# 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 1046794'
_audit_update_record             
;
2015-02-02 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H26 Dy F12 N5 Ni O10, H2 O'
_chemical_formula_sum            'C29 H28 Dy F12 N5 Ni O11'
_chemical_formula_weight         1071.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   17.8522(18)
_cell_length_b                   10.6611(14)
_cell_length_c                   19.9365(12)
_cell_angle_alpha                90
_cell_angle_beta                 106.854(2)
_cell_angle_gamma                90
_cell_volume                     3631.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      27.35

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_F_000             2108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    2.687
_shelx_estimated_absorpt_T_min   0.520
_shelx_estimated_absorpt_T_max   0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_process_details   'SADABS; Bruker, 2013'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex Duo CCD '
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30097
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.192
_diffrn_reflns_theta_max         26.999
_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             7911
_reflns_number_gt                6135
_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       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0800P)²+1.8800P]
 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         7911
_refine_ls_number_parameters     534
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.1512
_refine_ls_wR_factor_gt          0.1500
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3607(4) 0.2358(5) 0.2951(3) 0.0374(13) Uani 1 1 d . . . . .
C2 C 0.2953(4) 0.1997(5) 0.3133(3) 0.0406(13) Uani 1 1 d . . . . .
C3 C 0.2941(4) 0.2014(5) 0.3833(3) 0.0402(13) Uani 1 1 d . . . . .
H3 H 0.2484 0.1761 0.3949 0.048 Uiso 1 1 calc R U . . .
C4 C 0.3598(4) 0.2401(5) 0.4355(3) 0.0452(15) Uani 1 1 d . . . . .
H4 H 0.3591 0.2426 0.4829 0.054 Uiso 1 1 calc R U . . .
C5 C 0.4251(4) 0.2743(5) 0.4185(3) 0.0392(13) Uani 1 1 d . . . . .
H5 H 0.4697 0.3017 0.4545 0.047 Uiso 1 1 calc R U . . .
C6 C 0.4288(3) 0.2704(5) 0.3488(3) 0.0312(11) Uani 1 1 d . . . . .
C7 C 0.5041(3) 0.2947(5) 0.3385(3) 0.0358(12) Uani 1 1 d . . . . .
H7 H 0.5467 0.3025 0.3798 0.043 Uiso 1 1 calc R U . . .
C8 C 0.6042(4) 0.3181(5) 0.2854(4) 0.0429(14) Uani 1 1 d . . . . .
H8A H 0.6222 0.2391 0.2689 0.051 Uiso 1 1 calc R U . . .
H8B H 0.6347 0.3305 0.3350 0.051 Uiso 1 1 calc R U . . .
C9 C 0.6198(3) 0.4271(5) 0.2418(3) 0.0391(13) Uani 1 1 d . . . . .
H9A H 0.5947 0.5033 0.2538 0.047 Uiso 1 1 calc R U . . .
H9B H 0.6769 0.4425 0.2550 0.047 Uiso 1 1 calc R U . . .
C10 C 0.5906(4) 0.4073(6) 0.1637(4) 0.0540(17) Uani 1 1 d . . . . .
H10A H 0.6080 0.3242 0.1519 0.065 Uiso 1 1 calc R U . . .
H10B H 0.6133 0.4721 0.1398 0.065 Uiso 1 1 calc R U . . .
C11 C 0.4727(4) 0.4877(5) 0.0868(3) 0.0454(15) Uani 1 1 d . . . . .
H11 H 0.5095 0.5287 0.0682 0.054 Uiso 1 1 calc R U . . .
C12 C 0.3930(4) 0.5187(6) 0.0530(3) 0.0505(16) Uani 1 1 d . . . . .
C13 C 0.3748(4) 0.6158(6) 0.0064(3) 0.0508(16) Uani 1 1 d . . . . .
H13 H 0.4162 0.6595 -0.0045 0.061 Uiso 1 1 calc R U . . .
C14 C 0.2991(5) 0.6527(7) -0.0254(4) 0.063(2) Uani 1 1 d . . . . .
H14 H 0.2896 0.7205 -0.0578 0.076 Uiso 1 1 calc R U . . .
C15 C 0.2362(4) 0.5934(6) -0.0113(3) 0.0486(15) Uani 1 1 d . . . . .
H15 H 0.1838 0.6196 -0.0328 0.058 Uiso 1 1 calc R U . . .
C16 C 0.2536(4) 0.4923(5) 0.0364(3) 0.0436(14) Uani 1 1 d . . . . .
C17 C 0.3274(4) 0.4511(6) 0.0682(3) 0.0492(16) Uani 1 1 d . . . . .
C18 C 0.1701(4) 0.1011(6) 0.2742(3) 0.0458(14) Uani 1 1 d . . . . .
H18A H 0.1884 0.0197 0.2956 0.069 Uiso 1 1 calc R U . . .
H18B H 0.1274 0.0881 0.2311 0.069 Uiso 1 1 calc R U . . .
H18C H 0.1514 0.1519 0.3070 0.069 Uiso 1 1 calc R U . . .
C19 C 0.1179(4) 0.4497(7) 0.0166(4) 0.0560(18) Uani 1 1 d . . . . .
H19A H 0.1021 0.5341 0.0264 0.084 Uiso 1 1 calc R U . . .
H19B H 0.0838 0.3875 0.0291 0.084 Uiso 1 1 calc R U . . .
H19C H 0.1135 0.4425 -0.0335 0.084 Uiso 1 1 calc R U . . .
C20 C 0.0998(5) 0.1177(8) -0.0941(4) 0.068(2) Uani 1 1 d . . . . .
C21 C 0.1288(5) 0.0995(7) -0.0124(4) 0.065(2) Uani 1 1 d . . . . .
C22 C 0.1110(4) -0.0103(6) 0.0148(3) 0.0481(16) Uani 1 1 d . . . . .
H22 H 0.0772 -0.0689 -0.0153 0.058 Uiso 1 1 calc R U . . .
C23 C 0.1415(3) -0.0384(5) 0.0865(3) 0.0370(13) Uani 1 1 d . . . . .
C24 C 0.1297(4) -0.1695(6) 0.1108(4) 0.0463(15) Uani 1 1 d . . . . .
C25 C -0.0043(5) 0.3185(7) 0.1621(4) 0.0590(17) Uani 1 1 d . U . . .
C26 C 0.0806(3) 0.3481(6) 0.1716(3) 0.0433(14) Uani 1 1 d . . . . .
C27 C 0.1128(4) 0.4448(7) 0.2147(3) 0.0484(16) Uani 1 1 d . . . . .
H27 H 0.0806 0.4927 0.2355 0.058 Uiso 1 1 calc R U . . .
C28 C 0.1930(3) 0.4762(6) 0.2294(3) 0.0394(13) Uani 1 1 d . . . . .
C29 C 0.2243(4) 0.5830(7) 0.2834(4) 0.0615(19) Uani 1 1 d . . . . .
Dy1 Dy 0.24175(2) 0.23436(3) 0.13691(2) 0.03904(12) Uani 1 1 d . . . . .
F1 F 0.1597(3) 0.0993(4) -0.1193(2) 0.0693(12) Uani 1 1 d . . . . .
F2 F 0.0767(3) 0.2328(4) -0.1096(2) 0.0700(13) Uani 1 1 d . . . . .
F3 F 0.0435(3) 0.0386(4) -0.1242(2) 0.0713(13) Uani 1 1 d . . . . .
F4 F 0.1904(3) -0.2400(4) 0.1127(3) 0.0662(12) Uani 1 1 d . . . . .
F5 F 0.0680(3) -0.2290(4) 0.0663(2) 0.0622(11) Uani 1 1 d . . . . .
F6 F 0.1174(2) -0.1700(3) 0.17334(19) 0.0542(10) Uani 1 1 d . . . . .
F7 F -0.0436(3) 0.2871(4) 0.0962(2) 0.0682(12) Uani 1 1 d . . . . .
F8 F -0.0441(2) 0.4098(4) 0.1785(2) 0.0659(11) Uani 1 1 d . U . . .
F9 F -0.0121(3) 0.2194(4) 0.2004(3) 0.0720(13) Uani 1 1 d . . . . .
F10 F 0.2786(2) 0.5383(4) 0.3388(2) 0.0658(12) Uani 1 1 d . . . . .
F11 F 0.1720(2) 0.6410(4) 0.3044(2) 0.0599(10) Uani 1 1 d . . . . .
F12 F 0.2619(3) 0.6658(4) 0.2580(3) 0.0739(13) Uani 1 1 d . . . . .
N1 N 0.5207(3) 0.3071(4) 0.2806(3) 0.0363(11) Uani 1 1 d . . . . .
N2 N 0.5025(3) 0.4144(6) 0.1376(3) 0.0550(14) Uani 1 1 d . . . . .
N3 N 0.4774(3) 0.1406(5) 0.1583(3) 0.0520(14) Uani 1 1 d . . . . .
N4 N 0.5119(4) 0.1350(5) 0.1152(3) 0.0493(13) Uani 1 1 d . . . . .
N5 N 0.5438(4) 0.1293(7) 0.0712(3) 0.0671(17) Uani 1 1 d . . . . .
Ni1 Ni 0.43808(5) 0.32209(7) 0.18891(4) 0.0413(2) Uani 1 1 d . . . . .
O1 O 0.2337(2) 0.1650(4) 0.2579(2) 0.0400(9) Uani 1 1 d . . . . .
O2 O 0.3571(3) 0.2326(3) 0.2273(2) 0.0393(10) Uani 1 1 d . . . . .
O3 O 0.3380(3) 0.3499(4) 0.1079(2) 0.0465(11) Uani 1 1 d . . . . .
O4 O 0.1945(3) 0.4284(4) 0.0554(2) 0.0534(12) Uani 1 1 d . . . . .
O5 O 0.1720(3) 0.1859(4) 0.0190(2) 0.0494(12) Uani 1 1 d . . . . .
O6 O 0.1835(2) 0.0308(4) 0.13246(19) 0.0388(9) Uani 1 1 d . . . . .
O7 O 0.1149(3) 0.2731(4) 0.1408(2) 0.0461(11) Uani 1 1 d . . . . .
O8 O 0.2435(2) 0.4221(4) 0.2082(2) 0.0378(9) Uani 1 1 d . . . . .
O1W O 0.4049(2) 0.4974(3) 0.22488(18) 0.0376(9) Uani 1 1 d . . . . .
H1X H 0.3578 0.4902 0.2257 0.045 Uiso 1 1 d R U . . .
H1Y H 0.4422 0.5260 0.2555 0.045 Uiso 1 1 d R U . . .
O2W O 0.3227(3) 0.0848(4) 0.1032(2) 0.0549(12) Uani 1 1 d . . . . .
H2X H 0.3731 0.0797 0.1396 0.066 Uiso 1 1 d R U . . .
H2Y H 0.3314 0.1109 0.0588 0.066 Uiso 1 1 d R U . . .
O3W O 0.3304(3) 0.9687(6) 0.9868(3) 0.092(2) Uani 1 1 d . . . . .
H3X H 0.3697 0.9197 0.9965 0.110 Uiso 1 1 d R U . . .
H3Y H 0.3352 1.0231 0.9572 0.110 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.334(7) . ?
C1 C2 1.375(9) . ?
C1 C6 1.416(8) . ?
C2 O1 1.365(7) . ?
C2 C3 1.401(8) . ?
C3 C4 1.386(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.355(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.409(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.441(8) . ?
C7 N1 1.280(7) . ?
C7 H7 0.9500 . ?
C8 N1 1.471(7) . ?
C8 C9 1.524(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.507(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N2 1.508(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.268(8) . ?
C11 C12 1.426(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.366(9) . ?
C12 C17 1.479(9) . ?
C13 C14 1.374(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.411(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.359(9) . ?
C16 O4 1.399(7) . ?
C17 O3 1.318(8) . ?
C18 O1 1.440(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 O4 1.380(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 F2 1.303(9) . ?
C20 F3 1.316(8) . ?
C20 F1 1.321(10) . ?
C20 C21 1.571(11) . ?
C21 O5 1.247(8) . ?
C21 C22 1.367(10) . ?
C22 C23 1.406(8) . ?
C22 H22 0.9500 . ?
C23 O6 1.244(6) . ?
C23 C24 1.513(8) . ?
C24 F4 1.309(8) . ?
C24 F6 1.328(7) . ?
C24 F5 1.356(7) . ?
C25 F8 1.302(9) . ?
C25 F9 1.335(8) . ?
C25 F7 1.339(8) . ?
C25 C26 1.506(10) . ?
C26 O7 1.268(8) . ?
C26 C27 1.358(9) . ?
C27 C28 1.415(8) . ?
C27 H27 0.9500 . ?
C28 O8 1.243(7) . ?
C28 C29 1.555(9) . ?
C29 F11 1.287(8) . ?
C29 F12 1.296(8) . ?
C29 F10 1.329(9) . ?
Dy1 O2 2.310(4) . ?
Dy1 O3 2.320(4) . ?
Dy1 O7 2.326(5) . ?
Dy1 O5 2.376(4) . ?
Dy1 O2W 2.377(5) . ?
Dy1 O6 2.397(4) . ?
Dy1 O8 2.450(4) . ?
Dy1 O1 2.566(4) . ?
Dy1 O4 2.615(4) . ?
Dy1 Ni1 3.4823(9) . ?
N1 Ni1 1.994(5) . ?
N2 Ni1 2.004(6) . ?
N3 N4 1.195(7) . ?
N3 Ni1 2.204(5) . ?
N4 N5 1.177(8) . ?
Ni1 O3 2.053(4) . ?
Ni1 O2 2.056(4) . ?
Ni1 O1W 2.146(4) . ?
O1W H1X 0.8500 . ?
O1W H1Y 0.8201 . ?
O2W H2X 0.9800 . ?
O2W H2Y 0.9801 . ?
O3W H3X 0.8499 . ?
O3W H3Y 0.8499 . ?

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 C1 C2 117.7(5) . . ?
O2 C1 C6 123.5(6) . . ?
C2 C1 C6 118.8(6) . . ?
O1 C2 C1 114.1(5) . . ?
O1 C2 C3 124.7(6) . . ?
C1 C2 C3 121.2(6) . . ?
C4 C3 C2 119.8(6) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 119.7(6) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.9(6) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 118.5(5) . . ?
C5 C6 C7 116.6(5) . . ?
C1 C6 C7 124.8(5) . . ?
N1 C7 C6 128.2(6) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
N1 C8 C9 111.8(5) . . ?
N1 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C10 C9 C8 114.7(5) . . ?
C10 C9 H9A 108.6 . . ?
C8 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
C8 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 N2 111.2(6) . . ?
C9 C10 H10A 109.4 . . ?
N2 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
N2 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N2 C11 C12 130.6(6) . . ?
N2 C11 H11 114.7 . . ?
C12 C11 H11 114.7 . . ?
C13 C12 C11 120.3(6) . . ?
C13 C12 C17 117.6(6) . . ?
C11 C12 C17 122.1(6) . . ?
C12 C13 C14 122.6(6) . . ?
C12 C13 H13 118.7 . . ?
C14 C13 H13 118.7 . . ?
C13 C14 C15 121.5(6) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C14 C15 C16 116.8(7) . . ?
C14 C15 H15 121.6 . . ?
C16 C15 H15 121.6 . . ?
C17 C16 O4 114.9(6) . . ?
C17 C16 C15 123.9(6) . . ?
O4 C16 C15 121.2(6) . . ?
O3 C17 C16 119.8(6) . . ?
O3 C17 C12 122.5(6) . . ?
C16 C17 C12 117.6(6) . . ?
O1 C18 H18A 109.5 . . ?
O1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
F2 C20 F3 110.4(7) . . ?
F2 C20 F1 106.6(7) . . ?
F3 C20 F1 109.1(7) . . ?
F2 C20 C21 110.4(7) . . ?
F3 C20 C21 111.9(6) . . ?
F1 C20 C21 108.4(7) . . ?
O5 C21 C22 127.9(7) . . ?
O5 C21 C20 113.6(6) . . ?
C22 C21 C20 118.2(6) . . ?
C21 C22 C23 121.3(6) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
O6 C23 C22 126.5(5) . . ?
O6 C23 C24 115.0(5) . . ?
C22 C23 C24 118.2(5) . . ?
F4 C24 F6 109.3(6) . . ?
F4 C24 F5 105.1(5) . . ?
F6 C24 F5 106.7(5) . . ?
F4 C24 C23 110.5(5) . . ?
F6 C24 C23 112.3(5) . . ?
F5 C24 C23 112.7(6) . . ?
F8 C25 F9 107.0(7) . . ?
F8 C25 F7 105.3(6) . . ?
F9 C25 F7 104.6(5) . . ?
F8 C25 C26 114.5(6) . . ?
F9 C25 C26 111.2(6) . . ?
F7 C25 C26 113.4(6) . . ?
O7 C26 C27 127.6(6) . . ?
O7 C26 C25 114.6(6) . . ?
C27 C26 C25 117.7(6) . . ?
C26 C27 C28 121.9(7) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 H27 119.1 . . ?
O8 C28 C27 127.5(6) . . ?
O8 C28 C29 115.1(5) . . ?
C27 C28 C29 117.1(6) . . ?
F11 C29 F12 107.8(6) . . ?
F11 C29 F10 108.9(6) . . ?
F12 C29 F10 103.5(6) . . ?
F11 C29 C28 115.3(6) . . ?
F12 C29 C28 110.6(6) . . ?
F10 C29 C28 110.0(6) . . ?
O2 Dy1 O3 69.00(14) . . ?
O2 Dy1 O7 129.20(15) . . ?
O3 Dy1 O7 135.49(16) . . ?
O2 Dy1 O5 149.69(16) . . ?
O3 Dy1 O5 94.74(13) . . ?
O7 Dy1 O5 80.48(16) . . ?
O2 Dy1 O2W 74.80(15) . . ?
O3 Dy1 O2W 74.33(16) . . ?
O7 Dy1 O2W 143.78(14) . . ?
O5 Dy1 O2W 76.22(17) . . ?
O2 Dy1 O6 107.50(13) . . ?
O3 Dy1 O6 144.70(15) . . ?
O7 Dy1 O6 75.27(14) . . ?
O5 Dy1 O6 70.68(13) . . ?
O2W Dy1 O6 71.05(14) . . ?
O2 Dy1 O8 72.25(13) . . ?
O3 Dy1 O8 79.95(14) . . ?
O7 Dy1 O8 71.60(14) . . ?
O5 Dy1 O8 131.78(15) . . ?
O2W Dy1 O8 143.69(14) . . ?
O6 Dy1 O8 133.91(13) . . ?
O2 Dy1 O1 62.91(13) . . ?
O3 Dy1 O1 129.41(13) . . ?
O7 Dy1 O1 72.52(14) . . ?
O5 Dy1 O1 135.30(12) . . ?
O2W Dy1 O1 106.10(15) . . ?
O6 Dy1 O1 68.41(12) . . ?
O8 Dy1 O1 71.62(12) . . ?
O2 Dy1 O4 123.04(13) . . ?
O3 Dy1 O4 63.53(16) . . ?
O7 Dy1 O4 74.80(15) . . ?
O5 Dy1 O4 64.86(14) . . ?
O2W Dy1 O4 117.93(16) . . ?
O6 Dy1 O4 129.42(13) . . ?
O8 Dy1 O4 70.21(13) . . ?
O1 Dy1 O4 135.71(14) . . ?
O2 Dy1 Ni1 34.66(10) . . ?
O3 Dy1 Ni1 34.63(10) . . ?
O7 Dy1 Ni1 148.03(10) . . ?
O5 Dy1 Ni1 123.15(10) . . ?
O2W Dy1 Ni1 67.80(10) . . ?
O6 Dy1 Ni1 129.99(10) . . ?
O8 Dy1 Ni1 76.44(9) . . ?
O1 Dy1 Ni1 97.09(9) . . ?
O4 Dy1 Ni1 95.06(10) . . ?
C7 N1 C8 116.4(5) . . ?
C7 N1 Ni1 122.1(4) . . ?
C8 N1 Ni1 121.3(4) . . ?
C11 N2 C10 117.4(6) . . ?
C11 N2 Ni1 122.7(5) . . ?
C10 N2 Ni1 119.7(4) . . ?
N4 N3 Ni1 120.9(5) . . ?
N5 N4 N3 178.0(8) . . ?
N1 Ni1 N2 97.2(2) . . ?
N1 Ni1 O3 167.48(18) . . ?
N2 Ni1 O3 91.4(2) . . ?
N1 Ni1 O2 91.98(18) . . ?
N2 Ni1 O2 170.7(2) . . ?
O3 Ni1 O2 79.33(16) . . ?
N1 Ni1 O1W 88.05(16) . . ?
N2 Ni1 O1W 89.9(2) . . ?
O3 Ni1 O1W 82.89(16) . . ?
O2 Ni1 O1W 89.30(15) . . ?
N1 Ni1 N3 88.5(2) . . ?
N2 Ni1 N3 90.8(2) . . ?
O3 Ni1 N3 100.5(2) . . ?
O2 Ni1 N3 90.60(18) . . ?
O1W Ni1 N3 176.50(19) . . ?
N1 Ni1 Dy1 131.64(13) . . ?
N2 Ni1 Dy1 131.05(17) . . ?
O3 Ni1 Dy1 39.96(11) . . ?
O2 Ni1 Dy1 39.71(12) . . ?
O1W Ni1 Dy1 88.98(11) . . ?
N3 Ni1 Dy1 93.17(14) . . ?
C2 O1 C18 116.6(5) . . ?
C2 O1 Dy1 115.6(3) . . ?
C18 O1 Dy1 127.7(3) . . ?
C1 O2 Ni1 122.2(4) . . ?
C1 O2 Dy1 124.1(4) . . ?
Ni1 O2 Dy1 105.63(17) . . ?
C17 O3 Ni1 122.1(4) . . ?
C17 O3 Dy1 126.5(4) . . ?
Ni1 O3 Dy1 105.41(16) . . ?
C19 O4 C16 118.0(5) . . ?
C19 O4 Dy1 124.6(4) . . ?
C16 O4 Dy1 114.9(4) . . ?
C21 O5 Dy1 136.8(5) . . ?
C23 O6 Dy1 136.6(4) . . ?
C26 O7 Dy1 137.7(4) . . ?
C28 O8 Dy1 133.5(4) . . ?
Ni1 O1W H1X 107.4 . . ?
Ni1 O1W H1Y 109.2 . . ?
H1X O1W H1Y 127.8 . . ?
Dy1 O2W H2X 109.3 . . ?
Dy1 O2W H2Y 109.4 . . ?
H2X O2W H2Y 109.5 . . ?
H3X O3W H3Y 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 O1 -0.2(7) . . . . ?
C6 C1 C2 O1 -178.3(4) . . . . ?
O2 C1 C2 C3 -179.5(5) . . . . ?
C6 C1 C2 C3 2.5(8) . . . . ?
O1 C2 C3 C4 -179.1(5) . . . . ?
C1 C2 C3 C4 0.0(9) . . . . ?
C2 C3 C4 C5 -1.0(8) . . . . ?
C3 C4 C5 C6 -0.8(8) . . . . ?
C4 C5 C6 C1 3.3(8) . . . . ?
C4 C5 C6 C7 -172.9(5) . . . . ?
O2 C1 C6 C5 178.0(5) . . . . ?
C2 C1 C6 C5 -4.1(8) . . . . ?
O2 C1 C6 C7 -6.1(8) . . . . ?
C2 C1 C6 C7 171.8(5) . . . . ?
C5 C6 C7 N1 -173.4(5) . . . . ?
C1 C6 C7 N1 10.6(9) . . . . ?
N1 C8 C9 C10 -71.0(7) . . . . ?
C8 C9 C10 N2 72.1(7) . . . . ?
N2 C11 C12 C13 169.3(7) . . . . ?
N2 C11 C12 C17 -8.7(11) . . . . ?
C11 C12 C13 C14 -177.3(6) . . . . ?
C17 C12 C13 C14 0.9(10) . . . . ?
C12 C13 C14 C15 0.5(11) . . . . ?
C13 C14 C15 C16 -0.9(10) . . . . ?
C14 C15 C16 C17 -0.2(9) . . . . ?
C14 C15 C16 O4 178.3(6) . . . . ?
O4 C16 C17 O3 6.6(8) . . . . ?
C15 C16 C17 O3 -174.7(6) . . . . ?
O4 C16 C17 C12 -177.0(5) . . . . ?
C15 C16 C17 C12 1.6(9) . . . . ?
C13 C12 C17 O3 174.3(6) . . . . ?
C11 C12 C17 O3 -7.5(10) . . . . ?
C13 C12 C17 C16 -1.9(9) . . . . ?
C11 C12 C17 C16 176.3(6) . . . . ?
F2 C20 C21 O5 -44.8(10) . . . . ?
F3 C20 C21 O5 -168.1(7) . . . . ?
F1 C20 C21 O5 71.6(9) . . . . ?
F2 C20 C21 C22 141.0(8) . . . . ?
F3 C20 C21 C22 17.7(11) . . . . ?
F1 C20 C21 C22 -102.6(8) . . . . ?
O5 C21 C22 C23 0.3(13) . . . . ?
C20 C21 C22 C23 173.6(7) . . . . ?
C21 C22 C23 O6 3.1(11) . . . . ?
C21 C22 C23 C24 -170.4(7) . . . . ?
O6 C23 C24 F4 -80.1(7) . . . . ?
C22 C23 C24 F4 94.2(7) . . . . ?
O6 C23 C24 F6 42.2(7) . . . . ?
C22 C23 C24 F6 -143.5(6) . . . . ?
O6 C23 C24 F5 162.8(5) . . . . ?
C22 C23 C24 F5 -22.9(8) . . . . ?
F8 C25 C26 O7 -164.1(6) . . . . ?
F9 C25 C26 O7 74.5(8) . . . . ?
F7 C25 C26 O7 -43.1(8) . . . . ?
F8 C25 C26 C27 19.9(9) . . . . ?
F9 C25 C26 C27 -101.5(7) . . . . ?
F7 C25 C26 C27 140.8(6) . . . . ?
O7 C26 C27 C28 1.7(10) . . . . ?
C25 C26 C27 C28 177.1(6) . . . . ?
C26 C27 C28 O8 -1.9(10) . . . . ?
C26 C27 C28 C29 -176.0(6) . . . . ?
O8 C28 C29 F11 178.6(6) . . . . ?
C27 C28 C29 F11 -6.5(9) . . . . ?
O8 C28 C29 F12 56.0(8) . . . . ?
C27 C28 C29 F12 -129.1(6) . . . . ?
O8 C28 C29 F10 -57.8(8) . . . . ?
C27 C28 C29 F10 117.1(6) . . . . ?
C6 C7 N1 C8 -173.6(5) . . . . ?
C6 C7 N1 Ni1 10.3(8) . . . . ?
C9 C8 N1 C7 -132.0(5) . . . . ?
C9 C8 N1 Ni1 44.2(6) . . . . ?
C12 C11 N2 C10 -176.9(6) . . . . ?
C12 C11 N2 Ni1 -2.7(10) . . . . ?
C9 C10 N2 C11 128.2(6) . . . . ?
C9 C10 N2 Ni1 -46.2(7) . . . . ?
C1 C2 O1 C18 166.9(5) . . . . ?
C3 C2 O1 C18 -13.9(8) . . . . ?
C1 C2 O1 Dy1 -16.7(6) . . . . ?
C3 C2 O1 Dy1 162.5(4) . . . . ?
C2 C1 O2 Ni1 164.9(4) . . . . ?
C6 C1 O2 Ni1 -17.2(7) . . . . ?
C2 C1 O2 Dy1 20.8(6) . . . . ?
C6 C1 O2 Dy1 -161.3(4) . . . . ?
C16 C17 O3 Ni1 -152.9(5) . . . . ?
C12 C17 O3 Ni1 30.9(8) . . . . ?
C16 C17 O3 Dy1 -4.2(8) . . . . ?
C12 C17 O3 Dy1 179.7(4) . . . . ?
C17 C16 O4 C19 -168.8(6) . . . . ?
C15 C16 O4 C19 12.6(8) . . . . ?
C17 C16 O4 Dy1 -5.9(6) . . . . ?
C15 C16 O4 Dy1 175.5(4) . . . . ?
C22 C21 O5 Dy1 -5.2(14) . . . . ?
C20 C21 O5 Dy1 -178.7(5) . . . . ?
C22 C23 O6 Dy1 -2.0(10) . . . . ?
C24 C23 O6 Dy1 171.8(4) . . . . ?
C27 C26 O7 Dy1 4.1(10) . . . . ?
C25 C26 O7 Dy1 -171.5(4) . . . . ?
C27 C28 O8 Dy1 -3.1(9) . . . . ?
C29 C28 O8 Dy1 171.2(4) . . . . ?

_refine_diff_density_max         1.242
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.203

_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 1046795'
_audit_update_record             
;
2015-02-02 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H26 F12 Gd N5 Ni O10, H2 O'
_chemical_formula_sum            'C29 H28 F12 Gd N5 Ni O11'
_chemical_formula_weight         1066.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 '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/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   18.351(3)
_cell_length_b                   10.8682(15)
_cell_length_c                   19.911(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.184(2)
_cell_angle_gamma                90
_cell_volume                     3813.7(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    6159
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      24.35

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_F_000             2100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    2.338
_shelx_estimated_absorpt_T_min   0.541
_shelx_estimated_absorpt_T_max   0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_process_details   'SADABS; Bruker, 2013'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex Duo CCD '
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23999
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_av_R_equivalents  0.0106
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.155
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8330
_reflns_number_gt                5108
_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       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.07P)²+1.88P]
 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         8330
_refine_ls_number_parameters     534
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1527
_refine_ls_wR_factor_gt          0.1517
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3227(4) 0.0379(6) 0.0687(3) 0.0571(16) Uani 1 1 d . . . . .
C2 C 0.2483(4) 0.0055(6) 0.0375(3) 0.0597(16) Uani 1 1 d . . . . .
C3 C 0.2333(5) -0.0870(6) -0.0107(3) 0.073(2) Uani 1 1 d . . . . .
H3 H 0.1820 -0.1082 -0.0328 0.087 Uiso 1 1 calc R U . . .
C4 C 0.2903(6) -0.1507(8) -0.0286(4) 0.086(2) Uani 1 1 d . U . . .
H4 H 0.2784 -0.2144 -0.0626 0.103 Uiso 1 1 calc R U . . .
C5 C 0.3666(5) -0.1199(7) 0.0045(4) 0.082(2) Uani 1 1 d . U . . .
H5 H 0.4067 -0.1641 -0.0061 0.098 Uiso 1 1 calc R U . . .
C6 C 0.3825(4) -0.0243(6) 0.0527(3) 0.0601(17) Uani 1 1 d . . . . .
C7 C 0.4622(5) 0.0006(6) 0.0846(4) 0.0661(19) Uani 1 1 d . U . . .
H7 H 0.4969 -0.0420 0.0653 0.079 Uiso 1 1 calc R U . . .
C8 C 0.5774(4) 0.0832(9) 0.1628(5) 0.090(2) Uani 1 1 d . . . . .
H8A H 0.6006 0.0224 0.1379 0.108 Uiso 1 1 calc R U . . .
H8B H 0.5928 0.1661 0.1513 0.108 Uiso 1 1 calc R U . . .
C9 C 0.6074(5) 0.0637(7) 0.2367(5) 0.081(2) Uani 1 1 d . . . . .
H9A H 0.6624 0.0461 0.2475 0.097 Uiso 1 1 calc R U . . .
H9B H 0.5825 -0.0092 0.2504 0.097 Uiso 1 1 calc R U . . .
C10 C 0.5958(4) 0.1737(6) 0.2800(4) 0.072(2) Uani 1 1 d . . . . .
H10A H 0.6269 0.1627 0.3289 0.086 Uiso 1 1 calc DR U . . .
H10B H 0.6134 0.2492 0.2615 0.086 Uiso 1 1 calc R U . . .
C11 C 0.4969(4) 0.2044(6) 0.3374(4) 0.0700(19) Uani 1 1 d . . . . .
H11 H 0.5386 0.1977 0.3782 0.084 Uiso 1 1 calc DR U . . .
C12 C 0.4259(4) 0.2295(5) 0.3502(4) 0.0585(16) Uani 1 1 d . . . . .
C13 C 0.4274(5) 0.2302(6) 0.4183(4) 0.077(2) Uani 1 1 d . . . . .
H13 H 0.4723 0.2068 0.4528 0.092 Uiso 1 1 calc R U . . .
C14 C 0.3605(5) 0.2667(7) 0.4390(5) 0.079(2) Uani 1 1 d . . . . .
H14 H 0.3606 0.2682 0.4868 0.095 Uiso 1 1 calc R U . . .
C15 C 0.3000(5) 0.2975(7) 0.3888(4) 0.074(2) Uani 1 1 d . . . . .
H15 H 0.2556 0.3211 0.4012 0.089 Uiso 1 1 calc R U . . .
C16 C 0.2976(4) 0.2973(6) 0.3184(3) 0.0620(17) Uani 1 1 d . U . . .
C17 C 0.3618(4) 0.2615(5) 0.2972(3) 0.0589(16) Uani 1 1 d . U . . .
C18 C 0.1184(4) 0.0457(8) 0.0199(4) 0.083(2) Uani 1 1 d . . . . .
H18A H 0.1096 -0.0434 0.0177 0.124 Uiso 1 1 calc R U . . .
H18C H 0.1077 0.0788 -0.0276 0.124 Uiso 1 1 calc R U . . .
H18B H 0.0848 0.0848 0.0442 0.124 Uiso 1 1 calc R U . . .
C19 C 0.1772(5) 0.3950(8) 0.2837(4) 0.090(2) Uani 1 1 d . . . . .
H19A H 0.1611 0.3461 0.3184 0.136 Uiso 1 1 calc R U . . .
H19B H 0.1338 0.4088 0.2428 0.136 Uiso 1 1 calc R U . . .
H19C H 0.1970 0.4744 0.3043 0.136 Uiso 1 1 calc R U . . .
C20 C 0.2255(5) -0.0782(8) 0.2897(5) 0.085(2) Uani 1 1 d . U . . .
C21 C 0.1943(5) 0.0225(7) 0.2363(4) 0.078(2) Uani 1 1 d . U . . .
C22 C 0.1155(5) 0.0501(8) 0.2240(4) 0.093(3) Uani 1 1 d . U . . .
H22 H 0.0847 0.0022 0.2453 0.112 Uiso 1 1 calc R U . . .
C23 C 0.0843(5) 0.1490(8) 0.1802(4) 0.088(2) Uani 1 1 d . . . . .
C24 C -0.0037(5) 0.1721(10) 0.1656(5) 0.091(3) Uani 1 1 d . . . . .
C25 C 0.1460(6) 0.6653(8) 0.1238(6) 0.091(2) Uani 1 1 d . . . . .
C26 C 0.1521(4) 0.5329(8) 0.0928(4) 0.072(2) Uani 1 1 d . . . . .
C27 C 0.1193(4) 0.5094(7) 0.0229(4) 0.0701(19) Uani 1 1 d . . . . .
H27 H 0.0881 0.5700 -0.0057 0.084 Uiso 1 1 calc R U . . .
C28 C 0.1311(4) 0.4009(7) -0.0052(4) 0.0677(19) Uani 1 1 d . . . . .
C29 C 0.0926(6) 0.3832(9) -0.0834(5) 0.090(2) Uani 1 1 d . U . . .
F1 F 0.2678(3) -0.1503(5) 0.2684(3) 0.1008(14) Uani 1 1 d . U . . .
F2 F 0.2646(3) -0.0282(5) 0.3482(3) 0.0943(14) Uani 1 1 d . . . . .
F3 F 0.1725(3) -0.1429(5) 0.3058(2) 0.0991(15) Uani 1 1 d . . . . .
F4 F -0.0100(3) 0.2699(5) 0.1995(3) 0.0971(15) Uani 1 1 d . . . . .
F5 F -0.0376(3) 0.0917(5) 0.1876(3) 0.1082(16) Uani 1 1 d . . . . .
F6 F -0.0374(3) 0.2010(5) 0.1030(3) 0.1016(15) Uani 1 1 d . . . . .
F7 F 0.2076(3) 0.7238(4) 0.1295(3) 0.0966(14) Uani 1 1 d . . . . .
F8 F 0.1255(3) 0.6655(4) 0.1784(2) 0.0916(13) Uani 1 1 d . . . . .
F9 F 0.0965(3) 0.7343(4) 0.0754(3) 0.1008(16) Uani 1 1 d . . . . .
F10 F 0.0694(3) 0.2705(5) -0.1012(3) 0.1107(18) Uani 1 1 d . . . . .
F11 F 0.1445(3) 0.3712(5) -0.1154(3) 0.1059(16) Uani 1 1 d . U . . .
F12 F 0.0488(3) 0.4634(5) -0.1143(3) 0.1016(15) Uani 1 1 d . . . . .
Gd1 Gd 0.24074(2) 0.25844(3) 0.14008(2) 0.05786(14) Uani 1 1 d . . . . .
N1 N 0.4914(3) 0.0728(5) 0.1354(3) 0.0668(15) Uani 1 1 d . U . . .
N2 N 0.5141(3) 0.1891(4) 0.2787(3) 0.0586(13) Uani 1 1 d . . . . .
N3 N 0.4573(4) 0.3351(6) 0.1496(3) 0.0819(18) Uani 1 1 d . . . . .
N4 N 0.5094(4) 0.3594(6) 0.1189(3) 0.0821(19) Uani 1 1 d . . . . .
N5 N 0.5487(5) 0.3718(7) 0.0830(4) 0.103(2) Uani 1 1 d . . . . .
Ni1 Ni 0.43094(5) 0.16879(7) 0.18821(4) 0.0532(2) Uani 1 1 d . . . . .
O1 O 0.1942(3) 0.0697(4) 0.0564(2) 0.0613(11) Uani 1 1 d . . . . .
O2 O 0.3332(3) 0.1389(4) 0.1109(2) 0.0628(12) Uani 1 1 d . . . . .
O3 O 0.3559(3) 0.2596(4) 0.2291(2) 0.0656(12) Uani 1 1 d . . . . .
O4 O 0.2364(3) 0.3294(5) 0.2627(2) 0.0746(13) Uani 1 1 d . . . . .
O5 O 0.2420(3) 0.0737(4) 0.2119(2) 0.0736(13) Uani 1 1 d . . . . .
O6 O 0.1152(3) 0.2190(4) 0.1486(3) 0.0738(13) Uani 1 1 d . . . . .
O7 O 0.1905(3) 0.4642(4) 0.1380(3) 0.0686(12) Uani 1 1 d . . . . .
O8 O 0.1671(3) 0.3089(5) 0.0235(2) 0.0690(12) Uani 1 1 d . . . . .
O1W O 0.4019(3) -0.0002(4) 0.2280(2) 0.0671(12) Uani 1 1 d . . . . .
H1X H 0.4362 -0.0146 0.2747 0.081 Uiso 1 1 d R U . . .
H1Y H 0.3495 0.0046 0.2308 0.081 Uiso 1 1 d R U . . .
O2W O 0.3230(3) 0.4032(4) 0.1001(2) 0.0711(13) Uani 1 1 d . . . . .
H2X H 0.3048 0.4875 0.1024 0.085 Uiso 1 1 d R U . . .
H2Y H 0.3752 0.3961 0.1300 0.085 Uiso 1 1 d R U . . .
O3W O 0.4336(3) 0.5165(5) 0.0447(3) 0.0853(15) Uani 1 1 d . . . . .
H3X H 0.4724 0.4703 0.0568 0.102 Uiso 1 1 d R U . . .
H3Y H 0.4183 0.5215 0.0004 0.102 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.363(7) . ?
C1 C2 1.379(9) . ?
C1 C6 1.398(9) . ?
C2 O1 1.349(7) . ?
C2 C3 1.365(8) . ?
C3 C4 1.381(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.450(10) . ?
C7 N1 1.275(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.437(11) . ?
C8 N1 1.523(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.522(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N2 1.501(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.303(8) . ?
C11 C12 1.423(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.347(11) . ?
C12 C17 1.388(10) . ?
C13 C14 1.455(12) . ?
C13 H13 0.9500 . ?
C14 C15 1.314(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(9) . ?
C15 H15 0.9500 . ?
C16 O4 1.386(8) . ?
C16 C17 1.413(10) . ?
C17 O3 1.330(7) . ?
C18 O1 1.402(8) . ?
C18 H18A 0.9800 . ?
C18 H18C 0.9800 . ?
C18 H18B 0.9800 . ?
C19 O4 1.455(9) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 F1 1.257(9) . ?
C20 F2 1.304(9) . ?
C20 F3 1.310(9) . ?
C20 C21 1.522(11) . ?
C21 O5 1.246(8) . ?
C21 C22 1.429(11) . ?
C22 C23 1.402(11) . ?
C22 H22 0.9500 . ?
C23 O6 1.223(8) . ?
C23 C24 1.578(12) . ?
C24 F5 1.223(10) . ?
C24 F6 1.267(10) . ?
C24 F4 1.282(11) . ?
C25 F8 1.247(10) . ?
C25 F7 1.273(10) . ?
C25 F9 1.353(10) . ?
C25 C26 1.581(11) . ?
C26 O7 1.228(8) . ?
C26 C27 1.379(10) . ?
C27 C28 1.348(10) . ?
C27 H27 0.9500 . ?
C28 O8 1.247(8) . ?
C28 C29 1.533(11) . ?
C29 F12 1.228(10) . ?
C29 F11 1.292(10) . ?
C29 F10 1.312(10) . ?
Gd1 O2 2.336(4) . ?
Gd1 O3 2.349(5) . ?
Gd1 O6 2.395(5) . ?
Gd1 O8 2.401(5) . ?
Gd1 O7 2.415(5) . ?
Gd1 O5 2.461(5) . ?
Gd1 O2W 2.461(4) . ?
Gd1 O4 2.582(4) . ?
Gd1 O1 2.631(4) . ?
Gd1 Ni1 3.4908(10) . ?
N1 Ni1 2.019(5) . ?
N2 Ni1 2.022(6) . ?
N3 N4 1.297(9) . ?
N3 Ni1 2.074(6) . ?
N4 N5 1.155(9) . ?
Ni1 O2 2.039(5) . ?
Ni1 O3 2.040(4) . ?
Ni1 O1W 2.125(4) . ?
O1W H1X 0.9800 . ?
O1W H1Y 0.9800 . ?
O2W H2X 0.9800 . ?
O2W H2Y 0.9800 . ?
O3W H3X 0.8500 . ?
O3W H3Y 0.8499 . ?

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 C1 C2 115.7(6) . . ?
O2 C1 C6 123.0(6) . . ?
C2 C1 C6 121.0(6) . . ?
O1 C2 C3 123.8(7) . . ?
O1 C2 C1 117.2(6) . . ?
C3 C2 C1 119.0(7) . . ?
C2 C3 C4 122.1(8) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C5 119.0(8) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 119.3(8) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 119.5(7) . . ?
C5 C6 C7 115.7(7) . . ?
C1 C6 C7 124.8(6) . . ?
N1 C7 C6 127.8(6) . . ?
N1 C7 H7 116.1 . . ?
C6 C7 H7 116.1 . . ?
C9 C8 N1 114.7(7) . . ?
C9 C8 H8A 108.6 . . ?
N1 C8 H8A 108.6 . . ?
C9 C8 H8B 108.6 . . ?
N1 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
C8 C9 C10 112.9(6) . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
N2 C10 C9 112.0(6) . . ?
N2 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
N2 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 C12 130.4(7) . . ?
N2 C11 H11 114.8 . . ?
C12 C11 H11 114.8 . . ?
C13 C12 C17 122.6(7) . . ?
C13 C12 C11 114.8(7) . . ?
C17 C12 C11 122.4(7) . . ?
C12 C13 C14 120.3(8) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 117.0(8) . . ?
C15 C14 H14 121.5 . . ?
C13 C14 H14 121.5 . . ?
C14 C15 C16 123.4(8) . . ?
C14 C15 H15 118.3 . . ?
C16 C15 H15 118.3 . . ?
O4 C16 C15 126.8(7) . . ?
O4 C16 C17 112.8(5) . . ?
C15 C16 C17 120.4(7) . . ?
O3 C17 C12 125.6(6) . . ?
O3 C17 C16 118.1(6) . . ?
C12 C17 C16 116.3(6) . . ?
O1 C18 H18A 109.5 . . ?
O1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
O1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18C C18 H18B 109.5 . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
F1 C20 F2 108.8(8) . . ?
F1 C20 F3 108.6(7) . . ?
F2 C20 F3 105.5(7) . . ?
F1 C20 C21 111.1(7) . . ?
F2 C20 C21 109.3(7) . . ?
F3 C20 C21 113.4(8) . . ?
O5 C21 C22 128.8(7) . . ?
O5 C21 C20 115.2(8) . . ?
C22 C21 C20 115.9(7) . . ?
C23 C22 C21 119.1(8) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
O6 C23 C22 129.0(8) . . ?
O6 C23 C24 113.8(8) . . ?
C22 C23 C24 117.1(8) . . ?
F5 C24 F6 111.8(10) . . ?
F5 C24 F4 105.9(8) . . ?
F6 C24 F4 102.8(8) . . ?
F5 C24 C23 114.7(8) . . ?
F6 C24 C23 114.5(8) . . ?
F4 C24 C23 105.9(9) . . ?
F8 C25 F7 113.4(9) . . ?
F8 C25 F9 108.3(7) . . ?
F7 C25 F9 100.9(8) . . ?
F8 C25 C26 114.4(8) . . ?
F7 C25 C26 109.4(7) . . ?
F9 C25 C26 109.5(8) . . ?
O7 C26 C27 128.8(7) . . ?
O7 C26 C25 110.9(7) . . ?
C27 C26 C25 120.2(8) . . ?
C28 C27 C26 120.3(8) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
O8 C28 C27 129.6(7) . . ?
O8 C28 C29 113.6(7) . . ?
C27 C28 C29 116.7(7) . . ?
F12 C29 F11 107.2(8) . . ?
F12 C29 F10 114.2(8) . . ?
F11 C29 F10 90.1(7) . . ?
F12 C29 C28 118.1(8) . . ?
F11 C29 C28 108.6(7) . . ?
F10 C29 C28 114.5(8) . . ?
O2 Gd1 O3 68.17(15) . . ?
O2 Gd1 O6 134.25(16) . . ?
O3 Gd1 O6 128.88(17) . . ?
O2 Gd1 O8 97.94(15) . . ?
O3 Gd1 O8 150.89(16) . . ?
O6 Gd1 O8 79.42(17) . . ?
O2 Gd1 O7 144.22(16) . . ?
O3 Gd1 O7 105.49(16) . . ?
O6 Gd1 O7 78.27(16) . . ?
O8 Gd1 O7 70.27(17) . . ?
O2 Gd1 O5 78.50(16) . . ?
O3 Gd1 O5 72.84(16) . . ?
O6 Gd1 O5 70.53(17) . . ?
O8 Gd1 O5 131.26(16) . . ?
O7 Gd1 O5 135.03(16) . . ?
O2 Gd1 O2W 73.85(16) . . ?
O3 Gd1 O2W 74.77(15) . . ?
O6 Gd1 O2W 145.67(16) . . ?
O8 Gd1 O2W 76.80(16) . . ?
O7 Gd1 O2W 70.60(16) . . ?
O5 Gd1 O2W 143.33(16) . . ?
O2 Gd1 O4 128.15(16) . . ?
O3 Gd1 O4 62.83(15) . . ?
O6 Gd1 O4 72.67(17) . . ?
O8 Gd1 O4 133.49(17) . . ?
O7 Gd1 O4 68.15(16) . . ?
O5 Gd1 O4 72.08(15) . . ?
O2W Gd1 O4 107.37(16) . . ?
O2 Gd1 O1 62.52(15) . . ?
O3 Gd1 O1 123.17(14) . . ?
O6 Gd1 O1 75.91(15) . . ?
O8 Gd1 O1 64.52(15) . . ?
O7 Gd1 O1 130.99(15) . . ?
O5 Gd1 O1 71.37(14) . . ?
O2W Gd1 O1 114.44(14) . . ?
O4 Gd1 O1 137.84(15) . . ?
O2 Gd1 Ni1 34.21(11) . . ?
O3 Gd1 Ni1 34.34(10) . . ?
O6 Gd1 Ni1 146.97(12) . . ?
O8 Gd1 Ni1 125.39(11) . . ?
O7 Gd1 Ni1 127.66(12) . . ?
O5 Gd1 Ni1 76.46(12) . . ?
O2W Gd1 Ni1 67.11(11) . . ?
O4 Gd1 Ni1 96.67(12) . . ?
O1 Gd1 Ni1 94.57(10) . . ?
C7 N1 C8 119.6(6) . . ?
C7 N1 Ni1 124.1(5) . . ?
C8 N1 Ni1 116.1(5) . . ?
C11 N2 C10 119.2(6) . . ?
C11 N2 Ni1 120.2(5) . . ?
C10 N2 Ni1 120.3(4) . . ?
N4 N3 Ni1 129.1(5) . . ?
N5 N4 N3 169.6(8) . . ?
N1 Ni1 N2 97.6(2) . . ?
N1 Ni1 O2 91.1(2) . . ?
N2 Ni1 O2 167.67(19) . . ?
N1 Ni1 O3 171.3(2) . . ?
N2 Ni1 O3 91.0(2) . . ?
O2 Ni1 O3 80.14(17) . . ?
N1 Ni1 N3 92.2(2) . . ?
N2 Ni1 N3 92.2(2) . . ?
O2 Ni1 N3 96.1(2) . . ?
O3 Ni1 N3 88.9(2) . . ?
N1 Ni1 O1W 88.78(19) . . ?
N2 Ni1 O1W 88.15(19) . . ?
O2 Ni1 O1W 83.35(18) . . ?
O3 Ni1 O1W 90.11(18) . . ?
N3 Ni1 O1W 178.9(2) . . ?
N1 Ni1 Gd1 130.85(19) . . ?
N2 Ni1 Gd1 131.49(15) . . ?
O2 Ni1 Gd1 40.11(11) . . ?
O3 Ni1 Gd1 40.51(14) . . ?
N3 Ni1 Gd1 88.5(2) . . ?
O1W Ni1 Gd1 90.46(13) . . ?
C2 O1 C18 117.5(5) . . ?
C2 O1 Gd1 116.4(4) . . ?
C18 O1 Gd1 124.9(4) . . ?
C1 O2 Ni1 122.5(4) . . ?
C1 O2 Gd1 127.9(4) . . ?
Ni1 O2 Gd1 105.68(16) . . ?
C17 O3 Ni1 122.8(4) . . ?
C17 O3 Gd1 124.8(4) . . ?
Ni1 O3 Gd1 105.15(18) . . ?
C16 O4 C19 113.3(5) . . ?
C16 O4 Gd1 116.8(4) . . ?
C19 O4 Gd1 129.9(4) . . ?
C21 O5 Gd1 134.2(5) . . ?
C23 O6 Gd1 137.8(6) . . ?
C26 O7 Gd1 135.6(5) . . ?
C28 O8 Gd1 135.2(5) . . ?
Ni1 O1W H1X 109.3 . . ?
Ni1 O1W H1Y 109.1 . . ?
H1X O1W H1Y 109.5 . . ?
Gd1 O2W H2X 109.6 . . ?
Gd1 O2W H2Y 109.7 . . ?
H2X O2W H2Y 109.5 . . ?
H3X O3W H3Y 109.9 . . ?

_refine_diff_density_max         0.733
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.171

_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 1046796'
_audit_update_record             
;
2015-02-02 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H26 F12 N5 Ni O10 Tb, H2 O'
_chemical_formula_sum            'C29 H28 F12 N5 Ni O11 Tb'
_chemical_formula_weight         1068.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   17.8821(14)
_cell_length_b                   10.8892(11)
_cell_length_c                   20.0534(18)
_cell_angle_alpha                90
_cell_angle_beta                 106.038(2)
_cell_angle_gamma                90
_cell_volume                     3752.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    6357
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      25.72

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_F_000             2104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    2.494
_shelx_estimated_absorpt_T_min   0.542
_shelx_estimated_absorpt_T_max   0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_process_details   'SADABS; Bruker, 2013'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex Duo CCD '
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23618
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_av_R_equivalents  0.0100
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.113
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8159
_reflns_number_gt                5208
_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       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.06P)²+1.88P]
 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         8159
_refine_ls_number_parameters     534
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1330
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1361(3) 0.7381(5) 0.2062(3) 0.0441(13) Uani 1 1 d . . . . .
C2 C 0.2023(4) 0.6965(5) 0.1865(3) 0.0509(14) Uani 1 1 d . . . . .
C3 C 0.2054(4) 0.6961(6) 0.1186(4) 0.0637(18) Uani 1 1 d . . . . .
H3 H 0.2499 0.6656 0.1068 0.076 Uiso 1 1 calc R U . . .
C4 C 0.1419(5) 0.7415(7) 0.0679(4) 0.073(2) Uani 1 1 d . . . . .
H4 H 0.1450 0.7482 0.0215 0.088 Uiso 1 1 calc R U . . .
C5 C 0.0763(4) 0.7760(6) 0.0829(4) 0.0667(18) Uani 1 1 d . . . . .
H5 H 0.0325 0.8023 0.0470 0.080 Uiso 1 1 calc R U . . .
C6 C 0.0728(4) 0.7730(6) 0.1517(3) 0.0559(16) Uani 1 1 d . . . . .
C7 C -0.0033(3) 0.7986(6) 0.1599(3) 0.0615(17) Uani 1 1 d . . . . .
H7 H -0.0446 0.8090 0.1187 0.074 Uiso 1 1 calc DR U . . .
C8 C -0.1047(3) 0.8237(7) 0.2171(4) 0.078(2) Uani 1 1 d . . . . .
H8A H -0.1232 0.7468 0.2337 0.093 Uiso 1 1 calc R U . . .
H8B H -0.1355 0.8363 0.1683 0.093 Uiso 1 1 calc DR U . . .
C9 C -0.1195(4) 0.9268(6) 0.2593(4) 0.072(2) Uani 1 1 d . . . . .
H9A H -0.0937 1.0015 0.2481 0.087 Uiso 1 1 calc R U . . .
H9B H -0.1761 0.9430 0.2472 0.087 Uiso 1 1 calc R U . . .
C10 C -0.0906(4) 0.9023(7) 0.3346(4) 0.080(2) Uani 1 1 d . . . . .
H10A H -0.1062 0.8183 0.3442 0.096 Uiso 1 1 calc R U . . .
H10B H -0.1152 0.9608 0.3599 0.096 Uiso 1 1 calc R U . . .
C11 C 0.0256(5) 0.9874(6) 0.4112(4) 0.0661(19) Uani 1 1 d . . . . .
H11 H -0.0104 1.0286 0.4304 0.079 Uiso 1 1 calc R U . . .
C12 C 0.1086(5) 1.0168(6) 0.4434(3) 0.0658(19) Uani 1 1 d . . . . .
C13 C 0.1238(5) 1.1109(6) 0.4906(4) 0.074(2) Uani 1 1 d . U . . .
H13 H 0.0818 1.1517 0.5017 0.089 Uiso 1 1 calc R U . . .
C14 C 0.1987(6) 1.1471(8) 0.5222(4) 0.092(3) Uani 1 1 d . U . . .
H14 H 0.2087 1.2137 0.5540 0.111 Uiso 1 1 calc R U . . .
C15 C 0.2589(5) 1.0855(7) 0.5070(4) 0.079(2) Uani 1 1 d . . . . .
H15 H 0.3110 1.1098 0.5284 0.095 Uiso 1 1 calc R U . . .
C16 C 0.2445(4) 0.9903(6) 0.4619(3) 0.0553(16) Uani 1 1 d . . . . .
C17 C 0.1671(4) 0.9509(6) 0.4286(3) 0.0554(16) Uani 1 1 d . . . . .
C18 C 0.3257(4) 0.5985(7) 0.2257(4) 0.078(2) Uani 1 1 d . . . . .
H18A H 0.3088 0.5153 0.2099 0.117 Uiso 1 1 calc R U . . .
H18B H 0.3704 0.5938 0.2670 0.117 Uiso 1 1 calc R U . . .
H18C H 0.3407 0.6427 0.1889 0.117 Uiso 1 1 calc R U . . .
C19 C 0.3794(4) 0.9500(8) 0.4795(4) 0.083(2) Uani 1 1 d . . . . .
H19A H 0.3939 1.0292 0.4634 0.124 Uiso 1 1 calc R U . . .
H19B H 0.4141 0.8858 0.4712 0.124 Uiso 1 1 calc R U . . .
H19C H 0.3840 0.9548 0.5293 0.124 Uiso 1 1 calc R U . . .
C20 C 0.3980(5) 0.6144(10) 0.5890(4) 0.088(2) Uani 1 1 d . . . . .
C21 C 0.3670(4) 0.5992(8) 0.5097(4) 0.071(2) Uani 1 1 d . . . . .
C22 C 0.3820(5) 0.4928(8) 0.4843(4) 0.083(2) Uani 1 1 d . . . . .
H22 H 0.4139 0.4344 0.5143 0.100 Uiso 1 1 calc R U . . .
C23 C 0.3516(4) 0.4651(7) 0.4136(4) 0.073(2) Uani 1 1 d . . . . .
C24 C 0.3652(6) 0.3331(8) 0.3909(6) 0.094(2) Uani 1 1 d . U . . .
C25 C 0.5046(5) 0.8207(11) 0.3396(5) 0.089(3) Uani 1 1 d . . . . .
C26 C 0.4181(4) 0.8459(7) 0.3278(4) 0.0658(18) Uani 1 1 d . . . . .
C27 C 0.3840(4) 0.9412(7) 0.2838(4) 0.0674(19) Uani 1 1 d . . . . .
H27 H 0.4155 0.9895 0.2628 0.081 Uiso 1 1 calc R U . . .
C28 C 0.3063(4) 0.9676(6) 0.2697(3) 0.0568(16) Uani 1 1 d . . . . .
C29 C 0.2741(5) 1.0737(7) 0.2191(4) 0.076(2) Uani 1 1 d . . . . .
F1 F 0.3396(3) 0.6084(5) 0.6189(3) 0.1065(16) Uani 1 1 d . . . . .
F2 F 0.4231(3) 0.7307(5) 0.6019(3) 0.1055(16) Uani 1 1 d . . . . .
F3 F 0.4519(3) 0.5435(5) 0.6208(3) 0.1086(16) Uani 1 1 d . . . . .
F4 F 0.2986(3) 0.2693(4) 0.3810(3) 0.1031(16) Uani 1 1 d . . . . .
F5 F 0.4201(3) 0.2726(5) 0.4333(3) 0.1005(15) Uani 1 1 d . . . . .
F6 F 0.3796(3) 0.3323(5) 0.3291(3) 0.1013(15) Uani 1 1 d . U . . .
F7 F 0.5401(3) 0.7956(5) 0.4029(3) 0.1047(16) Uani 1 1 d . . . . .
F8 F 0.5141(3) 0.7167(6) 0.3089(3) 0.128(2) Uani 1 1 d . . . . .
F9 F 0.5428(3) 0.9002(5) 0.3190(3) 0.1170(19) Uani 1 1 d . . . . .
F10 F 0.2219(3) 1.0340(5) 0.1656(3) 0.1139(18) Uani 1 1 d . . . . .
F11 F 0.3279(3) 1.1326(5) 0.1979(3) 0.1012(15) Uani 1 1 d . . . . .
F12 F 0.2384(3) 1.1564(5) 0.2468(3) 0.1004(15) Uani 1 1 d . . . . .
N1 N -0.0208(3) 0.8088(4) 0.2193(3) 0.0584(14) Uani 1 1 d . . . . .
N2 N -0.0044(3) 0.9138(5) 0.3607(3) 0.0612(14) Uani 1 1 d . . . . .
N3 N -0.0473(4) 0.6276(7) 0.4327(4) 0.093(2) Uani 1 1 d . . . . .
N4 N -0.0146(4) 0.6336(5) 0.3878(4) 0.0733(17) Uani 1 1 d . . . . .
N5 N 0.0195(4) 0.6398(5) 0.3434(3) 0.0735(16) Uani 1 1 d . . . . .
Ni1 Ni 0.06054(4) 0.82286(7) 0.31031(4) 0.0468(2) Uani 1 1 d . . . . .
O1 O 0.1394(2) 0.7352(3) 0.27258(19) 0.0468(9) Uani 1 1 d . . . . .
O2 O 0.1586(2) 0.8514(4) 0.3881(2) 0.0548(10) Uani 1 1 d . . . . .
O3 O 0.2633(2) 0.6624(4) 0.2426(2) 0.0616(11) Uani 1 1 d . . . . .
O4 O 0.3011(3) 0.9215(4) 0.4427(2) 0.0713(13) Uani 1 1 d . . . . .
O5 O 0.3235(3) 0.6848(4) 0.4799(2) 0.0713(13) Uani 1 1 d . . . . .
O6 O 0.3117(3) 0.5301(4) 0.3670(2) 0.0668(12) Uani 1 1 d . . . . .
O7 O 0.3834(3) 0.7716(4) 0.3581(3) 0.0679(12) Uani 1 1 d . . . . .
O8 O 0.2558(2) 0.9168(4) 0.2918(2) 0.0561(10) Uani 1 1 d . . . . .
O1W O 0.0904(3) 1.0013(4) 0.2716(2) 0.0713(13) Uani 1 1 d . . . . .
H10C H 0.1403 1.0200 0.2749 0.086 Uiso 1 1 d R U . . .
H10D H 0.0524 1.0554 0.2526 0.086 Uiso 1 1 d R U . . .
O2W O 0.1725(3) 0.5892(4) 0.3966(3) 0.0775(14) Uani 1 1 d . . . . .
H10E H 0.1209 0.6031 0.3858 0.093 Uiso 1 1 d R U . . .
H10F H 0.1927 0.5212 0.4203 0.093 Uiso 1 1 d R U . . .
O3W O 0.1724(3) 0.4711(5) 0.4922(3) 0.0900(16) Uani 1 1 d . . . . .
H10I H 0.1249 0.4250 0.4829 0.108 Uiso 1 1 d R U . . .
H10G H 0.1864 0.4865 0.5381 0.108 Uiso 1 1 d R U . . .
Tb1 Tb 0.25552(2) 0.73345(3) 0.36244(2) 0.05131(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.316(7) . ?
C1 C6 1.392(9) . ?
C1 C2 1.420(8) . ?
C2 C3 1.379(8) . ?
C2 O3 1.383(7) . ?
C3 C4 1.388(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.344(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.442(8) . ?
C7 N1 1.316(8) . ?
C7 H7 0.9500 . ?
C8 N1 1.499(7) . ?
C8 C9 1.473(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.479(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N2 1.491(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.286(9) . ?
C11 C12 1.480(10) . ?
C11 H11 0.9500 . ?
C12 C17 1.367(9) . ?
C12 C13 1.370(9) . ?
C13 C14 1.371(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.372(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.352(9) . ?
C15 H15 0.9500 . ?
C16 O4 1.397(7) . ?
C16 C17 1.427(9) . ?
C17 O2 1.338(7) . ?
C18 O3 1.433(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 O4 1.425(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 F3 1.263(9) . ?
C20 F1 1.341(9) . ?
C20 F2 1.345(10) . ?
C20 C21 1.541(11) . ?
C21 O5 1.254(8) . ?
C21 C22 1.323(11) . ?
C22 C23 1.402(11) . ?
C22 H22 0.9500 . ?
C23 O6 1.232(8) . ?
C23 C24 1.547(12) . ?
C24 F5 1.288(10) . ?
C24 F6 1.335(10) . ?
C24 F4 1.346(10) . ?
C25 F9 1.242(10) . ?
C25 F7 1.283(10) . ?
C25 F8 1.322(10) . ?
C25 C26 1.523(10) . ?
C26 O7 1.272(8) . ?
C26 C27 1.389(10) . ?
C27 C28 1.370(9) . ?
C27 H27 0.9500 . ?
C28 O8 1.241(7) . ?
C28 C29 1.541(10) . ?
C29 F10 1.286(8) . ?
C29 F12 1.312(9) . ?
C29 F11 1.320(8) . ?
N1 Ni1 2.001(5) . ?
N2 Ni1 2.000(5) . ?
N3 N4 1.203(9) . ?
N4 N5 1.213(8) . ?
N5 Ni1 2.285(6) . ?
Ni1 O1 2.016(4) . ?
Ni1 O2 2.022(4) . ?
Ni1 O1W 2.211(4) . ?
Ni1 Tb1 3.4904(8) . ?
O1 Tb1 2.343(4) . ?
O2 Tb1 2.326(4) . ?
O3 Tb1 2.565(4) . ?
O4 Tb1 2.593(4) . ?
O5 Tb1 2.393(4) . ?
O6 Tb1 2.423(4) . ?
O7 Tb1 2.348(5) . ?
O8 Tb1 2.448(4) . ?
O1W H10C 0.8999 . ?
O1W H10D 0.9000 . ?
O2W Tb1 2.388(4) . ?
O2W H10E 0.9000 . ?
O2W H10F 0.9000 . ?
O3W H10I 0.9601 . ?
O3W H10G 0.8997 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 126.9(5) . . ?
O1 C1 C2 117.7(5) . . ?
C6 C1 C2 115.3(5) . . ?
C3 C2 O3 124.3(6) . . ?
C3 C2 C1 122.7(6) . . ?
O3 C2 C1 113.0(5) . . ?
C2 C3 C4 118.3(7) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 121.6(7) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C6 119.6(7) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 122.2(6) . . ?
C1 C6 C7 123.5(6) . . ?
C5 C6 C7 114.1(6) . . ?
N1 C7 C6 125.9(6) . . ?
N1 C7 H7 117.0 . . ?
C6 C7 H7 117.0 . . ?
N1 C8 C9 113.7(6) . . ?
N1 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 C8 112.4(6) . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 N2 112.2(6) . . ?
C9 C10 H10A 109.2 . . ?
N2 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
N2 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 C12 128.9(6) . . ?
N2 C11 H11 115.5 . . ?
C12 C11 H11 115.5 . . ?
C17 C12 C13 121.6(8) . . ?
C17 C12 C11 121.7(6) . . ?
C13 C12 C11 116.6(6) . . ?
C14 C13 C12 121.1(7) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 118.9(7) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C16 C15 C14 120.5(8) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 O4 125.3(7) . . ?
C15 C16 C17 121.6(7) . . ?
O4 C16 C17 113.1(5) . . ?
O2 C17 C12 126.3(6) . . ?
O2 C17 C16 117.5(5) . . ?
C12 C17 C16 116.2(6) . . ?
O3 C18 H18A 109.5 . . ?
O3 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O3 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
F3 C20 F1 108.9(8) . . ?
F3 C20 F2 108.1(8) . . ?
F1 C20 F2 102.7(7) . . ?
F3 C20 C21 117.5(8) . . ?
F1 C20 C21 110.7(7) . . ?
F2 C20 C21 107.8(8) . . ?
O5 C21 C22 129.2(8) . . ?
O5 C21 C20 114.3(7) . . ?
C22 C21 C20 116.0(7) . . ?
C21 C22 C23 121.0(7) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
O6 C23 C22 128.6(7) . . ?
O6 C23 C24 114.6(8) . . ?
C22 C23 C24 116.7(7) . . ?
F5 C24 F6 107.5(7) . . ?
F5 C24 F4 108.4(8) . . ?
F6 C24 F4 104.5(8) . . ?
F5 C24 C23 115.7(8) . . ?
F6 C24 C23 111.5(8) . . ?
F4 C24 C23 108.6(7) . . ?
F9 C25 F7 108.0(8) . . ?
F9 C25 F8 106.8(7) . . ?
F7 C25 F8 100.7(8) . . ?
F9 C25 C26 116.9(9) . . ?
F7 C25 C26 113.3(7) . . ?
F8 C25 C26 109.8(8) . . ?
O7 C26 C27 126.3(6) . . ?
O7 C26 C25 114.9(7) . . ?
C27 C26 C25 118.8(7) . . ?
C28 C27 C26 122.0(6) . . ?
C28 C27 H27 119.0 . . ?
C26 C27 H27 119.0 . . ?
O8 C28 C27 129.0(6) . . ?
O8 C28 C29 113.2(6) . . ?
C27 C28 C29 117.8(6) . . ?
F10 C29 F12 105.0(7) . . ?
F10 C29 F11 108.7(7) . . ?
F12 C29 F11 106.6(6) . . ?
F10 C29 C28 110.5(6) . . ?
F12 C29 C28 111.9(7) . . ?
F11 C29 C28 113.8(6) . . ?
C7 N1 C8 118.0(5) . . ?
C7 N1 Ni1 122.5(4) . . ?
C8 N1 Ni1 119.2(4) . . ?
C11 N2 C10 119.7(6) . . ?
C11 N2 Ni1 122.1(5) . . ?
C10 N2 Ni1 118.0(5) . . ?
N3 N4 N5 178.9(8) . . ?
N4 N5 Ni1 122.0(5) . . ?
N1 Ni1 N2 97.0(2) . . ?
N1 Ni1 O1 91.65(19) . . ?
N2 Ni1 O1 171.3(2) . . ?
N1 Ni1 O2 166.4(2) . . ?
N2 Ni1 O2 92.0(2) . . ?
O1 Ni1 O2 79.33(15) . . ?
N1 Ni1 O1W 86.11(18) . . ?
N2 Ni1 O1W 88.4(2) . . ?
O1 Ni1 O1W 91.29(17) . . ?
O2 Ni1 O1W 83.91(17) . . ?
N1 Ni1 N5 89.3(2) . . ?
N2 Ni1 N5 90.4(2) . . ?
O1 Ni1 N5 90.60(19) . . ?
O2 Ni1 N5 100.9(2) . . ?
O1W Ni1 N5 175.04(19) . . ?
N1 Ni1 Tb1 131.75(16) . . ?
N2 Ni1 Tb1 131.15(18) . . ?
O1 Ni1 Tb1 40.15(11) . . ?
O2 Ni1 Tb1 39.70(10) . . ?
O1W Ni1 Tb1 91.85(12) . . ?
N5 Ni1 Tb1 92.55(15) . . ?
C1 O1 Ni1 121.8(4) . . ?
C1 O1 Tb1 124.1(4) . . ?
Ni1 O1 Tb1 106.17(16) . . ?
C17 O2 Ni1 121.5(4) . . ?
C17 O2 Tb1 127.9(4) . . ?
Ni1 O2 Tb1 106.56(16) . . ?
C2 O3 C18 115.5(5) . . ?
C2 O3 Tb1 116.5(3) . . ?
C18 O3 Tb1 127.9(4) . . ?
C16 O4 C19 115.0(5) . . ?
C16 O4 Tb1 117.9(4) . . ?
C19 O4 Tb1 126.1(4) . . ?
C21 O5 Tb1 135.5(5) . . ?
C23 O6 Tb1 134.5(5) . . ?
C26 O7 Tb1 137.6(4) . . ?
C28 O8 Tb1 133.5(4) . . ?
Ni1 O1W H10C 120.2 . . ?
Ni1 O1W H10D 119.8 . . ?
H10C O1W H10D 120.0 . . ?
Tb1 O2W H10E 119.9 . . ?
Tb1 O2W H10F 120.1 . . ?
H10E O2W H10F 120.0 . . ?
H10I O3W H10G 106.1 . . ?
O2 Tb1 O1 67.00(13) . . ?
O2 Tb1 O7 134.66(16) . . ?
O1 Tb1 O7 129.41(15) . . ?
O2 Tb1 O2W 74.90(16) . . ?
O1 Tb1 O2W 74.75(15) . . ?
O7 Tb1 O2W 144.64(15) . . ?
O2 Tb1 O5 96.43(15) . . ?
O1 Tb1 O5 149.34(15) . . ?
O7 Tb1 O5 80.81(17) . . ?
O2W Tb1 O5 76.06(17) . . ?
O2 Tb1 O6 145.39(15) . . ?
O1 Tb1 O6 107.87(14) . . ?
O7 Tb1 O6 76.41(16) . . ?
O2W Tb1 O6 70.88(15) . . ?
O5 Tb1 O6 70.59(16) . . ?
O2 Tb1 O8 78.35(14) . . ?
O1 Tb1 O8 72.02(13) . . ?
O7 Tb1 O8 71.16(14) . . ?
O2W Tb1 O8 143.40(14) . . ?
O5 Tb1 O8 131.95(16) . . ?
O6 Tb1 O8 134.42(15) . . ?
O2 Tb1 O3 127.59(14) . . ?
O1 Tb1 O3 63.10(13) . . ?
O7 Tb1 O3 73.37(15) . . ?
O2W Tb1 O3 105.60(16) . . ?
O5 Tb1 O3 135.34(15) . . ?
O6 Tb1 O3 68.31(15) . . ?
O8 Tb1 O3 72.24(14) . . ?
O2 Tb1 O4 63.40(15) . . ?
O1 Tb1 O4 122.05(14) . . ?
O7 Tb1 O4 75.00(16) . . ?
O2W Tb1 O4 117.06(17) . . ?
O5 Tb1 O4 64.96(16) . . ?
O6 Tb1 O4 129.96(15) . . ?
O8 Tb1 O4 70.42(15) . . ?
O3 Tb1 O4 136.99(15) . . ?
O2 Tb1 Ni1 33.74(10) . . ?
O1 Tb1 Ni1 33.68(9) . . ?
O7 Tb1 Ni1 147.31(11) . . ?
O2W Tb1 Ni1 67.71(11) . . ?
O5 Tb1 Ni1 123.41(12) . . ?
O6 Tb1 Ni1 129.49(11) . . ?
O8 Tb1 Ni1 76.15(9) . . ?
O3 Tb1 Ni1 96.40(10) . . ?
O4 Tb1 Ni1 94.71(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -179.6(5) . . . . ?
C6 C1 C2 C3 3.1(8) . . . . ?
O1 C1 C2 O3 -2.4(7) . . . . ?
C6 C1 C2 O3 -179.6(5) . . . . ?
O3 C2 C3 C4 -175.2(6) . . . . ?
C1 C2 C3 C4 1.8(9) . . . . ?
C2 C3 C4 C5 -5.3(11) . . . . ?
C3 C4 C5 C6 3.6(11) . . . . ?
O1 C1 C6 C5 178.2(6) . . . . ?
C2 C1 C6 C5 -4.8(8) . . . . ?
O1 C1 C6 C7 -7.4(9) . . . . ?
C2 C1 C6 C7 169.6(6) . . . . ?
C4 C5 C6 C1 1.7(10) . . . . ?
C4 C5 C6 C7 -173.2(6) . . . . ?
C1 C6 C7 N1 9.6(10) . . . . ?
C5 C6 C7 N1 -175.5(6) . . . . ?
N1 C8 C9 C10 -71.7(8) . . . . ?
C8 C9 C10 N2 75.8(8) . . . . ?
N2 C11 C12 C17 -10.4(10) . . . . ?
N2 C11 C12 C13 171.7(7) . . . . ?
C17 C12 C13 C14 3.6(11) . . . . ?
C11 C12 C13 C14 -178.5(7) . . . . ?
C12 C13 C14 C15 -1.5(12) . . . . ?
C13 C14 C15 C16 -0.3(12) . . . . ?
C14 C15 C16 O4 179.9(7) . . . . ?
C14 C15 C16 C17 0.1(11) . . . . ?
C13 C12 C17 O2 174.0(6) . . . . ?
C11 C12 C17 O2 -3.7(10) . . . . ?
C13 C12 C17 C16 -3.6(9) . . . . ?
C11 C12 C17 C16 178.6(5) . . . . ?
C15 C16 C17 O2 -176.1(6) . . . . ?
O4 C16 C17 O2 4.1(8) . . . . ?
C15 C16 C17 C12 1.8(9) . . . . ?
O4 C16 C17 C12 -178.0(5) . . . . ?
F3 C20 C21 O5 -168.3(8) . . . . ?
F1 C20 C21 O5 65.6(10) . . . . ?
F2 C20 C21 O5 -46.0(10) . . . . ?
F3 C20 C21 C22 19.4(12) . . . . ?
F1 C20 C21 C22 -106.6(9) . . . . ?
F2 C20 C21 C22 141.7(8) . . . . ?
O5 C21 C22 C23 4.1(14) . . . . ?
C20 C21 C22 C23 175.0(7) . . . . ?
C21 C22 C23 O6 2.6(14) . . . . ?
C21 C22 C23 C24 -173.4(8) . . . . ?
O6 C23 C24 F5 164.8(7) . . . . ?
C22 C23 C24 F5 -18.6(12) . . . . ?
O6 C23 C24 F6 41.5(10) . . . . ?
C22 C23 C24 F6 -141.9(8) . . . . ?
O6 C23 C24 F4 -73.1(9) . . . . ?
C22 C23 C24 F4 103.5(9) . . . . ?
F9 C25 C26 O7 -170.4(7) . . . . ?
F7 C25 C26 O7 -43.8(12) . . . . ?
F8 C25 C26 O7 67.8(10) . . . . ?
F9 C25 C26 C27 12.5(12) . . . . ?
F7 C25 C26 C27 139.1(9) . . . . ?
F8 C25 C26 C27 -109.3(9) . . . . ?
O7 C26 C27 C28 1.9(12) . . . . ?
C25 C26 C27 C28 178.7(7) . . . . ?
C26 C27 C28 O8 0.6(12) . . . . ?
C26 C27 C28 C29 -179.0(7) . . . . ?
O8 C28 C29 F10 -60.8(9) . . . . ?
C27 C28 C29 F10 118.8(8) . . . . ?
O8 C28 C29 F12 55.8(8) . . . . ?
C27 C28 C29 F12 -124.6(7) . . . . ?
O8 C28 C29 F11 176.7(6) . . . . ?
C27 C28 C29 F11 -3.7(10) . . . . ?
C6 C7 N1 C8 -174.2(6) . . . . ?
C6 C7 N1 Ni1 12.4(9) . . . . ?
C9 C8 N1 C7 -130.0(7) . . . . ?
C9 C8 N1 Ni1 43.6(8) . . . . ?
C12 C11 N2 C10 -177.5(6) . . . . ?
C12 C11 N2 Ni1 -2.5(9) . . . . ?
C9 C10 N2 C11 124.4(7) . . . . ?
C9 C10 N2 Ni1 -50.7(7) . . . . ?
C6 C1 O1 Ni1 -16.1(7) . . . . ?
C2 C1 O1 Ni1 167.0(4) . . . . ?
C6 C1 O1 Tb1 -160.8(4) . . . . ?
C2 C1 O1 Tb1 22.3(6) . . . . ?
C12 C17 O2 Ni1 26.9(8) . . . . ?
C16 C17 O2 Ni1 -155.5(4) . . . . ?
C12 C17 O2 Tb1 -178.9(5) . . . . ?
C16 C17 O2 Tb1 -1.2(7) . . . . ?
C3 C2 O3 C18 -14.0(9) . . . . ?
C1 C2 O3 C18 168.8(5) . . . . ?
C3 C2 O3 Tb1 161.9(5) . . . . ?
C1 C2 O3 Tb1 -15.3(6) . . . . ?
C15 C16 O4 C19 5.8(9) . . . . ?
C17 C16 O4 C19 -174.4(5) . . . . ?
C15 C16 O4 Tb1 175.2(5) . . . . ?
C17 C16 O4 Tb1 -5.0(6) . . . . ?
C22 C21 O5 Tb1 -10.4(13) . . . . ?
C20 C21 O5 Tb1 178.6(5) . . . . ?
C22 C23 O6 Tb1 -3.0(13) . . . . ?
C24 C23 O6 Tb1 173.1(5) . . . . ?
C27 C26 O7 Tb1 2.3(12) . . . . ?
C25 C26 O7 Tb1 -174.6(5) . . . . ?
C27 C28 O8 Tb1 -6.8(11) . . . . ?
C29 C28 O8 Tb1 172.8(4) . . . . ?

_refine_diff_density_max         0.657
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.154

_shelxl_version_number           2013-2

