# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_1
_database_code_depnum_ccdc_archive 'CCDC 1408411'
_audit_update_record             
;
2015-08-06 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H24 Gd N7 Ni O15'
_chemical_formula_weight         842.44

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'
Ni Ni 0.3393 1.1124 '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           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   10.3265(19)
_cell_length_b                   17.115(3)
_cell_length_c                   17.194(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.575(3)
_cell_angle_gamma                90
_cell_volume                     3018.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_F_000             1668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    2.884
_shelx_estimated_absorpt_T_min   0.544
_shelx_estimated_absorpt_T_max   0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_T_max  0.595
_exptl_absorpt_process_details   'SADABS; Bruker, 2013'

_exptl_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            23995
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.684
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5918
_reflns_number_gt                5323
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0418P)²+0.1325P]
 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
_refine_ls_extinction_coef       0.0171(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5918
_refine_ls_number_parameters     420
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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
Gd1 Gd 0.57986(2) 0.75873(2) 0.12950(2) 0.03375(8) Uani 1 1 d . . . . .
Ni1 Ni 0.49093(3) 0.91243(2) 0.24478(2) 0.02746(10) Uani 1 1 d . . . . .
C1 C 0.2945(2) 0.85161(16) 0.11686(15) 0.0322(6) Uani 1 1 d . . . . .
C2 C 0.2499(3) 0.79101(19) 0.06438(17) 0.0396(7) Uani 1 1 d . . . . .
C3 C 0.1244(3) 0.7898(2) 0.0288(2) 0.0597(10) Uani 1 1 d . . . . .
H3 H 0.0970 0.7490 -0.0049 0.072 Uiso 1 1 calc R U . . .
C4 C 0.0384(3) 0.8485(3) 0.0422(2) 0.0726(12) Uani 1 1 d . . . . .
H4 H -0.0469 0.8471 0.0180 0.087 Uiso 1 1 calc R U . . .
C5 C 0.0783(3) 0.9084(2) 0.0908(2) 0.0606(10) Uani 1 1 d . . . . .
H5 H 0.0202 0.9483 0.0990 0.073 Uiso 1 1 calc R U . . .
C6 C 0.2061(3) 0.91115(19) 0.12909(17) 0.0389(7) Uani 1 1 d . . . . .
C7 C 0.3164(3) 1.05852(19) 0.34360(19) 0.0446(7) Uani 1 1 d . . . . .
H7A H 0.2254 1.0446 0.3438 0.054 Uiso 1 1 calc R U . . .
H7B H 0.3277 1.1108 0.3651 0.054 Uiso 1 1 calc R U . . .
C8 C 0.3972(3) 1.00349(18) 0.39621(18) 0.0407(7) Uani 1 1 d . . . . .
H8A H 0.3763 1.0102 0.4494 0.049 Uiso 1 1 calc R U . . .
H8B H 0.3755 0.9502 0.3804 0.049 Uiso 1 1 calc R U . . .
C9 C 0.7127(3) 0.96255(17) 0.35715(16) 0.0362(6) Uani 1 1 d . . . . .
H9 H 0.7492 0.9952 0.3970 0.043 Uiso 1 1 calc R U . . .
C10 C 0.8016(3) 0.91645(17) 0.31763(16) 0.0346(6) Uani 1 1 d . . . . .
C11 C 0.9350(3) 0.9307(2) 0.3398(2) 0.0455(8) Uani 1 1 d . . . . .
H11 H 0.9594 0.9701 0.3757 0.055 Uiso 1 1 calc R U . . .
C12 C 1.0289(3) 0.8880(2) 0.3100(2) 0.0538(9) Uani 1 1 d . . . . .
H12 H 1.1165 0.8990 0.3249 0.065 Uiso 1 1 calc R U . . .
C13 C 0.9936(3) 0.8281(2) 0.2574(2) 0.0485(8) Uani 1 1 d . . . . .
H13 H 1.0574 0.7987 0.2369 0.058 Uiso 1 1 calc R U . . .
C14 C 0.8642(3) 0.81270(17) 0.23571(17) 0.0370(6) Uani 1 1 d . . . . .
C15 C 0.7647(2) 0.85627(15) 0.26373(16) 0.0310(6) Uani 1 1 d . . . . .
C16 C 0.3168(4) 0.6849(3) -0.0122(2) 0.0784(13) Uani 1 1 d . . . . .
H16A H 0.2413 0.6539 -0.0057 0.118 Uiso 1 1 calc R U . . .
H16B H 0.3901 0.6512 -0.0159 0.118 Uiso 1 1 calc R U . . .
H16C H 0.3006 0.7154 -0.0591 0.118 Uiso 1 1 calc R U . . .
C17 C 0.9055(3) 0.6876(2) 0.1788(3) 0.0681(11) Uani 1 1 d . . . . .
H17A H 0.9762 0.7019 0.1500 0.102 Uiso 1 1 calc R U . . .
H17B H 0.8575 0.6453 0.1526 0.102 Uiso 1 1 calc R U . . .
H17C H 0.9395 0.6716 0.2306 0.102 Uiso 1 1 calc R U . . .
C18 C 0.2647(4) 0.7142(2) 0.3610(2) 0.0576(9) Uani 1 1 d . . . . .
H18A H 0.1970 0.7345 0.3892 0.086 Uiso 1 1 calc R U . . .
H18B H 0.3218 0.6817 0.3950 0.086 Uiso 1 1 calc R U . . .
H18C H 0.2265 0.6839 0.3173 0.086 Uiso 1 1 calc R U . . .
C19 C 0.3387(3) 0.77877(18) 0.33290(17) 0.0374(6) Uani 1 1 d . . . . .
C20 C 0.7150(4) 1.0734(3) 0.0880(2) 0.0709(12) Uani 1 1 d . . . . .
H20A H 0.6939 1.0562 0.0349 0.106 Uiso 1 1 calc R U . . .
H20B H 0.8065 1.0663 0.1034 0.106 Uiso 1 1 calc R U . . .
H20C H 0.6934 1.1277 0.0918 0.106 Uiso 1 1 calc R U . . .
C21 C 0.6416(3) 1.02832(18) 0.13874(18) 0.0402(7) Uani 1 1 d . . . . .
C24 C 0.2365(3) 0.97849(18) 0.17897(17) 0.0392(7) Uani 1 1 d . . . . .
H24 H 0.1801 1.0210 0.1728 0.047 Uiso 1 1 calc R U . . .
N1 N 0.3351(2) 0.98367(13) 0.23080(14) 0.0335(5) Uani 1 1 d . . . . .
N2 N 0.5881(2) 0.96304(13) 0.34289(12) 0.0323(5) Uani 1 1 d . . . . .
N3 N 0.3950(2) 0.82858(15) 0.31006(14) 0.0389(5) Uani 1 1 d . . . . .
N4 N 0.5852(2) 0.99132(15) 0.17772(14) 0.0393(6) Uani 1 1 d . . . . .
N5 N 0.5252(3) 0.64389(17) 0.24950(17) 0.0508(7) Uani 1 1 d . . . . .
N6 N 0.6608(4) 0.6340(2) 0.02602(18) 0.0660(10) Uani 1 1 d . . . . .
N7 N 0.6296(3) 0.87265(18) 0.00912(17) 0.0524(7) Uani 1 1 d . . . . .
O1 O 0.3442(3) 0.73596(13) 0.05385(15) 0.0511(6) Uani 1 1 d . . . . .
O2 O 0.41763(16) 0.84988(11) 0.14903(11) 0.0332(4) Uani 1 1 d . . . . .
O3 O 0.34537(19) 1.06003(11) 0.26451(12) 0.0416(5) Uani 1 1 d . . . . .
O4 O 0.53439(19) 1.01580(12) 0.39451(12) 0.0424(5) Uani 1 1 d . . . . .
O5 O 0.64144(17) 0.83793(11) 0.23911(11) 0.0314(4) Uani 1 1 d . . . . .
O6 O 0.8199(2) 0.75412(11) 0.18341(16) 0.0436(6) Uani 1 1 d . . . . .
O7 O 0.4376(2) 0.67902(13) 0.20571(14) 0.0506(6) Uani 1 1 d . . . . .
O8 O 0.6405(2) 0.65925(16) 0.23839(17) 0.0635(7) Uani 1 1 d . . . . .
O9 O 0.5004(3) 0.6005(2) 0.3006(2) 0.0934(12) Uani 1 1 d . . . . .
O10 O 0.5778(3) 0.62439(16) 0.07302(17) 0.0785(8) Uani 1 1 d . . . . .
O11 O 0.7126(3) 0.70038(19) 0.02755(18) 0.0841(9) Uani 1 1 d . . . . .
O12 O 0.6898(3) 0.5810(2) -0.01541(16) 0.0888(11) Uani 1 1 d . . . . .
O13 O 0.5346(3) 0.82531(17) -0.00092(14) 0.0638(7) Uani 1 1 d . . . . .
O14 O 0.7023(2) 0.86574(14) 0.07319(14) 0.0520(6) Uani 1 1 d . . . . .
O15 O 0.6495(3) 0.92088(18) -0.03884(17) 0.0820(9) 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
Gd1 O2 2.3414(18) . ?
Gd1 O5 2.3494(19) . ?
Gd1 O14 2.484(2) . ?
Gd1 O7 2.485(2) . ?
Gd1 O10 2.495(3) . ?
Gd1 O13 2.511(3) . ?
Gd1 O6 2.546(2) . ?
Gd1 O11 2.549(3) . ?
Gd1 O8 2.555(3) . ?
Gd1 O1 2.653(2) . ?
Gd1 Ni1 3.4798(6) . ?
Ni1 N1 2.011(2) . ?
Ni1 O5 2.0213(19) . ?
Ni1 O2 2.0357(18) . ?
Ni1 N2 2.053(2) . ?
Ni1 N4 2.088(3) . ?
Ni1 N3 2.134(3) . ?
C1 O2 1.328(3) . ?
C1 C6 1.400(4) . ?
C1 C2 1.417(4) . ?
C2 C3 1.368(4) . ?
C2 O1 1.382(4) . ?
C3 C4 1.378(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.357(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.406(4) . ?
C5 H5 0.9300 . ?
C6 C24 1.449(4) . ?
C7 O3 1.426(4) . ?
C7 C8 1.493(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O4 1.436(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.282(3) . ?
C9 C10 1.439(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.407(4) . ?
C10 C15 1.409(4) . ?
C11 C12 1.360(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.388(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.372(4) . ?
C13 H13 0.9300 . ?
C14 O6 1.389(4) . ?
C14 C15 1.399(4) . ?
C15 O5 1.332(3) . ?
C16 O1 1.435(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O6 1.449(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.457(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N3 1.128(4) . ?
C20 C21 1.443(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N4 1.131(4) . ?
C24 N1 1.277(4) . ?
C24 H24 0.9300 . ?
N1 O3 1.429(3) . ?
N2 O4 1.422(3) . ?
N5 O9 1.200(4) . ?
N5 O8 1.255(4) . ?
N5 O7 1.261(3) . ?
N6 O12 1.212(4) . ?
N6 O11 1.254(5) . ?
N6 O10 1.254(4) . ?
N7 O15 1.201(4) . ?
N7 O14 1.265(4) . ?
N7 O13 1.269(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Gd1 O5 68.46(6) . . ?
O2 Gd1 O14 88.22(7) . . ?
O5 Gd1 O14 77.53(7) . . ?
O2 Gd1 O7 79.30(7) . . ?
O5 Gd1 O7 90.91(7) . . ?
O14 Gd1 O7 165.49(8) . . ?
O2 Gd1 O10 134.07(9) . . ?
O5 Gd1 O10 146.45(9) . . ?
O14 Gd1 O10 120.65(9) . . ?
O7 Gd1 O10 73.76(9) . . ?
O2 Gd1 O13 76.27(8) . . ?
O5 Gd1 O13 117.39(8) . . ?
O14 Gd1 O13 50.83(8) . . ?
O7 Gd1 O13 131.23(8) . . ?
O10 Gd1 O13 94.49(10) . . ?
O2 Gd1 O6 130.63(6) . . ?
O5 Gd1 O6 64.09(7) . . ?
O14 Gd1 O6 69.34(7) . . ?
O7 Gd1 O6 113.61(8) . . ?
O10 Gd1 O6 94.45(9) . . ?
O13 Gd1 O6 114.40(9) . . ?
O2 Gd1 O11 144.04(8) . . ?
O5 Gd1 O11 131.32(10) . . ?
O14 Gd1 O11 71.53(9) . . ?
O7 Gd1 O11 122.97(10) . . ?
O10 Gd1 O11 49.65(10) . . ?
O13 Gd1 O11 67.88(9) . . ?
O6 Gd1 O11 70.16(10) . . ?
O2 Gd1 O8 117.28(8) . . ?
O5 Gd1 O8 77.03(9) . . ?
O14 Gd1 O8 133.16(8) . . ?
O7 Gd1 O8 50.05(7) . . ?
O10 Gd1 O8 70.22(10) . . ?
O13 Gd1 O8 164.10(9) . . ?
O6 Gd1 O8 64.27(7) . . ?
O11 Gd1 O8 97.87(10) . . ?
O2 Gd1 O1 62.42(7) . . ?
O5 Gd1 O1 128.81(7) . . ?
O14 Gd1 O1 113.35(8) . . ?
O7 Gd1 O1 67.27(8) . . ?
O10 Gd1 O1 72.99(9) . . ?
O13 Gd1 O1 64.05(9) . . ?
O6 Gd1 O1 166.86(7) . . ?
O11 Gd1 O1 98.07(10) . . ?
O8 Gd1 O1 113.29(8) . . ?
O2 Gd1 Ni1 34.39(4) . . ?
O5 Gd1 Ni1 34.08(4) . . ?
O14 Gd1 Ni1 81.02(6) . . ?
O7 Gd1 Ni1 84.50(6) . . ?
O10 Gd1 Ni1 158.02(7) . . ?
O13 Gd1 Ni1 97.54(6) . . ?
O6 Gd1 Ni1 97.21(5) . . ?
O11 Gd1 Ni1 152.32(8) . . ?
O8 Gd1 Ni1 98.33(7) . . ?
O1 Gd1 Ni1 95.92(5) . . ?
N1 Ni1 O5 170.31(9) . . ?
N1 Ni1 O2 90.22(8) . . ?
O5 Ni1 O2 81.14(7) . . ?
N1 Ni1 N2 98.71(9) . . ?
O5 Ni1 N2 89.98(8) . . ?
O2 Ni1 N2 171.06(8) . . ?
N1 Ni1 N4 87.67(9) . . ?
O5 Ni1 N4 88.36(9) . . ?
O2 Ni1 N4 92.71(9) . . ?
N2 Ni1 N4 88.05(9) . . ?
N1 Ni1 N3 93.30(9) . . ?
O5 Ni1 N3 90.39(9) . . ?
O2 Ni1 N3 85.40(9) . . ?
N2 Ni1 N3 93.68(9) . . ?
N4 Ni1 N3 177.87(9) . . ?
N1 Ni1 Gd1 130.54(7) . . ?
O5 Ni1 Gd1 40.64(5) . . ?
O2 Ni1 Gd1 40.51(5) . . ?
N2 Ni1 Gd1 130.61(6) . . ?
N4 Ni1 Gd1 90.24(7) . . ?
N3 Ni1 Gd1 87.70(7) . . ?
O2 C1 C6 124.3(2) . . ?
O2 C1 C2 118.4(2) . . ?
C6 C1 C2 117.3(2) . . ?
C3 C2 O1 125.2(3) . . ?
C3 C2 C1 121.2(3) . . ?
O1 C2 C1 113.6(2) . . ?
C2 C3 C4 120.7(3) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.9(3) . . ?
C1 C6 C24 124.5(2) . . ?
C5 C6 C24 115.6(3) . . ?
O3 C7 C8 115.2(2) . . ?
O3 C7 H7A 108.5 . . ?
C8 C7 H7A 108.5 . . ?
O3 C7 H7B 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
O4 C8 C7 112.3(3) . . ?
O4 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
O4 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
N2 C9 C10 126.5(3) . . ?
N2 C9 H9 116.8 . . ?
C10 C9 H9 116.8 . . ?
C11 C10 C15 119.2(3) . . ?
C11 C10 C9 115.8(3) . . ?
C15 C10 C9 124.9(2) . . ?
C12 C11 C10 121.6(3) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C11 C12 C13 119.7(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 119.6(3) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 O6 123.6(3) . . ?
C13 C14 C15 122.4(3) . . ?
O6 C14 C15 114.0(2) . . ?
O5 C15 C14 118.5(2) . . ?
O5 C15 C10 123.9(2) . . ?
C14 C15 C10 117.5(2) . . ?
O1 C16 H16A 109.5 . . ?
O1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O6 C17 H17A 109.5 . . ?
O6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 C18 179.0(3) . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N4 C21 C20 178.2(4) . . ?
N1 C24 C6 124.7(3) . . ?
N1 C24 H24 117.6 . . ?
C6 C24 H24 117.6 . . ?
C24 N1 O3 111.3(2) . . ?
C24 N1 Ni1 127.2(2) . . ?
O3 N1 Ni1 119.02(15) . . ?
C9 N2 O4 109.8(2) . . ?
C9 N2 Ni1 122.66(19) . . ?
O4 N2 Ni1 126.29(15) . . ?
C19 N3 Ni1 168.7(2) . . ?
C21 N4 Ni1 173.7(3) . . ?
O9 N5 O8 121.8(3) . . ?
O9 N5 O7 122.2(3) . . ?
O8 N5 O7 115.9(3) . . ?
O12 N6 O11 123.8(4) . . ?
O12 N6 O10 120.9(4) . . ?
O11 N6 O10 115.3(3) . . ?
O15 N7 O14 122.1(4) . . ?
O15 N7 O13 122.4(3) . . ?
O14 N7 O13 115.5(3) . . ?
C2 O1 C16 116.1(3) . . ?
C2 O1 Gd1 117.16(17) . . ?
C16 O1 Gd1 124.3(2) . . ?
C1 O2 Ni1 125.09(16) . . ?
C1 O2 Gd1 128.46(16) . . ?
Ni1 O2 Gd1 105.10(7) . . ?
C7 O3 N1 110.9(2) . . ?
N2 O4 C8 112.1(2) . . ?
C15 O5 Ni1 123.24(17) . . ?
C15 O5 Gd1 123.50(17) . . ?
Ni1 O5 Gd1 105.29(7) . . ?
C14 O6 C17 116.4(3) . . ?
C14 O6 Gd1 116.62(16) . . ?
C17 O6 Gd1 125.4(2) . . ?
N5 O7 Gd1 98.59(17) . . ?
N5 O8 Gd1 95.39(19) . . ?
N6 O10 Gd1 98.8(2) . . ?
N6 O11 Gd1 96.2(2) . . ?
N7 O13 Gd1 96.10(19) . . ?
N7 O14 Gd1 97.5(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C24 H24 O9 0.93 2.39 3.266(4) 156.0 2
C20 H20B O9 0.96 2.51 3.352(5) 146.7 2_655
C20 H20A O15 0.96 2.65 3.418(6) 136.9 .
C18 H18C O3 0.96 2.60 3.514(4) 158.1 2_545
C18 H18A O11 0.96 2.61 3.313(5) 129.9 4_576
C17 H17B O4 0.96 2.65 3.286(4) 124.2 2_645
C16 H16B O10 0.96 2.37 3.095(5) 131.7 .
C9 H9 O12 0.93 2.53 3.450(4) 169.7 2_655
C8 H8B N3 0.97 2.43 3.339(4) 156.4 .
C8 H8A O12 0.97 2.60 3.120(4) 113.5 4_576
C8 H8A O12 0.97 2.60 3.120(4) 113.5 4_576
C8 H8B N3 0.97 2.43 3.339(4) 156.4 .
C9 H9 O12 0.93 2.53 3.450(4) 169.7 2_655
C16 H16B O10 0.96 2.37 3.095(5) 131.7 .
C17 H17B O4 0.96 2.65 3.286(4) 124.2 2_645
C18 H18A O11 0.96 2.61 3.313(5) 129.9 4_576
C18 H18C O3 0.96 2.60 3.514(4) 158.1 2_545
C20 H20A O15 0.96 2.65 3.418(6) 136.9 .
C20 H20B O9 0.96 2.51 3.352(5) 146.7 2_655
C24 H24 O9 0.93 2.39 3.266(4) 156.0 2

_refine_diff_density_max         0.673
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.137

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1408412'
_audit_update_record             
;
2015-08-06 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H24 N7 Ni O15 Tb'
_chemical_formula_weight         844.11

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'
Ni Ni 0.3393 1.1124 '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           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   10.309(3)
_cell_length_b                   17.095(5)
_cell_length_c                   17.232(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.548(4)
_cell_angle_gamma                90
_cell_volume                     3017.2(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9926
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.55

_exptl_crystal_description       block
_exptl_crystal_colour            black-purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_F_000             1672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    3.031
_shelx_estimated_absorpt_T_min   0.495
_shelx_estimated_absorpt_T_max   0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_T_max  0.529
_exptl_absorpt_process_details   'SADABS; Bruker, 2013'

_exptl_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            17925
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.683
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5935
_reflns_number_gt                5319
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0220P)²+0.8575P]
 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
_refine_ls_extinction_coef       0.00552(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5935
_refine_ls_number_parameters     420
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0202
_refine_ls_wR_factor_ref         0.0508
_refine_ls_wR_factor_gt          0.0495
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.106
_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 0.08000(2) 0.24081(2) 0.13012(2) 0.03551(6) Uani 1 1 d . U . . .
Ni1 Ni -0.00953(3) 0.08762(2) 0.24488(2) 0.02849(8) Uani 1 1 d . . . . .
C1 C 0.2642(2) 0.14343(13) 0.26401(13) 0.0324(5) Uani 1 1 d . . . . .
C2 C 0.3640(2) 0.18749(14) 0.23544(15) 0.0377(5) Uani 1 1 d . . . . .
C3 C 0.4935(2) 0.17181(17) 0.25757(17) 0.0493(7) Uani 1 1 d . . . . .
H3 H 0.5576 0.2013 0.2373 0.059 Uiso 1 1 calc R U . . .
C4 C 0.5287(2) 0.11229(18) 0.30986(18) 0.0550(7) Uani 1 1 d . . . . .
H4 H 0.6165 0.1016 0.3247 0.066 Uiso 1 1 calc R U . . .
C5 C 0.4352(2) 0.06918(17) 0.33982(16) 0.0470(6) Uani 1 1 d . . . . .
H5 H 0.4599 0.0296 0.3755 0.056 Uiso 1 1 calc R U . . .
C6 C 0.3013(2) 0.08368(14) 0.31753(14) 0.0360(5) Uani 1 1 d . . . . .
C7 C 0.2119(2) 0.03727(14) 0.35741(14) 0.0361(5) Uani 1 1 d . . . . .
H7 H 0.2484 0.0046 0.3972 0.043 Uiso 1 1 calc R U . . .
C8 C -0.1037(2) -0.00356(15) 0.39624(15) 0.0426(6) Uani 1 1 d . . . . .
H8A H -0.1255 0.0497 0.3804 0.051 Uiso 1 1 calc R U . . .
H8B H -0.1248 -0.0103 0.4493 0.051 Uiso 1 1 calc R U . . .
C9 C -0.1845(2) -0.05901(15) 0.34348(16) 0.0459(6) Uani 1 1 d . . . . .
H9A H -0.1726 -0.1114 0.3647 0.055 Uiso 1 1 calc R U . . .
H9B H -0.2757 -0.0454 0.3437 0.055 Uiso 1 1 calc R U . . .
C10 C -0.2634(2) 0.02176(15) 0.17890(15) 0.0408(6) Uani 1 1 d . . . . .
H10 H -0.3196 -0.0209 0.1725 0.049 Uiso 1 1 calc R U . . .
C11 C -0.2939(2) 0.08892(16) 0.12906(14) 0.0405(6) Uani 1 1 d . . . . .
C12 C -0.4213(3) 0.0919(2) 0.09037(18) 0.0626(8) Uani 1 1 d . . . . .
H12 H -0.4796 0.0518 0.0979 0.075 Uiso 1 1 calc R U . . .
C13 C -0.4608(3) 0.1519(2) 0.0425(2) 0.0756(11) Uani 1 1 d . . . . .
H13 H -0.5462 0.1533 0.0184 0.091 Uiso 1 1 calc R U . . .
C14 C -0.3746(3) 0.2115(2) 0.02895(17) 0.0609(8) Uani 1 1 d . . . . .
H14 H -0.4020 0.2526 -0.0042 0.073 Uiso 1 1 calc R U . . .
C15 C -0.2491(2) 0.20922(16) 0.06472(14) 0.0408(6) Uani 1 1 d . . . . .
C16 C -0.2049(2) 0.14875(14) 0.11669(13) 0.0337(5) Uani 1 1 d . . . . .
C17 C 0.4050(3) 0.31184(17) 0.1783(2) 0.0674(9) Uani 1 1 d . . . . .
H17A H 0.4386 0.3285 0.2299 0.101 Uiso 1 1 calc R U . . .
H17B H 0.3571 0.3539 0.1515 0.101 Uiso 1 1 calc R U . . .
H17C H 0.4761 0.2971 0.1499 0.101 Uiso 1 1 calc R U . . .
C18 C -0.1813(4) 0.3154(2) -0.0118(2) 0.0823(11) Uani 1 1 d . . . . .
H18A H -0.1916 0.2849 -0.0589 0.123 Uiso 1 1 calc R U . . .
H18B H -0.1100 0.3513 -0.0135 0.123 Uiso 1 1 calc R U . . .
H18C H -0.2600 0.3442 -0.0074 0.123 Uiso 1 1 calc R U . . .
C19 C 0.2140(3) -0.0749(2) 0.08871(19) 0.0742(10) Uani 1 1 d . . . . .
H19A H 0.1639 -0.1201 0.0709 0.111 Uiso 1 1 calc R U . . .
H19B H 0.2949 -0.0913 0.1172 0.111 Uiso 1 1 calc R U . . .
H19C H 0.2318 -0.0441 0.0446 0.111 Uiso 1 1 calc R U . . .
C20 C 0.1410(2) -0.02848(15) 0.13909(15) 0.0423(6) Uani 1 1 d . . . . .
C21 C -0.2368(3) 0.28595(17) 0.36105(18) 0.0576(7) Uani 1 1 d . . . . .
H21A H -0.2711 0.3180 0.3178 0.086 Uiso 1 1 calc R U . . .
H21B H -0.1808 0.3168 0.3974 0.086 Uiso 1 1 calc R U . . .
H21C H -0.3076 0.2655 0.3866 0.086 Uiso 1 1 calc R U . . .
C22 C -0.1626(2) 0.22145(15) 0.33277(15) 0.0391(5) Uani 1 1 d . . . . .
N1 N 0.08757(17) 0.03692(11) 0.34304(11) 0.0329(4) Uani 1 1 d . . . . .
N2 N -0.16590(18) 0.01658(11) 0.23073(11) 0.0348(4) Uani 1 1 d . . . . .
N3 N 0.08503(19) 0.00849(12) 0.17793(12) 0.0407(5) Uani 1 1 d . . . . .
N4 N -0.10559(19) 0.17143(12) 0.31011(12) 0.0403(5) Uani 1 1 d . . . . .
N5 N 0.1291(3) 0.12757(15) 0.01046(14) 0.0543(6) Uani 1 1 d . . . . .
N6 N 0.0252(2) 0.35501(14) 0.24933(15) 0.0521(6) Uani 1 1 d . . . . .
N7 N 0.1608(3) 0.36538(17) 0.02682(15) 0.0684(8) Uani 1 1 d . U . . .
O1 O 0.14084(14) 0.16198(9) 0.23918(9) 0.0333(3) Uani 1 1 d . . . . .
O2 O 0.03339(16) -0.01570(10) 0.39469(10) 0.0439(4) Uani 1 1 d . . . . .
O3 O -0.15528(16) -0.06008(9) 0.26448(10) 0.0429(4) Uani 1 1 d . . . . .
O4 O -0.08184(14) 0.15012(9) 0.14923(9) 0.0348(4) Uani 1 1 d . . . . .
O5 O 0.31986(17) 0.24600(9) 0.18348(12) 0.0444(4) Uani 1 1 d . . . . .
O6 O -0.1547(2) 0.26472(11) 0.05410(12) 0.0523(5) Uani 1 1 d . . . . .
O7 O 0.20184(19) 0.13402(11) 0.07418(12) 0.0542(5) Uani 1 1 d . . . . .
O8 O 0.0348(2) 0.17478(14) 0.00022(12) 0.0656(6) Uani 1 1 d . U . . .
O9 O 0.1504(3) 0.07910(14) -0.03835(14) 0.0851(8) Uani 1 1 d . . . . .
O10 O 0.14081(18) 0.34009(13) 0.23853(13) 0.0632(6) Uani 1 1 d . U . . .
O11 O -0.06201(17) 0.32000(11) 0.20560(11) 0.0499(4) Uani 1 1 d . U . . .
O12 O -0.0005(2) 0.39902(16) 0.30018(17) 0.0930(9) Uani 1 1 d . . . . .
O13 O 0.0787(3) 0.37453(13) 0.07450(15) 0.0813(7) Uani 1 1 d . U . . .
O14 O 0.2120(3) 0.29889(16) 0.02811(15) 0.0875(8) Uani 1 1 d . U . . .
O15 O 0.1892(3) 0.41785(16) -0.01518(14) 0.0919(9) 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
Tb1 O4 2.3283(15) . ?
Tb1 O1 2.3394(16) . ?
Tb1 O11 2.4703(17) . ?
Tb1 O7 2.4730(19) . ?
Tb1 O13 2.478(2) . ?
Tb1 O8 2.503(2) . ?
Tb1 O5 2.5395(19) . ?
Tb1 O14 2.544(2) . ?
Tb1 O10 2.549(2) . ?
Tb1 O6 2.649(2) . ?
Tb1 Ni1 3.4695(7) . ?
Ni1 N2 2.0109(19) . ?
Ni1 O1 2.0158(15) . ?
Ni1 O4 2.0332(16) . ?
Ni1 N1 2.0562(19) . ?
Ni1 N3 2.090(2) . ?
Ni1 N4 2.133(2) . ?
C1 O1 1.333(3) . ?
C1 C6 1.400(3) . ?
C1 C2 1.408(3) . ?
C2 C3 1.372(3) . ?
C2 O5 1.384(3) . ?
C3 C4 1.380(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.361(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.412(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.448(3) . ?
C7 N1 1.278(3) . ?
C7 H7 0.9300 . ?
C8 O2 1.432(3) . ?
C8 C9 1.498(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O3 1.427(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.270(3) . ?
C10 C11 1.447(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.404(3) . ?
C11 C16 1.407(3) . ?
C12 C13 1.350(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.389(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.368(4) . ?
C14 H14 0.9300 . ?
C15 O6 1.386(3) . ?
C15 C16 1.409(3) . ?
C16 O4 1.327(3) . ?
C17 O5 1.436(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O6 1.431(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.449(4) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N3 1.126(3) . ?
C21 C22 1.458(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N4 1.132(3) . ?
N1 O2 1.424(2) . ?
N2 O3 1.433(2) . ?
N5 O9 1.218(3) . ?
N5 O8 1.261(3) . ?
N5 O7 1.262(3) . ?
N6 O12 1.207(3) . ?
N6 O10 1.253(3) . ?
N6 O11 1.257(3) . ?
N7 O15 1.209(3) . ?
N7 O14 1.252(4) . ?
N7 O13 1.254(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Tb1 O1 68.50(5) . . ?
O4 Tb1 O11 79.23(6) . . ?
O1 Tb1 O11 90.77(6) . . ?
O4 Tb1 O7 88.14(6) . . ?
O1 Tb1 O7 77.66(6) . . ?
O11 Tb1 O7 165.39(6) . . ?
O4 Tb1 O13 134.16(8) . . ?
O1 Tb1 O13 146.22(7) . . ?
O11 Tb1 O13 73.79(8) . . ?
O7 Tb1 O13 120.71(8) . . ?
O4 Tb1 O8 76.28(6) . . ?
O1 Tb1 O8 117.66(7) . . ?
O11 Tb1 O8 131.07(7) . . ?
O7 Tb1 O8 50.92(7) . . ?
O13 Tb1 O8 94.47(8) . . ?
O4 Tb1 O5 130.99(5) . . ?
O1 Tb1 O5 64.43(5) . . ?
O11 Tb1 O5 113.66(6) . . ?
O7 Tb1 O5 69.52(6) . . ?
O13 Tb1 O5 94.00(7) . . ?
O8 Tb1 O5 114.45(7) . . ?
O4 Tb1 O14 143.70(7) . . ?
O1 Tb1 O14 131.64(8) . . ?
O11 Tb1 O14 123.07(8) . . ?
O7 Tb1 O14 71.54(8) . . ?
O13 Tb1 O14 49.64(8) . . ?
O8 Tb1 O14 67.53(8) . . ?
O5 Tb1 O14 70.20(9) . . ?
O4 Tb1 O10 117.39(6) . . ?
O1 Tb1 O10 76.92(7) . . ?
O11 Tb1 O10 50.22(6) . . ?
O7 Tb1 O10 133.15(7) . . ?
O13 Tb1 O10 70.08(8) . . ?
O8 Tb1 O10 163.95(8) . . ?
O5 Tb1 O10 64.11(6) . . ?
O14 Tb1 O10 98.07(8) . . ?
O4 Tb1 O6 62.85(6) . . ?
O1 Tb1 O6 129.22(5) . . ?
O11 Tb1 O6 67.23(7) . . ?
O7 Tb1 O6 113.40(7) . . ?
O13 Tb1 O6 72.68(8) . . ?
O8 Tb1 O6 63.95(7) . . ?
O5 Tb1 O6 166.07(6) . . ?
O14 Tb1 O6 97.38(9) . . ?
O10 Tb1 O6 113.22(6) . . ?
O4 Tb1 Ni1 34.44(4) . . ?
O1 Tb1 Ni1 34.07(4) . . ?
O11 Tb1 Ni1 84.34(5) . . ?
O7 Tb1 Ni1 81.08(5) . . ?
O13 Tb1 Ni1 157.93(6) . . ?
O8 Tb1 Ni1 97.75(6) . . ?
O5 Tb1 Ni1 97.54(4) . . ?
O14 Tb1 Ni1 152.43(7) . . ?
O10 Tb1 Ni1 98.28(6) . . ?
O6 Tb1 Ni1 96.37(4) . . ?
N2 Ni1 O1 170.16(7) . . ?
N2 Ni1 O4 90.25(7) . . ?
O1 Ni1 O4 80.91(6) . . ?
N2 Ni1 N1 98.83(8) . . ?
O1 Ni1 N1 90.05(7) . . ?
O4 Ni1 N1 170.92(7) . . ?
N2 Ni1 N3 87.71(8) . . ?
O1 Ni1 N3 88.37(7) . . ?
O4 Ni1 N3 92.50(8) . . ?
N1 Ni1 N3 88.13(8) . . ?
N2 Ni1 N4 93.19(8) . . ?
O1 Ni1 N4 90.45(7) . . ?
O4 Ni1 N4 85.69(7) . . ?
N1 Ni1 N4 93.52(8) . . ?
N3 Ni1 N4 177.98(8) . . ?
N2 Ni1 Tb1 130.42(6) . . ?
O1 Ni1 Tb1 40.55(4) . . ?
O4 Ni1 Tb1 40.36(4) . . ?
N1 Ni1 Tb1 130.61(5) . . ?
N3 Ni1 Tb1 90.16(6) . . ?
N4 Ni1 Tb1 87.88(6) . . ?
O1 C1 C6 124.3(2) . . ?
O1 C1 C2 118.0(2) . . ?
C6 C1 C2 117.7(2) . . ?
C3 C2 O5 123.9(2) . . ?
C3 C2 C1 121.6(2) . . ?
O5 C2 C1 114.4(2) . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.1(2) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.0(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.5(2) . . ?
C1 C6 C7 124.9(2) . . ?
C5 C6 C7 115.5(2) . . ?
N1 C7 C6 126.1(2) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
O2 C8 C9 112.2(2) . . ?
O2 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
O2 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
O3 C9 C8 115.1(2) . . ?
O3 C9 H9A 108.5 . . ?
C8 C9 H9A 108.5 . . ?
O3 C9 H9B 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
N2 C10 C11 125.0(2) . . ?
N2 C10 H10 117.5 . . ?
C11 C10 H10 117.5 . . ?
C12 C11 C16 119.5(2) . . ?
C12 C11 C10 116.0(2) . . ?
C16 C11 C10 124.4(2) . . ?
C13 C12 C11 121.2(3) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 119.6(3) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 O6 124.3(2) . . ?
C14 C15 C16 121.9(3) . . ?
O6 C15 C16 113.9(2) . . ?
O4 C16 C11 123.9(2) . . ?
O4 C16 C15 118.7(2) . . ?
C11 C16 C15 117.4(2) . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 C19 179.1(3) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 C21 179.3(3) . . ?
C7 N1 O2 109.77(18) . . ?
C7 N1 Ni1 122.76(16) . . ?
O2 N1 Ni1 126.28(13) . . ?
C10 N2 O3 111.54(19) . . ?
C10 N2 Ni1 127.07(17) . . ?
O3 N2 Ni1 118.69(13) . . ?
C20 N3 Ni1 173.8(2) . . ?
C22 N4 Ni1 168.4(2) . . ?
O9 N5 O8 122.4(3) . . ?
O9 N5 O7 121.6(3) . . ?
O8 N5 O7 116.0(2) . . ?
O12 N6 O10 121.7(3) . . ?
O12 N6 O11 122.0(2) . . ?
O10 N6 O11 116.2(2) . . ?
O15 N7 O14 123.6(3) . . ?
O15 N7 O13 121.8(3) . . ?
O14 N7 O13 114.6(3) . . ?
C1 O1 Ni1 123.04(14) . . ?
C1 O1 Tb1 123.60(14) . . ?
Ni1 O1 Tb1 105.38(6) . . ?
N1 O2 C8 112.25(17) . . ?
C9 O3 N2 111.14(17) . . ?
C16 O4 Ni1 125.29(14) . . ?
C16 O4 Tb1 128.15(14) . . ?
Ni1 O4 Tb1 105.20(6) . . ?
C2 O5 C17 116.7(2) . . ?
C2 O5 Tb1 116.34(13) . . ?
C17 O5 Tb1 125.54(17) . . ?
C15 O6 C18 116.5(2) . . ?
C15 O6 Tb1 116.40(14) . . ?
C18 O6 Tb1 124.57(19) . . ?
N5 O7 Tb1 97.23(16) . . ?
N5 O8 Tb1 95.83(16) . . ?
N6 O10 Tb1 94.92(15) . . ?
N6 O11 Tb1 98.63(14) . . ?
N7 O13 Tb1 99.44(19) . . ?
N7 O14 Tb1 96.26(18) . . ?

_refine_diff_density_max         0.463
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.064

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1408413'
_audit_update_record             
;
2015-08-06 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H24 Dy N7 Ni O15'
_chemical_formula_weight         847.69

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           9
_space_group_name_H-M_alt        'C 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'

_cell_length_a                   21.577(3)
_cell_length_b                   9.4531(12)
_cell_length_c                   15.866(2)
_cell_angle_alpha                90
_cell_angle_beta                 114.880(2)
_cell_angle_gamma                90
_cell_volume                     2935.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8190
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.54

_exptl_crystal_description       block-like
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_F_000             1676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    3.251
_shelx_estimated_absorpt_T_min   0.485
_shelx_estimated_absorpt_T_max   0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_T_max  0.557
_exptl_absorpt_process_details   'SADABS; Bruker, 2013'

_exptl_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            8476
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.081
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_point_group_measured_fraction_full 0.853
_reflns_number_total             4915
_reflns_number_gt                4790
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.702
_reflns_Friedel_fraction_max     0.702
_reflns_Friedel_fraction_full    0.707

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)]
 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
_refine_ls_extinction_coef       0.00487(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1931 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.005(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4915
_refine_ls_number_parameters     420
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0153
_refine_ls_wR_factor_ref         0.0357
_refine_ls_wR_factor_gt          0.0354
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_restrained_S_all      0.874
_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
Dy1 Dy 1.00207(2) 0.56184(2) 0.73746(2) 0.02626(7) Uani 1 1 d . . . . .
Ni1 Ni 0.89533(2) 0.62627(5) 0.50736(3) 0.02735(11) Uani 1 1 d . . . . .
C1 C 1.0057(2) 0.8344(4) 0.6174(3) 0.0334(9) Uani 1 1 d . . . . .
C2 C 1.0664(2) 0.8630(5) 0.6955(3) 0.0406(10) Uani 1 1 d . . . . .
C3 C 1.1030(3) 0.9859(6) 0.7030(5) 0.0574(14) Uani 1 1 d . . . . .
H3 H 1.1435 1.0025 0.7551 0.069 Uiso 1 1 calc R U . . .
C4 C 1.0781(3) 1.0844(5) 0.6311(6) 0.0684(19) Uani 1 1 d . . . . .
H4 H 1.1020 1.1681 0.6358 0.082 Uiso 1 1 calc R U . . .
C5 C 1.0198(4) 1.0601(5) 0.5547(5) 0.0619(17) Uani 1 1 d . . . . .
H5 H 1.0043 1.1274 0.5076 0.074 Uiso 1 1 calc R U . . .
C6 C 0.9819(3) 0.9348(4) 0.5448(4) 0.0440(11) Uani 1 1 d . . . . .
C7 C 0.9161(3) 0.9249(5) 0.4663(4) 0.0452(12) Uani 1 1 d . . . . .
H7 H 0.8997 1.0058 0.4303 0.054 Uiso 1 1 calc R U . . .
C8 C 0.7949(3) 0.7939(7) 0.2881(3) 0.0625(15) Uani 1 1 d . . . . .
H8A H 0.8167 0.8545 0.2593 0.075 Uiso 1 1 calc R U . . .
H8B H 0.7460 0.8015 0.2517 0.075 Uiso 1 1 calc R U . . .
C9 C 0.8154(3) 0.6454(6) 0.2821(3) 0.0514(13) Uani 1 1 d . . . . .
H9A H 0.8042 0.6228 0.2177 0.062 Uiso 1 1 calc R U . . .
H9B H 0.8646 0.6369 0.3166 0.062 Uiso 1 1 calc R U . . .
C10 C 0.8095(2) 0.3744(5) 0.4229(3) 0.0401(10) Uani 1 1 d . . . . .
H10 H 0.7735 0.3319 0.3737 0.048 Uiso 1 1 calc R U . . .
C11 C 0.8409(2) 0.2931(4) 0.5083(3) 0.0350(9) Uani 1 1 d . . . . .
C12 C 0.8148(3) 0.1560(6) 0.5065(4) 0.0502(13) Uani 1 1 d . . . . .
H12 H 0.7783 0.1246 0.4530 0.060 Uiso 1 1 calc R U . . .
C13 C 0.8419(3) 0.0684(5) 0.5816(5) 0.0563(15) Uani 1 1 d . . . . .
H13 H 0.8238 -0.0216 0.5789 0.068 Uiso 1 1 calc R U . . .
C14 C 0.8966(3) 0.1131(5) 0.6621(4) 0.0500(12) Uani 1 1 d . . . . .
H14 H 0.9158 0.0528 0.7129 0.060 Uiso 1 1 calc R U . . .
C15 C 0.9219(2) 0.2477(4) 0.6656(3) 0.0340(9) Uani 1 1 d . . . . .
C16 C 0.8946(2) 0.3414(4) 0.5898(3) 0.0284(8) Uani 1 1 d . . . . .
C17 C 1.1342(3) 0.7928(7) 0.8541(4) 0.0740(17) Uani 1 1 d . . . . .
H17A H 1.1223 0.8825 0.8715 0.111 Uiso 1 1 calc R U . . .
H17B H 1.1790 0.7987 0.8553 0.111 Uiso 1 1 calc R U . . .
H17C H 1.1340 0.7215 0.8970 0.111 Uiso 1 1 calc R U . . .
C18 C 1.0130(3) 0.2076(5) 0.8164(3) 0.0510(12) Uani 1 1 d . . . . .
H18A H 1.0250 0.1256 0.7908 0.076 Uiso 1 1 calc R U . . .
H18B H 0.9852 0.1797 0.8475 0.076 Uiso 1 1 calc R U . . .
H18C H 1.0538 0.2525 0.8600 0.076 Uiso 1 1 calc R U . . .
C19 C 0.7278(3) 0.7106(8) 0.6156(4) 0.0736(18) Uani 1 1 d . . . . .
H19A H 0.7003 0.7924 0.5881 0.110 Uiso 1 1 calc R U . . .
H19B H 0.7507 0.7232 0.6817 0.110 Uiso 1 1 calc R U . . .
H19C H 0.6991 0.6284 0.6020 0.110 Uiso 1 1 calc R U . . .
C20 C 0.7783(2) 0.6923(5) 0.5779(3) 0.0384(9) Uani 1 1 d . . . . .
C21 C 0.6544(4) 0.1632(10) 0.5509(4) 0.097(3) Uani 1 1 d . . . . .
H21A H 0.6966 0.1123 0.5813 0.145 Uiso 1 1 calc R U . . .
H21B H 0.6245 0.1119 0.4969 0.145 Uiso 1 1 calc R U . . .
H21C H 0.6331 0.1737 0.5928 0.145 Uiso 1 1 calc R U . . .
C22 C 0.6679(3) 0.2992(10) 0.5240(5) 0.0784(19) Uani 1 1 d . . . . .
N1 N 0.87896(18) 0.8159(4) 0.4425(2) 0.0418(9) Uani 1 1 d . . . . .
N2 N 0.82658(16) 0.4986(4) 0.4088(2) 0.0355(8) Uani 1 1 d . . . . .
N3 N 0.91023(19) 0.7404(4) 0.7799(2) 0.0404(8) Uani 1 1 d . . . . .
N4 N 1.1271(2) 0.4404(4) 0.7470(3) 0.0442(10) Uani 1 1 d . . . . .
N5 N 0.99179(17) 0.4744(4) 0.4406(2) 0.0304(7) Uani 1 1 d . . . . .
N6 N 0.81781(19) 0.6788(4) 0.5506(2) 0.0391(8) Uani 1 1 d . . . . .
N7 N 0.6786(5) 0.4032(10) 0.5000(8) 0.129(3) Uani 1 1 d . . . . .
O1 O 1.08550(15) 0.7565(3) 0.7619(2) 0.0444(7) Uani 1 1 d . . . . .
O2 O 0.97207(14) 0.7164(3) 0.61612(18) 0.0317(6) Uani 1 1 d . . . . .
O3 O 0.81025(18) 0.8469(4) 0.3773(2) 0.0544(9) Uani 1 1 d . . . . .
O4 O 0.78251(17) 0.5450(4) 0.3181(2) 0.0529(9) Uani 1 1 d . . . . .
O5 O 0.92287(14) 0.4694(3) 0.60105(18) 0.0271(5) Uani 1 1 d . . . . .
O6 O 0.97523(16) 0.3059(3) 0.74230(18) 0.0382(7) Uani 1 1 d . . . . .
O7 O 0.86783(19) 0.8150(4) 0.7909(2) 0.0628(10) Uani 1 1 d . . . . .
O8 O 0.96669(17) 0.7877(3) 0.7890(2) 0.0444(7) Uani 1 1 d . . . . .
O9 O 0.89820(16) 0.6109(3) 0.7566(2) 0.0394(6) Uani 1 1 d . . . . .
O10 O 1.1810(2) 0.3941(6) 0.7528(3) 0.0785(13) Uani 1 1 d . . . . .
O11 O 1.07925(18) 0.4727(4) 0.6700(2) 0.0486(8) Uani 1 1 d . . . . .
O12 O 1.11509(18) 0.4588(4) 0.8177(2) 0.0494(8) Uani 1 1 d . . . . .
O13 O 0.97140(17) 0.5932(3) 0.4542(2) 0.0369(7) Uani 1 1 d . . . . .
O14 O 0.9760(2) 0.3661(3) 0.4660(2) 0.0496(8) Uani 1 1 d . . . . .
O15 O 1.03065(14) 0.5250(3) 0.89745(19) 0.0369(6) 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
Dy1 O2 2.283(3) . ?
Dy1 O5 2.293(3) . ?
Dy1 O15 2.372(3) . ?
Dy1 O9 2.429(3) . ?
Dy1 O12 2.430(3) . ?
Dy1 O11 2.476(3) . ?
Dy1 O1 2.488(3) . ?
Dy1 O6 2.497(3) . ?
Dy1 O8 2.517(3) . ?
Dy1 Ni1 3.4538(6) . ?
Ni1 O5 2.005(3) . ?
Ni1 O2 2.010(3) . ?
Ni1 N1 2.023(4) . ?
Ni1 N2 2.037(4) . ?
Ni1 N6 2.117(4) . ?
Ni1 O13 2.161(3) . ?
C1 O2 1.326(5) . ?
C1 C2 1.399(6) . ?
C1 C6 1.412(6) . ?
C2 C3 1.381(7) . ?
C2 O1 1.389(6) . ?
C3 C4 1.393(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.350(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.410(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.446(8) . ?
C7 N1 1.262(6) . ?
C7 H7 0.9300 . ?
C8 O3 1.403(6) . ?
C8 C9 1.488(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O4 1.440(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.278(7) . ?
C10 C11 1.454(6) . ?
C10 H10 0.9300 . ?
C11 C16 1.401(6) . ?
C11 C12 1.408(6) . ?
C12 C13 1.365(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.391(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.377(6) . ?
C14 H14 0.9300 . ?
C15 O6 1.389(5) . ?
C15 C16 1.408(6) . ?
C16 O5 1.332(4) . ?
C17 O1 1.438(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O6 1.450(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.457(6) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N6 1.115(5) . ?
C21 C22 1.423(11) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N7 1.113(11) . ?
N1 O3 1.436(5) . ?
N2 O4 1.420(5) . ?
N3 O7 1.224(5) . ?
N3 O8 1.248(5) . ?
N3 O9 1.274(5) . ?
N4 O10 1.209(5) . ?
N4 O11 1.261(6) . ?
N4 O12 1.265(5) . ?
N5 O14 1.202(5) . ?
N5 O13 1.257(5) . ?
N5 O15 1.286(4) 2_564 ?
O15 N5 1.286(4) 2_565 ?

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 Dy1 O5 67.27(9) . . ?
O2 Dy1 O15 148.23(10) . . ?
O5 Dy1 O15 135.16(10) . . ?
O2 Dy1 O9 91.95(11) . . ?
O5 Dy1 O9 80.22(10) . . ?
O15 Dy1 O9 74.50(10) . . ?
O2 Dy1 O12 124.36(11) . . ?
O5 Dy1 O12 121.80(11) . . ?
O15 Dy1 O12 68.21(10) . . ?
O9 Dy1 O12 141.85(11) . . ?
O2 Dy1 O11 81.77(11) . . ?
O5 Dy1 O11 80.32(10) . . ?
O15 Dy1 O11 119.57(11) . . ?
O9 Dy1 O11 160.49(11) . . ?
O12 Dy1 O11 51.74(11) . . ?
O2 Dy1 O1 65.67(10) . . ?
O5 Dy1 O1 129.22(10) . . ?
O15 Dy1 O1 95.53(10) . . ?
O9 Dy1 O1 118.97(11) . . ?
O12 Dy1 O1 73.38(11) . . ?
O11 Dy1 O1 75.23(12) . . ?
O2 Dy1 O6 131.23(9) . . ?
O5 Dy1 O6 64.48(9) . . ?
O15 Dy1 O6 77.53(10) . . ?
O9 Dy1 O6 86.73(11) . . ?
O12 Dy1 O6 77.87(11) . . ?
O11 Dy1 O6 83.71(11) . . ?
O1 Dy1 O6 150.93(10) . . ?
O2 Dy1 O8 73.36(10) . . ?
O5 Dy1 O8 114.99(10) . . ?
O15 Dy1 O8 75.82(10) . . ?
O9 Dy1 O8 51.39(11) . . ?
O12 Dy1 O8 123.00(11) . . ?
O11 Dy1 O8 141.27(12) . . ?
O1 Dy1 O8 67.67(10) . . ?
O6 Dy1 O8 134.94(10) . . ?
O2 Dy1 Ni1 33.83(6) . . ?
O5 Dy1 Ni1 33.76(6) . . ?
O15 Dy1 Ni1 156.13(7) . . ?
O9 Dy1 Ni1 81.85(8) . . ?
O12 Dy1 Ni1 134.46(8) . . ?
O11 Dy1 Ni1 82.74(8) . . ?
O1 Dy1 Ni1 98.71(7) . . ?
O6 Dy1 Ni1 98.24(6) . . ?
O8 Dy1 Ni1 92.01(7) . . ?
O5 Ni1 O2 78.28(10) . . ?
O5 Ni1 N1 165.19(14) . . ?
O2 Ni1 N1 88.03(14) . . ?
O5 Ni1 N2 91.37(13) . . ?
O2 Ni1 N2 168.75(13) . . ?
N1 Ni1 N2 102.67(16) . . ?
O5 Ni1 N6 87.78(13) . . ?
O2 Ni1 N6 95.75(13) . . ?
N1 Ni1 N6 87.98(14) . . ?
N2 Ni1 N6 88.19(14) . . ?
O5 Ni1 O13 98.37(11) . . ?
O2 Ni1 O13 84.83(12) . . ?
N1 Ni1 O13 85.88(13) . . ?
N2 Ni1 O13 92.40(13) . . ?
N6 Ni1 O13 173.81(13) . . ?
O5 Ni1 Dy1 39.46(7) . . ?
O2 Ni1 Dy1 39.22(7) . . ?
N1 Ni1 Dy1 126.18(11) . . ?
N2 Ni1 Dy1 130.79(11) . . ?
N6 Ni1 Dy1 88.00(10) . . ?
O13 Ni1 Dy1 96.25(9) . . ?
O2 C1 C2 118.6(4) . . ?
O2 C1 C6 123.0(4) . . ?
C2 C1 C6 118.4(4) . . ?
C3 C2 O1 124.6(5) . . ?
C3 C2 C1 121.8(5) . . ?
O1 C2 C1 113.6(4) . . ?
C2 C3 C4 118.8(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 120.9(5) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 121.3(6) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 118.6(5) . . ?
C5 C6 C7 117.6(5) . . ?
C1 C6 C7 123.2(4) . . ?
N1 C7 C6 125.5(4) . . ?
N1 C7 H7 117.3 . . ?
C6 C7 H7 117.3 . . ?
O3 C8 C9 116.8(4) . . ?
O3 C8 H8A 108.1 . . ?
C9 C8 H8A 108.1 . . ?
O3 C8 H8B 108.1 . . ?
C9 C8 H8B 108.1 . . ?
H8A C8 H8B 107.3 . . ?
O4 C9 C8 112.7(4) . . ?
O4 C9 H9A 109.0 . . ?
C8 C9 H9A 109.0 . . ?
O4 C9 H9B 109.0 . . ?
C8 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
N2 C10 C11 126.4(4) . . ?
N2 C10 H10 116.8 . . ?
C11 C10 H10 116.8 . . ?
C16 C11 C12 119.2(4) . . ?
C16 C11 C10 124.6(4) . . ?
C12 C11 C10 116.2(4) . . ?
C13 C12 C11 121.3(5) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 120.3(4) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 119.1(5) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 O6 124.7(4) . . ?
C14 C15 C16 122.1(4) . . ?
O6 C15 C16 113.2(3) . . ?
O5 C16 C11 125.0(3) . . ?
O5 C16 C15 117.0(3) . . ?
C11 C16 C15 118.0(4) . . ?
O1 C17 H17A 109.5 . . ?
O1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 C19 178.7(5) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N7 C22 C21 177.3(10) . . ?
C7 N1 O3 112.4(4) . . ?
C7 N1 Ni1 128.2(3) . . ?
O3 N1 Ni1 116.9(3) . . ?
C10 N2 O4 110.0(3) . . ?
C10 N2 Ni1 125.5(3) . . ?
O4 N2 Ni1 123.8(3) . . ?
O7 N3 O8 121.9(4) . . ?
O7 N3 O9 121.5(4) . . ?
O8 N3 O9 116.6(4) . . ?
O10 N4 O11 122.1(4) . . ?
O10 N4 O12 122.1(5) . . ?
O11 N4 O12 115.9(4) . . ?
O14 N5 O13 122.3(4) . . ?
O14 N5 O15 121.6(4) . 2_564 ?
O13 N5 O15 116.2(3) . 2_564 ?
C20 N6 Ni1 172.3(4) . . ?
C2 O1 C17 117.1(4) . . ?
C2 O1 Dy1 117.0(2) . . ?
C17 O1 Dy1 120.5(3) . . ?
C1 O2 Ni1 128.1(2) . . ?
C1 O2 Dy1 124.5(2) . . ?
Ni1 O2 Dy1 106.95(11) . . ?
C8 O3 N1 112.7(3) . . ?
N2 O4 C9 111.9(3) . . ?
C16 O5 Ni1 126.6(2) . . ?
C16 O5 Dy1 126.2(2) . . ?
Ni1 O5 Dy1 106.78(11) . . ?
C15 O6 C18 115.7(3) . . ?
C15 O6 Dy1 118.3(2) . . ?
C18 O6 Dy1 126.0(3) . . ?
N3 O8 Dy1 94.2(2) . . ?
N3 O9 Dy1 97.7(2) . . ?
N4 O11 Dy1 95.1(3) . . ?
N4 O12 Dy1 97.2(3) . . ?
N5 O13 Ni1 125.1(3) . . ?
N5 O15 Dy1 129.4(2) 2_565 . ?

_refine_diff_density_max         0.432
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.050

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1408414'
_audit_update_record             
;
2015-08-06 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H32 N5 Ni O17 Tb'
_chemical_formula_weight         868.16

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

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

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

_cell_length_a                   10.0281(14)
_cell_length_b                   12.0551(17)
_cell_length_c                   15.254(2)
_cell_angle_alpha                71.779(2)
_cell_angle_beta                 86.572(2)
_cell_angle_gamma                68.175(2)
_cell_volume                     1622.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7733
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      27.29

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_F_000             868
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    2.823
_shelx_estimated_absorpt_T_min   0.602
_shelx_estimated_absorpt_T_max   0.661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_process_details   'SADABS; Bruker, 2013'

_exptl_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            13045
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.408
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             6270
_reflns_number_gt                5741
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0569P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0157(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6270
_refine_ls_number_parameters     429
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      5.884
_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 0.30651(2) 0.24026(2) 0.69668(2) 0.03440(10) Uani 1 1 d . . . . .
Ni1 Ni 0.63320(5) 0.01051(4) 0.73939(3) 0.03224(12) Uani 1 1 d . . . . .
C1 C 0.5559(4) 0.2090(3) 0.5555(2) 0.0340(7) Uani 1 1 d . . . . .
C2 C 0.4616(4) 0.3297(3) 0.5043(2) 0.0389(8) Uani 1 1 d . . . . .
C3 C 0.5002(6) 0.4016(4) 0.4262(3) 0.0531(11) Uani 1 1 d . . . . .
H3 H 0.4356 0.4810 0.3934 0.064 Uiso 1 1 calc R U . . .
C4 C 0.6395(6) 0.3532(5) 0.3963(3) 0.0604(12) Uani 1 1 d . . . . .
H4 H 0.6678 0.4009 0.3434 0.073 Uiso 1 1 calc R U . . .
C5 C 0.7319(5) 0.2377(5) 0.4442(3) 0.0559(11) Uani 1 1 d . . . . .
H5 H 0.8231 0.2065 0.4233 0.067 Uiso 1 1 calc R U . . .
C6 C 0.6940(4) 0.1635(4) 0.5249(2) 0.0429(8) Uani 1 1 d . . . . .
C7 C 0.8013(5) 0.0399(4) 0.5725(3) 0.0520(10) Uani 1 1 d . . . . .
H7 H 0.8783 0.0055 0.5397 0.062 Uiso 1 1 calc R U . . .
C8 C 1.0065(7) -0.1644(7) 0.7486(4) 0.092(2) Uani 1 1 d . . . . .
H8A H 1.0719 -0.1238 0.7186 0.110 Uiso 1 1 calc R U . . .
H8B H 1.0628 -0.2539 0.7717 0.110 Uiso 1 1 calc R U . . .
C9 C 0.9587(5) -0.1225(5) 0.8280(4) 0.0698(14) Uani 1 1 d . . . . .
H9A H 1.0439 -0.1351 0.8627 0.084 Uiso 1 1 calc R U . . .
H9B H 0.9049 -0.0325 0.8051 0.084 Uiso 1 1 calc R U . . .
C10 C 0.6611(5) -0.1518(4) 0.9367(3) 0.0485(9) Uani 1 1 d . . . . .
H10 H 0.7167 -0.2114 0.9893 0.058 Uiso 1 1 calc R U . . .
C11 C 0.5063(4) -0.1123(4) 0.9399(2) 0.0415(8) Uani 1 1 d . . . . .
C12 C 0.4528(6) -0.1838(4) 1.0159(3) 0.0574(11) Uani 1 1 d . . . . .
H12 H 0.5168 -0.2527 1.0603 0.069 Uiso 1 1 calc R U . . .
C13 C 0.3085(6) -0.1519(5) 1.0240(3) 0.0649(13) Uani 1 1 d . . . . .
H13 H 0.2749 -0.1998 1.0738 0.078 Uiso 1 1 calc R U . . .
C14 C 0.2114(6) -0.0497(5) 0.9593(3) 0.0595(12) Uani 1 1 d . . . . .
H14 H 0.1130 -0.0281 0.9656 0.071 Uiso 1 1 calc R U . . .
C15 C 0.2623(4) 0.0199(4) 0.8854(3) 0.0433(8) Uani 1 1 d . . . . .
C16 C 0.4083(4) -0.0090(3) 0.8744(2) 0.0374(8) Uani 1 1 d . . . . .
C17 C 0.2177(6) 0.4844(4) 0.4859(3) 0.0672(13) Uani 1 1 d . . . . .
H17A H 0.2497 0.5525 0.4778 0.101 Uiso 1 1 calc R U . . .
H17B H 0.1300 0.4995 0.5173 0.101 Uiso 1 1 calc R U . . .
H17C H 0.2009 0.4783 0.4266 0.101 Uiso 1 1 calc R U . . .
C18 C 0.0248(5) 0.1799(6) 0.8336(5) 0.0862(18) Uani 1 1 d . . . . .
H18A H -0.0252 0.1278 0.8285 0.129 Uiso 1 1 calc R U . . .
H18B H -0.0179 0.2620 0.7892 0.129 Uiso 1 1 calc R U . . .
H18C H 0.0181 0.1871 0.8948 0.129 Uiso 1 1 calc R U . . .
C19 C 0.5557(8) -0.1369(5) 0.6291(3) 0.0806(18) Uani 1 1 d . . . . .
H19A H 0.6235 -0.1128 0.5880 0.121 Uiso 1 1 calc R U . . .
H19B H 0.4596 -0.0818 0.6046 0.121 Uiso 1 1 calc R U . . .
H19C H 0.5683 -0.2219 0.6353 0.121 Uiso 1 1 calc R U . . .
C20 C 0.6057(8) 0.3248(8) 0.1602(5) 0.092(2) Uani 1 1 d . . . . .
H20A H 0.6245 0.2768 0.2247 0.137 Uiso 1 1 calc R U . . .
H20B H 0.6736 0.3654 0.1417 0.137 Uiso 1 1 calc R U . . .
H20C H 0.6149 0.2697 0.1245 0.137 Uiso 1 1 calc R U . . .
C21 C 0.4613(7) 0.4188(6) 0.1450(6) 0.0927(19) Uani 1 1 d . . . . .
H21A H 0.4501 0.4711 0.1841 0.111 Uiso 1 1 calc R U . . .
H21B H 0.4455 0.4723 0.0811 0.111 Uiso 1 1 calc R U . . .
C22 C 0.2135(8) 0.4505(7) 0.1576(6) 0.106(2) Uani 1 1 d . . . . .
H22A H 0.1535 0.4043 0.1880 0.127 Uiso 1 1 calc R U . . .
H22B H 0.2103 0.5076 0.1912 0.127 Uiso 1 1 calc R U . . .
C23 C 0.1532(10) 0.5225(10) 0.0672(7) 0.141(3) Uani 1 1 d . . . . .
H23A H 0.1918 0.5859 0.0374 0.212 Uiso 1 1 d R U . . .
H23B H 0.0523 0.5619 0.0741 0.212 Uiso 1 1 d R U . . .
H23C H 0.1666 0.4681 0.0302 0.212 Uiso 1 1 d R U . . .
N1 N 0.7968(3) -0.0240(3) 0.6559(2) 0.0454(7) Uani 1 1 d . . . . .
N2 N 0.7275(3) -0.1115(3) 0.8676(2) 0.0446(7) Uani 1 1 d . . . . .
N3 N 0.6230(3) 0.2676(3) 0.74420(19) 0.0369(6) Uani 1 1 d . . . . .
N4 N 0.1927(4) 0.4309(4) 0.7849(3) 0.0551(9) Uani 1 1 d . . . . .
N5 N 0.1052(5) 0.1959(5) 0.6029(4) 0.0785(13) Uani 1 1 d . . . . .
O1 O 0.3272(3) 0.3675(2) 0.54044(18) 0.0477(6) Uani 1 1 d . . . . .
O2 O 0.5076(3) 0.1444(2) 0.62836(16) 0.0352(5) Uani 1 1 d . . . . .
O3 O 0.9086(4) -0.1465(3) 0.6812(3) 0.0805(11) Uani 1 1 d . . . . .
O4 O 0.8772(4) -0.1741(4) 0.8884(2) 0.0866(13) Uani 1 1 d . . . . .
O5 O 0.4497(3) 0.0641(2) 0.80173(17) 0.0377(5) Uani 1 1 d . . . . .
O6 O 0.1757(3) 0.1235(3) 0.8159(2) 0.0543(7) Uani 1 1 d . . . . .
O7 O 0.6839(3) 0.3359(3) 0.7506(2) 0.0619(8) Uani 1 1 d . . . . .
O8 O 0.6934(3) 0.1523(2) 0.75971(19) 0.0430(6) Uani 1 1 d . . . . .
O9 O 0.4891(3) 0.3148(2) 0.7243(2) 0.0482(6) Uani 1 1 d . . . . .
O10 O 0.1603(6) 0.5157(4) 0.8187(3) 0.1003(14) Uani 1 1 d . . . . .
O11 O 0.2466(4) 0.3169(3) 0.8328(2) 0.0611(8) Uani 1 1 d . . . . .
O12 O 0.1752(4) 0.4519(3) 0.6987(2) 0.0637(8) Uani 1 1 d . . . . .
O13 O 0.0163(6) 0.1757(7) 0.5675(5) 0.146(2) Uani 1 1 d . . . . .
O14 O 0.0752(4) 0.2958(3) 0.6237(3) 0.0698(9) Uani 1 1 d . . . . .
O15 O 0.2316(4) 0.1187(4) 0.6235(3) 0.0749(10) Uani 1 1 d . . . . .
O16 O 0.5789(4) -0.1281(3) 0.71631(19) 0.0540(7) Uani 1 1 d D . . . .
H16A H 0.5986 -0.1977 0.7579 0.065 Uiso 1 1 d R U . . .
O17 O 0.3595(4) 0.3622(3) 0.1648(3) 0.0731(9) Uani 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
Tb1 O5 2.240(2) . ?
Tb1 O2 2.293(2) . ?
Tb1 O14 2.399(3) . ?
Tb1 O12 2.407(3) . ?
Tb1 O9 2.427(3) . ?
Tb1 O15 2.428(3) . ?
Tb1 O1 2.443(3) . ?
Tb1 O11 2.483(3) . ?
Tb1 O6 2.548(3) . ?
Tb1 Ni1 3.3479(6) . ?
Ni1 O5 1.999(2) . ?
Ni1 N1 2.015(3) . ?
Ni1 O2 2.024(2) . ?
Ni1 N2 2.067(3) . ?
Ni1 O16 2.070(3) . ?
Ni1 O8 2.122(2) . ?
C1 O2 1.323(4) . ?
C1 C6 1.399(5) . ?
C1 C2 1.406(5) . ?
C2 C3 1.366(5) . ?
C2 O1 1.394(5) . ?
C3 C4 1.409(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.347(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.402(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.459(6) . ?
C7 N1 1.273(5) . ?
C7 H7 0.9300 . ?
C8 O3 1.375(7) . ?
C8 C9 1.443(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O4 1.354(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.276(5) . ?
C10 C11 1.448(6) . ?
C10 H10 0.9300 . ?
C11 C16 1.395(5) . ?
C11 C12 1.420(5) . ?
C12 C13 1.361(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.379(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(5) . ?
C14 H14 0.9300 . ?
C15 O6 1.383(5) . ?
C15 C16 1.387(5) . ?
C16 O5 1.336(4) . ?
C17 O1 1.452(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O6 1.459(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 O16 1.406(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.446(9) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O17 1.397(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.408(11) . ?
C22 O17 1.440(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N1 O3 1.432(4) . ?
N2 O4 1.410(4) . ?
N3 O7 1.221(4) . ?
N3 O8 1.254(4) . ?
N3 O9 1.261(4) . ?
N4 O10 1.215(5) . ?
N4 O11 1.257(5) . ?
N4 O12 1.268(5) . ?
N5 O13 1.202(6) . ?
N5 O15 1.249(6) . ?
N5 O14 1.264(6) . ?
O16 H16A 0.8388 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Tb1 O2 70.82(8) . . ?
O5 Tb1 O14 131.94(11) . . ?
O2 Tb1 O14 118.17(11) . . ?
O5 Tb1 O12 133.67(10) . . ?
O2 Tb1 O12 135.18(10) . . ?
O14 Tb1 O12 75.96(13) . . ?
O5 Tb1 O9 81.38(9) . . ?
O2 Tb1 O9 73.35(9) . . ?
O14 Tb1 O9 146.21(11) . . ?
O12 Tb1 O9 75.05(11) . . ?
O5 Tb1 O15 91.13(12) . . ?
O2 Tb1 O15 75.87(11) . . ?
O14 Tb1 O15 52.31(13) . . ?
O12 Tb1 O15 127.99(13) . . ?
O9 Tb1 O15 149.10(12) . . ?
O5 Tb1 O1 136.30(9) . . ?
O2 Tb1 O1 66.29(8) . . ?
O14 Tb1 O1 78.05(11) . . ?
O12 Tb1 O1 77.09(10) . . ?
O9 Tb1 O1 78.88(10) . . ?
O15 Tb1 O1 86.45(12) . . ?
O5 Tb1 O11 83.03(10) . . ?
O2 Tb1 O11 138.38(10) . . ?
O14 Tb1 O11 103.42(13) . . ?
O12 Tb1 O11 51.83(11) . . ?
O9 Tb1 O11 71.11(11) . . ?
O15 Tb1 O11 137.98(13) . . ?
O1 Tb1 O11 125.34(10) . . ?
O5 Tb1 O6 64.91(9) . . ?
O2 Tb1 O6 124.41(9) . . ?
O14 Tb1 O6 74.17(11) . . ?
O12 Tb1 O6 100.07(11) . . ?
O9 Tb1 O6 127.97(10) . . ?
O15 Tb1 O6 73.19(12) . . ?
O1 Tb1 O6 151.87(10) . . ?
O11 Tb1 O6 66.65(11) . . ?
O5 Tb1 Ni1 35.39(6) . . ?
O2 Tb1 Ni1 36.31(6) . . ?
O14 Tb1 Ni1 140.33(9) . . ?
O12 Tb1 Ni1 143.17(9) . . ?
O9 Tb1 Ni1 68.59(6) . . ?
O15 Tb1 Ni1 88.03(9) . . ?
O1 Tb1 Ni1 100.92(7) . . ?
O11 Tb1 Ni1 108.64(8) . . ?
O6 Tb1 Ni1 97.63(7) . . ?
O5 Ni1 N1 169.94(12) . . ?
O5 Ni1 O2 81.52(10) . . ?
N1 Ni1 O2 88.52(12) . . ?
O5 Ni1 N2 87.24(12) . . ?
N1 Ni1 N2 102.76(13) . . ?
O2 Ni1 N2 168.56(11) . . ?
O5 Ni1 O16 89.45(12) . . ?
N1 Ni1 O16 89.53(13) . . ?
O2 Ni1 O16 92.33(11) . . ?
N2 Ni1 O16 89.71(12) . . ?
O5 Ni1 O8 92.22(10) . . ?
N1 Ni1 O8 88.71(12) . . ?
O2 Ni1 O8 87.31(10) . . ?
N2 Ni1 O8 90.99(12) . . ?
O16 Ni1 O8 178.21(12) . . ?
O5 Ni1 Tb1 40.45(7) . . ?
N1 Ni1 Tb1 129.97(10) . . ?
O2 Ni1 Tb1 42.14(7) . . ?
N2 Ni1 Tb1 126.42(9) . . ?
O16 Ni1 Tb1 98.41(9) . . ?
O8 Ni1 Tb1 82.49(7) . . ?
O2 C1 C6 124.1(3) . . ?
O2 C1 C2 118.1(3) . . ?
C6 C1 C2 117.8(3) . . ?
C3 C2 O1 124.0(4) . . ?
C3 C2 C1 122.3(4) . . ?
O1 C2 C1 113.7(3) . . ?
C2 C3 C4 118.8(4) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 121.7(4) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 119.3(4) . . ?
C1 C6 C7 122.8(3) . . ?
C5 C6 C7 117.9(4) . . ?
N1 C7 C6 124.5(4) . . ?
N1 C7 H7 117.7 . . ?
C6 C7 H7 117.7 . . ?
O3 C8 C9 120.6(5) . . ?
O3 C8 H8A 107.2 . . ?
C9 C8 H8A 107.2 . . ?
O3 C8 H8B 107.2 . . ?
C9 C8 H8B 107.2 . . ?
H8A C8 H8B 106.8 . . ?
O4 C9 C8 120.0(5) . . ?
O4 C9 H9A 107.3 . . ?
C8 C9 H9A 107.3 . . ?
O4 C9 H9B 107.3 . . ?
C8 C9 H9B 107.3 . . ?
H9A C9 H9B 106.9 . . ?
N2 C10 C11 125.3(3) . . ?
N2 C10 H10 117.4 . . ?
C11 C10 H10 117.4 . . ?
C16 C11 C12 118.8(4) . . ?
C16 C11 C10 124.3(3) . . ?
C12 C11 C10 116.9(4) . . ?
C13 C12 C11 120.4(4) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 121.0(4) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C15 C14 C13 119.0(4) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 O6 124.4(4) . . ?
C14 C15 C16 122.0(4) . . ?
O6 C15 C16 113.7(3) . . ?
O5 C16 C15 118.6(3) . . ?
O5 C16 C11 122.5(3) . . ?
C15 C16 C11 118.9(3) . . ?
O1 C17 H17A 109.5 . . ?
O1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O16 C19 H19A 109.5 . . ?
O16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O17 C21 C20 110.8(5) . . ?
O17 C21 H21A 109.5 . . ?
C20 C21 H21A 109.5 . . ?
O17 C21 H21B 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
C23 C22 O17 115.9(7) . . ?
C23 C22 H22A 108.3 . . ?
O17 C22 H22A 108.3 . . ?
C23 C22 H22B 108.3 . . ?
O17 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C22 C23 H23A 113.6 . . ?
C22 C23 H23B 105.0 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.7 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C7 N1 O3 112.1(3) . . ?
C7 N1 Ni1 127.7(3) . . ?
O3 N1 Ni1 118.6(3) . . ?
C10 N2 O4 109.4(3) . . ?
C10 N2 Ni1 125.8(3) . . ?
O4 N2 Ni1 124.5(3) . . ?
O7 N3 O8 119.7(3) . . ?
O7 N3 O9 118.8(3) . . ?
O8 N3 O9 121.5(3) . . ?
O10 N4 O11 122.3(4) . . ?
O10 N4 O12 122.0(4) . . ?
O11 N4 O12 115.6(4) . . ?
O13 N5 O15 122.4(6) . . ?
O13 N5 O14 121.9(6) . . ?
O15 N5 O14 115.7(4) . . ?
C2 O1 C17 117.3(3) . . ?
C2 O1 Tb1 116.2(2) . . ?
C17 O1 Tb1 126.2(3) . . ?
C1 O2 Ni1 124.5(2) . . ?
C1 O2 Tb1 121.7(2) . . ?
Ni1 O2 Tb1 101.55(10) . . ?
C8 O3 N1 113.3(4) . . ?
C9 O4 N2 114.6(4) . . ?
C16 O5 Ni1 125.9(2) . . ?
C16 O5 Tb1 126.7(2) . . ?
Ni1 O5 Tb1 104.16(10) . . ?
C15 O6 C18 117.0(4) . . ?
C15 O6 Tb1 115.9(2) . . ?
C18 O6 Tb1 123.7(3) . . ?
N3 O8 Ni1 130.4(2) . . ?
N3 O9 Tb1 136.3(2) . . ?
N4 O11 Tb1 94.1(2) . . ?
N4 O12 Tb1 97.5(2) . . ?
N5 O14 Tb1 96.4(3) . . ?
N5 O15 Tb1 95.5(3) . . ?
C19 O16 Ni1 125.5(3) . . ?
C19 O16 H16A 111.6 . . ?
Ni1 O16 H16A 119.4 . . ?
C21 O17 C22 113.6(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O16 H16A O17 0.84 1.86 2.696(4) 170.9 2_656
C18 H18B O14 0.96 2.60 3.162(8) 117.5 .
C10 H10 O11 0.93 2.59 3.438(5) 151.1 2_657
C9 H9B O8 0.97 2.37 3.280(6) 155.1 .
C8 H8B O10 0.97 2.45 3.405(8) 168.0 1_645
C3 H3 O7 0.93 2.54 3.407(5) 155.5 2_666
C18 H18B O14 0.96 2.60 3.162(8) 117.5 .
C10 H10 O11 0.93 2.59 3.438(5) 151.1 2_657
C9 H9B O8 0.97 2.37 3.280(6) 155.1 .
C8 H8B O10 0.97 2.45 3.405(8) 168.0 1_645
C3 H3 O7 0.93 2.54 3.407(5) 155.5 2_666
C18 H18B O14 0.96 2.60 3.162(8) 117.5 .
C10 H10 O11 0.93 2.59 3.438(5) 151.1 2_657
C9 H9B O8 0.97 2.37 3.280(6) 155.1 .
C8 H8B O10 0.97 2.45 3.405(8) 168.0 1_645
C3 H3 O7 0.93 2.54 3.407(5) 155.5 2_666
C21 H21A O7 0.97 2.68 3.588(8) 156.1 2_666
C18 H18B O14 0.96 2.60 3.162(8) 117.5 .
C17 H17B O12 0.96 2.67 3.168(6) 112.5 .
C10 H10 O11 0.93 2.59 3.438(5) 151.1 2_657
C9 H9B O8 0.97 2.37 3.280(6) 155.1 .
C8 H8B O10 0.97 2.45 3.405(8) 168.0 1_645
C3 H3 O7 0.93 2.54 3.407(5) 155.5 2_666
C3 H3 O7 0.93 2.54 3.407(5) 155.5 2_666
C8 H8B O10 0.97 2.45 3.405(8) 168.0 1_645
C9 H9B O8 0.97 2.37 3.280(6) 155.1 .
C10 H10 O11 0.93 2.59 3.438(5) 151.1 2_657
C17 H17B O12 0.96 2.67 3.168(6) 112.5 .
C18 H18B O14 0.96 2.60 3.162(8) 117.5 .
C21 H21A O7 0.97 2.68 3.588(8) 156.1 2_666
C3 H3 O7 0.93 2.54 3.407(5) 155.5 2_666
C8 H8B O10 0.97 2.45 3.405(8) 168.0 1_645
C9 H9B O8 0.97 2.37 3.280(6) 155.1 .
C10 H10 O11 0.93 2.59 3.438(5) 151.1 2_657
C17 H17B O12 0.96 2.67 3.168(6) 112.5 .
C18 H18B O14 0.96 2.60 3.162(8) 117.5 .
C21 H21A O7 0.97 2.68 3.588(8) 156.1 2_666
C3 H3 O7 0.93 2.54 3.407(5) 155.5 2_666
C8 H8B O10 0.97 2.45 3.405(8) 168.0 1_645
C9 H9B O8 0.97 2.37 3.280(6) 155.1 .
C10 H10 O11 0.93 2.59 3.438(5) 151.1 2_657
C18 H18B O14 0.96 2.60 3.162(8) 117.5 .
C3 H3 O7 0.93 2.54 3.407(5) 155.5 2_666
C8 H8B O10 0.97 2.45 3.405(8) 168.0 1_645
C9 H9B O8 0.97 2.37 3.280(6) 155.1 .
C10 H10 O11 0.93 2.59 3.438(5) 151.1 2_657
C18 H18B O14 0.96 2.60 3.162(8) 117.5 .

_refine_diff_density_max         1.080
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.103

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1408415'
_audit_update_record             
;
2015-08-06 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H32 Dy N5 Ni O17'
_chemical_formula_weight         871.74

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

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

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

_cell_length_a                   10.0241(17)
_cell_length_b                   12.042(2)
_cell_length_c                   15.270(3)
_cell_angle_alpha                71.869(2)
_cell_angle_beta                 86.592(3)
_cell_angle_gamma                68.157(2)
_cell_volume                     1622.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6794
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      27.32

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_F_000             870
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.946
_shelx_estimated_absorpt_T_min   0.619
_shelx_estimated_absorpt_T_max   0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_process_details   'SADABS; Bruker, 2013'

_exptl_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            12929
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.918
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             6278
_reflns_number_gt                5635
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0882P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6278
_refine_ls_number_parameters     429
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.1108
_refine_ls_wR_factor_gt          0.1062
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_restrained_S_all      0.904
_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
Dy1 Dy 0.19352(2) 0.25924(2) 0.80273(2) 0.03325(10) Uani 1 1 d . . . . .
Ni1 Ni -0.13314(5) 0.48858(4) 0.76078(3) 0.02906(13) Uani 1 1 d . . . . .
C1 C -0.0552(4) 0.2904(4) 0.9441(3) 0.0303(8) Uani 1 1 d . . . . .
C2 C 0.0385(5) 0.1704(4) 0.9953(3) 0.0368(9) Uani 1 1 d . . . . .
C3 C -0.0005(6) 0.0985(5) 1.0740(3) 0.0491(12) Uani 1 1 d . . . . .
H3 H 0.0646 0.0196 1.1073 0.059 Uiso 1 1 calc R U . . .
C4 C -0.1394(7) 0.1457(6) 1.1033(4) 0.0612(15) Uani 1 1 d . . . . .
H4 H -0.1679 0.0969 1.1553 0.073 Uiso 1 1 calc R U . . .
C5 C -0.2326(6) 0.2624(6) 1.0560(4) 0.0523(12) Uani 1 1 d . . . . .
H5 H -0.3234 0.2940 1.0774 0.063 Uiso 1 1 calc R U . . .
C6 C -0.1944(5) 0.3364(5) 0.9751(3) 0.0405(10) Uani 1 1 d . . . . .
C7 C -0.3009(5) 0.4602(5) 0.9273(3) 0.0481(12) Uani 1 1 d . . . . .
H7 H -0.3776 0.4949 0.9603 0.058 Uiso 1 1 calc R U . . .
C8 C -0.5058(7) 0.6653(7) 0.7519(5) 0.083(2) Uani 1 1 d . . . . .
H8A H -0.5586 0.7554 0.7275 0.099 Uiso 1 1 calc R U . . .
H8B H -0.5743 0.6284 0.7817 0.099 Uiso 1 1 calc R U . . .
C9 C -0.4587(6) 0.6201(6) 0.6745(5) 0.0639(15) Uani 1 1 d . . . . .
H9A H -0.4035 0.5303 0.6986 0.077 Uiso 1 1 calc R U . . .
H9B H -0.5437 0.6304 0.6407 0.077 Uiso 1 1 calc R U . . .
C10 C -0.1611(5) 0.6499(4) 0.5636(3) 0.0458(11) Uani 1 1 d . . . . .
H10 H -0.2168 0.7086 0.5109 0.055 Uiso 1 1 calc R U . . .
C11 C -0.0072(5) 0.6118(4) 0.5604(3) 0.0377(9) Uani 1 1 d . . . . .
C12 C 0.0469(7) 0.6828(6) 0.4839(3) 0.0565(13) Uani 1 1 d . . . . .
H12 H -0.0172 0.7515 0.4395 0.068 Uiso 1 1 calc R U . . .
C13 C 0.1905(7) 0.6511(6) 0.4752(3) 0.0634(15) Uani 1 1 d . . . . .
H13 H 0.2243 0.6977 0.4247 0.076 Uiso 1 1 calc R U . . .
C14 C 0.2876(6) 0.5491(6) 0.5417(4) 0.0568(13) Uani 1 1 d . . . . .
H14 H 0.3861 0.5285 0.5361 0.068 Uiso 1 1 calc R U . . .
C15 C 0.2386(5) 0.4798(4) 0.6146(3) 0.0408(10) Uani 1 1 d . . . . .
C16 C 0.0908(5) 0.5080(4) 0.6261(3) 0.0331(8) Uani 1 1 d . . . . .
C17 C 0.2840(6) 0.0166(5) 1.0127(4) 0.0635(16) Uani 1 1 d . . . . .
H17A H 0.3087 0.0263 1.0689 0.095 Uiso 1 1 calc R U . . .
H17B H 0.3679 -0.0030 0.9779 0.095 Uiso 1 1 calc R U . . .
H17C H 0.2486 -0.0506 1.0271 0.095 Uiso 1 1 calc R U . . .
C18 C 0.4739(6) 0.3217(7) 0.6645(6) 0.081(2) Uani 1 1 d . . . . .
H18A H 0.4793 0.3158 0.6031 0.122 Uiso 1 1 calc R U . . .
H18B H 0.5190 0.2393 0.7080 0.122 Uiso 1 1 calc R U . . .
H18C H 0.5227 0.3749 0.6696 0.122 Uiso 1 1 calc R U . . .
C19 C -0.0584(9) 0.6385(7) 0.8715(4) 0.0737(19) Uani 1 1 d . . . . .
H19A H -0.1499 0.6711 0.8963 0.111 Uiso 1 1 calc R U . . .
H19B H -0.0078 0.6941 0.8655 0.111 Uiso 1 1 calc R U . . .
H19C H -0.0026 0.5566 0.9123 0.111 Uiso 1 1 calc R U . . .
C20 C 1.1075(9) 0.8231(9) 0.6590(6) 0.087(2) Uani 1 1 d . . . . .
H20A H 1.1234 0.7708 0.7224 0.131 Uiso 1 1 calc R U . . .
H20B H 1.1753 0.8644 0.6455 0.131 Uiso 1 1 calc R U . . .
H20C H 1.1201 0.7720 0.6196 0.131 Uiso 1 1 calc R U . . .
C21 C 0.9621(8) 0.9168(7) 0.6435(7) 0.093(2) Uani 1 1 d . . . . .
H21A H 0.9507 0.9695 0.6824 0.112 Uiso 1 1 calc R U . . .
H21B H 0.9471 0.9703 0.5797 0.112 Uiso 1 1 calc R U . . .
C22 C 0.7114(8) 0.9503(7) 0.6585(6) 0.095(2) Uani 1 1 d D . . . .
H22A H 0.6528 0.9032 0.6897 0.115 Uiso 1 1 calc R U . . .
H22B H 0.7086 1.0079 0.6917 0.115 Uiso 1 1 calc R U . . .
C23 C 0.6516(12) 1.0202(12) 0.5684(7) 0.162(5) Uani 1 1 d D . . . .
H23A H 0.5498 1.0633 0.5699 0.243 Uiso 1 1 calc R U . . .
H23B H 0.6686 0.9647 0.5320 0.243 Uiso 1 1 calc R U . . .
H23C H 0.6954 1.0807 0.5416 0.243 Uiso 1 1 calc R U . . .
N1 N -0.2974(4) 0.5238(4) 0.8451(3) 0.0432(9) Uani 1 1 d . . . . .
N2 N -0.2276(4) 0.6099(3) 0.6330(2) 0.0385(8) Uani 1 1 d . . . . .
N3 N 0.3958(6) 0.3034(6) 0.8962(4) 0.0759(15) Uani 1 1 d . . . . .
N4 N 0.3075(5) 0.0679(4) 0.7143(3) 0.0506(10) Uani 1 1 d . . . . .
N5 N -0.1224(4) 0.2317(3) 0.7554(2) 0.0331(7) Uani 1 1 d . . . . .
O1 O -0.0071(3) 0.3554(3) 0.87141(18) 0.0325(6) Uani 1 1 d . . . . .
O2 O -0.4084(5) 0.6461(4) 0.8194(3) 0.0743(13) Uani 1 1 d . . . . .
O3 O -0.3767(4) 0.6730(5) 0.6114(3) 0.0804(14) Uani 1 1 d . . . . .
O4 O 0.0504(3) 0.4356(3) 0.6981(2) 0.0354(6) Uani 1 1 d . . . . .
O5 O 0.1735(3) 0.1328(3) 0.9585(2) 0.0438(7) Uani 1 1 d . . . . .
O6 O 0.3250(3) 0.3746(3) 0.6841(3) 0.0510(8) Uani 1 1 d . . . . .
O7 O 0.4853(7) 0.3242(8) 0.9303(6) 0.140(3) Uani 1 1 d . . . . .
O8 O 0.2692(4) 0.3795(4) 0.8776(3) 0.0716(12) Uani 1 1 d . . . . .
O9 O 0.4258(4) 0.2030(4) 0.8759(3) 0.0701(11) Uani 1 1 d . . . . .
O10 O 0.3417(6) -0.0163(4) 0.6816(4) 0.0918(16) Uani 1 1 d . . . . .
O11 O 0.3250(4) 0.0474(3) 0.7984(3) 0.0606(10) Uani 1 1 d . . . . .
O12 O 0.2535(4) 0.1816(3) 0.6671(2) 0.0566(9) Uani 1 1 d . . . . .
O13 O -0.1853(4) 0.1638(3) 0.7495(3) 0.0565(9) Uani 1 1 d . . . . .
O14 O 0.0120(3) 0.1851(3) 0.7746(2) 0.0435(7) Uani 1 1 d . . . . .
O15 O -0.1935(3) 0.3468(3) 0.7406(2) 0.0393(7) Uani 1 1 d . . . . .
O16 O -0.0804(4) 0.6290(3) 0.7826(2) 0.0511(8) Uani 1 1 d . . . . .
H16A H -0.0995 0.7043 0.7329 0.061 Uiso 1 1 d R U . . .
O17 O 0.8592(5) 0.8631(4) 0.6622(3) 0.0711(11) 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
Dy1 O4 2.239(3) . ?
Dy1 O1 2.293(3) . ?
Dy1 O9 2.407(4) . ?
Dy1 O14 2.415(3) . ?
Dy1 O11 2.417(3) . ?
Dy1 O8 2.434(4) . ?
Dy1 O5 2.436(3) . ?
Dy1 O12 2.482(4) . ?
Dy1 O6 2.542(3) . ?
Dy1 N3 2.837(5) . ?
Dy1 N4 2.870(4) . ?
Dy1 Ni1 3.3435(7) . ?
Ni1 O4 2.002(3) . ?
Ni1 O1 2.020(3) . ?
Ni1 N1 2.029(4) . ?
Ni1 N2 2.063(4) . ?
Ni1 O16 2.071(3) . ?
Ni1 O15 2.120(3) . ?
C1 O1 1.325(5) . ?
C1 C2 1.399(6) . ?
C1 C6 1.409(6) . ?
C2 C3 1.376(6) . ?
C2 O5 1.401(6) . ?
C3 C4 1.398(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.357(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.407(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.458(7) . ?
C7 N1 1.258(6) . ?
C7 H7 0.9300 . ?
C8 O2 1.369(8) . ?
C8 C9 1.436(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O3 1.386(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.280(6) . ?
C10 C11 1.439(7) . ?
C10 H10 0.9300 . ?
C11 C16 1.399(6) . ?
C11 C12 1.427(6) . ?
C12 C13 1.355(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.392(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.356(7) . ?
C14 H14 0.9300 . ?
C15 O6 1.391(6) . ?
C15 C16 1.404(6) . ?
C16 O4 1.322(5) . ?
C17 O5 1.451(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O6 1.443(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 O16 1.434(6) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.451(11) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O17 1.383(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.401(8) . ?
C22 O17 1.455(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N1 O2 1.426(5) . ?
N2 O3 1.406(5) . ?
N3 O7 1.201(7) . ?
N3 O8 1.243(7) . ?
N3 O9 1.265(7) . ?
N4 O10 1.196(6) . ?
N4 O12 1.252(6) . ?
N4 O11 1.242(6) . ?
N5 O13 1.229(5) . ?
N5 O15 1.253(4) . ?
N5 O14 1.265(4) . ?
O16 H16A 0.9453 . ?

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 Dy1 O1 70.89(10) . . ?
O4 Dy1 O9 131.95(13) . . ?
O1 Dy1 O9 118.01(14) . . ?
O4 Dy1 O14 81.41(11) . . ?
O1 Dy1 O14 73.74(10) . . ?
O9 Dy1 O14 146.13(13) . . ?
O4 Dy1 O11 133.07(12) . . ?
O1 Dy1 O11 135.67(12) . . ?
O9 Dy1 O11 76.20(15) . . ?
O14 Dy1 O11 74.82(13) . . ?
O4 Dy1 O8 91.54(14) . . ?
O1 Dy1 O8 75.59(13) . . ?
O9 Dy1 O8 52.14(15) . . ?
O14 Dy1 O8 149.17(13) . . ?
O11 Dy1 O8 128.07(15) . . ?
O4 Dy1 O5 136.35(10) . . ?
O1 Dy1 O5 66.23(10) . . ?
O9 Dy1 O5 77.83(14) . . ?
O14 Dy1 O5 79.28(12) . . ?
O11 Dy1 O5 77.86(12) . . ?
O8 Dy1 O5 85.68(15) . . ?
O4 Dy1 O12 83.29(12) . . ?
O1 Dy1 O12 138.63(11) . . ?
O9 Dy1 O12 103.32(15) . . ?
O14 Dy1 O12 70.80(13) . . ?
O11 Dy1 O12 50.91(13) . . ?
O8 Dy1 O12 138.45(15) . . ?
O5 Dy1 O12 125.28(12) . . ?
O4 Dy1 O6 65.11(11) . . ?
O1 Dy1 O6 124.65(10) . . ?
O9 Dy1 O6 74.09(14) . . ?
O14 Dy1 O6 127.76(12) . . ?
O11 Dy1 O6 99.32(13) . . ?
O8 Dy1 O6 73.79(15) . . ?
O5 Dy1 O6 151.59(12) . . ?
O12 Dy1 O6 66.65(13) . . ?
O4 Dy1 N3 111.96(15) . . ?
O1 Dy1 N3 97.47(15) . . ?
O9 Dy1 N3 26.31(15) . . ?
O14 Dy1 N3 161.14(16) . . ?
O11 Dy1 N3 102.47(17) . . ?
O8 Dy1 N3 25.87(16) . . ?
O5 Dy1 N3 81.90(15) . . ?
O12 Dy1 N3 122.42(17) . . ?
O6 Dy1 N3 71.02(16) . . ?
O4 Dy1 N4 107.97(12) . . ?
O1 Dy1 N4 141.83(12) . . ?
O9 Dy1 N4 91.66(15) . . ?
O14 Dy1 N4 68.51(12) . . ?
O11 Dy1 N4 25.36(13) . . ?
O8 Dy1 N4 141.40(14) . . ?
O5 Dy1 N4 100.68(12) . . ?
O12 Dy1 N4 25.76(13) . . ?
O6 Dy1 N4 84.50(12) . . ?
N3 Dy1 N4 116.73(17) . . ?
O4 Dy1 Ni1 35.52(7) . . ?
O1 Dy1 Ni1 36.31(7) . . ?
O9 Dy1 Ni1 140.43(12) . . ?
O14 Dy1 Ni1 68.60(7) . . ?
O11 Dy1 Ni1 142.88(11) . . ?
O8 Dy1 Ni1 88.30(10) . . ?
O5 Dy1 Ni1 100.83(7) . . ?
O12 Dy1 Ni1 108.85(9) . . ?
O6 Dy1 Ni1 98.03(8) . . ?
N3 Dy1 Ni1 114.17(14) . . ?
N4 Dy1 Ni1 126.75(10) . . ?
O4 Ni1 O1 81.62(12) . . ?
O4 Ni1 N1 169.97(14) . . ?
O1 Ni1 N1 88.50(14) . . ?
O4 Ni1 N2 87.09(13) . . ?
O1 Ni1 N2 168.51(13) . . ?
N1 Ni1 N2 102.84(15) . . ?
O4 Ni1 O16 89.40(14) . . ?
O1 Ni1 O16 92.75(13) . . ?
N1 Ni1 O16 89.30(16) . . ?
N2 Ni1 O16 89.24(14) . . ?
O4 Ni1 O15 92.49(12) . . ?
O1 Ni1 O15 87.53(12) . . ?
N1 Ni1 O15 88.84(15) . . ?
N2 Ni1 O15 90.85(14) . . ?
O16 Ni1 O15 178.11(14) . . ?
O4 Ni1 Dy1 40.53(8) . . ?
O1 Ni1 Dy1 42.23(8) . . ?
N1 Ni1 Dy1 130.05(11) . . ?
N2 Ni1 Dy1 126.28(10) . . ?
O16 Ni1 Dy1 98.92(11) . . ?
O15 Ni1 Dy1 82.54(8) . . ?
O1 C1 C2 118.4(4) . . ?
O1 C1 C6 123.9(4) . . ?
C2 C1 C6 117.6(4) . . ?
C3 C2 C1 122.3(4) . . ?
C3 C2 O5 124.5(4) . . ?
C1 C2 O5 113.3(4) . . ?
C2 C3 C4 119.2(5) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.2(5) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 119.5(4) . . ?
C5 C6 C7 118.1(4) . . ?
C1 C6 C7 122.4(4) . . ?
N1 C7 C6 125.2(4) . . ?
N1 C7 H7 117.4 . . ?
C6 C7 H7 117.4 . . ?
O2 C8 C9 120.5(5) . . ?
O2 C8 H8A 107.2 . . ?
C9 C8 H8A 107.2 . . ?
O2 C8 H8B 107.2 . . ?
C9 C8 H8B 107.2 . . ?
H8A C8 H8B 106.8 . . ?
O3 C9 C8 119.1(6) . . ?
O3 C9 H9A 107.5 . . ?
C8 C9 H9A 107.5 . . ?
O3 C9 H9B 107.5 . . ?
C8 C9 H9B 107.5 . . ?
H9A C9 H9B 107.0 . . ?
N2 C10 C11 125.4(4) . . ?
N2 C10 H10 117.3 . . ?
C11 C10 H10 117.3 . . ?
C16 C11 C12 118.8(5) . . ?
C16 C11 C10 123.8(4) . . ?
C12 C11 C10 117.4(4) . . ?
C13 C12 C11 120.8(5) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 120.2(5) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 120.1(5) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 O6 125.2(4) . . ?
C14 C15 C16 121.9(5) . . ?
O6 C15 C16 112.9(4) . . ?
O4 C16 C15 118.8(4) . . ?
O4 C16 C11 122.9(4) . . ?
C15 C16 C11 118.3(4) . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O16 C19 H19A 109.5 . . ?
O16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O17 C21 C20 112.3(6) . . ?
O17 C21 H21A 109.2 . . ?
C20 C21 H21A 109.2 . . ?
O17 C21 H21B 109.2 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C23 C22 O17 113.5(8) . . ?
C23 C22 H22A 108.9 . . ?
O17 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
O17 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C7 N1 O2 112.8(4) . . ?
C7 N1 Ni1 127.3(3) . . ?
O2 N1 Ni1 118.2(3) . . ?
C10 N2 O3 108.8(4) . . ?
C10 N2 Ni1 125.7(3) . . ?
O3 N2 Ni1 125.1(3) . . ?
O7 N3 O8 122.3(7) . . ?
O7 N3 O9 121.6(7) . . ?
O8 N3 O9 116.1(5) . . ?
O7 N3 Dy1 175.8(6) . . ?
O8 N3 Dy1 58.7(3) . . ?
O9 N3 Dy1 57.5(3) . . ?
O10 N4 O12 123.2(5) . . ?
O10 N4 O11 121.5(5) . . ?
O12 N4 O11 115.3(4) . . ?
O10 N4 Dy1 172.1(4) . . ?
O12 N4 Dy1 59.6(2) . . ?
O11 N4 Dy1 56.5(2) . . ?
O13 N5 O15 118.8(4) . . ?
O13 N5 O14 119.8(3) . . ?
O15 N5 O14 121.4(3) . . ?
C1 O1 Ni1 124.4(2) . . ?
C1 O1 Dy1 121.5(2) . . ?
Ni1 O1 Dy1 101.45(11) . . ?
C8 O2 N1 113.9(4) . . ?
C9 O3 N2 113.3(4) . . ?
C16 O4 Ni1 126.1(3) . . ?
C16 O4 Dy1 126.9(3) . . ?
Ni1 O4 Dy1 103.95(12) . . ?
C2 O5 C17 117.4(4) . . ?
C2 O5 Dy1 116.5(2) . . ?
C17 O5 Dy1 125.9(3) . . ?
C15 O6 C18 115.4(4) . . ?
C15 O6 Dy1 116.0(3) . . ?
C18 O6 Dy1 125.5(4) . . ?
N3 O8 Dy1 95.5(4) . . ?
N3 O9 Dy1 96.2(3) . . ?
N4 O11 Dy1 98.2(3) . . ?
N4 O12 Dy1 94.7(3) . . ?
N5 O14 Dy1 136.6(2) . . ?
N5 O15 Ni1 130.3(3) . . ?
C19 O16 Ni1 124.8(3) . . ?
C19 O16 H16A 114.9 . . ?
Ni1 O16 H16A 117.5 . . ?
C21 O17 C22 115.6(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O16 H16A O17 0.95 1.78 2.707(5) 165.6 1_455
C17 H17B O11 0.96 2.64 3.195(8) 117.1 .
C10 H10 O12 0.93 2.61 3.454(6) 151.8 2_566
C9 H9A O15 0.97 2.35 3.264(6) 155.9 .
C8 H8A O10 0.97 2.43 3.385(9) 169.9 1_465
C3 H3 O13 0.93 2.54 3.411(6) 156.3 2_557

_refine_diff_density_max         0.933
_refine_diff_density_min         -2.133
_refine_diff_density_rms         0.127

_shelxl_version_number           2013-2

