# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2016

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

data_mo_20150107d606_0m
_database_code_depnum_ccdc_archive 'CCDC 1434582'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H30 La N5 Ni O15, C H4 O'
_chemical_formula_sum            'C27 H34 La N5 Ni O16'
_chemical_formula_weight         882.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '
_space_group_name_Hall           '-P 2yn   '

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                   9.3155(14)
_cell_length_b                   17.453(3)
_cell_length_c                   21.676(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.652(2)
_cell_angle_gamma                90.00
_cell_volume                     3512.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(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          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1772
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_T_max  0.7245
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17157
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.50
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6135
_reflns_number_gt                5051
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0677P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6135
_refine_ls_number_parameters     457
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.1204
_refine_ls_wR_factor_gt          0.0921
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0824(5) 0.3707(3) 0.39255(19) 0.0312(10) Uani 1 1 d . . .
C2 C -0.0785(5) 0.3822(3) 0.4571(2) 0.0404(12) Uani 1 1 d . . .
C3 C -0.1804(7) 0.4239(4) 0.4832(3) 0.0601(17) Uani 1 1 d . . .
H3 H -0.1750 0.4302 0.5259 0.072 Uiso 1 1 calc R . .
C4 C -0.2927(7) 0.4571(4) 0.4466(3) 0.072(2) Uani 1 1 d . . .
H4 H -0.3626 0.4855 0.4647 0.087 Uiso 1 1 calc R . .
C5 C -0.2999(6) 0.4478(4) 0.3832(3) 0.0571(16) Uani 1 1 d . . .
H5 H -0.3758 0.4696 0.3587 0.069 Uiso 1 1 calc R . .
C6 C -0.1950(5) 0.4061(3) 0.3554(2) 0.0394(12) Uani 1 1 d . . .
C7 C -0.2103(5) 0.4007(3) 0.2887(2) 0.0390(12) Uani 1 1 d . . .
H7 H -0.2960 0.4188 0.2690 0.047 Uiso 1 1 calc R . .
C8 C -0.1105(5) 0.3252(3) 0.1518(2) 0.0450(13) Uani 1 1 d . . .
H8A H -0.1857 0.3058 0.1223 0.054 Uiso 1 1 calc R . .
H8B H -0.0734 0.2826 0.1770 0.054 Uiso 1 1 calc R . .
C9 C 0.0074(6) 0.3581(4) 0.1178(2) 0.0513(14) Uani 1 1 d . . .
H9A H 0.0514 0.3171 0.0958 0.062 Uiso 1 1 calc R . .
H9B H -0.0343 0.3940 0.0872 0.062 Uiso 1 1 calc R . .
C10 C 0.3125(5) 0.3321(3) 0.1955(2) 0.0369(11) Uani 1 1 d . . .
H10 H 0.3468 0.3490 0.1587 0.044 Uiso 1 1 calc R . .
C11 C 0.4128(5) 0.2912(3) 0.2383(2) 0.0346(11) Uani 1 1 d . . .
C12 C 0.5430(6) 0.2684(4) 0.2156(3) 0.0486(14) Uani 1 1 d . . .
H12 H 0.5590 0.2792 0.1747 0.058 Uiso 1 1 calc R . .
C13 C 0.6451(6) 0.2314(4) 0.2512(3) 0.0513(15) Uani 1 1 d . . .
H13 H 0.7297 0.2162 0.2347 0.062 Uiso 1 1 calc R . .
C14 C 0.6248(5) 0.2155(3) 0.3131(3) 0.0469(13) Uani 1 1 d . . .
H14 H 0.6962 0.1910 0.3383 0.056 Uiso 1 1 calc R . .
C15 C 0.4977(5) 0.2368(3) 0.3362(2) 0.0347(11) Uani 1 1 d . . .
C16 C 0.3873(4) 0.2755(3) 0.2998(2) 0.0283(10) Uani 1 1 d . . .
C17 C 0.5839(7) 0.2007(5) 0.4385(3) 0.074(2) Uani 1 1 d . . .
H17A H 0.6143 0.1499 0.4287 0.111 Uiso 1 1 calc R . .
H17B H 0.5549 0.2016 0.4800 0.111 Uiso 1 1 calc R . .
H17C H 0.6622 0.2358 0.4352 0.111 Uiso 1 1 calc R . .
C18 C 0.0545(7) 0.3613(4) 0.5546(2) 0.0659(18) Uani 1 1 d . . .
H18A H 0.0537 0.4157 0.5609 0.099 Uiso 1 1 calc R . .
H18B H 0.1450 0.3407 0.5714 0.099 Uiso 1 1 calc R . .
H18C H -0.0223 0.3382 0.5750 0.099 Uiso 1 1 calc R . .
C19 C 0.0380(5) 0.1623(3) 0.2905(2) 0.0386(12) Uani 1 1 d . . .
C20 C -0.0298(7) 0.0922(4) 0.2623(3) 0.0563(15) Uani 1 1 d . . .
H20A H -0.1162 0.0808 0.2819 0.084 Uiso 1 1 calc R . .
H20B H 0.0360 0.0500 0.2681 0.084 Uiso 1 1 calc R . .
H20C H -0.0530 0.1005 0.2189 0.084 Uiso 1 1 calc R . .
C21 C 0.0953(6) 0.5136(3) 0.2697(2) 0.0486(13) Uani 1 1 d . . .
H21 H 0.0251 0.5052 0.2374 0.058 Uiso 1 1 calc R . .
C22 C 0.1396(7) 0.5858(3) 0.2814(3) 0.0591(16) Uani 1 1 d . . .
H22 H 0.1000 0.6259 0.2574 0.071 Uiso 1 1 calc R . .
C23 C 0.2442(7) 0.6006(4) 0.3289(3) 0.0565(16) Uani 1 1 d . . .
H23 H 0.2770 0.6501 0.3373 0.068 Uiso 1 1 calc R . .
C24 C 0.2975(6) 0.5393(3) 0.3631(2) 0.0509(14) Uani 1 1 d . . .
H24 H 0.3668 0.5465 0.3959 0.061 Uiso 1 1 calc R . .
C25 C 0.2477(5) 0.4679(3) 0.3483(2) 0.0398(12) Uani 1 1 d . . .
H25 H 0.2863 0.4271 0.3718 0.048 Uiso 1 1 calc R . .
C26 C 0.3336(10) 0.0500(4) 0.4157(3) 0.088(2) Uani 1 1 d . . .
H26A H 0.2549 0.0261 0.3917 0.132 Uiso 1 1 calc R . .
H26B H 0.3872 0.0119 0.4398 0.132 Uiso 1 1 calc R . .
H26C H 0.3956 0.0747 0.3885 0.132 Uiso 1 1 calc R . .
C27 C 0.1403(12) 0.9987(5) 0.5900(4) 0.104(3) Uani 1 1 d . . .
H27A H 0.1998 0.9735 0.6221 0.156 Uiso 1 1 calc R . .
H27B H 0.0494 0.9728 0.5840 0.156 Uiso 1 1 calc R . .
H27C H 0.1249 1.0509 0.6018 0.156 Uiso 1 1 calc R . .
La1 La 0.18907(3) 0.241856(15) 0.426162(11) 0.02855(12) Uani 1 1 d . . .
N1 N -0.1188(4) 0.3736(2) 0.25416(16) 0.0368(9) Uani 1 1 d . . .
N2 N 0.1814(4) 0.3469(2) 0.20383(16) 0.0335(9) Uani 1 1 d . . .
N3 N 0.1480(4) 0.4523(2) 0.30293(16) 0.0355(9) Uani 1 1 d . . .
N4 N -0.0356(5) 0.1694(3) 0.5085(2) 0.0518(12) Uani 1 1 d . . .
N5 N 0.4004(5) 0.3320(3) 0.5147(2) 0.0480(11) Uani 1 1 d . . .
Ni1 Ni 0.08487(6) 0.33637(3) 0.28395(2) 0.02780(16) Uani 1 1 d . . .
O1 O 0.0181(3) 0.32716(19) 0.37013(13) 0.0314(7) Uani 1 1 d . . .
O2 O 0.2712(3) 0.29535(19) 0.32695(12) 0.0290(7) Uani 1 1 d . . .
O3 O -0.1712(4) 0.3819(2) 0.19103(15) 0.0510(10) Uani 1 1 d . . .
O4 O 0.1193(4) 0.3974(2) 0.15619(14) 0.0436(9) Uani 1 1 d . . .
O5 O 0.0356(4) 0.3451(2) 0.48962(14) 0.0463(9) Uani 1 1 d . . .
O6 O 0.4662(4) 0.2225(2) 0.39670(16) 0.0438(9) Uani 1 1 d . . .
O7 O 0.2787(5) 0.1058(2) 0.45623(18) 0.0569(10) Uani 1 1 d . . .
H7A H 0.3456 0.1123 0.4848 0.068 Uiso 1 1 d R . .
O8 O 0.0870(4) 0.1860(2) 0.53253(16) 0.0529(10) Uani 1 1 d . . .
O9 O -0.0585(4) 0.1814(3) 0.45151(17) 0.0577(11) Uani 1 1 d . . .
O10 O -0.1292(5) 0.1419(3) 0.5379(2) 0.0837(15) Uani 1 1 d . . .
O11 O 0.3548(4) 0.2641(2) 0.52512(17) 0.0518(10) Uani 1 1 d . . .
O12 O 0.3526(4) 0.3624(2) 0.46576(17) 0.0524(10) Uani 1 1 d . . .
O13 O 0.4857(6) 0.3625(3) 0.5515(2) 0.0920(17) Uani 1 1 d . . .
O14 O 0.0236(4) 0.2242(2) 0.26127(14) 0.0371(8) Uani 1 1 d . . .
O15 O 0.1031(4) 0.1546(2) 0.34341(15) 0.0483(9) Uani 1 1 d . . .
O16 O 0.2060(10) 0.9973(4) 0.5371(3) 0.129(3) Uani 1 1 d . . .
H16 H 0.1461 0.9897 0.5079 0.194 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
C1 O1 1.328(5) . ?
C1 C2 1.411(6) . ?
C1 C6 1.412(6) . ?
C2 C3 1.355(7) . ?
C2 O5 1.387(6) . ?
C3 C4 1.388(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.394(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.444(6) . ?
C7 N1 1.270(6) . ?
C7 H7 0.9300 . ?
C8 O3 1.449(6) . ?
C8 C9 1.486(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O4 1.452(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.275(6) . ?
C10 C11 1.451(7) . ?
C10 H10 0.9300 . ?
C11 C16 1.399(6) . ?
C11 C12 1.404(7) . ?
C12 C13 1.341(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.397(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(7) . ?
C14 H14 0.9300 . ?
C15 O6 1.389(6) . ?
C15 C16 1.417(7) . ?
C16 O2 1.319(5) . ?
C17 O6 1.417(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O5 1.433(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 O14 1.255(6) . ?
C19 O15 1.261(6) . ?
C19 C20 1.485(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.343(8) . ?
C21 N3 1.359(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.383(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.372(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.358(8) . ?
C24 H24 0.9300 . ?
C25 N3 1.326(6) . ?
C25 H25 0.9300 . ?
C26 O7 1.433(7) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 O16 1.344(9) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
La1 O1 2.432(3) . ?
La1 O15 2.438(3) . ?
La1 O2 2.520(3) . ?
La1 O11 2.569(4) . ?
La1 O7 2.583(4) . ?
La1 O9 2.634(4) . ?
La1 O12 2.697(4) . ?
La1 O6 2.730(3) . ?
La1 O5 2.740(3) . ?
La1 O8 2.743(4) . ?
La1 N5 3.069(5) . ?
La1 Ni1 3.5608(7) . ?
N1 O3 1.423(5) . ?
N1 Ni1 2.059(4) . ?
N2 O4 1.443(5) . ?
N2 Ni1 2.028(4) . ?
N3 Ni1 2.138(4) . ?
N4 O10 1.220(5) . ?
N4 O8 1.251(6) . ?
N4 O9 1.253(6) . ?
N5 O13 1.203(6) . ?
N5 O12 1.236(6) . ?
N5 O11 1.285(6) . ?
Ni1 O1 2.023(3) . ?
Ni1 O2 2.033(3) . ?
Ni1 O14 2.086(4) . ?
O7 H7A 0.8500 . ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 118.8(4) . . ?
O1 C1 C6 123.7(4) . . ?
C2 C1 C6 117.5(4) . . ?
C3 C2 O5 124.9(4) . . ?
C3 C2 C1 121.9(5) . . ?
O5 C2 C1 113.3(4) . . ?
C2 C3 C4 120.4(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.8(5) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.7(4) . . ?
C5 C6 C7 116.8(5) . . ?
C1 C6 C7 123.4(4) . . ?
N1 C7 C6 126.7(4) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
O3 C8 C9 111.4(5) . . ?
O3 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
O3 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
O4 C9 C8 115.1(4) . . ?
O4 C9 H9A 108.5 . . ?
C8 C9 H9A 108.5 . . ?
O4 C9 H9B 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
N2 C10 C11 125.6(4) . . ?
N2 C10 H10 117.2 . . ?
C11 C10 H10 117.2 . . ?
C16 C11 C12 119.8(5) . . ?
C16 C11 C10 123.7(4) . . ?
C12 C11 C10 116.4(4) . . ?
C13 C12 C11 121.8(5) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C14 120.2(5) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 119.0(5) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 O6 123.4(5) . . ?
C14 C15 C16 122.3(5) . . ?
O6 C15 C16 114.4(4) . . ?
O2 C16 C11 125.6(4) . . ?
O2 C16 C15 117.4(4) . . ?
C11 C16 C15 116.9(4) . . ?
O6 C17 H17A 109.5 . . ?
O6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5 C18 H18A 109.5 . . ?
O5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O14 C19 O15 125.1(5) . . ?
O14 C19 C20 118.6(5) . . ?
O15 C19 C20 116.3(5) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N3 123.1(6) . . ?
C22 C21 H21 118.4 . . ?
N3 C21 H21 118.4 . . ?
C21 C22 C23 120.2(6) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C24 C23 C22 117.3(6) . . ?
C24 C23 H23 121.3 . . ?
C22 C23 H23 121.3 . . ?
C25 C24 C23 119.1(5) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
N3 C25 C24 124.6(5) . . ?
N3 C25 H25 117.7 . . ?
C24 C25 H25 117.7 . . ?
O7 C26 H26A 109.5 . . ?
O7 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O7 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O16 C27 H27A 109.5 . . ?
O16 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O16 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 La1 O15 81.50(12) . . ?
O1 La1 O2 65.09(9) . . ?
O15 La1 O2 73.00(11) . . ?
O1 La1 O11 130.49(12) . . ?
O15 La1 O11 148.01(13) . . ?
O2 La1 O11 116.94(11) . . ?
O1 La1 O7 150.92(13) . . ?
O15 La1 O7 72.04(13) . . ?
O2 La1 O7 116.21(11) . . ?
O11 La1 O7 76.60(13) . . ?
O1 La1 O9 78.49(12) . . ?
O15 La1 O9 70.28(12) . . ?
O2 La1 O9 131.15(10) . . ?
O11 La1 O9 111.32(12) . . ?
O7 La1 O9 81.35(14) . . ?
O1 La1 O12 90.65(11) . . ?
O15 La1 O12 149.85(12) . . ?
O2 La1 O12 77.28(10) . . ?
O11 La1 O12 47.97(12) . . ?
O7 La1 O12 118.32(12) . . ?
O9 La1 O12 136.68(12) . . ?
O1 La1 O6 123.54(10) . . ?
O15 La1 O6 90.62(12) . . ?
O2 La1 O6 59.20(10) . . ?
O11 La1 O6 72.44(12) . . ?
O7 La1 O6 69.67(12) . . ?
O9 La1 O6 149.26(13) . . ?
O12 La1 O6 69.57(12) . . ?
O1 La1 O5 60.04(10) . . ?
O15 La1 O5 128.81(12) . . ?
O2 La1 O5 113.06(10) . . ?
O11 La1 O5 77.53(12) . . ?
O7 La1 O5 130.49(11) . . ?
O9 La1 O5 69.97(13) . . ?
O12 La1 O5 68.35(12) . . ?
O6 La1 O5 137.81(12) . . ?
O1 La1 O8 112.32(10) . . ?
O15 La1 O8 106.32(12) . . ?
O2 La1 O8 177.35(10) . . ?
O11 La1 O8 65.02(12) . . ?
O7 La1 O8 65.68(12) . . ?
O9 La1 O8 46.64(11) . . ?
O12 La1 O8 103.59(12) . . ?
O6 La1 O8 123.45(11) . . ?
O5 La1 O8 65.24(11) . . ?
O1 La1 N5 111.05(12) . . ?
O15 La1 N5 159.37(13) . . ?
O2 La1 N5 96.89(11) . . ?
O11 La1 N5 24.33(12) . . ?
O7 La1 N5 97.81(13) . . ?
O9 La1 N5 127.07(11) . . ?
O12 La1 N5 23.64(11) . . ?
O6 La1 N5 68.85(12) . . ?
O5 La1 N5 71.52(12) . . ?
O8 La1 N5 84.55(12) . . ?
O1 La1 Ni1 33.14(6) . . ?
O15 La1 Ni1 66.56(8) . . ?
O2 La1 Ni1 33.88(6) . . ?
O11 La1 Ni1 139.11(9) . . ?
O7 La1 Ni1 134.76(9) . . ?
O9 La1 Ni1 100.63(9) . . ?
O12 La1 Ni1 91.22(8) . . ?
O6 La1 Ni1 92.95(7) . . ?
O5 La1 Ni1 90.75(7) . . ?
O8 La1 Ni1 143.47(8) . . ?
N5 La1 Ni1 114.82(9) . . ?
C7 N1 O3 109.5(4) . . ?
C7 N1 Ni1 125.3(3) . . ?
O3 N1 Ni1 124.7(3) . . ?
C10 N2 O4 110.8(4) . . ?
C10 N2 Ni1 126.9(3) . . ?
O4 N2 Ni1 119.2(3) . . ?
C25 N3 C21 115.6(5) . . ?
C25 N3 Ni1 120.2(3) . . ?
C21 N3 Ni1 124.2(3) . . ?
O10 N4 O8 122.7(5) . . ?
O10 N4 O9 120.6(5) . . ?
O8 N4 O9 116.7(4) . . ?
O13 N5 O12 123.5(5) . . ?
O13 N5 O11 120.1(5) . . ?
O12 N5 O11 116.5(4) . . ?
O13 N5 La1 175.3(4) . . ?
O12 N5 La1 61.0(3) . . ?
O11 N5 La1 55.5(2) . . ?
O1 Ni1 N2 171.56(14) . . ?
O1 Ni1 O2 82.17(11) . . ?
N2 Ni1 O2 90.16(14) . . ?
O1 Ni1 N1 88.29(13) . . ?
N2 Ni1 N1 99.46(15) . . ?
O2 Ni1 N1 170.33(13) . . ?
O1 Ni1 O14 92.54(13) . . ?
N2 Ni1 O14 90.85(15) . . ?
O2 Ni1 O14 89.13(13) . . ?
N1 Ni1 O14 89.69(15) . . ?
O1 Ni1 N3 89.88(14) . . ?
N2 Ni1 N3 86.85(15) . . ?
O2 Ni1 N3 91.93(14) . . ?
N1 Ni1 N3 89.64(16) . . ?
O14 Ni1 N3 177.47(13) . . ?
O1 Ni1 La1 41.09(8) . . ?
N2 Ni1 La1 132.41(11) . . ?
O2 Ni1 La1 43.72(8) . . ?
N1 Ni1 La1 126.67(11) . . ?
O14 Ni1 La1 79.61(9) . . ?
N3 Ni1 La1 102.74(10) . . ?
C1 O1 Ni1 124.8(3) . . ?
C1 O1 La1 128.3(3) . . ?
Ni1 O1 La1 105.77(12) . . ?
C16 O2 Ni1 126.0(3) . . ?
C16 O2 La1 126.9(3) . . ?
Ni1 O2 La1 102.40(11) . . ?
N1 O3 C8 112.1(4) . . ?
N2 O4 C9 110.4(4) . . ?
C2 O5 C18 115.9(4) . . ?
C2 O5 La1 117.5(3) . . ?
C18 O5 La1 126.5(3) . . ?
C15 O6 C17 116.2(4) . . ?
C15 O6 La1 118.3(3) . . ?
C17 O6 La1 125.5(3) . . ?
C26 O7 La1 126.5(4) . . ?
C26 O7 H7A 105.1 . . ?
La1 O7 H7A 105.4 . . ?
N4 O8 La1 95.6(3) . . ?
N4 O9 La1 101.0(3) . . ?
N5 O11 La1 100.2(3) . . ?
N5 O12 La1 95.3(3) . . ?
C19 O14 Ni1 132.3(3) . . ?
C19 O15 La1 135.1(3) . . ?
C27 O16 H16 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -177.8(5) . . . . ?
C6 C1 C2 C3 1.7(8) . . . . ?
O1 C1 C2 O5 0.4(7) . . . . ?
C6 C1 C2 O5 179.9(4) . . . . ?
O5 C2 C3 C4 -178.2(6) . . . . ?
C1 C2 C3 C4 -0.3(10) . . . . ?
C2 C3 C4 C5 -0.3(11) . . . . ?
C3 C4 C5 C6 -0.7(11) . . . . ?
C4 C5 C6 C1 2.3(9) . . . . ?
C4 C5 C6 C7 -178.9(6) . . . . ?
O1 C1 C6 C5 176.8(5) . . . . ?
C2 C1 C6 C5 -2.7(8) . . . . ?
O1 C1 C6 C7 -1.9(8) . . . . ?
C2 C1 C6 C7 178.6(5) . . . . ?
C5 C6 C7 N1 171.0(6) . . . . ?
C1 C6 C7 N1 -10.2(9) . . . . ?
O3 C8 C9 O4 52.1(6) . . . . ?
N2 C10 C11 C16 -13.0(8) . . . . ?
N2 C10 C11 C12 168.4(5) . . . . ?
C16 C11 C12 C13 0.1(8) . . . . ?
C10 C11 C12 C13 178.8(5) . . . . ?
C11 C12 C13 C14 -1.1(9) . . . . ?
C12 C13 C14 C15 1.6(9) . . . . ?
C13 C14 C15 O6 178.9(5) . . . . ?
C13 C14 C15 C16 -1.2(8) . . . . ?
C12 C11 C16 O2 178.3(5) . . . . ?
C10 C11 C16 O2 -0.2(8) . . . . ?
C12 C11 C16 C15 0.3(7) . . . . ?
C10 C11 C16 C15 -178.3(5) . . . . ?
C14 C15 C16 O2 -178.0(5) . . . . ?
O6 C15 C16 O2 2.0(6) . . . . ?
C14 C15 C16 C11 0.3(7) . . . . ?
O6 C15 C16 C11 -179.8(4) . . . . ?
N3 C21 C22 C23 0.3(9) . . . . ?
C21 C22 C23 C24 -0.8(9) . . . . ?
C22 C23 C24 C25 1.0(8) . . . . ?
C23 C24 C25 N3 -0.9(8) . . . . ?
C6 C7 N1 O3 -177.1(5) . . . . ?
C6 C7 N1 Ni1 -4.5(8) . . . . ?
C11 C10 N2 O4 172.0(4) . . . . ?
C11 C10 N2 Ni1 12.4(7) . . . . ?
C24 C25 N3 C21 0.3(7) . . . . ?
C24 C25 N3 Ni1 178.4(4) . . . . ?
C22 C21 N3 C25 0.0(8) . . . . ?
C22 C21 N3 Ni1 -178.0(4) . . . . ?
O1 La1 N5 O12 -31.9(3) . . . . ?
O15 La1 N5 O12 93.0(5) . . . . ?
O2 La1 N5 O12 34.0(3) . . . . ?
O11 La1 N5 O12 -178.8(5) . . . . ?
O7 La1 N5 O12 151.7(3) . . . . ?
O9 La1 N5 O12 -123.2(3) . . . . ?
O6 La1 N5 O12 87.1(3) . . . . ?
O5 La1 N5 O12 -78.1(3) . . . . ?
O8 La1 N5 O12 -143.8(3) . . . . ?
Ni1 La1 N5 O12 3.9(3) . . . . ?
O1 La1 N5 O11 146.9(3) . . . . ?
O15 La1 N5 O11 -88.2(4) . . . . ?
O2 La1 N5 O11 -147.2(3) . . . . ?
O7 La1 N5 O11 -29.4(3) . . . . ?
O9 La1 N5 O11 55.6(4) . . . . ?
O12 La1 N5 O11 178.8(5) . . . . ?
O6 La1 N5 O11 -94.0(3) . . . . ?
O5 La1 N5 O11 100.7(3) . . . . ?
O8 La1 N5 O11 35.1(3) . . . . ?
Ni1 La1 N5 O11 -177.3(3) . . . . ?
C10 N2 Ni1 O2 -1.9(4) . . . . ?
O4 N2 Ni1 O2 -160.0(3) . . . . ?
C10 N2 Ni1 N1 179.1(4) . . . . ?
O4 N2 Ni1 N1 21.1(3) . . . . ?
C10 N2 Ni1 O14 -91.1(4) . . . . ?
O4 N2 Ni1 O14 110.9(3) . . . . ?
C10 N2 Ni1 N3 90.0(4) . . . . ?
O4 N2 Ni1 N3 -68.0(3) . . . . ?
C10 N2 Ni1 La1 -14.4(5) . . . . ?
O4 N2 Ni1 La1 -172.4(2) . . . . ?
C7 N1 Ni1 N2 -157.1(4) . . . . ?
O3 N1 Ni1 N2 14.4(4) . . . . ?
C7 N1 Ni1 O14 112.1(4) . . . . ?
O3 N1 Ni1 O14 -76.4(4) . . . . ?
C7 N1 Ni1 N3 -70.3(4) . . . . ?
O3 N1 Ni1 N3 101.2(4) . . . . ?
C7 N1 Ni1 La1 35.3(5) . . . . ?
O3 N1 Ni1 La1 -153.1(3) . . . . ?
C25 N3 Ni1 O1 61.0(4) . . . . ?
C21 N3 Ni1 O1 -121.1(4) . . . . ?
C25 N3 Ni1 N2 -111.2(4) . . . . ?
C21 N3 Ni1 N2 66.7(4) . . . . ?
C25 N3 Ni1 O2 -21.1(4) . . . . ?
C21 N3 Ni1 O2 156.7(4) . . . . ?
C25 N3 Ni1 N1 149.3(4) . . . . ?
C21 N3 Ni1 N1 -32.8(4) . . . . ?
C25 N3 Ni1 La1 21.7(4) . . . . ?
C21 N3 Ni1 La1 -160.5(4) . . . . ?
O15 La1 Ni1 O1 111.69(17) . . . . ?
O2 La1 Ni1 O1 -154.05(19) . . . . ?
O11 La1 Ni1 O1 -92.6(2) . . . . ?
O7 La1 Ni1 O1 137.1(2) . . . . ?
O9 La1 Ni1 O1 48.79(17) . . . . ?
O12 La1 Ni1 O1 -89.32(17) . . . . ?
O6 La1 Ni1 O1 -158.92(17) . . . . ?
O5 La1 Ni1 O1 -20.96(17) . . . . ?
O8 La1 Ni1 O1 25.7(2) . . . . ?
N5 La1 Ni1 O1 -90.89(17) . . . . ?
O1 La1 Ni1 N2 172.3(2) . . . . ?
O15 La1 Ni1 N2 -76.04(18) . . . . ?
O2 La1 Ni1 N2 18.2(2) . . . . ?
O11 La1 Ni1 N2 79.7(2) . . . . ?
O7 La1 Ni1 N2 -50.6(2) . . . . ?
O9 La1 Ni1 N2 -138.93(18) . . . . ?
O12 La1 Ni1 N2 82.96(18) . . . . ?
O6 La1 Ni1 N2 13.35(18) . . . . ?
O5 La1 Ni1 N2 151.32(17) . . . . ?
O8 La1 Ni1 N2 -162.0(2) . . . . ?
N5 La1 Ni1 N2 81.38(18) . . . . ?
O1 La1 Ni1 O2 154.05(19) . . . . ?
O15 La1 Ni1 O2 -94.26(16) . . . . ?
O11 La1 Ni1 O2 61.44(19) . . . . ?
O7 La1 Ni1 O2 -68.85(19) . . . . ?
O9 La1 Ni1 O2 -157.16(16) . . . . ?
O12 La1 Ni1 O2 64.73(15) . . . . ?
O6 La1 Ni1 O2 -4.87(16) . . . . ?
O5 La1 Ni1 O2 133.09(15) . . . . ?
O8 La1 Ni1 O2 179.80(19) . . . . ?
N5 La1 Ni1 O2 63.16(16) . . . . ?
O1 La1 Ni1 N1 -24.4(2) . . . . ?
O15 La1 Ni1 N1 87.25(18) . . . . ?
O2 La1 Ni1 N1 -178.5(2) . . . . ?
O11 La1 Ni1 N1 -117.1(2) . . . . ?
O7 La1 Ni1 N1 112.7(2) . . . . ?
O9 La1 Ni1 N1 24.35(18) . . . . ?
O12 La1 Ni1 N1 -113.76(17) . . . . ?
O6 La1 Ni1 N1 176.64(17) . . . . ?
O5 La1 Ni1 N1 -45.40(17) . . . . ?
O8 La1 Ni1 N1 1.3(2) . . . . ?
N5 La1 Ni1 N1 -115.33(17) . . . . ?
O1 La1 Ni1 O14 -106.19(17) . . . . ?
O15 La1 Ni1 O14 5.50(14) . . . . ?
O2 La1 Ni1 O14 99.76(16) . . . . ?
O11 La1 Ni1 O14 161.20(17) . . . . ?
O7 La1 Ni1 O14 30.91(16) . . . . ?
O9 La1 Ni1 O14 -57.40(13) . . . . ?
O12 La1 Ni1 O14 164.49(13) . . . . ?
O6 La1 Ni1 O14 94.89(13) . . . . ?
O5 La1 Ni1 O14 -127.15(12) . . . . ?
O8 La1 Ni1 O14 -80.44(18) . . . . ?
N5 La1 Ni1 O14 162.92(13) . . . . ?
O1 La1 Ni1 N3 74.79(18) . . . . ?
O15 La1 Ni1 N3 -173.52(15) . . . . ?
O2 La1 Ni1 N3 -79.26(17) . . . . ?
O11 La1 Ni1 N3 -17.83(18) . . . . ?
O7 La1 Ni1 N3 -148.11(17) . . . . ?
O9 La1 Ni1 N3 123.58(14) . . . . ?
O12 La1 Ni1 N3 -14.53(14) . . . . ?
O6 La1 Ni1 N3 -84.13(14) . . . . ?
O5 La1 Ni1 N3 53.83(13) . . . . ?
O8 La1 Ni1 N3 100.53(18) . . . . ?
N5 La1 Ni1 N3 -16.10(14) . . . . ?
C2 C1 O1 Ni1 -153.6(4) . . . . ?
C6 C1 O1 Ni1 26.9(6) . . . . ?
C2 C1 O1 La1 12.9(6) . . . . ?
C6 C1 O1 La1 -166.6(4) . . . . ?
O2 Ni1 O1 C1 151.2(4) . . . . ?
N1 Ni1 O1 C1 -30.4(4) . . . . ?
O14 Ni1 O1 C1 -120.0(3) . . . . ?
N3 Ni1 O1 C1 59.2(4) . . . . ?
La1 Ni1 O1 C1 169.0(4) . . . . ?
O2 Ni1 O1 La1 -17.77(13) . . . . ?
N1 Ni1 O1 La1 160.61(16) . . . . ?
O14 Ni1 O1 La1 71.00(14) . . . . ?
N3 Ni1 O1 La1 -109.74(15) . . . . ?
O15 La1 O1 C1 132.0(4) . . . . ?
O2 La1 O1 C1 -152.9(4) . . . . ?
O11 La1 O1 C1 -47.8(4) . . . . ?
O7 La1 O1 C1 107.5(4) . . . . ?
O9 La1 O1 C1 60.5(4) . . . . ?
O12 La1 O1 C1 -77.2(4) . . . . ?
O6 La1 O1 C1 -142.9(3) . . . . ?
O5 La1 O1 C1 -12.9(3) . . . . ?
O8 La1 O1 C1 27.8(4) . . . . ?
N5 La1 O1 C1 -65.0(4) . . . . ?
Ni1 La1 O1 C1 -168.5(4) . . . . ?
O15 La1 O1 Ni1 -59.54(14) . . . . ?
O2 La1 O1 Ni1 15.60(12) . . . . ?
O11 La1 O1 Ni1 120.69(15) . . . . ?
O7 La1 O1 Ni1 -84.0(2) . . . . ?
O9 La1 O1 Ni1 -131.01(16) . . . . ?
O12 La1 O1 Ni1 91.24(15) . . . . ?
O6 La1 O1 Ni1 25.53(19) . . . . ?
O5 La1 O1 Ni1 155.62(19) . . . . ?
O8 La1 O1 Ni1 -163.77(13) . . . . ?
N5 La1 O1 Ni1 103.48(14) . . . . ?
C11 C16 O2 Ni1 11.8(6) . . . . ?
C15 C16 O2 Ni1 -170.1(3) . . . . ?
C11 C16 O2 La1 163.2(4) . . . . ?
C15 C16 O2 La1 -18.7(6) . . . . ?
O1 Ni1 O2 C16 173.8(4) . . . . ?
N2 Ni1 O2 C16 -9.7(4) . . . . ?
O14 Ni1 O2 C16 81.1(3) . . . . ?
N3 Ni1 O2 C16 -96.6(3) . . . . ?
La1 Ni1 O2 C16 156.9(4) . . . . ?
O1 Ni1 O2 La1 16.88(13) . . . . ?
N2 Ni1 O2 La1 -166.65(15) . . . . ?
O14 Ni1 O2 La1 -75.81(13) . . . . ?
N3 Ni1 O2 La1 106.49(14) . . . . ?
O1 La1 O2 C16 -171.9(3) . . . . ?
O15 La1 O2 C16 -83.6(3) . . . . ?
O11 La1 O2 C16 63.5(3) . . . . ?
O7 La1 O2 C16 -24.2(4) . . . . ?
O9 La1 O2 C16 -126.2(3) . . . . ?
O12 La1 O2 C16 91.3(3) . . . . ?
O6 La1 O2 C16 17.7(3) . . . . ?
O5 La1 O2 C16 150.8(3) . . . . ?
N5 La1 O2 C16 78.0(3) . . . . ?
Ni1 La1 O2 C16 -156.7(4) . . . . ?
O1 La1 O2 Ni1 -15.29(11) . . . . ?
O15 La1 O2 Ni1 73.08(14) . . . . ?
O11 La1 O2 Ni1 -139.84(13) . . . . ?
O7 La1 O2 Ni1 132.43(14) . . . . ?
O9 La1 O2 Ni1 30.4(2) . . . . ?
O12 La1 O2 Ni1 -112.05(14) . . . . ?
O6 La1 O2 Ni1 174.34(18) . . . . ?
O5 La1 O2 Ni1 -52.52(16) . . . . ?
N5 La1 O2 Ni1 -125.33(14) . . . . ?
C7 N1 O3 C8 -154.2(4) . . . . ?
Ni1 N1 O3 C8 33.1(5) . . . . ?
C9 C8 O3 N1 -101.3(5) . . . . ?
C10 N2 O4 C9 113.6(4) . . . . ?
Ni1 N2 O4 C9 -85.1(4) . . . . ?
C8 C9 O4 N2 56.4(6) . . . . ?
C3 C2 O5 C18 -8.4(8) . . . . ?
C1 C2 O5 C18 173.5(5) . . . . ?
C3 C2 O5 La1 167.5(5) . . . . ?
C1 C2 O5 La1 -10.6(5) . . . . ?
O1 La1 O5 C2 11.6(3) . . . . ?
O15 La1 O5 C2 -35.3(4) . . . . ?
O2 La1 O5 C2 50.9(4) . . . . ?
O11 La1 O5 C2 165.1(4) . . . . ?
O7 La1 O5 C2 -134.9(3) . . . . ?
O9 La1 O5 C2 -76.4(3) . . . . ?
O12 La1 O5 C2 115.7(3) . . . . ?
O6 La1 O5 C2 119.9(3) . . . . ?
O8 La1 O5 C2 -126.8(4) . . . . ?
N5 La1 O5 C2 140.7(4) . . . . ?
Ni1 La1 O5 C2 24.7(3) . . . . ?
O1 La1 O5 C18 -173.0(5) . . . . ?
O15 La1 O5 C18 140.0(4) . . . . ?
O2 La1 O5 C18 -133.7(4) . . . . ?
O11 La1 O5 C18 -19.5(5) . . . . ?
O7 La1 O5 C18 40.4(5) . . . . ?
O9 La1 O5 C18 99.0(5) . . . . ?
O12 La1 O5 C18 -69.0(5) . . . . ?
O6 La1 O5 C18 -64.7(5) . . . . ?
O8 La1 O5 C18 48.5(5) . . . . ?
N5 La1 O5 C18 -44.0(5) . . . . ?
Ni1 La1 O5 C18 -160.0(5) . . . . ?
C14 C15 O6 C17 14.3(8) . . . . ?
C16 C15 O6 C17 -165.7(5) . . . . ?
C14 C15 O6 La1 -167.3(4) . . . . ?
C16 C15 O6 La1 12.7(5) . . . . ?
O1 La1 O6 C15 -25.3(4) . . . . ?
O15 La1 O6 C15 54.9(3) . . . . ?
O2 La1 O6 C15 -14.8(3) . . . . ?
O11 La1 O6 C15 -152.7(4) . . . . ?
O7 La1 O6 C15 125.5(4) . . . . ?
O9 La1 O6 C15 105.0(4) . . . . ?
O12 La1 O6 C15 -101.8(3) . . . . ?
O5 La1 O6 C15 -106.0(3) . . . . ?
O8 La1 O6 C15 165.1(3) . . . . ?
N5 La1 O6 C15 -127.1(4) . . . . ?
Ni1 La1 O6 C15 -11.6(3) . . . . ?
O1 La1 O6 C17 153.0(5) . . . . ?
O15 La1 O6 C17 -126.8(5) . . . . ?
O2 La1 O6 C17 163.5(6) . . . . ?
O11 La1 O6 C17 25.6(5) . . . . ?
O7 La1 O6 C17 -56.3(5) . . . . ?
O9 La1 O6 C17 -76.8(6) . . . . ?
O12 La1 O6 C17 76.4(5) . . . . ?
O5 La1 O6 C17 72.2(5) . . . . ?
O8 La1 O6 C17 -16.7(6) . . . . ?
N5 La1 O6 C17 51.1(5) . . . . ?
Ni1 La1 O6 C17 166.6(5) . . . . ?
O1 La1 O7 C26 66.2(6) . . . . ?
O15 La1 O7 C26 40.7(5) . . . . ?
O2 La1 O7 C26 -19.1(6) . . . . ?
O11 La1 O7 C26 -132.8(6) . . . . ?
O9 La1 O7 C26 112.7(6) . . . . ?
O12 La1 O7 C26 -108.4(6) . . . . ?
O6 La1 O7 C26 -56.9(5) . . . . ?
O5 La1 O7 C26 166.9(5) . . . . ?
O8 La1 O7 C26 158.8(6) . . . . ?
N5 La1 O7 C26 -120.8(6) . . . . ?
Ni1 La1 O7 C26 16.3(6) . . . . ?
O10 N4 O8 La1 -179.1(5) . . . . ?
O9 N4 O8 La1 2.0(5) . . . . ?
O1 La1 O8 N4 45.7(3) . . . . ?
O15 La1 O8 N4 -41.7(3) . . . . ?
O11 La1 O8 N4 171.3(3) . . . . ?
O7 La1 O8 N4 -102.7(3) . . . . ?
O9 La1 O8 N4 -1.2(3) . . . . ?
O12 La1 O8 N4 142.1(3) . . . . ?
O6 La1 O8 N4 -143.6(3) . . . . ?
O5 La1 O8 N4 84.1(3) . . . . ?
N5 La1 O8 N4 156.2(3) . . . . ?
Ni1 La1 O8 N4 30.8(4) . . . . ?
O10 N4 O9 La1 179.0(5) . . . . ?
O8 N4 O9 La1 -2.1(5) . . . . ?
O1 La1 O9 N4 -135.3(3) . . . . ?
O15 La1 O9 N4 139.7(4) . . . . ?
O2 La1 O9 N4 -176.8(3) . . . . ?
O11 La1 O9 N4 -6.1(4) . . . . ?
O7 La1 O9 N4 65.8(3) . . . . ?
O12 La1 O9 N4 -56.8(4) . . . . ?
O6 La1 O9 N4 85.2(4) . . . . ?
O5 La1 O9 N4 -73.2(3) . . . . ?
O8 La1 O9 N4 1.2(3) . . . . ?
N5 La1 O9 N4 -27.5(4) . . . . ?
Ni1 La1 O9 N4 -160.1(3) . . . . ?
O13 N5 O11 La1 -178.4(5) . . . . ?
O12 N5 O11 La1 1.2(5) . . . . ?
O1 La1 O11 N5 -42.1(4) . . . . ?
O15 La1 O11 N5 138.3(3) . . . . ?
O2 La1 O11 N5 37.1(3) . . . . ?
O7 La1 O11 N5 150.0(3) . . . . ?
O9 La1 O11 N5 -135.0(3) . . . . ?
O12 La1 O11 N5 -0.6(3) . . . . ?
O6 La1 O11 N5 77.4(3) . . . . ?
O5 La1 O11 N5 -72.6(3) . . . . ?
O8 La1 O11 N5 -140.9(3) . . . . ?
Ni1 La1 O11 N5 3.8(4) . . . . ?
O13 N5 O12 La1 178.4(5) . . . . ?
O11 N5 O12 La1 -1.1(5) . . . . ?
O1 La1 O12 N5 150.4(3) . . . . ?
O15 La1 O12 N5 -135.5(3) . . . . ?
O2 La1 O12 N5 -145.3(3) . . . . ?
O11 La1 O12 N5 0.7(3) . . . . ?
O7 La1 O12 N5 -32.2(3) . . . . ?
O9 La1 O12 N5 76.6(3) . . . . ?
O6 La1 O12 N5 -83.7(3) . . . . ?
O5 La1 O12 N5 93.2(3) . . . . ?
O8 La1 O12 N5 37.3(3) . . . . ?
Ni1 La1 O12 N5 -176.4(3) . . . . ?
O15 C19 O14 Ni1 -3.0(8) . . . . ?
C20 C19 O14 Ni1 175.0(4) . . . . ?
O1 Ni1 O14 C19 -43.4(4) . . . . ?
N2 Ni1 O14 C19 128.8(4) . . . . ?
O2 Ni1 O14 C19 38.7(4) . . . . ?
N1 Ni1 O14 C19 -131.7(4) . . . . ?
La1 Ni1 O14 C19 -4.2(4) . . . . ?
O14 C19 O15 La1 14.8(8) . . . . ?
C20 C19 O15 La1 -163.3(4) . . . . ?
O1 La1 O15 C19 18.4(5) . . . . ?
O2 La1 O15 C19 -48.0(5) . . . . ?
O11 La1 O15 C19 -161.9(4) . . . . ?
O7 La1 O15 C19 -173.8(5) . . . . ?
O9 La1 O15 C19 99.2(5) . . . . ?
O12 La1 O15 C19 -58.0(6) . . . . ?
O6 La1 O15 C19 -105.4(5) . . . . ?
O5 La1 O15 C19 58.3(5) . . . . ?
O8 La1 O15 C19 129.3(5) . . . . ?
N5 La1 O15 C19 -110.9(5) . . . . ?
Ni1 La1 O15 C19 -12.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.141
####################################################################### 
# 
# 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_d691
_database_code_depnum_ccdc_archive 'CCDC 1434583'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_audit_creation_date             2015-07-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C25 H26 Dy N5 Ni O14'
_chemical_formula_sum            'C25 H26 Dy N5 Ni O14'
_chemical_formula_weight         841.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4571(15)
_cell_length_b                   12.3081(17)
_cell_length_c                   12.5899(17)
_cell_angle_alpha                65.463(13)
_cell_angle_beta                 75.741(12)
_cell_angle_gamma                85.765(11)
_cell_volume                     1564.5(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3302
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.3310
_cell_measurement_theta_min      3.6340
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.046
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.31
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11771
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.311
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -37.00   39.00   2.0000    3.0500
omega____ theta____ kappa____ phi______ frames
    -       20.8979  -57.0000  150.0000 38

#__ type_ start__ end____ width___ exp.time_
  2 omega  -47.00   37.00   2.0000    3.0500
omega____ theta____ kappa____ phi______ frames
    -       20.8979  -57.0000   30.0000 42

#__ type_ start__ end____ width___ exp.time_
  3 omega   -3.00   23.00   2.0000    3.0500
omega____ theta____ kappa____ phi______ frames
    -      -16.8354  -99.0000  -60.0000 13

#__ type_ start__ end____ width___ exp.time_
  4 omega  -17.00   21.00   2.0000    3.0500
omega____ theta____ kappa____ phi______ frames
    -      -16.8354  -99.0000 -180.0000 19

#__ type_ start__ end____ width___ exp.time_
  5 omega   53.00   85.00   2.0000    3.0500
omega____ theta____ kappa____ phi______ frames
    -       20.8979 -178.0000    0.0000 16

#__ type_ start__ end____ width___ exp.time_
  6 omega  -46.00   44.00   2.0000    3.0500
omega____ theta____ kappa____ phi______ frames
    -       20.8979  -77.0000  -60.0000 45

#__ type_ start__ end____ width___ exp.time_
  7 omega   -1.00   33.00   2.0000    3.0500
omega____ theta____ kappa____ phi______ frames
    -       20.8979   38.0000 -180.0000 17
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0312105000
_diffrn_orient_matrix_UB_12      -0.0535385000
_diffrn_orient_matrix_UB_13      0.0440221000
_diffrn_orient_matrix_UB_21      -0.0382410000
_diffrn_orient_matrix_UB_22      0.0332787000
_diffrn_orient_matrix_UB_23      0.0281692000
_diffrn_orient_matrix_UB_31      -0.0405958000
_diffrn_orient_matrix_UB_32      0.0065927000
_diffrn_orient_matrix_UB_33      -0.0365211000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5171
_reflns_number_total             6116
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0714
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C13(H13), C11(H11), C8(H8), C5(H5), C4(H4), C3(H3),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.23713(2) 0.80100(2) 0.28086(2) 0.01972(8) Uani 1 1 d . . . . .
Ni1 Ni 0.22276(6) 0.60367(5) 0.16027(5) 0.01870(15) Uani 1 1 d . . . . .
O8 O 0.1929(3) 0.6130(3) 0.4306(3) 0.0244(8) Uani 1 1 d . . . . .
O6 O 0.4374(3) 0.7582(3) 0.3264(3) 0.0255(8) Uani 1 1 d . . . . .
O7 O 0.1805(3) 0.4888(3) 0.3435(3) 0.0253(8) Uani 1 1 d . . . . .
O5 O 0.3517(3) 0.6794(3) 0.1979(3) 0.0179(7) Uani 1 1 d . . . . .
O4 O 0.3295(3) 0.4299(3) 0.0563(3) 0.0325(9) Uani 1 1 d . . . . .
O3 O 0.0620(3) 0.4344(3) 0.1287(3) 0.0350(10) Uani 1 1 d . . . . .
O2 O 0.1260(3) 0.7343(3) 0.1916(3) 0.0193(7) Uani 1 1 d . . . . .
O1 O 0.0750(3) 0.9437(3) 0.1856(3) 0.0240(8) Uani 1 1 d . . . . .
O12 O 0.0558(3) 0.8232(3) 0.4262(3) 0.0309(9) Uani 1 1 d . . . . .
O13 O 0.2266(3) 0.8379(3) 0.4613(3) 0.0382(10) Uani 1 1 d . . . . .
O14 O 0.0603(4) 0.8574(4) 0.5815(3) 0.0505(12) Uani 1 1 d . . . . .
O10 O 0.3168(3) 1.0016(3) 0.2178(3) 0.0300(9) Uani 1 1 d . . . . .
O9 O 0.3400(3) 0.9379(3) 0.0771(3) 0.0287(9) Uani 1 1 d . . . . .
O11 O 0.3940(3) 1.1224(3) 0.0296(3) 0.0358(10) Uani 1 1 d . . . . .
N3 N 0.2741(4) 0.7141(3) -0.0283(3) 0.0213(9) Uani 1 1 d . . . . .
N2 N 0.3447(4) 0.4861(4) 0.1319(3) 0.0237(10) Uani 1 1 d . . . . .
N1 N 0.0672(4) 0.5415(4) 0.1449(3) 0.0233(10) Uani 1 1 d . . . . .
N5 N 0.1130(4) 0.8394(4) 0.4925(4) 0.0296(11) Uani 1 1 d . . . . .
N4 N 0.3528(4) 1.0238(4) 0.1044(4) 0.0284(11) Uani 1 1 d . . . . .
C24 C 0.1682(4) 0.5131(4) 0.4337(4) 0.0196(11) Uani 1 1 d . . . . .
C18 C 0.4933(5) 0.8133(5) 0.3829(5) 0.0326(14) Uani 1 1 d . . . . .
H18A H 0.4520 0.8846 0.3811 0.049 Uiso 1 1 calc GR . . . .
H18B H 0.5761 0.8334 0.3406 0.049 Uiso 1 1 calc GR . . . .
H18C H 0.4890 0.7588 0.4649 0.049 Uiso 1 1 calc GR . . . .
C25 C 0.1238(5) 0.4138(4) 0.5546(4) 0.0281(13) Uani 1 1 d . . . . .
H25A H 0.0781 0.3561 0.5471 0.042 Uiso 1 1 calc GR . . . .
H25B H 0.0736 0.4453 0.6077 0.042 Uiso 1 1 calc GR . . . .
H25C H 0.1913 0.3760 0.5867 0.042 Uiso 1 1 calc GR . . . .
C16 C 0.4912(4) 0.6581(4) 0.3154(4) 0.0194(11) Uani 1 1 d . . . . .
C15 C 0.5822(5) 0.5998(5) 0.3667(4) 0.0297(13) Uani 1 1 d . . . . .
H15 H 0.6119 0.6269 0.4141 0.036 Uiso 1 1 calc R . . . .
C14 C 0.6311(5) 0.5004(5) 0.3489(5) 0.0346(14) Uani 1 1 d . . . . .
H14 H 0.6929 0.4610 0.3847 0.041 Uiso 1 1 calc R . . . .
C13 C 0.5882(5) 0.4601(5) 0.2787(4) 0.0304(13) Uani 1 1 d . . . . .
H13 H 0.6234 0.3954 0.2643 0.037 Uiso 1 1 calc R . . . .
C12 C 0.4908(4) 0.5164(4) 0.2281(4) 0.0232(12) Uani 1 1 d . . . . .
C17 C 0.4416(4) 0.6181(4) 0.2441(4) 0.0175(11) Uani 1 1 d . . . . .
C11 C 0.4471(5) 0.4652(4) 0.1596(4) 0.0245(12) Uani 1 1 d . . . . .
H11 H 0.4969 0.4133 0.1338 0.029 Uiso 1 1 calc R . . . .
C10 C 0.2513(5) 0.3256(5) 0.1238(5) 0.0366(15) Uani 1 1 d . . . . .
H10A H 0.2937 0.2640 0.1767 0.044 Uiso 1 1 calc R . . . .
H10B H 0.2349 0.2963 0.0681 0.044 Uiso 1 1 calc R . . . .
C9 C 0.1341(5) 0.3431(5) 0.1975(5) 0.0349(14) Uani 1 1 d . . . . .
H9A H 0.0881 0.2680 0.2379 0.042 Uiso 1 1 calc R . . . .
H9B H 0.1498 0.3644 0.2589 0.042 Uiso 1 1 calc R . . . .
C8 C -0.0324(5) 0.5960(5) 0.1374(4) 0.0233(12) Uani 1 1 d . . . . .
H8 H -0.0940 0.5574 0.1287 0.028 Uiso 1 1 calc R . . . .
C6 C -0.0583(4) 0.7113(4) 0.1412(4) 0.0207(11) Uani 1 1 d . . . . .
C5 C -0.1717(5) 0.7615(5) 0.1238(4) 0.0297(13) Uani 1 1 d . . . . .
H5 H -0.2264 0.7193 0.1104 0.036 Uiso 1 1 calc R . . . .
C4 C -0.2024(5) 0.8698(5) 0.1261(4) 0.0309(14) Uani 1 1 d . . . . .
H4 H -0.2775 0.8997 0.1151 0.037 Uiso 1 1 calc R . . . .
C3 C -0.1230(5) 0.9357(5) 0.1447(4) 0.0275(13) Uani 1 1 d . . . . .
H3 H -0.1432 1.0105 0.1441 0.033 Uiso 1 1 calc R . . . .
C2 C -0.0129(4) 0.8885(4) 0.1643(4) 0.0210(11) Uani 1 1 d . . . . .
C7 C 0.0206(4) 0.7762(4) 0.1644(4) 0.0190(11) Uani 1 1 d . . . . .
C1 C 0.0412(5) 1.0514(4) 0.2021(5) 0.0322(13) Uani 1 1 d . . . . .
H1A H 0.0264 1.1119 0.1288 0.048 Uiso 1 1 calc GR . . . .
H1B H 0.1052 1.0784 0.2230 0.048 Uiso 1 1 calc GR . . . .
H1C H -0.0306 1.0359 0.2653 0.048 Uiso 1 1 calc GR . . . .
C19 C 0.2130(5) 0.7200(5) -0.1092(4) 0.0286(13) Uani 1 1 d . . . . .
H19 H 0.1423 0.6740 -0.0821 0.034 Uiso 1 1 calc R . . . .
C20 C 0.2504(5) 0.7908(5) -0.2299(5) 0.0344(14) Uani 1 1 d . . . . .
H20 H 0.2044 0.7943 -0.2826 0.041 Uiso 1 1 calc R . . . .
C21 C 0.3564(6) 0.8563(5) -0.2716(5) 0.0388(15) Uani 1 1 d . . . . .
H21 H 0.3840 0.9042 -0.3531 0.047 Uiso 1 1 calc R . . . .
C22 C 0.4210(5) 0.8502(5) -0.1913(4) 0.0347(14) Uani 1 1 d . . . . .
H22 H 0.4934 0.8934 -0.2172 0.042 Uiso 1 1 calc R . . . .
C23 C 0.3768(5) 0.7791(4) -0.0719(4) 0.0302(13) Uani 1 1 d . . . . .
H23 H 0.4211 0.7760 -0.0180 0.036 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
Dy1 Ni1 3.3876(7) . ?
Dy1 O8 2.291(3) . ?
Dy1 O6 2.467(3) . ?
Dy1 O5 2.321(3) . ?
Dy1 O2 2.276(3) . ?
Dy1 O1 2.615(3) . ?
Dy1 O12 2.490(4) . ?
Dy1 O13 2.469(3) . ?
Dy1 O10 2.430(3) . ?
Dy1 O9 2.454(3) . ?
Dy1 N5 2.903(4) . ?
Dy1 N4 2.871(4) . ?
Ni1 O7 2.097(3) . ?
Ni1 O5 2.047(3) . ?
Ni1 O2 2.004(3) . ?
Ni1 N3 2.140(4) . ?
Ni1 N2 2.014(4) . ?
Ni1 N1 2.071(4) . ?
O8 C24 1.264(5) . ?
O6 C18 1.438(5) . ?
O6 C16 1.380(6) . ?
O7 C24 1.264(5) . ?
O5 C17 1.336(5) . ?
O4 N2 1.436(5) . ?
O4 C10 1.436(6) . ?
O3 N1 1.423(5) . ?
O3 C9 1.450(6) . ?
O2 C7 1.345(5) . ?
O1 C2 1.390(5) . ?
O1 C1 1.437(5) . ?
O12 N5 1.263(5) . ?
O13 N5 1.264(5) . ?
O14 N5 1.234(5) . ?
O10 N4 1.299(5) . ?
O9 N4 1.267(5) . ?
O11 N4 1.224(5) . ?
N3 C19 1.346(5) . ?
N3 C23 1.335(6) . ?
N2 C11 1.284(6) . ?
N1 C8 1.284(6) . ?
C24 C25 1.495(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C16 C15 1.362(6) . ?
C16 C17 1.426(6) . ?
C15 H15 0.9300 . ?
C15 C14 1.387(7) . ?
C14 H14 0.9300 . ?
C14 C13 1.372(7) . ?
C13 H13 0.9300 . ?
C13 C12 1.415(6) . ?
C12 C17 1.405(7) . ?
C12 C11 1.450(6) . ?
C11 H11 0.9300 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.490(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C8 H8 0.9300 . ?
C8 C6 1.447(7) . ?
C6 C5 1.423(7) . ?
C6 C7 1.405(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.364(7) . ?
C4 H4 0.9300 . ?
C4 C3 1.383(7) . ?
C3 H3 0.9300 . ?
C3 C2 1.384(7) . ?
C2 C7 1.406(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C19 H19 0.9300 . ?
C19 C20 1.373(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.372(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.368(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.371(6) . ?
C23 H23 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Dy1 Ni1 70.17(8) . . ?
O8 Dy1 O6 81.91(11) . . ?
O8 Dy1 O5 76.59(11) . . ?
O8 Dy1 O1 123.64(11) . . ?
O8 Dy1 O12 75.00(12) . . ?
O8 Dy1 O13 78.49(12) . . ?
O8 Dy1 O10 147.66(11) . . ?
O8 Dy1 O9 151.63(12) . . ?
O8 Dy1 N5 75.26(12) . . ?
O8 Dy1 N4 165.37(12) . . ?
O6 Dy1 Ni1 100.34(8) . . ?
O6 Dy1 O1 153.29(10) . . ?
O6 Dy1 O12 122.83(11) . . ?
O6 Dy1 O13 73.36(12) . . ?
O6 Dy1 N5 98.14(12) . . ?
O6 Dy1 N4 83.47(11) . . ?
O5 Dy1 Ni1 36.29(7) . . ?
O5 Dy1 O6 65.63(11) . . ?
O5 Dy1 O1 123.65(10) . . ?
O5 Dy1 O12 148.39(11) . . ?
O5 Dy1 O13 134.26(12) . . ?
O5 Dy1 O10 117.44(12) . . ?
O5 Dy1 O9 75.07(11) . . ?
O5 Dy1 N5 149.23(11) . . ?
O5 Dy1 N4 96.84(12) . . ?
O2 Dy1 Ni1 34.95(8) . . ?
O2 Dy1 O8 82.70(11) . . ?
O2 Dy1 O6 135.20(11) . . ?
O2 Dy1 O5 69.94(11) . . ?
O2 Dy1 O1 63.06(11) . . ?
O2 Dy1 O12 92.88(11) . . ?
O2 Dy1 O13 142.72(12) . . ?
O2 Dy1 O10 128.83(11) . . ?
O2 Dy1 O9 86.58(11) . . ?
O2 Dy1 N5 117.99(12) . . ?
O2 Dy1 N4 107.57(11) . . ?
O1 Dy1 Ni1 96.36(7) . . ?
O1 Dy1 N5 82.93(11) . . ?
O1 Dy1 N4 70.92(11) . . ?
O12 Dy1 Ni1 118.66(8) . . ?
O12 Dy1 O1 64.40(10) . . ?
O12 Dy1 N5 25.65(10) . . ?
O12 Dy1 N4 113.91(12) . . ?
O13 Dy1 Ni1 148.64(9) . . ?
O13 Dy1 O1 102.09(12) . . ?
O13 Dy1 O12 51.27(11) . . ?
O13 Dy1 N5 25.62(11) . . ?
O13 Dy1 N4 97.83(12) . . ?
O10 Dy1 Ni1 138.85(8) . . ?
O10 Dy1 O6 78.83(11) . . ?
O10 Dy1 O1 74.88(11) . . ?
O10 Dy1 O12 94.08(12) . . ?
O10 Dy1 O13 71.23(12) . . ?
O10 Dy1 O9 52.76(11) . . ?
O10 Dy1 N5 82.01(12) . . ?
O10 Dy1 N4 26.74(11) . . ?
O9 Dy1 Ni1 86.12(8) . . ?
O9 Dy1 O6 87.49(11) . . ?
O9 Dy1 O1 72.93(11) . . ?
O9 Dy1 O12 131.93(12) . . ?
O9 Dy1 O13 123.42(11) . . ?
O9 Dy1 N5 132.54(12) . . ?
O9 Dy1 N4 26.06(11) . . ?
N5 Dy1 Ni1 137.70(8) . . ?
N4 Dy1 Ni1 112.17(9) . . ?
N4 Dy1 N5 107.48(12) . . ?
O7 Ni1 Dy1 80.02(9) . . ?
O7 Ni1 N3 176.66(15) . . ?
O5 Ni1 Dy1 42.16(9) . . ?
O5 Ni1 O7 86.41(12) . . ?
O5 Ni1 N3 93.25(13) . . ?
O5 Ni1 N1 167.89(15) . . ?
O2 Ni1 Dy1 40.58(8) . . ?
O2 Ni1 O7 91.85(13) . . ?
O2 Ni1 O5 81.13(12) . . ?
O2 Ni1 N3 91.38(14) . . ?
O2 Ni1 N2 169.79(14) . . ?
O2 Ni1 N1 88.00(15) . . ?
N3 Ni1 Dy1 101.95(11) . . ?
N2 Ni1 Dy1 129.69(11) . . ?
N2 Ni1 O7 88.48(15) . . ?
N2 Ni1 O5 88.70(14) . . ?
N2 Ni1 N3 88.19(15) . . ?
N2 Ni1 N1 102.21(17) . . ?
N1 Ni1 Dy1 126.00(12) . . ?
N1 Ni1 O7 88.62(14) . . ?
N1 Ni1 N3 92.34(15) . . ?
C24 O8 Dy1 134.2(3) . . ?
C18 O6 Dy1 126.5(3) . . ?
C16 O6 Dy1 116.1(2) . . ?
C16 O6 C18 116.4(4) . . ?
C24 O7 Ni1 129.1(3) . . ?
Ni1 O5 Dy1 101.55(13) . . ?
C17 O5 Dy1 120.5(3) . . ?
C17 O5 Ni1 123.0(3) . . ?
N2 O4 C10 110.9(3) . . ?
N1 O3 C9 111.2(3) . . ?
Ni1 O2 Dy1 104.46(13) . . ?
C7 O2 Dy1 127.0(3) . . ?
C7 O2 Ni1 128.5(3) . . ?
C2 O1 Dy1 114.8(3) . . ?
C2 O1 C1 116.0(4) . . ?
C1 O1 Dy1 123.6(3) . . ?
N5 O12 Dy1 95.8(3) . . ?
N5 O13 Dy1 96.7(3) . . ?
N4 O10 Dy1 95.9(3) . . ?
N4 O9 Dy1 95.7(3) . . ?
C19 N3 Ni1 125.0(3) . . ?
C23 N3 Ni1 118.6(3) . . ?
C23 N3 C19 116.3(4) . . ?
O4 N2 Ni1 119.1(3) . . ?
C11 N2 Ni1 127.7(4) . . ?
C11 N2 O4 112.4(4) . . ?
O3 N1 Ni1 122.8(3) . . ?
C8 N1 Ni1 126.7(4) . . ?
C8 N1 O3 110.3(4) . . ?
O12 N5 Dy1 58.6(2) . . ?
O12 N5 O13 116.2(4) . . ?
O13 N5 Dy1 57.6(2) . . ?
O14 N5 Dy1 179.1(4) . . ?
O14 N5 O12 121.4(5) . . ?
O14 N5 O13 122.4(4) . . ?
O10 N4 Dy1 57.3(2) . . ?
O9 N4 Dy1 58.3(2) . . ?
O9 N4 O10 115.5(4) . . ?
O11 N4 Dy1 175.3(4) . . ?
O11 N4 O10 121.5(4) . . ?
O11 N4 O9 123.0(4) . . ?
O8 C24 O7 125.7(4) . . ?
O8 C24 C25 117.4(4) . . ?
O7 C24 C25 116.8(4) . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O6 C16 C17 113.3(4) . . ?
C15 C16 O6 125.3(4) . . ?
C15 C16 C17 121.4(5) . . ?
C16 C15 H15 119.6 . . ?
C16 C15 C14 120.7(5) . . ?
C14 C15 H15 119.6 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 C15 120.1(5) . . ?
C13 C14 H14 120.0 . . ?
C14 C13 H13 119.8 . . ?
C14 C13 C12 120.3(5) . . ?
C12 C13 H13 119.8 . . ?
C13 C12 C11 117.0(5) . . ?
C17 C12 C13 120.1(4) . . ?
C17 C12 C11 122.9(4) . . ?
O5 C17 C16 117.8(4) . . ?
O5 C17 C12 124.8(4) . . ?
C12 C17 C16 117.3(4) . . ?
N2 C11 C12 124.7(5) . . ?
N2 C11 H11 117.6 . . ?
C12 C11 H11 117.6 . . ?
O4 C10 H10A 108.4 . . ?
O4 C10 H10B 108.4 . . ?
O4 C10 C9 115.6(5) . . ?
H10A C10 H10B 107.5 . . ?
C9 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
O3 C9 C10 113.9(4) . . ?
O3 C9 H9A 108.8 . . ?
O3 C9 H9B 108.8 . . ?
C10 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
N1 C8 H8 116.8 . . ?
N1 C8 C6 126.4(4) . . ?
C6 C8 H8 116.8 . . ?
C5 C6 C8 118.6(4) . . ?
C7 C6 C8 123.9(4) . . ?
C7 C6 C5 117.4(5) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 C6 121.9(5) . . ?
C4 C5 H5 119.0 . . ?
C5 C4 H4 119.7 . . ?
C5 C4 C3 120.7(5) . . ?
C3 C4 H4 119.7 . . ?
C4 C3 H3 120.5 . . ?
C4 C3 C2 118.9(5) . . ?
C2 C3 H3 120.5 . . ?
O1 C2 C7 113.0(4) . . ?
C3 C2 O1 125.3(5) . . ?
C3 C2 C7 121.7(4) . . ?
O2 C7 C6 123.1(5) . . ?
O2 C7 C2 117.6(4) . . ?
C6 C7 C2 119.3(4) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N3 C19 H19 118.5 . . ?
N3 C19 C20 123.0(5) . . ?
C20 C19 H19 118.5 . . ?
C19 C20 H20 120.5 . . ?
C21 C20 C19 119.1(5) . . ?
C21 C20 H20 120.5 . . ?
C20 C21 H21 120.6 . . ?
C22 C21 C20 118.9(5) . . ?
C22 C21 H21 120.6 . . ?
C21 C22 H22 120.7 . . ?
C21 C22 C23 118.6(5) . . ?
C23 C22 H22 120.7 . . ?
N3 C23 C22 124.0(5) . . ?
N3 C23 H23 118.0 . . ?
C22 C23 H23 118.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O8 C24 O7 12.1(8) . . . . ?
Dy1 O8 C24 C25 -169.8(3) . . . . ?
Dy1 O6 C16 C15 -160.6(4) . . . . ?
Dy1 O6 C16 C17 18.9(5) . . . . ?
Dy1 O5 C17 C16 -20.8(5) . . . . ?
Dy1 O5 C17 C12 159.0(4) . . . . ?
Dy1 O2 C7 C6 -161.5(3) . . . . ?
Dy1 O2 C7 C2 15.8(6) . . . . ?
Dy1 O1 C2 C3 162.3(4) . . . . ?
Dy1 O1 C2 C7 -17.7(5) . . . . ?
Dy1 O12 N5 O13 0.0(4) . . . . ?
Dy1 O12 N5 O14 179.0(4) . . . . ?
Dy1 O13 N5 O12 0.0(4) . . . . ?
Dy1 O13 N5 O14 -179.0(4) . . . . ?
Dy1 O10 N4 O9 -4.0(4) . . . . ?
Dy1 O10 N4 O11 174.7(4) . . . . ?
Dy1 O9 N4 O10 3.9(4) . . . . ?
Dy1 O9 N4 O11 -174.7(4) . . . . ?
Ni1 O7 C24 O8 -8.7(7) . . . . ?
Ni1 O7 C24 C25 173.2(3) . . . . ?
Ni1 O5 C17 C16 -152.1(3) . . . . ?
Ni1 O5 C17 C12 27.6(6) . . . . ?
Ni1 O2 C7 C6 20.2(6) . . . . ?
Ni1 O2 C7 C2 -162.5(3) . . . . ?
Ni1 N3 C19 C20 -178.9(4) . . . . ?
Ni1 N3 C23 C22 177.9(4) . . . . ?
Ni1 N2 C11 C12 5.9(7) . . . . ?
Ni1 N1 C8 C6 -1.7(7) . . . . ?
O6 C16 C15 C14 -179.3(4) . . . . ?
O6 C16 C17 O5 -0.2(6) . . . . ?
O6 C16 C17 C12 -179.9(4) . . . . ?
O4 N2 C11 C12 175.7(4) . . . . ?
O4 C10 C9 O3 57.5(6) . . . . ?
O3 N1 C8 C6 -175.7(4) . . . . ?
O1 C2 C7 O2 4.0(6) . . . . ?
O1 C2 C7 C6 -178.5(4) . . . . ?
N3 C19 C20 C21 1.9(8) . . . . ?
N2 O4 C10 C9 50.8(6) . . . . ?
N1 O3 C9 C10 -103.6(5) . . . . ?
N1 C8 C6 C5 176.0(5) . . . . ?
N1 C8 C6 C7 -5.8(8) . . . . ?
C18 O6 C16 C15 8.8(7) . . . . ?
C18 O6 C16 C17 -171.7(4) . . . . ?
C16 C15 C14 C13 0.3(8) . . . . ?
C15 C16 C17 O5 179.3(4) . . . . ?
C15 C16 C17 C12 -0.4(7) . . . . ?
C15 C14 C13 C12 -2.6(8) . . . . ?
C14 C13 C12 C17 3.5(7) . . . . ?
C14 C13 C12 C11 -177.2(5) . . . . ?
C13 C12 C17 O5 178.4(4) . . . . ?
C13 C12 C17 C16 -1.9(7) . . . . ?
C13 C12 C11 N2 162.9(5) . . . . ?
C17 C16 C15 C14 1.2(8) . . . . ?
C17 C12 C11 N2 -17.7(8) . . . . ?
C11 C12 C17 O5 -0.9(7) . . . . ?
C11 C12 C17 C16 178.8(4) . . . . ?
C10 O4 N2 Ni1 -85.6(4) . . . . ?
C10 O4 N2 C11 103.7(5) . . . . ?
C9 O3 N1 Ni1 37.4(5) . . . . ?
C9 O3 N1 C8 -148.4(4) . . . . ?
C8 C6 C5 C4 -180.0(4) . . . . ?
C8 C6 C7 O2 -3.6(7) . . . . ?
C8 C6 C7 C2 179.1(4) . . . . ?
C6 C5 C4 C3 0.6(8) . . . . ?
C5 C6 C7 O2 174.6(4) . . . . ?
C5 C6 C7 C2 -2.6(6) . . . . ?
C5 C4 C3 C2 -1.8(7) . . . . ?
C4 C3 C2 O1 -179.2(4) . . . . ?
C4 C3 C2 C7 0.7(7) . . . . ?
C3 C2 C7 O2 -175.9(4) . . . . ?
C3 C2 C7 C6 1.5(7) . . . . ?
C7 C6 C5 C4 1.7(7) . . . . ?
C1 O1 C2 C3 7.6(6) . . . . ?
C1 O1 C2 C7 -172.3(4) . . . . ?
C19 N3 C23 C22 0.6(8) . . . . ?
C19 C20 C21 C22 -0.8(9) . . . . ?
C20 C21 C22 C23 -0.3(9) . . . . ?
C21 C22 C23 N3 0.5(9) . . . . ?
C23 N3 C19 C20 -1.8(8) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.285 0.149 0.464 80.5 8.3 ?
2 0.715 0.851 0.536 80.5 6.9 ?

_olex2_date_sample_data_collection 2015-06-02
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_20141219lzd573_0m
_database_code_depnum_ccdc_archive 'CCDC 1434584'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H30 La N7 Ni O16'
_chemical_formula_sum            'C29 H30 La N7 Ni O16'
_chemical_formula_weight         930.22

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)   '
_symmetry_space_group_name_Hall  'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   11.392(3)
_cell_length_b                   15.729(4)
_cell_length_c                   11.421(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.830(3)
_cell_angle_gamma                90.00
_cell_volume                     1842.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8283
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.60

_exptl_crystal_description       block-like
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             932
_exptl_absorpt_coefficient_mu    1.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6809
_exptl_absorpt_correction_T_max  0.7340
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12288
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5371
_reflns_number_gt                5103
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1420P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(3)
_refine_ls_number_reflns         5371
_refine_ls_number_parameters     491
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.1870
_refine_ls_wR_factor_gt          0.1800
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2677(11) 0.6033(7) 0.2681(10) 0.031(2) Uani 1 1 d . . .
C2 C 0.1671(10) 0.5450(7) 0.1863(10) 0.032(2) Uani 1 1 d . . .
C3 C 0.1998(13) 0.4702(8) 0.1475(13) 0.046(3) Uani 1 1 d . . .
H3 H 0.1349 0.4325 0.0962 0.055 Uiso 1 1 calc R . .
C4 C 0.3335(13) 0.4499(8) 0.1856(14) 0.050(3) Uani 1 1 d . . .
H4 H 0.3555 0.3994 0.1578 0.060 Uiso 1 1 calc R . .
C5 C 0.4266(12) 0.5029(7) 0.2607(13) 0.042(3) Uani 1 1 d . . .
H5 H 0.5134 0.4888 0.2851 0.050 Uiso 1 1 calc R . .
C6 C 0.3961(10) 0.5817(7) 0.3052(10) 0.029(2) Uani 1 1 d . . .
C7 C 0.5023(11) 0.6303(8) 0.3928(10) 0.039(3) Uani 1 1 d . . .
H7 H 0.5828 0.6032 0.4321 0.047 Uiso 1 1 calc R . .
C8 C 0.6370(18) 0.8157(11) 0.5604(16) 0.072(4) Uani 1 1 d DU . .
H8A H 0.7144 0.8170 0.6429 0.087 Uiso 1 1 calc R . .
H8B H 0.5639 0.8242 0.5813 0.087 Uiso 1 1 calc R . .
C9 C 0.6437(17) 0.8938(10) 0.4931(16) 0.077(5) Uani 1 1 d D . .
H9A H 0.7228 0.8918 0.4810 0.093 Uiso 1 1 calc R . .
H9B H 0.6516 0.9416 0.5498 0.093 Uiso 1 1 calc R . .
C10 C 0.3494(12) 0.9717(7) 0.3256(11) 0.043(3) Uani 1 1 d . . .
H10 H 0.3966 1.0194 0.3234 0.051 Uiso 1 1 calc R . .
C11 C 0.2112(12) 0.9837(7) 0.2842(11) 0.039(2) Uani 1 1 d . . .
C12 C 0.1658(17) 1.0702(9) 0.2658(13) 0.058(4) Uani 1 1 d . . .
H12 H 0.2269 1.1133 0.2819 0.070 Uiso 1 1 calc R . .
C13 C 0.0499(17) 1.0911(9) 0.2296(16) 0.062(4) Uani 1 1 d . . .
H13 H 0.0265 1.1482 0.2215 0.075 Uiso 1 1 calc R . .
C14 C -0.0121(11) 0.9405(8) 0.2164(10) 0.037(3) Uani 1 1 d . . .
C15 C 0.1212(11) 0.9167(7) 0.2629(9) 0.032(2) Uani 1 1 d . . .
C16 C -0.0559(13) 0.5115(10) 0.0792(15) 0.057(3) Uani 1 1 d . . .
H16A H -0.0645 0.5110 -0.0082 0.086 Uiso 1 1 calc R . .
H16B H -0.1373 0.5282 0.0786 0.086 Uiso 1 1 calc R . .
H16C H -0.0328 0.4557 0.1162 0.086 Uiso 1 1 calc R . .
C17 C -0.2251(14) 0.8903(12) 0.1798(16) 0.063(4) Uani 1 1 d . . .
H17A H -0.2213 0.9386 0.2326 0.095 Uiso 1 1 calc R . .
H17B H -0.2578 0.8421 0.2078 0.095 Uiso 1 1 calc R . .
H17C H -0.2819 0.9026 0.0905 0.095 Uiso 1 1 calc R . .
C18 C 0.2940(10) 0.8535(7) 0.5813(9) 0.030(2) Uani 1 1 d . . .
H18 H 0.2649 0.9011 0.5280 0.036 Uiso 1 1 calc R . .
C19 C 0.2912(10) 0.8546(7) 0.7003(10) 0.031(2) Uani 1 1 d . . .
H19 H 0.2569 0.9014 0.7244 0.037 Uiso 1 1 calc R . .
C20 C 0.3384(8) 0.7876(7) 0.7835(9) 0.029(2) Uani 1 1 d . . .
C21 C 0.3846(11) 0.7167(10) 0.7407(9) 0.042(2) Uani 1 1 d . . .
H21 H 0.4171 0.6687 0.7925 0.051 Uiso 1 1 calc R . .
C22 C 0.3791(10) 0.7223(9) 0.6178(9) 0.041(2) Uani 1 1 d . . .
H22 H 0.4086 0.6753 0.5889 0.049 Uiso 1 1 calc R . .
C23 C 0.4460(11) 0.7613(8) 1.1447(11) 0.041(3) Uani 1 1 d . . .
H23 H 0.5214 0.7468 1.2181 0.049 Uiso 1 1 calc R . .
C24 C 0.4487(10) 0.7616(8) 1.0242(10) 0.036(2) Uani 1 1 d . . .
H24 H 0.5245 0.7465 1.0177 0.043 Uiso 1 1 calc R . .
C25 C 0.3386(9) 0.7844(8) 0.9141(9) 0.030(2) Uani 1 1 d . . .
C26 C 0.2267(10) 0.8046(8) 0.9283(10) 0.037(2) Uani 1 1 d . . .
H26 H 0.1498 0.8199 0.8572 0.044 Uiso 1 1 calc R . .
C27 C 0.2344(9) 0.8011(8) 1.0533(10) 0.033(2) Uani 1 1 d . . .
H27 H 0.1589 0.8139 1.0620 0.040 Uiso 1 1 calc R . .
C28 C 0.124(3) 0.5523(12) 0.515(2) 0.096(7) Uani 1 1 d . . .
H28A H 0.0619 0.5314 0.5446 0.143 Uiso 1 1 calc R . .
H28B H 0.2102 0.5481 0.5849 0.143 Uiso 1 1 calc R . .
H28C H 0.1185 0.5191 0.4428 0.143 Uiso 1 1 calc R . .
C42 C -0.0520(14) 1.0232(9) 0.1992(13) 0.051(3) Uani 1 1 d . . .
H42 H -0.1396 1.0371 0.1696 0.061 Uiso 1 1 calc R . .
La1 La 0.00282(4) 0.71634(5) 0.26468(4) 0.0301(2) Uani 1 1 d . . .
N1 N 0.4983(6) 0.7088(7) 0.4237(6) 0.0277(16) Uani 1 1 d . . .
N2 N 0.4132(8) 0.9029(6) 0.3647(8) 0.034(2) Uani 1 1 d . . .
N3 N 0.3375(8) 0.7856(6) 0.5390(8) 0.0294(17) Uani 1 1 d . . .
N4 N 0.3372(8) 0.7816(6) 1.1590(8) 0.0309(17) Uani 1 1 d . . .
N5 N -0.0021(10) 0.8052(7) 0.5548(11) 0.049(3) Uani 1 1 d . . .
N6 N -0.1653(10) 0.7336(7) -0.0309(9) 0.048(3) Uani 1 1 d . . .
N7 N -0.2246(15) 0.6253(12) 0.2784(16) 0.080(5) Uani 1 1 d . . .
Ni1 Ni 0.33413(11) 0.78365(7) 0.34829(10) 0.0246(3) Uani 1 1 d . . .
O1 O 0.6267(10) 0.7338(8) 0.5197(11) 0.095(5) Uani 1 1 d . . .
O2 O 0.5384(10) 0.9098(8) 0.3716(12) 0.070(3) Uani 1 1 d . . .
O3 O 0.2278(7) 0.6749(5) 0.3014(7) 0.0292(15) Uani 1 1 d . . .
O4 O 0.1507(7) 0.8366(5) 0.2759(6) 0.0271(14) Uani 1 1 d . . .
O5 O -0.0966(7) 0.8718(6) 0.1924(8) 0.0411(18) Uani 1 1 d . . .
O6 O 0.0435(8) 0.5706(5) 0.1554(8) 0.0416(18) Uani 1 1 d . . .
O7 O -0.0451(9) 0.7485(7) 0.0195(9) 0.057(2) Uani 1 1 d . . .
O8 O -0.2094(9) 0.7060(8) 0.0497(9) 0.063(3) Uani 1 1 d . . .
O9 O -0.2379(11) 0.7447(7) -0.1447(9) 0.074(3) Uani 1 1 d . . .
O10 O -0.2131(10) 0.7016(7) 0.2958(11) 0.065(3) Uani 1 1 d . . .
O11 O -0.1448(11) 0.5836(7) 0.2588(12) 0.067(3) Uani 1 1 d . . .
O12 O -0.3394(18) 0.5965(14) 0.259(2) 0.119(6) Uani 1 1 d U . .
O13 O 0.0031(9) 0.8130(6) 0.4486(9) 0.050(2) Uani 1 1 d . . .
O14 O -0.0379(13) 0.8672(9) 0.6010(13) 0.081(3) Uani 1 1 d . . .
O15 O 0.0229(11) 0.7393(7) 0.6167(10) 0.065(3) Uani 1 1 d . . .
O16 O 0.0954(10) 0.6396(6) 0.4766(9) 0.057(2) Uani 1 1 d . . .
H16D H 0.0455 0.6543 0.5108 0.069 Uiso 1 1 d 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
C1 O3 1.330(13) . ?
C1 C6 1.377(15) . ?
C1 C2 1.447(15) . ?
C2 O6 1.354(13) . ?
C2 C3 1.366(16) . ?
C3 C4 1.426(19) . ?
C3 H3 0.9300 . ?
C4 C5 1.328(19) . ?
C4 H4 0.9300 . ?
C5 C6 1.437(15) . ?
C5 H5 0.9300 . ?
C6 C7 1.413(17) . ?
C7 N1 1.290(17) . ?
C7 H7 0.9300 . ?
C8 O1 1.36(2) . ?
C8 C9 1.468(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O2 1.406(19) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.272(16) . ?
C10 C11 1.445(17) . ?
C10 H10 0.9300 . ?
C11 C15 1.416(16) . ?
C11 C12 1.439(19) . ?
C12 C13 1.24(2) . ?
C12 H12 0.9300 . ?
C13 C42 1.50(2) . ?
C13 H13 0.9300 . ?
C14 C42 1.362(19) . ?
C14 O5 1.393(16) . ?
C14 C15 1.423(15) . ?
C15 O4 1.295(13) . ?
C16 O6 1.430(15) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O5 1.436(15) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N3 1.352(14) . ?
C18 C19 1.374(14) . ?
C18 H18 0.9300 . ?
C19 C20 1.362(15) . ?
C19 H19 0.9300 . ?
C20 C21 1.409(18) . ?
C20 C25 1.491(12) . ?
C21 C22 1.381(12) . ?
C21 H21 0.9300 . ?
C22 N3 1.286(15) . ?
C22 H22 0.9300 . ?
C23 N4 1.356(13) . ?
C23 C24 1.390(14) . ?
C23 H23 0.9300 . ?
C24 C25 1.381(15) . ?
C24 H24 0.9300 . ?
C25 C26 1.391(14) . ?
C26 C27 1.393(14) . ?
C26 H26 0.9300 . ?
C27 N4 1.300(14) . ?
C27 H27 0.9300 . ?
C28 O16 1.43(2) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C42 H42 0.9300 . ?
La1 O16 2.491(9) . ?
La1 O3 2.497(7) . ?
La1 O4 2.499(7) . ?
La1 O8 2.594(9) . ?
La1 O13 2.592(9) . ?
La1 O10 2.645(9) . ?
La1 O7 2.658(9) . ?
La1 O11 2.663(11) . ?
La1 O5 2.670(8) . ?
La1 O6 2.744(8) . ?
La1 N7 3.024(13) . ?
N1 O1 1.448(11) . ?
N1 Ni1 2.055(8) . ?
N2 O2 1.398(13) . ?
N2 Ni1 2.054(9) . ?
N3 Ni1 2.162(8) . ?
N4 Ni1 2.178(8) 1_556 ?
N5 O15 1.217(15) . ?
N5 O14 1.258(16) . ?
N5 O13 1.246(14) . ?
N6 O9 1.212(14) . ?
N6 O7 1.254(13) . ?
N6 O8 1.300(14) . ?
N7 O10 1.21(2) . ?
N7 O11 1.22(2) . ?
N7 O12 1.31(2) . ?
Ni1 O3 2.029(7) . ?
Ni1 O4 2.059(7) . ?
Ni1 N4 2.178(8) 1_554 ?
O16 H16D 0.8504 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 C1 C6 124.8(10) . . ?
O3 C1 C2 116.6(10) . . ?
C6 C1 C2 118.6(10) . . ?
O6 C2 C3 124.8(10) . . ?
O6 C2 C1 114.9(9) . . ?
C3 C2 C1 120.2(10) . . ?
C2 C3 C4 120.0(11) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.2(11) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.4(11) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C7 123.4(9) . . ?
C1 C6 C5 119.5(10) . . ?
C7 C6 C5 116.9(10) . . ?
N1 C7 C6 126.2(10) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
O1 C8 C9 129.1(17) . . ?
O1 C8 H8A 105.0 . . ?
C9 C8 H8A 105.0 . . ?
O1 C8 H8B 105.0 . . ?
C9 C8 H8B 105.0 . . ?
H8A C8 H8B 105.9 . . ?
C8 C9 O2 116.8(14) . . ?
C8 C9 H9A 108.1 . . ?
O2 C9 H9A 108.1 . . ?
C8 C9 H9B 108.1 . . ?
O2 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
N2 C10 C11 126.9(10) . . ?
N2 C10 H10 116.5 . . ?
C11 C10 H10 116.5 . . ?
C15 C11 C12 119.5(12) . . ?
C15 C11 C10 124.3(11) . . ?
C12 C11 C10 116.3(11) . . ?
C13 C12 C11 124.1(14) . . ?
C13 C12 H12 118.0 . . ?
C11 C12 H12 118.0 . . ?
C12 C13 C42 119.4(13) . . ?
C12 C13 H13 120.3 . . ?
C42 C13 H13 120.3 . . ?
C42 C14 O5 123.6(11) . . ?
C42 C14 C15 122.7(12) . . ?
O5 C14 C15 113.7(10) . . ?
O4 C15 C11 124.9(10) . . ?
O4 C15 C14 118.7(10) . . ?
C11 C15 C14 116.3(10) . . ?
O6 C16 H16A 109.5 . . ?
O6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 122.3(9) . . ?
N3 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C20 C19 C18 120.6(10) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C19 C20 C21 117.6(9) . . ?
C19 C20 C25 123.5(10) . . ?
C21 C20 C25 118.8(9) . . ?
C22 C21 C20 116.3(12) . . ?
C22 C21 H21 121.8 . . ?
C20 C21 H21 121.8 . . ?
N3 C22 C21 126.9(12) . . ?
N3 C22 H22 116.5 . . ?
C21 C22 H22 116.5 . . ?
N4 C23 C24 122.2(10) . . ?
N4 C23 H23 118.9 . . ?
C24 C23 H23 118.9 . . ?
C23 C24 C25 120.0(9) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C26 C25 C24 117.9(8) . . ?
C26 C25 C20 120.4(9) . . ?
C24 C25 C20 121.7(9) . . ?
C25 C26 C27 117.3(9) . . ?
C25 C26 H26 121.3 . . ?
C27 C26 H26 121.3 . . ?
N4 C27 C26 126.1(9) . . ?
N4 C27 H27 116.9 . . ?
C26 C27 H27 116.9 . . ?
O16 C28 H28A 109.5 . . ?
O16 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O16 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C14 C42 C13 117.9(12) . . ?
C14 C42 H42 121.0 . . ?
C13 C42 H42 121.0 . . ?
O16 La1 O3 75.0(3) . . ?
O16 La1 O4 109.1(3) . . ?
O3 La1 O4 64.5(2) . . ?
O16 La1 O8 135.6(4) . . ?
O3 La1 O8 127.4(3) . . ?
O4 La1 O8 115.2(3) . . ?
O16 La1 O13 69.3(3) . . ?
O3 La1 O13 112.3(3) . . ?
O4 La1 O13 75.6(3) . . ?
O8 La1 O13 118.4(3) . . ?
O16 La1 O10 81.5(4) . . ?
O3 La1 O10 154.4(3) . . ?
O4 La1 O10 134.9(3) . . ?
O8 La1 O10 65.4(3) . . ?
O13 La1 O10 67.4(3) . . ?
O16 La1 O7 157.2(3) . . ?
O3 La1 O7 87.2(3) . . ?
O4 La1 O7 74.6(3) . . ?
O8 La1 O7 48.4(3) . . ?
O13 La1 O7 132.0(3) . . ?
O10 La1 O7 112.5(3) . . ?
O16 La1 O11 68.9(4) . . ?
O3 La1 O11 113.0(3) . . ?
O4 La1 O11 177.3(3) . . ?
O8 La1 O11 67.0(4) . . ?
O13 La1 O11 105.0(3) . . ?
O10 La1 O11 47.2(3) . . ?
O7 La1 O11 106.6(3) . . ?
O16 La1 O5 133.4(3) . . ?
O3 La1 O5 123.9(2) . . ?
O4 La1 O5 60.6(2) . . ?
O8 La1 O5 70.7(3) . . ?
O13 La1 O5 64.1(3) . . ?
O10 La1 O5 80.1(3) . . ?
O7 La1 O5 68.6(3) . . ?
O11 La1 O5 122.1(3) . . ?
O16 La1 O6 87.3(3) . . ?
O3 La1 O6 59.6(2) . . ?
O4 La1 O6 114.3(2) . . ?
O8 La1 O6 77.8(3) . . ?
O13 La1 O6 156.6(3) . . ?
O10 La1 O6 109.8(3) . . ?
O7 La1 O6 71.2(3) . . ?
O11 La1 O6 64.1(3) . . ?
O5 La1 O6 139.2(3) . . ?
O16 La1 N7 74.3(4) . . ?
O3 La1 N7 135.0(4) . . ?
O4 La1 N7 158.4(4) . . ?
O8 La1 N7 63.4(4) . . ?
O13 La1 N7 86.2(4) . . ?
O10 La1 N7 23.5(4) . . ?
O7 La1 N7 110.9(4) . . ?
O11 La1 N7 23.7(4) . . ?
O5 La1 N7 101.1(4) . . ?
O6 La1 N7 86.9(4) . . ?
C7 N1 O1 108.8(8) . . ?
C7 N1 Ni1 124.6(7) . . ?
O1 N1 Ni1 126.6(8) . . ?
C10 N2 O2 111.5(9) . . ?
C10 N2 Ni1 125.7(7) . . ?
O2 N2 Ni1 118.2(7) . . ?
C22 N3 C18 116.2(8) . . ?
C22 N3 Ni1 122.3(7) . . ?
C18 N3 Ni1 121.5(7) . . ?
C27 N4 C23 116.4(9) . . ?
C27 N4 Ni1 121.4(6) . 1_556 ?
C23 N4 Ni1 122.2(7) . 1_556 ?
O15 N5 O14 117.0(13) . . ?
O15 N5 O13 123.4(12) . . ?
O14 N5 O13 119.6(12) . . ?
O9 N6 O7 124.3(12) . . ?
O9 N6 O8 120.9(11) . . ?
O7 N6 O8 114.8(10) . . ?
O10 N7 O11 121.7(13) . . ?
O10 N7 O12 113.4(18) . . ?
O11 N7 O12 123.7(17) . . ?
O10 N7 La1 60.4(7) . . ?
O11 N7 La1 61.3(7) . . ?
O12 N7 La1 166.2(16) . . ?
O3 Ni1 O4 81.4(3) . . ?
O3 Ni1 N2 169.1(3) . . ?
O4 Ni1 N2 89.7(3) . . ?
O3 Ni1 N1 87.5(3) . . ?
O4 Ni1 N1 168.3(4) . . ?
N2 Ni1 N1 101.7(4) . . ?
O3 Ni1 N3 91.4(3) . . ?
O4 Ni1 N3 88.2(3) . . ?
N2 Ni1 N3 94.6(3) . . ?
N1 Ni1 N3 88.4(3) . . ?
O3 Ni1 N4 89.5(3) . 1_554 ?
O4 Ni1 N4 93.4(3) . 1_554 ?
N2 Ni1 N4 84.7(3) . 1_554 ?
N1 Ni1 N4 90.1(3) . 1_554 ?
N3 Ni1 N4 178.2(3) . 1_554 ?
C8 O1 N1 115.2(11) . . ?
N2 O2 C9 116.8(11) . . ?
C1 O3 Ni1 123.4(6) . . ?
C1 O3 La1 128.8(6) . . ?
Ni1 O3 La1 106.0(3) . . ?
C15 O4 Ni1 127.4(7) . . ?
C15 O4 La1 126.5(7) . . ?
Ni1 O4 La1 105.0(3) . . ?
C14 O5 C17 116.7(11) . . ?
C14 O5 La1 119.1(6) . . ?
C17 O5 La1 119.5(9) . . ?
C2 O6 C16 115.1(9) . . ?
C2 O6 La1 119.4(6) . . ?
C16 O6 La1 125.0(7) . . ?
N6 O7 La1 97.4(7) . . ?
N6 O8 La1 99.2(6) . . ?
N7 O10 La1 96.0(9) . . ?
N7 O11 La1 95.0(9) . . ?
N5 O13 La1 138.4(8) . . ?
C28 O16 La1 135.0(10) . . ?
C28 O16 H16D 103.0 . . ?
La1 O16 H16D 103.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C1 C2 O6 -1.0(13) . . . . ?
C6 C1 C2 O6 179.3(9) . . . . ?
O3 C1 C2 C3 179.8(10) . . . . ?
C6 C1 C2 C3 0.1(15) . . . . ?
O6 C2 C3 C4 179.8(11) . . . . ?
C1 C2 C3 C4 -1.1(18) . . . . ?
C2 C3 C4 C5 1(2) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
O3 C1 C6 C7 5.5(16) . . . . ?
C2 C1 C6 C7 -174.8(10) . . . . ?
O3 C1 C6 C5 -178.9(10) . . . . ?
C2 C1 C6 C5 0.8(15) . . . . ?
C4 C5 C6 C1 -0.7(18) . . . . ?
C4 C5 C6 C7 175.2(12) . . . . ?
C1 C6 C7 N1 -18.8(17) . . . . ?
C5 C6 C7 N1 165.4(11) . . . . ?
O1 C8 C9 O2 58(3) . . . . ?
N2 C10 C11 C15 -9.7(18) . . . . ?
N2 C10 C11 C12 169.6(12) . . . . ?
C15 C11 C12 C13 -1(2) . . . . ?
C10 C11 C12 C13 179.5(14) . . . . ?
C11 C12 C13 C42 -2(2) . . . . ?
C12 C11 C15 O4 179.7(10) . . . . ?
C10 C11 C15 O4 -1.0(16) . . . . ?
C12 C11 C15 C14 3.6(15) . . . . ?
C10 C11 C15 C14 -177.1(10) . . . . ?
C42 C14 C15 O4 -179.7(10) . . . . ?
O5 C14 C15 O4 1.3(13) . . . . ?
C42 C14 C15 C11 -3.4(15) . . . . ?
O5 C14 C15 C11 177.6(9) . . . . ?
N3 C18 C19 C20 2.9(15) . . . . ?
C18 C19 C20 C21 -2.5(15) . . . . ?
C18 C19 C20 C25 179.9(9) . . . . ?
C19 C20 C21 C22 0.7(16) . . . . ?
C25 C20 C21 C22 178.4(10) . . . . ?
C20 C21 C22 N3 0.8(19) . . . . ?
N4 C23 C24 C25 1.1(19) . . . . ?
C23 C24 C25 C26 -1.5(18) . . . . ?
C23 C24 C25 C20 178.5(11) . . . . ?
C19 C20 C25 C26 48.3(16) . . . . ?
C21 C20 C25 C26 -129.2(12) . . . . ?
C19 C20 C25 C24 -131.6(12) . . . . ?
C21 C20 C25 C24 50.8(15) . . . . ?
C24 C25 C26 C27 0.5(17) . . . . ?
C20 C25 C26 C27 -179.4(11) . . . . ?
C25 C26 C27 N4 0.9(19) . . . . ?
O5 C14 C42 C13 179.7(11) . . . . ?
C15 C14 C42 C13 0.7(18) . . . . ?
C12 C13 C42 C14 2(2) . . . . ?
C6 C7 N1 O1 178.0(11) . . . . ?
C6 C7 N1 Ni1 -1.3(15) . . . . ?
C11 C10 N2 O2 167.8(12) . . . . ?
C11 C10 N2 Ni1 12.4(16) . . . . ?
C21 C22 N3 C18 -0.4(18) . . . . ?
C21 C22 N3 Ni1 -179.5(10) . . . . ?
C19 C18 N3 C22 -1.4(15) . . . . ?
C19 C18 N3 Ni1 177.7(7) . . . . ?
C26 C27 N4 C23 -1.3(18) . . . . ?
C26 C27 N4 Ni1 177.7(10) . . . 1_556 ?
C24 C23 N4 C27 0.3(17) . . . . ?
C24 C23 N4 Ni1 -178.7(9) . . . 1_556 ?
O16 La1 N7 O10 105.0(11) . . . . ?
O3 La1 N7 O10 153.6(9) . . . . ?
O4 La1 N7 O10 2.8(18) . . . . ?
O8 La1 N7 O10 -89.0(11) . . . . ?
O13 La1 N7 O10 35.5(10) . . . . ?
O7 La1 N7 O10 -98.4(10) . . . . ?
O11 La1 N7 O10 178.1(18) . . . . ?
O5 La1 N7 O10 -27.3(11) . . . . ?
O6 La1 N7 O10 -166.9(11) . . . . ?
O16 La1 N7 O11 -73.1(10) . . . . ?
O3 La1 N7 O11 -24.5(12) . . . . ?
O4 La1 N7 O11 -175.3(8) . . . . ?
O8 La1 N7 O11 92.9(10) . . . . ?
O13 La1 N7 O11 -142.6(10) . . . . ?
O10 La1 N7 O11 -178.1(18) . . . . ?
O7 La1 N7 O11 83.5(11) . . . . ?
O5 La1 N7 O11 154.7(10) . . . . ?
O6 La1 N7 O11 15.0(10) . . . . ?
O16 La1 N7 O12 172(6) . . . . ?
O3 La1 N7 O12 -140(6) . . . . ?
O4 La1 N7 O12 70(6) . . . . ?
O8 La1 N7 O12 -22(6) . . . . ?
O13 La1 N7 O12 102(6) . . . . ?
O10 La1 N7 O12 67(6) . . . . ?
O7 La1 N7 O12 -32(6) . . . . ?
O11 La1 N7 O12 -115(6) . . . . ?
O5 La1 N7 O12 40(6) . . . . ?
O6 La1 N7 O12 -100(6) . . . . ?
C10 N2 Ni1 O3 30(2) . . . . ?
O2 N2 Ni1 O3 -124.2(16) . . . . ?
C10 N2 Ni1 O4 -5.5(9) . . . . ?
O2 N2 Ni1 O4 -159.5(8) . . . . ?
C10 N2 Ni1 N1 177.0(9) . . . . ?
O2 N2 Ni1 N1 23.0(8) . . . . ?
C10 N2 Ni1 N3 -93.6(9) . . . . ?
O2 N2 Ni1 N3 112.4(8) . . . . ?
C10 N2 Ni1 N4 88.0(9) . . . 1_554 ?
O2 N2 Ni1 N4 -66.0(8) . . . 1_554 ?
C7 N1 Ni1 O3 21.2(8) . . . . ?
O1 N1 Ni1 O3 -158.1(10) . . . . ?
C7 N1 Ni1 O4 39.5(18) . . . . ?
O1 N1 Ni1 O4 -139.7(15) . . . . ?
C7 N1 Ni1 N2 -152.9(8) . . . . ?
O1 N1 Ni1 N2 27.8(10) . . . . ?
C7 N1 Ni1 N3 112.7(8) . . . . ?
O1 N1 Ni1 N3 -66.6(10) . . . . ?
C7 N1 Ni1 N4 -68.3(8) . . . 1_554 ?
O1 N1 Ni1 N4 112.5(10) . . . 1_554 ?
C22 N3 Ni1 O3 54.9(9) . . . . ?
C18 N3 Ni1 O3 -124.1(7) . . . . ?
C22 N3 Ni1 O4 136.3(9) . . . . ?
C18 N3 Ni1 O4 -42.8(7) . . . . ?
C22 N3 Ni1 N2 -134.1(9) . . . . ?
C18 N3 Ni1 N2 46.8(8) . . . . ?
C22 N3 Ni1 N1 -32.6(9) . . . . ?
C18 N3 Ni1 N1 148.4(8) . . . . ?
C9 C8 O1 N1 -76(2) . . . . ?
C7 N1 O1 C8 179.4(14) . . . . ?
Ni1 N1 O1 C8 -1.2(18) . . . . ?
C10 N2 O2 C9 122.4(13) . . . . ?
Ni1 N2 O2 C9 -80.1(14) . . . . ?
C8 C9 O2 N2 49(2) . . . . ?
C6 C1 O3 Ni1 25.4(13) . . . . ?
C2 C1 O3 Ni1 -154.2(7) . . . . ?
C6 C1 O3 La1 -172.2(7) . . . . ?
C2 C1 O3 La1 8.1(13) . . . . ?
O4 Ni1 O3 C1 151.2(8) . . . . ?
N2 Ni1 O3 C1 115.5(16) . . . . ?
N1 Ni1 O3 C1 -32.5(8) . . . . ?
N3 Ni1 O3 C1 -120.9(8) . . . . ?
N4 Ni1 O3 C1 57.6(7) 1_554 . . . ?
O4 Ni1 O3 La1 -14.6(3) . . . . ?
N2 Ni1 O3 La1 -50.3(17) . . . . ?
N1 Ni1 O3 La1 161.7(3) . . . . ?
N3 Ni1 O3 La1 73.4(3) . . . . ?
N4 Ni1 O3 La1 -108.1(3) 1_554 . . . ?
O16 La1 O3 C1 88.2(8) . . . . ?
O4 La1 O3 C1 -151.6(8) . . . . ?
O8 La1 O3 C1 -48.4(9) . . . . ?
O13 La1 O3 C1 147.9(8) . . . . ?
O10 La1 O3 C1 64.1(11) . . . . ?
O7 La1 O3 C1 -77.3(8) . . . . ?
O11 La1 O3 C1 29.5(8) . . . . ?
O5 La1 O3 C1 -139.1(7) . . . . ?
O6 La1 O3 C1 -7.5(7) . . . . ?
N7 La1 O3 C1 39.9(9) . . . . ?
O16 La1 O3 Ni1 -107.0(4) . . . . ?
O4 La1 O3 Ni1 13.1(2) . . . . ?
O8 La1 O3 Ni1 116.3(4) . . . . ?
O13 La1 O3 Ni1 -47.4(4) . . . . ?
O10 La1 O3 Ni1 -131.2(6) . . . . ?
O7 La1 O3 Ni1 87.4(3) . . . . ?
O11 La1 O3 Ni1 -165.8(3) . . . . ?
O5 La1 O3 Ni1 25.6(4) . . . . ?
O6 La1 O3 Ni1 157.2(4) . . . . ?
N7 La1 O3 Ni1 -155.4(5) . . . . ?
C11 C15 O4 Ni1 7.0(13) . . . . ?
C14 C15 O4 Ni1 -177.0(6) . . . . ?
C11 C15 O4 La1 172.5(7) . . . . ?
C14 C15 O4 La1 -11.4(12) . . . . ?
O3 Ni1 O4 C15 -177.5(8) . . . . ?
N2 Ni1 O4 C15 -3.8(7) . . . . ?
N1 Ni1 O4 C15 164.0(12) . . . . ?
N3 Ni1 O4 C15 90.8(8) . . . . ?
N4 Ni1 O4 C15 -88.6(8) 1_554 . . . ?
O3 Ni1 O4 La1 14.5(3) . . . . ?
N2 Ni1 O4 La1 -171.8(3) . . . . ?
N1 Ni1 O4 La1 -4.0(15) . . . . ?
N3 Ni1 O4 La1 -77.2(3) . . . . ?
N4 Ni1 O4 La1 103.5(3) 1_554 . . . ?
O16 La1 O4 C15 -118.9(7) . . . . ?
O3 La1 O4 C15 179.0(7) . . . . ?
O8 La1 O4 C15 57.7(7) . . . . ?
O13 La1 O4 C15 -57.3(7) . . . . ?
O10 La1 O4 C15 -21.9(8) . . . . ?
O7 La1 O4 C15 84.7(7) . . . . ?
O5 La1 O4 C15 10.9(7) . . . . ?
O6 La1 O4 C15 145.3(7) . . . . ?
N7 La1 O4 C15 -23.4(13) . . . . ?
O16 La1 O4 Ni1 49.2(3) . . . . ?
O3 La1 O4 Ni1 -12.9(2) . . . . ?
O8 La1 O4 Ni1 -134.2(3) . . . . ?
O13 La1 O4 Ni1 110.9(3) . . . . ?
O10 La1 O4 Ni1 146.2(4) . . . . ?
O7 La1 O4 Ni1 -107.2(3) . . . . ?
O5 La1 O4 Ni1 179.0(4) . . . . ?
O6 La1 O4 Ni1 -46.6(3) . . . . ?
N7 La1 O4 Ni1 144.7(10) . . . . ?
C42 C14 O5 C17 -15.4(16) . . . . ?
C15 C14 O5 C17 163.6(10) . . . . ?
C42 C14 O5 La1 -171.0(9) . . . . ?
C15 C14 O5 La1 8.0(11) . . . . ?
O16 La1 O5 C14 79.8(8) . . . . ?
O3 La1 O5 C14 -22.1(8) . . . . ?
O4 La1 O5 C14 -9.2(6) . . . . ?
O8 La1 O5 C14 -144.9(7) . . . . ?
O13 La1 O5 C14 78.3(7) . . . . ?
O10 La1 O5 C14 147.9(7) . . . . ?
O7 La1 O5 C14 -93.1(7) . . . . ?
O11 La1 O5 C14 170.3(7) . . . . ?
O6 La1 O5 C14 -103.2(7) . . . . ?
N7 La1 O5 C14 158.6(7) . . . . ?
O16 La1 O5 C17 -75.2(10) . . . . ?
O3 La1 O5 C17 -177.1(9) . . . . ?
O4 La1 O5 C17 -164.1(10) . . . . ?
O8 La1 O5 C17 60.2(9) . . . . ?
O13 La1 O5 C17 -76.6(10) . . . . ?
O10 La1 O5 C17 -7.0(10) . . . . ?
O7 La1 O5 C17 112.0(10) . . . . ?
O11 La1 O5 C17 15.4(10) . . . . ?
O6 La1 O5 C17 101.9(10) . . . . ?
N7 La1 O5 C17 3.7(10) . . . . ?
C3 C2 O6 C16 1.6(17) . . . . ?
C1 C2 O6 C16 -177.5(11) . . . . ?
C3 C2 O6 La1 174.0(9) . . . . ?
C1 C2 O6 La1 -5.1(12) . . . . ?
O16 La1 O6 C2 -68.0(8) . . . . ?
O3 La1 O6 C2 6.2(7) . . . . ?
O4 La1 O6 C2 41.7(8) . . . . ?
O8 La1 O6 C2 154.1(8) . . . . ?
O13 La1 O6 C2 -69.3(11) . . . . ?
O10 La1 O6 C2 -147.9(7) . . . . ?
O7 La1 O6 C2 104.2(8) . . . . ?
O11 La1 O6 C2 -135.8(8) . . . . ?
O5 La1 O6 C2 114.2(7) . . . . ?
N7 La1 O6 C2 -142.4(8) . . . . ?
O16 La1 O6 C16 103.5(11) . . . . ?
O3 La1 O6 C16 177.7(11) . . . . ?
O4 La1 O6 C16 -146.8(10) . . . . ?
O8 La1 O6 C16 -34.4(10) . . . . ?
O13 La1 O6 C16 102.2(12) . . . . ?
O10 La1 O6 C16 23.6(11) . . . . ?
O7 La1 O6 C16 -84.3(10) . . . . ?
O11 La1 O6 C16 35.7(10) . . . . ?
O5 La1 O6 C16 -74.3(11) . . . . ?
N7 La1 O6 C16 29.1(11) . . . . ?
O9 N6 O7 La1 174.9(10) . . . . ?
O8 N6 O7 La1 -4.0(11) . . . . ?
O16 La1 O7 N6 113.1(10) . . . . ?
O3 La1 O7 N6 151.5(7) . . . . ?
O4 La1 O7 N6 -144.2(8) . . . . ?
O8 La1 O7 N6 2.4(7) . . . . ?
O13 La1 O7 N6 -90.7(8) . . . . ?
O10 La1 O7 N6 -11.6(8) . . . . ?
O11 La1 O7 N6 38.3(8) . . . . ?
O5 La1 O7 N6 -80.3(7) . . . . ?
O6 La1 O7 N6 92.7(7) . . . . ?
N7 La1 O7 N6 13.7(9) . . . . ?
O9 N6 O8 La1 -174.8(10) . . . . ?
O7 N6 O8 La1 4.1(11) . . . . ?
O16 La1 O8 N6 -151.1(7) . . . . ?
O3 La1 O8 N6 -42.7(9) . . . . ?
O4 La1 O8 N6 33.4(9) . . . . ?
O13 La1 O8 N6 120.1(8) . . . . ?
O10 La1 O8 N6 163.4(9) . . . . ?
O7 La1 O8 N6 -2.4(7) . . . . ?
O11 La1 O8 N6 -144.7(9) . . . . ?
O5 La1 O8 N6 75.7(8) . . . . ?
O6 La1 O8 N6 -77.9(8) . . . . ?
N7 La1 O8 N6 -170.6(9) . . . . ?
O11 N7 O10 La1 2.0(19) . . . . ?
O12 N7 O10 La1 -166.2(15) . . . . ?
O16 La1 O10 N7 -70.1(11) . . . . ?
O3 La1 O10 N7 -46.6(14) . . . . ?
O4 La1 O10 N7 -178.6(9) . . . . ?
O8 La1 O10 N7 79.6(11) . . . . ?
O13 La1 O10 N7 -141.1(11) . . . . ?
O7 La1 O10 N7 91.1(11) . . . . ?
O11 La1 O10 N7 -1.0(10) . . . . ?
O5 La1 O10 N7 152.9(11) . . . . ?
O6 La1 O10 N7 13.9(11) . . . . ?
O10 N7 O11 La1 -2.0(18) . . . . ?
O12 N7 O11 La1 164.9(18) . . . . ?
O16 La1 O11 N7 99.2(10) . . . . ?
O3 La1 O11 N7 161.4(10) . . . . ?
O8 La1 O11 N7 -76.1(11) . . . . ?
O13 La1 O11 N7 38.8(11) . . . . ?
O10 La1 O11 N7 1.0(10) . . . . ?
O7 La1 O11 N7 -104.5(10) . . . . ?
O5 La1 O11 N7 -29.7(11) . . . . ?
O6 La1 O11 N7 -163.3(11) . . . . ?
O15 N5 O13 La1 19.1(19) . . . . ?
O14 N5 O13 La1 -159.0(10) . . . . ?
O16 La1 O13 N5 -27.8(12) . . . . ?
O3 La1 O13 N5 -90.8(12) . . . . ?
O4 La1 O13 N5 -145.0(12) . . . . ?
O8 La1 O13 N5 103.9(12) . . . . ?
O10 La1 O13 N5 61.4(12) . . . . ?
O7 La1 O13 N5 161.9(11) . . . . ?
O11 La1 O13 N5 32.3(12) . . . . ?
O5 La1 O13 N5 151.1(12) . . . . ?
O6 La1 O13 N5 -26.4(16) . . . . ?
N7 La1 O13 N5 46.9(12) . . . . ?
O3 La1 O16 C28 -73.4(17) . . . . ?
O4 La1 O16 C28 -129.0(17) . . . . ?
O8 La1 O16 C28 55.3(18) . . . . ?
O13 La1 O16 C28 165.3(18) . . . . ?
O10 La1 O16 C28 96.3(17) . . . . ?
O7 La1 O16 C28 -33(2) . . . . ?
O11 La1 O16 C28 49.1(17) . . . . ?
O5 La1 O16 C28 163.9(17) . . . . ?
O6 La1 O16 C28 -14.2(17) . . . . ?
N7 La1 O16 C28 73.4(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.643
_refine_diff_density_min         -1.843
_refine_diff_density_rms         0.242
####################################################################### 
# 
# 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_d777
_database_code_depnum_ccdc_archive 'CCDC 1434585'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_audit_creation_date             2015-09-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H26 N7 Ni O15 Tb'
_chemical_formula_sum            'C28 H26 N7 Ni O15 Tb'
_chemical_formula_weight         918.19
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   10.2398(4)
_cell_length_b                   20.6747(7)
_cell_length_c                   15.2449(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.096(3)
_cell_angle_gamma                90
_cell_volume                     3225.24(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6068
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.6550
_cell_measurement_theta_min      4.2730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8791
_diffrn_reflns_point_group_measured_fraction_full 0.695
_diffrn_reflns_point_group_measured_fraction_max 0.681
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.716
_diffrn_reflns_theta_min         4.277
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  146.00  176.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   30.0000 20

#__ type_ start__ end____ width___ exp.time_
  2 omega   99.00  178.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
  3 omega   92.00  119.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -90.0000 18

#__ type_ start__ end____ width___ exp.time_
  4 omega   86.00  140.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -120.0000 36

#__ type_ start__ end____ width___ exp.time_
  5 omega   54.00   94.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
  6 omega   63.00  130.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  -60.0000 45

#__ type_ start__ end____ width___ exp.time_
  7 omega   87.00  114.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 18

#__ type_ start__ end____ width___ exp.time_
  8 omega   51.00   78.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 18

#__ type_ start__ end____ width___ exp.time_
  9 omega   45.00   99.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -90.0000 36

#__ type_ start__ end____ width___ exp.time_
 10 omega   48.00  103.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -30.0000 37

#__ type_ start__ end____ width___ exp.time_
 11 omega   44.00   92.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -150.0000 32

#__ type_ start__ end____ width___ exp.time_
 12 omega   39.00   69.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 20

#__ type_ start__ end____ width___ exp.time_
 13 omega   42.00  123.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 54

#__ type_ start__ end____ width___ exp.time_
 14 omega   38.00   95.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000   30.0000 38

#__ type_ start__ end____ width___ exp.time_
 15 omega   55.00  113.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000  150.0000 39

#__ type_ start__ end____ width___ exp.time_
 16 omega   36.00   91.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 37

#__ type_ start__ end____ width___ exp.time_
 17 omega   39.00   67.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  120.0000 19

#__ type_ start__ end____ width___ exp.time_
 18 omega   46.00  109.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 42

#__ type_ start__ end____ width___ exp.time_
 19 omega   36.00   79.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   60.0000 29

#__ type_ start__ end____ width___ exp.time_
 20 omega   36.00   84.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 32

#__ type_ start__ end____ width___ exp.time_
 21 omega   28.00  101.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -132.0000 -135.0000 49

#__ type_ start__ end____ width___ exp.time_
 22 omega   -1.00   72.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -120.0000 49

#__ type_ start__ end____ width___ exp.time_
 23 omega   -6.00   19.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 17

#__ type_ start__ end____ width___ exp.time_
 24 omega  -15.00   55.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   60.0000 47

#__ type_ start__ end____ width___ exp.time_
 25 omega  -13.00   15.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 19

#__ type_ start__ end____ width___ exp.time_
 26 omega   27.00   66.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 27 omega  -62.00  -36.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  132.0000  -65.0000 17

#__ type_ start__ end____ width___ exp.time_
 28 omega  -65.00  -38.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 18
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0511612000
_diffrn_orient_matrix_UB_12      -0.0697108000
_diffrn_orient_matrix_UB_13      0.0113628000
_diffrn_orient_matrix_UB_21      0.0139141000
_diffrn_orient_matrix_UB_22      0.0103503000
_diffrn_orient_matrix_UB_23      0.0999434000
_diffrn_orient_matrix_UB_31      -0.1408765000
_diffrn_orient_matrix_UB_32      -0.0243040000
_diffrn_orient_matrix_UB_33      0.0100570000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.394
_reflns_Friedel_fraction_full    0.402
_reflns_Friedel_fraction_max     0.386
_reflns_number_gt                4065
_reflns_number_total             4154
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.006(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         4154
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0697P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1038
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq, Uanis(O15') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: O15'(0.5) O15(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C15(H15), C16(H16), C17(H17),
 C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb -0.00365(4) -0.09714(2) -0.26033(4) 0.03036(15) Uani 1 1 d . . . . .
Ni1 Ni 0.28787(11) -0.15991(5) -0.16527(9) 0.0245(3) Uani 1 1 d . . . . .
O1 O -0.1297(6) -0.0841(3) -0.1225(4) 0.0386(15) Uani 1 1 d . . . . .
O2 O 0.1135(5) -0.1224(3) -0.1302(3) 0.0262(11) Uani 1 1 d . . . . .
O3 O 0.4762(6) -0.1594(3) -0.0013(6) 0.0531(19) Uani 1 1 d . . . . .
O4 O 0.5353(9) -0.2382(5) -0.1782(8) 0.090(4) Uani 1 1 d . . . . .
O5 O 0.1989(5) -0.1423(2) -0.2858(4) 0.0258(11) Uani 1 1 d . . . . .
O6 O 0.0651(9) -0.0940(4) -0.4191(6) 0.057(2) Uani 1 1 d . . . . .
O7 O 0.0226(12) 0.0112(5) -0.1912(6) 0.091(3) Uani 1 1 d . . . . .
O8 O 0.1720(13) 0.0801(5) -0.2193(7) 0.094(4) Uani 1 1 d . . . . .
O9 O 0.1404(10) -0.0052(4) -0.2963(7) 0.071(2) Uani 1 1 d . . . . .
O10 O -0.0690(9) -0.1975(6) -0.3472(6) 0.082(3) Uani 1 1 d . . . . .
O11 O -0.0977(7) -0.1987(3) -0.2095(4) 0.0514(17) Uani 1 1 d . . . . .
O12 O -0.1815(11) -0.2765(6) -0.2862(8) 0.100(4) Uani 1 1 d . . . . .
O13 O -0.1663(10) -0.0285(7) -0.3267(8) 0.107(4) Uani 1 1 d . . . . .
O14 O -0.3437(11) -0.0410(8) -0.4060(7) 0.124(6) Uani 1 1 d . . . . .
N1 N 0.3428(6) -0.1643(3) -0.0325(5) 0.0320(15) Uani 1 1 d . . . . .
N2 N 0.4387(7) -0.2003(3) -0.2274(5) 0.0369(16) Uani 1 1 d . . . . .
N3 N 0.3779(6) -0.0638(3) -0.1677(5) 0.0287(14) Uani 1 1 d . . . . .
N4 N 0.2058(7) -0.2595(3) -0.1632(5) 0.0322(15) Uani 1 1 d . . . . .
N5 N 0.1131(11) 0.0297(5) -0.2345(6) 0.060(2) Uani 1 1 d . . . . .
N6 N -0.1200(9) -0.2264(5) -0.2824(6) 0.060(3) Uani 1 1 d . . . . .
N7 N -0.2651(11) -0.0609(7) -0.3552(7) 0.070(3) Uani 1 1 d . . . . .
C1 C -0.2381(11) -0.0421(6) -0.1146(8) 0.065(3) Uani 1 1 d . . . . .
H1A H -0.2508 -0.0176 -0.1678 0.097 Uiso 1 1 calc GR . . . .
H1B H -0.2220 -0.0132 -0.0662 0.097 Uiso 1 1 calc GR . . . .
H1C H -0.3151 -0.0672 -0.1046 0.097 Uiso 1 1 calc GR . . . .
C2 C -0.0700(9) -0.1072(4) -0.0442(7) 0.0317(18) Uani 1 1 d . . . . .
C3 C 0.0606(7) -0.1256(3) -0.0525(5) 0.0248(15) Uani 1 1 d . . . . .
C4 C 0.1306(8) -0.1434(4) 0.0252(5) 0.0310(17) Uani 1 1 d . . . . .
C5 C 0.0646(11) -0.1441(4) 0.1054(6) 0.045(2) Uani 1 1 d . . . . .
H5 H 0.1106 -0.1557 0.1568 0.054 Uiso 1 1 calc R . . . .
C6 C -0.0637(11) -0.1283(5) 0.1094(6) 0.049(2) Uani 1 1 d . . . . .
H6 H -0.1053 -0.1307 0.1625 0.059 Uiso 1 1 calc R . . . .
C7 C -0.1329(10) -0.1086(4) 0.0339(7) 0.043(2) Uani 1 1 d . . . . .
H7 H -0.2202 -0.0966 0.0362 0.052 Uiso 1 1 calc R . . . .
C8 C 0.2692(9) -0.1537(4) 0.0299(6) 0.037(2) Uani 1 1 d . . . . .
H8 H 0.3091 -0.1523 0.0856 0.044 Uiso 1 1 calc R . . . .
C9 C 0.5531(10) -0.2130(6) -0.0262(8) 0.056(3) Uani 1 1 d . . . . .
H9A H 0.5004 -0.2519 -0.0259 0.067 Uiso 1 1 calc R . . . .
H9B H 0.6254 -0.2185 0.0160 0.067 Uiso 1 1 calc R . . . .
C10 C 0.6042(13) -0.2033(8) -0.1144(12) 0.080(5) Uani 1 1 d . . . . .
H10A H 0.5999 -0.1577 -0.1291 0.096 Uiso 1 1 calc R . . . .
H10B H 0.6953 -0.2162 -0.1139 0.096 Uiso 1 1 calc R . . . .
C11 C 0.4459(10) -0.2093(5) -0.3111(7) 0.045(2) Uani 1 1 d . . . . .
H11 H 0.5166 -0.2337 -0.3285 0.054 Uiso 1 1 calc R . . . .
C12 C 0.3612(10) -0.1870(4) -0.3791(7) 0.039(2) Uani 1 1 d . . . . .
C13 C 0.2456(8) -0.1528(3) -0.3642(5) 0.0286(17) Uani 1 1 d . . . . .
C14 C 0.1734(9) -0.1290(4) -0.4390(6) 0.040(2) Uani 1 1 d . . . . .
C15 C 0.2118(12) -0.1410(6) -0.5225(7) 0.054(3) Uani 1 1 d . . . . .
H15 H 0.1630 -0.1246 -0.5701 0.065 Uiso 1 1 calc R . . . .
C16 C 0.3224(12) -0.1772(5) -0.5367(7) 0.057(3) Uani 1 1 d . . . . .
H16 H 0.3466 -0.1861 -0.5936 0.069 Uiso 1 1 calc R . . . .
C17 C 0.3962(10) -0.1999(5) -0.4665(7) 0.046(3) Uani 1 1 d . . . . .
H17 H 0.4706 -0.2242 -0.4764 0.056 Uiso 1 1 calc R . . . .
C18 C 0.017(2) -0.0484(10) -0.4823(11) 0.129(9) Uani 1 1 d . . . . .
H18A H -0.0718 -0.0374 -0.4702 0.193 Uiso 1 1 calc GR . . . .
H18B H 0.0198 -0.0669 -0.5400 0.193 Uiso 1 1 calc GR . . . .
H18C H 0.0698 -0.0101 -0.4795 0.193 Uiso 1 1 calc GR . . . .
C19 C 0.4306(8) -0.0406(4) -0.2403(6) 0.0331(17) Uani 1 1 d . . . . .
H19 H 0.4218 -0.0648 -0.2916 0.040 Uiso 1 1 calc R . . . .
C20 C 0.4983(10) 0.0180(4) -0.2436(6) 0.035(2) Uani 1 1 d . . . . .
H20 H 0.5345 0.0317 -0.2955 0.041 Uiso 1 1 calc R . . . .
C21 C 0.5105(7) 0.0553(3) -0.1685(6) 0.0260(15) Uani 1 1 d . . . . .
C22 C 0.3883(8) -0.0259(3) -0.0961(6) 0.0326(18) Uani 1 1 d . . . . .
H22 H 0.3488 -0.0397 -0.0453 0.039 Uiso 1 1 calc R . . . .
C23 C 0.4545(8) 0.0322(4) -0.0937(6) 0.0333(18) Uani 1 1 d . . . . .
H23 H 0.4613 0.0558 -0.0418 0.040 Uiso 1 1 calc R . . . .
C24 C 0.1557(10) -0.2850(4) -0.2377(7) 0.041(2) Uani 1 1 d . . . . .
H24 H 0.1610 -0.2610 -0.2890 0.049 Uiso 1 1 calc R . . . .
C25 C 0.0961(9) -0.3454(4) -0.2427(6) 0.0372(19) Uani 1 1 d . . . . .
H25 H 0.0641 -0.3610 -0.2965 0.045 Uiso 1 1 calc R . . . .
C26 C 0.0846(7) -0.3820(3) -0.1684(6) 0.0300(17) Uani 1 1 d . . . . .
C27 C 0.1419(9) -0.3574(4) -0.0919(6) 0.0345(18) Uani 1 1 d . . . . .
H27 H 0.1408 -0.3813 -0.0403 0.041 Uiso 1 1 calc R . . . .
C28 C 0.2010(8) -0.2969(4) -0.0922(6) 0.0333(17) Uani 1 1 d . . . . .
H28 H 0.2394 -0.2817 -0.0400 0.040 Uiso 1 1 calc R . . . .
O15' O -0.274(3) -0.1081(12) -0.292(2) 0.098(7) Uani 0.5 1 d . U P A 1
O15 O -0.255(4) -0.1136(18) -0.344(3) 0.132(11) Uani 0.5 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.520(6) . ?
Tb1 O2 2.340(5) . ?
Tb1 O5 2.320(5) . ?
Tb1 O6 2.547(9) . ?
Tb1 O7 2.486(9) . ?
Tb1 O9 2.480(9) . ?
Tb1 O10 2.538(9) . ?
Tb1 O11 2.448(7) . ?
Tb1 O13 2.384(10) . ?
Tb1 N5 2.902(10) . ?
Tb1 O15' 2.80(3) . ?
Tb1 O15 2.85(4) . ?
Ni1 O2 2.036(5) . ?
Ni1 O5 2.053(6) . ?
Ni1 N1 2.082(7) . ?
Ni1 N2 2.021(7) . ?
Ni1 N3 2.191(6) . ?
Ni1 N4 2.225(6) . ?
O1 C1 1.417(11) . ?
O1 C2 1.405(11) . ?
O2 C3 1.321(9) . ?
O3 N1 1.434(9) . ?
O3 C9 1.418(13) . ?
O4 N2 1.450(12) . ?
O4 C10 1.383(19) . ?
O5 C13 1.321(10) . ?
O6 C14 1.367(12) . ?
O6 C18 1.424(14) . ?
O7 N5 1.219(14) . ?
O8 N5 1.222(13) . ?
O9 N5 1.226(13) . ?
O10 N6 1.282(13) . ?
O11 N6 1.263(11) . ?
O12 N6 1.212(12) . ?
O13 N7 1.276(17) . ?
O14 N7 1.171(13) . ?
N1 C8 1.255(12) . ?
N2 C11 1.294(13) . ?
N3 C19 1.339(11) . ?
N3 C22 1.346(11) . ?
N4 C24 1.337(12) . ?
N4 C28 1.332(11) . ?
N7 O15' 1.38(3) . ?
N7 O15 1.11(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.401(12) . ?
C2 C7 1.374(14) . ?
C3 C4 1.411(11) . ?
C4 C5 1.419(12) . ?
C4 C8 1.434(12) . ?
C5 H5 0.9300 . ?
C5 C6 1.357(15) . ?
C6 H6 0.9300 . ?
C6 C7 1.391(15) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.47(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11 0.9300 . ?
C11 C12 1.405(15) . ?
C12 C13 1.405(13) . ?
C12 C17 1.418(14) . ?
C13 C14 1.425(13) . ?
C14 C15 1.369(13) . ?
C15 H15 0.9300 . ?
C15 C16 1.381(17) . ?
C16 H16 0.9300 . ?
C16 C17 1.371(17) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19 0.9300 . ?
C19 C20 1.397(10) . ?
C20 H20 0.9300 . ?
C20 C21 1.382(12) . ?
C21 C23 1.381(11) . ?
C21 C26 1.501(9) 3 ?
C22 H22 0.9300 . ?
C22 C23 1.380(11) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C24 C25 1.391(11) . ?
C25 H25 0.9300 . ?
C25 C26 1.370(12) . ?
C26 C21 1.501(9) 3_445 ?
C26 C27 1.384(12) . ?
C27 H27 0.9300 . ?
C27 C28 1.389(10) . ?
C28 H28 0.9300 . ?

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 Tb1 O6 163.2(2) . . ?
O1 Tb1 O10 112.9(3) . . ?
O1 Tb1 N5 90.6(3) . . ?
O1 Tb1 O15' 67.6(6) . . ?
O1 Tb1 O15 84.4(8) . . ?
O2 Tb1 O1 65.13(19) . . ?
O2 Tb1 O6 131.4(2) . . ?
O2 Tb1 O7 78.3(3) . . ?
O2 Tb1 O9 93.9(3) . . ?
O2 Tb1 O10 112.2(3) . . ?
O2 Tb1 O11 74.7(2) . . ?
O2 Tb1 O13 145.2(4) . . ?
O2 Tb1 N5 83.7(2) . . ?
O2 Tb1 O15' 126.9(6) . . ?
O2 Tb1 O15 141.1(8) . . ?
O5 Tb1 O1 132.1(2) . . ?
O5 Tb1 O2 67.56(18) . . ?
O5 Tb1 O6 64.6(2) . . ?
O5 Tb1 O7 110.5(3) . . ?
O5 Tb1 O9 74.3(2) . . ?
O5 Tb1 O10 78.7(3) . . ?
O5 Tb1 O11 94.1(2) . . ?
O5 Tb1 O13 141.6(3) . . ?
O5 Tb1 N5 91.1(3) . . ?
O5 Tb1 O15' 145.3(6) . . ?
O5 Tb1 O15 132.5(7) . . ?
O6 Tb1 N5 88.8(3) . . ?
O6 Tb1 O15' 98.3(6) . . ?
O6 Tb1 O15 81.7(8) . . ?
O7 Tb1 O1 66.5(3) . . ?
O7 Tb1 O6 110.5(3) . . ?
O7 Tb1 O10 168.6(4) . . ?
O7 Tb1 N5 24.6(3) . . ?
O7 Tb1 O15' 103.7(6) . . ?
O7 Tb1 O15 112.3(8) . . ?
O9 Tb1 O1 115.4(3) . . ?
O9 Tb1 O6 65.4(3) . . ?
O9 Tb1 O7 49.2(3) . . ?
O9 Tb1 O10 131.2(3) . . ?
O9 Tb1 N5 24.8(3) . . ?
O9 Tb1 O15' 128.0(5) . . ?
O9 Tb1 O15 121.8(8) . . ?
O10 Tb1 O6 66.5(3) . . ?
O10 Tb1 N5 155.3(3) . . ?
O10 Tb1 O15' 66.7(6) . . ?
O10 Tb1 O15 56.8(8) . . ?
O11 Tb1 O1 67.0(2) . . ?
O11 Tb1 O6 116.6(2) . . ?
O11 Tb1 O7 132.6(3) . . ?
O11 Tb1 O9 166.3(3) . . ?
O11 Tb1 O10 50.5(3) . . ?
O11 Tb1 N5 153.8(2) . . ?
O11 Tb1 O15' 65.6(5) . . ?
O11 Tb1 O15 71.3(8) . . ?
O13 Tb1 O1 85.3(3) . . ?
O13 Tb1 O6 78.2(3) . . ?
O13 Tb1 O7 73.0(5) . . ?
O13 Tb1 O9 82.1(4) . . ?
O13 Tb1 O10 95.6(4) . . ?
O13 Tb1 O11 111.6(4) . . ?
O13 Tb1 N5 78.4(4) . . ?
O13 Tb1 O15' 45.9(6) . . ?
O13 Tb1 O15 43.6(8) . . ?
O15' Tb1 N5 119.7(6) . . ?
O15 Tb1 N5 122.0(8) . . ?
O2 Ni1 O5 78.6(2) . . ?
O2 Ni1 N1 88.3(3) . . ?
O2 Ni1 N3 91.9(2) . . ?
O2 Ni1 N4 90.8(2) . . ?
O5 Ni1 N1 166.5(2) . . ?
O5 Ni1 N3 89.8(2) . . ?
O5 Ni1 N4 91.2(3) . . ?
N1 Ni1 N3 87.6(2) . . ?
N1 Ni1 N4 92.0(3) . . ?
N2 Ni1 O2 166.6(3) . . ?
N2 Ni1 O5 88.6(3) . . ?
N2 Ni1 N1 104.7(3) . . ?
N2 Ni1 N3 92.1(3) . . ?
N2 Ni1 N4 85.4(3) . . ?
N3 Ni1 N4 177.3(3) . . ?
C1 O1 Tb1 124.3(6) . . ?
C2 O1 Tb1 116.8(5) . . ?
C2 O1 C1 117.0(8) . . ?
Ni1 O2 Tb1 106.8(2) . . ?
C3 O2 Tb1 123.8(4) . . ?
C3 O2 Ni1 127.5(5) . . ?
C9 O3 N1 112.8(7) . . ?
C10 O4 N2 113.7(10) . . ?
Ni1 O5 Tb1 107.0(2) . . ?
C13 O5 Tb1 124.9(5) . . ?
C13 O5 Ni1 128.1(5) . . ?
C14 O6 Tb1 116.9(6) . . ?
C14 O6 C18 117.7(10) . . ?
C18 O6 Tb1 124.0(8) . . ?
N5 O7 Tb1 97.2(7) . . ?
N5 O9 Tb1 97.3(8) . . ?
N6 O10 Tb1 94.9(6) . . ?
N6 O11 Tb1 99.8(6) . . ?
N7 O13 Tb1 111.4(9) . . ?
O3 N1 Ni1 122.7(6) . . ?
C8 N1 Ni1 125.5(6) . . ?
C8 N1 O3 109.1(7) . . ?
O4 N2 Ni1 119.9(7) . . ?
C11 N2 Ni1 126.4(7) . . ?
C11 N2 O4 111.7(8) . . ?
C19 N3 Ni1 121.5(5) . . ?
C19 N3 C22 116.1(6) . . ?
C22 N3 Ni1 122.3(5) . . ?
C24 N4 Ni1 119.1(6) . . ?
C28 N4 Ni1 125.0(6) . . ?
C28 N4 C24 115.8(7) . . ?
O7 N5 Tb1 58.2(6) . . ?
O7 N5 O8 123.0(11) . . ?
O7 N5 O9 115.6(10) . . ?
O8 N5 Tb1 173.8(9) . . ?
O8 N5 O9 121.4(13) . . ?
O9 N5 Tb1 57.9(6) . . ?
O10 N6 Tb1 59.3(5) . . ?
O11 N6 Tb1 55.1(5) . . ?
O11 N6 O10 113.6(8) . . ?
O12 N6 Tb1 171.6(8) . . ?
O12 N6 O10 126.0(10) . . ?
O12 N6 O11 120.4(10) . . ?
O13 N7 O15' 101.7(16) . . ?
O14 N7 O13 123.9(16) . . ?
O14 N7 O15' 131(2) . . ?
O15 N7 O13 113(2) . . ?
O15 N7 O14 120(3) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 113.8(8) . . ?
C7 C2 O1 122.7(8) . . ?
C7 C2 C3 123.5(9) . . ?
O2 C3 C2 119.4(7) . . ?
O2 C3 C4 123.6(7) . . ?
C2 C3 C4 116.9(8) . . ?
C3 C4 C5 118.9(8) . . ?
C3 C4 C8 123.5(8) . . ?
C5 C4 C8 117.2(8) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.9(9) . . ?
C6 C5 H5 119.1 . . ?
C5 C6 H6 120.1 . . ?
C5 C6 C7 119.9(9) . . ?
C7 C6 H6 120.1 . . ?
C2 C7 C6 118.9(9) . . ?
C2 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
N1 C8 C4 127.5(8) . . ?
N1 C8 H8 116.2 . . ?
C4 C8 H8 116.2 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
O3 C9 C10 110.9(10) . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
O4 C10 C9 112.4(12) . . ?
O4 C10 H10A 109.1 . . ?
O4 C10 H10B 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 H11 115.7 . . ?
N2 C11 C12 128.6(9) . . ?
C12 C11 H11 115.7 . . ?
C11 C12 C13 123.2(9) . . ?
C11 C12 C17 117.5(9) . . ?
C13 C12 C17 119.4(10) . . ?
O5 C13 C12 124.4(8) . . ?
O5 C13 C14 118.3(7) . . ?
C12 C13 C14 117.4(8) . . ?
O6 C14 C13 114.0(8) . . ?
O6 C14 C15 124.4(10) . . ?
C15 C14 C13 121.6(9) . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.6(11) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.7(9) . . ?
C17 C16 H16 120.2 . . ?
C12 C17 H17 119.4 . . ?
C16 C17 C12 121.3(10) . . ?
C16 C17 H17 119.4 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19 118.1 . . ?
N3 C19 C20 123.9(8) . . ?
C20 C19 H19 118.1 . . ?
C19 C20 H20 120.5 . . ?
C21 C20 C19 118.9(8) . . ?
C21 C20 H20 120.5 . . ?
C20 C21 C26 120.9(7) . 3 ?
C23 C21 C20 117.6(7) . . ?
C23 C21 C26 121.5(7) . 3 ?
N3 C22 H22 118.2 . . ?
N3 C22 C23 123.5(8) . . ?
C23 C22 H22 118.2 . . ?
C21 C23 H23 120.0 . . ?
C22 C23 C21 119.9(8) . . ?
C22 C23 H23 120.0 . . ?
N4 C24 H24 118.1 . . ?
N4 C24 C25 123.7(10) . . ?
C25 C24 H24 118.1 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 120.1(9) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 122.3(8) . 3_445 ?
C25 C26 C27 116.5(7) . . ?
C27 C26 C21 121.2(7) . 3_445 ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 120.0(8) . . ?
C28 C27 H27 120.0 . . ?
N4 C28 C27 123.7(8) . . ?
N4 C28 H28 118.2 . . ?
C27 C28 H28 118.2 . . ?
N7 O15' Tb1 88.6(14) . . ?
N7 O15 Tb1 92(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C2 C3 9.1(9) . . . . ?
Tb1 O1 C2 C7 -173.8(7) . . . . ?
Tb1 O2 C3 C2 -6.2(9) . . . . ?
Tb1 O2 C3 C4 177.3(5) . . . . ?
Tb1 O5 C13 C12 -172.1(6) . . . . ?
Tb1 O5 C13 C14 6.8(9) . . . . ?
Tb1 O6 C14 C13 -10.8(10) . . . . ?
Tb1 O6 C14 C15 169.2(8) . . . . ?
Tb1 O7 N5 O8 -172.8(10) . . . . ?
Tb1 O7 N5 O9 8.7(12) . . . . ?
Tb1 O9 N5 O7 -8.7(12) . . . . ?
Tb1 O9 N5 O8 172.7(10) . . . . ?
Tb1 O10 N6 O11 -9.7(10) . . . . ?
Tb1 O10 N6 O12 172.2(13) . . . . ?
Tb1 O11 N6 O10 10.2(11) . . . . ?
Tb1 O11 N6 O12 -171.6(11) . . . . ?
Tb1 O13 N7 O14 -162.9(10) . . . . ?
Tb1 O13 N7 O15' 36.6(15) . . . . ?
Tb1 O13 N7 O15 0(2) . . . . ?
Ni1 O2 C3 C2 -168.6(5) . . . . ?
Ni1 O2 C3 C4 14.9(10) . . . . ?
Ni1 O5 C13 C12 9.2(10) . . . . ?
Ni1 O5 C13 C14 -171.9(5) . . . . ?
Ni1 N1 C8 C4 7.4(11) . . . . ?
Ni1 N2 C11 C12 8.4(16) . . . . ?
Ni1 N3 C19 C20 -174.7(7) . . . . ?
Ni1 N3 C22 C23 174.1(7) . . . . ?
Ni1 N4 C24 C25 -176.6(8) . . . . ?
Ni1 N4 C28 C27 175.9(7) . . . . ?
O1 C2 C3 O2 -2.6(11) . . . . ?
O1 C2 C3 C4 174.1(7) . . . . ?
O1 C2 C7 C6 -175.9(8) . . . . ?
O2 C3 C4 C5 178.9(7) . . . . ?
O2 C3 C4 C8 6.5(12) . . . . ?
O3 N1 C8 C4 169.0(7) . . . . ?
O3 C9 C10 O4 -102.4(13) . . . . ?
O4 N2 C11 C12 172.4(10) . . . . ?
O5 C13 C14 O6 3.5(11) . . . . ?
O5 C13 C14 C15 -176.4(8) . . . . ?
O6 C14 C15 C16 -179.6(10) . . . . ?
O13 N7 O15' Tb1 -28.3(12) . . . . ?
O13 N7 O15 Tb1 0.3(19) . . . . ?
O14 N7 O15' Tb1 173.2(15) . . . . ?
O14 N7 O15 Tb1 163.5(13) . . . . ?
N1 O3 C9 C10 85.6(11) . . . . ?
N2 O4 C10 C9 99.1(13) . . . . ?
N2 C11 C12 C13 -4.0(17) . . . . ?
N2 C11 C12 C17 175.7(10) . . . . ?
N3 C19 C20 C21 -1.1(14) . . . . ?
N3 C22 C23 C21 2.2(13) . . . . ?
N4 C24 C25 C26 0.9(16) . . . . ?
C1 O1 C2 C3 -155.9(9) . . . . ?
C1 O1 C2 C7 21.2(14) . . . . ?
C2 C3 C4 C5 2.3(11) . . . . ?
C2 C3 C4 C8 -170.1(7) . . . . ?
C3 C2 C7 C6 1.0(14) . . . . ?
C3 C4 C5 C6 0.2(13) . . . . ?
C3 C4 C8 N1 -18.8(13) . . . . ?
C4 C5 C6 C7 -2.3(15) . . . . ?
C5 C4 C8 N1 168.7(8) . . . . ?
C5 C6 C7 C2 1.7(15) . . . . ?
C7 C2 C3 O2 -179.7(8) . . . . ?
C7 C2 C3 C4 -3.0(12) . . . . ?
C8 C4 C5 C6 173.1(8) . . . . ?
C9 O3 N1 Ni1 -67.1(8) . . . . ?
C9 O3 N1 C8 130.6(8) . . . . ?
C10 O4 N2 Ni1 -62.5(13) . . . . ?
C10 O4 N2 C11 132.3(11) . . . . ?
C11 C12 C13 O5 -5.5(13) . . . . ?
C11 C12 C13 C14 175.6(9) . . . . ?
C11 C12 C17 C16 -176.8(9) . . . . ?
C12 C13 C14 O6 -177.5(8) . . . . ?
C12 C13 C14 C15 2.6(13) . . . . ?
C13 C12 C17 C16 2.9(14) . . . . ?
C13 C14 C15 C16 0.4(16) . . . . ?
C14 C15 C16 C17 -1.7(17) . . . . ?
C15 C16 C17 C12 0.1(15) . . . . ?
C17 C12 C13 O5 174.8(8) . . . . ?
C17 C12 C13 C14 -4.1(12) . . . . ?
C18 O6 C14 C13 156.1(14) . . . . ?
C18 O6 C14 C15 -24.0(19) . . . . ?
C19 N3 C22 C23 -3.2(12) . . . . ?
C19 C20 C21 C23 0.0(13) . . . . ?
C19 C20 C21 C26 178.8(8) . . . 3 ?
C20 C21 C23 C22 -0.5(13) . . . . ?
C21 C26 C27 C28 -174.9(8) 3_445 . . . ?
C22 N3 C19 C20 2.7(13) . . . . ?
C24 N4 C28 C27 -3.6(13) . . . . ?
C24 C25 C26 C21 174.3(8) . . . 3_445 ?
C24 C25 C26 C27 -4.0(13) . . . . ?
C25 C26 C27 C28 3.3(13) . . . . ?
C26 C21 C23 C22 -179.3(8) 3 . . . ?
C26 C27 C28 N4 0.5(14) . . . . ?
C28 N4 C24 C25 2.9(14) . . . . ?
O15' N7 O15 Tb1 -78(4) . . . . ?
O15 N7 O15' Tb1 85(4) . . . . ?

_olex2_date_sample_data_collection 2015-08-31
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_d781
_database_code_depnum_ccdc_archive 'CCDC 1434586'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_audit_creation_date             2015-10-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C30 H29 Dy N6 Ni O14'
_chemical_formula_sum            'C30 H29 Dy N6 Ni O14'
_chemical_formula_weight         918.80
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8105(7)
_cell_length_b                   12.7474(7)
_cell_length_c                   12.9606(7)
_cell_angle_alpha                115.947(6)
_cell_angle_beta                 98.650(5)
_cell_angle_gamma                94.593(5)
_cell_volume                     1711.10(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5047
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.8430
_cell_measurement_theta_min      4.9960
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.912
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10981
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.938
_diffrn_reflns_theta_min         3.910
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   28.00   60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  150.0000 32

#__ type_ start__ end____ width___ exp.time_
  2 omega   82.00  123.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000  120.0000 41

#__ type_ start__ end____ width___ exp.time_
  3 omega  108.00  164.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  150.0000 56

#__ type_ start__ end____ width___ exp.time_
  4 omega   96.00  123.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
  5 omega   88.00  121.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -120.0000 33

#__ type_ start__ end____ width___ exp.time_
  6 omega  139.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000 -120.0000 39

#__ type_ start__ end____ width___ exp.time_
  7 omega  127.00  160.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 33

#__ type_ start__ end____ width___ exp.time_
  8 omega  103.00  142.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000 -150.0000 39

#__ type_ start__ end____ width___ exp.time_
  9 omega   32.00  121.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 89

#__ type_ start__ end____ width___ exp.time_
 10 omega   80.00  135.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000 -120.0000 55

#__ type_ start__ end____ width___ exp.time_
 11 omega  106.00  143.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  -60.0000 37

#__ type_ start__ end____ width___ exp.time_
 12 omega   75.00  102.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
 13 omega   66.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 48

#__ type_ start__ end____ width___ exp.time_
 14 omega   42.00   92.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -90.0000 50

#__ type_ start__ end____ width___ exp.time_
 15 omega   48.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 61

#__ type_ start__ end____ width___ exp.time_
 16 omega   42.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  -60.0000 44

#__ type_ start__ end____ width___ exp.time_
 17 omega   44.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 43

#__ type_ start__ end____ width___ exp.time_
 18 omega   34.00   74.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
 19 omega   39.00   93.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   60.0000 54

#__ type_ start__ end____ width___ exp.time_
 20 omega   56.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000  150.0000 68

#__ type_ start__ end____ width___ exp.time_
 21 omega   74.00  176.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000  150.0000 102

#__ type_ start__ end____ width___ exp.time_
 22 omega   54.00   93.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  150.0000 39

#__ type_ start__ end____ width___ exp.time_
 23 omega   36.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  120.0000 31

#__ type_ start__ end____ width___ exp.time_
 24 omega   -2.00   51.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   60.0000 53

#__ type_ start__ end____ width___ exp.time_
 25 omega  -19.00    8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 26 omega  -65.00  -24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 41

#__ type_ start__ end____ width___ exp.time_
 27 omega  -24.00   25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  150.0000 49

#__ type_ start__ end____ width___ exp.time_
 28 omega   23.00  109.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -150.0000 86

#__ type_ start__ end____ width___ exp.time_
 29 omega   36.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -150.0000 55

#__ type_ start__ end____ width___ exp.time_
 30 omega   27.00   54.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
 31 omega  -15.00   75.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -150.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0530817000
_diffrn_orient_matrix_UB_12      -0.0552489000
_diffrn_orient_matrix_UB_13      -0.1321515000
_diffrn_orient_matrix_UB_21      -0.0542905000
_diffrn_orient_matrix_UB_22      0.1114954000
_diffrn_orient_matrix_UB_23      0.0197937000
_diffrn_orient_matrix_UB_31      0.1101131000
_diffrn_orient_matrix_UB_32      0.0554979000
_diffrn_orient_matrix_UB_33      -0.0199922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5573
_reflns_number_total             6277
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.081
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0494
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0844P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1334
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C15(H15), C16(H16), C17(H17),
 C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.24838(3) 0.02562(2) 0.26789(2) 0.03895(12) Uani 1 1 d . . . . .
Ni1 Ni 0.29435(7) -0.25937(6) 0.16196(6) 0.03305(19) Uani 1 1 d . . . . .
O1 O 0.0477(3) -0.0032(4) 0.2959(4) 0.0529(10) Uani 1 1 d . . . . .
O2 O 0.1567(3) -0.1705(3) 0.1840(3) 0.0352(7) Uani 1 1 d . . . . .
O14 O 0.2948(4) -0.0227(3) 0.4143(3) 0.0590(11) Uani 1 1 d . . . . .
O3 O 0.2211(4) -0.5204(3) 0.0593(3) 0.0560(10) Uani 1 1 d . . . . .
O13 O 0.3250(3) -0.2088(3) 0.3410(3) 0.0449(8) Uani 1 1 d . . . . .
O4 O 0.4695(4) -0.4293(4) 0.1507(4) 0.0580(10) Uani 1 1 d . . . . .
O5 O 0.3741(3) -0.1006(3) 0.1911(3) 0.0382(7) Uani 1 1 d . . . . .
O6 O 0.4117(4) 0.0966(3) 0.1849(3) 0.0494(9) Uani 1 1 d . . . . .
O7 O 0.3949(4) 0.1935(4) 0.4131(4) 0.0616(11) Uani 1 1 d . . . . .
O8 O 0.2247(4) 0.1934(4) 0.4506(4) 0.0549(10) Uani 1 1 d . . . . .
O9 O 0.3701(5) 0.3114(4) 0.5870(4) 0.0793(15) Uani 1 1 d . . . . .
O10 O 0.1580(4) -0.0034(4) 0.0715(3) 0.0525(9) Uani 1 1 d . . . . .
O11 O 0.1656(5) 0.1669(4) 0.2150(4) 0.0688(13) Uani 1 1 d . . . . .
O12 O 0.1002(5) 0.1371(6) 0.0350(5) 0.0853(16) Uani 1 1 d . . . . .
N1 N 0.1887(4) -0.4082(4) 0.1268(4) 0.0432(10) Uani 1 1 d . . . . .
N2 N 0.4527(4) -0.3180(4) 0.1574(4) 0.0428(10) Uani 1 1 d . . . . .
N3 N 0.2603(4) -0.3156(3) -0.0240(3) 0.0366(9) Uani 1 1 d . . . . .
N4 N 0.1297(6) -0.4771(5) -0.6313(4) 0.0634(14) Uani 1 1 d . . . . .
N5 N 0.3309(5) 0.2355(4) 0.4870(4) 0.0533(12) Uani 1 1 d . . . . .
N6 N 0.1389(5) 0.1012(5) 0.1036(5) 0.0561(12) Uani 1 1 d . . . . .
C1 C -0.0182(6) 0.0906(7) 0.3470(7) 0.074(2) Uani 1 1 d . . . . .
H1A H 0.0169 0.1608 0.3464 0.111 Uiso 1 1 calc GR . . . .
H1B H -0.0189 0.1061 0.4263 0.111 Uiso 1 1 calc GR . . . .
H1C H -0.0964 0.0672 0.3023 0.111 Uiso 1 1 calc GR . . . .
C2 C 0.0023(4) -0.1141(5) 0.2796(5) 0.0451(12) Uani 1 1 d . . . . .
C3 C 0.0656(4) -0.2028(5) 0.2185(4) 0.0377(10) Uani 1 1 d . . . . .
C4 C 0.0274(5) -0.3192(5) 0.1986(5) 0.0462(12) Uani 1 1 d . . . . .
C5 C -0.0717(6) -0.3453(7) 0.2351(6) 0.0624(17) Uani 1 1 d . . . . .
H5 H -0.0975 -0.4227 0.2192 0.075 Uiso 1 1 calc R . . . .
C6 C -0.1317(6) -0.2563(8) 0.2949(7) 0.074(2) Uani 1 1 d . . . . .
H6 H -0.1978 -0.2744 0.3188 0.089 Uiso 1 1 calc R . . . .
C7 C -0.0939(6) -0.1394(8) 0.3196(6) 0.0657(18) Uani 1 1 d . . . . .
H7 H -0.1327 -0.0794 0.3624 0.079 Uiso 1 1 calc R . . . .
C8 C 0.0854(5) -0.4177(5) 0.1420(4) 0.0474(13) Uani 1 1 d . . . . .
H8 H 0.0445 -0.4934 0.1148 0.057 Uiso 1 1 calc R . . . .
C9 C 0.2945(7) -0.5553(5) 0.1339(6) 0.0611(16) Uani 1 1 d . . . . .
H9A H 0.3211 -0.6274 0.0850 0.073 Uiso 1 1 calc R . . . .
H9B H 0.2485 -0.5732 0.1820 0.073 Uiso 1 1 calc R . . . .
C10 C 0.3986(6) -0.4643(5) 0.2130(5) 0.0574(16) Uani 1 1 d . . . . .
H10A H 0.3725 -0.3953 0.2683 0.069 Uiso 1 1 calc R . . . .
H10B H 0.4445 -0.4963 0.2575 0.069 Uiso 1 1 calc R . . . .
C11 C 0.5455(5) -0.2652(5) 0.1484(4) 0.0461(12) Uani 1 1 d . . . . .
H11 H 0.6105 -0.3024 0.1441 0.055 Uiso 1 1 calc R . . . .
C12 C 0.5581(5) -0.1538(5) 0.1446(4) 0.0425(11) Uani 1 1 d . . . . .
C13 C 0.4754(4) -0.0780(5) 0.1658(4) 0.0370(10) Uani 1 1 d . . . . .
C14 C 0.5000(5) 0.0296(5) 0.1613(4) 0.0445(12) Uani 1 1 d . . . . .
C15 C 0.6028(5) 0.0610(6) 0.1372(5) 0.0534(15) Uani 1 1 d . . . . .
H15 H 0.6170 0.1315 0.1328 0.064 Uiso 1 1 calc R . . . .
C16 C 0.6856(6) -0.0130(7) 0.1194(5) 0.0632(18) Uani 1 1 d . . . . .
H16 H 0.7563 0.0090 0.1051 0.076 Uiso 1 1 calc R . . . .
C17 C 0.6635(5) -0.1177(6) 0.1227(5) 0.0548(15) Uani 1 1 d . . . . .
H17 H 0.7197 -0.1666 0.1102 0.066 Uiso 1 1 calc R . . . .
C18 C 0.4351(7) 0.2127(6) 0.1944(7) 0.0708(19) Uani 1 1 d . . . . .
H18A H 0.3726 0.2545 0.2201 0.106 Uiso 1 1 calc GR . . . .
H18B H 0.4421 0.2068 0.1193 0.106 Uiso 1 1 calc GR . . . .
H18C H 0.5063 0.2546 0.2502 0.106 Uiso 1 1 calc GR . . . .
C19 C 0.3144(5) -0.3941(4) -0.0982(4) 0.0393(10) Uani 1 1 d . . . . .
H19 H 0.3709 -0.4261 -0.0685 0.047 Uiso 1 1 calc R . . . .
C20 C 0.2897(5) -0.4298(4) -0.2178(4) 0.0395(11) Uani 1 1 d . . . . .
H20 H 0.3289 -0.4854 -0.2666 0.047 Uiso 1 1 calc R . . . .
C21 C 0.2064(4) -0.3829(4) -0.2651(4) 0.0367(10) Uani 1 1 d . . . . .
C22 C 0.1508(5) -0.3017(5) -0.1867(4) 0.0439(12) Uani 1 1 d . . . . .
H22 H 0.0945 -0.2675 -0.2138 0.053 Uiso 1 1 calc R . . . .
C23 C 0.1783(5) -0.2715(5) -0.0693(4) 0.0427(11) Uani 1 1 d . . . . .
H23 H 0.1384 -0.2182 -0.0189 0.051 Uiso 1 1 calc R . . . .
C24 C 0.1796(5) -0.4160(4) -0.3914(4) 0.0413(11) Uani 1 1 d . . . . .
C25 C 0.1624(6) -0.5318(5) -0.4757(5) 0.0495(13) Uani 1 1 d . . . . .
H25 H 0.1665 -0.5925 -0.4544 0.059 Uiso 1 1 calc R . . . .
C26 C 0.1387(6) -0.5569(5) -0.5932(5) 0.0607(16) Uani 1 1 d . . . . .
H26 H 0.1285 -0.6357 -0.6489 0.073 Uiso 1 1 calc R . . . .
C27 C 0.1476(7) -0.3648(6) -0.5480(6) 0.071(2) Uani 1 1 d . . . . .
H27 H 0.1425 -0.3058 -0.5716 0.085 Uiso 1 1 calc R . . . .
C28 C 0.1728(6) -0.3314(5) -0.4307(5) 0.0553(15) Uani 1 1 d . . . . .
H28 H 0.1855 -0.2517 -0.3771 0.066 Uiso 1 1 calc R . . . .
C29 C 0.3243(5) -0.1113(5) 0.4241(4) 0.0419(11) Uani 1 1 d . . . . .
C30 C 0.3627(7) -0.0953(6) 0.5461(5) 0.0630(17) Uani 1 1 d . . . . .
H30A H 0.4319 -0.0372 0.5843 0.094 Uiso 1 1 calc GR . . . .
H30B H 0.3783 -0.1692 0.5433 0.094 Uiso 1 1 calc GR . . . .
H30C H 0.3025 -0.0693 0.5892 0.094 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Ni1 3.3990(8) . ?
Dy1 O1 2.474(4) . ?
Dy1 O2 2.332(3) . ?
Dy1 O14 2.246(4) . ?
Dy1 O5 2.283(3) . ?
Dy1 O6 2.626(4) . ?
Dy1 O7 2.454(4) . ?
Dy1 O8 2.475(4) . ?
Dy1 O10 2.460(4) . ?
Dy1 O11 2.414(4) . ?
Dy1 N5 2.877(5) . ?
Dy1 N6 2.881(5) . ?
Ni1 O2 2.039(3) . ?
Ni1 O13 2.081(3) . ?
Ni1 O5 2.011(3) . ?
Ni1 N1 2.015(4) . ?
Ni1 N2 2.068(4) . ?
Ni1 N3 2.153(4) . ?
O1 C1 1.444(7) . ?
O1 C2 1.383(7) . ?
O2 C3 1.327(6) . ?
O14 C29 1.260(7) . ?
O3 N1 1.432(6) . ?
O3 C9 1.440(8) . ?
O13 C29 1.241(6) . ?
O4 N2 1.415(5) . ?
O4 C10 1.419(8) . ?
O5 C13 1.330(6) . ?
O6 C14 1.386(7) . ?
O6 C18 1.430(7) . ?
O7 N5 1.269(6) . ?
O8 N5 1.256(6) . ?
O9 N5 1.216(6) . ?
O10 N6 1.262(7) . ?
O11 N6 1.283(7) . ?
O12 N6 1.215(7) . ?
N1 C8 1.270(8) . ?
N2 C11 1.288(7) . ?
N3 C19 1.333(6) . ?
N3 C23 1.343(7) . ?
N4 C26 1.315(9) . ?
N4 C27 1.339(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.411(8) . ?
C2 C7 1.389(8) . ?
C3 C4 1.413(8) . ?
C4 C5 1.395(8) . ?
C4 C8 1.437(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.383(12) . ?
C6 H6 0.9300 . ?
C6 C7 1.398(12) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.503(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11 0.9300 . ?
C11 C12 1.439(8) . ?
C12 C13 1.401(8) . ?
C12 C17 1.404(8) . ?
C13 C14 1.407(8) . ?
C14 C15 1.369(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.387(10) . ?
C16 H16 0.9300 . ?
C16 C17 1.359(10) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19 0.9300 . ?
C19 C20 1.386(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.391(7) . ?
C21 C22 1.388(7) . ?
C21 C24 1.475(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.374(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.374(7) . ?
C24 C28 1.383(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.390(8) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C27 C28 1.363(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.495(7) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

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 Dy1 Ni1 98.80(10) . . ?
O1 Dy1 O6 154.69(14) . . ?
O1 Dy1 O8 70.57(14) . . ?
O1 Dy1 N5 95.92(14) . . ?
O1 Dy1 N6 82.76(15) . . ?
O2 Dy1 Ni1 35.96(8) . . ?
O2 Dy1 O1 64.57(12) . . ?
O2 Dy1 O6 122.87(11) . . ?
O2 Dy1 O7 152.44(15) . . ?
O2 Dy1 O8 127.85(13) . . ?
O2 Dy1 O10 79.42(12) . . ?
O2 Dy1 O11 121.04(15) . . ?
O2 Dy1 N5 143.66(13) . . ?
O2 Dy1 N6 101.15(14) . . ?
O14 Dy1 Ni1 69.12(10) . . ?
O14 Dy1 O1 84.16(16) . . ?
O14 Dy1 O2 77.64(13) . . ?
O14 Dy1 O5 81.17(14) . . ?
O14 Dy1 O6 120.46(16) . . ?
O14 Dy1 O7 76.65(16) . . ?
O14 Dy1 O8 72.59(14) . . ?
O14 Dy1 O10 157.06(14) . . ?
O14 Dy1 O11 144.56(15) . . ?
O14 Dy1 N5 69.74(14) . . ?
O14 Dy1 N6 165.97(17) . . ?
O5 Dy1 Ni1 34.94(8) . . ?
O5 Dy1 O1 133.55(12) . . ?
O5 Dy1 O2 69.29(11) . . ?
O5 Dy1 O6 62.32(12) . . ?
O5 Dy1 O7 97.00(13) . . ?
O5 Dy1 O8 142.42(13) . . ?
O5 Dy1 O10 90.98(13) . . ?
O5 Dy1 O11 132.15(15) . . ?
O5 Dy1 N5 119.18(14) . . ?
O5 Dy1 N6 111.70(14) . . ?
O6 Dy1 Ni1 95.93(8) . . ?
O6 Dy1 N5 88.25(14) . . ?
O6 Dy1 N6 72.15(14) . . ?
O7 Dy1 Ni1 122.89(11) . . ?
O7 Dy1 O1 121.92(13) . . ?
O7 Dy1 O6 64.31(13) . . ?
O7 Dy1 O8 51.44(14) . . ?
O7 Dy1 O10 125.93(16) . . ?
O7 Dy1 N5 26.04(14) . . ?
O7 Dy1 N6 106.20(17) . . ?
O8 Dy1 Ni1 141.13(10) . . ?
O8 Dy1 O6 109.10(13) . . ?
O8 Dy1 N5 25.77(14) . . ?
O8 Dy1 N6 98.15(15) . . ?
O10 Dy1 Ni1 92.17(9) . . ?
O10 Dy1 O1 85.84(14) . . ?
O10 Dy1 O6 73.10(13) . . ?
O10 Dy1 O8 122.91(14) . . ?
O10 Dy1 N5 131.98(14) . . ?
O10 Dy1 N6 25.83(14) . . ?
O11 Dy1 Ni1 144.10(11) . . ?
O11 Dy1 O1 79.08(17) . . ?
O11 Dy1 O6 76.91(16) . . ?
O11 Dy1 O7 86.08(17) . . ?
O11 Dy1 O8 72.44(15) . . ?
O11 Dy1 O10 51.98(14) . . ?
O11 Dy1 N5 81.13(15) . . ?
O11 Dy1 N6 26.19(15) . . ?
N5 Dy1 Ni1 134.33(10) . . ?
N5 Dy1 N6 106.58(15) . . ?
N6 Dy1 Ni1 118.00(11) . . ?
O2 Ni1 Dy1 42.18(9) . . ?
O2 Ni1 O13 87.59(14) . . ?
O2 Ni1 N2 169.17(16) . . ?
O2 Ni1 N3 92.51(15) . . ?
O13 Ni1 Dy1 79.45(10) . . ?
O13 Ni1 N3 178.66(16) . . ?
O5 Ni1 Dy1 40.55(9) . . ?
O5 Ni1 O2 80.76(13) . . ?
O5 Ni1 O13 91.30(15) . . ?
O5 Ni1 N1 169.99(17) . . ?
O5 Ni1 N2 89.21(16) . . ?
O5 Ni1 N3 90.04(15) . . ?
N1 Ni1 Dy1 130.82(14) . . ?
N1 Ni1 O2 89.71(17) . . ?
N1 Ni1 O13 91.34(16) . . ?
N1 Ni1 N2 100.51(19) . . ?
N1 Ni1 N3 87.32(16) . . ?
N2 Ni1 Dy1 127.06(13) . . ?
N2 Ni1 O13 88.57(16) . . ?
N2 Ni1 N3 91.57(16) . . ?
N3 Ni1 Dy1 101.51(11) . . ?
C1 O1 Dy1 124.9(4) . . ?
C2 O1 Dy1 117.3(3) . . ?
C2 O1 C1 116.9(5) . . ?
Ni1 O2 Dy1 101.86(14) . . ?
C3 O2 Dy1 122.1(3) . . ?
C3 O2 Ni1 122.2(3) . . ?
C29 O14 Dy1 136.6(3) . . ?
N1 O3 C9 110.7(4) . . ?
C29 O13 Ni1 129.5(4) . . ?
N2 O4 C10 112.2(4) . . ?
Ni1 O5 Dy1 104.50(14) . . ?
C13 O5 Dy1 128.9(3) . . ?
C13 O5 Ni1 126.6(3) . . ?
C14 O6 Dy1 116.1(3) . . ?
C14 O6 C18 116.4(5) . . ?
C18 O6 Dy1 124.9(4) . . ?
N5 O7 Dy1 95.9(3) . . ?
N5 O8 Dy1 95.3(3) . . ?
N6 O10 Dy1 96.0(3) . . ?
N6 O11 Dy1 97.7(3) . . ?
O3 N1 Ni1 119.0(4) . . ?
C8 N1 Ni1 127.5(4) . . ?
C8 N1 O3 112.6(4) . . ?
O4 N2 Ni1 123.7(4) . . ?
C11 N2 Ni1 125.3(4) . . ?
C11 N2 O4 110.7(4) . . ?
C19 N3 Ni1 123.9(3) . . ?
C19 N3 C23 117.5(4) . . ?
C23 N3 Ni1 118.6(3) . . ?
C26 N4 C27 115.5(5) . . ?
O7 N5 Dy1 58.0(3) . . ?
O8 N5 Dy1 59.0(3) . . ?
O8 N5 O7 115.8(5) . . ?
O9 N5 Dy1 169.3(5) . . ?
O9 N5 O7 122.1(5) . . ?
O9 N5 O8 122.1(5) . . ?
O10 N6 Dy1 58.1(3) . . ?
O10 N6 O11 114.1(5) . . ?
O11 N6 Dy1 56.1(3) . . ?
O12 N6 Dy1 175.5(5) . . ?
O12 N6 O10 122.9(6) . . ?
O12 N6 O11 122.9(6) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 113.1(4) . . ?
O1 C2 C7 125.2(6) . . ?
C7 C2 C3 121.6(6) . . ?
O2 C3 C2 117.5(5) . . ?
O2 C3 C4 124.8(5) . . ?
C2 C3 C4 117.7(5) . . ?
C3 C4 C8 124.1(5) . . ?
C5 C4 C3 120.6(6) . . ?
C5 C4 C8 115.2(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.2(7) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.6(6) . . ?
C7 C6 H6 119.7 . . ?
C2 C7 C6 119.2(7) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
N1 C8 C4 124.3(5) . . ?
N1 C8 H8 117.8 . . ?
C4 C8 H8 117.8 . . ?
O3 C9 H9A 108.6 . . ?
O3 C9 H9B 108.6 . . ?
O3 C9 C10 114.6(5) . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
O4 C10 C9 112.8(5) . . ?
O4 C10 H10A 109.0 . . ?
O4 C10 H10B 109.0 . . ?
C9 C10 H10A 109.0 . . ?
C9 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
N2 C11 H11 117.0 . . ?
N2 C11 C12 126.1(5) . . ?
C12 C11 H11 117.0 . . ?
C13 C12 C11 124.8(5) . . ?
C13 C12 C17 118.5(5) . . ?
C17 C12 C11 116.7(5) . . ?
O5 C13 C12 124.0(5) . . ?
O5 C13 C14 117.1(5) . . ?
C12 C13 C14 118.8(5) . . ?
O6 C14 C13 113.0(5) . . ?
C15 C14 O6 125.8(5) . . ?
C15 C14 C13 121.2(6) . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.7(6) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.1(6) . . ?
C17 C16 H16 119.9 . . ?
C12 C17 H17 119.2 . . ?
C16 C17 C12 121.6(6) . . ?
C16 C17 H17 119.2 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19 118.7 . . ?
N3 C19 C20 122.6(5) . . ?
C20 C19 H19 118.7 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.2(4) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 C24 122.0(4) . . ?
C22 C21 C20 116.4(4) . . ?
C22 C21 C24 121.6(5) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 C21 120.4(5) . . ?
C23 C22 H22 119.8 . . ?
N3 C23 C22 122.8(5) . . ?
N3 C23 H23 118.6 . . ?
C22 C23 H23 118.6 . . ?
C25 C24 C21 121.9(5) . . ?
C25 C24 C28 116.7(5) . . ?
C28 C24 C21 121.4(5) . . ?
C24 C25 H25 120.5 . . ?
C24 C25 C26 119.0(5) . . ?
C26 C25 H25 120.5 . . ?
N4 C26 C25 124.7(5) . . ?
N4 C26 H26 117.7 . . ?
C25 C26 H26 117.7 . . ?
N4 C27 H27 118.0 . . ?
N4 C27 C28 124.1(6) . . ?
C28 C27 H27 118.0 . . ?
C24 C28 H28 120.0 . . ?
C27 C28 C24 120.1(6) . . ?
C27 C28 H28 120.0 . . ?
O14 C29 C30 116.6(5) . . ?
O13 C29 O14 125.0(5) . . ?
O13 C29 C30 118.4(5) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C2 C3 -16.4(6) . . . . ?
Dy1 O1 C2 C7 162.4(5) . . . . ?
Dy1 O2 C3 C2 19.6(6) . . . . ?
Dy1 O2 C3 C4 -160.3(4) . . . . ?
Dy1 O14 C29 O13 -7.2(10) . . . . ?
Dy1 O14 C29 C30 171.9(5) . . . . ?
Dy1 O5 C13 C12 164.6(3) . . . . ?
Dy1 O5 C13 C14 -14.8(6) . . . . ?
Dy1 O6 C14 C13 11.1(5) . . . . ?
Dy1 O6 C14 C15 -168.1(4) . . . . ?
Dy1 O7 N5 O8 -12.4(5) . . . . ?
Dy1 O7 N5 O9 167.3(6) . . . . ?
Dy1 O8 N5 O7 12.2(5) . . . . ?
Dy1 O8 N5 O9 -167.4(6) . . . . ?
Dy1 O10 N6 O11 -4.2(6) . . . . ?
Dy1 O10 N6 O12 174.8(6) . . . . ?
Dy1 O11 N6 O10 4.3(6) . . . . ?
Dy1 O11 N6 O12 -174.7(6) . . . . ?
Ni1 O2 C3 C2 152.6(4) . . . . ?
Ni1 O2 C3 C4 -27.3(6) . . . . ?
Ni1 O13 C29 O14 6.0(9) . . . . ?
Ni1 O13 C29 C30 -173.1(4) . . . . ?
Ni1 O5 C13 C12 -18.5(7) . . . . ?
Ni1 O5 C13 C14 162.1(3) . . . . ?
Ni1 N1 C8 C4 -5.9(8) . . . . ?
Ni1 N2 C11 C12 2.6(7) . . . . ?
Ni1 N3 C19 C20 179.1(4) . . . . ?
Ni1 N3 C23 C22 179.8(4) . . . . ?
O1 C2 C3 O2 -0.8(6) . . . . ?
O1 C2 C3 C4 179.1(4) . . . . ?
O1 C2 C7 C6 178.8(6) . . . . ?
O2 C3 C4 C5 -178.0(5) . . . . ?
O2 C3 C4 C8 2.6(8) . . . . ?
O3 N1 C8 C4 -175.0(5) . . . . ?
O3 C9 C10 O4 -56.4(7) . . . . ?
O4 N2 C11 C12 176.1(5) . . . . ?
O5 C13 C14 O6 0.0(6) . . . . ?
O5 C13 C14 C15 179.3(5) . . . . ?
O6 C14 C15 C16 177.7(5) . . . . ?
N1 O3 C9 C10 -52.7(7) . . . . ?
N2 O4 C10 C9 102.5(5) . . . . ?
N2 C11 C12 C13 9.0(8) . . . . ?
N2 C11 C12 C17 -173.8(5) . . . . ?
N3 C19 C20 C21 0.6(8) . . . . ?
N4 C27 C28 C24 -1.0(13) . . . . ?
C1 O1 C2 C3 173.9(5) . . . . ?
C1 O1 C2 C7 -7.3(8) . . . . ?
C2 C3 C4 C5 2.0(8) . . . . ?
C2 C3 C4 C8 -177.4(5) . . . . ?
C3 C2 C7 C6 -2.5(9) . . . . ?
C3 C4 C5 C6 -2.1(9) . . . . ?
C3 C4 C8 N1 16.1(8) . . . . ?
C4 C5 C6 C7 -0.1(11) . . . . ?
C5 C4 C8 N1 -163.3(5) . . . . ?
C5 C6 C7 C2 2.4(11) . . . . ?
C7 C2 C3 O2 -179.6(5) . . . . ?
C7 C2 C3 C4 0.3(8) . . . . ?
C8 C4 C5 C6 177.3(6) . . . . ?
C9 O3 N1 Ni1 86.8(5) . . . . ?
C9 O3 N1 C8 -103.1(6) . . . . ?
C10 O4 N2 Ni1 -34.6(6) . . . . ?
C10 O4 N2 C11 151.7(5) . . . . ?
C11 C12 C13 O5 -0.7(8) . . . . ?
C11 C12 C13 C14 178.8(5) . . . . ?
C11 C12 C17 C16 -178.8(5) . . . . ?
C12 C13 C14 O6 -179.5(4) . . . . ?
C12 C13 C14 C15 -0.2(7) . . . . ?
C13 C12 C17 C16 -1.4(8) . . . . ?
C13 C14 C15 C16 -1.5(8) . . . . ?
C14 C15 C16 C17 1.8(9) . . . . ?
C15 C16 C17 C12 -0.3(9) . . . . ?
C17 C12 C13 O5 -177.8(4) . . . . ?
C17 C12 C13 C14 1.6(7) . . . . ?
C18 O6 C14 C13 173.6(5) . . . . ?
C18 O6 C14 C15 -5.6(8) . . . . ?
C19 N3 C23 C22 -1.6(8) . . . . ?
C19 C20 C21 C22 -0.8(8) . . . . ?
C19 C20 C21 C24 178.3(5) . . . . ?
C20 C21 C22 C23 -0.1(8) . . . . ?
C20 C21 C24 C25 46.5(8) . . . . ?
C20 C21 C24 C28 -132.1(6) . . . . ?
C21 C22 C23 N3 1.4(9) . . . . ?
C21 C24 C25 C26 -179.2(6) . . . . ?
C21 C24 C28 C27 -179.9(6) . . . . ?
C22 C21 C24 C25 -134.3(6) . . . . ?
C22 C21 C24 C28 47.0(8) . . . . ?
C23 N3 C19 C20 0.6(8) . . . . ?
C24 C21 C22 C23 -179.3(5) . . . . ?
C24 C25 C26 N4 -1.0(11) . . . . ?
C25 C24 C28 C27 1.4(10) . . . . ?
C26 N4 C27 C28 -0.4(12) . . . . ?
C27 N4 C26 C25 1.4(11) . . . . ?
C28 C24 C25 C26 -0.5(9) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.500 0.500 69.5 16.9 ?

_olex2_date_sample_data_collection 2015-08-27
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_d655_2
_database_code_depnum_ccdc_archive 'CCDC 1434587'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_audit_creation_date             2015-10-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;

_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C52 H62 La2 N10 Ni2 O32'
_chemical_formula_sum            'C52 H62 La2 N10 Ni2 O32'
_chemical_formula_weight         1734.35
_chemical_melting_point          ?
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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.3389(3)
_cell_length_b                   13.0476(4)
_cell_length_c                   17.2529(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.2166(18)
_cell_angle_gamma                90
_cell_volume                     3425.58(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4817
_cell_measurement_temperature    293.42(10)
_cell_measurement_theta_max      27.4780
_cell_measurement_theta_min      3.5410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.857
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14180
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.352
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.42(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -16.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  120.0000 32

#__ type_ start__ end____ width___ exp.time_
  2 omega  -26.00   18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000  120.0000 44

#__ type_ start__ end____ width___ exp.time_
  3 omega   14.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   38.0000  -90.0000 79

#__ type_ start__ end____ width___ exp.time_
  4 omega   42.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000  150.0000 53

#__ type_ start__ end____ width___ exp.time_
  5 omega  -45.00  -13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000 -180.0000 32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0152966000
_diffrn_orient_matrix_UB_12      0.0009268000
_diffrn_orient_matrix_UB_13      -0.0405257000
_diffrn_orient_matrix_UB_21      -0.0112060000
_diffrn_orient_matrix_UB_22      -0.0526268000
_diffrn_orient_matrix_UB_23      0.0014652000
_diffrn_orient_matrix_UB_31      -0.0426260000
_diffrn_orient_matrix_UB_32      0.0134756000
_diffrn_orient_matrix_UB_33      0.0084611000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5138
_reflns_number_total             6714
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6714
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0414
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0232P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0904
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O13-H13
 0.85 with sigma of 0.01
 C23-H13
 1.898803 with sigma of 0.02
 Ni1-H13
 2.671219 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C21(H21), C8(H8), C7(H7), C22(H22), C26(H26), C11(H11),
 C5(H5), C13(H13A), C15(H15)
3.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C1(H1A,H1B,H1C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.67886(2) 0.04995(2) 0.67800(2) 0.03460(10) Uani 1 1 d . . . . .
Ni1 Ni 0.87096(3) 0.16963(5) 0.76468(3) 0.03175(15) Uani 1 1 d D . . . .
O3 O 0.97320(18) 0.3538(3) 0.82336(17) 0.0512(9) Uani 1 1 d . . . . .
O4 O 1.06337(18) 0.1535(3) 0.8464(2) 0.0644(11) Uani 1 1 d . . . . .
O15 O 0.5679(3) 0.2464(5) 0.8434(3) 0.132(2) Uani 1 1 d . . . . .
C6 C 0.7224(4) 0.4555(5) 0.5424(4) 0.0718(18) Uani 1 1 d . . . . .
H6 H 0.7133 0.5094 0.5071 0.086 Uiso 1 1 calc R . . . .
O12 O 0.5257(2) -0.0059(3) 0.6752(2) 0.0693(12) Uani 1 1 d . . . . .
O9 O 0.6302(2) -0.0254(4) 0.5389(2) 0.0771(14) Uani 1 1 d . . . . .
C23 C 0.8485(3) 0.2457(5) 0.9418(3) 0.0746(19) Uani 1 1 d D . . . .
H23A H 0.9044 0.2770 0.9381 0.112 Uiso 1 1 calc GR . . . .
H23B H 0.8560 0.1894 0.9778 0.112 Uiso 1 1 calc GR . . . .
H23C H 0.8094 0.2953 0.9599 0.112 Uiso 1 1 calc GR . . . .
N1 N 0.9110(2) 0.3177(3) 0.7609(2) 0.0384(9) Uani 1 1 d . . . . .
O5 O 0.81056(16) 0.0321(2) 0.77267(16) 0.0352(7) Uani 1 1 d . . . . .
O7 O 0.92369(16) 0.1277(3) 0.66691(16) 0.0399(8) Uani 1 1 d . . . . .
C20 C 0.9457(2) 0.0371(3) 0.5530(2) 0.0298(10) Uani 1 1 d . . . . .
O11 O 0.6638(3) -0.1736(5) 0.4978(3) 0.148(3) Uani 1 1 d . . . . .
O8 O 0.80806(16) 0.0464(3) 0.60205(16) 0.0423(8) Uani 1 1 d . . . . .
C14 C 0.8481(4) -0.1831(5) 0.9485(3) 0.0706(16) Uani 1 1 d . . . . .
H14 H 0.8555 -0.2316 0.9883 0.085 Uiso 1 1 calc R . . . .
O1 O 0.63696(18) 0.1973(3) 0.57790(16) 0.0484(9) Uani 1 1 d . . . . .
O2 O 0.75874(15) 0.2136(2) 0.69876(15) 0.0346(7) Uani 1 1 d . . . . .
O6 O 0.68659(19) -0.1012(3) 0.78470(19) 0.0525(9) Uani 1 1 d . . . . .
C21 C 1.0329(2) 0.0670(4) 0.5582(2) 0.0391(11) Uani 1 1 d . . . . .
H21 H 1.0560 0.1111 0.5979 0.047 Uiso 1 1 calc R . . . .
N2 N 0.9783(2) 0.1079(3) 0.8339(2) 0.0429(10) Uani 1 1 d . . . . .
C8 C 0.8755(3) 0.3905(4) 0.7201(3) 0.0447(12) Uani 1 1 d . . . . .
H8 H 0.8969 0.4563 0.7312 0.054 Uiso 1 1 calc R . . . .
C7 C 0.6710(3) 0.3680(5) 0.5328(3) 0.0627(16) Uani 1 1 d . . . . .
H7 H 0.6267 0.3634 0.4909 0.075 Uiso 1 1 calc R . . . .
C12 C 0.9030(3) -0.0384(4) 0.8824(3) 0.0419(11) Uani 1 1 d . . . . .
C17 C 0.8246(3) -0.0338(4) 0.8307(2) 0.0380(11) Uani 1 1 d . . . . .
N5 N 0.3835(3) -0.0099(5) 0.6937(3) 0.0796(16) Uani 1 1 d . . . . .
C22 C 0.9142(3) -0.0314(4) 0.4953(2) 0.0388(11) Uani 1 1 d . . . . .
H22 H 0.8564 -0.0541 0.4924 0.047 Uiso 1 1 calc R . . . .
C26 C 0.4483(4) -0.0085(5) 0.6524(3) 0.0761(19) Uani 1 1 d . . . . .
H26 H 0.4333 -0.0097 0.5985 0.091 Uiso 1 1 calc R . . . .
C18 C 0.6231(4) -0.1817(5) 0.7843(4) 0.102(3) Uani 1 1 d . . . . .
H18A H 0.5792 -0.1738 0.7399 0.152 Uiso 1 1 calc GR . . . .
H18B H 0.5957 -0.1784 0.8313 0.152 Uiso 1 1 calc GR . . . .
H18C H 0.6517 -0.2468 0.7815 0.152 Uiso 1 1 calc GR . . . .
C11 C 0.9764(3) 0.0292(4) 0.8771(3) 0.0463(12) Uani 1 1 d . . . . .
H11 H 1.0282 0.0135 0.9089 0.056 Uiso 1 1 calc R . . . .
O14 O 0.56821(19) 0.2004(3) 0.72421(19) 0.0606(10) Uani 1 1 d . . . . .
O10 O 0.6952(2) -0.1346(4) 0.6205(3) 0.0803(13) Uani 1 1 d . . . . .
N3 N 0.6633(3) -0.1130(6) 0.5512(4) 0.084(2) Uani 1 1 d . . . . .
O13 O 0.81275(17) 0.2096(3) 0.86801(17) 0.0518(9) Uani 1 1 d D . . . .
H13 H 0.7634(16) 0.181(3) 0.8720(15) 0.078 Uiso 1 1 d DR . . . .
O16 O 0.64694(18) 0.1195(3) 0.81714(17) 0.0506(9) Uani 1 1 d . . . . .
C5 C 0.7862(3) 0.4613(4) 0.6043(3) 0.0603(15) Uani 1 1 d . . . . .
H5 H 0.8191 0.5211 0.6121 0.072 Uiso 1 1 calc R . . . .
C1 C 0.5508(3) 0.2003(5) 0.5327(3) 0.079(2) Uani 1 1 d . . . . .
H1A H 0.5224 0.1351 0.5361 0.118 Uiso 1 1 calc GR . . . .
H1B H 0.5567 0.2149 0.4791 0.118 Uiso 1 1 calc GR . . . .
H1C H 0.5161 0.2528 0.5530 0.118 Uiso 1 1 calc GR . . . .
C13 C 0.9130(3) -0.1150(5) 0.9394(3) 0.0613(15) Uani 1 1 d . . . . .
H13A H 0.9658 -0.1195 0.9722 0.074 Uiso 1 1 calc R . . . .
C4 C 0.8039(3) 0.3794(4) 0.6573(3) 0.0442(12) Uani 1 1 d . . . . .
N4 N 0.5931(2) 0.1903(4) 0.7953(2) 0.0564(12) Uani 1 1 d . . . . .
C2 C 0.6848(3) 0.2877(4) 0.5845(3) 0.0448(12) Uani 1 1 d . . . . .
C15 C 0.7706(3) -0.1793(4) 0.8975(3) 0.0595(14) Uani 1 1 d . . . . .
H15 H 0.7257 -0.2257 0.9030 0.071 Uiso 1 1 calc R . . . .
C19 C 0.8873(3) 0.0735(4) 0.6120(2) 0.0338(10) Uani 1 1 d . . . . .
C16 C 0.7600(3) -0.1090(4) 0.8401(3) 0.0453(12) Uani 1 1 d . . . . .
C10 C 1.0791(3) 0.2244(5) 0.7867(3) 0.0594(16) Uani 1 1 d . . . . .
H10A H 1.0419 0.2070 0.7388 0.071 Uiso 1 1 calc R . . . .
H10B H 1.1398 0.2187 0.7769 0.071 Uiso 1 1 calc R . . . .
C9 C 1.0612(3) 0.3316(4) 0.8086(3) 0.0553(15) Uani 1 1 d . . . . .
H9A H 1.1008 0.3489 0.8551 0.066 Uiso 1 1 calc R . . . .
H9B H 1.0753 0.3763 0.7669 0.066 Uiso 1 1 calc R . . . .
C3 C 0.7510(3) 0.2907(4) 0.6493(2) 0.0373(11) Uani 1 1 d . . . . .
C24 C 0.4041(5) -0.0045(8) 0.7790(4) 0.141(4) Uani 1 1 d . . . . .
H24A H 0.3918 -0.0695 0.8014 0.211 Uiso 1 1 calc GR . . . .
H24B H 0.3688 0.0476 0.7990 0.211 Uiso 1 1 calc GR . . . .
H24C H 0.4652 0.0118 0.7925 0.211 Uiso 1 1 calc GR . . . .
C25 C 0.2922(4) -0.0209(8) 0.6602(5) 0.158(4) Uani 1 1 d . . . . .
H25A H 0.2600 0.0392 0.6716 0.237 Uiso 1 1 calc GR . . . .
H25B H 0.2673 -0.0800 0.6822 0.237 Uiso 1 1 calc GR . . . .
H25C H 0.2891 -0.0290 0.6046 0.237 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 Ni1 3.5000(5) . ?
La1 O12 2.454(3) . ?
La1 O9 2.615(4) . ?
La1 O5 2.444(2) . ?
La1 O8 2.510(3) . ?
La1 O1 2.610(3) . ?
La1 O2 2.466(3) . ?
La1 O6 2.690(3) . ?
La1 O14 2.777(3) . ?
La1 O10 2.628(4) . ?
La1 N3 3.038(5) . ?
La1 O16 2.668(3) . ?
Ni1 N1 2.031(4) . ?
Ni1 O5 2.032(3) . ?
Ni1 O7 2.035(3) . ?
Ni1 O2 2.023(3) . ?
Ni1 N2 2.071(4) . ?
Ni1 O13 2.156(3) . ?
O3 N1 1.426(4) . ?
O3 C9 1.434(5) . ?
O4 N2 1.425(4) . ?
O4 C10 1.426(6) . ?
O15 N4 1.207(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.386(8) . ?
C6 C5 1.356(7) . ?
O12 C26 1.203(5) . ?
O9 N3 1.257(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C23 O13 1.402(5) . ?
N1 C8 1.265(6) . ?
O5 C17 1.317(5) . ?
O7 C19 1.255(5) . ?
C20 C21 1.385(5) . ?
C20 C22 1.379(6) . ?
C20 C19 1.515(5) . ?
O11 N3 1.215(6) . ?
O8 C19 1.257(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.359(7) . ?
C14 C15 1.388(7) . ?
O1 C1 1.448(5) . ?
O1 C2 1.387(6) . ?
O2 C3 1.315(5) . ?
O6 C18 1.432(6) . ?
O6 C16 1.386(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.384(5) 3_756 ?
N2 C11 1.272(6) . ?
C8 H8 0.9300 . ?
C8 C4 1.449(6) . ?
C7 H7 0.9300 . ?
C7 C2 1.375(7) . ?
C12 C17 1.405(5) . ?
C12 C11 1.443(7) . ?
C12 C13 1.398(7) . ?
C17 C16 1.418(6) . ?
N5 C26 1.295(6) . ?
N5 C24 1.467(8) . ?
N5 C25 1.454(7) . ?
C22 C21 1.384(5) 3_756 ?
C22 H22 0.9300 . ?
C26 H26 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C11 H11 0.9300 . ?
O14 N4 1.244(5) . ?
O10 N3 1.266(7) . ?
O13 H13 0.853(9) . ?
O16 N4 1.265(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.411(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C13 H13A 0.9300 . ?
C4 C3 1.410(6) . ?
C2 C3 1.413(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.345(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.484(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?

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
O12 La1 Ni1 153.30(9) . . ?
O12 La1 O9 73.02(12) . . ?
O12 La1 O8 143.20(11) . . ?
O12 La1 O1 92.88(11) . . ?
O12 La1 O2 135.82(12) . . ?
O12 La1 O6 75.86(11) . . ?
O12 La1 O14 66.28(12) . . ?
O12 La1 O10 81.76(13) . . ?
O12 La1 N3 77.84(13) . . ?
O12 La1 O16 80.53(11) . . ?
O9 La1 Ni1 133.47(9) . . ?
O9 La1 O6 109.60(14) . . ?
O9 La1 O14 114.54(12) . . ?
O9 La1 O10 48.60(14) . . ?
O9 La1 N3 24.25(15) . . ?
O9 La1 O16 152.91(10) . . ?
O5 La1 Ni1 34.52(7) . . ?
O5 La1 O12 133.93(11) . . ?
O5 La1 O9 133.98(12) . . ?
O5 La1 O8 72.93(9) . . ?
O5 La1 O1 128.78(9) . . ?
O5 La1 O2 68.37(10) . . ?
O5 La1 O6 60.75(9) . . ?
O5 La1 O14 111.04(9) . . ?
O5 La1 O10 93.16(12) . . ?
O5 La1 N3 113.47(14) . . ?
O5 La1 O16 70.18(9) . . ?
O8 La1 Ni1 63.49(6) . . ?
O8 La1 O9 70.54(10) . . ?
O8 La1 O1 79.22(10) . . ?
O8 La1 O6 111.96(10) . . ?
O8 La1 O14 135.57(11) . . ?
O8 La1 O10 70.56(11) . . ?
O8 La1 N3 66.86(11) . . ?
O8 La1 O16 136.23(9) . . ?
O1 La1 Ni1 94.49(7) . . ?
O1 La1 O9 69.59(14) . . ?
O1 La1 O6 168.17(9) . . ?
O1 La1 O14 63.94(10) . . ?
O1 La1 O10 116.89(13) . . ?
O1 La1 N3 92.77(17) . . ?
O1 La1 O16 106.69(11) . . ?
O2 La1 Ni1 34.43(6) . . ?
O2 La1 O9 122.57(13) . . ?
O2 La1 O8 71.41(9) . . ?
O2 La1 O1 62.28(9) . . ?
O2 La1 O6 123.86(9) . . ?
O2 La1 O14 69.91(10) . . ?
O2 La1 O10 141.18(10) . . ?
O2 La1 N3 134.69(13) . . ?
O2 La1 O16 73.68(10) . . ?
O6 La1 Ni1 94.15(6) . . ?
O6 La1 O14 107.33(10) . . ?
O6 La1 N3 88.42(18) . . ?
O14 La1 Ni1 94.24(7) . . ?
O14 La1 N3 134.90(13) . . ?
O10 La1 Ni1 117.06(9) . . ?
O10 La1 O6 65.69(13) . . ?
O10 La1 O14 147.87(11) . . ?
O10 La1 N3 24.47(15) . . ?
O10 La1 O16 133.46(13) . . ?
N3 La1 Ni1 127.27(9) . . ?
O16 La1 Ni1 72.77(6) . . ?
O16 La1 O6 68.34(11) . . ?
O16 La1 O14 46.65(9) . . ?
O16 La1 N3 151.51(15) . . ?
N1 Ni1 La1 130.75(10) . . ?
N1 Ni1 O5 169.94(12) . . ?
N1 Ni1 O7 94.33(13) . . ?
N1 Ni1 N2 99.57(15) . . ?
N1 Ni1 O13 87.42(14) . . ?
O5 Ni1 La1 42.98(7) . . ?
O5 Ni1 O7 92.92(12) . . ?
O5 Ni1 N2 87.36(14) . . ?
O5 Ni1 O13 85.29(13) . . ?
O7 Ni1 La1 85.81(8) . . ?
O7 Ni1 N2 90.18(13) . . ?
O7 Ni1 O13 178.20(13) . . ?
O2 Ni1 La1 43.55(9) . . ?
O2 Ni1 N1 87.24(13) . . ?
O2 Ni1 O5 85.73(11) . . ?
O2 Ni1 O7 90.51(11) . . ?
O2 Ni1 N2 173.09(15) . . ?
O2 Ni1 O13 89.13(11) . . ?
N2 Ni1 La1 129.68(12) . . ?
N2 Ni1 O13 89.96(13) . . ?
O13 Ni1 La1 92.72(8) . . ?
N1 O3 C9 110.7(3) . . ?
N2 O4 C10 113.3(3) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.9(5) . . ?
C26 O12 La1 156.6(4) . . ?
N3 O9 La1 97.1(3) . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O13 C23 H23A 109.5 . . ?
O13 C23 H23B 109.5 . . ?
O13 C23 H23C 109.5 . . ?
O3 N1 Ni1 117.8(3) . . ?
C8 N1 Ni1 128.4(3) . . ?
C8 N1 O3 111.9(4) . . ?
Ni1 O5 La1 102.49(12) . . ?
C17 O5 La1 127.8(3) . . ?
C17 O5 Ni1 126.6(3) . . ?
C19 O7 Ni1 126.3(2) . . ?
C21 C20 C19 121.0(4) . . ?
C22 C20 C21 118.6(4) . . ?
C22 C20 C19 120.3(3) . . ?
C19 O8 La1 137.5(2) . . ?
C13 C14 H14 120.5 . . ?
C13 C14 C15 119.0(5) . . ?
C15 C14 H14 120.5 . . ?
C1 O1 La1 120.5(3) . . ?
C2 O1 La1 119.2(2) . . ?
C2 O1 C1 117.3(4) . . ?
Ni1 O2 La1 102.02(12) . . ?
C3 O2 La1 124.5(2) . . ?
C3 O2 Ni1 125.6(2) . . ?
C18 O6 La1 124.3(3) . . ?
C16 O6 La1 119.2(3) . . ?
C16 O6 C18 116.3(4) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.3(4) 3_756 . ?
C22 C21 H21 119.9 3_756 . ?
O4 N2 Ni1 124.8(3) . . ?
C11 N2 Ni1 125.2(3) . . ?
C11 N2 O4 109.6(4) . . ?
N1 C8 H8 117.5 . . ?
N1 C8 C4 125.0(5) . . ?
C4 C8 H8 117.5 . . ?
C6 C7 H7 119.6 . . ?
C2 C7 C6 120.8(5) . . ?
C2 C7 H7 119.6 . . ?
C17 C12 C11 123.2(4) . . ?
C13 C12 C17 119.1(5) . . ?
C13 C12 C11 117.6(4) . . ?
O5 C17 C12 123.7(4) . . ?
O5 C17 C16 119.2(4) . . ?
C12 C17 C16 116.9(4) . . ?
C26 N5 C24 117.9(5) . . ?
C26 N5 C25 123.4(6) . . ?
C25 N5 C24 118.6(5) . . ?
C20 C22 C21 121.1(4) . 3_756 ?
C20 C22 H22 119.5 . . ?
C21 C22 H22 119.5 3_756 . ?
O12 C26 N5 127.9(6) . . ?
O12 C26 H26 116.0 . . ?
N5 C26 H26 116.0 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C11 C12 127.3(4) . . ?
N2 C11 H11 116.4 . . ?
C12 C11 H11 116.4 . . ?
N4 O14 La1 94.9(3) . . ?
N3 O10 La1 96.2(4) . . ?
O9 N3 La1 58.7(3) . . ?
O9 N3 O10 117.6(5) . . ?
O11 N3 La1 173.7(5) . . ?
O11 N3 O9 120.3(7) . . ?
O11 N3 O10 122.2(8) . . ?
O10 N3 La1 59.3(3) . . ?
Ni1 O13 H13 115.2(14) . . ?
C23 O13 Ni1 132.6(3) . . ?
C23 O13 H13 108.8(14) . . ?
N4 O16 La1 99.6(2) . . ?
C6 C5 H5 119.0 . . ?
C6 C5 C4 122.0(5) . . ?
C4 C5 H5 119.0 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C14 C13 C12 122.1(5) . . ?
C14 C13 H13A 118.9 . . ?
C12 C13 H13A 118.9 . . ?
C5 C4 C8 118.4(5) . . ?
C3 C4 C8 121.9(4) . . ?
C3 C4 C5 119.7(4) . . ?
O15 N4 O14 121.9(5) . . ?
O15 N4 O16 119.5(4) . . ?
O14 N4 O16 118.7(4) . . ?
O1 C2 C3 114.2(4) . . ?
C7 C2 O1 123.9(4) . . ?
C7 C2 C3 121.9(5) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.4(5) . . ?
C16 C15 H15 119.8 . . ?
O7 C19 C20 116.1(3) . . ?
O7 C19 O8 126.3(4) . . ?
O8 C19 C20 117.6(4) . . ?
O6 C16 C17 112.9(4) . . ?
C15 C16 O6 124.7(4) . . ?
C15 C16 C17 122.3(4) . . ?
O4 C10 H10A 109.2 . . ?
O4 C10 H10B 109.2 . . ?
O4 C10 C9 112.0(4) . . ?
H10A C10 H10B 107.9 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
O3 C9 C10 116.3(4) . . ?
O3 C9 H9A 108.2 . . ?
O3 C9 H9B 108.2 . . ?
C10 C9 H9A 108.2 . . ?
C10 C9 H9B 108.2 . . ?
H9A C9 H9B 107.4 . . ?
O2 C3 C4 124.1(4) . . ?
O2 C3 C2 119.3(4) . . ?
C4 C3 C2 116.7(4) . . ?
N5 C24 H24A 109.5 . . ?
N5 C24 H24B 109.5 . . ?
N5 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C25 H25A 109.5 . . ?
N5 C25 H25B 109.5 . . ?
N5 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 O12 C26 N5 -136.8(8) . . . . ?
La1 O9 N3 O11 -172.8(5) . . . . ?
La1 O9 N3 O10 7.3(5) . . . . ?
La1 O5 C17 C12 179.9(3) . . . . ?
La1 O5 C17 C16 3.6(6) . . . . ?
La1 O8 C19 O7 -10.6(7) . . . . ?
La1 O8 C19 C20 168.9(3) . . . . ?
La1 O1 C2 C7 176.7(4) . . . . ?
La1 O1 C2 C3 -2.5(5) . . . . ?
La1 O2 C3 C4 -172.6(3) . . . . ?
La1 O2 C3 C2 9.0(5) . . . . ?
La1 O6 C16 C17 -1.6(5) . . . . ?
La1 O6 C16 C15 178.2(4) . . . . ?
La1 O14 N4 O15 174.5(5) . . . . ?
La1 O14 N4 O16 -4.9(5) . . . . ?
La1 O10 N3 O9 -7.3(5) . . . . ?
La1 O10 N3 O11 172.9(5) . . . . ?
La1 O16 N4 O15 -174.3(5) . . . . ?
La1 O16 N4 O14 5.1(5) . . . . ?
Ni1 N1 C8 C4 -10.0(6) . . . . ?
Ni1 O5 C17 C12 -23.7(6) . . . . ?
Ni1 O5 C17 C16 160.0(3) . . . . ?
Ni1 O7 C19 C20 -169.3(3) . . . . ?
Ni1 O7 C19 O8 10.2(6) . . . . ?
Ni1 O2 C3 C4 -29.3(6) . . . . ?
Ni1 O2 C3 C2 152.3(3) . . . . ?
Ni1 N2 C11 C12 5.9(7) . . . . ?
O3 N1 C8 C4 -173.8(4) . . . . ?
O4 N2 C11 C12 179.9(4) . . . . ?
O4 C10 C9 O3 -60.3(5) . . . . ?
C6 C7 C2 O1 -179.0(5) . . . . ?
C6 C7 C2 C3 0.2(8) . . . . ?
C6 C5 C4 C8 177.6(5) . . . . ?
C6 C5 C4 C3 -3.9(8) . . . . ?
N1 O3 C9 C10 -50.5(5) . . . . ?
N1 C8 C4 C5 -163.8(4) . . . . ?
N1 C8 C4 C3 17.7(7) . . . . ?
O5 C17 C16 O6 -0.9(6) . . . . ?
O5 C17 C16 C15 179.2(4) . . . . ?
C14 C15 C16 O6 177.6(5) . . . . ?
C14 C15 C16 C17 -2.5(8) . . . . ?
O1 C2 C3 O2 -3.7(6) . . . . ?
O1 C2 C3 C4 177.8(4) . . . . ?
C21 C20 C22 C21 -2.4(7) . . . 3_756 ?
C21 C20 C19 O7 -3.0(6) . . . . ?
C21 C20 C19 O8 177.4(4) . . . . ?
N2 O4 C10 C9 96.0(5) . . . . ?
C8 C4 C3 O2 3.2(7) . . . . ?
C8 C4 C3 C2 -178.3(4) . . . . ?
C7 C6 C5 C4 2.5(9) . . . . ?
C7 C2 C3 O2 177.0(4) . . . . ?
C7 C2 C3 C4 -1.5(7) . . . . ?
C12 C17 C16 O6 -177.5(4) . . . . ?
C12 C17 C16 C15 2.7(7) . . . . ?
C17 C12 C11 N2 9.3(8) . . . . ?
C17 C12 C13 C14 -2.5(8) . . . . ?
C22 C20 C21 C22 2.3(7) . . . 3_756 ?
C22 C20 C19 O7 173.3(4) . . . . ?
C22 C20 C19 O8 -6.3(6) . . . . ?
C18 O6 C16 C17 172.7(5) . . . . ?
C18 O6 C16 C15 -7.4(7) . . . . ?
C11 C12 C17 O5 0.1(7) . . . . ?
C11 C12 C17 C16 176.4(4) . . . . ?
C11 C12 C13 C14 -179.3(5) . . . . ?
C5 C6 C7 C2 -0.7(9) . . . . ?
C5 C4 C3 O2 -175.2(4) . . . . ?
C5 C4 C3 C2 3.2(6) . . . . ?
C1 O1 C2 C7 -22.3(7) . . . . ?
C1 O1 C2 C3 158.4(4) . . . . ?
C13 C14 C15 C16 -0.2(9) . . . . ?
C13 C12 C17 O5 -176.5(4) . . . . ?
C13 C12 C17 C16 -0.2(7) . . . . ?
C13 C12 C11 N2 -174.0(5) . . . . ?
C15 C14 C13 C12 2.7(9) . . . . ?
C19 C20 C21 C22 178.7(4) . . . 3_756 ?
C19 C20 C22 C21 -178.8(4) . . . 3_756 ?
C10 O4 N2 Ni1 -21.8(5) . . . . ?
C10 O4 N2 C11 164.1(4) . . . . ?
C9 O3 N1 Ni1 86.2(4) . . . . ?
C9 O3 N1 C8 -108.2(4) . . . . ?
C24 N5 C26 O12 2.1(12) . . . . ?
C25 N5 C26 O12 -175.2(7) . . . . ?

_olex2_date_sample_data_collection 2015-04-08
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_d743
_database_code_depnum_ccdc_archive 'CCDC 1434588'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_audit_creation_date             2015-09-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C52 H62 Gd2 N10 Ni2 O32'
_chemical_formula_sum            'C52 H62 Gd2 N10 Ni2 O32'
_chemical_formula_weight         1771.03
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.1274(7)
_cell_length_b                   12.9696(7)
_cell_length_c                   17.1643(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.274(4)
_cell_angle_gamma                90
_cell_volume                     3340.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5259
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.6000
_cell_measurement_theta_min      10.3730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    14.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12619
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.891
_diffrn_reflns_theta_min         10.399
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   98.00  123.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 17

#__ type_ start__ end____ width___ exp.time_
  2 omega   93.00  133.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega  148.00  175.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  120.0000 18

#__ type_ start__ end____ width___ exp.time_
  4 omega  119.00  146.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 18

#__ type_ start__ end____ width___ exp.time_
  5 omega   60.00   87.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 18

#__ type_ start__ end____ width___ exp.time_
  6 omega   44.00  123.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 53

#__ type_ start__ end____ width___ exp.time_
  7 omega   43.00   94.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 34

#__ type_ start__ end____ width___ exp.time_
  8 omega   36.00   94.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -60.0000 39

#__ type_ start__ end____ width___ exp.time_
  9 omega   44.00  131.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
 10 omega   43.00  112.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -150.0000 46

#__ type_ start__ end____ width___ exp.time_
 11 omega   35.00   93.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 39

#__ type_ start__ end____ width___ exp.time_
 12 omega   36.00   72.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 24

#__ type_ start__ end____ width___ exp.time_
 13 omega   41.00   68.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 18

#__ type_ start__ end____ width___ exp.time_
 14 omega   43.00   89.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 31

#__ type_ start__ end____ width___ exp.time_
 15 omega   43.00  107.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 43

#__ type_ start__ end____ width___ exp.time_
 16 omega    5.00   86.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  -90.0000 54

#__ type_ start__ end____ width___ exp.time_
 17 omega  -14.00   23.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -180.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0872110000
_diffrn_orient_matrix_UB_12      -0.0110367000
_diffrn_orient_matrix_UB_13      0.0564121000
_diffrn_orient_matrix_UB_21      -0.0121971000
_diffrn_orient_matrix_UB_22      -0.1178318000
_diffrn_orient_matrix_UB_23      0.0000476000
_diffrn_orient_matrix_UB_31      0.0528806000
_diffrn_orient_matrix_UB_32      -0.0089172000
_diffrn_orient_matrix_UB_33      -0.0707801000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5111
_reflns_number_total             6098
_reflns_odcompleteness_completeness 98.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6098
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0423
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0661P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1152
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C15(H15), C16(H16), C17(H17),
 C19(H19), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C5AA(H5AA,H5AB,H5AC), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.18303(2) 0.55413(2) 0.17790(2) 0.02331(10) Uani 1 1 d . . . . .
Ni1 Ni 0.37122(5) 0.67093(6) 0.26525(4) 0.02230(19) Uani 1 1 d . . . . .
O1 O 0.1347(2) 0.6945(3) 0.0790(2) 0.0340(8) Uani 1 1 d . . . . .
O2 O 0.2567(2) 0.7132(3) 0.19945(18) 0.0242(7) Uani 1 1 d . . . . .
O3 O 0.4734(3) 0.8559(3) 0.3261(2) 0.0424(10) Uani 1 1 d . . . . .
O4 O 0.5655(3) 0.6540(4) 0.3475(3) 0.0524(12) Uani 1 1 d . . . . .
O5 O 0.3097(2) 0.5320(3) 0.26958(19) 0.0258(7) Uani 1 1 d . . . . .
O6 O 0.1823(3) 0.4030(3) 0.2811(2) 0.0417(9) Uani 1 1 d . . . . .
O7 O 0.4245(2) 0.6322(3) 0.16613(18) 0.0302(8) Uani 1 1 d . . . . .
O8 O 0.3061(2) 0.5518(3) 0.1019(2) 0.0318(8) Uani 1 1 d . . . . .
O9 O 0.0339(2) 0.5037(4) 0.1756(2) 0.0518(11) Uani 1 1 d . . . . .
O10 O 0.0690(3) 0.7087(4) 0.2241(2) 0.0546(12) Uani 1 1 d . . . . .
O11 O 0.1479(2) 0.6173(3) 0.3109(2) 0.0369(9) Uani 1 1 d . . . . .
O12 O 0.0711(5) 0.7446(6) 0.3453(3) 0.109(3) Uani 1 1 d . . . . .
O13 O 0.1333(3) 0.4803(4) 0.0427(3) 0.0536(12) Uani 1 1 d . . . . .
O14 O 0.2023(3) 0.3761(4) 0.1258(3) 0.0544(11) Uani 1 1 d . . . . .
O15 O 0.1703(4) 0.3322(6) 0.0031(4) 0.107(3) Uani 1 1 d . . . . .
N1 N 0.4102(3) 0.8197(3) 0.2627(2) 0.0309(10) Uani 1 1 d . . . . .
N2 N 0.4792(3) 0.6098(4) 0.3344(3) 0.0317(10) Uani 1 1 d . . . . .
N3 N 0.0955(3) 0.6926(4) 0.2937(3) 0.0436(12) Uani 1 1 d . . . . .
N4 N 0.1686(4) 0.3932(5) 0.0559(4) 0.0564(16) Uani 1 1 d . . . . .
N5 N -0.1097(4) 0.4930(6) 0.1929(4) 0.0611(16) Uani 1 1 d . . . . .
C2 C 0.1803(4) 0.7864(5) 0.0852(3) 0.0354(12) Uani 1 1 d . . . . .
C3 C 0.1644(4) 0.8670(5) 0.0334(4) 0.0496(16) Uani 1 1 d . . . . .
H3 H 0.1190 0.8619 -0.0084 0.060 Uiso 1 1 calc R . . . .
C4 C 0.2155(5) 0.9557(5) 0.0432(5) 0.060(2) Uani 1 1 d . . . . .
H4 H 0.2052 1.0098 0.0076 0.072 Uiso 1 1 calc R . . . .
C5 C 0.2813(4) 0.9634(5) 0.1054(4) 0.0495(16) Uani 1 1 d . . . . .
H5 H 0.3139 1.0242 0.1129 0.059 Uiso 1 1 calc R . . . .
C5AA C 0.0476(4) 0.6959(6) 0.0331(4) 0.0533(17) Uani 1 1 d . . . . .
H5AA H 0.0181 0.6314 0.0392 0.080 Uiso 1 1 calc GR . . . .
H5AB H 0.0540 0.7063 -0.0213 0.080 Uiso 1 1 calc GR . . . .
H5AC H 0.0128 0.7510 0.0510 0.080 Uiso 1 1 calc GR . . . .
C6 C 0.3006(3) 0.8806(4) 0.1587(3) 0.0342(12) Uani 1 1 d . . . . .
C7 C 0.2478(3) 0.7911(4) 0.1503(3) 0.0268(10) Uani 1 1 d . . . . .
C8 C 0.3732(4) 0.8944(4) 0.2215(3) 0.0373(12) Uani 1 1 d . . . . .
H8 H 0.3941 0.9609 0.2325 0.045 Uiso 1 1 calc R . . . .
C9 C 0.5629(4) 0.8346(5) 0.3115(4) 0.0454(15) Uani 1 1 d . . . . .
H9A H 0.6028 0.8515 0.3585 0.054 Uiso 1 1 calc R . . . .
H9B H 0.5771 0.8802 0.2700 0.054 Uiso 1 1 calc R . . . .
C10 C 0.5811(4) 0.7269(6) 0.2887(4) 0.0476(15) Uani 1 1 d . . . . .
H10A H 0.5435 0.7102 0.2403 0.057 Uiso 1 1 calc R . . . .
H10B H 0.6427 0.7217 0.2788 0.057 Uiso 1 1 calc R . . . .
C11 C 0.4771(4) 0.5287(5) 0.3774(3) 0.0392(13) Uani 1 1 d . . . . .
H11 H 0.5294 0.5118 0.4094 0.047 Uiso 1 1 calc R . . . .
C12 C 0.4017(4) 0.4613(4) 0.3810(3) 0.0334(12) Uani 1 1 d . . . . .
C13 C 0.3224(3) 0.4670(4) 0.3287(3) 0.0251(10) Uani 1 1 d . . . . .
C14 C 0.2557(4) 0.3950(4) 0.3369(3) 0.0333(11) Uani 1 1 d . . . . .
C15 C 0.2641(5) 0.3221(5) 0.3960(4) 0.0472(15) Uani 1 1 d . . . . .
H15 H 0.2180 0.2760 0.4009 0.057 Uiso 1 1 calc R . . . .
C16 C 0.3426(5) 0.3183(5) 0.4483(4) 0.0580(18) Uani 1 1 d . . . . .
H16 H 0.3484 0.2706 0.4891 0.070 Uiso 1 1 calc R . . . .
C17 C 0.4109(5) 0.3846(5) 0.4398(4) 0.0497(16) Uani 1 1 d . . . . .
H17 H 0.4641 0.3791 0.4731 0.060 Uiso 1 1 calc R . . . .
C18 C 0.1178(5) 0.3218(6) 0.2782(5) 0.076(3) Uani 1 1 d . . . . .
H18A H 0.0850 0.3276 0.3224 0.115 Uiso 1 1 calc GR . . . .
H18B H 0.1476 0.2563 0.2799 0.115 Uiso 1 1 calc GR . . . .
H18C H 0.0775 0.3270 0.2304 0.115 Uiso 1 1 calc GR . . . .
C19 C -0.0449(4) 0.4949(6) 0.1505(4) 0.0550(18) Uani 1 1 d . . . . .
H19 H -0.0596 0.4892 0.0964 0.066 Uiso 1 1 calc R . . . .
C20 C -0.0921(7) 0.4993(10) 0.2772(5) 0.097(3) Uani 1 1 d . . . . .
H20A H -0.0290 0.5046 0.2927 0.146 Uiso 1 1 calc GR . . . .
H20B H -0.1143 0.4384 0.3000 0.146 Uiso 1 1 calc GR . . . .
H20C H -0.1212 0.5589 0.2951 0.146 Uiso 1 1 calc GR . . . .
C21 C -0.2010(5) 0.4798(12) 0.1579(7) 0.128(5) Uani 1 1 d . . . . .
H21A H -0.2345 0.5408 0.1665 0.192 Uiso 1 1 calc GR . . . .
H21B H -0.2266 0.4217 0.1815 0.192 Uiso 1 1 calc GR . . . .
H21C H -0.2027 0.4682 0.1025 0.192 Uiso 1 1 calc GR . . . .
C22 C 0.3866(3) 0.5772(4) 0.1106(3) 0.0247(10) Uani 1 1 d . . . . .
C23 C 0.4451(3) 0.5388(4) 0.0531(3) 0.0229(10) Uani 1 1 d . . . . .
C24 C 0.5337(3) 0.5691(4) 0.0576(3) 0.0301(11) Uani 1 1 d . . . . .
H24 H 0.5566 0.6164 0.0956 0.036 Uiso 1 1 calc R . . . .
C25 C 0.4117(3) 0.4709(4) -0.0058(3) 0.0280(11) Uani 1 1 d . . . . .
H25 H 0.3520 0.4519 -0.0106 0.034 Uiso 1 1 calc R . . . .
O16 O 0.3129(3) 0.7067(4) 0.3696(2) 0.0418(10) Uani 1 1 d . . . . .
C26 C 0.3479(5) 0.7426(7) 0.4445(4) 0.065(2) Uani 1 1 d . . . . .
H26A H 0.4054 0.7729 0.4420 0.098 Uiso 1 1 calc GR . . . .
H26B H 0.3537 0.6860 0.4808 0.098 Uiso 1 1 calc GR . . . .
H26C H 0.3086 0.7934 0.4617 0.098 Uiso 1 1 calc GR . . . .
H16A H 0.271(5) 0.681(6) 0.376(5) 0.07(3) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 Ni1 3.4010(8) . ?
Gd1 O1 2.532(4) . ?
Gd1 O2 2.351(3) . ?
Gd1 O5 2.339(3) . ?
Gd1 O6 2.643(4) . ?
Gd1 O8 2.405(3) . ?
Gd1 O9 2.344(4) . ?
Gd1 O10 2.823(5) . ?
Gd1 O11 2.544(4) . ?
Gd1 O13 2.535(4) . ?
Gd1 O14 2.506(5) . ?
Gd1 N4 2.945(5) . ?
Ni1 O2 2.020(3) . ?
Ni1 O5 2.033(3) . ?
Ni1 O7 2.035(3) . ?
Ni1 N1 2.020(4) . ?
Ni1 N2 2.053(4) . ?
Ni1 O16 2.144(4) . ?
O1 C2 1.375(7) . ?
O1 C5AA 1.448(6) . ?
O2 C7 1.312(6) . ?
O3 N1 1.434(5) . ?
O3 C9 1.434(7) . ?
O4 N2 1.417(5) . ?
O4 C10 1.425(8) . ?
O5 C13 1.314(6) . ?
O6 C14 1.376(6) . ?
O6 C18 1.432(7) . ?
O7 C22 1.268(6) . ?
O8 C22 1.252(6) . ?
O9 C19 1.221(7) . ?
O10 N3 1.229(6) . ?
O11 N3 1.269(6) . ?
O12 N3 1.207(7) . ?
O13 N4 1.258(8) . ?
O14 N4 1.262(7) . ?
O15 N4 1.206(7) . ?
N1 C8 1.285(7) . ?
N2 C11 1.287(7) . ?
N5 C19 1.292(8) . ?
N5 C20 1.441(10) . ?
N5 C21 1.445(10) . ?
C2 C3 1.373(8) . ?
C2 C7 1.417(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.386(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.368(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.417(8) . ?
C5AA H5AA 0.9600 . ?
C5AA H5AB 0.9600 . ?
C5AA H5AC 0.9600 . ?
C6 C7 1.406(7) . ?
C6 C8 1.448(8) . ?
C8 H8 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.486(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11 0.9300 . ?
C11 C12 1.444(8) . ?
C12 C13 1.406(7) . ?
C12 C17 1.411(8) . ?
C13 C14 1.396(7) . ?
C14 C15 1.382(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.395(9) . ?
C16 H16 0.9300 . ?
C16 C17 1.367(10) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.492(6) . ?
C23 C24 1.388(7) . ?
C23 C25 1.387(7) . ?
C24 H24 0.9300 . ?
C24 C25 1.388(7) 3_665 ?
C25 C24 1.388(7) 3_665 ?
C25 H25 0.9300 . ?
O16 C26 1.406(7) . ?
O16 H16A 0.74(8) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

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 Gd1 Ni1 97.46(8) . . ?
O1 Gd1 O6 163.09(12) . . ?
O1 Gd1 O10 62.82(12) . . ?
O1 Gd1 O11 107.13(12) . . ?
O1 Gd1 O13 68.34(15) . . ?
O1 Gd1 N4 92.51(17) . . ?
O2 Gd1 Ni1 35.55(8) . . ?
O2 Gd1 O1 64.27(11) . . ?
O2 Gd1 O6 125.99(11) . . ?
O2 Gd1 O8 73.28(11) . . ?
O2 Gd1 O10 68.11(13) . . ?
O2 Gd1 O11 74.02(12) . . ?
O2 Gd1 O13 123.72(15) . . ?
O2 Gd1 O14 142.20(13) . . ?
O2 Gd1 N4 136.42(15) . . ?
O5 Gd1 Ni1 35.80(8) . . ?
O5 Gd1 O1 132.97(11) . . ?
O5 Gd1 O2 70.73(11) . . ?
O5 Gd1 O6 62.03(11) . . ?
O5 Gd1 O8 74.85(12) . . ?
O5 Gd1 O9 133.01(14) . . ?
O5 Gd1 O10 112.09(12) . . ?
O5 Gd1 O11 71.46(12) . . ?
O5 Gd1 O13 133.83(14) . . ?
O5 Gd1 O14 90.27(14) . . ?
O5 Gd1 N4 111.84(15) . . ?
O6 Gd1 Ni1 96.29(8) . . ?
O6 Gd1 O10 106.49(13) . . ?
O6 Gd1 N4 86.82(18) . . ?
O8 Gd1 Ni1 65.32(8) . . ?
O8 Gd1 O1 79.81(12) . . ?
O8 Gd1 O6 115.06(13) . . ?
O8 Gd1 O10 134.73(13) . . ?
O8 Gd1 O11 138.99(12) . . ?
O8 Gd1 O13 70.06(13) . . ?
O8 Gd1 O14 70.26(14) . . ?
O8 Gd1 N4 66.30(13) . . ?
O9 Gd1 Ni1 151.86(11) . . ?
O9 Gd1 O1 89.64(15) . . ?
O9 Gd1 O2 133.10(15) . . ?
O9 Gd1 O6 73.65(14) . . ?
O9 Gd1 O8 142.81(14) . . ?
O9 Gd1 O10 65.29(16) . . ?
O9 Gd1 O11 78.20(14) . . ?
O9 Gd1 O13 72.89(15) . . ?
O9 Gd1 O14 83.79(17) . . ?
O9 Gd1 N4 78.80(16) . . ?
O10 Gd1 Ni1 93.85(10) . . ?
O10 Gd1 N4 135.25(15) . . ?
O11 Gd1 Ni1 73.68(9) . . ?
O11 Gd1 O6 67.59(13) . . ?
O11 Gd1 O10 46.74(12) . . ?
O11 Gd1 N4 149.47(16) . . ?
O13 Gd1 Ni1 134.95(11) . . ?
O13 Gd1 O6 107.89(15) . . ?
O13 Gd1 O10 113.86(14) . . ?
O13 Gd1 O11 150.67(13) . . ?
O13 Gd1 N4 25.14(17) . . ?
O14 Gd1 Ni1 116.04(11) . . ?
O14 Gd1 O1 117.37(14) . . ?
O14 Gd1 O6 64.28(15) . . ?
O14 Gd1 O10 148.99(15) . . ?
O14 Gd1 O11 131.59(14) . . ?
O14 Gd1 O13 50.20(16) . . ?
O14 Gd1 N4 25.17(17) . . ?
N4 Gd1 Ni1 127.70(10) . . ?
O2 Ni1 Gd1 42.58(9) . . ?
O2 Ni1 O5 84.08(13) . . ?
O2 Ni1 O7 90.10(14) . . ?
O2 Ni1 N2 172.36(16) . . ?
O2 Ni1 O16 89.65(15) . . ?
O5 Ni1 Gd1 42.28(9) . . ?
O5 Ni1 O7 92.46(14) . . ?
O5 Ni1 N2 88.33(16) . . ?
O5 Ni1 O16 85.56(16) . . ?
O7 Ni1 Gd1 85.37(9) . . ?
O7 Ni1 N2 91.04(16) . . ?
O7 Ni1 O16 178.02(16) . . ?
N1 Ni1 Gd1 130.25(13) . . ?
N1 Ni1 O2 87.74(16) . . ?
N1 Ni1 O5 169.56(16) . . ?
N1 Ni1 O7 94.02(16) . . ?
N1 Ni1 N2 99.71(18) . . ?
N1 Ni1 O16 87.92(18) . . ?
N2 Ni1 Gd1 130.03(13) . . ?
N2 Ni1 O16 88.96(17) . . ?
O16 Ni1 Gd1 93.13(11) . . ?
C2 O1 Gd1 118.2(3) . . ?
C2 O1 C5AA 116.3(5) . . ?
C5AA O1 Gd1 122.7(4) . . ?
Ni1 O2 Gd1 101.88(14) . . ?
C7 O2 Gd1 124.5(3) . . ?
C7 O2 Ni1 125.4(3) . . ?
C9 O3 N1 111.0(4) . . ?
N2 O4 C10 112.8(4) . . ?
Ni1 O5 Gd1 101.92(13) . . ?
C13 O5 Gd1 128.7(3) . . ?
C13 O5 Ni1 125.0(3) . . ?
C14 O6 Gd1 116.8(3) . . ?
C14 O6 C18 117.0(5) . . ?
C18 O6 Gd1 125.7(4) . . ?
C22 O7 Ni1 125.3(3) . . ?
C22 O8 Gd1 137.8(3) . . ?
C19 O9 Gd1 158.0(5) . . ?
N3 O10 Gd1 90.9(3) . . ?
N3 O11 Gd1 103.6(3) . . ?
N4 O13 Gd1 96.0(3) . . ?
N4 O14 Gd1 97.2(4) . . ?
O3 N1 Ni1 117.7(3) . . ?
C8 N1 Ni1 128.6(4) . . ?
C8 N1 O3 111.9(4) . . ?
O4 N2 Ni1 125.8(3) . . ?
C11 N2 Ni1 124.8(4) . . ?
C11 N2 O4 109.2(4) . . ?
O10 N3 O11 118.3(5) . . ?
O12 N3 O10 121.7(6) . . ?
O12 N3 O11 120.0(5) . . ?
O13 N4 Gd1 58.9(3) . . ?
O13 N4 O14 116.1(5) . . ?
O14 N4 Gd1 57.6(3) . . ?
O15 N4 Gd1 173.1(5) . . ?
O15 N4 O13 120.2(7) . . ?
O15 N4 O14 123.7(7) . . ?
C19 N5 C20 120.5(6) . . ?
C19 N5 C21 121.4(7) . . ?
C20 N5 C21 118.0(7) . . ?
O1 C2 C7 113.7(5) . . ?
C3 C2 O1 124.4(5) . . ?
C3 C2 C7 121.8(6) . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.3(6) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.6(6) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.3(6) . . ?
C6 C5 H5 119.4 . . ?
O1 C5AA H5AA 109.5 . . ?
O1 C5AA H5AB 109.5 . . ?
O1 C5AA H5AC 109.5 . . ?
H5AA C5AA H5AB 109.5 . . ?
H5AA C5AA H5AC 109.5 . . ?
H5AB C5AA H5AC 109.5 . . ?
C5 C6 C8 117.5(5) . . ?
C7 C6 C5 119.4(5) . . ?
C7 C6 C8 123.0(5) . . ?
O2 C7 C2 118.6(5) . . ?
O2 C7 C6 124.0(4) . . ?
C6 C7 C2 117.4(5) . . ?
N1 C8 C6 123.6(5) . . ?
N1 C8 H8 118.2 . . ?
C6 C8 H8 118.2 . . ?
O3 C9 H9A 108.3 . . ?
O3 C9 H9B 108.3 . . ?
O3 C9 C10 116.0(5) . . ?
H9A C9 H9B 107.4 . . ?
C10 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
O4 C10 C9 112.7(5) . . ?
O4 C10 H10A 109.1 . . ?
O4 C10 H10B 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N2 C11 H11 116.7 . . ?
N2 C11 C12 126.6(5) . . ?
C12 C11 H11 116.7 . . ?
C13 C12 C11 123.7(5) . . ?
C13 C12 C17 119.5(5) . . ?
C17 C12 C11 116.8(5) . . ?
O5 C13 C12 123.8(5) . . ?
O5 C13 C14 118.0(4) . . ?
C14 C13 C12 118.0(5) . . ?
O6 C14 C13 114.2(5) . . ?
O6 C14 C15 123.7(5) . . ?
C15 C14 C13 122.1(5) . . ?
C14 C15 H15 120.4 . . ?
C14 C15 C16 119.3(6) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.1(6) . . ?
C17 C16 H16 119.9 . . ?
C12 C17 H17 119.6 . . ?
C16 C17 C12 120.9(6) . . ?
C16 C17 H17 119.6 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O9 C19 N5 125.4(6) . . ?
O9 C19 H19 117.3 . . ?
N5 C19 H19 117.3 . . ?
N5 C20 H20A 109.5 . . ?
N5 C20 H20B 109.5 . . ?
N5 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N5 C21 H21A 109.5 . . ?
N5 C21 H21B 109.5 . . ?
N5 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O7 C22 C23 115.8(4) . . ?
O8 C22 O7 125.3(4) . . ?
O8 C22 C23 118.9(4) . . ?
C24 C23 C22 121.2(4) . . ?
C25 C23 C22 120.1(4) . . ?
C25 C23 C24 118.7(4) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.5(5) 3_665 . ?
C25 C24 H24 119.8 3_665 . ?
C23 C25 C24 120.8(5) . 3_665 ?
C23 C25 H25 119.6 . . ?
C24 C25 H25 119.6 3_665 . ?
Ni1 O16 H16A 118(6) . . ?
C26 O16 Ni1 133.5(4) . . ?
C26 O16 H16A 105(6) . . ?
O16 C26 H26A 109.5 . . ?
O16 C26 H26B 109.5 . . ?
O16 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O1 C2 C3 176.5(5) . . . . ?
Gd1 O1 C2 C7 -2.7(6) . . . . ?
Gd1 O2 C7 C2 9.6(6) . . . . ?
Gd1 O2 C7 C6 -171.3(4) . . . . ?
Gd1 O5 C13 C12 -179.2(4) . . . . ?
Gd1 O5 C13 C14 5.1(6) . . . . ?
Gd1 O6 C14 C13 -2.4(6) . . . . ?
Gd1 O6 C14 C15 178.1(5) . . . . ?
Gd1 O8 C22 O7 -12.7(8) . . . . ?
Gd1 O8 C22 C23 165.6(3) . . . . ?
Gd1 O9 C19 N5 -146.5(10) . . . . ?
Gd1 O10 N3 O11 -6.2(5) . . . . ?
Gd1 O10 N3 O12 175.8(7) . . . . ?
Gd1 O11 N3 O10 7.1(6) . . . . ?
Gd1 O11 N3 O12 -174.8(6) . . . . ?
Gd1 O13 N4 O14 6.7(5) . . . . ?
Gd1 O13 N4 O15 -172.1(6) . . . . ?
Gd1 O14 N4 O13 -6.8(6) . . . . ?
Gd1 O14 N4 O15 172.0(6) . . . . ?
Ni1 O2 C7 C2 152.2(4) . . . . ?
Ni1 O2 C7 C6 -28.6(6) . . . . ?
Ni1 O5 C13 C12 -27.1(6) . . . . ?
Ni1 O5 C13 C14 157.3(4) . . . . ?
Ni1 O7 C22 O8 11.9(7) . . . . ?
Ni1 O7 C22 C23 -166.5(3) . . . . ?
Ni1 N1 C8 C6 -9.5(8) . . . . ?
Ni1 N2 C11 C12 5.0(8) . . . . ?
O1 C2 C3 C4 -178.2(6) . . . . ?
O1 C2 C7 O2 -3.9(7) . . . . ?
O1 C2 C7 C6 176.9(4) . . . . ?
O3 N1 C8 C6 -173.7(5) . . . . ?
O3 C9 C10 O4 -60.4(7) . . . . ?
O4 N2 C11 C12 -179.6(5) . . . . ?
O5 C13 C14 O6 -1.1(7) . . . . ?
O5 C13 C14 C15 178.4(5) . . . . ?
O6 C14 C15 C16 177.9(6) . . . . ?
O7 C22 C23 C24 -4.9(7) . . . . ?
O7 C22 C23 C25 174.4(5) . . . . ?
O8 C22 C23 C24 176.6(5) . . . . ?
O8 C22 C23 C25 -4.0(7) . . . . ?
N1 O3 C9 C10 -50.3(7) . . . . ?
N2 O4 C10 C9 95.0(6) . . . . ?
N2 C11 C12 C13 9.6(9) . . . . ?
N2 C11 C12 C17 -171.9(6) . . . . ?
C2 C3 C4 C5 -1.0(11) . . . . ?
C3 C2 C7 O2 176.9(5) . . . . ?
C3 C2 C7 C6 -2.3(8) . . . . ?
C3 C4 C5 C6 2.5(12) . . . . ?
C4 C5 C6 C7 -3.9(10) . . . . ?
C4 C5 C6 C8 178.1(6) . . . . ?
C5 C6 C7 O2 -175.5(5) . . . . ?
C5 C6 C7 C2 3.7(8) . . . . ?
C5 C6 C8 N1 -164.2(6) . . . . ?
C5AA O1 C2 C3 -21.8(8) . . . . ?
C5AA O1 C2 C7 159.0(5) . . . . ?
C7 C2 C3 C4 0.9(10) . . . . ?
C7 C6 C8 N1 17.9(9) . . . . ?
C8 C6 C7 O2 2.4(8) . . . . ?
C8 C6 C7 C2 -178.4(5) . . . . ?
C9 O3 N1 Ni1 85.7(5) . . . . ?
C9 O3 N1 C8 -108.2(5) . . . . ?
C10 O4 N2 Ni1 -20.1(6) . . . . ?
C10 O4 N2 C11 164.6(5) . . . . ?
C11 C12 C13 O5 2.3(8) . . . . ?
C11 C12 C13 C14 177.9(5) . . . . ?
C11 C12 C17 C16 179.0(6) . . . . ?
C12 C13 C14 O6 -177.0(5) . . . . ?
C12 C13 C14 C15 2.5(8) . . . . ?
C13 C12 C17 C16 -2.4(9) . . . . ?
C13 C14 C15 C16 -1.5(9) . . . . ?
C14 C15 C16 C17 -1.5(11) . . . . ?
C15 C16 C17 C12 3.5(11) . . . . ?
C17 C12 C13 O5 -176.2(5) . . . . ?
C17 C12 C13 C14 -0.6(8) . . . . ?
C18 O6 C14 C13 170.3(6) . . . . ?
C18 O6 C14 C15 -9.2(9) . . . . ?
C20 N5 C19 O9 -1.3(14) . . . . ?
C21 N5 C19 O9 -178.5(10) . . . . ?
C22 C23 C24 C25 177.2(5) . . . 3_665 ?
C22 C23 C25 C24 -177.2(5) . . . 3_665 ?
C24 C23 C25 C24 2.2(9) . . . 3_665 ?
C25 C23 C24 C25 -2.2(9) . . . 3_665 ?

_olex2_date_sample_data_collection 2015-08-28
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_d791
_database_code_depnum_ccdc_archive 'CCDC 1434589'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_audit_creation_date             2015-08-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C50 H54 N10 Ni2 O30 Tb2'
_chemical_formula_sum            'C50 H54 N10 Ni2 O30 Tb2'
_chemical_formula_weight         1710.29
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5724(8)
_cell_length_b                   12.5483(12)
_cell_length_c                   13.8671(7)
_cell_angle_alpha                99.027(6)
_cell_angle_beta                 95.068(5)
_cell_angle_gamma                101.985(7)
_cell_volume                     1763.3(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3843
_cell_measurement_temperature    296.71(10)
_cell_measurement_theta_max      25.3830
_cell_measurement_theta_min      3.5040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13785
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.493
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.71(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -46.00   41.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
  2 omega  -19.00   11.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  -30.0000 20

#__ type_ start__ end____ width___ exp.time_
  3 omega  -14.00   25.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega  -36.00   36.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000  150.0000 48

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00   40.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -38.0000  -90.0000 60

#__ type_ start__ end____ width___ exp.time_
  6 omega  -20.00   55.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -99.0000  -90.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0260956000
_diffrn_orient_matrix_UB_12      -0.0472838000
_diffrn_orient_matrix_UB_13      -0.0127515000
_diffrn_orient_matrix_UB_21      -0.0604205000
_diffrn_orient_matrix_UB_22      -0.0347874000
_diffrn_orient_matrix_UB_23      0.0046572000
_diffrn_orient_matrix_UB_31      -0.0211450000
_diffrn_orient_matrix_UB_32      -0.0021945000
_diffrn_orient_matrix_UB_33      -0.0504059000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5551
_reflns_number_total             6907
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6907
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0400
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0268P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0851
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C15(H15), C16(H16), C17(H17),
 C19(H19), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.62515(2) 0.25106(2) 0.31089(2) 0.03080(8) Uani 1 1 d . . . . .
Ni1 Ni 0.84344(6) 0.26195(5) 0.14489(4) 0.03222(15) Uani 1 1 d . . . . .
O1 O 0.7316(3) 0.4163(3) 0.4343(2) 0.0386(8) Uani 1 1 d . . . . .
O2 O 0.8380(3) 0.3329(3) 0.2876(2) 0.0317(7) Uani 1 1 d . . . . .
O3 O 1.1160(3) 0.3674(4) 0.0859(3) 0.0589(11) Uani 1 1 d . . . . .
O4 O 0.8472(4) 0.2022(4) -0.0844(2) 0.0662(12) Uani 1 1 d . . . . .
O5 O 0.6768(3) 0.1601(3) 0.1715(2) 0.0343(8) Uani 1 1 d . . . . .
O6 O 0.5340(3) 0.0431(3) 0.2754(2) 0.0459(9) Uani 1 1 d . . . . .
O7 O 0.7458(3) 0.3705(3) 0.0978(2) 0.0367(8) Uani 1 1 d . . . . .
O8 O 0.5962(3) 0.3689(3) 0.2033(2) 0.0399(8) Uani 1 1 d . . . . .
O9 O 0.7702(3) 0.1632(3) 0.4060(2) 0.0448(9) Uani 1 1 d . . . . .
O10 O 0.5995(4) 0.1962(3) 0.4717(2) 0.0512(10) Uani 1 1 d . . . . .
O11 O 0.7421(4) 0.1267(4) 0.5519(3) 0.0771(14) Uani 1 1 d . . . . .
O12 O 0.4544(3) 0.3387(3) 0.3722(2) 0.0501(10) Uani 1 1 d . . . . .
O13 O 0.3852(3) 0.1998(3) 0.2555(3) 0.0502(9) Uani 1 1 d . . . . .
O14 O 0.2541(4) 0.3027(4) 0.3041(3) 0.0743(13) Uani 1 1 d . . . . .
O15 O 0.9429(3) 0.1478(3) 0.1817(2) 0.0390(8) Uani 1 1 d . . . . .
N1 N 1.0214(4) 0.3768(4) 0.1511(3) 0.0423(11) Uani 1 1 d . . . . .
N2 N 0.8034(4) 0.1664(4) 0.0021(3) 0.0463(12) Uani 1 1 d . . . . .
N3 N 0.7062(5) 0.1610(4) 0.4800(3) 0.0523(12) Uani 1 1 d . . . . .
N4 N 0.3596(4) 0.2813(4) 0.3101(3) 0.0461(11) Uani 1 1 d . . . . .
N5 N 1.0335(5) 0.0676(4) 0.2950(3) 0.0578(14) Uani 1 1 d . . . . .
C1 C 0.6758(5) 0.4596(5) 0.5198(3) 0.0552(16) Uani 1 1 d . . . . .
H1A H 0.6429 0.5226 0.5075 0.083 Uiso 1 1 calc GR . . . .
H1B H 0.7418 0.4815 0.5758 0.083 Uiso 1 1 calc GR . . . .
H1C H 0.6060 0.4034 0.5328 0.083 Uiso 1 1 calc GR . . . .
C2 C 0.8386(5) 0.4864(4) 0.4094(3) 0.0371(12) Uani 1 1 d . . . . .
C3 C 0.8908(5) 0.5929(5) 0.4584(4) 0.0489(14) Uani 1 1 d . . . . .
H3 H 0.8549 0.6223 0.5126 0.059 Uiso 1 1 calc R . . . .
C4 C 0.9960(6) 0.6553(5) 0.4269(4) 0.0577(16) Uani 1 1 d . . . . .
H4 H 1.0308 0.7278 0.4589 0.069 Uiso 1 1 calc R . . . .
C5 C 1.0506(5) 0.6111(5) 0.3477(4) 0.0532(15) Uani 1 1 d . . . . .
H5 H 1.1234 0.6535 0.3278 0.064 Uiso 1 1 calc R . . . .
C6 C 0.9978(5) 0.5028(4) 0.2968(4) 0.0408(12) Uani 1 1 d . . . . .
C7 C 0.8910(4) 0.4380(4) 0.3285(3) 0.0310(11) Uani 1 1 d . . . . .
C8 C 1.0631(5) 0.4642(5) 0.2159(4) 0.0455(13) Uani 1 1 d . . . . .
H8 H 1.1440 0.5075 0.2104 0.055 Uiso 1 1 calc R . . . .
C9 C 1.0672(6) 0.2813(6) 0.0045(4) 0.0578(17) Uani 1 1 d . . . . .
H9A H 1.0428 0.2119 0.0279 0.069 Uiso 1 1 calc R . . . .
H9B H 1.1358 0.2752 -0.0368 0.069 Uiso 1 1 calc R . . . .
C10 C 0.9511(6) 0.2994(6) -0.0563(4) 0.0662(19) Uani 1 1 d . . . . .
H10A H 0.9182 0.3577 -0.0192 0.079 Uiso 1 1 calc R . . . .
H10B H 0.9790 0.3245 -0.1154 0.079 Uiso 1 1 calc R . . . .
C11 C 0.7379(6) 0.0655(6) -0.0192(4) 0.0554(16) Uani 1 1 d . . . . .
H11 H 0.7354 0.0289 -0.0833 0.066 Uiso 1 1 calc R . . . .
C12 C 0.6685(5) 0.0041(5) 0.0454(4) 0.0457(13) Uani 1 1 d . . . . .
C13 C 0.6399(5) 0.0526(4) 0.1352(3) 0.0364(11) Uani 1 1 d . . . . .
C14 C 0.5618(5) -0.0143(4) 0.1892(4) 0.0429(13) Uani 1 1 d . . . . .
C15 C 0.5185(6) -0.1272(5) 0.1563(5) 0.0645(18) Uani 1 1 d . . . . .
H15 H 0.4673 -0.1710 0.1929 0.077 Uiso 1 1 calc R . . . .
C16 C 0.5523(7) -0.1736(5) 0.0685(5) 0.076(2) Uani 1 1 d . . . . .
H16 H 0.5261 -0.2497 0.0471 0.092 Uiso 1 1 calc R . . . .
C17 C 0.6224(6) -0.1111(6) 0.0130(4) 0.0646(18) Uani 1 1 d . . . . .
H17 H 0.6408 -0.1441 -0.0474 0.077 Uiso 1 1 calc R . . . .
C18 C 0.4411(5) -0.0167(5) 0.3301(4) 0.0591(16) Uani 1 1 d . . . . .
H18A H 0.4770 -0.0726 0.3553 0.089 Uiso 1 1 calc GR . . . .
H18B H 0.3618 -0.0511 0.2873 0.089 Uiso 1 1 calc GR . . . .
H18C H 0.4230 0.0339 0.3838 0.089 Uiso 1 1 calc GR . . . .
C19 C 0.9859(5) 0.1451(4) 0.2664(4) 0.0416(13) Uani 1 1 d . . . . .
H19 H 0.9836 0.2052 0.3144 0.050 Uiso 1 1 calc R . . . .
C20 C 1.0551(12) -0.0178(8) 0.2235(6) 0.154(5) Uani 1 1 d . . . . .
H20A H 0.9730 -0.0621 0.1906 0.231 Uiso 1 1 calc GR . . . .
H20B H 1.1021 -0.0635 0.2549 0.231 Uiso 1 1 calc GR . . . .
H20C H 1.1051 0.0140 0.1763 0.231 Uiso 1 1 calc GR . . . .
C21 C 1.0867(8) 0.0738(6) 0.3948(4) 0.093(3) Uani 1 1 d . . . . .
H21A H 1.0742 0.1399 0.4344 0.139 Uiso 1 1 calc GR . . . .
H21B H 1.1781 0.0755 0.3978 0.139 Uiso 1 1 calc GR . . . .
H21C H 1.0433 0.0102 0.4192 0.139 Uiso 1 1 calc GR . . . .
C22 C 0.6424(4) 0.3924(4) 0.1261(3) 0.0309(10) Uani 1 1 d . . . . .
C23 C 0.5687(4) 0.4497(4) 0.0626(3) 0.0273(10) Uani 1 1 d . . . . .
C24 C 0.6248(4) 0.4905(4) -0.0157(3) 0.0340(11) Uani 1 1 d . . . . .
H24 H 0.7086 0.4836 -0.0264 0.041 Uiso 1 1 calc R . . . .
C25 C 0.4441(4) 0.4591(4) 0.0771(3) 0.0340(11) Uani 1 1 d . . . . .
H25 H 0.4060 0.4313 0.1286 0.041 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
Tb1 Ni1 3.3985(6) . ?
Tb1 O1 2.464(3) . ?
Tb1 O2 2.344(3) . ?
Tb1 O5 2.256(3) . ?
Tb1 O6 2.540(3) . ?
Tb1 O8 2.304(3) . ?
Tb1 O9 2.472(3) . ?
Tb1 O10 2.456(3) . ?
Tb1 O12 2.448(3) . ?
Tb1 O13 2.502(3) . ?
Tb1 N3 2.896(4) . ?
Tb1 N4 2.909(4) . ?
Ni1 O2 2.050(3) . ?
Ni1 O5 2.049(3) . ?
Ni1 O7 2.023(3) . ?
Ni1 O15 2.045(3) . ?
Ni1 N1 2.105(4) . ?
Ni1 N2 2.106(4) . ?
O1 C1 1.450(5) . ?
O1 C2 1.387(6) . ?
O2 C7 1.333(5) . ?
O3 N1 1.417(5) . ?
O3 C9 1.411(7) . ?
O4 N2 1.426(5) . ?
O4 C10 1.437(7) . ?
O5 C13 1.326(5) . ?
O6 C14 1.383(6) . ?
O6 C18 1.452(5) . ?
O7 C22 1.261(5) . ?
O8 C22 1.266(5) . ?
O9 N3 1.278(5) . ?
O10 N3 1.297(5) . ?
O11 N3 1.208(5) . ?
O12 N4 1.272(5) . ?
O13 N4 1.266(5) . ?
O14 N4 1.198(5) . ?
O15 C19 1.229(5) . ?
N1 C8 1.274(6) . ?
N2 C11 1.286(7) . ?
N5 C19 1.284(6) . ?
N5 C20 1.412(8) . ?
N5 C21 1.431(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.377(7) . ?
C2 C7 1.404(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.369(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.378(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.404(7) . ?
C6 C7 1.395(6) . ?
C6 C8 1.440(7) . ?
C8 H8 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.504(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11 0.9300 . ?
C11 C12 1.426(8) . ?
C12 C13 1.385(7) . ?
C12 C17 1.412(8) . ?
C13 C14 1.402(7) . ?
C14 C15 1.385(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.374(8) . ?
C16 H16 0.9300 . ?
C16 C17 1.344(9) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.488(6) . ?
C23 C24 1.398(6) . ?
C23 C25 1.376(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.382(6) 2_665 ?
C25 C24 1.382(6) 2_665 ?
C25 H25 0.9300 . ?

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 Tb1 Ni1 100.27(7) . . ?
O1 Tb1 O6 147.13(11) . . ?
O1 Tb1 O9 82.45(11) . . ?
O1 Tb1 O13 123.23(11) . . ?
O1 Tb1 N3 76.13(12) . . ?
O1 Tb1 N4 97.57(12) . . ?
O2 Tb1 Ni1 36.30(7) . . ?
O2 Tb1 O1 65.20(10) . . ?
O2 Tb1 O6 123.08(11) . . ?
O2 Tb1 O9 74.05(10) . . ?
O2 Tb1 O10 115.76(11) . . ?
O2 Tb1 O12 129.32(12) . . ?
O2 Tb1 O13 150.55(11) . . ?
O2 Tb1 N3 94.39(11) . . ?
O2 Tb1 N4 144.59(12) . . ?
O5 Tb1 Ni1 35.78(8) . . ?
O5 Tb1 O1 135.77(11) . . ?
O5 Tb1 O2 70.68(11) . . ?
O5 Tb1 O6 64.70(11) . . ?
O5 Tb1 O8 79.00(11) . . ?
O5 Tb1 O9 88.64(11) . . ?
O5 Tb1 O10 130.85(12) . . ?
O5 Tb1 O12 141.13(11) . . ?
O5 Tb1 O13 94.30(11) . . ?
O5 Tb1 N3 110.93(13) . . ?
O5 Tb1 N4 117.38(12) . . ?
O6 Tb1 Ni1 97.98(8) . . ?
O6 Tb1 N3 71.64(12) . . ?
O6 Tb1 N4 88.63(12) . . ?
O8 Tb1 Ni1 67.17(8) . . ?
O8 Tb1 O1 87.64(11) . . ?
O8 Tb1 O2 76.19(11) . . ?
O8 Tb1 O6 124.77(11) . . ?
O8 Tb1 O9 150.12(11) . . ?
O8 Tb1 O10 149.55(12) . . ?
O8 Tb1 O12 75.84(11) . . ?
O8 Tb1 O13 76.12(12) . . ?
O8 Tb1 N3 163.58(13) . . ?
O8 Tb1 N4 72.23(11) . . ?
O9 Tb1 Ni1 86.92(8) . . ?
O9 Tb1 O6 71.46(11) . . ?
O9 Tb1 O13 132.39(12) . . ?
O9 Tb1 N3 26.03(11) . . ?
O9 Tb1 N4 136.93(11) . . ?
O10 Tb1 Ni1 139.24(9) . . ?
O10 Tb1 O1 74.25(12) . . ?
O10 Tb1 O6 74.06(12) . . ?
O10 Tb1 O9 52.43(11) . . ?
O10 Tb1 O13 93.34(12) . . ?
O10 Tb1 N3 26.44(11) . . ?
O10 Tb1 N4 85.88(12) . . ?
O12 Tb1 Ni1 142.61(9) . . ?
O12 Tb1 O1 72.24(11) . . ?
O12 Tb1 O6 107.60(12) . . ?
O12 Tb1 O9 126.59(11) . . ?
O12 Tb1 O10 75.40(12) . . ?
O12 Tb1 O13 51.15(12) . . ?
O12 Tb1 N3 101.06(13) . . ?
O12 Tb1 N4 25.66(11) . . ?
O13 Tb1 Ni1 120.91(8) . . ?
O13 Tb1 O6 67.25(12) . . ?
O13 Tb1 N3 114.85(12) . . ?
O13 Tb1 N4 25.66(11) . . ?
N3 Tb1 Ni1 112.82(10) . . ?
N3 Tb1 N4 111.94(13) . . ?
N4 Tb1 Ni1 134.54(8) . . ?
O2 Ni1 Tb1 42.59(8) . . ?
O2 Ni1 N1 87.00(15) . . ?
O2 Ni1 N2 165.87(15) . . ?
O5 Ni1 Tb1 40.08(8) . . ?
O5 Ni1 O2 80.98(12) . . ?
O5 Ni1 N1 167.54(14) . . ?
O5 Ni1 N2 85.03(15) . . ?
O7 Ni1 Tb1 82.58(8) . . ?
O7 Ni1 O2 89.54(12) . . ?
O7 Ni1 O5 92.98(12) . . ?
O7 Ni1 O15 175.71(12) . . ?
O7 Ni1 N1 90.17(14) . . ?
O7 Ni1 N2 89.24(15) . . ?
O15 Ni1 Tb1 100.75(9) . . ?
O15 Ni1 O2 94.75(12) . . ?
O15 Ni1 O5 87.94(12) . . ?
O15 Ni1 N1 89.82(15) . . ?
O15 Ni1 N2 86.66(15) . . ?
N1 Ni1 Tb1 128.78(12) . . ?
N1 Ni1 N2 107.08(17) . . ?
N2 Ni1 Tb1 123.33(12) . . ?
C1 O1 Tb1 125.2(3) . . ?
C2 O1 Tb1 117.0(3) . . ?
C2 O1 C1 116.2(4) . . ?
Ni1 O2 Tb1 101.11(13) . . ?
C7 O2 Tb1 120.3(3) . . ?
C7 O2 Ni1 125.6(3) . . ?
C9 O3 N1 111.4(4) . . ?
N2 O4 C10 109.2(4) . . ?
Ni1 O5 Tb1 104.14(13) . . ?
C13 O5 Tb1 127.4(3) . . ?
C13 O5 Ni1 124.5(3) . . ?
C14 O6 Tb1 116.4(3) . . ?
C14 O6 C18 117.7(4) . . ?
C18 O6 Tb1 125.2(3) . . ?
C22 O7 Ni1 126.8(3) . . ?
C22 O8 Tb1 136.2(3) . . ?
N3 O9 Tb1 95.9(3) . . ?
N3 O10 Tb1 96.1(3) . . ?
N4 O12 Tb1 97.9(3) . . ?
N4 O13 Tb1 95.5(3) . . ?
C19 O15 Ni1 123.9(3) . . ?
O3 N1 Ni1 125.4(3) . . ?
C8 N1 Ni1 125.4(3) . . ?
C8 N1 O3 109.1(4) . . ?
O4 N2 Ni1 125.6(4) . . ?
C11 N2 Ni1 124.4(4) . . ?
C11 N2 O4 110.0(5) . . ?
O9 N3 Tb1 58.1(2) . . ?
O9 N3 O10 115.5(4) . . ?
O10 N3 Tb1 57.5(2) . . ?
O11 N3 Tb1 178.0(4) . . ?
O11 N3 O9 122.0(5) . . ?
O11 N3 O10 122.5(5) . . ?
O12 N4 Tb1 56.5(2) . . ?
O13 N4 Tb1 58.9(2) . . ?
O13 N4 O12 114.8(4) . . ?
O14 N4 Tb1 173.0(4) . . ?
O14 N4 O12 122.5(5) . . ?
O14 N4 O13 122.7(5) . . ?
C19 N5 C20 118.9(5) . . ?
C19 N5 C21 122.5(5) . . ?
C20 N5 C21 117.7(5) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C7 113.4(4) . . ?
C3 C2 O1 124.4(5) . . ?
C3 C2 C7 122.2(5) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.5(5) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.9(5) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C8 116.4(5) . . ?
C7 C6 C5 119.5(5) . . ?
C7 C6 C8 124.0(5) . . ?
O2 C7 C2 118.5(4) . . ?
O2 C7 C6 123.8(4) . . ?
C6 C7 C2 117.7(5) . . ?
N1 C8 C6 126.7(5) . . ?
N1 C8 H8 116.6 . . ?
C6 C8 H8 116.6 . . ?
O3 C9 H9A 109.0 . . ?
O3 C9 H9B 109.0 . . ?
O3 C9 C10 112.9(5) . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
O4 C10 C9 113.7(5) . . ?
O4 C10 H10A 108.8 . . ?
O4 C10 H10B 108.8 . . ?
C9 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 H11 116.7 . . ?
N2 C11 C12 126.6(5) . . ?
C12 C11 H11 116.7 . . ?
C13 C12 C11 123.2(5) . . ?
C13 C12 C17 119.2(5) . . ?
C17 C12 C11 117.5(5) . . ?
O5 C13 C12 123.9(5) . . ?
O5 C13 C14 117.5(4) . . ?
C12 C13 C14 118.5(5) . . ?
O6 C14 C13 113.9(4) . . ?
O6 C14 C15 124.9(5) . . ?
C15 C14 C13 121.2(5) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 C14 118.9(6) . . ?
C16 C15 H15 120.6 . . ?
C15 C16 H16 119.3 . . ?
C17 C16 C15 121.4(6) . . ?
C17 C16 H16 119.3 . . ?
C12 C17 H17 119.6 . . ?
C16 C17 C12 120.7(6) . . ?
C16 C17 H17 119.6 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O15 C19 N5 126.3(5) . . ?
O15 C19 H19 116.8 . . ?
N5 C19 H19 116.8 . . ?
N5 C20 H20A 109.5 . . ?
N5 C20 H20B 109.5 . . ?
N5 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N5 C21 H21A 109.5 . . ?
N5 C21 H21B 109.5 . . ?
N5 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O7 C22 O8 125.5(4) . . ?
O7 C22 C23 116.8(4) . . ?
O8 C22 C23 117.7(4) . . ?
C24 C23 C22 119.4(4) . . ?
C25 C23 C22 121.0(4) . . ?
C25 C23 C24 119.5(4) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.1(4) 2_665 . ?
C25 C24 H24 120.0 2_665 . ?
C23 C25 C24 120.4(4) . 2_665 ?
C23 C25 H25 119.8 . . ?
C24 C25 H25 119.8 2_665 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C2 C3 164.6(4) . . . . ?
Tb1 O1 C2 C7 -16.0(5) . . . . ?
Tb1 O2 C7 C2 20.9(5) . . . . ?
Tb1 O2 C7 C6 -160.4(3) . . . . ?
Tb1 O5 C13 C12 175.4(3) . . . . ?
Tb1 O5 C13 C14 -1.3(6) . . . . ?
Tb1 O6 C14 C13 1.4(5) . . . . ?
Tb1 O6 C14 C15 -178.5(4) . . . . ?
Tb1 O8 C22 O7 -17.1(8) . . . . ?
Tb1 O8 C22 C23 162.3(3) . . . . ?
Tb1 O9 N3 O10 3.6(5) . . . . ?
Tb1 O9 N3 O11 -177.6(5) . . . . ?
Tb1 O10 N3 O9 -3.6(5) . . . . ?
Tb1 O10 N3 O11 177.6(5) . . . . ?
Tb1 O12 N4 O13 8.6(4) . . . . ?
Tb1 O12 N4 O14 -171.7(4) . . . . ?
Tb1 O13 N4 O12 -8.4(4) . . . . ?
Tb1 O13 N4 O14 171.9(5) . . . . ?
Ni1 O2 C7 C2 154.9(3) . . . . ?
Ni1 O2 C7 C6 -26.4(6) . . . . ?
Ni1 O5 C13 C12 -30.6(6) . . . . ?
Ni1 O5 C13 C14 152.8(3) . . . . ?
Ni1 O7 C22 O8 16.1(7) . . . . ?
Ni1 O7 C22 C23 -163.3(3) . . . . ?
Ni1 O15 C19 N5 170.2(4) . . . . ?
Ni1 N1 C8 C6 -0.6(7) . . . . ?
Ni1 N2 C11 C12 7.6(8) . . . . ?
O1 C2 C3 C4 -179.4(4) . . . . ?
O1 C2 C7 O2 -2.2(6) . . . . ?
O1 C2 C7 C6 179.0(4) . . . . ?
O3 N1 C8 C6 -178.6(4) . . . . ?
O3 C9 C10 O4 -135.5(5) . . . . ?
O4 N2 C11 C12 -174.0(5) . . . . ?
O5 C13 C14 O6 -0.3(6) . . . . ?
O5 C13 C14 C15 179.6(4) . . . . ?
O6 C14 C15 C16 179.3(5) . . . . ?
O7 C22 C23 C24 -9.2(7) . . . . ?
O7 C22 C23 C25 168.1(4) . . . . ?
O8 C22 C23 C24 171.4(4) . . . . ?
O8 C22 C23 C25 -11.4(7) . . . . ?
N1 O3 C9 C10 61.3(6) . . . . ?
N2 O4 C10 C9 60.1(6) . . . . ?
N2 C11 C12 C13 14.0(9) . . . . ?
N2 C11 C12 C17 -168.9(5) . . . . ?
C1 O1 C2 C3 -1.8(6) . . . . ?
C1 O1 C2 C7 177.6(4) . . . . ?
C2 C3 C4 C5 -1.2(8) . . . . ?
C3 C2 C7 O2 177.3(4) . . . . ?
C3 C2 C7 C6 -1.5(7) . . . . ?
C3 C4 C5 C6 1.5(8) . . . . ?
C4 C5 C6 C7 -1.9(8) . . . . ?
C4 C5 C6 C8 -179.3(5) . . . . ?
C5 C6 C7 O2 -176.9(4) . . . . ?
C5 C6 C7 C2 1.8(7) . . . . ?
C5 C6 C8 N1 -168.5(5) . . . . ?
C7 C2 C3 C4 1.2(7) . . . . ?
C7 C6 C8 N1 14.2(8) . . . . ?
C8 C6 C7 O2 0.4(7) . . . . ?
C8 C6 C7 C2 179.1(4) . . . . ?
C9 O3 N1 Ni1 10.7(5) . . . . ?
C9 O3 N1 C8 -171.4(4) . . . . ?
C10 O4 N2 Ni1 16.0(5) . . . . ?
C10 O4 N2 C11 -162.4(5) . . . . ?
C11 C12 C13 O5 -1.9(8) . . . . ?
C11 C12 C13 C14 174.7(5) . . . . ?
C11 C12 C17 C16 -177.6(6) . . . . ?
C12 C13 C14 O6 -177.1(4) . . . . ?
C12 C13 C14 C15 2.8(7) . . . . ?
C13 C12 C17 C16 -0.4(9) . . . . ?
C13 C14 C15 C16 -0.6(8) . . . . ?
C14 C15 C16 C17 -2.3(9) . . . . ?
C15 C16 C17 C12 2.8(10) . . . . ?
C17 C12 C13 O5 -178.9(5) . . . . ?
C17 C12 C13 C14 -2.3(7) . . . . ?
C18 O6 C14 C13 172.7(4) . . . . ?
C18 O6 C14 C15 -7.2(7) . . . . ?
C20 N5 C19 O15 8.4(10) . . . . ?
C21 N5 C19 O15 177.2(6) . . . . ?
C22 C23 C24 C25 178.1(4) . . . 2_665 ?
C22 C23 C25 C24 -178.0(4) . . . 2_665 ?
C24 C23 C25 C24 -0.8(8) . . . 2_665 ?
C25 C23 C24 C25 0.8(8) . . . 2_665 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 11.9 0.3 ?
2 0.361 0.271 0.692 167.3 0.5 ?
3 -0.361 0.729 0.308 167.3 1.5 ?

_olex2_date_sample_data_collection 2015-07-03
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_d729
_database_code_depnum_ccdc_archive 'CCDC 1434590'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_audit_creation_date             2015-10-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C50 H54 Dy2 N10 Ni2 O30'
_chemical_formula_sum            'C50 H54 Dy2 N10 Ni2 O30'
_chemical_formula_weight         1717.45
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6782(12)
_cell_length_b                   12.6632(11)
_cell_length_c                   14.0108(12)
_cell_angle_alpha                98.892(7)
_cell_angle_beta                 94.930(8)
_cell_angle_gamma                101.762(8)
_cell_volume                     1818.9(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4574
_cell_measurement_temperature    293.33(10)
_cell_measurement_theta_max      26.7580
_cell_measurement_theta_min      3.7490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14126
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.445
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.33(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -10.00   45.50   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -38.0000   30.0000 37

#__ type_ start__ end____ width___ exp.time_
  2 omega  -19.00   62.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -99.0000   60.0000 54

#__ type_ start__ end____ width___ exp.time_
  3 omega   -4.00   23.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000 -150.0000 18

#__ type_ start__ end____ width___ exp.time_
  4 omega  -35.00   -5.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479   57.0000  -60.0000 20

#__ type_ start__ end____ width___ exp.time_
  5 omega   -6.00   24.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   77.0000 -180.0000 20

#__ type_ start__ end____ width___ exp.time_
  6 omega  -45.00   37.50   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000  -60.0000 55

#__ type_ start__ end____ width___ exp.time_
  7 omega  -47.00   41.50   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000 -180.0000 59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0592344000
_diffrn_orient_matrix_UB_12      -0.0021733000
_diffrn_orient_matrix_UB_13      -0.0187186000
_diffrn_orient_matrix_UB_21      -0.0179581000
_diffrn_orient_matrix_UB_22      0.0270467000
_diffrn_orient_matrix_UB_23      -0.0380049000
_diffrn_orient_matrix_UB_31      0.0290028000
_diffrn_orient_matrix_UB_32      0.0514024000
_diffrn_orient_matrix_UB_33      0.0295026000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5917
_reflns_number_total             7144
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7144
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0274P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0839
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C14(H14), C15(H15), C16(H16),
 C21(H21), C22(H22), C23(H23)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.37429(2) 0.24601(2) 0.19143(2) 0.04129(8) Uani 1 1 d . . . . .
Ni1 Ni 0.15834(5) 0.23769(4) 0.35631(4) 0.04390(15) Uani 1 1 d . . . . .
O1 O 0.2701(3) 0.0810(2) 0.0710(2) 0.0557(8) Uani 1 1 d . . . . .
O2 O 0.1656(3) 0.1659(2) 0.21649(19) 0.0418(7) Uani 1 1 d . . . . .
O3 O -0.1110(4) 0.1337(4) 0.4165(3) 0.0969(13) Uani 1 1 d . . . . .
O4 O 0.1510(5) 0.3009(4) 0.5830(3) 0.0928(13) Uani 1 1 d . . . . .
O5 O 0.3212(3) 0.3381(2) 0.3275(2) 0.0472(7) Uani 1 1 d . . . . .
O6 O 0.4651(3) 0.4518(2) 0.2239(3) 0.0629(9) Uani 1 1 d . . . . .
O7 O 0.4055(3) 0.1338(2) 0.3009(2) 0.0532(8) Uani 1 1 d . . . . .
O8 O 0.2573(3) 0.1326(2) 0.4054(2) 0.0524(8) Uani 1 1 d . . . . .
O9 O 0.0569(3) 0.3502(2) 0.3184(2) 0.0575(8) Uani 1 1 d . . . . .
O10 O 0.2312(3) 0.3316(3) 0.0948(3) 0.0646(9) Uani 1 1 d . . . . .
O11 O 0.4015(4) 0.2984(3) 0.0314(3) 0.0739(10) Uani 1 1 d . . . . .
O12 O 0.2639(5) 0.3708(4) -0.0473(3) 0.1211(19) Uani 1 1 d . . . . .
O13 O 0.5448(3) 0.1585(3) 0.1325(3) 0.0715(10) Uani 1 1 d . . . . .
O14 O 0.6107(3) 0.2962(3) 0.2456(3) 0.0745(11) Uani 1 1 d . . . . .
O15 O 0.7417(4) 0.1934(4) 0.1975(4) 0.1152(17) Uani 1 1 d . . . . .
N1 N -0.0180(4) 0.1247(4) 0.3520(3) 0.0606(11) Uani 1 1 d . . . . .
N2 N 0.1961(4) 0.3342(4) 0.4971(3) 0.0633(11) Uani 1 1 d . . . . .
N3 N -0.0318(5) 0.4308(4) 0.2073(3) 0.0763(14) Uani 1 1 d . . . . .
N4 N 0.2976(5) 0.3345(4) 0.0236(4) 0.0724(13) Uani 1 1 d . . . . .
N5 N 0.6361(4) 0.2157(4) 0.1921(3) 0.0660(12) Uani 1 1 d . . . . .
C1 C 0.1100(4) 0.0624(3) 0.1744(3) 0.0439(10) Uani 1 1 d . . . . .
C2 C 0.1629(5) 0.0149(4) 0.0943(3) 0.0501(11) Uani 1 1 d . . . . .
C3 C 0.1077(6) -0.0903(4) 0.0452(4) 0.0699(16) Uani 1 1 d . . . . .
H3 H 0.1427 -0.1200 -0.0084 0.084 Uiso 1 1 calc R . . . .
C4 C 0.0020(7) -0.1502(5) 0.0756(5) 0.088(2) Uani 1 1 d . . . . .
H4 H -0.0340 -0.2211 0.0428 0.106 Uiso 1 1 calc R . . . .
C5 C -0.0511(6) -0.1078(4) 0.1529(5) 0.0832(19) Uani 1 1 d . . . . .
H5 H -0.1231 -0.1501 0.1723 0.100 Uiso 1 1 calc R . . . .
C6 C 0.0017(5) 0.0016(4) 0.2058(4) 0.0553(12) Uani 1 1 d . . . . .
C7 C -0.0610(5) 0.0393(4) 0.2870(4) 0.0642(14) Uani 1 1 d . . . . .
H7 H -0.1412 -0.0028 0.2928 0.077 Uiso 1 1 calc R . . . .
C8 C -0.0651(6) 0.2164(6) 0.4960(5) 0.0900(19) Uani 1 1 d . . . . .
H8A H -0.1338 0.2204 0.5366 0.108 Uiso 1 1 calc R . . . .
H8B H -0.0440 0.2854 0.4729 0.108 Uiso 1 1 calc R . . . .
C9 C 0.0535(7) 0.2038(6) 0.5592(4) 0.094(2) Uani 1 1 d . . . . .
H9A H 0.0270 0.1814 0.6189 0.112 Uiso 1 1 calc R . . . .
H9B H 0.0888 0.1461 0.5250 0.112 Uiso 1 1 calc R . . . .
C10 C 0.2622(6) 0.4325(5) 0.5179(4) 0.0723(17) Uani 1 1 d . . . . .
H10 H 0.2655 0.4686 0.5815 0.087 Uiso 1 1 calc R . . . .
C11 C 0.3324(6) 0.4936(4) 0.4530(4) 0.0644(14) Uani 1 1 d . . . . .
C12 C 0.3603(5) 0.4452(4) 0.3625(3) 0.0532(12) Uani 1 1 d . . . . .
C13 C 0.4382(5) 0.5097(4) 0.3090(4) 0.0595(13) Uani 1 1 d . . . . .
C14 C 0.4830(6) 0.6200(4) 0.3411(5) 0.0834(19) Uani 1 1 d . . . . .
H14 H 0.5336 0.6624 0.3041 0.100 Uiso 1 1 calc R . . . .
C15 C 0.4519(8) 0.6677(5) 0.4296(6) 0.111(3) Uani 1 1 d . . . . .
H15 H 0.4814 0.7427 0.4512 0.134 Uiso 1 1 calc R . . . .
C16 C 0.3797(7) 0.6075(5) 0.4850(5) 0.092(2) Uani 1 1 d . . . . .
H16 H 0.3610 0.6410 0.5443 0.110 Uiso 1 1 calc R . . . .
C17 C 0.3249(6) 0.0370(5) -0.0132(4) 0.0774(17) Uani 1 1 d . . . . .
H17A H 0.4003 0.0888 -0.0221 0.116 Uiso 1 1 calc GR . . . .
H17B H 0.2627 0.0232 -0.0698 0.116 Uiso 1 1 calc GR . . . .
H17C H 0.3482 -0.0303 -0.0034 0.116 Uiso 1 1 calc GR . . . .
C18 C 0.5573(6) 0.5100(4) 0.1691(5) 0.0878(19) Uani 1 1 d . . . . .
H18A H 0.5752 0.4593 0.1164 0.132 Uiso 1 1 calc GR . . . .
H18B H 0.6356 0.5440 0.2111 0.132 Uiso 1 1 calc GR . . . .
H18C H 0.5219 0.5652 0.1435 0.132 Uiso 1 1 calc GR . . . .
C19 C 0.3582(4) 0.1106(3) 0.3775(3) 0.0438(10) Uani 1 1 d . . . . .
C20 C 0.4314(4) 0.0525(3) 0.4412(3) 0.0388(9) Uani 1 1 d . . . . .
C21 C 0.3766(4) 0.0085(3) 0.5146(3) 0.0473(11) Uani 1 1 d . . . . .
H21 H 0.2929 0.0136 0.5245 0.057 Uiso 1 1 calc R . . . .
C22 C 0.5568(4) 0.0434(3) 0.4258(3) 0.0471(11) Uani 1 1 d . . . . .
H22 H 0.5950 0.0724 0.3755 0.056 Uiso 1 1 calc R . . . .
C23 C 0.0162(5) 0.3530(4) 0.2358(4) 0.0611(13) Uani 1 1 d . . . . .
H23 H 0.0197 0.2940 0.1883 0.073 Uiso 1 1 calc R . . . .
C24 C -0.0581(12) 0.5124(7) 0.2786(6) 0.194(5) Uani 1 1 d . . . . .
H24A H -0.1116 0.4785 0.3219 0.291 Uiso 1 1 calc GR . . . .
H24B H -0.1018 0.5594 0.2474 0.291 Uiso 1 1 calc GR . . . .
H24C H 0.0214 0.5549 0.3147 0.291 Uiso 1 1 calc GR . . . .
C25 C -0.0809(9) 0.4258(6) 0.1069(4) 0.125(3) Uani 1 1 d . . . . .
H25A H -0.0460 0.4938 0.0867 0.187 Uiso 1 1 calc GR . . . .
H25B H -0.1731 0.4136 0.1007 0.187 Uiso 1 1 calc GR . . . .
H25C H -0.0560 0.3669 0.0667 0.187 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Ni1 3.3995(7) . ?
Dy1 O1 2.468(3) . ?
Dy1 O2 2.333(3) . ?
Dy1 O5 2.255(3) . ?
Dy1 O6 2.543(3) . ?
Dy1 O7 2.294(3) . ?
Dy1 O10 2.473(3) . ?
Dy1 O11 2.459(3) . ?
Dy1 O13 2.455(3) . ?
Dy1 O14 2.494(3) . ?
Dy1 N4 2.883(5) . ?
Dy1 N5 2.897(5) . ?
Ni1 O2 2.043(3) . ?
Ni1 O5 2.045(3) . ?
Ni1 O8 2.022(3) . ?
Ni1 O9 2.061(3) . ?
Ni1 N1 2.110(4) . ?
Ni1 N2 2.113(4) . ?
O1 C2 1.369(5) . ?
O1 C17 1.447(6) . ?
O2 C1 1.342(4) . ?
O3 N1 1.408(5) . ?
O3 C8 1.384(7) . ?
O4 N2 1.425(5) . ?
O4 C9 1.414(7) . ?
O5 C12 1.335(5) . ?
O6 C13 1.384(6) . ?
O6 C18 1.454(6) . ?
O7 C19 1.274(5) . ?
O8 C19 1.246(5) . ?
O9 C23 1.208(5) . ?
O10 N4 1.273(6) . ?
O11 N4 1.286(6) . ?
O12 N4 1.215(5) . ?
O13 N5 1.248(5) . ?
O14 N5 1.259(5) . ?
O15 N5 1.217(6) . ?
N1 C7 1.278(6) . ?
N2 C10 1.276(6) . ?
N3 C23 1.298(6) . ?
N3 C24 1.411(8) . ?
N3 C25 1.446(7) . ?
C1 C2 1.407(6) . ?
C1 C6 1.398(6) . ?
C2 C3 1.386(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.365(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.354(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.441(7) . ?
C6 C7 1.437(7) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.532(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10 0.9300 . ?
C10 C11 1.444(8) . ?
C11 C12 1.404(7) . ?
C11 C16 1.414(7) . ?
C12 C13 1.393(7) . ?
C13 C14 1.370(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.392(9) . ?
C15 H15 0.9300 . ?
C15 C16 1.350(10) . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.506(6) . ?
C20 C21 1.363(6) . ?
C20 C22 1.399(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.376(6) 2_656 ?
C22 C21 1.376(6) 2_656 ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?

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 Dy1 Ni1 100.38(8) . . ?
O1 Dy1 O6 147.27(11) . . ?
O1 Dy1 O10 82.39(11) . . ?
O1 Dy1 O14 122.95(12) . . ?
O1 Dy1 N4 76.77(12) . . ?
O1 Dy1 N5 97.32(12) . . ?
O2 Dy1 Ni1 36.04(6) . . ?
O2 Dy1 O1 65.50(10) . . ?
O2 Dy1 O6 123.49(10) . . ?
O2 Dy1 O10 74.69(11) . . ?
O2 Dy1 O11 116.64(12) . . ?
O2 Dy1 O13 129.40(11) . . ?
O2 Dy1 O14 150.02(12) . . ?
O2 Dy1 N4 95.57(12) . . ?
O2 Dy1 N5 144.38(11) . . ?
O5 Dy1 Ni1 35.64(7) . . ?
O5 Dy1 O1 135.65(11) . . ?
O5 Dy1 O2 70.22(10) . . ?
O5 Dy1 O6 64.79(11) . . ?
O5 Dy1 O7 78.91(11) . . ?
O5 Dy1 O10 88.48(12) . . ?
O5 Dy1 O11 130.56(12) . . ?
O5 Dy1 O13 141.39(11) . . ?
O5 Dy1 O14 94.80(12) . . ?
O5 Dy1 N4 110.45(14) . . ?
O5 Dy1 N5 118.03(12) . . ?
O6 Dy1 Ni1 98.24(9) . . ?
O6 Dy1 N4 71.18(11) . . ?
O6 Dy1 N5 88.28(12) . . ?
O7 Dy1 Ni1 67.11(8) . . ?
O7 Dy1 O1 88.45(11) . . ?
O7 Dy1 O2 76.35(10) . . ?
O7 Dy1 O6 123.71(11) . . ?
O7 Dy1 O10 150.88(12) . . ?
O7 Dy1 O11 149.70(13) . . ?
O7 Dy1 O13 75.80(12) . . ?
O7 Dy1 O14 75.31(12) . . ?
O7 Dy1 N4 165.11(12) . . ?
O7 Dy1 N5 72.04(12) . . ?
O10 Dy1 Ni1 87.38(9) . . ?
O10 Dy1 O6 71.80(11) . . ?
O10 Dy1 O14 132.38(12) . . ?
O10 Dy1 N4 26.08(13) . . ?
O10 Dy1 N5 136.43(12) . . ?
O11 Dy1 Ni1 139.72(10) . . ?
O11 Dy1 O1 74.49(11) . . ?
O11 Dy1 O6 73.88(12) . . ?
O11 Dy1 O10 52.43(13) . . ?
O11 Dy1 O14 92.96(13) . . ?
O11 Dy1 N4 26.35(13) . . ?
O11 Dy1 N5 85.28(14) . . ?
O13 Dy1 Ni1 142.46(9) . . ?
O13 Dy1 O1 72.35(11) . . ?
O13 Dy1 O6 107.11(12) . . ?
O13 Dy1 O10 126.40(12) . . ?
O13 Dy1 O11 75.23(13) . . ?
O13 Dy1 O14 50.77(11) . . ?
O13 Dy1 N4 100.93(15) . . ?
O13 Dy1 N5 25.27(11) . . ?
O14 Dy1 Ni1 120.85(9) . . ?
O14 Dy1 O6 67.06(12) . . ?
O14 Dy1 N4 114.20(14) . . ?
O14 Dy1 N5 25.63(11) . . ?
N4 Dy1 Ni1 113.40(12) . . ?
N4 Dy1 N5 111.19(15) . . ?
N5 Dy1 Ni1 134.64(9) . . ?
O2 Ni1 Dy1 42.20(8) . . ?
O2 Ni1 O5 80.41(11) . . ?
O2 Ni1 O9 95.22(12) . . ?
O2 Ni1 N1 87.51(15) . . ?
O2 Ni1 N2 165.88(15) . . ?
O5 Ni1 Dy1 39.97(8) . . ?
O5 Ni1 O9 87.92(13) . . ?
O5 Ni1 N1 167.23(14) . . ?
O5 Ni1 N2 85.64(15) . . ?
O8 Ni1 Dy1 82.51(9) . . ?
O8 Ni1 O2 89.63(12) . . ?
O8 Ni1 O5 93.04(12) . . ?
O8 Ni1 O9 175.14(13) . . ?
O8 Ni1 N1 90.98(14) . . ?
O8 Ni1 N2 88.95(14) . . ?
O9 Ni1 Dy1 101.19(10) . . ?
O9 Ni1 N1 89.09(15) . . ?
O9 Ni1 N2 86.38(14) . . ?
N1 Ni1 Dy1 128.99(13) . . ?
N1 Ni1 N2 106.56(18) . . ?
N2 Ni1 Dy1 123.72(13) . . ?
C2 O1 Dy1 117.2(3) . . ?
C2 O1 C17 116.2(3) . . ?
C17 O1 Dy1 125.5(3) . . ?
Ni1 O2 Dy1 101.76(10) . . ?
C1 O2 Dy1 121.0(3) . . ?
C1 O2 Ni1 126.6(3) . . ?
C8 O3 N1 112.0(4) . . ?
C9 O4 N2 110.6(4) . . ?
Ni1 O5 Dy1 104.39(11) . . ?
C12 O5 Dy1 126.9(3) . . ?
C12 O5 Ni1 125.7(3) . . ?
C13 O6 Dy1 116.4(3) . . ?
C13 O6 C18 117.5(4) . . ?
C18 O6 Dy1 125.4(3) . . ?
C19 O7 Dy1 136.2(3) . . ?
C19 O8 Ni1 126.9(3) . . ?
C23 O9 Ni1 124.2(3) . . ?
N4 O10 Dy1 95.3(3) . . ?
N4 O11 Dy1 95.6(3) . . ?
N5 O13 Dy1 97.6(3) . . ?
N5 O14 Dy1 95.4(3) . . ?
O3 N1 Ni1 126.1(4) . . ?
C7 N1 Ni1 125.3(4) . . ?
C7 N1 O3 108.6(4) . . ?
O4 N2 Ni1 125.8(4) . . ?
C10 N2 Ni1 124.8(4) . . ?
C10 N2 O4 109.4(4) . . ?
C23 N3 C24 118.5(5) . . ?
C23 N3 C25 122.1(5) . . ?
C24 N3 C25 118.4(6) . . ?
O10 N4 Dy1 58.7(2) . . ?
O10 N4 O11 116.7(4) . . ?
O11 N4 Dy1 58.1(2) . . ?
O12 N4 Dy1 179.2(4) . . ?
O12 N4 O10 121.0(6) . . ?
O12 N4 O11 122.3(6) . . ?
O13 N5 Dy1 57.1(3) . . ?
O13 N5 O14 115.7(4) . . ?
O14 N5 Dy1 59.0(2) . . ?
O15 N5 Dy1 172.9(4) . . ?
O15 N5 O13 121.3(5) . . ?
O15 N5 O14 123.1(5) . . ?
O2 C1 C2 117.9(4) . . ?
O2 C1 C6 122.9(4) . . ?
C6 C1 C2 119.2(4) . . ?
O1 C2 C1 114.3(4) . . ?
O1 C2 C3 124.7(5) . . ?
C3 C2 C1 120.9(5) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.1(6) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.8(5) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.3(6) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 117.6(5) . . ?
C1 C6 C7 125.1(4) . . ?
C7 C6 C5 117.3(5) . . ?
N1 C7 C6 126.8(5) . . ?
N1 C7 H7 116.6 . . ?
C6 C7 H7 116.6 . . ?
O3 C8 H8A 108.4 . . ?
O3 C8 H8B 108.4 . . ?
O3 C8 C9 115.5(6) . . ?
H8A C8 H8B 107.5 . . ?
C9 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
O4 C9 C8 113.3(5) . . ?
O4 C9 H9A 108.9 . . ?
O4 C9 H9B 108.9 . . ?
C8 C9 H9A 108.9 . . ?
C8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
N2 C10 H10 116.7 . . ?
N2 C10 C11 126.7(5) . . ?
C11 C10 H10 116.7 . . ?
C12 C11 C10 123.5(5) . . ?
C12 C11 C16 118.8(6) . . ?
C16 C11 C10 117.6(6) . . ?
O5 C12 C11 122.8(5) . . ?
O5 C12 C13 118.1(4) . . ?
C13 C12 C11 119.1(4) . . ?
O6 C13 C12 113.8(4) . . ?
C14 C13 O6 124.9(5) . . ?
C14 C13 C12 121.2(6) . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.2(6) . . ?
C15 C14 H14 120.4 . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.4(6) . . ?
C16 C15 H15 119.3 . . ?
C11 C16 H16 119.9 . . ?
C15 C16 C11 120.2(6) . . ?
C15 C16 H16 119.9 . . ?
O1 C17 H17A 109.5 . . ?
O1 C17 H17B 109.5 . . ?
O1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O7 C19 C20 117.3(4) . . ?
O8 C19 O7 126.0(4) . . ?
O8 C19 C20 116.7(4) . . ?
C21 C20 C19 120.5(4) . . ?
C21 C20 C22 119.3(4) . . ?
C22 C20 C19 120.2(4) . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 121.1(4) . 2_656 ?
C22 C21 H21 119.5 2_656 . ?
C20 C22 H22 120.2 . . ?
C21 C22 C20 119.6(4) 2_656 . ?
C21 C22 H22 120.2 2_656 . ?
O9 C23 N3 126.0(5) . . ?
O9 C23 H23 117.0 . . ?
N3 C23 H23 117.0 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C2 C1 13.3(5) . . . . ?
Dy1 O1 C2 C3 -166.8(4) . . . . ?
Dy1 O2 C1 C2 -18.3(5) . . . . ?
Dy1 O2 C1 C6 162.9(3) . . . . ?
Dy1 O5 C12 C11 -173.5(3) . . . . ?
Dy1 O5 C12 C13 2.6(6) . . . . ?
Dy1 O6 C13 C12 -2.2(5) . . . . ?
Dy1 O6 C13 C14 177.1(4) . . . . ?
Dy1 O7 C19 O8 14.3(7) . . . . ?
Dy1 O7 C19 C20 -164.9(3) . . . . ?
Dy1 O10 N4 O11 -1.5(4) . . . . ?
Dy1 O10 N4 O12 179.2(4) . . . . ?
Dy1 O11 N4 O10 1.5(4) . . . . ?
Dy1 O11 N4 O12 -179.2(4) . . . . ?
Dy1 O13 N5 O14 -7.7(5) . . . . ?
Dy1 O13 N5 O15 171.8(5) . . . . ?
Dy1 O14 N5 O13 7.6(5) . . . . ?
Dy1 O14 N5 O15 -171.9(5) . . . . ?
Ni1 O2 C1 C2 -156.1(3) . . . . ?
Ni1 O2 C1 C6 25.0(5) . . . . ?
Ni1 O5 C12 C11 29.5(6) . . . . ?
Ni1 O5 C12 C13 -154.4(3) . . . . ?
Ni1 O8 C19 O7 -14.0(7) . . . . ?
Ni1 O8 C19 C20 165.2(2) . . . . ?
Ni1 O9 C23 N3 -169.7(4) . . . . ?
Ni1 N1 C7 C6 1.4(7) . . . . ?
Ni1 N2 C10 C11 -5.6(8) . . . . ?
O1 C2 C3 C4 178.7(5) . . . . ?
O2 C1 C2 O1 2.2(6) . . . . ?
O2 C1 C2 C3 -177.7(4) . . . . ?
O2 C1 C6 C5 178.4(4) . . . . ?
O2 C1 C6 C7 -1.9(7) . . . . ?
O3 N1 C7 C6 178.2(5) . . . . ?
O3 C8 C9 O4 133.2(5) . . . . ?
O4 N2 C10 C11 175.2(5) . . . . ?
O5 C12 C13 O6 0.1(6) . . . . ?
O5 C12 C13 C14 -179.3(4) . . . . ?
O6 C13 C14 C15 -178.1(5) . . . . ?
O7 C19 C20 C21 -168.7(4) . . . . ?
O7 C19 C20 C22 11.5(6) . . . . ?
O8 C19 C20 C21 12.1(6) . . . . ?
O8 C19 C20 C22 -167.7(4) . . . . ?
N1 O3 C8 C9 -60.1(7) . . . . ?
N2 O4 C9 C8 -60.9(6) . . . . ?
N2 C10 C11 C12 -14.1(9) . . . . ?
N2 C10 C11 C16 168.6(6) . . . . ?
C1 C2 C3 C4 -1.3(8) . . . . ?
C1 C6 C7 N1 -12.1(8) . . . . ?
C2 C1 C6 C5 -0.5(6) . . . . ?
C2 C1 C6 C7 179.2(4) . . . . ?
C2 C3 C4 C5 0.7(9) . . . . ?
C3 C4 C5 C6 0.0(10) . . . . ?
C4 C5 C6 C1 -0.1(8) . . . . ?
C4 C5 C6 C7 -179.8(5) . . . . ?
C5 C6 C7 N1 167.6(5) . . . . ?
C6 C1 C2 O1 -178.8(4) . . . . ?
C6 C1 C2 C3 1.2(7) . . . . ?
C8 O3 N1 Ni1 -10.9(6) . . . . ?
C8 O3 N1 C7 172.4(5) . . . . ?
C9 O4 N2 Ni1 -13.2(6) . . . . ?
C9 O4 N2 C10 166.0(5) . . . . ?
C10 C11 C12 O5 1.7(7) . . . . ?
C10 C11 C12 C13 -174.4(5) . . . . ?
C10 C11 C16 C15 176.5(6) . . . . ?
C11 C12 C13 O6 176.4(4) . . . . ?
C11 C12 C13 C14 -3.1(7) . . . . ?
C12 C11 C16 C15 -1.0(9) . . . . ?
C12 C13 C14 C15 1.3(8) . . . . ?
C13 C14 C15 C16 0.7(10) . . . . ?
C14 C15 C16 C11 -0.8(11) . . . . ?
C16 C11 C12 O5 178.9(5) . . . . ?
C16 C11 C12 C13 2.9(7) . . . . ?
C17 O1 C2 C1 -177.8(4) . . . . ?
C17 O1 C2 C3 2.2(7) . . . . ?
C18 O6 C13 C12 -173.3(4) . . . . ?
C18 O6 C13 C14 6.1(7) . . . . ?
C19 C20 C21 C22 -179.0(3) . . . 2_656 ?
C19 C20 C22 C21 179.1(3) . . . 2_656 ?
C21 C20 C22 C21 -0.7(7) . . . 2_656 ?
C22 C20 C21 C22 0.8(7) . . . 2_656 ?
C24 N3 C23 O9 -10.2(10) . . . . ?
C25 N3 C23 O9 -178.6(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.366 0.229 0.804 188.5 3.0 ?
2 0.000 0.500 0.500 17.0 0.6 ?
3 0.366 0.771 0.196 188.5 1.7 ?

_olex2_date_sample_data_collection 2015-07-02
_olex2_submission_special_instructions 'No special instructions were received'
