# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_cpd4
_audit_block_doi                 10.5517/cc14cg76
_database_code_depnum_ccdc_archive 'CCDC 1053697'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.poly.2015.04.022 2015
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H19 Gd N4 Ni O16'
_chemical_formula_weight         763.33

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'

_cell_length_a                   9.9098(14)
_cell_length_b                   15.519(2)
_cell_length_c                   16.211(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.695(15)
_cell_angle_gamma                90.00
_cell_volume                     2484.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.041
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1500
_exptl_absorpt_coefficient_mu    3.491
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.3722
_exptl_absorpt_correction_T_max  0.5116
_exptl_absorpt_process_details   'X-SHAPE (Stoe & Cie, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Imaging Plate Detector System'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17331
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         24.18
_reflns_number_total             3917
_reflns_number_gt                3765
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE-IPDS software (Stoe, 2.87, 1997)'
_computing_cell_refinement       'STOE-IPDS software (Stoe, 2.87, 1997)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1996)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+2.0176P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3917
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0183
_refine_ls_wR_factor_ref         0.0442
_refine_ls_wR_factor_gt          0.0437
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.004
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.280102(11) 0.314866(7) 0.139394(7) 0.01256(6) Uani 1 d . . .
Ni Ni 0.18853(3) 0.098670(19) 0.166163(18) 0.01302(8) Uani 1 d . . .
O1 O 0.33703(16) 0.16813(11) 0.12196(11) 0.0160(4) Uani 1 d . . .
C1 C 0.4530(2) 0.13846(16) 0.10075(14) 0.0144(5) Uani 1 d . . .
C2 C 0.5443(2) 0.19830(16) 0.07042(16) 0.0180(5) Uani 1 d . . .
C3 C 0.6691(3) 0.17374(18) 0.04869(18) 0.0245(6) Uani 1 d . . .
H3 H 0.7286 0.2152 0.0282 0.027 Uiso 1 calc R . .
C4 C 0.7090(3) 0.08732(18) 0.05671(17) 0.0247(6) Uani 1 d . . .
H4 H 0.7967 0.0705 0.0432 0.027 Uiso 1 calc R . .
C5 C 0.6226(2) 0.02724(17) 0.08377(16) 0.0215(5) Uani 1 d . . .
H5 H 0.6499 -0.0314 0.0877 0.024 Uiso 1 calc R . .
C6 C 0.4930(2) 0.05107(16) 0.10600(15) 0.0171(5) Uani 1 d . . .
C7 C 0.4059(2) -0.01769(16) 0.12781(15) 0.0192(5) Uani 1 d . . .
H7 H 0.4435 -0.0740 0.1272 0.021 Uiso 1 calc R . .
O3 O 0.49377(17) 0.28106(11) 0.06638(11) 0.0200(4) Uani 1 d . . .
C8 C 0.5661(3) 0.34196(19) 0.01935(19) 0.0277(6) Uani 1 d . . .
H8A H 0.5218 0.3984 0.0205 0.030 Uiso 1 calc R . .
H8B H 0.5659 0.3221 -0.0380 0.030 Uiso 1 calc R . .
H8C H 0.6596 0.3468 0.0436 0.030 Uiso 1 calc R . .
O5 O 0.28814(16) -0.01287(11) 0.14733(10) 0.0191(4) Uani 1 d . . .
O2 O 0.11903(15) 0.21885(10) 0.18293(10) 0.0143(3) Uani 1 d . . .
C9 C -0.0053(2) 0.23969(16) 0.19933(14) 0.0131(5) Uani 1 d . . .
C10 C -0.0491(2) 0.32510(15) 0.18578(15) 0.0148(5) Uani 1 d . . .
C11 C -0.1730(2) 0.35315(16) 0.20720(16) 0.0198(5) Uani 1 d . . .
H11 H -0.1987 0.4117 0.1987 0.022 Uiso 1 calc R . .
C12 C -0.2605(2) 0.29567(18) 0.24128(17) 0.0220(6) Uani 1 d . . .
H12 H -0.3453 0.3151 0.2575 0.024 Uiso 1 calc R . .
C13 C -0.2242(2) 0.21095(17) 0.25143(16) 0.0202(5) Uani 1 d . . .
H13 H -0.2855 0.1717 0.2735 0.022 Uiso 1 calc R . .
C14 C -0.0979(2) 0.18098(15) 0.22985(16) 0.0162(5) Uani 1 d . . .
C15 C -0.0737(2) 0.08973(17) 0.23634(16) 0.0205(6) Uani 1 d . . .
H15 H -0.1420 0.0571 0.2599 0.023 Uiso 1 calc R . .
O4 O 0.04381(16) 0.37819(11) 0.15094(11) 0.0176(4) Uani 1 d . . .
C16 C -0.0147(3) 0.44368(17) 0.09613(17) 0.0229(6) Uani 1 d . . .
H16A H 0.0577 0.4779 0.0746 0.025 Uiso 1 calc R . .
H16B H -0.0727 0.4813 0.1265 0.025 Uiso 1 calc R . .
H16C H -0.0689 0.4164 0.0500 0.025 Uiso 1 calc R . .
O6 O 0.02397(16) 0.04835(10) 0.21533(11) 0.0189(4) Uani 1 d . . .
O7 O 0.27693(18) 0.08507(12) 0.28480(11) 0.0218(4) Uani 1 d . . .
H7A H 0.244(3) 0.112(2) 0.3235(19) 0.045(10) Uiso 1 d . . .
H7B H 0.362(2) 0.084(2) 0.292(2) 0.052(11) Uiso 1 d . . .
N1 N 0.0914(2) 0.09073(13) 0.04855(14) 0.0194(5) Uani 1 d . . .
C17 C 0.0504(2) 0.10583(15) -0.01737(16) 0.0178(5) Uani 1 d . . .
C18 C -0.0030(3) 0.12678(19) -0.10090(16) 0.0273(6) Uani 1 d . . .
H18A H -0.0955 0.1046 -0.1104 0.030 Uiso 1 calc R . .
H18B H 0.0541 0.1004 -0.1406 0.030 Uiso 1 calc R . .
H18C H -0.0036 0.1895 -0.1082 0.030 Uiso 1 calc R . .
O8 O 0.12804(19) 0.27686(12) 0.01542(11) 0.0266(4) Uani 1 d . . .
O9 O 0.26121(19) 0.38172(12) -0.00532(12) 0.0278(4) Uani 1 d . . .
N2 N 0.1689(2) 0.33133(14) -0.03391(13) 0.0200(5) Uani 1 d . . .
O10 O 0.1208(2) 0.33597(14) -0.10587(12) 0.0318(5) Uani 1 d . . .
O11 O 0.40989(18) 0.26320(12) 0.26687(11) 0.0241(4) Uani 1 d . . .
O12 O 0.25722(18) 0.35922(12) 0.28295(11) 0.0237(4) Uani 1 d . . .
N3 N 0.3451(2) 0.30702(14) 0.31614(14) 0.0224(5) Uani 1 d . . .
O13 O 0.3648(2) 0.30035(14) 0.39100(12) 0.0391(5) Uani 1 d . . .
O14 O 0.27610(16) 0.47877(12) 0.14194(11) 0.0242(4) Uani 1 d . . .
O15 O 0.47043(17) 0.42290(11) 0.17716(12) 0.0246(4) Uani 1 d . . .
N4 N 0.3990(2) 0.48972(13) 0.16620(13) 0.0184(5) Uani 1 d . . .
O16 O 0.44545(19) 0.56227(12) 0.17786(13) 0.0298(4) Uani 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
Gd O2 2.3347(16) . ?
Gd O1 2.3685(17) . ?
Gd O12 2.4550(18) . ?
Gd O11 2.4764(18) . ?
Gd O8 2.4824(18) . ?
Gd O14 2.5443(19) . ?
Gd O9 2.5579(19) . ?
Gd O15 2.5600(18) . ?
Gd O4 2.5604(16) . ?
Gd O3 2.5632(17) . ?
Ni O1 2.0034(17) . ?
Ni O2 2.0143(16) . ?
Ni O5 2.0280(17) . ?
Ni O6 2.0291(17) . ?
Ni O7 2.0578(18) . ?
Ni N1 2.068(2) . ?
O1 C1 1.310(3) . ?
C1 C2 1.413(4) . ?
C1 C6 1.413(4) . ?
C2 C3 1.368(4) . ?
C2 O3 1.378(3) . ?
C3 C4 1.401(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.363(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.412(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.434(4) . ?
C7 O5 1.236(3) . ?
C7 H7 0.9500 . ?
O3 C8 1.441(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
O2 C9 1.322(3) . ?
C9 C10 1.406(3) . ?
C9 C14 1.411(3) . ?
C10 C11 1.374(4) . ?
C10 O4 1.389(3) . ?
C11 C12 1.390(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.369(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.406(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.439(4) . ?
C15 O6 1.233(3) . ?
C15 H15 0.9500 . ?
O4 C16 1.440(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O7 H7A 0.84(3) . ?
O7 H7B 0.84(2) . ?
N1 C17 1.136(3) . ?
C17 C18 1.450(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
O8 N2 1.253(3) . ?
O9 N2 1.262(3) . ?
N2 O10 1.226(3) . ?
O11 N3 1.264(3) . ?
O12 N3 1.275(3) . ?
N3 O13 1.218(3) . ?
O14 N4 1.261(3) . ?
O15 N4 1.260(3) . ?
N4 O16 1.225(3) . ?

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 Gd O1 66.29(6) . . ?
O2 Gd O12 76.93(6) . . ?
O1 Gd O12 115.09(6) . . ?
O2 Gd O11 82.09(6) . . ?
O1 Gd O11 71.08(6) . . ?
O12 Gd O11 51.81(6) . . ?
O2 Gd O8 73.04(6) . . ?
O1 Gd O8 79.03(6) . . ?
O12 Gd O8 137.48(6) . . ?
O11 Gd O8 146.94(6) . . ?
O2 Gd O14 128.40(5) . . ?
O1 Gd O14 165.31(5) . . ?
O12 Gd O14 72.64(6) . . ?
O11 Gd O14 108.54(6) . . ?
O8 Gd O14 103.97(6) . . ?
O2 Gd O9 122.38(6) . . ?
O1 Gd O9 106.31(6) . . ?
O12 Gd O9 138.60(6) . . ?
O11 Gd O9 152.96(6) . . ?
O8 Gd O9 50.20(6) . . ?
O14 Gd O9 67.00(6) . . ?
O2 Gd O15 148.68(6) . . ?
O1 Gd O15 118.69(6) . . ?
O12 Gd O15 73.33(6) . . ?
O11 Gd O15 71.96(6) . . ?
O8 Gd O15 137.37(6) . . ?
O14 Gd O15 49.73(5) . . ?
O9 Gd O15 87.18(6) . . ?
O2 Gd O4 64.59(5) . . ?
O1 Gd O4 127.30(5) . . ?
O12 Gd O4 70.56(6) . . ?
O11 Gd O4 118.62(6) . . ?
O8 Gd O4 69.64(6) . . ?
O14 Gd O4 66.39(5) . . ?
O9 Gd O4 84.99(6) . . ?
O15 Gd O4 113.05(5) . . ?
O2 Gd O3 128.32(5) . . ?
O1 Gd O3 62.24(5) . . ?
O12 Gd O3 129.72(6) . . ?
O11 Gd O3 85.80(6) . . ?
O8 Gd O3 92.70(6) . . ?
O14 Gd O3 103.10(6) . . ?
O9 Gd O3 70.17(6) . . ?
O15 Gd O3 67.92(6) . . ?
O4 Gd O3 155.14(6) . . ?
O1 Ni O2 79.59(7) . . ?
O1 Ni O5 91.41(7) . . ?
O2 Ni O5 170.61(7) . . ?
O1 Ni O6 170.08(7) . . ?
O2 Ni O6 90.49(7) . . ?
O5 Ni O6 98.48(7) . . ?
O1 Ni O7 96.92(7) . . ?
O2 Ni O7 95.33(7) . . ?
O5 Ni O7 82.99(7) . . ?
O6 Ni O7 83.56(7) . . ?
O1 Ni N1 90.13(8) . . ?
O2 Ni N1 92.36(7) . . ?
O5 Ni N1 90.33(8) . . ?
O6 Ni N1 90.63(8) . . ?
O7 Ni N1 170.38(8) . . ?
C1 O1 Ni 126.20(15) . . ?
C1 O1 Gd 126.30(15) . . ?
Ni O1 Gd 106.59(7) . . ?
O1 C1 C2 117.4(2) . . ?
O1 C1 C6 124.7(2) . . ?
C2 C1 C6 117.9(2) . . ?
C3 C2 O3 125.5(2) . . ?
C3 C2 C1 121.7(2) . . ?
O3 C2 C1 112.9(2) . . ?
C2 C3 C4 119.8(2) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.3(2) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 120.8(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.5(2) . . ?
C5 C6 C7 116.5(2) . . ?
C1 C6 C7 123.9(2) . . ?
O5 C7 C6 128.1(2) . . ?
O5 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
C2 O3 C8 116.2(2) . . ?
C2 O3 Gd 118.64(14) . . ?
C8 O3 Gd 125.12(15) . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 O5 Ni 124.86(16) . . ?
C9 O2 Ni 126.04(15) . . ?
C9 O2 Gd 125.20(14) . . ?
Ni O2 Gd 107.48(7) . . ?
O2 C9 C10 118.7(2) . . ?
O2 C9 C14 123.8(2) . . ?
C10 C9 C14 117.5(2) . . ?
C11 C10 O4 123.4(2) . . ?
C11 C10 C9 122.0(2) . . ?
O4 C10 C9 114.6(2) . . ?
C10 C11 C12 119.8(2) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 121.2(2) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C9 119.4(2) . . ?
C13 C14 C15 117.0(2) . . ?
C9 C14 C15 123.5(2) . . ?
O6 C15 C14 128.5(2) . . ?
O6 C15 H15 115.8 . . ?
C14 C15 H15 115.8 . . ?
C10 O4 C16 115.00(18) . . ?
C10 O4 Gd 116.26(13) . . ?
C16 O4 Gd 123.38(14) . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 O6 Ni 125.64(16) . . ?
Ni O7 H7A 119(2) . . ?
Ni O7 H7B 118(2) . . ?
H7A O7 H7B 111(3) . . ?
C17 N1 Ni 163.44(19) . . ?
N1 C17 C18 178.8(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 O8 Gd 98.62(14) . . ?
N2 O9 Gd 94.69(14) . . ?
O10 N2 O8 121.7(2) . . ?
O10 N2 O9 121.8(2) . . ?
O8 N2 O9 116.5(2) . . ?
N3 O11 Gd 95.56(14) . . ?
N3 O12 Gd 96.26(14) . . ?
O13 N3 O11 122.4(2) . . ?
O13 N3 O12 121.5(2) . . ?
O11 N3 O12 116.1(2) . . ?
N4 O14 Gd 97.12(13) . . ?
N4 O15 Gd 96.38(13) . . ?
O16 N4 O15 122.4(2) . . ?
O16 N4 O14 120.9(2) . . ?
O15 N4 O14 116.8(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
O7 H7A O10 0.84(3) 1.92(3) 2.736(3) 163(3) 2
O7 H7B O16 0.84(2) 1.96(2) 2.791(3) 169(4) 4_656

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        24.18
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.068

####################################################################### 
# 
# 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 1581928'
_audit_update_record             
;
2017-10-24 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H18 Gd1 N3 Ni1 O17'
_chemical_formula_sum            'C16 H18 Gd N3 Ni O17'
_chemical_formula_weight         740.29
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'

_cell_length_a                   9.3439(5)
_cell_length_b                   18.1612(7)
_cell_length_c                   14.3985(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.594(6)
_cell_angle_gamma                90
_cell_volume                     2341.63(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    13463
_cell_measurement_theta_min      2.9443
_cell_measurement_theta_max      31.8949
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    2.1
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1452
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.27 (release 29-05-2008 CrysAlis171 .NET)
        (compiled May 29 2008,13:12:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.237
_exptl_absorpt_correction_T_max  0.789

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       ω-φ
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_orient_matrix_ub_11      0.0251735928
_diffrn_orient_matrix_ub_12      0.0327289934
_diffrn_orient_matrix_ub_13      0.0266565994
_diffrn_orient_matrix_ub_21      0.0427815385
_diffrn_orient_matrix_ub_22      -0.0213647232
_diffrn_orient_matrix_ub_23      0.0393458786
_diffrn_orient_matrix_ub_31      0.0615949012
_diffrn_orient_matrix_ub_32      0.0013213297
_diffrn_orient_matrix_ub_33      -0.0194854981
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_number            16403
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             4277
_reflns_number_gt                3735
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0185P)²+2.8493P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4277
_refine_ls_number_parameters     351
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0492
_refine_ls_wR_factor_gt          0.0469
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.082

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0452(3) 0.57815(17) 0.8309(2) 0.0190(6) Uani 1 1 d . . .
C2 C 0.0363(3) 0.64943(18) 0.8679(2) 0.0209(7) Uani 1 1 d . . .
C3 C -0.0563(4) 0.6644(2) 0.9241(2) 0.0281(8) Uani 1 1 d . . .
H3 H -0.0603 0.7127 0.9486 0.034 Uiso 1 1 calc R . .
C4 C -0.1446(4) 0.6085(2) 0.9451(3) 0.0326(8) Uani 1 1 d . . .
H4 H -0.2089 0.6188 0.984 0.039 Uiso 1 1 calc R . .
C5 C -0.1390(4) 0.5392(2) 0.9100(3) 0.0322(8) Uani 1 1 d . . .
H5 H -0.201 0.5018 0.9236 0.039 Uiso 1 1 calc R . .
C6 C -0.0418(4) 0.52234(19) 0.8535(2) 0.0242(7) Uani 1 1 d . . .
C7 C 0.0986(4) 0.77669(18) 0.8565(3) 0.0284(8) Uani 1 1 d . . .
H7A H -0.0086 0.7865 0.8302 0.043 Uiso 1 1 calc R . .
H7B H 0.1544 0.8079 0.8235 0.043 Uiso 1 1 calc R . .
H7C H 0.13 0.7876 0.9261 0.043 Uiso 1 1 calc R . .
C8 C -0.0373(4) 0.4459(2) 0.8246(2) 0.0312(8) Uani 1 1 d . . .
H8 H -0.1112 0.4145 0.8369 0.037 Uiso 1 1 calc R . .
C10 C 0.4699(3) 0.51913(18) 0.6807(2) 0.0203(7) Uani 1 1 d . . .
C11 C 0.5690(4) 0.57434(19) 0.6707(2) 0.0240(7) Uani 1 1 d . . .
C12 C 0.6823(4) 0.5602(2) 0.6302(3) 0.0347(9) Uani 1 1 d . . .
H12 H 0.7475 0.5986 0.6234 0.042 Uiso 1 1 calc R . .
C13 C 0.7015(4) 0.4889(2) 0.5992(3) 0.0405(10) Uani 1 1 d . . .
H13 H 0.7789 0.4791 0.5701 0.049 Uiso 1 1 calc R . .
C14 C 0.6096(4) 0.4336(2) 0.6104(3) 0.0358(9) Uani 1 1 d . . .
H14 H 0.6243 0.3853 0.5895 0.043 Uiso 1 1 calc R . .
C15 C 0.4933(4) 0.44679(19) 0.6523(2) 0.0263(7) Uani 1 1 d . . .
C16 C 0.6371(4) 0.7022(2) 0.6989(3) 0.0335(8) Uani 1 1 d . . .
H16A H 0.7404 0.6878 0.7312 0.05 Uiso 1 1 calc R . .
H16B H 0.6113 0.7458 0.7307 0.05 Uiso 1 1 calc R . .
H16C H 0.6268 0.7134 0.6307 0.05 Uiso 1 1 calc R . .
C17 C 0.4088(4) 0.38402(19) 0.6676(2) 0.0288(8) Uani 1 1 d . . .
H17 H 0.4314 0.3387 0.6421 0.035 Uiso 1 1 calc R . .
N1 N 0.4898(3) 0.66989(14) 0.93658(18) 0.0195(6) Uani 1 1 d . . .
N2 N 0.0132(3) 0.65542(14) 0.57346(18) 0.0201(6) Uani 1 1 d . . .
N3 N 0.3033(3) 0.79503(15) 0.62778(19) 0.0232(6) Uani 1 1 d . . .
O1 O 0.1355(2) 0.56913(11) 0.77554(15) 0.0193(5) Uani 1 1 d . . .
O2 O 0.1279(2) 0.70026(11) 0.84155(15) 0.0208(5) Uani 1 1 d . . .
O3 O 0.3589(2) 0.53874(11) 0.71477(15) 0.0189(5) Uani 1 1 d . . .
O4 O 0.5378(2) 0.64239(12) 0.70467(16) 0.0243(5) Uani 1 1 d . . .
O5 O 0.0501(3) 0.41698(13) 0.78636(17) 0.0286(5) Uani 1 1 d . . .
O6 O 0.3102(3) 0.38148(12) 0.70977(17) 0.0274(5) Uani 1 1 d . . .
O7 O 0.4575(3) 0.72468(12) 0.88013(16) 0.0256(5) Uani 1 1 d . . .
O8 O 0.4321(2) 0.60917(12) 0.90068(15) 0.0239(5) Uani 1 1 d . . .
O9 O 0.5700(2) 0.67487(12) 1.01894(15) 0.0243(5) Uani 1 1 d . . .
O10 O 0.0303(2) 0.70224(12) 0.63978(15) 0.0239(5) Uani 1 1 d . . .
O11 O 0.1234(2) 0.61334(12) 0.57654(15) 0.0210(5) Uani 1 1 d . . .
O12 O -0.1038(2) 0.64995(13) 0.50788(16) 0.0267(5) Uani 1 1 d . . .
O13 O 0.3048(3) 0.73265(12) 0.58980(16) 0.0253(5) Uani 1 1 d . . .
O14 O 0.3077(3) 0.79515(13) 0.71714(16) 0.0273(5) Uani 1 1 d . . .
O15 O 0.2997(3) 0.85200(13) 0.58326(18) 0.0346(6) Uani 1 1 d . . .
Ni2 Ni 0.21336(4) 0.47072(2) 0.74915(3) 0.01875(9) Uani 1 1 d . . .
Gd1 Gd 0.288094(16) 0.659720(8) 0.737838(10) 0.01614(5) Uani 1 1 d . . .
O16 O 0.0739(3) 0.47025(12) 0.60892(15) 0.0237(5) Uani 1 1 d D . .
H161 H 0.093(4) 0.4363(11) 0.574(2) 0.028 Uiso 1 1 d D . .
H162 H 0.094(4) 0.5079(9) 0.581(2) 0.028 Uiso 1 1 d D . .
O17 O 0.3433(3) 0.46351(13) 0.89158(17) 0.03 Uani 1 1 d D . .
H17A H 0.404(3) 0.4983(11) 0.910(2) 0.036 Uiso 1 1 d D . .
H17B H 0.394(3) 0.4267(10) 0.916(2) 0.036 Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.326(4) . ?
C1 C6 1.394(4) . ?
C1 C2 1.411(4) . ?
C2 C3 1.369(4) . ?
C2 O2 1.383(4) . ?
C3 C4 1.395(5) . ?
C3 H3 0.95 . ?
C4 C5 1.362(5) . ?
C4 H4 0.95 . ?
C5 C6 1.415(5) . ?
C5 H5 0.95 . ?
C6 C8 1.453(5) . ?
C7 O2 1.443(4) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 O5 1.227(4) . ?
C8 H8 0.95 . ?
C10 O3 1.317(4) . ?
C10 C11 1.399(5) . ?
C10 C15 1.411(5) . ?
C11 C12 1.371(5) . ?
C11 O4 1.390(4) . ?
C12 C13 1.397(6) . ?
C12 H12 0.95 . ?
C13 C14 1.360(6) . ?
C13 H13 0.95 . ?
C14 C15 1.406(5) . ?
C14 H14 0.95 . ?
C15 C17 1.439(5) . ?
C16 O4 1.445(4) . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 O6 1.240(4) . ?
C17 H17 0.95 . ?
N1 O9 1.212(3) . ?
N1 O7 1.266(3) . ?
N1 O8 1.271(3) . ?
N1 Gd1 2.949(3) . ?
N2 O12 1.227(3) . ?
N2 O10 1.254(3) . ?
N2 O11 1.273(3) . ?
N2 Gd1 2.955(3) . ?
N3 O15 1.213(3) . ?
N3 O13 1.260(3) . ?
N3 O14 1.276(3) . ?
N3 Gd1 2.949(3) . ?
O1 Ni2 2.007(2) . ?
O1 Gd1 2.340(2) . ?
O2 Gd1 2.508(2) . ?
O3 Ni2 2.001(2) . ?
O3 Gd1 2.345(2) . ?
O4 Gd1 2.532(2) . ?
O5 Ni2 2.008(2) . ?
O6 Ni2 2.015(2) . ?
O7 Gd1 2.499(2) . ?
O8 Gd1 2.520(2) . ?
O10 Gd1 2.540(2) . ?
O11 Gd1 2.536(2) . ?
O13 Gd1 2.552(2) . ?
O14 Gd1 2.491(2) . ?
Ni2 O16 2.067(2) . ?
Ni2 O17 2.068(2) . ?
O16 H161 0.85(3) . ?
O16 H162 0.841(10) . ?
O17 H17A 0.841(10) . ?
O17 H17B 0.837(10) . ?

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 124.3(3) . . ?
O1 C1 C2 117.1(3) . . ?
C6 C1 C2 118.5(3) . . ?
C3 C2 O2 125.0(3) . . ?
C3 C2 C1 121.3(3) . . ?
O2 C2 C1 113.6(3) . . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.8(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 119.3(3) . . ?
C1 C6 C8 124.1(3) . . ?
C5 C6 C8 116.6(3) . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O5 C8 C6 128.0(3) . . ?
O5 C8 H8 116 . . ?
C6 C8 H8 116 . . ?
O3 C10 C11 117.3(3) . . ?
O3 C10 C15 124.3(3) . . ?
C11 C10 C15 118.4(3) . . ?
C12 C11 O4 125.5(3) . . ?
C12 C11 C10 121.5(3) . . ?
O4 C11 C10 112.9(3) . . ?
C11 C12 C13 119.7(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 121.1(4) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C14 C15 C10 119.0(3) . . ?
C14 C15 C17 117.1(3) . . ?
C10 C15 C17 123.8(3) . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O6 C17 C15 128.4(3) . . ?
O6 C17 H17 115.8 . . ?
C15 C17 H17 115.8 . . ?
O9 N1 O7 122.5(3) . . ?
O9 N1 O8 122.3(3) . . ?
O7 N1 O8 115.2(2) . . ?
O9 N1 Gd1 178.5(2) . . ?
O7 N1 Gd1 57.11(14) . . ?
O8 N1 Gd1 58.10(14) . . ?
O12 N2 O10 122.2(3) . . ?
O12 N2 O11 120.8(3) . . ?
O10 N2 O11 117.0(2) . . ?
O12 N2 Gd1 176.0(2) . . ?
O10 N2 Gd1 58.64(14) . . ?
O11 N2 Gd1 58.56(14) . . ?
O15 N3 O13 122.7(3) . . ?
O15 N3 O14 121.3(3) . . ?
O13 N3 O14 116.0(2) . . ?
O15 N3 Gd1 175.3(2) . . ?
O13 N3 Gd1 59.47(14) . . ?
O14 N3 Gd1 56.77(14) . . ?
C1 O1 Ni2 123.46(19) . . ?
C1 O1 Gd1 125.95(19) . . ?
Ni2 O1 Gd1 107.72(9) . . ?
C2 O2 C7 116.2(2) . . ?
C2 O2 Gd1 119.26(17) . . ?
C7 O2 Gd1 122.85(18) . . ?
C10 O3 Ni2 126.0(2) . . ?
C10 O3 Gd1 126.15(19) . . ?
Ni2 O3 Gd1 107.72(9) . . ?
C11 O4 C16 116.4(3) . . ?
C11 O4 Gd1 118.27(18) . . ?
C16 O4 Gd1 124.0(2) . . ?
C8 O5 Ni2 124.4(2) . . ?
C17 O6 Ni2 124.3(2) . . ?
N1 O7 Gd1 97.72(17) . . ?
N1 O8 Gd1 96.55(16) . . ?
N2 O10 Gd1 96.41(17) . . ?
N2 O11 Gd1 96.08(16) . . ?
N3 O13 Gd1 95.36(16) . . ?
N3 O14 Gd1 97.86(17) . . ?
O3 Ni2 O1 78.79(8) . . ?
O3 Ni2 O5 170.94(9) . . ?
O1 Ni2 O5 92.19(9) . . ?
O3 Ni2 O6 92.03(9) . . ?
O1 Ni2 O6 170.41(9) . . ?
O5 Ni2 O6 96.92(10) . . ?
O3 Ni2 O16 92.54(9) . . ?
O1 Ni2 O16 91.55(9) . . ?
O5 Ni2 O16 86.76(9) . . ?
O6 Ni2 O16 86.00(9) . . ?
O3 Ni2 O17 92.08(9) . . ?
O1 Ni2 O17 90.60(9) . . ?
O5 Ni2 O17 88.87(10) . . ?
O6 Ni2 O17 92.55(10) . . ?
O16 Ni2 O17 175.20(9) . . ?
O3 Ni2 Gd1 39.45(6) . . ?
O1 Ni2 Gd1 39.35(6) . . ?
O5 Ni2 Gd1 131.52(7) . . ?
O6 Ni2 Gd1 131.38(7) . . ?
O16 Ni2 Gd1 92.12(6) . . ?
O17 Ni2 Gd1 92.27(7) . . ?
O1 Gd1 O3 65.76(7) . . ?
O1 Gd1 O14 142.42(7) . . ?
O3 Gd1 O14 151.03(7) . . ?
O1 Gd1 O7 115.28(7) . . ?
O3 Gd1 O7 114.85(7) . . ?
O14 Gd1 O7 65.22(7) . . ?
O1 Gd1 O2 63.98(7) . . ?
O3 Gd1 O2 126.85(7) . . ?
O14 Gd1 O2 81.84(7) . . ?
O7 Gd1 O2 73.70(7) . . ?
O1 Gd1 O8 74.14(7) . . ?
O3 Gd1 O8 72.13(7) . . ?
O14 Gd1 O8 115.67(7) . . ?
O7 Gd1 O8 50.51(7) . . ?
O2 Gd1 O8 78.69(7) . . ?
O1 Gd1 O4 127.73(7) . . ?
O3 Gd1 O4 62.90(7) . . ?
O14 Gd1 O4 89.83(7) . . ?
O7 Gd1 O4 79.11(8) . . ?
O2 Gd1 O4 152.62(7) . . ?
O8 Gd1 O4 81.62(7) . . ?
O1 Gd1 O11 74.24(7) . . ?
O3 Gd1 O11 71.40(7) . . ?
O14 Gd1 O11 105.34(7) . . ?
O7 Gd1 O11 169.90(7) . . ?
O2 Gd1 O11 109.48(7) . . ?
O8 Gd1 O11 138.97(7) . . ?
O4 Gd1 O11 97.87(7) . . ?
O1 Gd1 O10 78.38(7) . . ?
O3 Gd1 O10 117.85(7) . . ?
O14 Gd1 O10 73.96(7) . . ?
O7 Gd1 O10 126.20(7) . . ?
O2 Gd1 O10 66.98(7) . . ?
O8 Gd1 O10 142.91(7) . . ?
O4 Gd1 O10 135.40(7) . . ?
O11 Gd1 O10 50.26(7) . . ?
O1 Gd1 O13 138.18(7) . . ?
O3 Gd1 O13 106.32(7) . . ?
O14 Gd1 O13 50.46(7) . . ?
O7 Gd1 O13 105.33(7) . . ?
O2 Gd1 O13 122.29(7) . . ?
O8 Gd1 O13 145.35(7) . . ?
O4 Gd1 O13 68.13(7) . . ?
O11 Gd1 O13 64.74(7) . . ?
O10 Gd1 O13 69.66(7) . . ?
O1 Gd1 N1 94.69(7) . . ?
O3 Gd1 N1 93.91(7) . . ?
O14 Gd1 N1 90.34(7) . . ?
O7 Gd1 N1 25.17(7) . . ?
O2 Gd1 N1 74.25(7) . . ?
O8 Gd1 N1 25.35(7) . . ?
O4 Gd1 N1 79.79(7) . . ?
O11 Gd1 N1 164.19(7) . . ?
O10 Gd1 N1 139.67(7) . . ?
O13 Gd1 N1 127.12(7) . . ?
O1 Gd1 N3 146.77(7) . . ?
O3 Gd1 N3 130.21(7) . . ?
O14 Gd1 N3 25.37(7) . . ?
O7 Gd1 N3 86.03(7) . . ?
O2 Gd1 N3 101.77(7) . . ?
O8 Gd1 N3 135.13(7) . . ?
O4 Gd1 N3 79.26(7) . . ?
O11 Gd1 N3 83.94(7) . . ?
O10 Gd1 N3 68.39(7) . . ?
O13 Gd1 N3 25.17(7) . . ?
N1 Gd1 N3 110.72(7) . . ?
Ni2 O16 H161 114(2) . . ?
Ni2 O16 H162 107(2) . . ?
H161 O16 H162 101.4(15) . . ?
Ni2 O17 H17A 114(2) . . ?
Ni2 O17 H17B 125(2) . . ?
H17A O17 H17B 102.5(15) . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1581926'
_audit_update_record             
;
2017-10-24 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H30 N3 Ni O17 Tb'
_chemical_formula_weight         826.12

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.5216(19)
_cell_length_b                   16.757(3)
_cell_length_c                   19.565(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.34(3)
_cell_angle_gamma                90.00
_cell_volume                     3116.3(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.075
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    2.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25121
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7149
_reflns_number_gt                5037
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0020P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7149
_refine_ls_number_parameters     403
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0481
_refine_ls_wR_factor_gt          0.0450
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.26123(4) 0.24034(3) 0.26390(2) 0.02743(12) Uani 1 1 d . . .
Tb1 Tb 0.213845(17) 0.091768(12) 0.137399(9) 0.02549(6) Uani 1 1 d . . .
N1 N 0.0657(3) 0.1922(2) 0.03465(19) 0.0409(9) Uani 1 1 d . . .
N2 N 0.4124(3) 0.00951(19) 0.2326(2) 0.0352(8) Uani 1 1 d . . .
N3 N 0.2242(3) -0.0720(2) 0.08915(18) 0.0355(9) Uani 1 1 d . . .
O1 O 0.1160(2) 0.16361(14) 0.22637(12) 0.0289(6) Uani 1 1 d . . .
O2 O 0.1366(2) 0.28616(16) 0.33267(13) 0.0359(7) Uani 1 1 d . . .
O3 O -0.0460(2) 0.07059(15) 0.15505(12) 0.0294(7) Uani 1 1 d . . .
O4 O 0.3613(2) 0.18887(14) 0.18803(12) 0.0273(6) Uani 1 1 d . . .
O5 O 0.4293(2) 0.30697(15) 0.29232(13) 0.0340(7) Uani 1 1 d . . .
O6 O 0.4056(2) 0.14220(15) 0.06444(13) 0.0320(6) Uani 1 1 d . . .
O7 O 0.3380(2) 0.15634(15) 0.33482(13) 0.0348(7) Uani 1 1 d . . .
H29 H 0.3363 0.1028 0.3176 0.042 Uiso 1 1 d R . .
O8 O 0.1840(3) 0.32425(16) 0.19320(14) 0.0482(8) Uani 1 1 d . . .
H30 H 0.1475 0.3006 0.1503 0.058 Uiso 1 1 d R . .
O9 O 0.0034(3) 0.2367(2) -0.00517(16) 0.0641(10) Uani 1 1 d . . .
O10 O 0.1214(3) 0.21744(17) 0.09134(14) 0.0439(7) Uani 1 1 d . . .
O11 O 0.0841(2) 0.11857(18) 0.02392(13) 0.0408(7) Uani 1 1 d . . .
O12 O 0.4976(3) -0.01817(17) 0.27512(16) 0.0520(8) Uani 1 1 d . . .
O13 O 0.4364(2) 0.01769(16) 0.17006(15) 0.0377(7) Uani 1 1 d . . .
O14 O 0.2897(2) 0.03247(15) 0.24977(13) 0.0334(7) Uani 1 1 d . . .
O15 O 0.2520(3) -0.14112(16) 0.07558(15) 0.0476(8) Uani 1 1 d . . .
O16 O 0.2574(2) -0.01393(16) 0.05196(13) 0.0377(7) Uani 1 1 d . . .
O17 O 0.1624(2) -0.05422(15) 0.14275(13) 0.0335(7) Uani 1 1 d . . .
C1 C -0.0153(3) 0.1610(2) 0.24539(19) 0.0233(8) Uani 1 1 d . . .
C2 C -0.1076(3) 0.1091(2) 0.20825(18) 0.0244(9) Uani 1 1 d . . .
C3 C -0.2439(3) 0.0986(2) 0.22629(19) 0.0279(9) Uani 1 1 d . . .
H1 H -0.3041 0.0640 0.2016 0.033 Uiso 1 1 calc R . .
C4 C -0.2900(4) 0.1402(2) 0.2818(2) 0.0368(11) Uani 1 1 d . . .
H2 H -0.3810 0.1317 0.2952 0.044 Uiso 1 1 calc R . .
C5 C -0.2064(3) 0.1930(2) 0.3172(2) 0.0332(10) Uani 1 1 d . . .
H3 H -0.2410 0.2212 0.3536 0.040 Uiso 1 1 calc R . .
C6 C -0.0662(3) 0.2054(2) 0.29902(18) 0.0250(9) Uani 1 1 d . . .
C7 C 0.0129(4) 0.2651(2) 0.33807(19) 0.0322(10) Uani 1 1 d . . .
H4 H -0.0352 0.2911 0.3716 0.039 Uiso 1 1 calc R . .
C8 C -0.1360(3) 0.0194(2) 0.1129(2) 0.0404(11) Uani 1 1 d . . .
H5 H -0.1626 -0.0260 0.1392 0.061 Uiso 1 1 calc R . .
H6 H -0.0867 0.0017 0.0743 0.061 Uiso 1 1 calc R . .
H7 H -0.2188 0.0483 0.0972 0.061 Uiso 1 1 calc R . .
C9 C 0.4704(3) 0.2218(2) 0.15901(19) 0.0259(9) Uani 1 1 d . . .
C10 C 0.5030(3) 0.1957(2) 0.0952(2) 0.0304(10) Uani 1 1 d . . .
C11 C 0.6207(4) 0.2217(3) 0.0633(2) 0.0402(11) Uani 1 1 d . . .
H8 H 0.6411 0.2027 0.0203 0.048 Uiso 1 1 calc R . .
C12 C 0.7083(4) 0.2778(3) 0.0979(2) 0.0474(12) Uani 1 1 d . . .
H9 H 0.7883 0.2961 0.0778 0.057 Uiso 1 1 calc R . .
C13 C 0.6775(4) 0.3055(3) 0.1605(2) 0.0442(12) Uani 1 1 d . . .
H10 H 0.7374 0.3422 0.1828 0.053 Uiso 1 1 calc R . .
C14 C 0.5563(3) 0.2797(2) 0.1922(2) 0.0284(9) Uani 1 1 d . . .
C15 C 0.5334(4) 0.3131(2) 0.2573(2) 0.0321(10) Uani 1 1 d . . .
H11 H 0.6067 0.3440 0.2764 0.039 Uiso 1 1 calc R . .
C16 C 0.4265(4) 0.1191(3) -0.0050(2) 0.0465(12) Uani 1 1 d . . .
H12 H 0.4288 0.1659 -0.0332 0.070 Uiso 1 1 calc R . .
H13 H 0.3507 0.0851 -0.0214 0.070 Uiso 1 1 calc R . .
H14 H 0.5140 0.0909 -0.0067 0.070 Uiso 1 1 calc R . .
C17 C 0.3267(4) 0.1513(3) 0.4075(2) 0.0545(13) Uani 1 1 d . . .
H15 H 0.3042 0.2044 0.4248 0.082 Uiso 1 1 calc R . .
C18 C 0.4646(4) 0.1251(4) 0.4405(3) 0.106(2) Uani 1 1 d . . .
H16 H 0.4798 0.0698 0.4304 0.159 Uiso 1 1 calc R . .
H17 H 0.4635 0.1321 0.4892 0.159 Uiso 1 1 calc R . .
H18 H 0.5389 0.1565 0.4232 0.159 Uiso 1 1 calc R . .
C19 C 0.2098(5) 0.0955(4) 0.4223(3) 0.109(2) Uani 1 1 d . . .
H19 H 0.1310 0.1051 0.3905 0.163 Uiso 1 1 calc R . .
H20 H 0.1823 0.1042 0.4681 0.163 Uiso 1 1 calc R . .
H21 H 0.2412 0.0414 0.4177 0.163 Uiso 1 1 calc R . .
C20 C 0.1713(3) 0.4088(2) 0.1904(2) 0.0358(10) Uani 1 1 d . . .
H22 H 0.2257 0.4315 0.2298 0.054 Uiso 1 1 calc R . .
C21 C 0.2321(4) 0.4388(3) 0.1263(2) 0.0764(17) Uani 1 1 d . . .
H23 H 0.3278 0.4210 0.1249 0.115 Uiso 1 1 calc R . .
H24 H 0.2296 0.4960 0.1257 0.115 Uiso 1 1 calc R . .
H25 H 0.1780 0.4184 0.0871 0.115 Uiso 1 1 calc R . .
C22 C 0.0192(4) 0.4327(3) 0.1950(2) 0.0575(14) Uani 1 1 d . . .
H26 H -0.0356 0.4113 0.1566 0.086 Uiso 1 1 calc R . .
H27 H 0.0119 0.4899 0.1948 0.086 Uiso 1 1 calc R . .
H28 H -0.0154 0.4122 0.2367 0.086 Uiso 1 1 calc R . .


_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
Ni1 O1 1.997(2) . ?
Ni1 O2 1.998(2) . ?
Ni1 O5 2.003(2) . ?
Ni1 O4 2.005(2) . ?
Ni1 O8 2.077(3) . ?
Ni1 O7 2.079(3) . ?
Tb1 O4 2.332(2) . ?
Tb1 O1 2.353(2) . ?
Tb1 O10 2.435(3) . ?
Tb1 O14 2.481(3) . ?
Tb1 O16 2.487(3) . ?
Tb1 O17 2.498(3) . ?
Tb1 O13 2.507(2) . ?
Tb1 O11 2.517(3) . ?
Tb1 O6 2.527(2) . ?
Tb1 O3 2.543(2) . ?
Tb1 N3 2.905(3) . ?
Tb1 N1 2.921(4) . ?
N1 O9 1.208(4) . ?
N1 O11 1.266(4) . ?
N1 O10 1.273(4) . ?
N2 O12 1.220(4) . ?
N2 O13 1.265(4) . ?
N2 O14 1.294(3) . ?
N3 O15 1.221(4) . ?
N3 O16 1.266(4) . ?
N3 O17 1.267(3) . ?
O1 C1 1.325(3) . ?
O2 C7 1.241(4) . ?
O3 C2 1.384(4) . ?
O3 C8 1.438(4) . ?
O4 C9 1.332(4) . ?
O5 C15 1.242(4) . ?
O6 C10 1.400(4) . ?
O6 C16 1.437(4) . ?
O7 C17 1.435(5) . ?
O8 C20 1.423(5) . ?
C1 C6 1.396(5) . ?
C1 C2 1.408(5) . ?
C2 C3 1.376(4) . ?
C3 C4 1.384(5) . ?
C4 C5 1.353(5) . ?
C5 C6 1.416(4) . ?
C6 C7 1.444(5) . ?
C9 C10 1.375(5) . ?
C9 C14 1.404(5) . ?
C10 C11 1.385(4) . ?
C11 C12 1.404(5) . ?
C12 C13 1.357(5) . ?
C13 C14 1.409(4) . ?
C14 C15 1.419(5) . ?
C17 C18 1.495(6) . ?
C17 C19 1.495(6) . ?
C20 C21 1.499(5) . ?
C20 C22 1.510(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
O1 Ni1 O2 93.98(9) . . ?
O1 Ni1 O5 170.39(9) . . ?
O2 Ni1 O5 95.45(10) . . ?
O1 Ni1 O4 78.44(9) . . ?
O2 Ni1 O4 171.95(9) . . ?
O5 Ni1 O4 92.22(9) . . ?
O1 Ni1 O8 88.86(11) . . ?
O2 Ni1 O8 89.27(11) . . ?
O5 Ni1 O8 93.08(11) . . ?
O4 Ni1 O8 87.89(10) . . ?
O1 Ni1 O7 91.07(10) . . ?
O2 Ni1 O7 90.59(10) . . ?
O5 Ni1 O7 87.01(10) . . ?
O4 Ni1 O7 92.23(10) . . ?
O8 Ni1 O7 179.84(11) . . ?
O4 Tb1 O1 65.38(7) . . ?
O4 Tb1 O10 75.50(9) . . ?
O1 Tb1 O10 71.40(9) . . ?
O4 Tb1 O14 76.48(9) . . ?
O1 Tb1 O14 69.92(8) . . ?
O10 Tb1 O14 138.98(9) . . ?
O4 Tb1 O16 131.50(8) . . ?
O1 Tb1 O16 161.88(8) . . ?
O10 Tb1 O16 115.98(9) . . ?
O14 Tb1 O16 105.02(9) . . ?
O4 Tb1 O17 141.26(8) . . ?
O1 Tb1 O17 112.52(8) . . ?
O10 Tb1 O17 142.64(8) . . ?
O14 Tb1 O17 67.57(8) . . ?
O16 Tb1 O17 51.06(8) . . ?
O4 Tb1 O13 75.99(8) . . ?
O1 Tb1 O13 115.47(9) . . ?
O10 Tb1 O13 143.59(8) . . ?
O14 Tb1 O13 51.52(9) . . ?
O16 Tb1 O13 69.33(9) . . ?
O17 Tb1 O13 70.68(8) . . ?
O4 Tb1 O11 120.17(9) . . ?
O1 Tb1 O11 111.47(8) . . ?
O10 Tb1 O11 51.03(9) . . ?
O14 Tb1 O11 162.81(8) . . ?
O16 Tb1 O11 68.08(9) . . ?
O17 Tb1 O11 97.14(9) . . ?
O13 Tb1 O11 132.64(9) . . ?
O4 Tb1 O6 64.52(8) . . ?
O1 Tb1 O6 125.23(8) . . ?
O10 Tb1 O6 76.08(8) . . ?
O14 Tb1 O6 116.86(8) . . ?
O16 Tb1 O6 72.80(8) . . ?
O17 Tb1 O6 120.05(7) . . ?
O13 Tb1 O6 71.45(8) . . ?
O11 Tb1 O6 77.04(8) . . ?
O4 Tb1 O3 127.32(8) . . ?
O1 Tb1 O3 62.65(8) . . ?
O10 Tb1 O3 80.63(8) . . ?
O14 Tb1 O3 93.38(8) . . ?
O16 Tb1 O3 101.16(8) . . ?
O17 Tb1 O3 70.31(7) . . ?
O13 Tb1 O3 135.32(8) . . ?
O11 Tb1 O3 73.34(8) . . ?
O6 Tb1 O3 149.76(8) . . ?
O4 Tb1 N3 139.99(8) . . ?
O1 Tb1 N3 138.24(9) . . ?
O10 Tb1 N3 135.64(9) . . ?
O14 Tb1 N3 84.03(9) . . ?
O16 Tb1 N3 25.68(8) . . ?
O17 Tb1 N3 25.74(7) . . ?
O13 Tb1 N3 64.59(9) . . ?
O11 Tb1 N3 84.62(10) . . ?
O6 Tb1 N3 95.34(8) . . ?
O3 Tb1 N3 87.93(8) . . ?
O4 Tb1 N1 98.34(10) . . ?
O1 Tb1 N1 91.04(9) . . ?
O10 Tb1 N1 25.49(9) . . ?
O14 Tb1 N1 160.79(9) . . ?
O16 Tb1 N1 92.32(10) . . ?
O17 Tb1 N1 120.34(10) . . ?
O13 Tb1 N1 145.90(9) . . ?
O11 Tb1 N1 25.55(9) . . ?
O6 Tb1 N1 75.79(8) . . ?
O3 Tb1 N1 74.88(8) . . ?
N3 Tb1 N1 110.17(10) . . ?
O9 N1 O11 124.2(4) . . ?
O9 N1 O10 121.4(4) . . ?
O11 N1 O10 114.4(4) . . ?
O9 N1 Tb1 176.5(3) . . ?
O11 N1 Tb1 59.1(2) . . ?
O10 N1 Tb1 55.4(2) . . ?
O12 N2 O13 123.4(3) . . ?
O12 N2 O14 120.7(4) . . ?
O13 N2 O14 115.9(3) . . ?
O12 N2 Tb1 174.1(3) . . ?
O13 N2 Tb1 58.61(18) . . ?
O14 N2 Tb1 57.61(17) . . ?
O15 N3 O16 122.7(3) . . ?
O15 N3 O17 121.3(3) . . ?
O16 N3 O17 116.0(3) . . ?
O15 N3 Tb1 168.1(3) . . ?
O16 N3 Tb1 58.35(18) . . ?
O17 N3 Tb1 58.87(18) . . ?
C1 O1 Ni1 124.2(2) . . ?
C1 O1 Tb1 127.7(2) . . ?
Ni1 O1 Tb1 107.82(9) . . ?
C7 O2 Ni1 123.5(2) . . ?
C2 O3 C8 116.4(2) . . ?
C2 O3 Tb1 119.70(19) . . ?
C8 O3 Tb1 123.9(2) . . ?
C9 O4 Ni1 123.6(2) . . ?
C9 O4 Tb1 125.0(2) . . ?
Ni1 O4 Tb1 108.31(9) . . ?
C15 O5 Ni1 122.9(3) . . ?
C10 O6 C16 117.0(3) . . ?
C10 O6 Tb1 117.0(2) . . ?
C16 O6 Tb1 126.0(2) . . ?
C17 O7 Ni1 131.1(2) . . ?
C20 O8 Ni1 136.5(2) . . ?
N1 O10 Tb1 99.1(2) . . ?
N1 O11 Tb1 95.4(2) . . ?
N2 O13 Tb1 95.9(2) . . ?
N2 O14 Tb1 96.3(2) . . ?
N3 O16 Tb1 96.0(2) . . ?
N3 O17 Tb1 95.4(2) . . ?
O1 C1 C6 124.7(3) . . ?
O1 C1 C2 116.5(3) . . ?
C6 C1 C2 118.8(3) . . ?
C3 C2 O3 125.5(3) . . ?
C3 C2 C1 121.1(3) . . ?
O3 C2 C1 113.4(3) . . ?
C2 C3 C4 118.9(3) . . ?
C5 C4 C3 121.8(3) . . ?
C4 C5 C6 120.2(4) . . ?
C1 C6 C5 119.0(3) . . ?
C1 C6 C7 125.0(3) . . ?
C5 C6 C7 116.0(3) . . ?
O2 C7 C6 128.4(3) . . ?
O4 C9 C10 118.6(3) . . ?
O4 C9 C14 122.5(3) . . ?
C10 C9 C14 118.9(3) . . ?
C11 C10 C9 122.7(4) . . ?
C11 C10 O6 122.8(4) . . ?
C9 C10 O6 114.5(3) . . ?
C10 C11 C12 117.8(4) . . ?
C13 C12 C11 120.8(3) . . ?
C12 C13 C14 121.2(4) . . ?
C13 C14 C9 118.6(4) . . ?
C13 C14 C15 116.6(3) . . ?
C9 C14 C15 124.8(3) . . ?
O5 C15 C14 129.2(3) . . ?
O7 C17 C18 109.3(4) . . ?
O7 C17 C19 109.2(4) . . ?
C18 C17 C19 112.2(5) . . ?
O8 C20 C21 109.2(3) . . ?
O8 C20 C22 110.0(3) . . ?
C21 C20 C22 112.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.108
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1581923'
_audit_update_record             
;
2017-10-24 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H37 Gd2 N4 Ni2 O27'
_chemical_formula_sum            'C36 H37 Gd2 N4 Ni2 O27'
_chemical_formula_weight         1389.62
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7627(5)
_cell_length_b                   11.1417(5)
_cell_length_c                   12.7244(6)
_cell_angle_alpha                73.703(2)
_cell_angle_beta                 66.381(2)
_cell_angle_gamma                64.462(2)
_cell_volume                     1250.65(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9923
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      31.4
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             681
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_T_max  0.912

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       ω-φ
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_number            19324
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_reflns_number_total             5063
_reflns_number_gt                4308
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1105P)²+2.3020P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.026(2)
_refine_ls_number_reflns         5063
_refine_ls_number_parameters     337
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.173
_refine_ls_wR_factor_gt          0.139
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.188
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.447
_refine_diff_density_min         -2.084
_refine_diff_density_rms         0.528

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0681(9) 0.4118(8) 0.7859(7) 0.0438(17) Uani 1 1 d . . .
C2 C -0.0172(10) 0.3939(9) 0.9018(7) 0.0506(19) Uani 1 1 d . . .
C3 C 0.0458(14) 0.3225(12) 0.9879(9) 0.073(3) Uani 1 1 d . . .
H3 H -0.0137 0.3095 1.0657 0.088 Uiso 1 1 calc R . .
C4 C 0.1982(15) 0.2698(13) 0.9588(11) 0.084(3) Uani 1 1 d . . .
H4 H 0.2419 0.217 1.0165 0.101 Uiso 1 1 calc R . .
C5 C 0.2812(13) 0.2934(11) 0.8514(11) 0.075(3) Uani 1 1 d . . .
H5 H 0.3836 0.2616 0.8345 0.091 Uiso 1 1 calc R . .
C6 C 0.2197(10) 0.3665(9) 0.7588(8) 0.052(2) Uani 1 1 d . . .
C7 C -0.2634(13) 0.4320(11) 1.0335(8) 0.067(3) Uani 1 1 d . . .
H7A H -0.2369 0.3357 1.0613 0.101 Uiso 1 1 calc R . .
H7B H -0.3639 0.4696 1.0327 0.101 Uiso 1 1 calc R . .
H7C H -0.255 0.477 1.085 0.101 Uiso 1 1 calc R . .
C8 C 0.3196(10) 0.3923(10) 0.6472(9) 0.060(2) Uani 1 1 d . . .
H8 H 0.4194 0.3595 0.6409 0.072 Uiso 1 1 calc R . .
C9 C 0.1945(7) 0.7347(7) 0.3814(6) 0.0350(14) Uani 1 1 d . . .
C10 C 0.2656(8) 0.7991(8) 0.2758(7) 0.0434(17) Uani 1 1 d . . .
C11 C 0.2941(9) 0.9101(8) 0.2776(8) 0.054(2) Uani 1 1 d . . .
H11 H 0.341 0.9537 0.207 0.065 Uiso 1 1 calc R . .
C12 C 0.2558(10) 0.9563(8) 0.3787(9) 0.058(2) Uani 1 1 d . . .
H12 H 0.2784 1.0299 0.3785 0.069 Uiso 1 1 calc R . .
C13 C 0.1839(9) 0.8959(8) 0.4813(8) 0.0507(19) Uani 1 1 d . . .
H13 H 0.1558 0.9291 0.5517 0.061 Uiso 1 1 calc R . .
C14 C 0.1530(8) 0.7893(8) 0.4828(7) 0.0424(16) Uani 1 1 d . . .
C15 C 0.0400(9) 0.7601(9) 0.6868(8) 0.0501(19) Uani 1 1 d . . .
H15A H 0.1293 0.7343 0.7048 0.075 Uiso 1 1 calc R . .
H15B H -0.0233 0.7153 0.7469 0.075 Uiso 1 1 calc R . .
H15C H -0.0107 0.8575 0.6837 0.075 Uiso 1 1 calc R . .
C16 C 0.3077(12) 0.7574(12) 0.1643(9) 0.067(3) Uani 1 1 d . . .
H16 H 0.352 0.8086 0.0983 0.081 Uiso 1 1 calc R . .
N1 N -0.5174(9) 0.6333(15) 0.6834(10) 0.084(3) Uani 1 1 d . . .
N2 N -0.3987(7) 0.7621(7) 0.8581(6) 0.0481(16) Uani 1 1 d . . .
O1 O -0.0006(5) 0.4707(6) 0.7083(4) 0.0413(12) Uani 1 1 d . . .
O3 O 0.2887(6) 0.4508(7) 0.5625(6) 0.0560(15) Uani 1 1 d . . .
O4 O 0.0753(6) 0.7217(6) 0.5792(5) 0.0510(13) Uani 1 1 d . . .
O5 O 0.1659(5) 0.6300(5) 0.3857(5) 0.0427(12) Uani 1 1 d . . .
O6 O -0.1678(7) 0.4518(7) 0.9188(5) 0.0580(15) Uani 1 1 d . . .
O7 O -0.4781(7) 0.5211(10) 0.7378(7) 0.073(2) Uani 1 1 d . . .
O8 O -0.4365(7) 0.7030(8) 0.6517(6) 0.074(2) Uani 1 1 d . . .
O9 O -0.6321(10) 0.6828(15) 0.6626(13) 0.150(5) Uani 1 1 d . . .
O10 O -0.4481(6) 0.6692(6) 0.8864(5) 0.0562(15) Uani 1 1 d . . .
O11 O -0.2772(6) 0.7442(6) 0.7776(5) 0.0484(13) Uani 1 1 d . . .
O12 O -0.4619(7) 0.8628(7) 0.9047(6) 0.0657(17) Uani 1 1 d . . .
O13 O -0.2927(9) 0.3342(8) 0.8530(6) 0.075(2) Uani 1 1 d . . .
Ni1 Ni 0.08681(9) 0.53888(9) 0.54449(7) 0.0323(2) Uani 1 1 d . . .
Gd1 Gd -0.24963(3) 0.53018(4) 0.73461(3) 0.0387(2) Uani 1 1 d . . .
O2 O -0.1220(5) 0.6061(4) 0.5438(4) 0.0286(9) Uani 1 1 d . . .
C17 C -0.1683(13) 0.7369(11) 0.4894(10) 0.031(3) Uani 0.5 1 d PD A 1
H17A H -0.0952 0.7461 0.414 0.047 Uiso 0.5 1 calc PR A 1
H17B H -0.1813 0.7992 0.5375 0.047 Uiso 0.5 1 calc PR A 1
H17C H -0.2609 0.7576 0.4786 0.047 Uiso 0.5 1 calc PR A 1
O20 O -0.1648(16) 0.8563(12) 0.3903(12) 0.075(4) Uani 0.5 1 d PD B 2
C20 C -0.195(3) 1.003(2) 0.218(2) 0.079(4) Uani 0.5 1 d P B 2
H20A H -0.1049 1.0099 0.2133 0.119 Uiso 0.5 1 calc PR B 2
H20B H -0.2673 1.0927 0.2095 0.119 Uiso 0.5 1 calc PR B 2
H20C H -0.1746 0.9536 0.1569 0.119 Uiso 0.5 1 calc PR B 2
C21 C -0.251(3) 0.9312(19) 0.330(2) 0.079(4) Uani 0.5 1 d PD B 2
C26 C -0.408(3) 0.952(2) 0.383(2) 0.079(4) Uani 0.5 1 d P B 2
H26A H -0.4314 0.9025 0.3457 0.119 Uiso 0.5 1 calc PR B 2
H26B H -0.4653 1.0479 0.3717 0.119 Uiso 0.5 1 calc PR B 2
H26C H -0.4296 0.9195 0.4658 0.119 Uiso 0.5 1 calc PR B 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.325(9) . ?
C1 C2 1.402(12) . ?
C1 C6 1.405(12) . ?
C2 C3 1.391(13) . ?
C2 O6 1.409(11) . ?
C3 C4 1.406(17) . ?
C3 H3 0.95 . ?
C4 C5 1.326(18) . ?
C4 H4 0.95 . ?
C5 C6 1.453(13) . ?
C5 H5 0.95 . ?
C6 C8 1.439(14) . ?
C7 O6 1.432(10) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 O3 1.184(12) . ?
C8 H8 0.95 . ?
C9 O5 1.312(8) . ?
C9 C14 1.406(11) . ?
C9 C10 1.420(10) . ?
C10 C11 1.404(11) . ?
C10 C16 1.451(13) . ?
C11 C12 1.361(14) . ?
C11 H11 0.95 . ?
C12 C13 1.380(13) . ?
C12 H12 0.95 . ?
C13 C14 1.358(11) . ?
C13 H13 0.95 . ?
C14 O4 1.405(10) . ?
C15 O4 1.405(9) . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
C16 O13 1.189(12) 2_566 ?
C16 H16 0.95 . ?
N1 O9 1.221(12) . ?
N1 O7 1.230(15) . ?
N1 O8 1.284(14) . ?
N1 Gd1 2.877(8) . ?
N2 O12 1.210(9) . ?
N2 O10 1.263(9) . ?
N2 O11 1.271(9) . ?
N2 Gd1 2.900(7) . ?
O1 Ni1 1.991(5) . ?
O1 Gd1 2.369(5) . ?
O3 Ni1 2.043(5) . ?
O4 Ni1 2.145(6) . ?
O5 Ni1 2.013(5) . ?
O5 Gd1 2.319(5) 2_566 ?
O6 Gd1 2.622(6) . ?
O7 Gd1 2.489(6) . ?
O8 Gd1 2.467(7) . ?
O10 Gd1 2.492(6) . ?
O11 Gd1 2.463(6) . ?
O13 C16 1.189(12) 2_566 ?
O13 Gd1 2.391(7) . ?
Ni1 O2 2.041(4) 2_566 ?
Ni1 O2 2.042(4) . ?
Ni1 Gd1 3.4146(9) 2_566 ?
Ni1 Gd1 3.4821(9) . ?
Gd1 O5 2.319(5) 2_566 ?
Gd1 O2 2.383(4) . ?
Gd1 Ni1 3.4146(9) 2_566 ?
O2 C17 1.391(12) . ?
O2 Ni1 2.041(4) 2_566 ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
O20 C21 1.293(10) . ?
C20 C21 1.45(4) . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C21 C26 1.48(4) . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?

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 C2 117.3(7) . . ?
O1 C1 C6 124.0(7) . . ?
C2 C1 C6 118.7(7) . . ?
C3 C2 C1 121.4(9) . . ?
C3 C2 O6 125.3(9) . . ?
C1 C2 O6 113.3(7) . . ?
C2 C3 C4 119.4(10) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 120.4(10) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 121.7(10) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C8 125.2(8) . . ?
C1 C6 C5 118.0(9) . . ?
C8 C6 C5 116.7(9) . . ?
O6 C7 H7A 109.5 . . ?
O6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 C6 125.9(8) . . ?
O3 C8 H8 117 . . ?
C6 C8 H8 117 . . ?
O5 C9 C14 120.6(6) . . ?
O5 C9 C10 122.2(7) . . ?
C14 C9 C10 117.1(6) . . ?
C11 C10 C9 119.2(7) . . ?
C11 C10 C16 117.9(8) . . ?
C9 C10 C16 122.9(7) . . ?
C12 C11 C10 121.3(8) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C13 119.7(7) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 120.6(8) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 O4 127.0(8) . . ?
C13 C14 C9 121.9(7) . . ?
O4 C14 C9 111.0(6) . . ?
O4 C15 H15A 109.5 . . ?
O4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O13 C16 C10 126.8(10) 2_566 . ?
O13 C16 H16 116.6 2_566 . ?
C10 C16 H16 116.6 . . ?
O9 N1 O7 122.9(13) . . ?
O9 N1 O8 118.9(14) . . ?
O7 N1 O8 118.1(8) . . ?
O9 N1 Gd1 177.0(11) . . ?
O7 N1 Gd1 59.4(4) . . ?
O8 N1 Gd1 58.7(5) . . ?
O12 N2 O10 122.6(7) . . ?
O12 N2 O11 121.1(7) . . ?
O10 N2 O11 116.3(7) . . ?
O12 N2 Gd1 176.8(6) . . ?
O10 N2 Gd1 58.8(4) . . ?
O11 N2 Gd1 57.5(4) . . ?
C1 O1 Ni1 125.7(5) . . ?
C1 O1 Gd1 128.5(5) . . ?
Ni1 O1 Gd1 105.7(2) . . ?
C8 O3 Ni1 128.0(7) . . ?
C14 O4 C15 115.8(6) . . ?
C14 O4 Ni1 113.1(5) . . ?
C15 O4 Ni1 128.3(5) . . ?
C9 O5 Ni1 116.4(5) . . ?
C9 O5 Gd1 136.0(5) . 2_566 ?
Ni1 O5 Gd1 103.8(2) . 2_566 ?
C2 O6 C7 117.3(7) . . ?
C2 O6 Gd1 117.4(4) . . ?
C7 O6 Gd1 123.2(6) . . ?
N1 O7 Gd1 95.4(6) . . ?
N1 O8 Gd1 94.9(7) . . ?
N2 O10 Gd1 95.5(4) . . ?
N2 O11 Gd1 96.6(5) . . ?
C16 O13 Gd1 134.0(7) 2_566 . ?
O1 Ni1 O5 172.9(2) . . ?
O1 Ni1 O2 102.9(2) . 2_566 ?
O5 Ni1 O2 83.97(19) . 2_566 ?
O1 Ni1 O2 82.60(19) . . ?
O5 Ni1 O2 96.3(2) . . ?
O2 Ni1 O2 84.28(18) 2_566 . ?
O1 Ni1 O3 90.4(2) . . ?
O5 Ni1 O3 91.1(3) . . ?
O2 Ni1 O3 93.6(2) 2_566 . ?
O2 Ni1 O3 172.0(2) . . ?
O1 Ni1 O4 96.3(2) . . ?
O5 Ni1 O4 76.8(2) . . ?
O2 Ni1 O4 160.8(2) 2_566 . ?
O2 Ni1 O4 96.9(2) . . ?
O3 Ni1 O4 87.7(2) . . ?
O1 Ni1 Gd1 145.76(16) . 2_566 ?
O5 Ni1 Gd1 41.27(15) . 2_566 ?
O2 Ni1 Gd1 43.27(12) 2_566 2_566 ?
O2 Ni1 Gd1 95.95(12) . 2_566 ?
O3 Ni1 Gd1 87.66(18) . 2_566 ?
O4 Ni1 Gd1 117.75(16) . 2_566 ?
O1 Ni1 Gd1 40.91(14) . . ?
O5 Ni1 Gd1 137.74(15) . . ?
O2 Ni1 Gd1 93.99(12) 2_566 . ?
O2 Ni1 Gd1 41.70(12) . . ?
O3 Ni1 Gd1 131.1(2) . . ?
O4 Ni1 Gd1 99.60(16) . . ?
Gd1 Ni1 Gd1 127.93(2) 2_566 . ?
O5 Gd1 O1 85.01(18) 2_566 . ?
O5 Gd1 O2 70.43(17) 2_566 . ?
O1 Gd1 O2 68.15(16) . . ?
O5 Gd1 O13 72.2(2) 2_566 . ?
O1 Gd1 O13 101.0(2) . . ?
O2 Gd1 O13 141.8(2) . . ?
O5 Gd1 O11 153.76(19) 2_566 . ?
O1 Gd1 O11 84.26(19) . . ?
O2 Gd1 O11 83.35(16) . . ?
O13 Gd1 O11 133.4(2) . . ?
O5 Gd1 O8 97.9(2) 2_566 . ?
O1 Gd1 O8 138.3(2) . . ?
O2 Gd1 O8 73.72(19) . . ?
O13 Gd1 O8 119.6(3) . . ?
O11 Gd1 O8 75.0(2) . . ?
O5 Gd1 O7 77.0(2) 2_566 . ?
O1 Gd1 O7 161.1(3) . . ?
O2 Gd1 O7 110.0(2) . . ?
O13 Gd1 O7 68.3(3) . . ?
O11 Gd1 O7 114.5(3) . . ?
O8 Gd1 O7 51.6(3) . . ?
O5 Gd1 O10 150.37(18) 2_566 . ?
O1 Gd1 O10 122.15(19) . . ?
O2 Gd1 O10 127.71(18) . . ?
O13 Gd1 O10 89.6(2) . . ?
O11 Gd1 O10 51.49(18) . . ?
O8 Gd1 O10 70.5(2) . . ?
O7 Gd1 O10 74.6(2) . . ?
O5 Gd1 O6 116.8(2) 2_566 . ?
O1 Gd1 O6 61.74(18) . . ?
O2 Gd1 O6 127.83(17) . . ?
O13 Gd1 O6 64.8(2) . . ?
O11 Gd1 O6 78.3(2) . . ?
O8 Gd1 O6 143.1(2) . . ?
O7 Gd1 O6 122.1(2) . . ?
O10 Gd1 O6 73.0(2) . . ?
O5 Gd1 N1 86.7(3) 2_566 . ?
O1 Gd1 N1 160.3(3) . . ?
O2 Gd1 N1 92.3(3) . . ?
O13 Gd1 N1 93.4(4) . . ?
O11 Gd1 N1 95.5(3) . . ?
O8 Gd1 N1 26.4(3) . . ?
O7 Gd1 N1 25.2(3) . . ?
O10 Gd1 N1 70.8(2) . . ?
O6 Gd1 N1 137.6(3) . . ?
O5 Gd1 N2 167.67(19) 2_566 . ?
O1 Gd1 N2 104.56(18) . . ?
O2 Gd1 N2 105.55(18) . . ?
O13 Gd1 N2 112.6(2) . . ?
O11 Gd1 N2 25.81(18) . . ?
O8 Gd1 N2 69.8(2) . . ?
O7 Gd1 N2 94.1(2) . . ?
O10 Gd1 N2 25.71(19) . . ?
O6 Gd1 N2 75.0(2) . . ?
N1 Gd1 N2 81.7(3) . . ?
O5 Gd1 Ni1 34.93(13) 2_566 2_566 ?
O1 Gd1 Ni1 77.95(12) . 2_566 ?
O2 Gd1 Ni1 35.95(11) . 2_566 ?
O13 Gd1 Ni1 107.18(17) . 2_566 ?
O11 Gd1 Ni1 119.07(13) . 2_566 ?
O8 Gd1 Ni1 81.18(17) . 2_566 ?
O7 Gd1 Ni1 90.11(17) . 2_566 ?
O10 Gd1 Ni1 151.53(16) . 2_566 ?
O6 Gd1 Ni1 134.76(14) . 2_566 ?
N1 Gd1 Ni1 85.1(2) . 2_566 ?
N2 Gd1 Ni1 138.59(14) . 2_566 ?
C17 O2 Ni1 115.2(6) . 2_566 ?
C17 O2 Ni1 113.2(6) . . ?
Ni1 O2 Ni1 95.72(18) 2_566 . ?
C17 O2 Gd1 124.0(6) . . ?
Ni1 O2 Gd1 100.78(18) 2_566 . ?
Ni1 O2 Gd1 103.53(18) . . ?
O2 C17 H17A 109.5 . . ?
O2 C17 H17B 109.5 . . ?
O2 C17 H17C 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 . . ?
O20 C21 C20 120(2) . . ?
O20 C21 C26 119(2) . . ?
C20 C21 C26 121.2(16) . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1581927'
_audit_update_record             
;
2017-10-24 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H18 Ce N3 Ni O17'
_chemical_formula_weight         723.16

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'
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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'

_cell_length_a                   9.4537(6)
_cell_length_b                   18.3586(14)
_cell_length_c                   14.5970(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.503(6)
_cell_angle_gamma                90.00
_cell_volume                     2429.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      14.0
_cell_measurement_theta_max      18.0

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Light-green
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1428
_exptl_absorpt_coefficient_mu    2.713
_exptl_absorpt_correction_type   Psi-scans
_exptl_absorpt_correction_T_min  0.8392
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_process_details   
;
[c.f. North, A.C.T., Phillips, D.C. and Mathews, F.S. Acta Cryst.
(1968), A24, 351-359]
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       Omega-2Theta
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        -2.3
_diffrn_reflns_number            6185
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         27.97
_reflns_number_total             5853
_reflns_number_gt                4602
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CAD4-EXPRESS
_computing_cell_refinement       CAD4-EXPRESS
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1996)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+1.7146P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5853
_refine_ls_number_parameters     359
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_ref         0.0577
_refine_ls_wR_factor_gt          0.0478
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.005
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce Ce 0.211564(15) 0.657836(7) 0.266017(9) 0.03220(4) Uani 1 d . . .
Ni Ni 0.28506(4) 0.468325(18) 0.24814(2) 0.03751(8) Uani 1 d . . .
O1 O 0.1421(2) 0.53335(9) 0.28767(13) 0.0376(4) Uani 1 d . . .
C1 C 0.0350(3) 0.51154(14) 0.32276(17) 0.0379(5) Uani 1 d . . .
C2 C -0.0637(3) 0.56428(17) 0.3373(2) 0.0448(6) Uani 1 d . . .
C3 C -0.1734(4) 0.5455(2) 0.3785(3) 0.0657(9) Uani 1 d . . .
H3 H -0.2377 0.5809 0.3884 0.072 Uiso 1 calc R . .
C4 C -0.1878(4) 0.4738(2) 0.4050(3) 0.0749(11) Uani 1 d . . .
H4 H -0.2610 0.4617 0.4336 0.082 Uiso 1 calc R . .
C5 C -0.0967(4) 0.4218(2) 0.3898(3) 0.0648(9) Uani 1 d . . .
H5 H -0.1079 0.3741 0.4080 0.071 Uiso 1 calc R . .
C6 C 0.0151(3) 0.43837(17) 0.3468(2) 0.0479(7) Uani 1 d . . .
C7 C 0.1007(4) 0.37815(16) 0.3280(2) 0.0540(8) Uani 1 d . . .
H7 H 0.0804 0.3331 0.3506 0.059 Uiso 1 calc R . .
O3 O -0.0362(2) 0.63333(11) 0.30886(15) 0.0476(5) Uani 1 d . . .
C8 C -0.1352(4) 0.6905(2) 0.3183(3) 0.0686(10) Uani 1 d . . .
H8A H -0.1050 0.7356 0.2964 0.075 Uiso 1 calc R . .
H8B H -0.1332 0.6952 0.3842 0.075 Uiso 1 calc R . .
H8C H -0.2336 0.6788 0.2807 0.075 Uiso 1 calc R . .
O5 O 0.1967(2) 0.37803(11) 0.28624(16) 0.0527(5) Uani 1 d . . .
O2 O 0.3621(2) 0.56519(10) 0.22111(13) 0.0386(4) Uani 1 d . . .
C9 C 0.4552(3) 0.57460(15) 0.16961(18) 0.0382(5) Uani 1 d . . .
C10 C 0.4710(3) 0.64563(16) 0.13714(19) 0.0423(6) Uani 1 d . . .
C11 C 0.5666(4) 0.6604(2) 0.0835(2) 0.0599(8) Uani 1 d . . .
H11 H 0.5738 0.7074 0.0613 0.066 Uiso 1 calc R . .
C12 C 0.6520(4) 0.6045(2) 0.0628(3) 0.0725(11) Uani 1 d . . .
H12 H 0.7171 0.6143 0.0271 0.080 Uiso 1 calc R . .
C13 C 0.6411(4) 0.5357(2) 0.0941(3) 0.0699(10) Uani 1 d . . .
H13 H 0.7005 0.4992 0.0807 0.077 Uiso 1 calc R . .
C14 C 0.5406(3) 0.51850(18) 0.1470(2) 0.0505(7) Uani 1 d . . .
C15 C 0.5313(4) 0.4436(2) 0.1723(3) 0.0642(9) Uani 1 d . . .
H15 H 0.6016 0.4127 0.1598 0.071 Uiso 1 calc R . .
O4 O 0.3818(2) 0.69682(10) 0.16267(13) 0.0439(4) Uani 1 d . . .
C16 C 0.4105(4) 0.77209(17) 0.1484(3) 0.0627(9) Uani 1 d . . .
H16A H 0.3417 0.8020 0.1688 0.069 Uiso 1 calc R . .
H16B H 0.3997 0.7806 0.0819 0.069 Uiso 1 calc R . .
H16C H 0.5092 0.7841 0.1851 0.069 Uiso 1 calc R . .
O6 O 0.4430(3) 0.41495(12) 0.20815(17) 0.0618(6) Uani 1 d . . .
O7 O 0.4284(3) 0.46896(13) 0.38542(16) 0.0526(5) Uani 1 d . . .
H71 H 0.420(5) 0.4344(19) 0.420(3) 0.092(14) Uiso 1 d . . .
H72 H 0.417(5) 0.5094(18) 0.411(3) 0.087(14) Uiso 1 d . . .
O8 O 0.1491(3) 0.46262(13) 0.10938(17) 0.0667(7) Uani 1 d . . .
H81 H 0.098(4) 0.4999(17) 0.087(3) 0.079(13) Uiso 1 d . . .
H82 H 0.110(4) 0.4211(16) 0.093(3) 0.080(13) Uiso 1 d . . .
O9 O 0.0581(2) 0.60898(10) 0.09906(14) 0.0513(5) Uani 1 d . . .
O10 O 0.0416(3) 0.72325(11) 0.11951(15) 0.0553(5) Uani 1 d . . .
N1 N 0.0067(2) 0.66964(12) 0.06436(16) 0.0394(5) Uani 1 d . . .
O11 O -0.0720(2) 0.67540(12) -0.01713(14) 0.0527(5) Uani 1 d . . .
O12 O 0.3879(2) 0.61165(11) 0.42751(14) 0.0494(5) Uani 1 d . . .
O13 O 0.4782(2) 0.70099(12) 0.36669(15) 0.0560(5) Uani 1 d . . .
N2 N 0.4953(3) 0.65412(12) 0.43102(16) 0.0420(5) Uani 1 d . . .
O14 O 0.6103(2) 0.64974(13) 0.49598(16) 0.0624(6) Uani 1 d . . .
O15 O 0.1921(3) 0.79583(11) 0.28994(15) 0.0592(6) Uani 1 d . . .
O16 O 0.1988(3) 0.73373(12) 0.41487(15) 0.0582(5) Uani 1 d . . .
N3 N 0.1988(3) 0.79527(14) 0.37705(18) 0.0495(6) Uani 1 d . . .
O17 O 0.2055(3) 0.85118(13) 0.4222(2) 0.0797(8) Uani 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
Ce O1 2.4235(17) . ?
Ce O2 2.4247(17) . ?
Ce O15 2.571(2) . ?
Ce O10 2.578(2) . ?
Ce O4 2.5997(18) . ?
Ce O12 2.612(2) . ?
Ce O16 2.613(2) . ?
Ce O9 2.6154(19) . ?
Ce O3 2.6288(19) . ?
Ce O13 2.653(2) . ?
Ce N3 3.020(2) . ?
Ce Ni 3.5719(4) . ?
Ni O2 2.0030(18) . ?
Ni O5 2.005(2) . ?
Ni O6 2.007(2) . ?
Ni O1 2.0072(17) . ?
Ni O8 2.071(2) . ?
Ni O7 2.076(2) . ?
O1 C1 1.320(3) . ?
C1 C2 1.402(4) . ?
C1 C6 1.414(4) . ?
C2 C3 1.381(4) . ?
C2 O3 1.382(4) . ?
C3 C4 1.389(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.346(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.408(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.441(5) . ?
C7 O5 1.229(4) . ?
C7 H7 0.9300 . ?
O3 C8 1.439(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
O2 C9 1.321(3) . ?
C9 C14 1.404(4) . ?
C9 C10 1.410(4) . ?
C10 C11 1.381(4) . ?
C10 O4 1.382(3) . ?
C11 C12 1.391(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.356(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.420(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.433(5) . ?
C15 O6 1.223(4) . ?
C15 H15 0.9300 . ?
O4 C16 1.435(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O7 H71 0.83(4) . ?
O7 H72 0.85(4) . ?
O8 H81 0.85(3) . ?
O8 H82 0.85(3) . ?
O9 N1 1.262(3) . ?
O10 N1 1.255(3) . ?
N1 O11 1.215(3) . ?
O12 N2 1.270(3) . ?
O13 N2 1.250(3) . ?
N2 O14 1.225(3) . ?
O15 N3 1.255(3) . ?
O16 N3 1.258(3) . ?
N3 O17 1.212(3) . ?

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 Ce O2 64.88(6) . . ?
O1 Ce O15 151.52(7) . . ?
O2 Ce O15 142.95(7) . . ?
O1 Ce O10 114.79(6) . . ?
O2 Ce O10 112.21(6) . . ?
O15 Ce O10 66.54(7) . . ?
O1 Ce O4 124.81(6) . . ?
O2 Ce O4 61.86(6) . . ?
O15 Ce O4 83.54(7) . . ?
O10 Ce O4 74.52(7) . . ?
O1 Ce O12 72.74(6) . . ?
O2 Ce O12 75.11(6) . . ?
O15 Ce O12 104.43(7) . . ?
O10 Ce O12 170.96(6) . . ?
O4 Ce O12 105.75(7) . . ?
O1 Ce O16 108.43(6) . . ?
O2 Ce O16 140.21(7) . . ?
O15 Ce O16 48.67(7) . . ?
O10 Ce O16 106.04(7) . . ?
O4 Ce O16 121.23(7) . . ?
O12 Ce O16 65.86(7) . . ?
O1 Ce O9 72.48(6) . . ?
O2 Ce O9 73.76(6) . . ?
O15 Ce O9 114.98(6) . . ?
O10 Ce O9 48.44(6) . . ?
O4 Ce O9 79.91(7) . . ?
O12 Ce O9 140.58(6) . . ?
O16 Ce O9 144.42(7) . . ?
O1 Ce O3 60.97(6) . . ?
O2 Ce O3 125.13(6) . . ?
O15 Ce O3 91.91(7) . . ?
O10 Ce O3 83.66(7) . . ?
O4 Ce O3 157.74(7) . . ?
O12 Ce O3 96.49(7) . . ?
O16 Ce O3 68.81(7) . . ?
O9 Ce O3 82.36(7) . . ?
O1 Ce O13 117.36(6) . . ?
O2 Ce O13 79.68(7) . . ?
O15 Ce O13 73.97(7) . . ?
O10 Ce O13 126.21(7) . . ?
O4 Ce O13 65.90(6) . . ?
O12 Ce O13 48.28(6) . . ?
O16 Ce O13 68.98(7) . . ?
O9 Ce O13 143.80(7) . . ?
O3 Ce O13 133.62(7) . . ?
O1 Ce N3 131.63(6) . . ?
O2 Ce N3 147.91(7) . . ?
O15 Ce N3 24.28(7) . . ?
O10 Ce N3 86.88(7) . . ?
O4 Ce N3 101.95(6) . . ?
O12 Ce N3 84.23(7) . . ?
O16 Ce N3 24.46(7) . . ?
O9 Ce N3 133.67(7) . . ?
O3 Ce N3 80.86(6) . . ?
O13 Ce N3 68.26(7) . . ?
O1 Ce Ni 32.49(4) . . ?
O2 Ce Ni 32.40(4) . . ?
O15 Ce Ni 173.02(6) . . ?
O10 Ce Ni 118.78(4) . . ?
O4 Ce Ni 93.46(4) . . ?
O12 Ce Ni 70.26(4) . . ?
O16 Ce Ni 129.50(5) . . ?
O9 Ce Ni 70.48(4) . . ?
O3 Ce Ni 93.19(4) . . ?
O13 Ce Ni 99.06(5) . . ?
N3 Ce Ni 153.04(5) . . ?
O2 Ni O5 172.89(8) . . ?
O2 Ni O6 91.94(9) . . ?
O5 Ni O6 94.59(9) . . ?
O2 Ni O1 80.86(7) . . ?
O5 Ni O1 92.54(8) . . ?
O6 Ni O1 172.65(9) . . ?
O2 Ni O8 90.67(9) . . ?
O5 Ni O8 92.16(10) . . ?
O6 Ni O8 89.85(11) . . ?
O1 Ni O8 91.69(9) . . ?
O2 Ni O7 90.63(8) . . ?
O5 Ni O7 86.90(9) . . ?
O6 Ni O7 87.02(10) . . ?
O1 Ni O7 91.57(9) . . ?
O8 Ni O7 176.65(10) . . ?
O2 Ni Ce 40.44(5) . . ?
O5 Ni Ce 132.86(7) . . ?
O6 Ni Ce 132.32(7) . . ?
O1 Ni Ce 40.43(5) . . ?
O8 Ni Ce 92.36(7) . . ?
O7 Ni Ce 90.64(7) . . ?
C1 O1 Ni 125.78(16) . . ?
C1 O1 Ce 127.08(16) . . ?
Ni O1 Ce 107.07(7) . . ?
O1 C1 C2 117.8(2) . . ?
O1 C1 C6 123.7(3) . . ?
C2 C1 C6 118.5(2) . . ?
C3 C2 O3 126.1(3) . . ?
C3 C2 C1 120.5(3) . . ?
O3 C2 C1 113.4(2) . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 120.5(3) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 119.0(3) . . ?
C5 C6 C7 116.9(3) . . ?
C1 C6 C7 124.1(3) . . ?
O5 C7 C6 129.0(3) . . ?
O5 C7 H7 115.5 . . ?
C6 C7 H7 115.5 . . ?
C2 O3 C8 117.2(2) . . ?
C2 O3 Ce 119.04(16) . . ?
C8 O3 Ce 123.10(19) . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 O5 Ni 124.1(2) . . ?
C9 O2 Ni 124.52(17) . . ?
C9 O2 Ce 126.81(16) . . ?
Ni O2 Ce 107.17(7) . . ?
O2 C9 C14 123.9(3) . . ?
O2 C9 C10 117.6(2) . . ?
C14 C9 C10 118.5(2) . . ?
C11 C10 O4 124.5(3) . . ?
C11 C10 C9 121.4(3) . . ?
O4 C10 C9 114.1(2) . . ?
C10 C11 C12 119.5(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 120.6(3) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 121.2(3) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C9 C14 C13 118.8(3) . . ?
C9 C14 C15 124.2(3) . . ?
C13 C14 C15 116.9(3) . . ?
O6 C15 C14 128.4(3) . . ?
O6 C15 H15 115.8 . . ?
C14 C15 H15 115.8 . . ?
C10 O4 C16 117.5(2) . . ?
C10 O4 Ce 119.65(15) . . ?
C16 O4 Ce 121.51(18) . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 O6 Ni 124.7(2) . . ?
Ni O7 H71 116(3) . . ?
Ni O7 H72 107(3) . . ?
H71 O7 H72 111(4) . . ?
Ni O8 H81 118(2) . . ?
Ni O8 H82 115(2) . . ?
H81 O8 H82 117(3) . . ?
N1 O9 Ce 96.87(14) . . ?
N1 O10 Ce 98.93(15) . . ?
O11 N1 O10 122.4(2) . . ?
O11 N1 O9 121.9(2) . . ?
O10 N1 O9 115.7(2) . . ?
N2 O12 Ce 97.77(14) . . ?
N2 O13 Ce 96.34(16) . . ?
O14 N2 O13 121.6(3) . . ?
O14 N2 O12 120.9(2) . . ?
O13 N2 O12 117.5(2) . . ?
N3 O15 Ce 98.31(17) . . ?
N3 O16 Ce 96.20(15) . . ?
O17 N3 O15 121.6(3) . . ?
O17 N3 O16 121.9(3) . . ?
O15 N3 O16 116.5(2) . . ?
O17 N3 Ce 174.8(2) . . ?
O15 N3 Ce 57.41(13) . . ?
O16 N3 Ce 59.34(13) . . ?

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
O7 H71 O14 0.83(4) 2.04(4) 2.870(3) 177(4) 3_666
O7 H72 O12 0.85(4) 1.92(3) 2.742(3) 162(4) .
O8 H81 O9 0.85(3) 2.06(3) 2.812(3) 148(3) .
O8 H82 O11 0.85(3) 2.06(3) 2.865(3) 156(4) 3_565

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.97
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1581924'
_audit_update_record             
;
2017-10-24 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H25 N2 Ni O16 Tb'
_chemical_formula_weight         827.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_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                   11.1842(11)
_cell_length_b                   15.6136(13)
_cell_length_c                   16.5063(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.277(11)
_cell_angle_gamma                90.00
_cell_volume                     2882.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_absorpt_coefficient_mu    3.169
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.4360
_exptl_absorpt_correction_T_max  0.8426
_exptl_absorpt_process_details   'X-SHAPE (Stoe & Cie, 1996)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Imaging Plate Detector System'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28070
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         26.10
_reflns_number_total             5523
_reflns_number_gt                4177
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE-IPDS software (Stoe, 2.93, 1997)'
_computing_cell_refinement       'STOE-IPDS software (Stoe, 2.93, 1997)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1996)'
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0436P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5523
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0673
_refine_ls_wR_factor_gt          0.0623
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_restrained_S_all      0.934
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb Tb 0.633160(17) 0.105635(13) 0.212755(14) 0.02305(7) Uani 1 1 d . . .
Ni Ni 0.47379(5) 0.27304(4) 0.27852(4) 0.02555(13) Uani 1 1 d . . .
O1 O 0.6356(2) 0.22197(19) 0.29876(19) 0.0266(7) Uani 1 1 d . . .
O2 O 0.4500(2) 0.17396(18) 0.20433(19) 0.0249(7) Uani 1 1 d . . .
O3 O 0.8062(2) 0.1155(2) 0.3202(2) 0.0291(7) Uani 1 1 d . . .
O4 O 0.4610(2) 0.02052(19) 0.1485(2) 0.0304(7) Uani 1 1 d . . .
O5 O 0.5114(3) 0.3693(2) 0.3561(2) 0.0325(8) Uani 1 1 d . . .
O6 O 0.3046(3) 0.3137(2) 0.2550(2) 0.0346(8) Uani 1 1 d . . .
O7 O 0.4107(3) 0.2025(2) 0.3756(2) 0.0364(8) Uani 1 1 d . . .
H7A H 0.4552 0.1535 0.3919 0.040 Uiso 1 1 calc R . .
O8 O 0.5362(3) 0.3442(2) 0.1815(2) 0.0354(8) Uani 1 1 d . . .
O9 O 0.6425(3) 0.2404(2) 0.1263(2) 0.0331(8) Uani 1 1 d . . .
N1 N 0.5937(3) 0.3132(3) 0.1222(3) 0.0320(9) Uani 1 1 d . . .
O10 O 0.6023(3) 0.3554(3) 0.0594(2) 0.0487(10) Uani 1 1 d . . .
C1 C 0.7031(3) 0.2372(3) 0.3621(3) 0.0219(9) Uani 1 1 d . . .
C2 C 0.7995(3) 0.1813(3) 0.3769(3) 0.0267(10) Uani 1 1 d . . .
C3 C 0.8776(4) 0.1932(3) 0.4400(3) 0.0364(11) Uani 1 1 d . . .
H3 H 0.9426 0.1549 0.4480 0.040 Uiso 1 1 calc R . .
C4 C 0.8609(4) 0.2626(4) 0.4927(3) 0.0396(12) Uani 1 1 d . . .
H4 H 0.9143 0.2713 0.5369 0.044 Uiso 1 1 calc R . .
C5 C 0.7678(4) 0.3174(3) 0.4804(3) 0.0340(11) Uani 1 1 d . . .
H5 H 0.7570 0.3641 0.5165 0.037 Uiso 1 1 calc R . .
C6 C 0.6871(4) 0.3065(3) 0.4155(3) 0.0274(10) Uani 1 1 d . . .
C7 C 0.5919(4) 0.3683(3) 0.4060(3) 0.0296(10) Uani 1 1 d . . .
H7 H 0.5922 0.4143 0.4437 0.033 Uiso 1 1 calc R . .
C8 C 0.9058(4) 0.0575(3) 0.3283(3) 0.0365(12) Uani 1 1 d . . .
H8A H 0.9020 0.0143 0.2853 0.040 Uiso 1 1 calc R . .
H8B H 0.9023 0.0291 0.3812 0.040 Uiso 1 1 calc R . .
H8C H 0.9808 0.0896 0.3241 0.040 Uiso 1 1 calc R . .
C9 C 0.3462(3) 0.1371(3) 0.1916(3) 0.0237(9) Uani 1 1 d . . .
C10 C 0.3458(4) 0.0529(3) 0.1613(3) 0.0265(10) Uani 1 1 d . . .
C11 C 0.2419(4) 0.0094(3) 0.1451(3) 0.0356(11) Uani 1 1 d . . .
H11 H 0.2438 -0.0481 0.1263 0.039 Uiso 1 1 calc R . .
C12 C 0.1328(4) 0.0516(3) 0.1569(4) 0.0397(13) Uani 1 1 d . . .
H12 H 0.0602 0.0223 0.1457 0.044 Uiso 1 1 calc R . .
C13 C 0.1288(4) 0.1333(3) 0.1840(3) 0.0349(12) Uani 1 1 d . . .
H13 H 0.0538 0.1610 0.1907 0.038 Uiso 1 1 calc R . .
C14 C 0.2361(4) 0.1779(3) 0.2027(3) 0.0292(10) Uani 1 1 d . . .
C15 C 0.2248(4) 0.2649(3) 0.2294(3) 0.0328(11) Uani 1 1 d . . .
H15 H 0.1464 0.2883 0.2274 0.036 Uiso 1 1 calc R . .
C16 C 0.4696(4) -0.0616(3) 0.1098(3) 0.0372(12) Uani 1 1 d . . .
H16A H 0.5539 -0.0774 0.1042 0.041 Uiso 1 1 calc R . .
H16B H 0.4322 -0.0588 0.0560 0.041 Uiso 1 1 calc R . .
H16C H 0.4285 -0.1046 0.1427 0.041 Uiso 1 1 calc R . .
O11 O 0.8300(2) 0.1147(2) 0.1493(2) 0.0293(7) Uani 1 1 d . . .
O12 O 0.6885(3) 0.0673(2) 0.0729(2) 0.0346(8) Uani 1 1 d . . .
N2 N 0.7977(3) 0.0888(2) 0.0796(3) 0.0318(9) Uani 1 1 d . . .
O13 O 0.8660(3) 0.0842(3) 0.0237(2) 0.0507(10) Uani 1 1 d . . .
O14 O 0.7070(3) -0.03454(19) 0.2216(2) 0.0315(7) Uani 1 1 d . . .
O15 O 0.5357(3) 0.0469(2) 0.3193(2) 0.0307(7) Uani 1 1 d . . .
C17 C 0.6832(4) -0.0956(3) 0.2665(3) 0.0298(10) Uani 1 1 d . . .
H17 H 0.7304 -0.1455 0.2589 0.033 Uiso 1 1 calc R . .
C18 C 0.5954(4) -0.1010(3) 0.3275(3) 0.0302(10) Uani 1 1 d . . .
C19 C 0.5220(4) -0.0293(3) 0.3474(3) 0.0290(10) Uani 1 1 d . . .
C20 C 0.4283(4) -0.0452(3) 0.4048(3) 0.0393(12) Uani 1 1 d . . .
C21 C 0.4154(5) -0.1229(3) 0.4413(4) 0.0459(14) Uani 1 1 d . . .
H21 H 0.3534 -0.1312 0.4796 0.050 Uiso 1 1 calc R . .
C22 C 0.4932(5) -0.1911(4) 0.4226(4) 0.0462(14) Uani 1 1 d . . .
H22 H 0.4846 -0.2447 0.4492 0.051 Uiso 1 1 calc R . .
C23 C 0.5795(4) -0.1802(3) 0.3672(3) 0.0382(12) Uani 1 1 d . . .
H23 H 0.6308 -0.2267 0.3544 0.042 Uiso 1 1 calc R . .
O16 O 0.3558(4) 0.0240(2) 0.4176(3) 0.0568(12) Uani 1 1 d . . .
C24 C 0.2511(6) 0.0071(5) 0.4639(5) 0.071(2) Uani 1 1 d . . .
H24A H 0.2058 0.0603 0.4710 0.078 Uiso 1 1 calc R . .
H24B H 0.2743 -0.0156 0.5171 0.078 Uiso 1 1 calc R . .
H24C H 0.2014 -0.0351 0.4355 0.078 Uiso 1 1 calc R . .
C25 C 0.3027(6) 0.2229(5) 0.4206(5) 0.0668(19) Uani 1 1 d . . .
H25A H 0.2915 0.1806 0.4638 0.074 Uiso 1 1 calc R . .
H25B H 0.2337 0.2217 0.3839 0.074 Uiso 1 1 calc R . .
H25C H 0.3104 0.2801 0.4444 0.074 Uiso 1 1 calc R . .


_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
Tb O15 2.267(3) . ?
Tb O1 2.305(3) . ?
Tb O2 2.314(3) . ?
Tb O14 2.344(3) . ?
Tb O11 2.447(3) . ?
Tb O12 2.467(3) . ?
Tb O9 2.545(3) . ?
Tb O4 2.565(3) . ?
Tb O3 2.623(3) . ?
Tb N2 2.886(4) . ?
Tb Ni 3.3476(6) . ?
Ni O2 1.990(3) . ?
Ni O1 2.004(3) . ?
Ni O5 2.017(3) . ?
Ni O6 2.031(3) . ?
Ni O7 2.071(3) . ?
Ni O8 2.073(4) . ?
O1 C1 1.308(5) . ?
O2 C9 1.312(5) . ?
O3 C2 1.393(6) . ?
O3 C8 1.441(5) . ?
O4 C10 1.401(5) . ?
O4 C16 1.436(5) . ?
O5 C7 1.218(6) . ?
O6 C15 1.246(5) . ?
O7 C25 1.456(7) . ?
O7 H7A 0.9500 . ?
O8 N1 1.270(5) . ?
O9 N1 1.263(5) . ?
N1 O10 1.231(5) . ?
C1 C6 1.408(6) . ?
C1 C2 1.408(6) . ?
C2 C3 1.368(7) . ?
C3 C4 1.403(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.362(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.408(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.445(6) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C14 1.399(6) . ?
C9 C10 1.406(6) . ?
C10 C11 1.371(6) . ?
C11 C12 1.401(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.352(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.420(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.434(7) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O11 N2 1.270(5) . ?
O12 N2 1.272(5) . ?
N2 O13 1.203(5) . ?
O14 C17 1.236(6) . ?
O15 C19 1.286(5) . ?
C17 C18 1.413(7) . ?
C17 H17 0.9500 . ?
C18 C23 1.410(7) . ?
C18 C19 1.427(6) . ?
C19 C20 1.438(7) . ?
C20 C21 1.363(7) . ?
C20 O16 1.369(6) . ?
C21 C22 1.409(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.345(8) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
O16 C24 1.425(7) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?

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
O15 Tb O1 81.13(11) . . ?
O15 Tb O2 78.71(11) . . ?
O1 Tb O2 71.43(10) . . ?
O15 Tb O14 75.18(11) . . ?
O1 Tb O14 133.96(11) . . ?
O2 Tb O14 138.26(10) . . ?
O15 Tb O11 142.41(11) . . ?
O1 Tb O11 102.12(10) . . ?
O2 Tb O11 138.25(11) . . ?
O14 Tb O11 76.30(11) . . ?
O15 Tb O12 138.69(11) . . ?
O1 Tb O12 139.93(11) . . ?
O2 Tb O12 106.36(11) . . ?
O14 Tb O12 75.04(12) . . ?
O11 Tb O12 51.92(10) . . ?
O15 Tb O9 142.23(10) . . ?
O1 Tb O9 72.12(11) . . ?
O2 Tb O9 67.89(10) . . ?
O14 Tb O9 142.37(11) . . ?
O11 Tb O9 70.91(10) . . ?
O12 Tb O9 70.44(11) . . ?
O15 Tb O4 75.42(11) . . ?
O1 Tb O4 132.03(9) . . ?
O2 Tb O4 63.34(10) . . ?
O14 Tb O4 78.79(10) . . ?
O11 Tb O4 121.88(10) . . ?
O12 Tb O4 71.23(10) . . ?
O9 Tb O4 103.26(10) . . ?
O15 Tb O3 81.69(11) . . ?
O1 Tb O3 62.04(9) . . ?
O2 Tb O3 131.61(10) . . ?
O14 Tb O3 75.74(10) . . ?
O11 Tb O3 67.88(10) . . ?
O12 Tb O3 117.34(10) . . ?
O9 Tb O3 107.36(10) . . ?
O4 Tb O3 149.30(10) . . ?
O15 Tb N2 149.85(11) . . ?
O1 Tb N2 122.34(11) . . ?
O2 Tb N2 124.34(11) . . ?
O14 Tb N2 74.74(11) . . ?
O11 Tb N2 25.92(11) . . ?
O12 Tb N2 26.01(10) . . ?
O9 Tb N2 67.68(10) . . ?
O4 Tb N2 96.79(11) . . ?
O3 Tb N2 92.80(11) . . ?
O15 Tb Ni 78.80(8) . . ?
O1 Tb Ni 35.89(7) . . ?
O2 Tb Ni 35.58(7) . . ?
O14 Tb Ni 153.76(8) . . ?
O11 Tb Ni 125.12(8) . . ?
O12 Tb Ni 129.00(8) . . ?
O9 Tb Ni 63.85(7) . . ?
O4 Tb Ni 97.98(7) . . ?
O3 Tb Ni 97.32(7) . . ?
N2 Tb Ni 131.34(8) . . ?
O2 Ni O1 84.92(11) . . ?
O2 Ni O5 175.21(12) . . ?
O1 Ni O5 90.30(12) . . ?
O2 Ni O6 90.19(12) . . ?
O1 Ni O6 174.65(13) . . ?
O5 Ni O6 94.59(13) . . ?
O2 Ni O7 91.01(13) . . ?
O1 Ni O7 88.29(13) . . ?
O5 Ni O7 88.62(14) . . ?
O6 Ni O7 89.63(14) . . ?
O2 Ni O8 89.20(13) . . ?
O1 Ni O8 91.99(13) . . ?
O5 Ni O8 91.18(14) . . ?
O6 Ni O8 90.10(14) . . ?
O7 Ni O8 179.66(14) . . ?
O2 Ni Tb 42.56(7) . . ?
O1 Ni Tb 42.40(8) . . ?
O5 Ni Tb 132.66(9) . . ?
O6 Ni Tb 132.75(10) . . ?
O7 Ni Tb 91.13(9) . . ?
O8 Ni Tb 89.22(9) . . ?
C1 O1 Ni 125.3(3) . . ?
C1 O1 Tb 129.8(3) . . ?
Ni O1 Tb 101.70(12) . . ?
C9 O2 Ni 123.8(3) . . ?
C9 O2 Tb 126.2(3) . . ?
Ni O2 Tb 101.86(11) . . ?
C2 O3 C8 116.4(3) . . ?
C2 O3 Tb 117.1(2) . . ?
C8 O3 Tb 126.4(3) . . ?
C10 O4 C16 116.9(3) . . ?
C10 O4 Tb 116.1(2) . . ?
C16 O4 Tb 126.5(2) . . ?
C7 O5 Ni 124.8(3) . . ?
C15 O6 Ni 122.6(3) . . ?
C25 O7 Ni 124.4(4) . . ?
C25 O7 H7A 117.8 . . ?
Ni O7 H7A 117.8 . . ?
N1 O8 Ni 124.4(3) . . ?
N1 O9 Tb 139.1(3) . . ?
O10 N1 O9 119.4(4) . . ?
O10 N1 O8 119.2(4) . . ?
O9 N1 O8 121.4(4) . . ?
O1 C1 C6 124.4(4) . . ?
O1 C1 C2 117.7(4) . . ?
C6 C1 C2 117.8(4) . . ?
C3 C2 O3 125.1(4) . . ?
C3 C2 C1 122.3(4) . . ?
O3 C2 C1 112.6(4) . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 119.8(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.6(5) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C5 119.1(4) . . ?
C1 C6 C7 122.8(4) . . ?
C5 C6 C7 118.1(4) . . ?
O5 C7 C6 128.6(4) . . ?
O5 C7 H7 115.7 . . ?
C6 C7 H7 115.7 . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C9 C14 123.9(4) . . ?
O2 C9 C10 117.9(4) . . ?
C14 C9 C10 118.1(4) . . ?
C11 C10 O4 124.8(4) . . ?
C11 C10 C9 122.2(4) . . ?
O4 C10 C9 113.0(3) . . ?
C10 C11 C12 118.6(5) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C13 C12 C11 121.3(4) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 120.3(4) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C9 C14 C13 119.4(4) . . ?
C9 C14 C15 123.4(4) . . ?
C13 C14 C15 117.1(4) . . ?
O6 C15 C14 128.3(4) . . ?
O6 C15 H15 115.9 . . ?
C14 C15 H15 115.9 . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 O11 Tb 96.7(2) . . ?
N2 O12 Tb 95.7(3) . . ?
O13 N2 O11 122.4(4) . . ?
O13 N2 O12 122.0(4) . . ?
O11 N2 O12 115.6(4) . . ?
O13 N2 Tb 178.2(3) . . ?
O11 N2 Tb 57.37(19) . . ?
O12 N2 Tb 58.3(2) . . ?
C17 O14 Tb 132.9(3) . . ?
C19 O15 Tb 135.4(3) . . ?
O14 C17 C18 128.7(4) . . ?
O14 C17 H17 115.6 . . ?
C18 C17 H17 115.6 . . ?
C23 C18 C17 118.2(4) . . ?
C23 C18 C19 120.5(4) . . ?
C17 C18 C19 121.3(4) . . ?
O15 C19 C18 125.0(4) . . ?
O15 C19 C20 119.1(4) . . ?
C18 C19 C20 116.0(4) . . ?
C21 C20 O16 124.8(5) . . ?
C21 C20 C19 121.6(5) . . ?
O16 C20 C19 113.6(4) . . ?
C20 C21 C22 120.6(5) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C23 C22 C21 119.9(5) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C18 121.3(5) . . ?
C22 C23 H23 119.4 . . ?
C18 C23 H23 119.4 . . ?
C20 O16 C24 115.2(4) . . ?
O16 C24 H24A 109.5 . . ?
O16 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O16 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O7 C25 H25A 109.5 . . ?
O7 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O7 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

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
O7 H7A O15 0.95 2.24 2.956(4) 131.1 .
O7 H7A O16 0.95 2.35 2.937(5) 119.7 .

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        26.10
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.109
