 1 calc R U . . .
C34 C 0.4030(3) 0.2714(5) 0.6930(4) 0.105(4) Uani 1 1 d G . . . .
H34 H 0.4383 0.2910 0.6917 0.127 Uiso 1 1 calc R U . . .
C35 C 0.3724(4) 0.2031(4) 0.6574(3) 0.101(4) Uani 1 1 d G . . . .
H35 H 0.3873 0.1769 0.6324 0.122 Uiso 1 1 calc R U . . .
C36 C 0.3197(3) 0.1737(3) 0.6594(3) 0.093(3) Uani 1 1 d G . . . .
H36 H 0.2993 0.1280 0.6356 0.111 Uiso 1 1 calc R U . . .
C37 C 0.2975(3) 0.2128(4) 0.6969(3) 0.073(3) Uani 1 1 d G . . . .
H37 H 0.2622 0.1932 0.6982 0.088 Uiso 1 1 calc R U . . .
C38 C 0.0048(5) 0.3629(7) 0.6070(5) 0.097(3) Uani 1 1 d . . . . .
H38A H -0.0307 0.3806 0.6112 0.145 Uiso 1 1 calc R U . . .
H38B H -0.0047 0.3118 0.5860 0.145 Uiso 1 1 calc R U . . .
H38C H 0.0118 0.3994 0.5793 0.145 Uiso 1 1 calc R U . . .
C39 C 0.1189(10) 0.1752(8) 0.6806(8) 0.178(8) Uani 1 1 d . . . . .
H39A H 0.1583 0.1457 0.7052 0.268 Uiso 1 1 calc R U . . .
H39B H 0.0888 0.1468 0.6402 0.268 Uiso 1 1 calc R U . . .
H39C H 0.1008 0.1826 0.7091 0.268 Uiso 1 1 calc R U . . .
Co2 Co 0.08889(5) 0.39756(6) 0.77577(5) 0.0459(3) Uani 1 1 d . . . . .
N1 N 0.0333(3) 0.3014(3) 0.7719(3) 0.0491(15) Uani 1 1 d . . . . .
N2 N 0.0236(3) 0.4880(4) 0.7410(3) 0.0475(15) Uani 1 1 d . . . . .
O1 O 0.2286(3) 0.4982(4) 0.7231(3) 0.0752(17) Uani 1 1 d . . . . .
O2 O 0.1495(2) 0.4705(3) 0.7644(2) 0.0513(13) Uani 1 1 d . . . . .
O3 O 0.2857(3) 0.2924(4) 0.9073(3) 0.083(2) Uani 1 1 d . . . . .
O4 O 0.1681(2) 0.3260(3) 0.8182(2) 0.0561(14) Uani 1 1 d . . . . .
O5 O 0.2190(2) 0.4622(3) 0.9104(2) 0.0585(14) Uani 1 1 d . . . . .
O6 O 0.1160(3) 0.4392(3) 0.8735(3) 0.0573(14) Uani 1 1 d . . . . .
O7 O 0.3353(3) 0.3783(5) 0.8113(3) 0.088(2) Uani 1 1 d . . . . .
O8 O 0.2462(3) 0.3131(4) 0.7564(3) 0.0799(19) Uani 1 1 d . . . . .
O9 O 0.3494(3) 0.4449(5) 0.9399(3) 0.084(2) Uani 1 1 d . . . . .
O10 O 0.3030(3) 0.5442(4) 0.8704(3) 0.0827(19) Uani 1 1 d . . . . .
O11 O 0.0601(3) 0.3585(4) 0.6716(3) 0.0734(17) Uani 1 1 d D . . . .
O12 O 0.1313(4) 0.2469(6) 0.6627(4) 0.117(3) Uani 1 1 d . . . . .
H12A H 0.1689 0.2592 0.6897 0.176 Uiso 1 1 calc R U . . .
Tb1 Tb 0.25120(2) 0.41608(3) 0.83500(2) 0.06157(19) Uani 1 1 d . . . . .
H11A H 0.081(3) 0.319(2) 0.676(4) 0.04(2) Uiso 1 1 d 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
C1 O1 1.439(10) . ?
C2 O1 1.367(7) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C6 C8 1.457(9) . ?
C7 O2 1.323(6) . ?
C8 N2 1.277(9) . ?
C9 O3 1.457(10) . ?
C10 O3 1.353(9) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C14 C16 1.437(9) . ?
C15 O4 1.325(7) . ?
C16 N1 1.291(9) . ?
C17 O5 1.243(8) . ?
C17 O6 1.254(9) . ?
C17 C18 1.483(8) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C24 O9 1.237(12) . ?
C24 O10 1.284(11) . ?
C24 C25 1.483(11) . ?
C24 Tb1 2.776(10) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C31 O7 1.235(10) . ?
C31 O8 1.251(10) . ?
C31 C32 1.498(9) . ?
C31 Tb1 2.819(8) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C38 O11 1.390(10) . ?
C39 O12 1.365(15) . ?
Co2 O2 2.034(5) . ?
Co2 O4 2.041(5) . ?
Co2 N2 2.046(6) . ?
Co2 N1 2.087(6) . ?
Co2 O6 2.096(5) . ?
Co2 O11 2.207(6) . ?
Co2 Tb1 3.4426(11) . ?
N1 N1 1.389(12) 2_556 ?
N2 N2 1.397(11) 2_556 ?
O1 Tb1 2.706(6) . ?
O2 Tb1 2.325(5) . ?
O3 Tb1 2.530(7) . ?
O4 Tb1 2.392(5) . ?
O5 Tb1 2.357(5) . ?
O7 Tb1 2.442(6) . ?
O8 Tb1 2.462(6) . ?
O9 Tb1 2.396(6) . ?
O10 Tb1 2.430(7) . ?

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
O1 C2 C3 123.7(5) . . ?
O1 C2 C7 116.2(5) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C5 C4 C3 120.0 . . ?
C6 C5 C4 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C8 117.0(5) . . ?
C7 C6 C8 123.0(5) . . ?
O2 C7 C6 124.1(4) . . ?
O2 C7 C2 115.9(4) . . ?
C6 C7 C2 120.0 . . ?
N2 C8 C6 124.3(7) . . ?
O3 C10 C11 125.0(5) . . ?
O3 C10 C15 114.9(5) . . ?
C11 C10 C15 120.0 . . ?
C12 C11 C10 120.0 . . ?
C11 C12 C13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 C16 124.6(5) . . ?
C13 C14 C16 115.3(5) . . ?
O4 C15 C14 122.9(5) . . ?
O4 C15 C10 117.0(5) . . ?
C14 C15 C10 120.0 . . ?
N1 C16 C14 128.8(8) . . ?
O5 C17 O6 124.8(7) . . ?
O5 C17 C18 116.1(7) . . ?
O6 C17 C18 119.0(6) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 120.1(5) . . ?
C23 C18 C17 119.9(5) . . ?
C20 C19 C18 120.0 . . ?
C19 C20 C21 120.0 . . ?
C20 C21 C22 120.0 . . ?
C21 C22 C23 120.0 . . ?
C22 C23 C18 120.0 . . ?
O9 C24 O10 120.3(9) . . ?
O9 C24 C25 121.1(9) . . ?
O10 C24 C25 118.6(11) . . ?
O9 C24 Tb1 59.4(5) . . ?
O10 C24 Tb1 61.0(5) . . ?
C25 C24 Tb1 175.1(6) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 123.2(8) . . ?
C30 C25 C24 116.7(7) . . ?
C27 C26 C25 120.0 . . ?
C26 C27 C28 120.0 . . ?
C29 C28 C27 120.0 . . ?
C28 C29 C30 120.0 . . ?
C29 C30 C25 120.0 . . ?
O7 C31 O8 120.4(8) . . ?
O7 C31 C32 120.7(8) . . ?
O8 C31 C32 118.9(8) . . ?
O7 C31 Tb1 59.7(4) . . ?
O8 C31 Tb1 60.7(4) . . ?
C32 C31 Tb1 179.1(6) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 118.9(6) . . ?
C37 C32 C31 120.9(6) . . ?
C32 C33 C34 120.0 . . ?
C35 C34 C33 120.0 . . ?
C34 C35 C36 120.0 . . ?
C35 C36 C37 120.0 . . ?
C36 C37 C32 120.0 . . ?
O2 Co2 O4 82.0(2) . . ?
O2 Co2 N2 87.5(2) . . ?
O4 Co2 N2 167.9(2) . . ?
O2 Co2 N1 163.9(2) . . ?
O4 Co2 N1 88.9(2) . . ?
N2 Co2 N1 102.6(2) . . ?
O2 Co2 O6 94.5(2) . . ?
O4 Co2 O6 89.6(2) . . ?
N2 Co2 O6 85.1(2) . . ?
N1 Co2 O6 98.6(2) . . ?
O2 Co2 O11 83.9(2) . . ?
O4 Co2 O11 91.8(2) . . ?
N2 Co2 O11 93.2(2) . . ?
N1 Co2 O11 83.2(2) . . ?
O6 Co2 O11 177.7(2) . . ?
O2 Co2 Tb1 40.91(13) . . ?
O4 Co2 Tb1 42.90(16) . . ?
N2 Co2 Tb1 125.39(16) . . ?
N1 Co2 Tb1 131.83(16) . . ?
O6 Co2 Tb1 83.28(15) . . ?
O11 Co2 Tb1 96.50(18) . . ?
C16 N1 N1 117.4(5) . 2_556 ?
C16 N1 Co2 121.8(5) . . ?
N1 N1 Co2 120.8(3) 2_556 . ?
C8 N2 N2 116.6(6) . 2_556 ?
C8 N2 Co2 125.4(5) . . ?
N2 N2 Co2 118.0(3) 2_556 . ?
C2 O1 C1 117.7(7) . . ?
C2 O1 Tb1 115.0(4) . . ?
C1 O1 Tb1 126.3(6) . . ?
C7 O2 Co2 121.6(4) . . ?
C7 O2 Tb1 131.2(4) . . ?
Co2 O2 Tb1 104.1(2) . . ?
C10 O3 C9 117.7(8) . . ?
C10 O3 Tb1 119.6(4) . . ?
C9 O3 Tb1 122.6(7) . . ?
C15 O4 Co2 124.5(4) . . ?
C15 O4 Tb1 124.3(4) . . ?
Co2 O4 Tb1 101.6(2) . . ?
C17 O5 Tb1 140.0(5) . . ?
C17 O6 Co2 123.5(5) . . ?
C31 O7 Tb1 94.4(5) . . ?
C31 O8 Tb1 93.0(5) . . ?
C24 O9 Tb1 94.2(6) . . ?
C24 O10 Tb1 91.4(7) . . ?
C38 O11 Co2 136.3(6) . . ?
O2 Tb1 O5 75.25(17) . . ?
O2 Tb1 O4 69.03(17) . . ?
O5 Tb1 O4 76.28(18) . . ?
O2 Tb1 O9 139.5(2) . . ?
O5 Tb1 O9 74.5(2) . . ?
O4 Tb1 O9 127.4(2) . . ?
O2 Tb1 O10 93.1(2) . . ?
O5 Tb1 O10 76.6(2) . . ?
O4 Tb1 O10 150.57(19) . . ?
O9 Tb1 O10 53.9(3) . . ?
O2 Tb1 O7 130.84(19) . . ?
O5 Tb1 O7 150.90(19) . . ?
O4 Tb1 O7 121.5(2) . . ?
O9 Tb1 O7 76.5(2) . . ?
O10 Tb1 O7 87.9(2) . . ?
O2 Tb1 O8 98.01(19) . . ?
O5 Tb1 O8 148.9(2) . . ?
O4 Tb1 O8 73.02(19) . . ?
O9 Tb1 O8 121.6(2) . . ?
O10 Tb1 O8 134.5(2) . . ?
O7 Tb1 O8 52.2(2) . . ?
O2 Tb1 O3 131.0(2) . . ?
O5 Tb1 O3 85.49(19) . . ?
O4 Tb1 O3 62.75(19) . . ?
O9 Tb1 O3 72.2(3) . . ?
O10 Tb1 O3 125.8(2) . . ?
O7 Tb1 O3 83.9(2) . . ?
O8 Tb1 O3 76.2(2) . . ?
O2 Tb1 O1 60.96(17) . . ?
O5 Tb1 O1 122.40(19) . . ?
O4 Tb1 O1 115.69(17) . . ?
O9 Tb1 O1 116.9(2) . . ?
O10 Tb1 O1 70.8(2) . . ?
O7 Tb1 O1 73.3(2) . . ?
O8 Tb1 O1 76.6(2) . . ?
O3 Tb1 O1 151.7(2) . . ?
O2 Tb1 C24 117.1(3) . . ?
O5 Tb1 C24 72.5(2) . . ?
O4 Tb1 C24 144.7(2) . . ?
O9 Tb1 C24 26.4(2) . . ?
O10 Tb1 C24 27.5(3) . . ?
O7 Tb1 C24 82.3(2) . . ?
O8 Tb1 C24 134.4(2) . . ?
O3 Tb1 C24 98.3(3) . . ?
O1 Tb1 C24 95.1(3) . . ?
O2 Tb1 C31 115.9(2) . . ?
O5 Tb1 C31 165.0(2) . . ?
O4 Tb1 C31 97.8(3) . . ?
O9 Tb1 C31 99.4(2) . . ?
O10 Tb1 C31 111.2(3) . . ?
O7 Tb1 C31 25.9(2) . . ?
O8 Tb1 C31 26.3(2) . . ?
O3 Tb1 C31 79.6(2) . . ?
O1 Tb1 C31 72.6(2) . . ?
C24 Tb1 C31 108.2(3) . . ?
O2 Tb1 Co2 34.96(12) . . ?
O5 Tb1 Co2 65.10(13) . . ?
O4 Tb1 Co2 35.49(12) . . ?
O9 Tb1 Co2 138.78(17) . . ?
O10 Tb1 Co2 120.00(15) . . ?
O7 Tb1 Co2 143.04(15) . . ?
O8 Tb1 Co2 91.76(14) . . ?
O3 Tb1 Co2 96.10(16) . . ?
O1 Tb1 Co2 92.38(12) . . ?
C24 Tb1 Co2 133.7(2) . . ?
C31 Tb1 Co2 117.6(2) . . ?

_refine_diff_density_max         1.168
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.123

####################################################################### 
# 
# 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_Tb2Ni2
_audit_block_doi                 10.5517/cc14hthy
_database_code_depnum_ccdc_archive 'CCDC 1057890'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H72 N4 Ni2 O25 Tb2'
_chemical_formula_sum            'C78 H72 N4 Ni2 O25 Tb2'
_chemical_formula_weight         1900.65

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'
Ni Ni 0.3393 1.1124 '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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.177(7)
_cell_length_b                   16.899(5)
_cell_length_c                   22.727(10)
_cell_angle_alpha                90
_cell_angle_beta                 121.326(18)
_cell_angle_gamma                90
_cell_volume                     7932(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2026
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      20.21

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_F_000             3816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.308
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22061
_diffrn_reflns_av_unetI/netI     0.1937
_diffrn_reflns_av_R_equivalents  0.1731
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.972
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_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             6987
_reflns_number_gt                2914
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 The command 'isor' was also used to restrain the O and C atom with NPD and ADP
 problems. The restraint command lead to restraint number 174, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The H-atoms on water cannot be determined.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0708P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6987
_refine_ls_number_parameters     447
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.1866
_refine_ls_R_factor_gt           0.0719
_refine_ls_wR_factor_ref         0.2229
_refine_ls_wR_factor_gt          0.1626
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.996
_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
C1 C 0.2265(8) 0.5237(10) 0.2948(9) 0.102(5) Uani 1 1 d . U . . .
H1A H 0.2429 0.5111 0.3423 0.153 Uiso 1 1 calc R U . . .
H1B H 0.1865 0.4961 0.2663 0.153 Uiso 1 1 calc R U . . .
H1C H 0.2193 0.5796 0.2880 0.153 Uiso 1 1 calc R U . . .
C2 C 0.3322(4) 0.5340(6) 0.3124(5) 0.074(4) Uani 1 1 d G U . . .
C3 C 0.3527(5) 0.5811(7) 0.3702(6) 0.117(6) Uani 1 1 d G U . . .
H3 H 0.3254 0.5900 0.3870 0.140 Uiso 1 1 calc R U . . .
C4 C 0.4139(6) 0.6151(6) 0.4030(5) 0.130(7) Uani 1 1 d G U . . .
H4 H 0.4276 0.6467 0.4417 0.156 Uiso 1 1 calc R U . . .
C5 C 0.4547(4) 0.6020(6) 0.3779(5) 0.098(5) Uani 1 1 d G U . . .
H5 H 0.4957 0.6247 0.3998 0.117 Uiso 1 1 calc R U . . .
C6 C 0.4343(4) 0.5548(6) 0.3201(5) 0.076(4) Uani 1 1 d G . . . .
C7 C 0.3730(4) 0.5208(5) 0.2873(4) 0.062(4) Uani 1 1 d G . . . .
C8 C 0.4414(6) 0.2430(8) 0.1894(7) 0.063(4) Uani 1 1 d . . . . .
H8 H 0.4704 0.2054 0.1914 0.075 Uiso 1 1 calc R U . . .
C9 C 0.3742(3) 0.2264(6) 0.1455(4) 0.063(4) Uani 1 1 d G . . . .
C10 C 0.3607(5) 0.1609(6) 0.1032(5) 0.100(5) Uani 1 1 d G U . . .
H10 H 0.3943 0.1318 0.1053 0.120 Uiso 1 1 calc R U . . .
C11 C 0.2968(6) 0.1387(5) 0.0578(5) 0.103(6) Uani 1 1 d G . . . .
H11 H 0.2878 0.0948 0.0295 0.123 Uiso 1 1 calc R U . . .
C12 C 0.2465(4) 0.1820(6) 0.0547(4) 0.093(5) Uani 1 1 d G U . . .
H12 H 0.2038 0.1672 0.0244 0.112 Uiso 1 1 calc R U . . .
C13 C 0.2601(4) 0.2476(6) 0.0970(5) 0.077(5) Uani 1 1 d G . . . .
C14 C 0.3239(5) 0.2698(5) 0.1424(4) 0.062(4) Uani 1 1 d G . . . .
C15 C 0.1487(7) 0.2731(9) 0.0488(9) 0.116(6) Uani 1 1 d . U . . .
H15A H 0.1433 0.2539 0.0064 0.174 Uiso 1 1 calc R U . . .
H15B H 0.1220 0.3190 0.0398 0.174 Uiso 1 1 calc R U . . .
H15C H 0.1362 0.2327 0.0693 0.174 Uiso 1 1 calc R U . . .
C16 C 0.3312(7) 0.4700(8) 0.0886(6) 0.052(3) Uani 1 1 d . . . . .
C17 C 0.3254(5) 0.5251(5) 0.0353(4) 0.057(4) Uani 1 1 d G . . . .
C18 C 0.3756(4) 0.5306(6) 0.0225(5) 0.078(4) Uani 1 1 d G . . . .
H18 H 0.4122 0.4989 0.0469 0.094 Uiso 1 1 calc R U . . .
C19 C 0.3712(5) 0.5833(7) -0.0266(6) 0.110(6) Uani 1 1 d G U . . .
H19 H 0.4048 0.5870 -0.0352 0.132 Uiso 1 1 calc R U . . .
C20 C 0.3166(6) 0.6307(6) -0.0631(5) 0.103(6) Uani 1 1 d G U . . .
H20 H 0.3137 0.6660 -0.0960 0.123 Uiso 1 1 calc R U . . .
C21 C 0.2664(4) 0.6253(5) -0.0503(5) 0.092(5) Uani 1 1 d G U . . .
H21 H 0.2299 0.6569 -0.0747 0.111 Uiso 1 1 calc R U . . .
C22 C 0.2708(4) 0.5725(6) -0.0011(5) 0.075(4) Uani 1 1 d G . . . .
H22 H 0.2372 0.5689 0.0074 0.090 Uiso 1 1 calc R U . . .
C23 C 0.1541(7) 0.5150(11) 0.0727(8) 0.073(4) Uani 1 1 d . . . . .
C24 C 0.1038(5) 0.5721(7) 0.0212(5) 0.083(5) Uani 1 1 d G U . . .
C25 C 0.0457(6) 0.5402(6) -0.0307(7) 0.121(7) Uani 1 1 d G U . . .
H25 H 0.0385 0.4860 -0.0322 0.146 Uiso 1 1 calc R U . . .
C26 C -0.0016(5) 0.5894(8) -0.0804(6) 0.127(7) Uani 1 1 d G U . . .
H26 H -0.0405 0.5680 -0.1152 0.152 Uiso 1 1 calc R U . . .
C27 C 0.0091(6) 0.6704(8) -0.0782(6) 0.138(8) Uani 1 1 d G U . . .
H27 H -0.0226 0.7033 -0.1115 0.165 Uiso 1 1 calc R U . . .
C28 C 0.0672(7) 0.7023(5) -0.0263(7) 0.164(9) Uani 1 1 d G U . . .
H28 H 0.0744 0.7565 -0.0248 0.197 Uiso 1 1 calc R U . . .
C29 C 0.1145(5) 0.6532(7) 0.0234(6) 0.113(6) Uani 1 1 d G U . . .
H29 H 0.1534 0.6745 0.0582 0.136 Uiso 1 1 calc R U . . .
C30 C 0.1977(8) 0.3287(9) 0.2328(8) 0.076(4) Uani 1 1 d . U . . .
C31 C 0.1728(5) 0.2808(6) 0.2686(5) 0.068(4) Uani 1 1 d G U . . .
C32 C 0.1195(5) 0.3090(6) 0.2700(6) 0.111(6) Uani 1 1 d G . . . .
H32 H 0.0991 0.3553 0.2467 0.133 Uiso 1 1 calc R U . . .
C33 C 0.0968(5) 0.2680(9) 0.3063(6) 0.116(6) Uani 1 1 d G . . . .
H33 H 0.0611 0.2869 0.3072 0.139 Uiso 1 1 calc R U . . .
C34 C 0.1273(6) 0.1988(8) 0.3411(6) 0.110(6) Uani 1 1 d G . . . .
H34 H 0.1121 0.1714 0.3654 0.132 Uiso 1 1 calc R U . . .
C35 C 0.1806(6) 0.1706(5) 0.3397(5) 0.103(6) Uani 1 1 d G . . . .
H35 H 0.2011 0.1243 0.3630 0.123 Uiso 1 1 calc R U . . .
C36 C 0.2034(4) 0.2116(7) 0.3034(6) 0.090(5) Uani 1 1 d G . . . .
H36 H 0.2390 0.1927 0.3025 0.108 Uiso 1 1 calc R U . . .
C37 C 0.4933(8) 0.3634(10) 0.3917(7) 0.095(5) Uani 1 1 d . U . . .
H37A H 0.5309 0.3660 0.3878 0.143 Uiso 1 1 calc R U . . .
H37B H 0.4960 0.3176 0.4181 0.143 Uiso 1 1 calc R U . . .
H37C H 0.4910 0.4101 0.4144 0.143 Uiso 1 1 calc R U . . .
C38 C 0.3875(12) 0.1738(12) 0.3226(12) 0.165(9) Uani 1 1 d . U . . .
H38A H 0.4336 0.1722 0.3434 0.247 Uiso 1 1 calc R U . . .
H38B H 0.3670 0.1672 0.2736 0.247 Uiso 1 1 calc R U . . .
H38C H 0.3741 0.1321 0.3411 0.247 Uiso 1 1 calc R U . . .
C65 C 0.4798(6) 0.5449(8) 0.2968(7) 0.064(4) Uani 1 1 d . . . . .
H65 H 0.5121 0.5826 0.3092 0.077 Uiso 1 1 calc R U . . .
N1 N 0.4658(5) 0.3066(6) 0.2272(5) 0.056(3) Uani 1 1 d . . . . .
N2 N 0.4770(5) 0.4866(6) 0.2601(5) 0.051(3) Uani 1 1 d . . . . .
Ni1 Ni 0.41135(7) 0.39837(10) 0.22503(8) 0.0512(5) Uani 1 1 d . . . . .
O1 O 0.2729(5) 0.4999(6) 0.2767(5) 0.079(3) Uani 1 1 d . U . . .
O2 O 0.3513(4) 0.4729(5) 0.2343(4) 0.058(2) Uani 1 1 d . . . . .
O3 O 0.2140(5) 0.2933(6) 0.0942(5) 0.077(3) Uani 1 1 d . U . . .
O4 O 0.3337(4) 0.3288(5) 0.1843(4) 0.062(2) Uani 1 1 d . . . . .
O5 O 0.1650(5) 0.3797(6) 0.1888(5) 0.088(3) Uani 1 1 d . U . . .
O6 O 0.2551(5) 0.3142(6) 0.2439(5) 0.087(3) Uani 1 1 d . U . . .
O7 O 0.1509(5) 0.4444(7) 0.0598(5) 0.082(3) Uani 1 1 d . U . . .
O8 O 0.1968(5) 0.5456(6) 0.1297(5) 0.084(3) Uani 1 1 d . U . . .
O9 O 0.2819(4) 0.4599(5) 0.0910(4) 0.067(2) Uani 1 1 d . . . . .
O10 O 0.3855(4) 0.4395(5) 0.1294(4) 0.059(2) Uani 1 1 d . . . . .
O11 O 0.4369(4) 0.3581(5) 0.3250(4) 0.072(3) Uani 1 1 d . . . . .
H11A H 0.4365 0.3155 0.3076 0.109 Uiso 1 1 calc R U . . .
O12 O 0.3692(7) 0.2478(9) 0.3367(6) 0.128(4) Uani 1 1 d . U . . .
H12A H 0.3362 0.2637 0.3022 0.192 Uiso 1 1 calc R U . . .
O13 O 0.5000 0.030(2) 0.2500 0.36(2) Uani 1 2 d S TU P . .
Tb1 Tb 0.24970(3) 0.41734(4) 0.16597(3) 0.0662(3) 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
C1 O1 1.438(15) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.355(11) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C65 1.458(14) . ?
C7 O2 1.314(10) . ?
C8 N1 1.309(14) . ?
C8 C9 1.424(14) . ?
C8 H8 0.9300 . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C10 H10 0.9300 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 O3 1.330(12) . ?
C13 C14 1.3900 . ?
C14 O4 1.313(10) . ?
C15 O3 1.407(16) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 O9 1.234(14) . ?
C16 O10 1.258(14) . ?
C16 C17 1.475(14) . ?
C17 C18 1.3900 . ?
C17 C22 1.3900 . ?
C18 C19 1.3900 . ?
C18 H18 0.9300 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O7 1.221(16) . ?
C23 O8 1.273(16) . ?
C23 C24 1.517(17) . ?
C23 Tb1 2.732(16) . ?
C24 C25 1.3900 . ?
C24 C29 1.3900 . ?
C25 C26 1.3900 . ?
C25 H25 0.9300 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 O5 1.244(16) . ?
C30 O6 1.297(17) . ?
C30 C31 1.481(16) . ?
C30 Tb1 2.848(16) . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C32 C33 1.3900 . ?
C32 H32 0.9300 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 O11 1.420(15) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 O12 1.42(2) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C65 N2 1.270(14) . ?
C65 H65 0.9300 . ?
N1 N1 1.42(2) 2_655 ?
N1 Ni1 2.018(10) . ?
N2 N2 1.406(19) 2_655 ?
N2 Ni1 2.015(10) . ?
Ni1 O4 1.989(8) . ?
Ni1 O2 2.014(9) . ?
Ni1 O10 2.045(8) . ?
Ni1 O11 2.132(9) . ?
Ni1 Tb1 3.424(2) . ?
O1 Tb1 2.669(9) . ?
O2 Tb1 2.314(8) . ?
O3 Tb1 2.516(9) . ?
O4 Tb1 2.378(9) . ?
O5 Tb1 2.443(9) . ?
O6 Tb1 2.440(9) . ?
O7 Tb1 2.397(10) . ?
O8 Tb1 2.432(10) . ?
O9 Tb1 2.325(9) . ?
O11 H11A 0.8200 . ?
O12 H12A 0.8200 . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.7(8) . . ?
O1 C2 C7 116.2(8) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C65 116.4(9) . . ?
C7 C6 C65 123.6(9) . . ?
O2 C7 C6 123.6(8) . . ?
O2 C7 C2 116.4(8) . . ?
C6 C7 C2 120.0 . . ?
N1 C8 C9 125.6(12) . . ?
N1 C8 H8 117.2 . . ?
C9 C8 H8 117.2 . . ?
C10 C9 C14 120.0 . . ?
C10 C9 C8 114.5(9) . . ?
C14 C9 C8 125.5(9) . . ?
C9 C10 C11 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
O3 C13 C12 122.7(8) . . ?
O3 C13 C14 117.3(8) . . ?
C12 C13 C14 120.0 . . ?
O4 C14 C13 117.1(8) . . ?
O4 C14 C9 122.8(8) . . ?
C13 C14 C9 120.0 . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O9 C16 O10 124.9(12) . . ?
O9 C16 C17 116.2(12) . . ?
O10 C16 C17 118.8(11) . . ?
C18 C17 C22 120.0 . . ?
C18 C17 C16 119.5(9) . . ?
C22 C17 C16 120.5(9) . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C17 120.0 . . ?
C21 C22 H22 120.0 . . ?
C17 C22 H22 120.0 . . ?
O7 C23 O8 123.9(15) . . ?
O7 C23 C24 120.7(14) . . ?
O8 C23 C24 115.3(15) . . ?
O7 C23 Tb1 61.2(8) . . ?
O8 C23 Tb1 62.9(8) . . ?
C24 C23 Tb1 176.9(11) . . ?
C25 C24 C29 120.0 . . ?
C25 C24 C23 117.3(11) . . ?
C29 C24 C23 122.7(11) . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 120.0 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C24 120.0 . . ?
C28 C29 H29 120.0 . . ?
C24 C29 H29 120.0 . . ?
O5 C30 O6 117.2(14) . . ?
O5 C30 C31 123.4(14) . . ?
O6 C30 C31 119.3(14) . . ?
O5 C30 Tb1 58.6(8) . . ?
O6 C30 Tb1 58.7(8) . . ?
C31 C30 Tb1 178.0(11) . . ?
C32 C31 C36 120.0 . . ?
C32 C31 C30 118.2(11) . . ?
C36 C31 C30 121.7(11) . . ?
C31 C32 C33 120.0 . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C31 120.0 . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?
O11 C37 H37A 109.5 . . ?
O11 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O11 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O12 C38 H38A 109.5 . . ?
O12 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O12 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N2 C65 C6 122.3(11) . . ?
N2 C65 H65 118.8 . . ?
C6 C65 H65 118.8 . . ?
C8 N1 N1 115.7(8) . 2_655 ?
C8 N1 Ni1 123.3(9) . . ?
N1 N1 Ni1 120.9(5) 2_655 . ?
C65 N2 N2 115.6(9) . 2_655 ?
C65 N2 Ni1 126.6(8) . . ?
N2 N2 Ni1 117.7(6) 2_655 . ?
O4 Ni1 O2 82.0(4) . . ?
O4 Ni1 N2 168.5(4) . . ?
O2 Ni1 N2 87.6(4) . . ?
O4 Ni1 N1 90.2(4) . . ?
O2 Ni1 N1 167.0(4) . . ?
N2 Ni1 N1 100.9(4) . . ?
O4 Ni1 O10 90.8(3) . . ?
O2 Ni1 O10 93.4(3) . . ?
N2 Ni1 O10 84.9(4) . . ?
N1 Ni1 O10 97.0(4) . . ?
O4 Ni1 O11 89.2(4) . . ?
O2 Ni1 O11 85.0(3) . . ?
N2 Ni1 O11 94.7(4) . . ?
N1 Ni1 O11 84.6(4) . . ?
O10 Ni1 O11 178.4(4) . . ?
O4 Ni1 Tb1 42.6(3) . . ?
O2 Ni1 Tb1 40.9(2) . . ?
N2 Ni1 Tb1 126.1(3) . . ?
N1 Ni1 Tb1 132.7(3) . . ?
O10 Ni1 Tb1 84.0(2) . . ?
O11 Ni1 Tb1 95.0(3) . . ?
C2 O1 C1 116.7(11) . . ?
C2 O1 Tb1 115.1(7) . . ?
C1 O1 Tb1 127.1(9) . . ?
C7 O2 Ni1 121.0(6) . . ?
C7 O2 Tb1 130.1(7) . . ?
Ni1 O2 Tb1 104.4(3) . . ?
C13 O3 C15 119.1(12) . . ?
C13 O3 Tb1 117.1(7) . . ?
C15 O3 Tb1 123.6(10) . . ?
C14 O4 Ni1 123.8(7) . . ?
C14 O4 Tb1 122.4(6) . . ?
Ni1 O4 Tb1 102.9(4) . . ?
C30 O5 Tb1 95.6(9) . . ?
C30 O6 Tb1 94.3(9) . . ?
C23 O7 Tb1 92.2(9) . . ?
C23 O8 Tb1 89.3(9) . . ?
C16 O9 Tb1 140.8(9) . . ?
C16 O10 Ni1 123.3(8) . . ?
C37 O11 Ni1 134.7(9) . . ?
C37 O11 H11A 109.5 . . ?
Ni1 O11 H11A 80.9 . . ?
C38 O12 H12A 109.5 . . ?
O2 Tb1 O9 73.9(3) . . ?
O2 Tb1 O4 68.0(3) . . ?
O9 Tb1 O4 75.1(3) . . ?
O2 Tb1 O7 138.8(3) . . ?
O9 Tb1 O7 75.0(3) . . ?
O4 Tb1 O7 127.6(3) . . ?
O2 Tb1 O8 93.0(3) . . ?
O9 Tb1 O8 78.0(3) . . ?
O4 Tb1 O8 150.5(3) . . ?
O7 Tb1 O8 54.2(4) . . ?
O2 Tb1 O6 99.5(3) . . ?
O9 Tb1 O6 147.2(3) . . ?
O4 Tb1 O6 72.8(3) . . ?
O7 Tb1 O6 121.1(4) . . ?
O8 Tb1 O6 134.7(3) . . ?
O2 Tb1 O5 132.6(3) . . ?
O9 Tb1 O5 150.8(3) . . ?
O4 Tb1 O5 122.2(3) . . ?
O7 Tb1 O5 75.9(3) . . ?
O8 Tb1 O5 87.3(3) . . ?
O6 Tb1 O5 52.7(3) . . ?
O2 Tb1 O3 131.2(3) . . ?
O9 Tb1 O3 85.1(3) . . ?
O4 Tb1 O3 64.1(3) . . ?
O7 Tb1 O3 71.3(4) . . ?
O8 Tb1 O3 125.4(3) . . ?
O6 Tb1 O3 75.3(3) . . ?
O5 Tb1 O3 83.0(3) . . ?
O2 Tb1 O1 61.7(3) . . ?
O9 Tb1 O1 122.9(3) . . ?
O4 Tb1 O1 114.9(3) . . ?
O7 Tb1 O1 117.4(4) . . ?
O8 Tb1 O1 70.7(3) . . ?
O6 Tb1 O1 77.5(3) . . ?
O5 Tb1 O1 74.0(3) . . ?
O3 Tb1 O1 151.6(3) . . ?
O2 Tb1 C23 116.8(4) . . ?
O9 Tb1 C23 73.5(4) . . ?
O4 Tb1 C23 144.8(4) . . ?
O7 Tb1 C23 26.5(3) . . ?
O8 Tb1 C23 27.8(4) . . ?
O6 Tb1 C23 134.3(4) . . ?
O5 Tb1 C23 81.8(4) . . ?
O3 Tb1 C23 97.7(4) . . ?
O1 Tb1 C23 95.4(4) . . ?
O2 Tb1 C30 117.7(4) . . ?
O9 Tb1 C30 164.1(4) . . ?
O4 Tb1 C30 98.5(4) . . ?
O7 Tb1 C30 98.8(4) . . ?
O8 Tb1 C30 110.5(4) . . ?
O6 Tb1 C30 27.0(4) . . ?
O5 Tb1 C30 25.8(4) . . ?
O3 Tb1 C30 79.0(4) . . ?
O1 Tb1 C30 73.0(4) . . ?
C23 Tb1 C30 107.5(5) . . ?
O2 Tb1 Ni1 34.7(2) . . ?
O9 Tb1 Ni1 64.4(2) . . ?
O4 Tb1 Ni1 34.49(19) . . ?
O7 Tb1 Ni1 138.5(3) . . ?
O8 Tb1 Ni1 120.5(2) . . ?
O6 Tb1 Ni1 91.7(2) . . ?
O5 Tb1 Ni1 143.5(2) . . ?
O3 Tb1 Ni1 96.5(2) . . ?
O1 Tb1 Ni1 92.4(2) . . ?
C23 Tb1 Ni1 133.9(3) . . ?
C30 Tb1 Ni1 118.1(3) . . ?

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
O1 C2 C3 C4 -178.7(11) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C65 179.3(11) . . . . ?
C5 C6 C7 O2 -177.0(10) . . . . ?
C65 C6 C7 O2 3.8(12) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C65 C6 C7 C2 -179.2(11) . . . . ?
O1 C2 C7 O2 -4.0(10) . . . . ?
C3 C2 C7 O2 177.2(9) . . . . ?
O1 C2 C7 C6 178.8(10) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
N1 C8 C9 C10 171.0(10) . . . . ?
N1 C8 C9 C14 -8.8(17) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C8 C9 C10 C11 -179.8(9) . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 O3 177.0(10) . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
O3 C13 C14 O4 7.5(9) . . . . ?
C12 C13 C14 O4 -175.4(8) . . . . ?
O3 C13 C14 C9 -177.2(9) . . . . ?
C12 C13 C14 C9 0.0 . . . . ?
C10 C9 C14 O4 175.1(9) . . . . ?
C8 C9 C14 O4 -5.2(11) . . . . ?
C10 C9 C14 C13 0.0 . . . . ?
C8 C9 C14 C13 179.8(10) . . . . ?
O9 C16 C17 C18 -170.4(9) . . . . ?
O10 C16 C17 C18 12.3(14) . . . . ?
O9 C16 C17 C22 10.8(14) . . . . ?
O10 C16 C17 C22 -166.5(9) . . . . ?
C22 C17 C18 C19 0.0 . . . . ?
C16 C17 C18 C19 -178.8(9) . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C17 0.0 . . . . ?
C18 C17 C22 C21 0.0 . . . . ?
C16 C17 C22 C21 178.8(9) . . . . ?
O7 C23 C24 C25 17.9(18) . . . . ?
O8 C23 C24 C25 -159.6(11) . . . . ?
O7 C23 C24 C29 -160.5(12) . . . . ?
O8 C23 C24 C29 22.0(17) . . . . ?
C29 C24 C25 C26 0.0 . . . . ?
C23 C24 C25 C26 -178.4(11) . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C24 0.0 . . . . ?
C25 C24 C29 C28 0.0 . . . . ?
C23 C24 C29 C28 178.3(11) . . . . ?
O5 C30 C31 C32 -20.4(18) . . . . ?
O6 C30 C31 C32 164.1(11) . . . . ?
O5 C30 C31 C36 163.1(12) . . . . ?
O6 C30 C31 C36 -12.4(17) . . . . ?
C36 C31 C32 C33 0.0 . . . . ?
C30 C31 C32 C33 -176.5(10) . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C31 0.0 . . . . ?
C32 C31 C36 C35 0.0 . . . . ?
C30 C31 C36 C35 176.4(11) . . . . ?
C5 C6 C65 N2 157.6(11) . . . . ?
C7 C6 C65 N2 -23.2(18) . . . . ?
C9 C8 N1 N1 173.3(12) . . . 2_655 ?
C9 C8 N1 Ni1 -4.5(17) . . . . ?
C6 C65 N2 N2 178.1(12) . . . 2_655 ?
C6 C65 N2 Ni1 1.1(19) . . . . ?
C3 C2 O1 C1 8.9(14) . . . . ?
C7 C2 O1 C1 -169.8(10) . . . . ?
C3 C2 O1 Tb1 178.0(5) . . . . ?
C7 C2 O1 Tb1 -0.7(10) . . . . ?
C6 C7 O2 Ni1 33.5(11) . . . . ?
C2 C7 O2 Ni1 -143.6(6) . . . . ?
C6 C7 O2 Tb1 -174.5(5) . . . . ?
C2 C7 O2 Tb1 8.4(11) . . . . ?
C12 C13 O3 C15 2.8(15) . . . . ?
C14 C13 O3 C15 179.8(10) . . . . ?
C12 C13 O3 Tb1 -173.3(5) . . . . ?
C14 C13 O3 Tb1 3.8(10) . . . . ?
C13 C14 O4 Ni1 -154.3(5) . . . . ?
C9 C14 O4 Ni1 30.4(10) . . . . ?
C13 C14 O4 Tb1 -16.4(9) . . . . ?
C9 C14 O4 Tb1 168.4(5) . . . . ?
O6 C30 O5 Tb1 -4.1(15) . . . . ?
C31 C30 O5 Tb1 -179.7(12) . . . . ?
O5 C30 O6 Tb1 4.1(15) . . . . ?
C31 C30 O6 Tb1 179.9(11) . . . . ?
O8 C23 O7 Tb1 -5.5(16) . . . . ?
C24 C23 O7 Tb1 177.3(11) . . . . ?
O7 C23 O8 Tb1 5.4(16) . . . . ?
C24 C23 O8 Tb1 -177.2(10) . . . . ?
O10 C16 O9 Tb1 18(2) . . . . ?
C17 C16 O9 Tb1 -158.9(9) . . . . ?
O9 C16 O10 Ni1 -21.3(18) . . . . ?
C17 C16 O10 Ni1 155.8(7) . . . . ?

_refine_diff_density_max         0.902
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.134


# start Validation Reply Form
_vrf_PLAT973_x                   
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_Tb2Zn2
_audit_block_doi                 10.5517/cc14htjz
_database_code_depnum_ccdc_archive 'CCDC 1057891'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C76 H70 N4 O24 Tb2 Zn2'
_chemical_formula_sum            'C76 H70 N4 O24 Tb2 Zn2'
_chemical_formula_weight         1851.94

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.847(4)
_cell_length_b                   16.792(4)
_cell_length_c                   23.040(5)
_cell_angle_alpha                90
_cell_angle_beta                 120.204(15)
_cell_angle_gamma                90
_cell_volume                     7974(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4924
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      23.51

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_F_000             3744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.423
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            22110
_diffrn_reflns_av_unetI/netI     0.1143
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.564
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_full        25.100
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             7038
_reflns_number_gt                3305
_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.

 The command 'isor' was also used to restrain the C, O and Tb atom 
 with NPD and ADP problems. The restraint command lead to restraint number 247, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the O8 O12 distance to
 be in the reasonable range.

 In the final refinement, the compounds show large solvent accessible void 
 and the sovlents cannot be determined.
;

_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7038
_refine_ls_number_parameters     430
_refine_ls_number_restraints     247
_refine_ls_R_factor_all          0.1886
_refine_ls_R_factor_gt           0.1024
_refine_ls_wR_factor_ref         0.3576
_refine_ls_wR_factor_gt          0.2730
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.114
_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
Tb1 Tb 0.75369(4) 0.08267(6) 0.33573(4) 0.0888(5) Uani 1 1 d . U . . .
Zn1 Zn 0.59177(8) 0.09949(11) 0.28514(10) 0.0723(6) Uani 1 1 d . . . . .
C1 C 0.7813(9) -0.0233(14) 0.2107(11) 0.121(7) Uani 1 1 d . U . . .
H1A H 0.7880 -0.0797 0.2178 0.182 Uiso 1 1 calc R U . . .
H1B H 0.8215 0.0040 0.2387 0.182 Uiso 1 1 calc R U . . .
H1C H 0.7664 -0.0114 0.1644 0.182 Uiso 1 1 calc R U . . .
C2 C 0.6742(5) -0.0309(8) 0.1901(7) 0.095(5) Uani 1 1 d G U . . .
C3 C 0.6555(7) -0.0783(9) 0.1338(8) 0.143(8) Uani 1 1 d G U . . .
H3 H 0.6848 -0.0889 0.1193 0.172 Uiso 1 1 calc R U . . .
C4 C 0.5932(8) -0.1097(9) 0.0992(7) 0.190(12) Uani 1 1 d G U . . .
H4 H 0.5807 -0.1413 0.0615 0.228 Uiso 1 1 calc R U . . .
C5 C 0.5495(6) -0.0937(8) 0.1209(7) 0.140(8) Uani 1 1 d G U . . .
H5 H 0.5078 -0.1147 0.0978 0.168 Uiso 1 1 calc R U . . .
C6 C 0.5681(5) -0.0464(8) 0.1772(7) 0.095(5) Uani 1 1 d G U . . .
C7 C 0.6305(5) -0.0150(7) 0.2118(5) 0.070(4) Uani 1 1 d G . . . .
C8 C 0.5221(7) -0.0422(10) 0.2021(9) 0.081(5) Uani 1 1 d . . . . .
H8 H 0.4895 -0.0803 0.1878 0.097 Uiso 1 1 calc R U . . .
C9 C 0.8574(11) 0.2240(14) 0.4555(13) 0.164(10) Uani 1 1 d . U . . .
H9A H 0.8772 0.2368 0.4292 0.245 Uiso 1 1 calc R U . . .
H9B H 0.8778 0.1776 0.4822 0.245 Uiso 1 1 calc R U . . .
H9C H 0.8625 0.2679 0.4844 0.245 Uiso 1 1 calc R U . . .
C10 C 0.7414(6) 0.2568(8) 0.4047(6) 0.099(6) Uani 1 1 d G U . . .
C11 C 0.7535(6) 0.3240(8) 0.4445(5) 0.118(7) Uani 1 1 d G U . . .
H11 H 0.7960 0.3387 0.4750 0.141 Uiso 1 1 calc R U . . .
C12 C 0.7021(8) 0.3692(7) 0.4387(6) 0.146(9) Uani 1 1 d G U . . .
H12 H 0.7101 0.4142 0.4653 0.175 Uiso 1 1 calc R U . . .
C13 C 0.6386(7) 0.3472(8) 0.3930(7) 0.131(8) Uani 1 1 d G U . . .
H13 H 0.6042 0.3774 0.3891 0.158 Uiso 1 1 calc R U . . .
C14 C 0.6265(5) 0.2800(8) 0.3532(5) 0.085(5) Uani 1 1 d G U . . .
C15 C 0.6780(7) 0.2348(6) 0.3591(5) 0.085(5) Uani 1 1 d G . . . .
C16 C 0.5588(9) 0.2624(10) 0.3091(8) 0.086(5) Uani 1 1 d . . . . .
H16 H 0.5295 0.3009 0.3064 0.104 Uiso 1 1 calc R U . . .
C17 C 0.8056(11) 0.1719(12) 0.2714(11) 0.101(6) Uani 1 1 d . U . . .
C18 C 0.8312(7) 0.2176(8) 0.2325(6) 0.100(6) Uani 1 1 d G U . . .
C19 C 0.8007(6) 0.2868(8) 0.1978(7) 0.113(6) Uani 1 1 d G U . . .
H19 H 0.7647 0.3062 0.1989 0.136 Uiso 1 1 calc R U . . .
C20 C 0.8239(7) 0.3269(7) 0.1614(7) 0.122(7) Uani 1 1 d G U . . .
H20 H 0.8035 0.3732 0.1382 0.147 Uiso 1 1 calc R U . . .
C21 C 0.8777(7) 0.2979(9) 0.1598(7) 0.120(7) Uani 1 1 d G U . . .
H21 H 0.8933 0.3248 0.1354 0.145 Uiso 1 1 calc R U . . .
C22 C 0.9082(6) 0.2288(9) 0.1945(8) 0.116(6) Uani 1 1 d G U . . .
H22 H 0.9442 0.2094 0.1934 0.139 Uiso 1 1 calc R U . . .
C23 C 0.8850(7) 0.1886(7) 0.2309(7) 0.126(7) Uani 1 1 d G U . . .
H23 H 0.9054 0.1423 0.2541 0.151 Uiso 1 1 calc R U . . .
C24 C 0.8481(10) -0.0172(14) 0.4280(10) 0.093(5) Uani 1 1 d . U . . .
C25 C 0.8949(8) -0.0780(11) 0.4771(8) 0.110(6) Uani 1 1 d G U . . .
C26 C 0.9524(10) -0.0483(9) 0.5299(10) 0.157(9) Uani 1 1 d G U . . .
H26 H 0.9603 0.0062 0.5337 0.188 Uiso 1 1 calc R U . . .
C27 C 0.9980(8) -0.1000(14) 0.5771(8) 0.172(11) Uani 1 1 d G U . . .
H27 H 1.0365 -0.0802 0.6125 0.206 Uiso 1 1 calc R U . . .
C28 C 0.9862(11) -0.1815(13) 0.5715(10) 0.202(13) Uani 1 1 d G U . . .
H28 H 1.0167 -0.2162 0.6031 0.242 Uiso 1 1 calc R U . . .
C29 C 0.9287(13) -0.2113(9) 0.5187(13) 0.219(14) Uani 1 1 d G U . . .
H29 H 0.9208 -0.2658 0.5149 0.263 Uiso 1 1 calc R U . . .
C30 C 0.8830(9) -0.1595(13) 0.4715(10) 0.187(12) Uani 1 1 d G U . . .
H30 H 0.8446 -0.1794 0.4361 0.224 Uiso 1 1 calc R U . . .
C31 C 0.6677(9) 0.0262(10) 0.4136(8) 0.078(4) Uani 1 1 d . . . . .
C32 C 0.6758(6) -0.0286(6) 0.4699(5) 0.088(5) Uani 1 1 d G . . . .
C33 C 0.7309(5) -0.0757(7) 0.5047(6) 0.071(4) Uani 1 1 d G . . . .
H33 H 0.7638 -0.0732 0.4942 0.086 Uiso 1 1 calc R U . . .
C34 C 0.7368(6) -0.1265(7) 0.5551(6) 0.119(7) Uani 1 1 d G U . . .
H34 H 0.7736 -0.1580 0.5783 0.143 Uiso 1 1 calc R U . . .
C35 C 0.6877(8) -0.1302(8) 0.5707(7) 0.141(8) Uani 1 1 d G U . . .
H35 H 0.6916 -0.1642 0.6044 0.169 Uiso 1 1 calc R U . . .
C36 C 0.6326(7) -0.0832(9) 0.5360(8) 0.157(10) Uani 1 1 d G U . . .
H36 H 0.5997 -0.0856 0.5464 0.189 Uiso 1 1 calc R U . . .
C37 C 0.6267(5) -0.0323(8) 0.4856(7) 0.114(6) Uani 1 1 d G U . . .
H37 H 0.5899 -0.0008 0.4623 0.137 Uiso 1 1 calc R U . . .
C38 C 0.5036(14) 0.1488(17) 0.0977(13) 0.166(10) Uani 1 1 d . U . . .
H38A H 0.4627 0.1611 0.0943 0.249 Uiso 1 1 calc R U . . .
H38B H 0.5021 0.0959 0.0813 0.249 Uiso 1 1 calc R U . . .
H38C H 0.5120 0.1861 0.0715 0.249 Uiso 1 1 calc R U . . .
N1 N 0.5335(6) 0.1981(7) 0.2723(6) 0.071(3) Uani 1 1 d . . . . .
N2 N 0.5252(5) 0.0106(7) 0.2417(7) 0.064(3) Uani 1 1 d . . . . .
O1 O 0.7342(5) 0.0019(8) 0.2271(6) 0.099(4) Uani 1 1 d . . . . .
O2 O 0.6502(4) 0.0335(6) 0.2619(5) 0.062(2) Uani 1 1 d . . . . .
O3 O 0.7870(6) 0.2078(8) 0.4099(6) 0.110(4) Uani 1 1 d . U . . .
O4 O 0.6706(5) 0.1718(7) 0.3229(5) 0.089(3) Uani 1 1 d . . . . .
O5 O 0.8490(7) 0.0490(10) 0.4371(7) 0.121(5) Uani 1 1 d . U . . .
O6 O 0.8054(7) -0.0506(9) 0.3693(8) 0.120(4) Uani 1 1 d . U . . .
O7 O 0.8386(6) 0.1223(9) 0.3133(7) 0.108(4) Uani 1 1 d . U . . .
O8 O 0.7492(6) 0.1881(8) 0.2596(6) 0.109(4) Uani 1 1 d D U . . .
O9 O 0.7175(5) 0.0326(7) 0.4085(5) 0.087(3) Uani 1 1 d . U . . .
O10 O 0.6149(5) 0.0578(6) 0.3786(5) 0.077(3) Uani 1 1 d . U . . .
O11 O 0.5548(10) 0.1537(12) 0.1674(10) 0.185(7) Uani 1 1 d . U . . .
H11A H 0.5850 0.1799 0.1702 0.278 Uiso 1 1 calc R U . . .
O12 O 0.6364(11) 0.2832(17) 0.1774(13) 0.137(10) Uani 0.5 1 d D U P . .


_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 O2 2.333(9) . ?
Tb1 O5 2.366(14) . ?
Tb1 O4 2.381(13) . ?
Tb1 O9 2.390(10) . ?
Tb1 O7 2.422(11) . ?
Tb1 O8 2.456(12) . ?
Tb1 O6 2.483(15) . ?
Tb1 O3 2.569(14) . ?
Tb1 O1 2.674(12) . ?
Tb1 C24 2.75(2) . ?
Tb1 C17 2.795(18) . ?
Tb1 Zn1 3.438(2) . ?
Zn1 O4 2.029(10) . ?
Zn1 N2 2.038(11) . ?
Zn1 O2 2.051(9) . ?
Zn1 O10 2.059(11) . ?
Zn1 N1 2.085(13) . ?
C1 O1 1.419(19) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.360(14) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.473(18) . ?
C7 O2 1.291(12) . ?
C8 N2 1.246(17) . ?
C8 H8 0.9300 . ?
C9 O3 1.49(2) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.318(17) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C16 1.44(2) . ?
C15 O4 1.302(14) . ?
C16 N1 1.318(18) . ?
C16 H16 0.9300 . ?
C17 O7 1.22(2) . ?
C17 O8 1.26(2) . ?
C17 C18 1.522(19) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O5 1.13(2) . ?
C24 O6 1.34(2) . ?
C24 C25 1.52(2) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O10 1.223(18) . ?
C31 O9 1.255(18) . ?
C31 C32 1.522(17) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 O11 1.45(3) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
N1 N1 1.40(2) 2_655 ?
N2 N2 1.44(2) 2_655 ?
O11 H11A 0.8200 . ?

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
O2 Tb1 O5 140.7(4) . . ?
O2 Tb1 O4 67.8(3) . . ?
O5 Tb1 O4 126.8(5) . . ?
O2 Tb1 O9 76.4(3) . . ?
O5 Tb1 O9 74.4(4) . . ?
O4 Tb1 O9 74.7(4) . . ?
O2 Tb1 O7 129.3(4) . . ?
O5 Tb1 O7 77.6(5) . . ?
O4 Tb1 O7 122.3(4) . . ?
O9 Tb1 O7 151.9(4) . . ?
O2 Tb1 O8 94.8(4) . . ?
O5 Tb1 O8 123.5(4) . . ?
O4 Tb1 O8 73.9(4) . . ?
O9 Tb1 O8 148.5(4) . . ?
O7 Tb1 O8 52.4(4) . . ?
O2 Tb1 O6 94.9(4) . . ?
O5 Tb1 O6 53.0(5) . . ?
O4 Tb1 O6 149.0(4) . . ?
O9 Tb1 O6 76.3(4) . . ?
O7 Tb1 O6 88.7(5) . . ?
O8 Tb1 O6 135.1(4) . . ?
O2 Tb1 O3 129.3(4) . . ?
O5 Tb1 O3 73.6(5) . . ?
O4 Tb1 O3 61.8(4) . . ?
O9 Tb1 O3 85.5(4) . . ?
O7 Tb1 O3 84.6(5) . . ?
O8 Tb1 O3 76.9(4) . . ?
O6 Tb1 O3 126.3(5) . . ?
O2 Tb1 O1 61.0(3) . . ?
O5 Tb1 O1 115.5(5) . . ?
O4 Tb1 O1 117.4(3) . . ?
O9 Tb1 O1 121.6(4) . . ?
O7 Tb1 O1 73.1(4) . . ?
O8 Tb1 O1 76.9(4) . . ?
O6 Tb1 O1 70.1(4) . . ?
O3 Tb1 O1 152.6(4) . . ?
O2 Tb1 C24 120.1(5) . . ?
O5 Tb1 C24 24.0(5) . . ?
O4 Tb1 C24 141.7(5) . . ?
O9 Tb1 C24 71.8(5) . . ?
O7 Tb1 C24 83.4(5) . . ?
O8 Tb1 C24 135.7(5) . . ?
O6 Tb1 C24 29.1(5) . . ?
O3 Tb1 C24 97.2(6) . . ?
O1 Tb1 C24 95.9(5) . . ?
O2 Tb1 C17 113.0(5) . . ?
O5 Tb1 C17 100.9(6) . . ?
O4 Tb1 C17 99.2(6) . . ?
O9 Tb1 C17 166.4(5) . . ?
O7 Tb1 C17 25.7(5) . . ?
O8 Tb1 C17 26.8(5) . . ?
O6 Tb1 C17 111.4(6) . . ?
O3 Tb1 C17 81.0(5) . . ?
O1 Tb1 C17 72.0(5) . . ?
C24 Tb1 C17 109.1(6) . . ?
O2 Tb1 Zn1 35.5(2) . . ?
O5 Tb1 Zn1 135.4(4) . . ?
O4 Tb1 Zn1 35.2(2) . . ?
O9 Tb1 Zn1 61.8(3) . . ?
O7 Tb1 Zn1 145.3(3) . . ?
O8 Tb1 Zn1 93.5(3) . . ?
O6 Tb1 Zn1 118.5(3) . . ?
O3 Tb1 Zn1 94.4(3) . . ?
O1 Tb1 Zn1 95.0(2) . . ?
C24 Tb1 Zn1 130.8(4) . . ?
C17 Tb1 Zn1 119.8(5) . . ?
O4 Zn1 N2 166.8(5) . . ?
O4 Zn1 O2 80.3(4) . . ?
N2 Zn1 O2 86.5(4) . . ?
O4 Zn1 O10 93.0(4) . . ?
N2 Zn1 O10 89.9(5) . . ?
O2 Zn1 O10 103.3(4) . . ?
O4 Zn1 N1 89.6(5) . . ?
N2 Zn1 N1 102.3(5) . . ?
O2 Zn1 N1 152.1(4) . . ?
O10 Zn1 N1 103.1(4) . . ?
O4 Zn1 Tb1 42.6(4) . . ?
N2 Zn1 Tb1 124.8(3) . . ?
O2 Zn1 Tb1 41.4(3) . . ?
O10 Zn1 Tb1 87.3(3) . . ?
N1 Zn1 Tb1 131.9(3) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.9(10) . . ?
O1 C2 C7 116.1(10) . . ?
C3 C2 C7 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C8 116.1(10) . . ?
C7 C6 C8 123.4(10) . . ?
O2 C7 C6 123.7(9) . . ?
O2 C7 C2 116.1(9) . . ?
C6 C7 C2 120.0 . . ?
N2 C8 C6 122.5(13) . . ?
N2 C8 H8 118.8 . . ?
C6 C8 H8 118.8 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 124.0(11) . . ?
O3 C10 C15 115.9(11) . . ?
C11 C10 C15 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C16 114.7(12) . . ?
C15 C14 C16 125.3(12) . . ?
O4 C15 C14 123.5(11) . . ?
O4 C15 C10 116.4(11) . . ?
C14 C15 C10 120.0 . . ?
N1 C16 C14 127.5(15) . . ?
N1 C16 H16 116.2 . . ?
C14 C16 H16 116.2 . . ?
O7 C17 O8 121.0(17) . . ?
O7 C17 C18 121.3(19) . . ?
O8 C17 C18 117.7(18) . . ?
O7 C17 Tb1 59.7(9) . . ?
O8 C17 Tb1 61.4(9) . . ?
C18 C17 Tb1 176.5(13) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 120.7(13) . . ?
C23 C18 C17 119.3(13) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O5 C24 O6 122(2) . . ?
O5 C24 C25 126(2) . . ?
O6 C24 C25 111.8(19) . . ?
O5 C24 Tb1 58.4(12) . . ?
O6 C24 Tb1 64.2(11) . . ?
C25 C24 Tb1 174.5(14) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 116.3(17) . . ?
C30 C25 C24 123.7(17) . . ?
C25 C26 C27 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O10 C31 O9 127.7(15) . . ?
O10 C31 C32 118.0(13) . . ?
O9 C31 C32 114.3(15) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 120.9(10) . . ?
C37 C32 C31 119.1(10) . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O11 C38 H38A 109.5 . . ?
O11 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O11 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C16 N1 N1 117.2(11) . 2_655 ?
C16 N1 Zn1 120.2(11) . . ?
N1 N1 Zn1 122.6(5) 2_655 . ?
C8 N2 N2 116.5(11) . 2_655 ?
C8 N2 Zn1 128.7(10) . . ?
N2 N2 Zn1 114.8(8) 2_655 . ?
C2 O1 C1 115.9(14) . . ?
C2 O1 Tb1 115.1(8) . . ?
C1 O1 Tb1 127.8(11) . . ?
C7 O2 Zn1 125.7(7) . . ?
C7 O2 Tb1 130.6(7) . . ?
Zn1 O2 Tb1 103.1(4) . . ?
C10 O3 C9 122.3(17) . . ?
C10 O3 Tb1 119.0(9) . . ?
C9 O3 Tb1 118.6(15) . . ?
C15 O4 Zn1 123.9(9) . . ?
C15 O4 Tb1 126.5(9) . . ?
Zn1 O4 Tb1 102.2(5) . . ?
C24 O5 Tb1 97.6(15) . . ?
C24 O6 Tb1 86.8(12) . . ?
C17 O7 Tb1 94.5(12) . . ?
C17 O8 Tb1 91.8(11) . . ?
C31 O9 Tb1 142.0(11) . . ?
C31 O10 Zn1 118.8(10) . . ?
C38 O11 H11A 109.5 . . ?

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
O1 C2 C3 C4 179.7(14) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C8 -171.5(14) . . . . ?
C5 C6 C7 O2 175.4(13) . . . . ?
C8 C6 C7 O2 -13.7(16) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C8 C6 C7 C2 170.9(15) . . . . ?
O1 C2 C7 O2 4.5(13) . . . . ?
C3 C2 C7 O2 -175.7(12) . . . . ?
O1 C2 C7 C6 -179.8(13) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C5 C6 C8 N2 -163.5(14) . . . . ?
C7 C6 C8 N2 25(2) . . . . ?
O3 C10 C11 C12 -175.6(13) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C16 178.6(11) . . . . ?
C13 C14 C15 O4 -179.0(11) . . . . ?
C16 C14 C15 O4 2.6(15) . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C16 C14 C15 C10 -178.4(13) . . . . ?
O3 C10 C15 O4 -5.0(12) . . . . ?
C11 C10 C15 O4 179.0(10) . . . . ?
O3 C10 C15 C14 175.9(12) . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C13 C14 C16 N1 -171.2(13) . . . . ?
C15 C14 C16 N1 7(2) . . . . ?
O7 C17 C18 C19 -163.9(16) . . . . ?
O8 C17 C18 C19 15(2) . . . . ?
O7 C17 C18 C23 17(2) . . . . ?
O8 C17 C18 C23 -163.7(15) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 -178.7(14) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C17 C18 C23 C22 178.7(14) . . . . ?
O5 C24 C25 C26 -17(3) . . . . ?
O6 C24 C25 C26 160.3(13) . . . . ?
O5 C24 C25 C30 163.2(18) . . . . ?
O6 C24 C25 C30 -20(2) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 -179.9(15) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 179.9(16) . . . . ?
O10 C31 C32 C33 170.0(12) . . . . ?
O9 C31 C32 C33 -9.2(19) . . . . ?
O10 C31 C32 C37 -8.7(19) . . . . ?
O9 C31 C32 C37 172.0(12) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C34 -178.8(12) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C31 C32 C37 C36 178.8(12) . . . . ?
C14 C16 N1 N1 -173.2(14) . . . 2_655 ?
C14 C16 N1 Zn1 10(2) . . . . ?
C6 C8 N2 N2 176.0(14) . . . 2_655 ?
C6 C8 N2 Zn1 -3(3) . . . . ?
C3 C2 O1 C1 -8.2(18) . . . . ?
C7 C2 O1 C1 171.5(13) . . . . ?
C3 C2 O1 Tb1 -176.8(7) . . . . ?
C7 C2 O1 Tb1 3.0(13) . . . . ?
C6 C7 O2 Zn1 -18.4(14) . . . . ?
C2 C7 O2 Zn1 157.2(7) . . . . ?
C6 C7 O2 Tb1 171.9(7) . . . . ?
C2 C7 O2 Tb1 -12.5(14) . . . . ?
C11 C10 O3 C9 -5.6(19) . . . . ?
C15 C10 O3 C9 178.6(13) . . . . ?
C11 C10 O3 Tb1 176.7(5) . . . . ?
C15 C10 O3 Tb1 0.9(12) . . . . ?
C14 C15 O4 Zn1 -29.0(13) . . . . ?
C10 C15 O4 Zn1 152.0(7) . . . . ?
C14 C15 O4 Tb1 -173.4(6) . . . . ?
C10 C15 O4 Tb1 7.5(12) . . . . ?
O6 C24 O5 Tb1 7(2) . . . . ?
C25 C24 O5 Tb1 -175.8(16) . . . . ?
O5 C24 O6 Tb1 -7(2) . . . . ?
C25 C24 O6 Tb1 175.8(13) . . . . ?
O8 C17 O7 Tb1 5(2) . . . . ?
C18 C17 O7 Tb1 -176.1(16) . . . . ?
O7 C17 O8 Tb1 -5(2) . . . . ?
C18 C17 O8 Tb1 176.1(15) . . . . ?
O10 C31 O9 Tb1 -10(3) . . . . ?
C32 C31 O9 Tb1 168.8(10) . . . . ?
O9 C31 O10 Zn1 20(2) . . . . ?
C32 C31 O10 Zn1 -159.3(10) . . . . ?

_refine_diff_density_max         3.073
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.203


# start Validation Reply Form
_vrf_PLAT973_x                   
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_Y2Co2
_audit_block_doi                 10.5517/cc14htk0
_database_code_depnum_ccdc_archive 'CCDC 1057892'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H74 Co2 N4 O26 Y2'
_chemical_formula_sum            'C78 H74 Co2 N4 O26 Y2'
_chemical_formula_weight         1779.09

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'
Co Co 0.3494 0.9721 '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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.133(2)
_cell_length_b                   17.0815(15)
_cell_length_c                   22.658(3)
_cell_angle_alpha                90
_cell_angle_beta                 121.2330(10)
_cell_angle_gamma                90
_cell_volume                     7986.5(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3731
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      23.69

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             3640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    1.928
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_T_max  0.667
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24208
_diffrn_reflns_av_unetI/netI     0.1398
_diffrn_reflns_av_R_equivalents  0.1170
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.548
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        25.242
_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             7858
_reflns_number_gt                3649
_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.

 The command 'isor' was also used to restrain all O and C atom with NPD and ADP
 problems. The restraint command lead to restraint number 313, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the H11a-H12a distance to
 be in the reasonable range

 The H-atoms on water cannot be determined.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.0869P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7858
_refine_ls_number_parameters     447
_refine_ls_number_restraints     313
_refine_ls_R_factor_all          0.1699
_refine_ls_R_factor_gt           0.0657
_refine_ls_wR_factor_ref         0.1953
_refine_ls_wR_factor_gt          0.1543
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.996
_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
C1 C 0.2235(4) -0.0188(6) 0.2941(5) 0.096(3) Uani 1 1 d . U . . .
H1A H 0.2151 -0.0740 0.2875 0.144 Uiso 1 1 calc R U . . .
H1B H 0.1841 0.0095 0.2649 0.144 Uiso 1 1 calc R U . . .
H1C H 0.2394 -0.0057 0.3415 0.144 Uiso 1 1 calc R U . . .
C2 C 0.33066(19) -0.0328(3) 0.3127(3) 0.061(2) Uani 1 1 d G U . . .
C3 C 0.3505(3) -0.0812(4) 0.3695(3) 0.100(3) Uani 1 1 d G U . . .
H3 H 0.3231 -0.0900 0.3864 0.120 Uiso 1 1 calc R U . . .
C4 C 0.4111(3) -0.1166(3) 0.4011(3) 0.117(4) Uani 1 1 d G U . . .
H4 H 0.4243 -0.1490 0.4391 0.141 Uiso 1 1 calc R U . . .
C5 C 0.4519(2) -0.1036(3) 0.3758(3) 0.096(3) Uani 1 1 d G U . . .
H5 H 0.4925 -0.1273 0.3970 0.115 Uiso 1 1 calc R U . . .
C6 C 0.4321(2) -0.0551(3) 0.3190(3) 0.059(2) Uani 1 1 d G U . . .
C7 C 0.3715(2) -0.0197(3) 0.2875(2) 0.0516(19) Uani 1 1 d G U . . .
C8 C 0.4777(3) -0.0455(4) 0.2970(4) 0.058(2) Uani 1 1 d . U . . .
H8 H 0.5104 -0.0826 0.3111 0.069 Uiso 1 1 calc R U . . .
C9 C 0.1475(3) 0.2242(5) 0.0479(5) 0.108(4) Uani 1 1 d . U . . .
H9A H 0.1210 0.1912 0.0576 0.162 Uiso 1 1 calc R U . . .
H9B H 0.1363 0.2164 0.0010 0.162 Uiso 1 1 calc R U . . .
H9C H 0.1404 0.2780 0.0544 0.162 Uiso 1 1 calc R U . . .
C10 C 0.25916(19) 0.2531(3) 0.0953(3) 0.063(2) Uani 1 1 d G U . . .
C11 C 0.2456(2) 0.3187(3) 0.0536(2) 0.076(3) Uani 1 1 d G U . . .
H11 H 0.2028 0.3331 0.0230 0.091 Uiso 1 1 calc R U . . .
C12 C 0.2959(3) 0.3628(3) 0.0578(3) 0.096(3) Uani 1 1 d G U . . .
H12 H 0.2868 0.4066 0.0300 0.115 Uiso 1 1 calc R U . . .
C13 C 0.3598(3) 0.3412(3) 0.1036(3) 0.084(3) Uani 1 1 d G U . . .
H13 H 0.3935 0.3707 0.1065 0.101 Uiso 1 1 calc R U . . .
C14 C 0.37343(18) 0.2756(3) 0.1453(2) 0.056(2) Uani 1 1 d G U . . .
C15 C 0.3231(2) 0.2316(2) 0.1411(2) 0.0482(18) Uani 1 1 d G U . . .
C16 C 0.4408(3) 0.2579(4) 0.1898(4) 0.0530(19) Uani 1 1 d . U . . .
H16 H 0.4700 0.2949 0.1917 0.064 Uiso 1 1 calc R U . . .
C17 C 0.1538(3) -0.0159(6) 0.0736(4) 0.060(2) Uani 1 1 d . U . . .
C18 C 0.1047(2) -0.0698(4) 0.0207(3) 0.067(2) Uani 1 1 d G U . . .
C19 C 0.0461(3) -0.0396(3) -0.0316(3) 0.098(3) Uani 1 1 d G U . . .
H19 H 0.0385 0.0140 -0.0342 0.118 Uiso 1 1 calc R U . . .
C20 C -0.0011(2) -0.0895(5) -0.0799(3) 0.110(4) Uani 1 1 d G U . . .
H20 H -0.0403 -0.0694 -0.1149 0.132 Uiso 1 1 calc R U . . .
C21 C 0.0103(3) -0.1697(4) -0.0760(3) 0.116(4) Uani 1 1 d G U . . .
H21 H -0.0213 -0.2031 -0.1084 0.139 Uiso 1 1 calc R U . . .
C22 C 0.0689(4) -0.1999(3) -0.0237(4) 0.125(4) Uani 1 1 d G U . . .
H22 H 0.0765 -0.2535 -0.0211 0.150 Uiso 1 1 calc R U . . .
C23 C 0.1161(3) -0.1499(4) 0.0247(3) 0.092(3) Uani 1 1 d G U . . .
H23 H 0.1553 -0.1701 0.0597 0.111 Uiso 1 1 calc R U . . .
C24 C 0.1994(4) 0.1708(5) 0.2305(4) 0.062(2) Uani 1 1 d . U . . .
C25 C 0.1735(3) 0.2187(3) 0.2672(2) 0.063(2) Uani 1 1 d G U . . .
C26 C 0.1202(3) 0.1910(3) 0.2689(3) 0.091(3) Uani 1 1 d G U . . .
H26 H 0.0997 0.1451 0.2458 0.109 Uiso 1 1 calc R U . . .
C27 C 0.0974(2) 0.2320(4) 0.3051(3) 0.101(3) Uani 1 1 d G U . . .
H27 H 0.0617 0.2135 0.3062 0.121 Uiso 1 1 calc R U . . .
C28 C 0.1280(3) 0.3007(4) 0.3396(3) 0.095(3) Uani 1 1 d G U . . .
H28 H 0.1128 0.3281 0.3638 0.114 Uiso 1 1 calc R U . . .
C29 C 0.1813(3) 0.3283(3) 0.3379(3) 0.084(3) Uani 1 1 d G U . . .
H29 H 0.2018 0.3743 0.3610 0.101 Uiso 1 1 calc R U . . .
C30 C 0.2041(2) 0.2873(3) 0.3017(3) 0.070(2) Uani 1 1 d G U . . .
H30 H 0.2398 0.3058 0.3006 0.084 Uiso 1 1 calc R U . . .
C31 C 0.3302(3) 0.0286(4) 0.0871(3) 0.0411(16) Uani 1 1 d . U . . .
C32 C 0.3240(2) -0.0276(3) 0.0331(2) 0.0471(18) Uani 1 1 d G U . . .
C33 C 0.3743(2) -0.0342(3) 0.0204(3) 0.071(2) Uani 1 1 d G U . . .
H33 H 0.4108 -0.0026 0.0442 0.085 Uiso 1 1 calc R U . . .
C34 C 0.3701(2) -0.0881(4) -0.0278(3) 0.086(3) Uani 1 1 d G U . . .
H34 H 0.4037 -0.0925 -0.0363 0.103 Uiso 1 1 calc R U . . .
C35 C 0.3155(3) -0.1353(3) -0.0632(2) 0.086(3) Uani 1 1 d G U . . .
H35 H 0.3127 -0.1713 -0.0955 0.103 Uiso 1 1 calc R U . . .
C36 C 0.2653(2) -0.1287(3) -0.0505(3) 0.084(3) Uani 1 1 d G U . . .
H36 H 0.2288 -0.1602 -0.0743 0.100 Uiso 1 1 calc R U . . .
C37 C 0.2695(2) -0.0748(3) -0.0023(3) 0.061(2) Uani 1 1 d G U . . .
H37 H 0.2358 -0.0704 0.0062 0.073 Uiso 1 1 calc R U . . .
C38 C 0.4961(4) 0.1330(6) 0.3950(4) 0.083(3) Uani 1 1 d . U . . .
H38A H 0.5304 0.1095 0.3915 0.124 Uiso 1 1 calc R U . . .
H38B H 0.4869 0.1013 0.4239 0.124 Uiso 1 1 calc R U . . .
H38C H 0.5091 0.1843 0.4147 0.124 Uiso 1 1 calc R U . . .
C39 C 0.3852(6) 0.3214(7) 0.3221(6) 0.130(4) Uani 1 1 d . U . . .
H39A H 0.3613 0.3621 0.3283 0.195 Uiso 1 1 calc R U . . .
H39B H 0.3743 0.3206 0.2749 0.195 Uiso 1 1 calc R U . . .
H39C H 0.4308 0.3310 0.3517 0.195 Uiso 1 1 calc R U . . .
Co1 Co 0.41112(4) 0.10137(5) 0.22409(4) 0.0401(3) Uani 1 1 d . . . . .
N1 N 0.4654(2) 0.1965(3) 0.2274(3) 0.0431(14) Uani 1 1 d . . . . .
N2 N 0.4760(2) 0.0111(3) 0.2589(3) 0.0437(14) Uani 1 1 d . . . . .
O1 O 0.2718(2) 0.0023(3) 0.2767(2) 0.0666(15) Uani 1 1 d . U . . .
O2 O 0.34977(19) 0.0295(3) 0.2345(2) 0.0465(12) Uani 1 1 d . U . . .
O3 O 0.2135(2) 0.2051(3) 0.0930(2) 0.0648(15) Uani 1 1 d . U . . .
O4 O 0.33205(19) 0.1706(3) 0.1819(2) 0.0465(12) Uani 1 1 d . U . . .
O5 O 0.1655(2) 0.1198(4) 0.1870(3) 0.0784(18) Uani 1 1 d . U . . .
O6 O 0.2564(2) 0.1833(3) 0.2444(3) 0.0704(16) Uani 1 1 d . U . . .
O7 O 0.1514(2) 0.0565(4) 0.0595(3) 0.0647(15) Uani 1 1 d . U . . .
O8 O 0.1982(2) -0.0430(3) 0.1307(3) 0.0664(15) Uani 1 1 d . U . . .
O9 O 0.2801(2) 0.0389(3) 0.0895(2) 0.0508(12) Uani 1 1 d . U . . .
O10 O 0.3840(2) 0.0602(3) 0.1259(2) 0.0476(12) Uani 1 1 d . U . . .
O11 O 0.4401(2) 0.1388(3) 0.3288(2) 0.0656(15) Uani 1 1 d . U . . .
H11A H 0.4165 0.1733 0.3287 0.098 Uiso 1 1 calc DR U . . .
O12 O 0.3694(3) 0.2476(4) 0.3393(3) 0.0931(19) Uani 1 1 d . U . . .
H12A H 0.3309 0.2382 0.3125 0.140 Uiso 1 1 calc DR U . . .
O13 O 0.5000 0.4743(17) 0.2500 0.447(17) Uani 1 2 d S TU P . .
Y1 Y 0.24942(3) 0.08341(5) 0.16471(3) 0.0505(3) 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
C1 O1 1.456(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.358(6) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.434(8) . ?
C7 O2 1.330(5) . ?
C8 N2 1.283(8) . ?
C8 H8 0.9300 . ?
C9 O3 1.414(8) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.354(6) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C16 1.433(7) . ?
C15 O4 1.334(5) . ?
C16 N1 1.285(8) . ?
C16 H16 0.9300 . ?
C17 O8 1.265(9) . ?
C17 O7 1.271(9) . ?
C17 C18 1.487(9) . ?
C17 Y1 2.744(8) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O5 1.250(9) . ?
C24 O6 1.259(8) . ?
C24 C25 1.513(8) . ?
C24 Y1 2.788(8) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O10 1.252(7) . ?
C31 O9 1.251(7) . ?
C31 C32 1.500(7) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 O11 1.409(7) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 O12 1.427(11) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
Co1 O4 2.015(4) . ?
Co1 O2 2.029(4) . ?
Co1 N2 2.043(5) . ?
Co1 N1 2.065(5) . ?
Co1 O10 2.088(4) . ?
Co1 O11 2.191(5) . ?
Co1 Y1 3.4187(10) . ?
N1 N1 1.437(9) 2_655 ?
N2 N2 1.410(10) 2_655 ?
O1 Y1 2.689(5) . ?
O2 Y1 2.290(4) . ?
O3 Y1 2.500(5) . ?
O4 Y1 2.354(4) . ?
O5 Y1 2.410(5) . ?
O6 Y1 2.426(5) . ?
O7 Y1 2.374(5) . ?
O8 Y1 2.407(5) . ?
O9 Y1 2.311(5) . ?
O11 H11A 0.8200 . ?
O12 H12A 0.8200 . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.7(4) . . ?
O1 C2 C7 115.2(4) . . ?
C3 C2 C7 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C8 115.7(4) . . ?
C7 C6 C8 124.3(4) . . ?
O2 C7 C6 123.8(4) . . ?
O2 C7 C2 116.1(4) . . ?
C6 C7 C2 120.0 . . ?
N2 C8 C6 123.9(6) . . ?
N2 C8 H8 118.1 . . ?
C6 C8 H8 118.1 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 124.2(4) . . ?
O3 C10 C15 115.8(4) . . ?
C11 C10 C15 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C16 115.5(4) . . ?
C15 C14 C16 124.5(4) . . ?
O4 C15 C14 123.6(4) . . ?
O4 C15 C10 116.3(4) . . ?
C14 C15 C10 120.0 . . ?
N1 C16 C14 127.2(6) . . ?
N1 C16 H16 116.4 . . ?
C14 C16 H16 116.4 . . ?
O8 C17 O7 121.1(8) . . ?
O8 C17 C18 119.7(8) . . ?
O7 C17 C18 119.2(7) . . ?
O8 C17 Y1 61.3(4) . . ?
O7 C17 Y1 59.8(4) . . ?
C18 C17 Y1 175.1(5) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 119.3(6) . . ?
C23 C18 C17 120.6(6) . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O5 C24 O6 120.0(7) . . ?
O5 C24 C25 121.4(7) . . ?
O6 C24 C25 118.7(7) . . ?
O5 C24 Y1 59.6(4) . . ?
O6 C24 Y1 60.3(4) . . ?
C25 C24 Y1 179.0(6) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 119.0(5) . . ?
C30 C25 C24 121.0(5) . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 120.0 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O10 C31 O9 125.7(6) . . ?
O10 C31 C32 118.5(6) . . ?
O9 C31 C32 115.8(6) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 119.5(4) . . ?
C37 C32 C31 120.4(4) . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O11 C38 H38A 109.5 . . ?
O11 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O11 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O12 C39 H39A 109.5 . . ?
O12 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O12 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O4 Co1 O2 80.89(18) . . ?
O4 Co1 N2 166.90(19) . . ?
O2 Co1 N2 87.59(19) . . ?
O4 Co1 N1 88.97(19) . . ?
O2 Co1 N1 163.7(2) . . ?
N2 Co1 N1 103.6(2) . . ?
O4 Co1 O10 89.76(17) . . ?
O2 Co1 O10 94.38(18) . . ?
N2 Co1 O10 84.91(19) . . ?
N1 Co1 O10 98.38(19) . . ?
O4 Co1 O11 91.99(17) . . ?
O2 Co1 O11 83.9(2) . . ?
N2 Co1 O11 92.9(2) . . ?
N1 Co1 O11 83.7(2) . . ?
O10 Co1 O11 177.30(19) . . ?
O4 Co1 Y1 42.19(13) . . ?
O2 Co1 Y1 40.42(12) . . ?
N2 Co1 Y1 125.06(14) . . ?
N1 Co1 Y1 131.16(14) . . ?
O10 Co1 Y1 83.55(12) . . ?
O11 Co1 Y1 96.38(14) . . ?
C16 N1 N1 116.0(4) . 2_655 ?
C16 N1 Co1 123.5(4) . . ?
N1 N1 Co1 120.4(2) 2_655 . ?
C8 N2 N2 116.6(5) . 2_655 ?
C8 N2 Co1 125.4(5) . . ?
N2 N2 Co1 117.9(3) 2_655 . ?
C2 O1 C1 117.6(6) . . ?
C2 O1 Y1 115.5(3) . . ?
C1 O1 Y1 125.9(5) . . ?
C7 O2 Co1 121.2(3) . . ?
C7 O2 Y1 131.2(3) . . ?
Co1 O2 Y1 104.50(18) . . ?
C10 O3 C9 118.5(6) . . ?
C10 O3 Y1 118.5(3) . . ?
C9 O3 Y1 122.9(5) . . ?
C15 O4 Co1 124.1(3) . . ?
C15 O4 Y1 124.1(3) . . ?
Co1 O4 Y1 102.70(19) . . ?
C24 O5 Y1 93.8(5) . . ?
C24 O6 Y1 92.8(5) . . ?
C17 O7 Y1 92.6(4) . . ?
C17 O8 Y1 91.2(5) . . ?
C31 O9 Y1 139.9(4) . . ?
C31 O10 Co1 122.1(4) . . ?
C38 O11 Co1 136.4(5) . . ?
C38 O11 H11A 109.5 . . ?
Co1 O11 H11A 112.2 . . ?
C39 O12 H12A 109.5 . . ?
O2 Y1 O9 75.45(15) . . ?
O2 Y1 O4 68.79(15) . . ?
O9 Y1 O4 76.24(15) . . ?
O2 Y1 O7 139.62(18) . . ?
O9 Y1 O7 74.28(16) . . ?
O4 Y1 O7 127.28(18) . . ?
O2 Y1 O8 92.53(17) . . ?
O9 Y1 O8 77.12(17) . . ?
O4 Y1 O8 150.56(16) . . ?
O7 Y1 O8 55.01(18) . . ?
O2 Y1 O5 131.43(17) . . ?
O9 Y1 O5 149.93(16) . . ?
O4 Y1 O5 122.27(18) . . ?
O7 Y1 O5 75.70(18) . . ?
O8 Y1 O5 87.17(19) . . ?
O2 Y1 O6 97.37(16) . . ?
O9 Y1 O6 148.78(18) . . ?
O4 Y1 O6 72.89(16) . . ?
O7 Y1 O6 122.14(18) . . ?
O8 Y1 O6 134.01(18) . . ?
O5 Y1 O6 53.39(17) . . ?
O2 Y1 O3 132.05(16) . . ?
O9 Y1 O3 86.01(16) . . ?
O4 Y1 O3 63.92(15) . . ?
O7 Y1 O3 71.28(19) . . ?
O8 Y1 O3 126.17(17) . . ?
O5 Y1 O3 82.83(19) . . ?
O6 Y1 O3 76.43(17) . . ?
O2 Y1 O1 61.19(15) . . ?
O9 Y1 O1 122.86(16) . . ?
O4 Y1 O1 115.56(14) . . ?
O7 Y1 O1 117.13(18) . . ?
O8 Y1 O1 70.03(16) . . ?
O5 Y1 O1 73.38(18) . . ?
O6 Y1 O1 75.95(18) . . ?
O3 Y1 O1 150.87(17) . . ?
O2 Y1 C17 116.6(2) . . ?
O9 Y1 C17 73.01(19) . . ?
O4 Y1 C17 145.7(2) . . ?
O7 Y1 C17 27.57(19) . . ?
O8 Y1 C17 27.5(2) . . ?
O5 Y1 C17 81.2(2) . . ?
O6 Y1 C17 134.57(19) . . ?
O3 Y1 C17 98.7(2) . . ?
O1 Y1 C17 94.1(2) . . ?
O2 Y1 C24 116.22(19) . . ?
O9 Y1 C24 164.5(2) . . ?
O4 Y1 C24 97.9(2) . . ?
O7 Y1 C24 99.1(2) . . ?
O8 Y1 C24 111.0(2) . . ?
O5 Y1 C24 26.58(19) . . ?
O6 Y1 C24 26.81(19) . . ?
O3 Y1 C24 78.5(2) . . ?
O1 Y1 C24 72.6(2) . . ?
C17 Y1 C24 107.8(2) . . ?
O2 Y1 Co1 35.08(11) . . ?
O9 Y1 Co1 65.35(11) . . ?
O4 Y1 Co1 35.10(10) . . ?
O7 Y1 Co1 138.74(13) . . ?
O8 Y1 Co1 119.90(13) . . ?
O5 Y1 Co1 143.73(13) . . ?
O6 Y1 Co1 91.11(12) . . ?
O3 Y1 Co1 97.01(11) . . ?
O1 Y1 Co1 92.60(10) . . ?
C17 Y1 Co1 134.02(16) . . ?
C24 Y1 Co1 117.61(18) . . ?

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
O1 C2 C3 C4 177.6(6) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C8 -179.9(6) . . . . ?
C5 C6 C7 O2 177.6(5) . . . . ?
C8 C6 C7 O2 -2.5(7) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C8 C6 C7 C2 179.9(6) . . . . ?
O1 C2 C7 O2 4.5(5) . . . . ?
C3 C2 C7 O2 -177.7(5) . . . . ?
O1 C2 C7 C6 -177.8(5) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C5 C6 C8 N2 -160.7(6) . . . . ?
C7 C6 C8 N2 19.4(10) . . . . ?
O3 C10 C11 C12 -177.5(5) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C16 179.0(5) . . . . ?
C13 C14 C15 O4 -176.0(5) . . . . ?
C16 C14 C15 O4 5.0(6) . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C16 C14 C15 C10 -178.9(6) . . . . ?
O3 C10 C15 O4 -5.9(5) . . . . ?
C11 C10 C15 O4 176.3(4) . . . . ?
O3 C10 C15 C14 177.7(5) . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C13 C14 C16 N1 -172.1(6) . . . . ?
C15 C14 C16 N1 6.8(10) . . . . ?
O8 C17 C18 C19 160.3(5) . . . . ?
O7 C17 C18 C19 -21.8(9) . . . . ?
O8 C17 C18 C23 -17.5(9) . . . . ?
O7 C17 C18 C23 160.3(6) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 -177.8(6) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C17 C18 C23 C22 177.8(6) . . . . ?
O5 C24 C25 C26 19.4(9) . . . . ?
O6 C24 C25 C26 -160.7(6) . . . . ?
O5 C24 C25 C30 -163.7(6) . . . . ?
O6 C24 C25 C30 16.1(9) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 176.9(5) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 -176.8(5) . . . . ?
O10 C31 C32 C33 -9.7(7) . . . . ?
O9 C31 C32 C33 171.0(5) . . . . ?
O10 C31 C32 C37 168.1(4) . . . . ?
O9 C31 C32 C37 -11.3(7) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C34 177.8(5) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C31 C32 C37 C36 -177.7(5) . . . . ?
C14 C16 N1 N1 -174.1(6) . . . 2_655 ?
C14 C16 N1 Co1 6.7(10) . . . . ?
C6 C8 N2 N2 -179.1(6) . . . 2_655 ?
C6 C8 N2 Co1 2.2(10) . . . . ?
C3 C2 O1 C1 -6.9(8) . . . . ?
C7 C2 O1 C1 170.8(5) . . . . ?
C3 C2 O1 Y1 -175.9(3) . . . . ?
C7 C2 O1 Y1 1.8(5) . . . . ?
C6 C7 O2 Co1 -32.2(6) . . . . ?
C2 C7 O2 Co1 145.4(3) . . . . ?
C6 C7 O2 Y1 171.2(3) . . . . ?
C2 C7 O2 Y1 -11.2(6) . . . . ?
C11 C10 O3 C9 -3.0(8) . . . . ?
C15 C10 O3 C9 179.4(5) . . . . ?
C11 C10 O3 Y1 174.2(2) . . . . ?
C15 C10 O3 Y1 -3.4(5) . . . . ?
C14 C15 O4 Co1 -28.9(6) . . . . ?
C10 C15 O4 Co1 154.9(3) . . . . ?
C14 C15 O4 Y1 -170.0(3) . . . . ?
C10 C15 O4 Y1 13.9(5) . . . . ?
O6 C24 O5 Y1 0.5(8) . . . . ?
C25 C24 O5 Y1 -179.7(6) . . . . ?
O5 C24 O6 Y1 -0.5(8) . . . . ?
C25 C24 O6 Y1 179.7(6) . . . . ?
O8 C17 O7 Y1 3.3(7) . . . . ?
C18 C17 O7 Y1 -174.5(5) . . . . ?
O7 C17 O8 Y1 -3.2(7) . . . . ?
C18 C17 O8 Y1 174.6(6) . . . . ?
O10 C31 O9 Y1 -19.5(11) . . . . ?
C32 C31 O9 Y1 159.8(4) . . . . ?
O9 C31 O10 Co1 24.4(9) . . . . ?
C32 C31 O10 Co1 -154.9(4) . . . . ?

_refine_diff_density_max         1.039
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_Y2Cu2
_audit_block_doi                 10.5517/cc14htl1
_database_code_depnum_ccdc_archive 'CCDC 1057893'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H66 Cu2 N4 O24 Y2'
_chemical_formula_sum            'C74 H66 Cu2 N4 O24 Y2'
_chemical_formula_weight         1700.20

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'
Cu Cu 0.3201 1.2651 '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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.530(12)
_cell_length_b                   16.641(8)
_cell_length_c                   23.044(16)
_cell_angle_alpha                90
_cell_angle_beta                 119.75(3)
_cell_angle_gamma                90
_cell_volume                     7834(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2988
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      21.79

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_F_000             3464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.079
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23802
_diffrn_reflns_av_unetI/netI     0.1755
_diffrn_reflns_av_R_equivalents  0.1545
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.587
_diffrn_reflns_theta_max         26.197
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7733
_reflns_number_gt                3115
_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.

 The command 'isor' was also used to restrain the all O and C atom with NPD and ADP
 problems. The restraint command lead to restraint number 298, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the H11-H9A, H3-H1A and O11-O12 distance to
 be in the reasonable range

 The H-atoms on water cannot be determined.

 The DELU command has been used to refine the  High Ueq of O6. 

 The compounds show large solvent accessible void 
 and the sovlents cannot be determined.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.1674P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7733
_refine_ls_number_parameters     420
_refine_ls_number_restraints     298
_refine_ls_R_factor_all          0.2204
_refine_ls_R_factor_gt           0.0899
_refine_ls_wR_factor_ref         0.3214
_refine_ls_wR_factor_gt          0.2499
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      1.010
_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
C1 C 0.1463(6) 0.2284(9) 0.0455(7) 0.122(6) Uani 1 1 d . U . . .
H1A H 0.1390 0.2831 0.0533 0.183 Uiso 1 1 calc DR U . . .
H1B H 0.1175 0.1937 0.0522 0.183 Uiso 1 1 calc R U . . .
H1C H 0.1378 0.2229 0.0004 0.183 Uiso 1 1 calc R U . . .
C2 C 0.2598(3) 0.2561(5) 0.0933(4) 0.070(3) Uani 1 1 d G U . . .
C3 C 0.2477(4) 0.3235(5) 0.0531(4) 0.097(4) Uani 1 1 d G U . . .
H3 H 0.2050 0.3380 0.0225 0.117 Uiso 1 1 calc DR U . . .
C4 C 0.2997(5) 0.3693(4) 0.0588(4) 0.110(5) Uani 1 1 d G U . . .
H4 H 0.2916 0.4144 0.0320 0.132 Uiso 1 1 calc R U . . .
C5 C 0.3637(4) 0.3477(5) 0.1046(5) 0.105(5) Uani 1 1 d G U . . .
H5 H 0.3984 0.3783 0.1085 0.126 Uiso 1 1 calc R U . . .
C6 C 0.3757(3) 0.2803(5) 0.1448(4) 0.067(3) Uani 1 1 d G U . . .
C7 C 0.3237(4) 0.2345(4) 0.1391(3) 0.059(3) Uani 1 1 d G U . . .
C8 C 0.4440(6) 0.2606(7) 0.1918(6) 0.068(3) Uani 1 1 d . U . . .
H8 H 0.4750 0.2984 0.1959 0.082 Uiso 1 1 calc R U . . .
C9 C 0.2150(6) -0.0279(9) 0.2838(8) 0.106(5) Uani 1 1 d . U . . .
H9A H 0.2153 -0.0855 0.2858 0.159 Uiso 1 1 calc DR U . . .
H9B H 0.1728 -0.0098 0.2495 0.159 Uiso 1 1 calc R U . . .
H9C H 0.2238 -0.0062 0.3261 0.159 Uiso 1 1 calc R U . . .
C10 C 0.3259(3) -0.0303(5) 0.3078(4) 0.075(3) Uani 1 1 d G U . . .
C11 C 0.3436(4) -0.0808(6) 0.3622(5) 0.115(5) Uani 1 1 d G U . . .
H11 H 0.3133 -0.0937 0.3754 0.138 Uiso 1 1 calc DR U . . .
C12 C 0.4066(5) -0.1122(6) 0.3967(4) 0.147(7) Uani 1 1 d G U . . .
H12 H 0.4184 -0.1460 0.4330 0.176 Uiso 1 1 calc R U . . .
C13 C 0.4519(4) -0.0930(6) 0.3768(5) 0.118(5) Uani 1 1 d G U . . .
H13 H 0.4941 -0.1139 0.3999 0.142 Uiso 1 1 calc R U . . .
C14 C 0.4342(3) -0.0424(5) 0.3225(4) 0.069(3) Uani 1 1 d G U . . .
C15 C 0.3712(3) -0.0111(4) 0.2880(3) 0.059(3) Uani 1 1 d G U . . .
C16 C 0.4806(5) -0.0299(6) 0.3013(6) 0.064(3) Uani 1 1 d . U . . .
H16 H 0.5175 -0.0626 0.3192 0.077 Uiso 1 1 calc R U . . .
C17 C 0.1524(7) -0.0227(10) 0.0731(8) 0.082(4) Uani 1 1 d . U . . .
C18 C 0.1044(4) -0.0787(6) 0.0208(4) 0.079(4) Uani 1 1 d G U . . .
C19 C 0.1182(4) -0.1603(6) 0.0238(5) 0.115(5) Uani 1 1 d G U . . .
H19 H 0.1577 -0.1801 0.0579 0.138 Uiso 1 1 calc R U . . .
C20 C 0.0730(6) -0.2122(5) -0.0241(6) 0.131(6) Uani 1 1 d G U . . .
H20 H 0.0822 -0.2668 -0.0221 0.157 Uiso 1 1 calc R U . . .
C21 C 0.0140(5) -0.1826(7) -0.0750(5) 0.139(6) Uani 1 1 d G U . . .
H21 H -0.0163 -0.2173 -0.1071 0.167 Uiso 1 1 calc R U . . .
C22 C 0.0002(4) -0.1009(7) -0.0781(5) 0.115(5) Uani 1 1 d G U . . .
H22 H -0.0393 -0.0811 -0.1121 0.138 Uiso 1 1 calc R U . . .
C23 C 0.0454(5) -0.0490(5) -0.0302(5) 0.120(6) Uani 1 1 d G U . . .
H23 H 0.0362 0.0056 -0.0322 0.144 Uiso 1 1 calc R U . . .
C24 C 0.1966(7) 0.1711(9) 0.2266(6) 0.079(4) Uani 1 1 d . U . . .
C25 C 0.1705(4) 0.2208(6) 0.2642(4) 0.079(4) Uani 1 1 d G U . . .
C26 C 0.1152(4) 0.1925(5) 0.2648(4) 0.104(5) Uani 1 1 d G U . . .
H26 H 0.0939 0.1468 0.2405 0.125 Uiso 1 1 calc R U . . .
C27 C 0.0918(4) 0.2325(7) 0.3016(5) 0.114(5) Uani 1 1 d G U . . .
H27 H 0.0547 0.2135 0.3019 0.137 Uiso 1 1 calc R U . . .
C28 C 0.1236(5) 0.3008(6) 0.3379(5) 0.116(5) Uani 1 1 d G U . . .
H28 H 0.1079 0.3275 0.3625 0.139 Uiso 1 1 calc R U . . .
C29 C 0.1789(5) 0.3291(5) 0.3374(4) 0.102(5) Uani 1 1 d G U . . .
H29 H 0.2003 0.3748 0.3617 0.122 Uiso 1 1 calc R U . . .
C30 C 0.2024(4) 0.2891(6) 0.3006(5) 0.084(4) Uani 1 1 d G U . . .
H30 H 0.2394 0.3081 0.3002 0.101 Uiso 1 1 calc R U . . .
C31 C 0.3315(5) 0.0242(7) 0.0838(5) 0.051(3) Uani 1 1 d . U . . .
C32 C 0.3225(4) -0.0302(5) 0.0277(3) 0.061(3) Uani 1 1 d G U . . .
C33 C 0.2679(4) -0.0794(5) -0.0055(4) 0.074(4) Uani 1 1 d G U . . .
H33 H 0.2360 -0.0796 0.0071 0.089 Uiso 1 1 calc R U . . .
C34 C 0.2610(4) -0.1282(5) -0.0575(4) 0.108(5) Uani 1 1 d G U . . .
H34 H 0.2245 -0.1612 -0.0798 0.130 Uiso 1 1 calc R U . . .
C35 C 0.3087(5) -0.1279(5) -0.0764(4) 0.111(5) Uani 1 1 d G U . . .
H35 H 0.3041 -0.1606 -0.1112 0.133 Uiso 1 1 calc R U . . .
C36 C 0.3633(5) -0.0787(6) -0.0431(5) 0.118(5) Uani 1 1 d G U . . .
H36 H 0.3953 -0.0784 -0.0557 0.141 Uiso 1 1 calc R U . . .
C37 C 0.3703(3) -0.0298(5) 0.0089(4) 0.085(4) Uani 1 1 d G U . . .
H37 H 0.4068 0.0031 0.0311 0.102 Uiso 1 1 calc R U . . .
Cu1 Cu 0.40769(5) 0.10452(7) 0.21652(6) 0.0492(4) Uani 1 1 d . . . . .
N1 N 0.4749(3) 0.0243(5) 0.2586(4) 0.047(2) Uani 1 1 d . . . . .
N2 N 0.4665(4) 0.1968(5) 0.2284(4) 0.047(2) Uani 1 1 d . . . . .
O1 O 0.2134(3) 0.2066(5) 0.0913(4) 0.078(3) Uani 1 1 d . U . . .
O2 O 0.3323(3) 0.1723(4) 0.1777(3) 0.0582(19) Uani 1 1 d . U . . .
O3 O 0.2648(3) -0.0009(5) 0.2687(4) 0.080(3) Uani 1 1 d . U . . .
O4 O 0.3510(3) 0.0377(4) 0.2374(3) 0.0535(18) Uani 1 1 d . U . . .
O5 O 0.1954(4) -0.0485(6) 0.1298(4) 0.089(3) Uani 1 1 d . U . . .
O6 O 0.1499(4) 0.0507(6) 0.0603(4) 0.085(3) Uani 1 1 d . U . . .
O7 O 0.1614(4) 0.1192(6) 0.1836(4) 0.094(3) Uani 1 1 d . U . . .
O8 O 0.2543(4) 0.1846(6) 0.2395(4) 0.083(3) Uani 1 1 d . U . . .
O9 O 0.2818(3) 0.0312(5) 0.0915(3) 0.067(2) Uani 1 1 d . U . . .
O10 O 0.3849(3) 0.0563(5) 0.1193(3) 0.060(2) Uani 1 1 d . U . . .
Y1 Y 0.24608(5) 0.08266(8) 0.16136(5) 0.0639(4) Uani 1 1 d . . . . .
O11 O 0.4854(13) 0.1663(15) 0.3939(13) 0.359(14) Uani 1 1 d D U . . .
O12 O 0.3867(12) 0.2864(14) 0.3268(11) 0.320(12) 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
C1 O1 1.443(13) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.351(11) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.462(13) . ?
C7 O2 1.315(9) . ?
C8 N2 1.295(13) . ?
C8 H8 0.9300 . ?
C9 O3 1.448(13) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.354(9) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C16 1.416(12) . ?
C15 O4 1.301(8) . ?
C16 N1 1.290(12) . ?
C16 H16 0.9300 . ?
C17 O6 1.251(15) . ?
C17 O5 1.266(16) . ?
C17 C18 1.498(16) . ?
C17 Y1 2.761(15) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O8 1.258(14) . ?
C24 O7 1.265(15) . ?
C24 C25 1.530(13) . ?
C24 Y1 2.742(12) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O10 1.231(11) . ?
C31 O9 1.272(11) . ?
C31 C32 1.504(12) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
Cu1 O2 1.909(7) . ?
Cu1 N1 1.924(8) . ?
Cu1 O4 1.971(7) . ?
Cu1 N2 1.993(8) . ?
Cu1 O10 2.180(7) . ?
Cu1 Y1 3.378(2) . ?
N1 N1 1.420(15) 2_655 ?
N2 N2 1.387(14) 2_655 ?
O1 Y1 2.493(9) . ?
O2 Y1 2.391(7) . ?
O3 Y1 2.678(8) . ?
O4 Y1 2.330(6) . ?
O5 Y1 2.419(10) . ?
O6 Y1 2.366(7) . ?
O7 Y1 2.369(8) . ?
O8 Y1 2.410(8) . ?
O9 Y1 2.318(7) . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 125.2(6) . . ?
O1 C2 C7 114.8(6) . . ?
C3 C2 C7 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C8 122.6(7) . . ?
C5 C6 C8 117.4(7) . . ?
O2 C7 C6 122.4(6) . . ?
O2 C7 C2 117.5(6) . . ?
C6 C7 C2 120.0 . . ?
N2 C8 C6 127.6(10) . . ?
N2 C8 H8 116.2 . . ?
C6 C8 H8 116.2 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 124.2(6) . . ?
O3 C10 C15 115.7(6) . . ?
C11 C10 C15 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C16 117.6(7) . . ?
C15 C14 C16 122.3(7) . . ?
O4 C15 C14 124.0(6) . . ?
O4 C15 C10 116.0(6) . . ?
C14 C15 C10 120.0 . . ?
N1 C16 C14 124.0(10) . . ?
N1 C16 H16 118.0 . . ?
C14 C16 H16 118.0 . . ?
O6 C17 O5 119.6(14) . . ?
O6 C17 C18 119.3(13) . . ?
O5 C17 C18 121.2(14) . . ?
O6 C17 Y1 58.7(7) . . ?
O5 C17 Y1 61.2(8) . . ?
C18 C17 Y1 174.4(9) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 120.2(10) . . ?
C23 C18 C17 119.8(10) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O8 C24 O7 121.1(11) . . ?
O8 C24 C25 117.3(12) . . ?
O7 C24 C25 121.6(11) . . ?
O8 C24 Y1 61.5(6) . . ?
O7 C24 Y1 59.6(6) . . ?
C25 C24 Y1 178.7(9) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 117.5(9) . . ?
C30 C25 C24 122.4(9) . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 120.0 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O10 C31 O9 125.0(10) . . ?
O10 C31 C32 119.6(9) . . ?
O9 C31 C32 115.4(9) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 121.6(7) . . ?
C37 C32 C31 118.4(7) . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.0 . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O2 Cu1 N1 170.5(3) . . ?
O2 Cu1 O4 82.1(3) . . ?
N1 Cu1 O4 88.4(3) . . ?
O2 Cu1 N2 91.7(3) . . ?
N1 Cu1 N2 97.2(3) . . ?
O4 Cu1 N2 155.4(3) . . ?
O2 Cu1 O10 92.2(3) . . ?
N1 Cu1 O10 89.1(3) . . ?
O4 Cu1 O10 101.1(3) . . ?
N2 Cu1 O10 103.0(3) . . ?
O2 Cu1 Y1 43.6(2) . . ?
N1 Cu1 Y1 127.2(2) . . ?
O4 Cu1 Y1 42.18(19) . . ?
N2 Cu1 Y1 135.2(2) . . ?
O10 Cu1 Y1 85.23(19) . . ?
C16 N1 N1 115.2(8) . 2_655 ?
C16 N1 Cu1 128.2(7) . . ?
N1 N1 Cu1 116.7(5) 2_655 . ?
C8 N2 N2 114.8(7) . 2_655 ?
C8 N2 Cu1 120.8(7) . . ?
N2 N2 Cu1 124.3(4) 2_655 . ?
C2 O1 C1 116.2(10) . . ?
C2 O1 Y1 119.9(5) . . ?
C1 O1 Y1 123.8(9) . . ?
C7 O2 Cu1 125.2(5) . . ?
C7 O2 Y1 123.5(5) . . ?
Cu1 O2 Y1 103.0(3) . . ?
C10 O3 C9 116.6(9) . . ?
C10 O3 Y1 115.8(5) . . ?
C9 O3 Y1 126.9(7) . . ?
C15 O4 Cu1 125.4(5) . . ?
C15 O4 Y1 130.9(5) . . ?
Cu1 O4 Y1 103.2(3) . . ?
C17 O5 Y1 91.6(9) . . ?
C17 O6 Y1 94.5(9) . . ?
C24 O7 Y1 92.9(7) . . ?
C24 O8 Y1 91.2(8) . . ?
C31 O9 Y1 143.7(7) . . ?
C31 O10 Cu1 119.5(6) . . ?
O9 Y1 O4 77.9(2) . . ?
O9 Y1 O6 74.5(3) . . ?
O4 Y1 O6 143.8(3) . . ?
O9 Y1 O7 151.5(3) . . ?
O4 Y1 O7 127.6(3) . . ?
O6 Y1 O7 76.9(3) . . ?
O9 Y1 O2 76.6(3) . . ?
O4 Y1 O2 65.3(2) . . ?
O6 Y1 O2 128.2(3) . . ?
O7 Y1 O2 123.0(3) . . ?
O9 Y1 O8 148.9(3) . . ?
O4 Y1 O8 90.1(3) . . ?
O6 Y1 O8 125.2(3) . . ?
O7 Y1 O8 54.7(3) . . ?
O2 Y1 O8 72.3(3) . . ?
O9 Y1 O5 75.6(3) . . ?
O4 Y1 O5 96.7(3) . . ?
O6 Y1 O5 54.1(3) . . ?
O7 Y1 O5 87.4(3) . . ?
O2 Y1 O5 149.6(3) . . ?
O8 Y1 O5 134.8(3) . . ?
O9 Y1 O1 87.6(3) . . ?
O4 Y1 O1 128.6(3) . . ?
O6 Y1 O1 73.3(3) . . ?
O7 Y1 O1 84.6(3) . . ?
O2 Y1 O1 63.3(2) . . ?
O8 Y1 O1 77.6(3) . . ?
O5 Y1 O1 127.1(3) . . ?
O9 Y1 O3 120.0(3) . . ?
O4 Y1 O3 60.8(2) . . ?
O6 Y1 O3 115.5(3) . . ?
O7 Y1 O3 72.8(3) . . ?
O2 Y1 O3 116.1(2) . . ?
O8 Y1 O3 76.1(3) . . ?
O5 Y1 O3 68.9(3) . . ?
O1 Y1 O3 152.1(3) . . ?
O9 Y1 C24 167.9(3) . . ?
O4 Y1 C24 109.8(3) . . ?
O6 Y1 C24 101.6(4) . . ?
O7 Y1 C24 27.4(3) . . ?
O2 Y1 C24 97.9(4) . . ?
O8 Y1 C24 27.3(3) . . ?
O5 Y1 C24 111.7(4) . . ?
O1 Y1 C24 80.4(3) . . ?
O3 Y1 C24 72.0(3) . . ?
O9 Y1 C17 71.7(3) . . ?
O4 Y1 C17 120.7(4) . . ?
O6 Y1 C17 26.8(3) . . ?
O7 Y1 C17 82.7(4) . . ?
O2 Y1 C17 144.7(3) . . ?
O8 Y1 C17 137.4(3) . . ?
O5 Y1 C17 27.3(4) . . ?
O1 Y1 C17 99.9(4) . . ?
O3 Y1 C17 93.2(4) . . ?
C24 Y1 C17 110.1(4) . . ?
O9 Y1 Cu1 64.69(18) . . ?
O4 Y1 Cu1 34.62(17) . . ?
O6 Y1 Cu1 138.0(2) . . ?
O7 Y1 Cu1 143.3(2) . . ?
O2 Y1 Cu1 33.42(16) . . ?
O8 Y1 Cu1 89.15(19) . . ?
O5 Y1 Cu1 120.3(2) . . ?
O1 Y1 Cu1 94.74(18) . . ?
O3 Y1 Cu1 94.02(15) . . ?
C24 Y1 Cu1 116.2(3) . . ?
C17 Y1 Cu1 133.1(3) . . ?

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
O1 C2 C3 C4 -178.8(8) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C8 179.8(8) . . . . ?
C5 C6 C7 O2 -177.1(8) . . . . ?
C8 C6 C7 O2 3.1(10) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C8 C6 C7 C2 -179.8(9) . . . . ?
O1 C2 C7 O2 -3.8(8) . . . . ?
C3 C2 C7 O2 177.2(7) . . . . ?
O1 C2 C7 C6 178.9(8) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C7 C6 C8 N2 7.8(15) . . . . ?
C5 C6 C8 N2 -172.1(9) . . . . ?
O3 C10 C11 C12 175.8(10) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C16 -175.2(9) . . . . ?
C13 C14 C15 O4 178.7(9) . . . . ?
C16 C14 C15 O4 -6.3(11) . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C16 C14 C15 C10 175.0(10) . . . . ?
O3 C10 C15 O4 5.0(9) . . . . ?
C11 C10 C15 O4 -178.8(8) . . . . ?
O3 C10 C15 C14 -176.1(9) . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C13 C14 C16 N1 -169.1(9) . . . . ?
C15 C14 C16 N1 15.8(15) . . . . ?
O6 C17 C18 C19 158.8(10) . . . . ?
O5 C17 C18 C19 -21.2(16) . . . . ?
O6 C17 C18 C23 -22.4(15) . . . . ?
O5 C17 C18 C23 157.6(10) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 178.8(10) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C17 C18 C23 C22 -178.8(10) . . . . ?
O8 C24 C25 C26 -162.7(9) . . . . ?
O7 C24 C25 C26 18.2(15) . . . . ?
O8 C24 C25 C30 13.2(14) . . . . ?
O7 C24 C25 C30 -165.9(10) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 176.0(8) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 -175.8(9) . . . . ?
O10 C31 C32 C33 167.6(8) . . . . ?
O9 C31 C32 C33 -10.3(12) . . . . ?
O10 C31 C32 C37 -13.1(12) . . . . ?
O9 C31 C32 C37 169.0(8) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C34 179.3(8) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C31 C32 C37 C36 -179.3(8) . . . . ?
C14 C16 N1 N1 -176.9(10) . . . 2_655 ?
C14 C16 N1 Cu1 3.7(16) . . . . ?
C6 C8 N2 N2 -176.1(10) . . . 2_655 ?
C6 C8 N2 Cu1 8.0(15) . . . . ?
C3 C2 O1 C1 -2.6(12) . . . . ?
C7 C2 O1 C1 178.5(8) . . . . ?
C3 C2 O1 Y1 175.1(4) . . . . ?
C7 C2 O1 Y1 -3.8(8) . . . . ?
C6 C7 O2 Cu1 -29.7(9) . . . . ?
C2 C7 O2 Cu1 153.2(5) . . . . ?
C6 C7 O2 Y1 -172.4(4) . . . . ?
C2 C7 O2 Y1 10.4(8) . . . . ?
C11 C10 O3 C9 -3.0(13) . . . . ?
C15 C10 O3 C9 172.9(9) . . . . ?
C11 C10 O3 Y1 -174.1(5) . . . . ?
C15 C10 O3 Y1 1.8(9) . . . . ?
C14 C15 O4 Cu1 -20.9(10) . . . . ?
C10 C15 O4 Cu1 157.9(5) . . . . ?
C14 C15 O4 Y1 169.2(5) . . . . ?
C10 C15 O4 Y1 -12.1(10) . . . . ?
O6 C17 O5 Y1 -5.9(13) . . . . ?
C18 C17 O5 Y1 174.1(10) . . . . ?
O5 C17 O6 Y1 6.1(13) . . . . ?
C18 C17 O6 Y1 -173.9(10) . . . . ?
O8 C24 O7 Y1 1.5(13) . . . . ?
C25 C24 O7 Y1 -179.4(10) . . . . ?
O7 C24 O8 Y1 -1.5(13) . . . . ?
C25 C24 O8 Y1 179.4(9) . . . . ?
O10 C31 O9 Y1 -6(2) . . . . ?
C32 C31 O9 Y1 171.4(8) . . . . ?
O9 C31 O10 Cu1 16.1(14) . . . . ?
C32 C31 O10 Cu1 -161.7(6) . . . . ?

_refine_diff_density_max         1.030
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.132

####################################################################### 
# 
# 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_Y2Ni2
_audit_block_doi                 10.5517/cc14htm2
_database_code_depnum_ccdc_archive 'CCDC 1057894'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H74 N4 Ni2 O24 Y2'
_chemical_formula_sum            'C78 H74 N4 Ni2 O24 Y2'
_chemical_formula_weight         1746.65

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'
Ni Ni 0.3393 1.1124 '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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.185(3)
_cell_length_b                   17.062(2)
_cell_length_c                   22.656(4)
_cell_angle_alpha                90
_cell_angle_beta                 121.363(2)
_cell_angle_gamma                90
_cell_volume                     7983(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4541
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      23.36

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_F_000             3584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    1.981
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24613
_diffrn_reflns_av_unetI/netI     0.1151
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.548
_diffrn_reflns_theta_max         26.141
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7945
_reflns_number_gt                4193
_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.
 
 The command 'isor' was also used to restrain the N3 atom with NPD and ADP
 problems. The restraint command lead to restraint number 159, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The DFIX command has been used to refine the H1a-H3 H9a-H11 H11a-H12a distance to
 be in the reasonable range.
 
 The omit command has been used to omit most disagreeable reflections.
 
 In the final refinement, the compounds show large solvent accessible void 
 and the sovlents cannot be determined.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.1068P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7945
_refine_ls_number_parameters     442
_refine_ls_number_restraints     159
_refine_ls_R_factor_all          0.1408
_refine_ls_R_factor_gt           0.0625
_refine_ls_wR_factor_ref         0.2025
_refine_ls_wR_factor_gt          0.1647
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.994
_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
C1 C 0.3507(4) 0.2738(5) 0.4470(5) 0.093(3) Uani 1 1 d . U . . .
H1A H 0.3609 0.2692 0.4939 0.140 Uiso 1 1 calc DR U . . .
H1B H 0.3782 0.3125 0.4445 0.140 Uiso 1 1 calc R U . . .
H1C H 0.3574 0.2241 0.4318 0.140 Uiso 1 1 calc R U . . .
C2 C 0.24006(17) 0.2487(3) 0.4029(2) 0.0512(18) Uani 1 1 d G U . . .
C3 C 0.25376(18) 0.1836(3) 0.4452(2) 0.069(2) Uani 1 1 d G U . . .
H3 H 0.2965 0.1688 0.4755 0.083 Uiso 1 1 calc DR U . . .
C4 C 0.2036(2) 0.1405(2) 0.4422(2) 0.082(3) Uani 1 1 d G U . . .
H4 H 0.2127 0.0969 0.4705 0.099 Uiso 1 1 calc R U . . .
C5 C 0.1397(2) 0.1625(3) 0.3968(3) 0.073(2) Uani 1 1 d G U . . .
H5 H 0.1061 0.1337 0.3948 0.088 Uiso 1 1 calc R U . . .
C6 C 0.12597(16) 0.2277(2) 0.3546(2) 0.0489(17) Uani 1 1 d G U . . .
C7 C 0.1762(2) 0.2708(2) 0.3576(2) 0.0432(16) Uani 1 1 d G U . . .
C8 C 0.0578(3) 0.2454(4) 0.3094(3) 0.0474(16) Uani 1 1 d . . . . .
H8 H 0.0285 0.2082 0.3067 0.057 Uiso 1 1 calc R U . . .
C9 C 0.2749(4) 0.5202(6) 0.2068(5) 0.093(3) Uani 1 1 d . U . . .
H9A H 0.2582 0.5112 0.1586 0.139 Uiso 1 1 calc DR U . . .
H9B H 0.3129 0.4887 0.2339 0.139 Uiso 1 1 calc R U . . .
H9C H 0.2859 0.5746 0.2173 0.139 Uiso 1 1 calc R U . . .
C10 C 0.16709(18) 0.5337(3) 0.1860(2) 0.0546(18) Uani 1 1 d G . . . .
C11 C 0.1464(2) 0.5806(3) 0.1281(3) 0.087(3) Uani 1 1 d G U . . .
H11 H 0.1736 0.5894 0.1111 0.104 Uiso 1 1 calc DR U . . .
C12 C 0.0852(3) 0.6144(3) 0.0955(2) 0.101(3) Uani 1 1 d G U . . .
H12 H 0.0714 0.6459 0.0568 0.121 Uiso 1 1 calc R U . . .
C13 C 0.0447(2) 0.6013(3) 0.1209(3) 0.085(3) Uani 1 1 d G U . . .
H13 H 0.0037 0.6239 0.0992 0.102 Uiso 1 1 calc R U . . .
C14 C 0.06530(19) 0.5543(3) 0.1789(2) 0.0498(17) Uani 1 1 d G . . . .
C15 C 0.1265(2) 0.5205(2) 0.21140(19) 0.0447(16) Uani 1 1 d G . . . .
C16 C 0.0207(3) 0.5437(3) 0.2019(4) 0.0490(17) Uani 1 1 d . . . . .
H16 H -0.0123 0.5803 0.1881 0.059 Uiso 1 1 calc R U . . .
C17 C 0.1698(3) 0.4709(4) 0.4123(3) 0.0396(15) Uani 1 1 d . . . . .
C18 C 0.1754(2) 0.5261(2) 0.4663(2) 0.0424(15) Uani 1 1 d G . . . .
C19 C 0.12527(19) 0.5323(3) 0.4791(2) 0.061(2) Uani 1 1 d G . . . .
H19 H 0.0888 0.5008 0.4552 0.074 Uiso 1 1 calc R U . . .
C20 C 0.1297(2) 0.5857(3) 0.5277(3) 0.084(3) Uani 1 1 d G . . . .
H20 H 0.0962 0.5899 0.5363 0.101 Uiso 1 1 calc R U . . .
C21 C 0.1843(3) 0.6329(3) 0.5635(2) 0.083(3) Uani 1 1 d G . . . .
H21 H 0.1872 0.6686 0.5960 0.099 Uiso 1 1 calc R U . . .
C22 C 0.2344(2) 0.6266(3) 0.5507(2) 0.080(3) Uani 1 1 d G . . . .
H22 H 0.2709 0.6581 0.5747 0.096 Uiso 1 1 calc R U . . .
C23 C 0.22997(19) 0.5732(3) 0.5021(2) 0.060(2) Uani 1 1 d G . . . .
H23 H 0.2635 0.5690 0.4935 0.073 Uiso 1 1 calc R U . . .
C24 C 0.3453(3) 0.5175(5) 0.4254(4) 0.0523(18) Uani 1 1 d . U . . .
C25 C 0.3955(2) 0.5702(3) 0.4783(2) 0.063(2) Uani 1 1 d G U . . .
C26 C 0.3834(2) 0.6502(3) 0.4758(3) 0.089(3) Uani 1 1 d G U . . .
H26 H 0.3438 0.6703 0.4415 0.107 Uiso 1 1 calc R U . . .
C27 C 0.4304(3) 0.7000(3) 0.5247(3) 0.110(3) Uani 1 1 d G U . . .
H27 H 0.4223 0.7535 0.5231 0.132 Uiso 1 1 calc R U . . .
C28 C 0.4896(3) 0.6698(4) 0.5761(3) 0.110(3) Uani 1 1 d G U . . .
H28 H 0.5211 0.7032 0.6088 0.132 Uiso 1 1 calc R U . . .
C29 C 0.5017(2) 0.5899(4) 0.5786(3) 0.104(3) Uani 1 1 d G U . . .
H29 H 0.5413 0.5698 0.6130 0.125 Uiso 1 1 calc R U . . .
C30 C 0.4546(3) 0.5401(3) 0.5297(3) 0.097(3) Uani 1 1 d G U . . .
H30 H 0.4627 0.4866 0.5314 0.116 Uiso 1 1 calc R U . . .
C31 C 0.2999(4) 0.3300(5) 0.2679(4) 0.0573(19) Uani 1 1 d . . . . .
C32 C 0.3254(2) 0.2818(3) 0.2326(2) 0.060(2) Uani 1 1 d G . . . .
C33 C 0.2946(2) 0.2137(3) 0.1971(3) 0.063(2) Uani 1 1 d G . . . .
H33 H 0.2585 0.1954 0.1974 0.076 Uiso 1 1 calc R U . . .
C34 C 0.3177(3) 0.1728(3) 0.1611(3) 0.079(2) Uani 1 1 d G U . . .
H34 H 0.2970 0.1272 0.1374 0.095 Uiso 1 1 calc R U . . .
C35 C 0.3716(3) 0.2002(3) 0.1607(3) 0.095(3) Uani 1 1 d G U . . .
H35 H 0.3870 0.1729 0.1366 0.114 Uiso 1 1 calc R U . . .
C36 C 0.4024(2) 0.2684(4) 0.1962(3) 0.095(3) Uani 1 1 d G U . . .
H36 H 0.4385 0.2867 0.1959 0.114 Uiso 1 1 calc R U . . .
C37 C 0.3794(2) 0.3092(3) 0.2321(3) 0.081(3) Uani 1 1 d G U . . .
H37 H 0.4000 0.3548 0.2559 0.097 Uiso 1 1 calc R U . . .
C38 C 0.0062(4) 0.3675(5) 0.1060(3) 0.071(2) Uani 1 1 d . U . . .
H38A H -0.0021 0.3184 0.0821 0.107 Uiso 1 1 calc R U . . .
H38B H 0.0137 0.4073 0.0810 0.107 Uiso 1 1 calc R U . . .
H38C H -0.0306 0.3817 0.1091 0.107 Uiso 1 1 calc R U . . .
C39 C 0.1154(6) 0.1785(6) 0.1784(6) 0.120(4) Uani 1 1 d . . . . .
H39A H 0.1484 0.1414 0.1862 0.179 Uiso 1 1 calc R U . . .
H39B H 0.0743 0.1605 0.1410 0.179 Uiso 1 1 calc R U . . .
H39C H 0.1135 0.1834 0.2195 0.179 Uiso 1 1 calc R U . . .
N1 N 0.0342(2) 0.3073(3) 0.2729(2) 0.0377(12) Uani 1 1 d . . . . .
N2 N 0.0234(2) 0.4871(3) 0.2402(3) 0.0376(12) Uani 1 1 d . . . . .
Ni1 Ni 0.08867(3) 0.39910(4) 0.27484(4) 0.0355(2) Uani 1 1 d . . . . .
O1 O 0.2853(2) 0.2964(3) 0.4042(2) 0.0583(13) Uani 1 1 d . . . . .
O2 O 0.16682(19) 0.3301(2) 0.3160(2) 0.0432(11) Uani 1 1 d . . . . .
O3 O 0.2266(2) 0.4992(3) 0.2230(2) 0.0595(13) Uani 1 1 d . . . . .
O4 O 0.14940(19) 0.4730(2) 0.2658(2) 0.0434(10) Uani 1 1 d . . . . .
O5 O 0.2200(2) 0.4598(3) 0.4106(2) 0.0469(11) Uani 1 1 d . . . . .
O6 O 0.1155(2) 0.4402(2) 0.3724(2) 0.0438(10) Uani 1 1 d . . . . .
O7 O 0.3483(2) 0.4446(3) 0.4391(2) 0.0617(14) Uani 1 1 d . . . . .
O8 O 0.3010(2) 0.5441(3) 0.3686(2) 0.0609(13) Uani 1 1 d . . . . .
O9 O 0.2427(2) 0.3176(3) 0.2536(2) 0.0642(14) Uani 1 1 d . U . . .
O10 O 0.3337(2) 0.3820(3) 0.3114(3) 0.0718(15) Uani 1 1 d . U . . .
O11 O 0.0615(2) 0.3603(3) 0.1733(2) 0.0562(12) Uani 1 1 d . . . . .
H11A H 0.0820 0.3211 0.1752 0.084 Uiso 1 1 calc DR U . . .
O12 O 0.1299(3) 0.2515(4) 0.1614(3) 0.0888(18) Uani 1 1 d . U . . .
H12A H 0.1682 0.2618 0.1883 0.133 Uiso 1 1 calc DR U . . .
Y1 Y 0.24973(3) 0.41803(4) 0.33396(3) 0.0459(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
C1 O1 1.412(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.351(6) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.449(7) . ?
C7 O2 1.320(5) . ?
C8 N1 1.278(7) . ?
C8 H8 0.9300 . ?
C9 O3 1.439(8) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.365(6) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C16 1.434(7) . ?
C15 O4 1.331(5) . ?
C16 N2 1.277(7) . ?
C16 H16 0.9300 . ?
C17 O5 1.248(7) . ?
C17 O6 1.257(7) . ?
C17 C18 1.492(7) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 O8 1.255(8) . ?
C24 O7 1.276(8) . ?
C24 C25 1.484(8) . ?
C24 Y1 2.745(7) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O10 1.261(9) . ?
C31 O9 1.263(8) . ?
C31 C32 1.487(8) . ?
C31 Y1 2.804(7) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 O11 1.417(7) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 O12 1.402(10) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
N1 N1 1.423(9) 2 ?
N1 Ni1 2.032(5) . ?
N2 N2 1.416(9) 2 ?
N2 Ni1 2.017(5) . ?
Ni1 O2 1.998(4) . ?
Ni1 O4 2.026(4) . ?
Ni1 O6 2.075(4) . ?
Ni1 O11 2.142(4) . ?
Ni1 Y1 3.4118(10) . ?
O1 Y1 2.481(5) . ?
O2 Y1 2.364(4) . ?
O3 Y1 2.663(5) . ?
O4 Y1 2.292(4) . ?
O5 Y1 2.311(4) . ?
O7 Y1 2.376(4) . ?
O8 Y1 2.401(5) . ?
O9 Y1 2.442(5) . ?
O10 Y1 2.418(5) . ?
O11 H11A 0.8200 . ?
O12 H12A 0.8200 . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.5(4) . . ?
O1 C2 C7 115.4(4) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C8 115.4(4) . . ?
C7 C6 C8 124.6(4) . . ?
O2 C7 C6 123.3(3) . . ?
O2 C7 C2 116.5(3) . . ?
C6 C7 C2 120.0 . . ?
N1 C8 C6 126.2(6) . . ?
N1 C8 H8 116.9 . . ?
C6 C8 H8 116.9 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 124.9(4) . . ?
O3 C10 C15 115.0(4) . . ?
C11 C10 C15 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C16 116.6(4) . . ?
C15 C14 C16 123.4(4) . . ?
O4 C15 C14 124.0(3) . . ?
O4 C15 C10 116.0(3) . . ?
C14 C15 C10 120.0 . . ?
N2 C16 C14 124.1(5) . . ?
N2 C16 H16 118.0 . . ?
C14 C16 H16 118.0 . . ?
O5 C17 O6 125.7(6) . . ?
O5 C17 C18 116.5(5) . . ?
O6 C17 C18 117.8(5) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 120.2(4) . . ?
C23 C18 C17 119.7(4) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O8 C24 O7 120.7(7) . . ?
O8 C24 C25 120.9(7) . . ?
O7 C24 C25 118.4(6) . . ?
O8 C24 Y1 61.0(4) . . ?
O7 C24 Y1 59.9(4) . . ?
C25 C24 Y1 175.9(5) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 119.7(5) . . ?
C30 C25 C24 120.3(5) . . ?
C25 C26 C27 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O10 C31 O9 119.8(6) . . ?
O10 C31 C32 121.9(7) . . ?
O9 C31 C32 118.3(7) . . ?
O10 C31 Y1 59.3(4) . . ?
O9 C31 Y1 60.5(3) . . ?
C32 C31 Y1 178.7(5) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 121.7(5) . . ?
C37 C32 C31 118.2(5) . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.0 . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O11 C38 H38A 109.5 . . ?
O11 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O11 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O12 C39 H39A 109.5 . . ?
O12 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O12 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C8 N1 N1 115.5(4) . 2 ?
C8 N1 Ni1 123.8(4) . . ?
N1 N1 Ni1 120.7(2) 2 . ?
C16 N2 N2 116.5(4) . 2 ?
C16 N2 Ni1 125.5(4) . . ?
N2 N2 Ni1 118.0(3) 2 . ?
O2 Ni1 N2 168.01(18) . . ?
O2 Ni1 O4 81.62(17) . . ?
N2 Ni1 O4 87.66(18) . . ?
O2 Ni1 N1 90.06(17) . . ?
N2 Ni1 N1 101.42(19) . . ?
O4 Ni1 N1 166.77(18) . . ?
O2 Ni1 O6 90.34(16) . . ?
N2 Ni1 O6 84.87(18) . . ?
O4 Ni1 O6 93.22(17) . . ?
N1 Ni1 O6 97.13(18) . . ?
O2 Ni1 O11 90.38(16) . . ?
N2 Ni1 O11 94.10(18) . . ?
O4 Ni1 O11 85.25(18) . . ?
N1 Ni1 O11 84.52(19) . . ?
O6 Ni1 O11 178.20(18) . . ?
O2 Ni1 Y1 42.54(12) . . ?
N2 Ni1 Y1 125.76(13) . . ?
O4 Ni1 Y1 40.62(11) . . ?
N1 Ni1 Y1 132.55(13) . . ?
O6 Ni1 Y1 83.64(12) . . ?
O11 Ni1 Y1 95.78(13) . . ?
C2 O1 C1 117.1(5) . . ?
C2 O1 Y1 118.9(3) . . ?
C1 O1 Y1 124.0(5) . . ?
C7 O2 Ni1 123.7(3) . . ?
C7 O2 Y1 123.3(3) . . ?
Ni1 O2 Y1 102.60(17) . . ?
C10 O3 C9 118.3(5) . . ?
C10 O3 Y1 116.0(3) . . ?
C9 O3 Y1 124.7(5) . . ?
C15 O4 Ni1 119.9(3) . . ?
C15 O4 Y1 131.1(3) . . ?
Ni1 O4 Y1 104.25(17) . . ?
C17 O5 Y1 139.2(4) . . ?
C17 O6 Ni1 122.5(4) . . ?
C24 O7 Y1 92.4(4) . . ?
C24 O8 Y1 91.8(5) . . ?
C31 O9 Y1 92.8(4) . . ?
C31 O10 Y1 94.0(4) . . ?
C38 O11 Ni1 136.0(4) . . ?
C38 O11 H11A 109.5 . . ?
Ni1 O11 H11A 110.9 . . ?
C39 O12 H12A 109.5 . . ?
O4 Y1 O5 75.30(14) . . ?
O4 Y1 O2 68.77(14) . . ?
O5 Y1 O2 75.92(14) . . ?
O4 Y1 O7 139.05(16) . . ?
O5 Y1 O7 74.34(15) . . ?
O2 Y1 O7 127.70(17) . . ?
O4 Y1 O8 92.24(15) . . ?
O5 Y1 O8 77.73(16) . . ?
O2 Y1 O8 150.65(15) . . ?
O7 Y1 O8 54.83(17) . . ?
O4 Y1 O10 132.29(17) . . ?
O5 Y1 O10 149.46(17) . . ?
O2 Y1 O10 122.25(16) . . ?
O7 Y1 O10 75.25(17) . . ?
O8 Y1 O10 87.10(18) . . ?
O4 Y1 O9 98.42(16) . . ?
O5 Y1 O9 148.10(16) . . ?
O2 Y1 O9 72.74(15) . . ?
O7 Y1 O9 121.68(16) . . ?
O8 Y1 O9 134.15(17) . . ?
O10 Y1 O9 53.41(16) . . ?
O4 Y1 O1 131.81(15) . . ?
O5 Y1 O1 85.14(15) . . ?
O2 Y1 O1 63.85(14) . . ?
O7 Y1 O1 71.61(17) . . ?
O8 Y1 O1 126.30(16) . . ?
O10 Y1 O1 82.76(18) . . ?
O9 Y1 O1 75.96(16) . . ?
O4 Y1 O3 61.47(14) . . ?
O5 Y1 O3 123.72(15) . . ?
O2 Y1 O3 115.18(14) . . ?
O7 Y1 O3 117.09(17) . . ?
O8 Y1 O3 70.25(15) . . ?
O10 Y1 O3 73.69(17) . . ?
O9 Y1 O3 76.22(16) . . ?
O1 Y1 O3 150.82(15) . . ?
O4 Y1 C24 115.86(19) . . ?
O5 Y1 C24 73.24(17) . . ?
O2 Y1 C24 145.92(18) . . ?
O7 Y1 C24 27.68(18) . . ?
O8 Y1 C24 27.18(18) . . ?
O10 Y1 C24 81.14(19) . . ?
O9 Y1 C24 134.52(18) . . ?
O1 Y1 C24 99.1(2) . . ?
O3 Y1 C24 94.08(19) . . ?
O4 Y1 C31 117.37(18) . . ?
O5 Y1 C31 163.11(19) . . ?
O2 Y1 C31 97.6(2) . . ?
O7 Y1 C31 98.65(19) . . ?
O8 Y1 C31 111.2(2) . . ?
O10 Y1 C31 26.67(19) . . ?
O9 Y1 C31 26.74(18) . . ?
O1 Y1 C31 78.03(18) . . ?
O3 Y1 C31 73.18(18) . . ?
C24 Y1 C31 107.8(2) . . ?
O4 Y1 Ni1 35.13(10) . . ?
O5 Y1 Ni1 65.55(10) . . ?
O2 Y1 Ni1 34.85(9) . . ?
O7 Y1 Ni1 139.10(12) . . ?
O8 Y1 Ni1 120.16(12) . . ?
O10 Y1 Ni1 143.74(13) . . ?
O9 Y1 Ni1 91.09(12) . . ?
O1 Y1 Ni1 96.68(11) . . ?
O3 Y1 Ni1 92.46(10) . . ?
C24 Y1 Ni1 134.11(14) . . ?
C31 Y1 Ni1 117.56(17) . . ?

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
O1 C2 C3 C4 176.9(5) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C8 -180.0(4) . . . . ?
C5 C6 C7 O2 175.5(4) . . . . ?
C8 C6 C7 O2 -4.5(5) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C8 C6 C7 C2 180.0(5) . . . . ?
O1 C2 C7 O2 7.0(4) . . . . ?
C3 C2 C7 O2 -175.8(4) . . . . ?
O1 C2 C7 C6 -177.2(4) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C5 C6 C8 N1 170.6(5) . . . . ?
C7 C6 C8 N1 -9.4(8) . . . . ?
O3 C10 C11 C12 -178.3(5) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C16 179.9(5) . . . . ?
C13 C14 C15 O4 -177.9(5) . . . . ?
C16 C14 C15 O4 2.2(6) . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C16 C14 C15 C10 -179.9(5) . . . . ?
O3 C10 C15 O4 -3.5(5) . . . . ?
C11 C10 C15 O4 178.1(4) . . . . ?
O3 C10 C15 C14 178.4(5) . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C13 C14 C16 N2 159.3(5) . . . . ?
C15 C14 C16 N2 -20.8(9) . . . . ?
O5 C17 C18 C19 -169.7(4) . . . . ?
O6 C17 C18 C19 10.7(7) . . . . ?
O5 C17 C18 C23 12.6(6) . . . . ?
O6 C17 C18 C23 -167.1(4) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C17 C18 C19 C20 -177.7(4) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C17 C18 C23 C22 177.7(4) . . . . ?
O8 C24 C25 C26 20.2(8) . . . . ?
O7 C24 C25 C26 -159.5(5) . . . . ?
O8 C24 C25 C30 -158.9(5) . . . . ?
O7 C24 C25 C30 21.4(8) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 -179.2(6) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 179.2(6) . . . . ?
O10 C31 C32 C33 165.2(6) . . . . ?
O9 C31 C32 C33 -14.4(8) . . . . ?
O10 C31 C32 C37 -18.8(8) . . . . ?
O9 C31 C32 C37 161.6(5) . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C34 176.0(5) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
C31 C32 C37 C36 -176.1(5) . . . . ?
C6 C8 N1 N1 173.6(5) . . . 2 ?
C6 C8 N1 Ni1 -3.8(9) . . . . ?
C14 C16 N2 N2 178.1(6) . . . 2 ?
C14 C16 N2 Ni1 -1.6(9) . . . . ?
C3 C2 O1 C1 6.1(7) . . . . ?
C7 C2 O1 C1 -176.9(5) . . . . ?
C3 C2 O1 Y1 -172.9(2) . . . . ?
C7 C2 O1 Y1 4.2(5) . . . . ?
C6 C7 O2 Ni1 29.4(5) . . . . ?
C2 C7 O2 Ni1 -154.9(3) . . . . ?
C6 C7 O2 Y1 168.1(2) . . . . ?
C2 C7 O2 Y1 -16.2(4) . . . . ?
C11 C10 O3 C9 8.2(8) . . . . ?
C15 C10 O3 C9 -170.1(5) . . . . ?
C11 C10 O3 Y1 177.6(2) . . . . ?
C15 C10 O3 Y1 -0.7(5) . . . . ?
C14 C15 O4 Ni1 34.1(5) . . . . ?
C10 C15 O4 Ni1 -143.9(3) . . . . ?
C14 C15 O4 Y1 -174.3(3) . . . . ?
C10 C15 O4 Y1 7.7(5) . . . . ?
O6 C17 O5 Y1 21.7(10) . . . . ?
C18 C17 O5 Y1 -157.9(4) . . . . ?
O5 C17 O6 Ni1 -23.9(8) . . . . ?
C18 C17 O6 Ni1 155.8(3) . . . . ?
O8 C24 O7 Y1 -4.0(7) . . . . ?
C25 C24 O7 Y1 175.7(5) . . . . ?
O7 C24 O8 Y1 3.9(7) . . . . ?
C25 C24 O8 Y1 -175.8(5) . . . . ?
O10 C31 O9 Y1 -0.3(7) . . . . ?
C32 C31 O9 Y1 179.3(5) . . . . ?
O9 C31 O10 Y1 0.3(7) . . . . ?
C32 C31 O10 Y1 -179.3(6) . . . . ?

_refine_diff_density_max         1.074
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.104

####################################################################### 
# 
# 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_Tb2Cu2
_database_code_depnum_ccdc_archive 'CCDC 1063586'
_audit_update_record             
;
2015-05-06 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H62 Cu2 N4 O22 Tb2'
_chemical_formula_sum            'C74 H62 Cu2 N4 O22 Tb2'
_chemical_formula_weight         1804.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.8031(14)
_cell_length_b                   16.5092(10)
_cell_length_c                   23.023(2)
_cell_angle_alpha                90
_cell_angle_beta                 119.9340(10)
_cell_angle_gamma                90
_cell_volume                     7840.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5510
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      24.24

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_F_000             3592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.390
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22251
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.580
_diffrn_reflns_theta_max         25.134
_diffrn_reflns_theta_full        25.134
_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             6987
_reflns_number_gt                4684
_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.
 
 The command 'isor' was also used to restrain the C and O atom with NPD and ADP
 problems. The restraint command lead to restraint number 186, but cannot be
 completely avoided. Refinement of F² against ALL reflections.

 The H-atoms on water cannot be determined.

 In the final refinement, the compounds show large solvent accessible void 
 and the sovlents cannot be determined.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  ?
_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)+(0.1186P)²+13.0167P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6987
_refine_ls_number_parameters     411
_refine_ls_number_restraints     186
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.2005
_refine_ls_wR_factor_gt          0.1719
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.062
_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
C1 C 0.3506(5) 0.7316(7) 0.9585(7) 0.115(5) Uani 1 1 d . U . . .
H1A H 0.3574 0.7879 0.9533 0.173 Uiso 1 1 calc R U . . .
H1B H 0.3804 0.6993 0.9518 0.173 Uiso 1 1 calc R U . . .
H1C H 0.3575 0.7225 1.0028 0.173 Uiso 1 1 calc R U . . .
C2 C 0.2384(2) 0.7605(4) 0.9073(3) 0.062(3) Uani 1 1 d G . . . .
C3 C 0.2499(3) 0.8293(4) 0.9464(3) 0.082(3) Uani 1 1 d G U . . .
H3 H 0.2921 0.8449 0.9767 0.099 Uiso 1 1 calc R U . . .
C4 C 0.1981(4) 0.8749(4) 0.9403(4) 0.098(4) Uani 1 1 d G U . . .
H4 H 0.2057 0.9209 0.9665 0.118 Uiso 1 1 calc R U . . .
C5 C 0.1349(3) 0.8516(4) 0.8951(4) 0.089(3) Uani 1 1 d G U . . .
H5 H 0.1002 0.8821 0.8910 0.107 Uiso 1 1 calc R U . . .
C6 C 0.1234(2) 0.7827(4) 0.8560(3) 0.062(2) Uani 1 1 d G . . . .
C7 C 0.1752(3) 0.7372(3) 0.8621(3) 0.050(2) Uani 1 1 d G . . . .
C8 C 0.0564(5) 0.7625(5) 0.8097(5) 0.062(2) Uani 1 1 d . . . . .
H8 H 0.0257 0.7998 0.8066 0.074 Uiso 1 1 calc R U . . .
C9 C 0.2847(5) 0.4694(8) 0.7216(7) 0.095(4) Uani 1 1 d . U . . .
H9A H 0.2888 0.4116 0.7267 0.142 Uiso 1 1 calc R U . . .
H9B H 0.3245 0.4945 0.7540 0.142 Uiso 1 1 calc R U . . .
H9C H 0.2752 0.4840 0.6773 0.142 Uiso 1 1 calc R U . . .
C10 C 0.1723(2) 0.4687(4) 0.6911(3) 0.066(3) Uani 1 1 d G U . . .
C11 C 0.1539(3) 0.4179(5) 0.6364(4) 0.104(4) Uani 1 1 d G U . . .
H11 H 0.1838 0.4040 0.6231 0.125 Uiso 1 1 calc R U . . .
C12 C 0.0911(4) 0.3878(5) 0.6014(4) 0.130(5) Uani 1 1 d G U . . .
H12 H 0.0788 0.3538 0.5648 0.155 Uiso 1 1 calc R U . . .
C13 C 0.0465(3) 0.4086(5) 0.6212(4) 0.100(4) Uani 1 1 d G U . . .
H13 H 0.0044 0.3885 0.5979 0.120 Uiso 1 1 calc R U . . .
C14 C 0.0648(2) 0.4594(4) 0.6759(3) 0.064(3) Uani 1 1 d G . . . .
C15 C 0.1277(3) 0.4895(4) 0.7109(3) 0.048(2) Uani 1 1 d G U . . .
C16 C 0.0189(4) 0.4717(5) 0.6978(5) 0.056(2) Uani 1 1 d . U . . .
H16 H -0.0179 0.4391 0.6792 0.067 Uiso 1 1 calc R U . . .
C17 C 0.3486(5) 0.4797(7) 0.9296(5) 0.064(3) Uani 1 1 d . U . . .
C18 C 0.3964(3) 0.4240(4) 0.9818(3) 0.063(3) Uani 1 1 d G U . . .
C19 C 0.3827(3) 0.3420(5) 0.9810(4) 0.093(4) Uani 1 1 d G U . . .
H19 H 0.3431 0.3216 0.9481 0.112 Uiso 1 1 calc R U . . .
C20 C 0.4284(5) 0.2906(4) 1.0292(5) 0.118(5) Uani 1 1 d G U . . .
H20 H 0.4193 0.2357 1.0287 0.141 Uiso 1 1 calc R U . . .
C21 C 0.4877(4) 0.3211(5) 1.0783(4) 0.112(4) Uani 1 1 d G U . . .
H21 H 0.5183 0.2867 1.1106 0.134 Uiso 1 1 calc R U . . .
C22 C 0.5014(3) 0.4031(6) 1.0791(4) 0.112(5) Uani 1 1 d G U . . .
H22 H 0.5410 0.4236 1.1120 0.135 Uiso 1 1 calc R U . . .
C23 C 0.4557(4) 0.4546(4) 1.0309(4) 0.092(4) Uani 1 1 d G U . . .
H23 H 0.4648 0.5094 1.0314 0.110 Uiso 1 1 calc R U . . .
C24 C 0.3028(5) 0.6750(7) 0.7732(5) 0.066(3) Uani 1 1 d . . . . .
C25 C 0.3288(3) 0.7216(4) 0.7350(3) 0.063(3) Uani 1 1 d G . . . .
C26 C 0.3843(3) 0.6945(4) 0.7356(4) 0.097(4) Uani 1 1 d G U . . .
H26 H 0.4062 0.6492 0.7607 0.116 Uiso 1 1 calc R U . . .
C27 C 0.4072(3) 0.7352(5) 0.6986(4) 0.104(4) Uani 1 1 d G U . . .
H27 H 0.4444 0.7171 0.6990 0.125 Uiso 1 1 calc R U . . .
C28 C 0.3745(4) 0.8029(5) 0.6611(4) 0.109(4) Uani 1 1 d G U . . .
H28 H 0.3897 0.8302 0.6364 0.131 Uiso 1 1 calc R U . . .
C29 C 0.3189(4) 0.8300(4) 0.6605(4) 0.086(3) Uani 1 1 d G U . . .
H29 H 0.2970 0.8753 0.6354 0.103 Uiso 1 1 calc R U . . .
C30 C 0.2961(3) 0.7893(4) 0.6975(3) 0.065(3) Uani 1 1 d G . . . .
H30 H 0.2589 0.8075 0.6971 0.078 Uiso 1 1 calc R U . . .
C31 C 0.1678(4) 0.5223(5) 0.9163(4) 0.0451(19) Uani 1 1 d . . . . .
C32 C 0.1754(3) 0.4702(4) 0.9734(3) 0.051(2) Uani 1 1 d G . . . .
C33 C 0.2296(3) 0.4210(4) 1.0081(3) 0.064(3) Uani 1 1 d G . . . .
H33 H 0.2618 0.4206 0.9964 0.077 Uiso 1 1 calc R U . . .
C34 C 0.2356(3) 0.3724(4) 1.0602(4) 0.090(3) Uani 1 1 d G U . . .
H34 H 0.2718 0.3395 1.0834 0.108 Uiso 1 1 calc R U . . .
C35 C 0.1874(4) 0.3730(5) 1.0775(3) 0.098(4) Uani 1 1 d G U . . .
H35 H 0.1914 0.3404 1.1124 0.117 Uiso 1 1 calc R U . . .
C36 C 0.1332(3) 0.4222(5) 1.0428(4) 0.103(4) Uani 1 1 d G U . . .
H36 H 0.1010 0.4225 1.0545 0.123 Uiso 1 1 calc R U . . .
C37 C 0.1272(3) 0.4708(4) 0.9907(4) 0.081(3) Uani 1 1 d G . . . .
H37 H 0.0910 0.5037 0.9675 0.097 Uiso 1 1 calc R U . . .
Cu1 Cu 0.09236(4) 0.60455(6) 0.78502(5) 0.0417(3) Uani 1 1 d . . . . .
N1 N 0.0341(3) 0.6998(4) 0.7726(3) 0.0443(15) Uani 1 1 d . . . . .
N2 N 0.0249(3) 0.5246(4) 0.7416(3) 0.0405(15) Uani 1 1 d . . . . .
O1 O 0.2857(3) 0.7096(4) 0.9102(3) 0.0689(18) Uani 1 1 d . U . . .
O2 O 0.1677(2) 0.6724(3) 0.8239(3) 0.0475(13) Uani 1 1 d . . . . .
O3 O 0.2336(3) 0.4960(4) 0.7319(3) 0.0626(17) Uani 1 1 d . . . . .
O4 O 0.1484(2) 0.5388(4) 0.7626(3) 0.0493(14) Uani 1 1 d . . . . .
O5 O 0.2454(3) 0.6882(4) 0.7598(3) 0.0693(18) Uani 1 1 d . U . . .
O6 O 0.3382(3) 0.6219(5) 0.8156(3) 0.074(2) Uani 1 1 d . U . . .
O7 O 0.3499(3) 0.5551(5) 0.9422(3) 0.0712(19) Uani 1 1 d . U . . .
O8 O 0.3065(3) 0.4518(4) 0.8725(3) 0.0669(17) Uani 1 1 d . U . . .
O9 O 0.2173(3) 0.5301(4) 0.9102(3) 0.0559(15) Uani 1 1 d . . . . .
O10 O 0.1148(3) 0.5564(4) 0.8811(3) 0.0572(15) Uani 1 1 d . . . . .
Tb1 Tb 0.25368(2) 0.58325(3) 0.83912(2) 0.0534(2) Uani 1 1 d . . . . .
O11 O 0.0857(11) 0.7582(13) 0.6538(10) 0.285(9) 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
C1 O1 1.427(11) . ?
C2 O1 1.379(8) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C6 C8 1.448(10) . ?
C7 O2 1.338(7) . ?
C8 N1 1.277(10) . ?
C9 O3 1.418(10) . ?
C10 O3 1.360(7) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C14 C16 1.428(9) . ?
C15 O4 1.319(7) . ?
C16 N2 1.288(10) . ?
C17 O7 1.274(12) . ?
C17 O8 1.277(12) . ?
C17 C18 1.490(12) . ?
C17 Tb1 2.769(10) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C24 O5 1.259(11) . ?
C24 O6 1.269(11) . ?
C24 C25 1.514(10) . ?
C24 Tb1 2.781(9) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C31 O10 1.243(10) . ?
C31 O9 1.260(9) . ?
C31 C32 1.504(9) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
Cu1 O2 1.916(5) . ?
Cu1 N2 1.928(6) . ?
Cu1 O4 1.977(5) . ?
Cu1 N1 2.021(7) . ?
Cu1 O10 2.153(6) . ?
Cu1 Tb1 3.4126(10) . ?
N1 N1 1.425(12) 2_556 ?
N2 N2 1.416(11) 2_556 ?
O1 Tb1 2.523(7) . ?
O2 Tb1 2.401(5) . ?
O3 Tb1 2.687(6) . ?
O4 Tb1 2.349(5) . ?
O5 Tb1 2.454(6) . ?
O6 Tb1 2.416(6) . ?
O7 Tb1 2.382(6) . ?
O8 Tb1 2.433(7) . ?
O9 Tb1 2.369(5) . ?

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
O1 C2 C3 125.1(5) . . ?
O1 C2 C7 114.9(5) . . ?
C3 C2 C7 120.0 . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C4 C5 C6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C8 123.1(5) . . ?
C5 C6 C8 116.9(5) . . ?
O2 C7 C6 123.0(4) . . ?
O2 C7 C2 116.9(4) . . ?
C6 C7 C2 120.0 . . ?
N1 C8 C6 128.1(8) . . ?
O3 C10 C11 124.7(5) . . ?
O3 C10 C15 115.0(5) . . ?
C11 C10 C15 120.0 . . ?
C12 C11 C10 120.0 . . ?
C11 C12 C13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C16 117.1(5) . . ?
C15 C14 C16 122.6(5) . . ?
O4 C15 C14 123.5(4) . . ?
O4 C15 C10 116.5(4) . . ?
C14 C15 C10 120.0 . . ?
N2 C16 C14 124.6(7) . . ?
O7 C17 O8 120.3(10) . . ?
O7 C17 C18 119.8(9) . . ?
O8 C17 C18 119.9(9) . . ?
O7 C17 Tb1 59.2(5) . . ?
O8 C17 Tb1 61.5(5) . . ?
C18 C17 Tb1 174.8(6) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 120.7(7) . . ?
C23 C18 C17 119.3(7) . . ?
C18 C19 C20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C20 C21 C22 120.0 . . ?
C21 C22 C23 120.0 . . ?
C22 C23 C18 120.0 . . ?
O5 C24 O6 122.1(8) . . ?
O5 C24 C25 118.5(9) . . ?
O6 C24 C25 119.4(8) . . ?
O5 C24 Tb1 61.9(5) . . ?
O6 C24 Tb1 60.2(4) . . ?
C25 C24 Tb1 177.3(7) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 119.6(6) . . ?
C30 C25 C24 120.3(6) . . ?
C27 C26 C25 120.0 . . ?
C26 C27 C28 120.0 . . ?
C29 C28 C27 120.0 . . ?
C28 C29 C30 120.0 . . ?
C29 C30 C25 120.0 . . ?
O10 C31 O9 125.6(8) . . ?
O10 C31 C32 117.9(7) . . ?
O9 C31 C32 116.4(7) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C31 120.6(5) . . ?
C37 C32 C31 119.4(5) . . ?
C34 C33 C32 120.0 . . ?
C35 C34 C33 120.0 . . ?
C34 C35 C36 120.0 . . ?
C37 C36 C35 120.0 . . ?
C36 C37 C32 120.0 . . ?
O2 Cu1 N2 170.4(2) . . ?
O2 Cu1 O4 81.2(2) . . ?
N2 Cu1 O4 89.1(2) . . ?
O2 Cu1 N1 91.6(2) . . ?
N2 Cu1 N1 97.1(2) . . ?
O4 Cu1 N1 153.5(3) . . ?
O2 Cu1 O10 92.4(2) . . ?
N2 Cu1 O10 89.7(3) . . ?
O4 Cu1 O10 102.2(2) . . ?
N1 Cu1 O10 103.5(3) . . ?
O2 Cu1 Tb1 43.07(16) . . ?
N2 Cu1 Tb1 127.83(17) . . ?
O4 Cu1 Tb1 41.94(16) . . ?
N1 Cu1 Tb1 134.41(18) . . ?
O10 Cu1 Tb1 85.98(15) . . ?
C8 N1 N1 115.5(6) . 2_556 ?
C8 N1 Cu1 120.6(6) . . ?
N1 N1 Cu1 123.7(3) 2_556 . ?
C16 N2 N2 115.6(6) . 2_556 ?
C16 N2 Cu1 127.4(5) . . ?
N2 N2 Cu1 116.9(4) 2_556 . ?
C2 O1 C1 115.0(8) . . ?
C2 O1 Tb1 119.8(4) . . ?
C1 O1 Tb1 125.1(7) . . ?
C7 O2 Cu1 124.2(4) . . ?
C7 O2 Tb1 124.7(4) . . ?
Cu1 O2 Tb1 103.9(2) . . ?
C10 O3 C9 119.7(7) . . ?
C10 O3 Tb1 116.8(4) . . ?
C9 O3 Tb1 123.0(6) . . ?
C15 O4 Cu1 125.4(4) . . ?
C15 O4 Tb1 130.4(4) . . ?
Cu1 O4 Tb1 103.8(2) . . ?
C24 O5 Tb1 91.2(6) . . ?
C24 O6 Tb1 92.7(5) . . ?
C17 O7 Tb1 93.5(6) . . ?
C17 O8 Tb1 91.1(6) . . ?
C31 O9 Tb1 143.0(5) . . ?
C31 O10 Cu1 119.2(5) . . ?
O4 Tb1 O9 77.36(19) . . ?
O4 Tb1 O7 145.3(2) . . ?
O9 Tb1 O7 75.0(2) . . ?
O4 Tb1 O2 64.48(18) . . ?
O9 Tb1 O2 75.47(19) . . ?
O7 Tb1 O2 126.3(2) . . ?
O4 Tb1 O6 127.6(2) . . ?
O9 Tb1 O6 152.3(2) . . ?
O7 Tb1 O6 77.3(2) . . ?
O2 Tb1 O6 123.4(2) . . ?
O4 Tb1 O8 98.5(2) . . ?
O9 Tb1 O8 76.2(2) . . ?
O7 Tb1 O8 54.7(2) . . ?
O2 Tb1 O8 149.5(2) . . ?
O6 Tb1 O8 87.1(2) . . ?
O4 Tb1 O5 90.2(2) . . ?
O9 Tb1 O5 148.7(2) . . ?
O7 Tb1 O5 124.0(2) . . ?
O2 Tb1 O5 73.3(2) . . ?
O6 Tb1 O5 54.0(2) . . ?
O8 Tb1 O5 134.6(2) . . ?
O4 Tb1 O1 127.5(2) . . ?
O9 Tb1 O1 87.4(2) . . ?
O7 Tb1 O1 71.7(2) . . ?
O2 Tb1 O1 63.11(19) . . ?
O6 Tb1 O1 84.9(2) . . ?
O8 Tb1 O1 126.2(2) . . ?
O5 Tb1 O1 77.6(2) . . ?
O4 Tb1 O3 60.63(17) . . ?
O9 Tb1 O3 118.5(2) . . ?
O7 Tb1 O3 116.9(2) . . ?
O2 Tb1 O3 116.53(18) . . ?
O6 Tb1 O3 73.8(2) . . ?
O8 Tb1 O3 68.8(2) . . ?
O5 Tb1 O3 77.5(2) . . ?
O1 Tb1 O3 153.7(2) . . ?
O4 Tb1 C17 122.4(3) . . ?
O9 Tb1 C17 72.2(2) . . ?
O7 Tb1 C17 27.3(3) . . ?
O2 Tb1 C17 143.5(2) . . ?
O6 Tb1 C17 82.8(3) . . ?
O8 Tb1 C17 27.5(3) . . ?
O5 Tb1 C17 136.8(2) . . ?
O1 Tb1 C17 98.8(3) . . ?
O3 Tb1 C17 93.7(3) . . ?
O4 Tb1 C24 110.0(2) . . ?
O9 Tb1 C24 167.6(3) . . ?
O7 Tb1 C24 101.1(3) . . ?
O2 Tb1 C24 98.4(3) . . ?
O6 Tb1 C24 27.1(2) . . ?
O8 Tb1 C24 111.5(3) . . ?
O5 Tb1 C24 26.9(2) . . ?
O1 Tb1 C24 80.2(3) . . ?
O3 Tb1 C24 73.8(3) . . ?
C17 Tb1 C24 109.9(3) . . ?
O4 Tb1 Cu1 34.24(13) . . ?
O9 Tb1 Cu1 63.74(14) . . ?
O7 Tb1 Cu1 137.02(17) . . ?
O2 Tb1 Cu1 33.02(12) . . ?
O6 Tb1 Cu1 143.36(16) . . ?
O8 Tb1 Cu1 121.16(16) . . ?
O5 Tb1 Cu1 89.89(14) . . ?
O1 Tb1 Cu1 94.16(15) . . ?
O3 Tb1 Cu1 93.91(11) . . ?
C17 Tb1 Cu1 133.2(2) . . ?
C24 Tb1 Cu1 116.6(2) . . ?

_refine_diff_density_max         1.516
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.158

