# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_Ni2Tb
_database_code_depnum_ccdc_archive 'CCDC 1054073'
_audit_update_record             
;
2016-01-02 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86 H83 Cl0.50 N6.50 Ni2 O16.49 Tb'
_chemical_formula_weight         1765.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   22.819(5)
_cell_length_b                   23.509(6)
_cell_length_c                   18.669(4)
_cell_angle_alpha                90
_cell_angle_beta                 119.960(5)
_cell_angle_gamma                90
_cell_volume                     8677(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5970
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      25.79

_exptl_crystal_description       Needle
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_F_000             3624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    1.318
_shelx_estimated_absorpt_T_min   0.858
_shelx_estimated_absorpt_T_max   0.913
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8755
_exptl_absorpt_correction_T_max  0.9204
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30422
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.346
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7657
_reflns_number_gt                5118
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX-II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
  All the non-hydrogen atoms were refined anisotropically except the solvate
molecules and the hydrogen atoms were refined as riding model.

  There is Q-peak with high density lies in an random position which is not 
further considered for modelling.

  Hydrogen atoms were not added in the solvate molecules, but in the chemical
formula.

  The anions nitrate and halides are partially occupied. For the smooth convergence
of these atoms and other disordered atoms restraints/contraints such as DFIX, DANG,
SIMU, DELU, ISOR, FLAT etc. were used.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1448P)²+173.3099P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7657
_refine_ls_number_parameters     517
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0833
_refine_ls_wR_factor_ref         0.2721
_refine_ls_wR_factor_gt          0.2333
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84838(5) 0.40274(5) 0.73286(6) 0.0125(3) Uani 1 1 d . . . . .
Tb1 Tb 1.0000 0.40236(3) 0.7500 0.0176(2) Uani 1 2 d S T P . .
O11 O 0.8828(3) 0.3967(3) 0.6496(4) 0.0148(13) Uani 1 1 d . . . . .
O12 O 0.9475(3) 0.4054(3) 0.5719(4) 0.0181(14) Uani 1 1 d . . . . .
O31 O 1.0677(3) 0.3517(3) 0.7059(4) 0.0174(14) Uani 1 1 d . . . . .
O32 O 0.9627(3) 0.2903(3) 0.6638(4) 0.0218(15) Uani 1 1 d . . . . .
O51 O 0.9262(3) 0.4599(3) 0.7765(4) 0.0140(13) Uani 1 1 d . . . . .
O52 O 1.0412(3) 0.5103(3) 0.8485(4) 0.0171(14) Uani 1 1 d . . . . .
N11 N 0.7767(4) 0.3388(3) 0.6624(5) 0.0198(18) Uani 1 1 d . . . . .
N31 N 1.1631(4) 0.3960(3) 0.6608(5) 0.0212(18) Uani 1 1 d . . . . .
N51 N 0.7809(4) 0.4724(3) 0.6784(5) 0.0196(18) Uani 1 1 d . . . . .
C11 C 0.7902(5) 0.3448(4) 0.5398(6) 0.022(2) Uani 1 1 d . . . . .
C12 C 0.7614(6) 0.3236(4) 0.4570(6) 0.028(2) Uani 1 1 d . . . . .
H12A H 0.7194 0.3040 0.4326 0.034 Uiso 1 1 calc R U . . .
C13 C 0.7937(5) 0.3312(4) 0.4129(6) 0.029(2) Uani 1 1 d . . . . .
H13A H 0.7738 0.3169 0.3581 0.034 Uiso 1 1 calc R U . . .
C14 C 0.8563(5) 0.3600(4) 0.4476(6) 0.022(2) Uani 1 1 d . . . . .
H14A H 0.8780 0.3655 0.4160 0.026 Uiso 1 1 calc R U . . .
C15 C 0.8857(5) 0.3802(4) 0.5280(6) 0.018(2) Uani 1 1 d . . . . .
C16 C 0.8528(5) 0.3744(4) 0.5747(6) 0.0144(19) Uani 1 1 d . . . . .
C17 C 0.7581(5) 0.3276(4) 0.5858(6) 0.027(2) Uani 1 1 d . . . . .
H17A H 0.7183 0.3053 0.5565 0.033 Uiso 1 1 calc R U . . .
C18 C 0.7370(5) 0.3112(5) 0.6929(6) 0.027(2) Uani 1 1 d . . . . .
C19 C 0.6691(5) 0.3232(5) 0.6617(7) 0.034(3) Uani 1 1 d . . . . .
H19A H 0.6470 0.3494 0.6174 0.041 Uiso 1 1 calc R U . . .
C20 C 0.6327(7) 0.2970(6) 0.6947(8) 0.049(4) Uani 1 1 d . . . . .
H20A H 0.5860 0.3051 0.6724 0.059 Uiso 1 1 calc R U . . .
C21 C 0.6652(7) 0.2594(6) 0.7599(7) 0.048(4) Uani 1 1 d . . . . .
H21A H 0.6410 0.2424 0.7836 0.057 Uiso 1 1 calc R U . . .
C22 C 0.7336(8) 0.2461(5) 0.7910(8) 0.047(3) Uani 1 1 d . . . . .
H22A H 0.7554 0.2196 0.8351 0.056 Uiso 1 1 calc R U . . .
C23 C 0.7698(7) 0.2716(5) 0.7575(7) 0.035(3) Uani 1 1 d . . . . .
H23A H 0.8160 0.2623 0.7780 0.042 Uiso 1 1 calc R U . . .
C24 C 0.9777(5) 0.4273(5) 0.5260(6) 0.025(2) Uani 1 1 d . . . . .
H24A H 1.0217 0.4443 0.5643 0.038 Uiso 1 1 calc R U . . .
H24B H 0.9839 0.3963 0.4954 0.038 Uiso 1 1 calc R U . . .
H24C H 0.9480 0.4564 0.4871 0.038 Uiso 1 1 calc R U . . .
C31 C 1.0840(5) 0.3161(4) 0.5973(6) 0.025(2) Uani 1 1 d . . . . .
C32 C 1.0617(6) 0.2755(5) 0.5317(6) 0.032(3) Uani 1 1 d . . . . .
H32A H 1.0818 0.2756 0.4977 0.039 Uiso 1 1 calc R U . . .
C33 C 1.0126(6) 0.2368(5) 0.5165(7) 0.038(3) Uani 1 1 d . . . . .
H33A H 1.0019 0.2080 0.4762 0.046 Uiso 1 1 calc R U . . .
C34 C 0.9774(6) 0.2396(5) 0.5609(7) 0.031(3) Uani 1 1 d . . . . .
H34A H 0.9417 0.2137 0.5489 0.037 Uiso 1 1 calc R U . . .
C35 C 0.9954(5) 0.2797(4) 0.6209(6) 0.021(2) Uani 1 1 d . . . . .
C36 C 1.0506(5) 0.3175(4) 0.6430(6) 0.019(2) Uani 1 1 d . . . . .
C37 C 1.1354(6) 0.3555(5) 0.6074(7) 0.029(2) Uani 1 1 d . . . . .
H37A H 1.1391 0.3606 0.5566 0.034 Uiso 1 1 calc R U . A 1
C38 C 1.2117(3) 0.4282(3) 0.6510(4) 0.027(2) Uani 1 1 d G U . . .
C39 C 1.2679(3) 0.4000(2) 0.6580(5) 0.028(2) Uani 1 1 d G U . . .
H39A H 1.2726 0.3601 0.6679 0.034 Uiso 1 1 calc R U . . .
C40 C 1.3171(3) 0.4299(3) 0.6506(5) 0.033(2) Uani 1 1 d G U . . .
H40A H 1.3554 0.4106 0.6554 0.040 Uiso 1 1 calc R U . . .
C41 C 1.3101(3) 0.4882(3) 0.6361(5) 0.034(2) Uani 1 1 d G U . . .
H41A H 1.3437 0.5087 0.6310 0.041 Uiso 1 1 calc R U . . .
C42 C 1.2540(3) 0.5165(2) 0.6290(4) 0.031(2) Uani 1 1 d G U . . .
H42A H 1.2492 0.5563 0.6191 0.038 Uiso 1 1 calc R U . . .
C43 C 1.2048(3) 0.4865(3) 0.6364(4) 0.027(2) Uani 1 1 d G U . . .
H43A H 1.1664 0.5058 0.6316 0.032 Uiso 1 1 calc R U . . .
C44 C 0.9146(5) 0.2484(5) 0.6589(7) 0.030(2) Uani 1 1 d . . . . .
H44A H 0.8947 0.2609 0.6921 0.045 Uiso 1 1 calc R U . . .
H44B H 0.8789 0.2439 0.6012 0.045 Uiso 1 1 calc R U . . .
H44C H 0.9377 0.2119 0.6800 0.045 Uiso 1 1 calc R U . . .
C51 C 0.8645(5) 0.5481(4) 0.7533(6) 0.020(2) Uani 1 1 d . . . . .
C52 C 0.8692(5) 0.6072(4) 0.7678(6) 0.022(2) Uani 1 1 d . . . . .
H52A H 0.8289 0.6289 0.7477 0.026 Uiso 1 1 calc R U . . .
C53 C 0.9310(5) 0.6342(4) 0.8107(6) 0.024(2) Uani 1 1 d . . . . .
H53A H 0.9328 0.6742 0.8193 0.029 Uiso 1 1 calc R U . . .
C54 C 0.9907(5) 0.6031(4) 0.8413(6) 0.018(2) Uani 1 1 d . . . . .
H54A H 1.0333 0.6215 0.8717 0.022 Uiso 1 1 calc R U . . .
C55 C 0.9874(5) 0.5452(4) 0.8269(6) 0.017(2) Uani 1 1 d . . . . .
C56 C 0.9239(5) 0.5155(4) 0.7845(5) 0.0167(19) Uani 1 1 d . . . . .
C57 C 0.7984(5) 0.5244(4) 0.7018(6) 0.017(2) Uani 1 1 d . . . . .
H57A H 0.7621 0.5508 0.6821 0.020 Uiso 1 1 calc R U . . .
C58 C 0.7093(5) 0.4631(4) 0.6225(6) 0.021(2) Uani 1 1 d . . . . .
C59 C 0.6631(5) 0.4736(5) 0.6496(7) 0.028(2) Uani 1 1 d . . . . .
H59A H 0.6780 0.4878 0.7037 0.033 Uiso 1 1 calc R U . . .
C60 C 0.5944(6) 0.4629(6) 0.5952(7) 0.041(3) Uani 1 1 d . . . . .
H60A H 0.5627 0.4676 0.6135 0.049 Uiso 1 1 calc R U . . .
C61 C 0.5721(6) 0.4453(5) 0.5139(7) 0.038(3) Uani 1 1 d . . . . .
H61A H 0.5253 0.4392 0.4768 0.045 Uiso 1 1 calc R U . . .
C62 C 0.6189(5) 0.4368(5) 0.4879(7) 0.033(3) Uani 1 1 d . . . . .
H62A H 0.6041 0.4246 0.4330 0.039 Uiso 1 1 calc R U . . .
C63 C 0.6871(5) 0.4462(5) 0.5423(6) 0.026(2) Uani 1 1 d . . . . .
H63A H 0.7189 0.4409 0.5240 0.032 Uiso 1 1 calc R U . . .
C64 C 1.1067(5) 0.5313(5) 0.9085(6) 0.025(2) Uani 1 1 d . . . . .
H64A H 1.1410 0.5024 0.9188 0.038 Uiso 1 1 calc R U . . .
H64B H 1.1167 0.5660 0.8875 0.038 Uiso 1 1 calc R U . . .
H64C H 1.1072 0.5398 0.9602 0.038 Uiso 1 1 calc R U . . .
Cl1 Cl 1.0819(4) 0.3984(4) 0.6126(5) 0.018(2) Uani 0.264(8) 1 d . U P B 1
O72 O 0.4853(11) 0.4889(9) 0.6794(9) 0.068(7) Uani 0.472(15) 1 d D U P B 2
N71 N 0.5000 0.4670(10) 0.7500 0.066(8) Uani 0.472(15) 2 d DS TU P B 2
O71 O 0.5000 0.4106(10) 0.7500 0.067(8) Uani 0.472(15) 2 d DS TU P B 2
O1S O 0.4562(12) 0.2552(10) 0.6691(13) 0.079(7) Uiso 0.5 1 d D U P . .
O2WS O 0.3369(15) 0.1859(13) 0.5655(18) 0.032(7) Uiso 0.25 1 d . . P . .
C1S C 0.5000 0.279(2) 0.7500 0.108(15) Uiso 0.5 2 d DS U P . .
O2S O 0.4513(13) 0.3660(12) 0.5958(15) 0.093(8) Uiso 0.5 1 d D U P . .
C2S C 0.4064(16) 0.3952(13) 0.5203(17) 0.064(8) Uiso 0.5 1 d D U P . .
O3S O 0.590(2) 0.618(2) 0.718(3) 0.068(11) Uiso 0.25 1 d D U P . .
C3S C 0.549(3) 0.606(3) 0.754(4) 0.071(15) Uiso 0.25 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O51 2.044(6) . ?
Ni1 O31 2.057(6) 2_756 ?
Ni1 O11 2.068(6) . ?
Ni1 N11 2.125(8) . ?
Ni1 N51 2.127(8) . ?
Ni1 N31 2.133(8) 2_756 ?
Ni1 Cl1 2.505(8) 2_756 ?
Ni1 Tb1 3.3117(13) . ?
Tb1 O11 2.382(6) 2_756 ?
Tb1 O11 2.382(6) . ?
Tb1 O51 2.396(6) 2_756 ?
Tb1 O51 2.396(6) . ?
Tb1 O31 2.398(6) . ?
Tb1 O31 2.398(6) 2_756 ?
Tb1 O12 2.918(7) . ?
Tb1 O12 2.918(7) 2_756 ?
Tb1 Ni1 3.3117(13) 2_756 ?
O11 C16 1.320(11) . ?
O12 C15 1.362(11) . ?
O12 C24 1.436(11) . ?
O31 C36 1.312(11) . ?
O31 Ni1 2.057(6) 2_756 ?
O32 C35 1.363(12) . ?
O32 C44 1.443(12) . ?
O51 C56 1.319(11) . ?
O52 C55 1.360(11) . ?
O52 C64 1.435(11) . ?
N11 C17 1.300(13) . ?
N11 C18 1.443(13) . ?
N31 C37 1.292(13) . ?
N31 C38 1.431(9) . ?
N31 Cl1 1.606(12) . ?
N31 Ni1 2.133(8) 2_756 ?
N51 C57 1.291(12) . ?
N51 C58 1.450(12) . ?
C11 C16 1.420(13) . ?
C11 C12 1.435(13) . ?
C11 C17 1.437(14) . ?
C12 C13 1.363(16) . ?
C12 H12A 0.9500 . ?
C13 C14 1.411(14) . ?
C13 H13A 0.9500 . ?
C14 C15 1.386(13) . ?
C14 H14A 0.9500 . ?
C15 C16 1.415(13) . ?
C17 H17A 0.9500 . ?
C18 C19 1.384(15) . ?
C18 C23 1.408(16) . ?
C19 C20 1.400(17) . ?
C19 H19A 0.9500 . ?
C20 C21 1.38(2) . ?
C20 H20A 0.9500 . ?
C21 C22 1.40(2) . ?
C21 H21A 0.9500 . ?
C22 C23 1.396(16) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C36 1.399(13) . ?
C31 C32 1.432(14) . ?
C31 C37 1.432(15) . ?
C31 Cl1 1.961(13) . ?
C32 C33 1.358(16) . ?
C32 H32A 0.9500 . ?
C33 C34 1.412(16) . ?
C33 H33A 0.9500 . ?
C34 C35 1.362(14) . ?
C34 H34A 0.9500 . ?
C35 C36 1.423(14) . ?
C36 Cl1 2.204(13) . ?
C37 Cl1 1.625(14) . ?
C37 H37A 1.0000 . ?
C38 C39 1.3900 . ?
C38 C43 1.3900 . ?
C39 C40 1.3900 . ?
C39 H39A 0.9500 . ?
C40 C41 1.3900 . ?
C40 H40A 0.9500 . ?
C41 C42 1.3900 . ?
C41 H41A 0.9500 . ?
C42 C43 1.3900 . ?
C42 H42A 0.9500 . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C51 C56 1.406(13) . ?
C51 C52 1.408(14) . ?
C51 C57 1.438(14) . ?
C52 C53 1.380(15) . ?
C52 H52A 0.9500 . ?
C53 C54 1.393(14) . ?
C53 H53A 0.9500 . ?
C54 C55 1.384(13) . ?
C54 H54A 0.9500 . ?
C55 C56 1.438(13) . ?
C57 H57A 0.9500 . ?
C58 C63 1.379(14) . ?
C58 C59 1.402(14) . ?
C59 C60 1.401(16) . ?
C59 H59A 0.9500 . ?
C60 C61 1.399(17) . ?
C60 H60A 0.9500 . ?
C61 C62 1.390(16) . ?
C61 H61A 0.9500 . ?
C62 C63 1.388(15) . ?
C62 H62A 0.9500 . ?
C63 H63A 0.9500 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
Cl1 Ni1 2.505(8) 2_756 ?
O72 N71 1.293(9) . ?
N71 O72 1.293(9) 2_656 ?
N71 O71 1.324(10) . ?
O1S C1S 1.445(10) . ?
C1S O1S 1.445(10) 2_656 ?
O2S C2S 1.437(10) . ?
O3S C3S 1.433(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O51 Ni1 O31 77.3(2) . 2_756 ?
O51 Ni1 O11 76.3(2) . . ?
O31 Ni1 O11 77.3(2) 2_756 . ?
O51 Ni1 N11 163.4(3) . . ?
O31 Ni1 N11 98.4(3) 2_756 . ?
O11 Ni1 N11 87.1(3) . . ?
O51 Ni1 N51 87.8(3) . . ?
O31 Ni1 N51 165.0(3) 2_756 . ?
O11 Ni1 N51 98.6(3) . . ?
N11 Ni1 N51 95.7(3) . . ?
O51 Ni1 N31 99.4(3) . 2_756 ?
O31 Ni1 N31 87.3(3) 2_756 2_756 ?
O11 Ni1 N31 164.5(3) . 2_756 ?
N11 Ni1 N31 96.3(3) . 2_756 ?
N51 Ni1 N31 96.1(3) . 2_756 ?
O51 Ni1 Cl1 69.0(3) . 2_756 ?
O31 Ni1 Cl1 57.1(3) 2_756 2_756 ?
O11 Ni1 Cl1 127.0(3) . 2_756 ?
N11 Ni1 Cl1 122.3(3) . 2_756 ?
N51 Ni1 Cl1 118.2(3) . 2_756 ?
N31 Ni1 Cl1 39.5(3) 2_756 2_756 ?
O51 Ni1 Tb1 46.01(16) . . ?
O31 Ni1 Tb1 46.09(17) 2_756 . ?
O11 Ni1 Tb1 45.67(17) . . ?
N11 Ni1 Tb1 120.1(2) . . ?
N51 Ni1 Tb1 121.3(2) . . ?
N31 Ni1 Tb1 121.2(2) 2_756 . ?
Cl1 Ni1 Tb1 81.7(2) 2_756 . ?
O11 Tb1 O11 173.6(3) 2_756 . ?
O11 Tb1 O51 64.2(2) 2_756 2_756 ?
O11 Tb1 O51 119.8(2) . 2_756 ?
O11 Tb1 O51 119.8(2) 2_756 . ?
O11 Tb1 O51 64.2(2) . . ?
O51 Tb1 O51 111.3(3) 2_756 . ?
O11 Tb1 O31 65.2(2) 2_756 . ?
O11 Tb1 O31 111.4(2) . . ?
O51 Tb1 O31 64.6(2) 2_756 . ?
O51 Tb1 O31 172.2(2) . . ?
O11 Tb1 O31 111.4(2) 2_756 2_756 ?
O11 Tb1 O31 65.2(2) . 2_756 ?
O51 Tb1 O31 172.2(2) 2_756 2_756 ?
O51 Tb1 O31 64.6(2) . 2_756 ?
O31 Tb1 O31 120.4(3) . 2_756 ?
O11 Tb1 O12 123.99(19) 2_756 . ?
O11 Tb1 O12 56.20(19) . . ?
O51 Tb1 O12 71.47(19) 2_756 . ?
O51 Tb1 O12 106.87(19) . . ?
O31 Tb1 O12 65.8(2) . . ?
O31 Tb1 O12 115.8(2) 2_756 . ?
O11 Tb1 O12 56.20(19) 2_756 2_756 ?
O11 Tb1 O12 123.99(19) . 2_756 ?
O51 Tb1 O12 106.87(19) 2_756 2_756 ?
O51 Tb1 O12 71.47(19) . 2_756 ?
O31 Tb1 O12 115.8(2) . 2_756 ?
O31 Tb1 O12 65.8(2) 2_756 2_756 ?
O12 Tb1 O12 177.2(2) . 2_756 ?
O11 Tb1 Ni1 38.40(15) 2_756 2_756 ?
O11 Tb1 Ni1 141.63(15) . 2_756 ?
O51 Tb1 Ni1 37.86(15) 2_756 2_756 ?
O51 Tb1 Ni1 141.86(15) . 2_756 ?
O31 Tb1 Ni1 38.17(15) . 2_756 ?
O31 Tb1 Ni1 142.08(15) 2_756 2_756 ?
O12 Tb1 Ni1 85.69(13) . 2_756 ?
O12 Tb1 Ni1 94.30(13) 2_756 2_756 ?
O11 Tb1 Ni1 141.63(15) 2_756 . ?
O11 Tb1 Ni1 38.40(15) . . ?
O51 Tb1 Ni1 141.86(15) 2_756 . ?
O51 Tb1 Ni1 37.86(15) . . ?
O31 Tb1 Ni1 142.08(15) . . ?
O31 Tb1 Ni1 38.16(15) 2_756 . ?
O12 Tb1 Ni1 94.30(13) . . ?
O12 Tb1 Ni1 85.69(13) 2_756 . ?
Ni1 Tb1 Ni1 179.69(5) 2_756 . ?
C16 O11 Ni1 129.2(6) . . ?
C16 O11 Tb1 129.9(6) . . ?
Ni1 O11 Tb1 95.9(2) . . ?
C15 O12 C24 117.2(7) . . ?
C15 O12 Tb1 112.9(5) . . ?
C24 O12 Tb1 129.9(5) . . ?
C36 O31 Ni1 129.3(6) . 2_756 ?
C36 O31 Tb1 131.1(6) . . ?
Ni1 O31 Tb1 95.7(2) 2_756 . ?
C35 O32 C44 117.3(8) . . ?
C56 O51 Ni1 128.4(6) . . ?
C56 O51 Tb1 130.9(6) . . ?
Ni1 O51 Tb1 96.1(2) . . ?
C55 O52 C64 117.3(7) . . ?
C17 N11 C18 114.8(8) . . ?
C17 N11 Ni1 123.5(7) . . ?
C18 N11 Ni1 120.9(6) . . ?
C37 N31 C38 113.7(8) . . ?
C37 N31 Cl1 67.2(7) . . ?
C38 N31 Cl1 131.4(7) . . ?
C37 N31 Ni1 122.3(7) . 2_756 ?
C38 N31 Ni1 122.9(6) . 2_756 ?
Cl1 N31 Ni1 82.9(4) . 2_756 ?
C57 N51 C58 115.6(8) . . ?
C57 N51 Ni1 122.6(6) . . ?
C58 N51 Ni1 121.0(6) . . ?
C16 C11 C12 118.7(9) . . ?
C16 C11 C17 124.0(9) . . ?
C12 C11 C17 116.7(9) . . ?
C13 C12 C11 120.6(10) . . ?
C13 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
C12 C13 C14 121.0(9) . . ?
C12 C13 H13A 119.5 . . ?
C14 C13 H13A 119.5 . . ?
C15 C14 C13 119.5(9) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
O12 C15 C14 126.7(9) . . ?
O12 C15 C16 112.3(8) . . ?
C14 C15 C16 121.0(9) . . ?
O11 C16 C15 117.4(8) . . ?
O11 C16 C11 123.5(8) . . ?
C15 C16 C11 119.1(8) . . ?
N11 C17 C11 128.0(9) . . ?
N11 C17 H17A 116.0 . . ?
C11 C17 H17A 116.0 . . ?
C19 C18 C23 120.0(10) . . ?
C19 C18 N11 122.3(10) . . ?
C23 C18 N11 117.7(10) . . ?
C18 C19 C20 120.8(12) . . ?
C18 C19 H19A 119.6 . . ?
C20 C19 H19A 119.6 . . ?
C21 C20 C19 119.6(13) . . ?
C21 C20 H20A 120.2 . . ?
C19 C20 H20A 120.2 . . ?
C20 C21 C22 120.2(11) . . ?
C20 C21 H21A 119.9 . . ?
C22 C21 H21A 119.9 . . ?
C23 C22 C21 120.3(12) . . ?
C23 C22 H22A 119.9 . . ?
C21 C22 H22A 119.9 . . ?
C22 C23 C18 119.1(12) . . ?
C22 C23 H23A 120.4 . . ?
C18 C23 H23A 120.4 . . ?
O12 C24 H24A 109.5 . . ?
O12 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O12 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C36 C31 C32 117.9(9) . . ?
C36 C31 C37 124.4(9) . . ?
C32 C31 C37 117.5(9) . . ?
C36 C31 Cl1 80.0(7) . . ?
C32 C31 Cl1 139.4(9) . . ?
C37 C31 Cl1 54.6(6) . . ?
C33 C32 C31 121.8(10) . . ?
C33 C32 H32A 119.1 . . ?
C31 C32 H32A 119.1 . . ?
C32 C33 C34 119.9(10) . . ?
C32 C33 H33A 120.0 . . ?
C34 C33 H33A 120.0 . . ?
C35 C34 C33 119.2(10) . . ?
C35 C34 H34A 120.4 . . ?
C33 C34 H34A 120.4 . . ?
C34 C35 O32 125.6(9) . . ?
C34 C35 C36 122.0(9) . . ?
O32 C35 C36 112.3(8) . . ?
O31 C36 C31 123.5(9) . . ?
O31 C36 C35 117.8(8) . . ?
C31 C36 C35 118.7(9) . . ?
O31 C36 Cl1 73.3(6) . . ?
C31 C36 Cl1 61.2(6) . . ?
C35 C36 Cl1 144.9(8) . . ?
N31 C37 C31 129.0(10) . . ?
N31 C37 Cl1 65.6(7) . . ?
C31 C37 Cl1 79.5(7) . . ?
N31 C37 H37A 113.9 . . ?
C31 C37 H37A 113.9 . . ?
Cl1 C37 H37A 113.9 . . ?
C39 C38 C43 120.0 . . ?
C39 C38 N31 118.2(5) . . ?
C43 C38 N31 121.8(5) . . ?
C40 C39 C38 120.0 . . ?
C40 C39 H39A 120.0 . . ?
C38 C39 H39A 120.0 . . ?
C41 C40 C39 120.0 . . ?
C41 C40 H40A 120.0 . . ?
C39 C40 H40A 120.0 . . ?
C40 C41 C42 120.0 . . ?
C40 C41 H41A 120.0 . . ?
C42 C41 H41A 120.0 . . ?
C43 C42 C41 120.0 . . ?
C43 C42 H42A 120.0 . . ?
C41 C42 H42A 120.0 . . ?
C42 C43 C38 120.0 . . ?
C42 C43 H43A 120.0 . . ?
C38 C43 H43A 120.0 . . ?
O32 C44 H44A 109.5 . . ?
O32 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O32 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C56 C51 C52 119.6(9) . . ?
C56 C51 C57 122.6(9) . . ?
C52 C51 C57 117.7(9) . . ?
C53 C52 C51 121.6(9) . . ?
C53 C52 H52A 119.2 . . ?
C51 C52 H52A 119.2 . . ?
C52 C53 C54 120.1(9) . . ?
C52 C53 H53A 119.9 . . ?
C54 C53 H53A 119.9 . . ?
C55 C54 C53 119.4(9) . . ?
C55 C54 H54A 120.3 . . ?
C53 C54 H54A 120.3 . . ?
O52 C55 C54 125.7(9) . . ?
O52 C55 C56 112.5(8) . . ?
C54 C55 C56 121.8(9) . . ?
O51 C56 C51 125.3(9) . . ?
O51 C56 C55 117.2(8) . . ?
C51 C56 C55 117.5(9) . . ?
N51 C57 C51 129.6(9) . . ?
N51 C57 H57A 115.2 . . ?
C51 C57 H57A 115.2 . . ?
C63 C58 C59 120.6(9) . . ?
C63 C58 N51 119.7(9) . . ?
C59 C58 N51 119.6(9) . . ?
C60 C59 C58 118.5(10) . . ?
C60 C59 H59A 120.8 . . ?
C58 C59 H59A 120.8 . . ?
C61 C60 C59 120.6(11) . . ?
C61 C60 H60A 119.7 . . ?
C59 C60 H60A 119.7 . . ?
C62 C61 C60 119.6(11) . . ?
C62 C61 H61A 120.2 . . ?
C60 C61 H61A 120.2 . . ?
C63 C62 C61 120.0(10) . . ?
C63 C62 H62A 120.0 . . ?
C61 C62 H62A 120.0 . . ?
C58 C63 C62 120.6(10) . . ?
C58 C63 H63A 119.7 . . ?
C62 C63 H63A 119.7 . . ?
O52 C64 H64A 109.5 . . ?
O52 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
O52 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N31 Cl1 C37 47.1(5) . . ?
N31 Cl1 C31 86.6(6) . . ?
C37 Cl1 C31 45.9(5) . . ?
N31 Cl1 C36 104.8(6) . . ?
C37 Cl1 C36 80.2(6) . . ?
C31 Cl1 C36 38.7(4) . . ?
N31 Cl1 Ni1 57.7(4) . 2_756 ?
C37 Cl1 Ni1 91.7(5) . 2_756 ?
C31 Cl1 Ni1 99.2(4) . 2_756 ?
C36 Cl1 Ni1 80.8(4) . 2_756 ?
O72 N71 O72 133(2) 2_656 . ?
O72 N71 O71 113.5(10) 2_656 . ?
O72 N71 O71 113.5(10) . . ?
O1S C1S O1S 134(4) 2_656 . ?

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
C16 C11 C12 C13 0.6(16) . . . . ?
C17 C11 C12 C13 -171.0(10) . . . . ?
C11 C12 C13 C14 0.1(17) . . . . ?
C12 C13 C14 C15 0.8(16) . . . . ?
C24 O12 C15 C14 18.2(14) . . . . ?
Tb1 O12 C15 C14 -159.9(8) . . . . ?
C24 O12 C15 C16 -163.8(8) . . . . ?
Tb1 O12 C15 C16 18.1(9) . . . . ?
C13 C14 C15 O12 175.4(9) . . . . ?
C13 C14 C15 C16 -2.5(15) . . . . ?
Ni1 O11 C16 C15 174.8(6) . . . . ?
Tb1 O11 C16 C15 -36.5(11) . . . . ?
Ni1 O11 C16 C11 -5.7(13) . . . . ?
Tb1 O11 C16 C11 142.9(8) . . . . ?
O12 C15 C16 O11 4.4(12) . . . . ?
C14 C15 C16 O11 -177.4(8) . . . . ?
O12 C15 C16 C11 -175.0(8) . . . . ?
C14 C15 C16 C11 3.2(14) . . . . ?
C12 C11 C16 O11 178.4(9) . . . . ?
C17 C11 C16 O11 -10.7(15) . . . . ?
C12 C11 C16 C15 -2.2(14) . . . . ?
C17 C11 C16 C15 168.7(9) . . . . ?
C18 N11 C17 C11 -174.9(10) . . . . ?
Ni1 N11 C17 C11 15.1(16) . . . . ?
C16 C11 C17 N11 5.1(18) . . . . ?
C12 C11 C17 N11 176.2(11) . . . . ?
C17 N11 C18 C19 -64.6(13) . . . . ?
Ni1 N11 C18 C19 105.6(10) . . . . ?
C17 N11 C18 C23 116.3(11) . . . . ?
Ni1 N11 C18 C23 -73.4(11) . . . . ?
C23 C18 C19 C20 1.2(16) . . . . ?
N11 C18 C19 C20 -177.8(10) . . . . ?
C18 C19 C20 C21 0.8(18) . . . . ?
C19 C20 C21 C22 -2.0(19) . . . . ?
C20 C21 C22 C23 1.2(19) . . . . ?
C21 C22 C23 C18 0.8(17) . . . . ?
C19 C18 C23 C22 -2.0(16) . . . . ?
N11 C18 C23 C22 177.1(10) . . . . ?
C36 C31 C32 C33 -4.1(17) . . . . ?
C37 C31 C32 C33 -179.2(11) . . . . ?
Cl1 C31 C32 C33 -112.6(14) . . . . ?
C31 C32 C33 C34 6.3(19) . . . . ?
C32 C33 C34 C35 -2.8(18) . . . . ?
C33 C34 C35 O32 174.4(10) . . . . ?
C33 C34 C35 C36 -2.8(17) . . . . ?
C44 O32 C35 C34 14.3(14) . . . . ?
C44 O32 C35 C36 -168.3(8) . . . . ?
Ni1 O31 C36 C31 -9.7(14) 2_756 . . . ?
Tb1 O31 C36 C31 142.5(8) . . . . ?
Ni1 O31 C36 C35 169.7(6) 2_756 . . . ?
Tb1 O31 C36 C35 -38.1(12) . . . . ?
Ni1 O31 C36 Cl1 -46.5(6) 2_756 . . . ?
Tb1 O31 C36 Cl1 105.7(6) . . . . ?
C32 C31 C36 O31 178.0(9) . . . . ?
C37 C31 C36 O31 -7.3(17) . . . . ?
Cl1 C31 C36 O31 -40.8(10) . . . . ?
C32 C31 C36 C35 -1.4(15) . . . . ?
C37 C31 C36 C35 173.3(10) . . . . ?
Cl1 C31 C36 C35 139.8(9) . . . . ?
C32 C31 C36 Cl1 -141.2(11) . . . . ?
C37 C31 C36 Cl1 33.5(9) . . . . ?
C34 C35 C36 O31 -174.6(9) . . . . ?
O32 C35 C36 O31 7.9(12) . . . . ?
C34 C35 C36 C31 4.8(15) . . . . ?
O32 C35 C36 C31 -172.7(9) . . . . ?
C34 C35 C36 Cl1 84.8(16) . . . . ?
O32 C35 C36 Cl1 -92.7(13) . . . . ?
C38 N31 C37 C31 -178.2(10) . . . . ?
Cl1 N31 C37 C31 -51.4(12) . . . . ?
Ni1 N31 C37 C31 13.4(16) 2_756 . . . ?
C38 N31 C37 Cl1 -126.8(8) . . . . ?
Ni1 N31 C37 Cl1 64.8(7) 2_756 . . . ?
C36 C31 C37 N31 4.5(19) . . . . ?
C32 C31 C37 N31 179.3(11) . . . . ?
Cl1 C31 C37 N31 46.4(11) . . . . ?
C36 C31 C37 Cl1 -41.9(11) . . . . ?
C32 C31 C37 Cl1 132.8(10) . . . . ?
C37 N31 C38 C39 -60.5(10) . . . . ?
Cl1 N31 C38 C39 -140.3(7) . . . . ?
Ni1 N31 C38 C39 107.8(6) 2_756 . . . ?
C37 N31 C38 C43 120.8(8) . . . . ?
Cl1 N31 C38 C43 41.1(11) . . . . ?
Ni1 N31 C38 C43 -70.9(8) 2_756 . . . ?
C43 C38 C39 C40 0.0 . . . . ?
N31 C38 C39 C40 -178.7(7) . . . . ?
C38 C39 C40 C41 0.0 . . . . ?
C39 C40 C41 C42 0.0 . . . . ?
C40 C41 C42 C43 0.0 . . . . ?
C41 C42 C43 C38 0.0 . . . . ?
C39 C38 C43 C42 0.0 . . . . ?
N31 C38 C43 C42 178.6(7) . . . . ?
C56 C51 C52 C53 1.5(14) . . . . ?
C57 C51 C52 C53 -174.5(9) . . . . ?
C51 C52 C53 C54 -0.5(15) . . . . ?
C52 C53 C54 C55 1.3(14) . . . . ?
C64 O52 C55 C54 16.6(13) . . . . ?
C64 O52 C55 C56 -164.5(8) . . . . ?
C53 C54 C55 O52 175.7(8) . . . . ?
C53 C54 C55 C56 -3.1(14) . . . . ?
Ni1 O51 C56 C51 -9.5(13) . . . . ?
Tb1 O51 C56 C51 140.4(8) . . . . ?
Ni1 O51 C56 C55 172.2(6) . . . . ?
Tb1 O51 C56 C55 -37.9(11) . . . . ?
C52 C51 C56 O51 178.6(8) . . . . ?
C57 C51 C56 O51 -5.6(15) . . . . ?
C52 C51 C56 C55 -3.1(13) . . . . ?
C57 C51 C56 C55 172.7(8) . . . . ?
O52 C55 C56 O51 3.4(11) . . . . ?
C54 C55 C56 O51 -177.6(8) . . . . ?
O52 C55 C56 C51 -175.0(8) . . . . ?
C54 C55 C56 C51 4.0(13) . . . . ?
C58 N51 C57 C51 -177.0(9) . . . . ?
Ni1 N51 C57 C51 13.2(14) . . . . ?
C56 C51 C57 N51 2.9(16) . . . . ?
C52 C51 C57 N51 178.8(9) . . . . ?
C57 N51 C58 C63 113.4(10) . . . . ?
Ni1 N51 C58 C63 -76.6(10) . . . . ?
C57 N51 C58 C59 -64.1(12) . . . . ?
Ni1 N51 C58 C59 106.0(9) . . . . ?
C63 C58 C59 C60 4.2(16) . . . . ?
N51 C58 C59 C60 -178.3(10) . . . . ?
C58 C59 C60 C61 -3.8(18) . . . . ?
C59 C60 C61 C62 2.0(19) . . . . ?
C60 C61 C62 C63 -0.5(19) . . . . ?
C59 C58 C63 C62 -2.9(16) . . . . ?
N51 C58 C63 C62 179.7(9) . . . . ?
C61 C62 C63 C58 1.0(17) . . . . ?
C38 N31 Cl1 C37 102.2(10) . . . . ?
Ni1 N31 Cl1 C37 -129.5(7) 2_756 . . . ?
C37 N31 Cl1 C31 26.4(7) . . . . ?
C38 N31 Cl1 C31 128.5(9) . . . . ?
Ni1 N31 Cl1 C31 -103.1(4) 2_756 . . . ?
C37 N31 Cl1 C36 60.9(7) . . . . ?
C38 N31 Cl1 C36 163.0(7) . . . . ?
Ni1 N31 Cl1 C36 -68.7(4) 2_756 . . . ?
C37 N31 Cl1 Ni1 129.5(7) . . . 2_756 ?
C38 N31 Cl1 Ni1 -128.3(9) . . . 2_756 ?
C31 C37 Cl1 N31 141.8(9) . . . . ?
N31 C37 Cl1 C31 -141.8(9) . . . . ?
N31 C37 Cl1 C36 -121.0(7) . . . . ?
C31 C37 Cl1 C36 20.8(6) . . . . ?
N31 C37 Cl1 Ni1 -40.7(5) . . . 2_756 ?
C31 C37 Cl1 Ni1 101.2(6) . . . 2_756 ?

_refine_diff_density_max         4.498
_refine_diff_density_min         -3.607
_refine_diff_density_rms         0.312

####################################################################### 
# 
# 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_Ni2Prl_SQ
_database_code_depnum_ccdc_archive 'CCDC 1054074'
_audit_update_record             
;
2016-01-02 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H72 N6.48 Ni2 O13.95 Pr'
_chemical_formula_weight         1653.73

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   22.935(5)
_cell_length_b                   23.393(5)
_cell_length_c                   18.574(4)
_cell_angle_alpha                90
_cell_angle_beta                 120.310(4)
_cell_angle_gamma                90
_cell_volume                     8603(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9973
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      27.28

_exptl_crystal_description       Needle
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_F_000             3392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.052
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8751
_exptl_absorpt_correction_T_max  0.9204
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            66136
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.741
_diffrn_reflns_theta_max         28.342
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             10632
_reflns_number_gt                7438
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
All non-hydrogen atoms were refined anisotropically except disorded nitrate anion ligands and free hydroxo which are refined iostropically.
Several constrains/restrains were used like DFIX, DANG, SIMU etc. Hydrogen atoms are
added in its calculated geometric position which are refined as riding model. 

Due to the diffused electron density, the solvent molecules could not be
modelled, hence SQUZZEE routine was employed.

Nitrate was found with 48% occupency. Rest of which occupied by hydroxo(51%). 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1103P)²+71.2293P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10632
_refine_ls_number_parameters     475
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.2039
_refine_ls_wR_factor_gt          0.1690
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.5000 0.09508(2) 0.2500 0.01440(12) Uani 1 2 d S T P . .
Ni1 Ni 0.34563(3) 0.09492(2) 0.23397(3) 0.01358(15) Uani 1 1 d . . . . .
C11 C 0.4155(3) 0.1826(2) 0.4055(3) 0.0257(11) Uani 1 1 d . . . . .
N11 N 0.3354(2) 0.10284(18) 0.3405(3) 0.0207(9) Uani 1 1 d . . . . .
O11 O 0.42854(18) 0.14658(13) 0.2935(2) 0.0169(7) Uani 1 1 d . . . . .
C12 C 0.4378(3) 0.2236(3) 0.4710(4) 0.0359(14) Uani 1 1 d . . . . .
H12A H 0.4167 0.2251 0.5038 0.043 Uiso 1 1 calc R U . . .
O12 O 0.53511(19) 0.20596(14) 0.3362(2) 0.0211(7) Uani 1 1 d . . . . .
C13 C 0.4888(4) 0.2606(3) 0.4874(4) 0.0421(17) Uani 1 1 d . . . . .
H13A H 0.5008 0.2894 0.5286 0.051 Uiso 1 1 calc R U . . .
C14 C 0.5236(3) 0.2565(2) 0.4439(4) 0.0333(13) Uani 1 1 d . . . . .
H14A H 0.5609 0.2809 0.4576 0.040 Uiso 1 1 calc R U . . .
C15 C 0.5034(3) 0.2167(2) 0.3809(3) 0.0229(11) Uani 1 1 d . . . . .
C16 C 0.4470(3) 0.18072(19) 0.3577(3) 0.0182(10) Uani 1 1 d . . . . .
C17 C 0.3637(3) 0.1432(2) 0.3953(3) 0.0259(11) Uani 1 1 d . . . . .
H17A H 0.3483 0.1472 0.4338 0.031 Uiso 1 1 calc R U . . .
C18 C 0.2863(3) 0.0711(2) 0.3512(3) 0.0244(11) Uani 1 1 d . . . . .
C19 C 0.2943(3) 0.0129(2) 0.3670(3) 0.0258(11) Uani 1 1 d . . . . .
H19A H 0.3326 -0.0064 0.3720 0.031 Uiso 1 1 calc R U . . .
C20 C 0.2456(3) -0.0169(3) 0.3755(4) 0.0324(13) Uani 1 1 d . . . . .
H20A H 0.2511 -0.0568 0.3868 0.039 Uiso 1 1 calc R U . . .
C21 C 0.1887(3) 0.0112(3) 0.3675(4) 0.0362(14) Uani 1 1 d . . . . .
H21A H 0.1556 -0.0097 0.3730 0.043 Uiso 1 1 calc R U . . .
C22 C 0.1808(3) 0.0690(3) 0.3517(4) 0.0369(14) Uani 1 1 d . . . . .
H22A H 0.1421 0.0884 0.3455 0.044 Uiso 1 1 calc R U . . .
C23 C 0.2315(4) 0.0991(3) 0.3448(4) 0.0338(14) Uani 1 1 d . . . . .
H23A H 0.2274 0.1392 0.3357 0.041 Uiso 1 1 calc R U . . .
C24 C 0.5839(3) 0.2471(2) 0.3422(4) 0.0300(12) Uani 1 1 d . . . . .
H24A H 0.6028 0.2347 0.3078 0.045 Uiso 1 1 calc R U . . .
H24B H 0.5619 0.2844 0.3224 0.045 Uiso 1 1 calc R U . . .
H24C H 0.6202 0.2504 0.4004 0.045 Uiso 1 1 calc R U . . .
C31 C 0.3625(3) -0.0506(2) 0.2563(3) 0.0190(10) Uani 1 1 d . . . . .
O31 O 0.42349(18) 0.03762(13) 0.2798(2) 0.0161(7) Uani 1 1 d . . . . .
N31 N 0.2789(2) 0.02512(17) 0.1814(3) 0.0189(8) Uani 1 1 d . . . . .
C32 C 0.3682(3) -0.1106(2) 0.2703(3) 0.0244(11) Uani 1 1 d . . . . .
H32A H 0.3283 -0.1328 0.2504 0.029 Uiso 1 1 calc R U . . .
O32 O 0.53872(18) -0.01142(14) 0.3457(2) 0.0179(7) Uani 1 1 d . . . . .
C33 C 0.4294(3) -0.1372(2) 0.3115(3) 0.0267(12) Uani 1 1 d . . . . .
H33A H 0.4316 -0.1772 0.3210 0.032 Uiso 1 1 calc R U . . .
C34 C 0.4900(3) -0.1053(2) 0.3402(3) 0.0220(10) Uani 1 1 d . . . . .
H34A H 0.5328 -0.1236 0.3683 0.026 Uiso 1 1 calc R U . . .
C35 C 0.4851(3) -0.04714(19) 0.3262(3) 0.0168(9) Uani 1 1 d . . . . .
C36 C 0.4224(3) -0.01808(19) 0.2870(3) 0.0159(9) Uani 1 1 d . . . . .
C37 C 0.2960(3) -0.0271(2) 0.2046(3) 0.0208(10) Uani 1 1 d . . . . .
H37A H 0.2598 -0.0537 0.1849 0.025 Uiso 1 1 calc R U . . .
C38 C 0.2074(3) 0.0342(2) 0.1257(3) 0.0237(11) Uani 1 1 d . . . . .
C39 C 0.1851(3) 0.0515(2) 0.0440(3) 0.0278(12) Uani 1 1 d . . . . .
H39A H 0.2165 0.0564 0.0254 0.033 Uiso 1 1 calc R U . . .
C40 C 0.1170(3) 0.0616(3) -0.0101(4) 0.0330(13) Uani 1 1 d . . . . .
H40A H 0.1020 0.0742 -0.0654 0.040 Uiso 1 1 calc R U . . .
C41 C 0.0705(3) 0.0535(3) 0.0159(4) 0.0401(15) Uani 1 1 d . . . . .
H41A H 0.0238 0.0600 -0.0215 0.048 Uiso 1 1 calc R U . . .
C42 C 0.0929(3) 0.0356(3) 0.0973(4) 0.0405(15) Uani 1 1 d . . . . .
H42A H 0.0614 0.0305 0.1157 0.049 Uiso 1 1 calc R U . . .
C43 C 0.1612(3) 0.0251(3) 0.1516(4) 0.0297(12) Uani 1 1 d . . . . .
H43A H 0.1761 0.0117 0.2065 0.036 Uiso 1 1 calc R U . . .
C44 C 0.6050(3) -0.0326(2) 0.4032(3) 0.0247(11) Uani 1 1 d . . . . .
H44A H 0.6386 -0.0034 0.4120 0.037 Uiso 1 1 calc R U . . .
H44B H 0.6079 -0.0415 0.4565 0.037 Uiso 1 1 calc R U . . .
H44C H 0.6137 -0.0672 0.3805 0.037 Uiso 1 1 calc R U . . .
C51 C 0.2864(3) 0.1542(2) 0.0391(3) 0.0206(10) Uani 1 1 d . . . . .
N51 N 0.2738(2) 0.15843(17) 0.1630(3) 0.0194(8) Uani 1 1 d . . . . .
O51 O 0.37667(17) 0.10002(13) 0.1484(2) 0.0150(6) Uani 1 1 d . . . . .
C52 C 0.2581(3) 0.1766(2) -0.0425(3) 0.0287(12) Uani 1 1 d . . . . .
H52A H 0.2160 0.1961 -0.0670 0.034 Uiso 1 1 calc R U . . .
O52 O 0.44305(19) 0.09379(14) 0.0712(2) 0.0194(7) Uani 1 1 d . . . . .
C53 C 0.2912(3) 0.1705(2) -0.0870(3) 0.0283(12) Uani 1 1 d . . . . .
H53A H 0.2715 0.1853 -0.1420 0.034 Uiso 1 1 calc R U . . .
C54 C 0.3535(3) 0.1427(2) -0.0513(3) 0.0234(11) Uani 1 1 d . . . . .
H54A H 0.3768 0.1396 -0.0814 0.028 Uiso 1 1 calc R U . . .
C55 C 0.3812(3) 0.1198(2) 0.0276(3) 0.0180(9) Uani 1 1 d . . . . .
C56 C 0.3475(3) 0.12356(19) 0.0737(3) 0.0173(9) Uani 1 1 d . . . . .
C57 C 0.2547(3) 0.1705(2) 0.0866(3) 0.0238(11) Uani 1 1 d . . . . .
H57A H 0.2148 0.1929 0.0578 0.029 Uiso 1 1 calc R U . . .
C58 C 0.2354(2) 0.18717(16) 0.1937(2) 0.0296(12) Uani 1 1 d G . . . .
C59 C 0.1676(2) 0.17483(17) 0.1633(2) 0.0386(15) Uani 1 1 d G . . . .
H59A H 0.1449 0.1483 0.1190 0.046 Uiso 1 1 calc R U . . .
C60 C 0.13310(17) 0.2013(2) 0.1978(3) 0.0498(19) Uani 1 1 d G . . . .
H60A H 0.0868 0.1929 0.1770 0.060 Uiso 1 1 calc R U . . .
C61 C 0.1664(2) 0.2402(2) 0.2626(3) 0.049(2) Uani 1 1 d G . . . .
H61A H 0.1428 0.2583 0.2862 0.059 Uiso 1 1 calc R U . . .
C62 C 0.2341(2) 0.25253(16) 0.2931(2) 0.050(2) Uani 1 1 d G . . . .
H62A H 0.2569 0.2791 0.3374 0.060 Uiso 1 1 calc R U . . .
C63 C 0.26865(17) 0.22602(16) 0.2586(2) 0.0356(14) Uani 1 1 d G . . . .
H63A H 0.3150 0.2345 0.2794 0.043 Uiso 1 1 calc R U . . .
C64 C 0.4729(3) 0.0738(2) 0.0244(3) 0.0257(11) Uani 1 1 d . . . . .
H64A H 0.5167 0.0561 0.0622 0.039 Uiso 1 1 calc R U . . .
H64B H 0.4431 0.0454 -0.0166 0.039 Uiso 1 1 calc R U . . .
H64C H 0.4794 0.1060 -0.0046 0.039 Uiso 1 1 calc R U . . .
N71 N 0.0000 0.0287(4) 0.2500 0.052(4) Uiso 0.4822 2 d DS U P A 1
O71 O 0.0000 0.0864(4) 0.2500 0.067(5) Uiso 0.4822 2 d DS U P A 1
O72 O -0.0198(8) 0.0140(4) 0.1707(2) 0.077(4) Uiso 0.4822 1 d D U P A 1
O1 O 0.4538(7) 0.2529(6) 0.6658(8) 0.022(3) Uiso 0.2589 1 d . . P B 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
Pr1 O11 2.475(3) 2_655 ?
Pr1 O11 2.475(3) . ?
Pr1 O31 2.485(3) . ?
Pr1 O31 2.485(3) 2_655 ?
Pr1 O51 2.487(3) . ?
Pr1 O51 2.487(3) 2_655 ?
Pr1 O52 2.891(3) 2_655 ?
Pr1 O52 2.891(3) . ?
Pr1 O32 2.926(3) 2_655 ?
Pr1 O32 2.926(3) . ?
Pr1 O12 2.940(3) 2_655 ?
Pr1 O12 2.940(3) . ?
Ni1 O31 2.043(3) . ?
Ni1 O11 2.044(3) . ?
Ni1 O51 2.046(3) . ?
Ni1 N31 2.110(4) . ?
Ni1 N51 2.114(4) . ?
Ni1 N11 2.115(4) . ?
C11 C16 1.398(8) . ?
C11 C12 1.426(7) . ?
C11 C17 1.439(8) . ?
N11 C17 1.297(7) . ?
N11 C18 1.443(7) . ?
O11 C16 1.316(5) . ?
C12 C13 1.360(10) . ?
C12 H12A 0.9500 . ?
O12 C15 1.373(7) . ?
O12 C24 1.438(6) . ?
C13 C14 1.396(9) . ?
C13 H13A 0.9500 . ?
C14 C15 1.379(7) . ?
C14 H14A 0.9500 . ?
C15 C16 1.418(7) . ?
C17 H17A 0.9500 . ?
C18 C23 1.369(9) . ?
C18 C19 1.384(8) . ?
C19 C20 1.391(8) . ?
C19 H19A 0.9500 . ?
C20 C21 1.402(9) . ?
C20 H20A 0.9500 . ?
C21 C22 1.378(9) . ?
C21 H21A 0.9500 . ?
C22 C23 1.419(9) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C36 1.414(7) . ?
C31 C32 1.422(7) . ?
C31 C37 1.439(7) . ?
O31 C36 1.311(5) . ?
N31 C37 1.288(6) . ?
N31 C38 1.447(7) . ?
C32 C33 1.363(8) . ?
C32 H32A 0.9500 . ?
O32 C35 1.376(6) . ?
O32 C44 1.434(6) . ?
C33 C34 1.422(8) . ?
C33 H33A 0.9500 . ?
C34 C35 1.379(6) . ?
C34 H34A 0.9500 . ?
C35 C36 1.415(7) . ?
C37 H37A 0.9500 . ?
C38 C43 1.384(8) . ?
C38 C39 1.395(8) . ?
C39 C40 1.386(8) . ?
C39 H39A 0.9500 . ?
C40 C41 1.387(10) . ?
C40 H40A 0.9500 . ?
C41 C42 1.393(9) . ?
C41 H41A 0.9500 . ?
C42 C43 1.392(9) . ?
C42 H42A 0.9500 . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C51 C56 1.407(7) . ?
C51 C52 1.414(7) . ?
C51 C57 1.451(8) . ?
N51 C57 1.288(7) . ?
N51 C58 1.435(5) . ?
O51 C56 1.319(6) . ?
C52 C53 1.382(9) . ?
C52 H52A 0.9500 . ?
O52 C55 1.371(6) . ?
O52 C64 1.430(6) . ?
C53 C54 1.395(8) . ?
C53 H53A 0.9500 . ?
C54 C55 1.378(7) . ?
C54 H54A 0.9500 . ?
C55 C56 1.417(7) . ?
C57 H57A 0.9500 . ?
C58 C59 1.3900 . ?
C58 C63 1.3900 . ?
C59 C60 1.3900 . ?
C59 H59A 0.9500 . ?
C60 C61 1.3900 . ?
C60 H60A 0.9500 . ?
C61 C62 1.3900 . ?
C61 H61A 0.9500 . ?
C62 C63 1.3900 . ?
C62 H62A 0.9500 . ?
C63 H63A 0.9500 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
N71 O72 1.3478(11) . ?
N71 O72 1.3478(11) 2 ?
N71 O71 1.3490(11) . ?

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
O11 Pr1 O11 121.74(15) 2_655 . ?
O11 Pr1 O31 173.99(11) 2_655 . ?
O11 Pr1 O31 62.11(11) . . ?
O11 Pr1 O31 62.11(11) 2_655 2_655 ?
O11 Pr1 O31 173.99(11) . 2_655 ?
O31 Pr1 O31 114.50(15) . 2_655 ?
O11 Pr1 O51 114.63(11) 2_655 . ?
O11 Pr1 O51 62.48(11) . . ?
O31 Pr1 O51 62.19(11) . . ?
O31 Pr1 O51 121.12(11) 2_655 . ?
O11 Pr1 O51 62.48(11) 2_655 2_655 ?
O11 Pr1 O51 114.63(11) . 2_655 ?
O31 Pr1 O51 121.12(11) . 2_655 ?
O31 Pr1 O51 62.19(11) 2_655 2_655 ?
O51 Pr1 O51 174.67(14) . 2_655 ?
O11 Pr1 O52 112.97(11) 2_655 2_655 ?
O11 Pr1 O52 67.66(11) . 2_655 ?
O31 Pr1 O52 72.47(10) . 2_655 ?
O31 Pr1 O52 106.86(11) 2_655 2_655 ?
O51 Pr1 O52 123.58(11) . 2_655 ?
O51 Pr1 O52 56.48(11) 2_655 2_655 ?
O11 Pr1 O52 67.66(11) 2_655 . ?
O11 Pr1 O52 112.97(11) . . ?
O31 Pr1 O52 106.86(11) . . ?
O31 Pr1 O52 72.46(10) 2_655 . ?
O51 Pr1 O52 56.48(11) . . ?
O51 Pr1 O52 123.58(11) 2_655 . ?
O52 Pr1 O52 178.81(13) 2_655 . ?
O11 Pr1 O32 105.32(10) 2_655 2_655 ?
O11 Pr1 O32 124.38(10) . 2_655 ?
O31 Pr1 O32 69.07(10) . 2_655 ?
O31 Pr1 O32 55.66(10) 2_655 2_655 ?
O51 Pr1 O32 72.45(10) . 2_655 ?
O51 Pr1 O32 112.38(10) 2_655 2_655 ?
O52 Pr1 O32 120.78(9) 2_655 2_655 ?
O52 Pr1 O32 58.03(9) . 2_655 ?
O11 Pr1 O32 124.39(10) 2_655 . ?
O11 Pr1 O32 105.31(10) . . ?
O31 Pr1 O32 55.66(10) . . ?
O31 Pr1 O32 69.08(10) 2_655 . ?
O51 Pr1 O32 112.37(10) . . ?
O51 Pr1 O32 72.45(10) 2_655 . ?
O52 Pr1 O32 58.03(9) 2_655 . ?
O52 Pr1 O32 120.78(9) . . ?
O32 Pr1 O32 63.28(13) 2_655 . ?
O11 Pr1 O12 55.74(11) 2_655 2_655 ?
O11 Pr1 O12 72.77(11) . 2_655 ?
O31 Pr1 O12 124.67(11) . 2_655 ?
O31 Pr1 O12 112.71(10) 2_655 2_655 ?
O51 Pr1 O12 69.62(10) . 2_655 ?
O51 Pr1 O12 105.44(10) 2_655 2_655 ?
O52 Pr1 O12 118.42(10) 2_655 2_655 ?
O52 Pr1 O12 62.77(10) . 2_655 ?
O32 Pr1 O12 120.30(10) 2_655 2_655 ?
O32 Pr1 O12 176.42(9) . 2_655 ?
O11 Pr1 O12 72.77(11) 2_655 . ?
O11 Pr1 O12 55.74(11) . . ?
O31 Pr1 O12 112.70(10) . . ?
O31 Pr1 O12 124.67(11) 2_655 . ?
O51 Pr1 O12 105.44(10) . . ?
O51 Pr1 O12 69.62(10) 2_655 . ?
O52 Pr1 O12 62.77(10) 2_655 . ?
O52 Pr1 O12 118.42(10) . . ?
O32 Pr1 O12 176.43(9) 2_655 . ?
O32 Pr1 O12 120.30(10) . . ?
O12 Pr1 O12 56.13(14) 2_655 . ?
O31 Ni1 O11 77.51(14) . . ?
O31 Ni1 O51 77.79(13) . . ?
O11 Ni1 O51 78.00(13) . . ?
O31 Ni1 N31 87.83(15) . . ?
O11 Ni1 N31 165.31(15) . . ?
O51 Ni1 N31 98.11(15) . . ?
O31 Ni1 N51 164.43(16) . . ?
O11 Ni1 N51 98.13(15) . . ?
O51 Ni1 N51 86.69(15) . . ?
N31 Ni1 N51 95.76(17) . . ?
O31 Ni1 N11 98.87(15) . . ?
O11 Ni1 N11 87.41(16) . . ?
O51 Ni1 N11 165.41(16) . . ?
N31 Ni1 N11 95.93(17) . . ?
N51 Ni1 N11 95.83(17) . . ?
O31 Ni1 Pr1 46.52(10) . . ?
O11 Ni1 Pr1 46.25(10) . . ?
O51 Ni1 Pr1 46.60(9) . . ?
N31 Ni1 Pr1 121.42(12) . . ?
N51 Ni1 Pr1 120.24(13) . . ?
N11 Ni1 Pr1 121.37(13) . . ?
C16 C11 C12 119.0(5) . . ?
C16 C11 C17 123.4(5) . . ?
C12 C11 C17 117.4(5) . . ?
C17 N11 C18 112.6(5) . . ?
C17 N11 Ni1 123.3(4) . . ?
C18 N11 Ni1 123.1(3) . . ?
C16 O11 Ni1 129.4(3) . . ?
C16 O11 Pr1 129.0(3) . . ?
Ni1 O11 Pr1 97.14(12) . . ?
C13 C12 C11 121.1(6) . . ?
C13 C12 H12A 119.5 . . ?
C11 C12 H12A 119.5 . . ?
C15 O12 C24 117.3(4) . . ?
C15 O12 Pr1 114.1(3) . . ?
C24 O12 Pr1 128.4(3) . . ?
C12 C13 C14 120.3(5) . . ?
C12 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
C15 C14 C13 119.6(6) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
O12 C15 C14 125.7(5) . . ?
O12 C15 C16 112.9(4) . . ?
C14 C15 C16 121.4(5) . . ?
O11 C16 C11 124.2(5) . . ?
O11 C16 C15 117.5(5) . . ?
C11 C16 C15 118.3(4) . . ?
N11 C17 C11 128.6(5) . . ?
N11 C17 H17A 115.7 . . ?
C11 C17 H17A 115.7 . . ?
C23 C18 C19 120.4(5) . . ?
C23 C18 N11 119.2(5) . . ?
C19 C18 N11 120.4(5) . . ?
C18 C19 C20 119.4(6) . . ?
C18 C19 H19A 120.3 . . ?
C20 C19 H19A 120.3 . . ?
C19 C20 C21 120.7(6) . . ?
C19 C20 H20A 119.7 . . ?
C21 C20 H20A 119.7 . . ?
C22 C21 C20 119.9(6) . . ?
C22 C21 H21A 120.0 . . ?
C20 C21 H21A 120.0 . . ?
C21 C22 C23 118.7(6) . . ?
C21 C22 H22A 120.6 . . ?
C23 C22 H22A 120.6 . . ?
C18 C23 C22 120.9(6) . . ?
C18 C23 H23A 119.5 . . ?
C22 C23 H23A 119.5 . . ?
O12 C24 H24A 109.5 . . ?
O12 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O12 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C36 C31 C32 118.4(5) . . ?
C36 C31 C37 123.4(4) . . ?
C32 C31 C37 117.9(5) . . ?
C36 O31 Ni1 129.5(3) . . ?
C36 O31 Pr1 127.7(3) . . ?
Ni1 O31 Pr1 96.84(12) . . ?
C37 N31 C38 115.0(4) . . ?
C37 N31 Ni1 123.5(4) . . ?
C38 N31 Ni1 120.8(3) . . ?
C33 C32 C31 121.8(5) . . ?
C33 C32 H32A 119.1 . . ?
C31 C32 H32A 119.1 . . ?
C35 O32 C44 117.2(4) . . ?
C35 O32 Pr1 113.6(3) . . ?
C44 O32 Pr1 129.0(3) . . ?
C32 C33 C34 120.4(5) . . ?
C32 C33 H33A 119.8 . . ?
C34 C33 H33A 119.8 . . ?
C35 C34 C33 118.3(5) . . ?
C35 C34 H34A 120.8 . . ?
C33 C34 H34A 120.8 . . ?
O32 C35 C34 124.9(5) . . ?
O32 C35 C36 112.6(4) . . ?
C34 C35 C36 122.4(5) . . ?
O31 C36 C31 123.9(4) . . ?
O31 C36 C35 117.6(4) . . ?
C31 C36 C35 118.5(4) . . ?
N31 C37 C31 128.7(5) . . ?
N31 C37 H37A 115.6 . . ?
C31 C37 H37A 115.6 . . ?
C43 C38 C39 119.9(5) . . ?
C43 C38 N31 121.2(5) . . ?
C39 C38 N31 118.8(5) . . ?
C40 C39 C38 119.9(6) . . ?
C40 C39 H39A 120.1 . . ?
C38 C39 H39A 120.1 . . ?
C39 C40 C41 120.5(6) . . ?
C39 C40 H40A 119.8 . . ?
C41 C40 H40A 119.8 . . ?
C40 C41 C42 119.4(6) . . ?
C40 C41 H41A 120.3 . . ?
C42 C41 H41A 120.3 . . ?
C43 C42 C41 120.3(6) . . ?
C43 C42 H42A 119.9 . . ?
C41 C42 H42A 119.9 . . ?
C38 C43 C42 119.9(6) . . ?
C38 C43 H43A 120.0 . . ?
C42 C43 H43A 120.0 . . ?
O32 C44 H44A 109.5 . . ?
O32 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O32 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C56 C51 C52 119.4(5) . . ?
C56 C51 C57 123.0(5) . . ?
C52 C51 C57 117.1(5) . . ?
C57 N51 C58 113.6(4) . . ?
C57 N51 Ni1 124.4(4) . . ?
C58 N51 Ni1 121.6(3) . . ?
C56 O51 Ni1 130.6(3) . . ?
C56 O51 Pr1 126.6(3) . . ?
Ni1 O51 Pr1 96.69(12) . . ?
C53 C52 C51 120.6(5) . . ?
C53 C52 H52A 119.7 . . ?
C51 C52 H52A 119.7 . . ?
C55 O52 C64 117.2(4) . . ?
C55 O52 Pr1 114.0(3) . . ?
C64 O52 Pr1 128.7(3) . . ?
C52 C53 C54 120.3(5) . . ?
C52 C53 H53A 119.9 . . ?
C54 C53 H53A 119.9 . . ?
C55 C54 C53 119.8(5) . . ?
C55 C54 H54A 120.1 . . ?
C53 C54 H54A 120.1 . . ?
O52 C55 C54 125.8(5) . . ?
O52 C55 C56 112.8(4) . . ?
C54 C55 C56 121.4(5) . . ?
O51 C56 C51 123.6(5) . . ?
O51 C56 C55 118.0(4) . . ?
C51 C56 C55 118.4(4) . . ?
N51 C57 C51 128.1(5) . . ?
N51 C57 H57A 115.9 . . ?
C51 C57 H57A 115.9 . . ?
C59 C58 C63 120.0 . . ?
C59 C58 N51 121.7(3) . . ?
C63 C58 N51 118.2(3) . . ?
C60 C59 C58 120.0 . . ?
C60 C59 H59A 120.0 . . ?
C58 C59 H59A 120.0 . . ?
C59 C60 C61 120.0 . . ?
C59 C60 H60A 120.0 . . ?
C61 C60 H60A 120.0 . . ?
C62 C61 C60 120.0 . . ?
C62 C61 H61A 120.0 . . ?
C60 C61 H61A 120.0 . . ?
C61 C62 C63 120.0 . . ?
C61 C62 H62A 120.0 . . ?
C63 C62 H62A 120.0 . . ?
C62 C63 C58 120.0 . . ?
C62 C63 H63A 120.0 . . ?
C58 C63 H63A 120.0 . . ?
O52 C64 H64A 109.5 . . ?
O52 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
O52 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O72 N71 O72 150.5(2) . 2 ?
O72 N71 O71 104.76(11) . . ?
O72 N71 O71 104.76(11) 2 . ?

_refine_diff_density_max         5.919
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.180



####################################################################### 
# 
# 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_ni2lal_sq
_database_code_depnum_ccdc_archive 'CCDC 1054075'
_audit_update_record             
;
2016-01-02 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H72 La N6.45 Ni2 O13.90'
_chemical_formula_weight         1650.51

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'

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

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

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

_cell_length_a                   23.047(3)
_cell_length_b                   23.509(3)
_cell_length_c                   18.570(2)
_cell_angle_alpha                90
_cell_angle_beta                 120.378(3)
_cell_angle_gamma                90
_cell_volume                     8679.8(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4206
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      27.96

_exptl_crystal_description       Needle
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_F_000             3381
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.974
_shelx_estimated_absorpt_T_min   0.892
_shelx_estimated_absorpt_T_max   0.935
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8913
_exptl_absorpt_correction_T_max  0.9345
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40058
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.449
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9475
_reflns_number_gt                6416
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
All non-hydrogen atoms were refined anisotropically except disorded nitrate anion ligands and free hydroxo which are refined iostropically.
Several constrains/restrains were used like DFIX, DANG, SIMU etc. Hydrogen atoms are
added in its calculated geometric position which are refined as riding model. 

Due to the diffused electron density, the solvent molecules could not be
modelled, hence SQUZZEE routine was employed.

Nitrate was found with 45% occupency. Rest of which occupied by hydroxo(55%). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0851P)²+16.7923P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9475
_refine_ls_number_parameters     490
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1648
_refine_ls_wR_factor_gt          0.1435
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.65512(3) 0.09482(2) 0.26577(3) 0.01351(15) Uani 1 1 d . . . . .
La1 La 0.5000 0.09498(2) 0.2500 0.01265(11) Uani 1 2 d S T P . .
N11 N 0.66481(19) 0.10278(17) 0.1585(2) 0.0187(9) Uani 1 1 d . . . . .
O11 O 0.57297(15) 0.14698(13) 0.20670(18) 0.0154(7) Uani 1 1 d . . . . .
C11 C 0.5847(2) 0.1818(2) 0.0933(3) 0.0218(11) Uani 1 1 d . . . . .
O12 O 0.46579(16) 0.20502(13) 0.1632(2) 0.0201(7) Uani 1 1 d . . . . .
C12 C 0.5619(3) 0.2214(2) 0.0265(3) 0.0321(13) Uani 1 1 d . . . . .
H12A H 0.5830 0.2229 -0.0062 0.039 Uiso 1 1 calc R U . . .
C13 C 0.5096(3) 0.2575(3) 0.0093(4) 0.0392(15) Uani 1 1 d . . . . .
H13A H 0.4960 0.2850 -0.0338 0.047 Uiso 1 1 calc R U . . .
C14 C 0.4763(3) 0.2542(2) 0.0542(3) 0.0323(13) Uani 1 1 d . . . . .
H14A H 0.4395 0.2788 0.0411 0.039 Uiso 1 1 calc R U . . .
C24 C 0.4158(3) 0.2456(2) 0.1563(4) 0.0291(12) Uani 1 1 d . . . . .
H24A H 0.4360 0.2836 0.1714 0.044 Uiso 1 1 calc R U . . .
H24B H 0.3998 0.2345 0.1941 0.044 Uiso 1 1 calc R U . . .
H24C H 0.3780 0.2461 0.0988 0.044 Uiso 1 1 calc R U . . .
C15 C 0.4971(2) 0.2154(2) 0.1174(3) 0.0190(10) Uani 1 1 d . . . . .
C16 C 0.5533(2) 0.1805(2) 0.1414(3) 0.0187(10) Uani 1 1 d . . . . .
C17 C 0.6361(2) 0.1428(2) 0.1033(3) 0.0221(11) Uani 1 1 d . . . . .
H17A H 0.6512 0.1468 0.0645 0.026 Uiso 1 1 calc R U . . .
C18 C 0.7142(2) 0.0711(2) 0.1485(3) 0.0216(10) Uani 1 1 d . . . . .
C19 C 0.7701(3) 0.0988(2) 0.1550(3) 0.0281(12) Uani 1 1 d . . . . .
H19A H 0.7751 0.1387 0.1646 0.034 Uiso 1 1 calc R U . . .
C20 C 0.8180(3) 0.0688(3) 0.1476(4) 0.0347(13) Uani 1 1 d . . . . .
H20A H 0.8566 0.0877 0.1537 0.042 Uiso 1 1 calc R U . . .
C21 C 0.8102(3) 0.0112(3) 0.1313(4) 0.0348(14) Uani 1 1 d . . . . .
H21A H 0.8431 -0.0093 0.1255 0.042 Uiso 1 1 calc R U . . .
C22 C 0.7533(3) -0.0170(2) 0.1233(3) 0.0299(12) Uani 1 1 d . . . . .
H22A H 0.7474 -0.0566 0.1117 0.036 Uiso 1 1 calc R U . . .
C23 C 0.7060(2) 0.0134(2) 0.1325(3) 0.0232(11) Uani 1 1 d . . . . .
H23A H 0.6678 -0.0055 0.1279 0.028 Uiso 1 1 calc R U . . .
N31 N 0.72149(18) 0.02488(17) 0.3174(2) 0.0170(8) Uani 1 1 d . . . . .
O31 O 0.57788(14) 0.03765(13) 0.21969(19) 0.0148(7) Uani 1 1 d . . . . .
C31 C 0.6377(2) -0.0504(2) 0.2427(3) 0.0174(10) Uani 1 1 d . . . . .
O32 O 0.46276(14) -0.01110(13) 0.15529(19) 0.0163(7) Uani 1 1 d . . . . .
C32 C 0.6325(2) -0.1098(2) 0.2290(3) 0.0209(10) Uani 1 1 d . . . . .
H32A H 0.6723 -0.1318 0.2487 0.025 Uiso 1 1 calc R U . . .
C33 C 0.5704(3) -0.1363(2) 0.1874(3) 0.0230(11) Uani 1 1 d . . . . .
H33A H 0.5677 -0.1760 0.1769 0.028 Uiso 1 1 calc R U . . .
C34 C 0.5112(2) -0.1045(2) 0.1604(3) 0.0202(10) Uani 1 1 d . . . . .
H34A H 0.4685 -0.1227 0.1333 0.024 Uiso 1 1 calc R U . . .
C35 C 0.5160(2) -0.0464(2) 0.1739(3) 0.0158(9) Uani 1 1 d . . . . .
C36 C 0.5788(2) -0.01773(19) 0.2123(3) 0.0160(9) Uani 1 1 d . . . . .
C37 C 0.7046(2) -0.0271(2) 0.2950(3) 0.0191(10) Uani 1 1 d . . . . .
H37A H 0.7406 -0.0536 0.3153 0.023 Uiso 1 1 calc R U . . .
C38 C 0.7927(2) 0.0341(2) 0.3732(3) 0.0222(11) Uani 1 1 d . . . . .
C39 C 0.8148(2) 0.0512(2) 0.4552(3) 0.0248(11) Uani 1 1 d . . . . .
H39A H 0.7835 0.0560 0.4738 0.030 Uiso 1 1 calc R U . . .
C40 C 0.8826(3) 0.0611(3) 0.5092(3) 0.0327(13) Uani 1 1 d . . . . .
H40A H 0.8976 0.0732 0.5646 0.039 Uiso 1 1 calc R U . . .
C41 C 0.9291(3) 0.0535(3) 0.4835(4) 0.0410(15) Uani 1 1 d . . . . .
H41A H 0.9755 0.0608 0.5208 0.049 Uiso 1 1 calc R U . . .
C42 C 0.9068(3) 0.0351(3) 0.4017(4) 0.0363(14) Uani 1 1 d . . . . .
H42A H 0.9381 0.0294 0.3835 0.044 Uiso 1 1 calc R U . . .
C43 C 0.8388(2) 0.0252(2) 0.3475(3) 0.0276(12) Uani 1 1 d . . . . .
H43A H 0.8238 0.0122 0.2924 0.033 Uiso 1 1 calc R U . . .
C44 C 0.3967(2) -0.0328(2) 0.0985(3) 0.0231(11) Uani 1 1 d . . . . .
H44A H 0.3944 -0.0449 0.0466 0.035 Uiso 1 1 calc R U . . .
H44B H 0.3632 -0.0030 0.0863 0.035 Uiso 1 1 calc R U . . .
H44C H 0.3873 -0.0654 0.1240 0.035 Uiso 1 1 calc R U . . .
N51 N 0.72658(18) 0.15818(17) 0.3374(2) 0.0180(8) Uani 1 1 d . . . . .
O51 O 0.62488(15) 0.09951(13) 0.35228(18) 0.0155(7) Uani 1 1 d . . . . .
C51 C 0.7145(2) 0.1545(2) 0.4610(3) 0.0190(10) Uani 1 1 d . . . . .
O52 O 0.55860(15) 0.09358(13) 0.42928(19) 0.0166(7) Uani 1 1 d . . . . .
C52 C 0.7419(2) 0.1767(2) 0.5428(3) 0.0220(11) Uani 1 1 d . . . . .
H52A H 0.7839 0.1960 0.5674 0.026 Uiso 1 1 calc R U . . .
C53 C 0.7098(3) 0.1711(2) 0.5872(3) 0.0265(12) Uani 1 1 d . . . . .
H53A H 0.7295 0.1861 0.6421 0.032 Uiso 1 1 calc R U . . .
C54 C 0.6472(2) 0.1430(2) 0.5511(3) 0.0212(10) Uani 1 1 d . . . . .
H54A H 0.6237 0.1397 0.5806 0.025 Uiso 1 1 calc R U . . .
C55 C 0.6209(2) 0.12040(19) 0.4724(3) 0.0151(9) Uani 1 1 d . . . . .
C56 C 0.6534(2) 0.12359(19) 0.4260(3) 0.0157(9) Uani 1 1 d . . . . .
C57 C 0.7456(2) 0.1703(2) 0.4137(3) 0.0202(10) Uani 1 1 d . . . . .
H57A H 0.7853 0.1925 0.4424 0.024 Uiso 1 1 calc R U . . .
C58 C 0.7646(3) 0.1867(2) 0.3053(3) 0.0257(11) Uani 1 1 d . . . . .
C59 C 0.7315(3) 0.2259(2) 0.2416(3) 0.0293(12) Uani 1 1 d . . . . .
H59A H 0.6855 0.2343 0.2218 0.035 Uiso 1 1 calc R U . . .
C60 C 0.7649(3) 0.2531(3) 0.2060(4) 0.0419(16) Uani 1 1 d . . . . .
H60A H 0.7421 0.2798 0.1620 0.050 Uiso 1 1 calc R U . . .
C61 C 0.8318(3) 0.2403(3) 0.2362(4) 0.0470(18) Uani 1 1 d . . . . .
H61A H 0.8549 0.2580 0.2119 0.056 Uiso 1 1 calc R U . . .
C62 C 0.8654(3) 0.2025(3) 0.3005(4) 0.0462(17) Uani 1 1 d . . . . .
H62A H 0.9118 0.1950 0.3214 0.055 Uiso 1 1 calc R U . . .
C63 C 0.8317(3) 0.1752(3) 0.3353(3) 0.0333(13) Uani 1 1 d . . . . .
H63A H 0.8548 0.1487 0.3795 0.040 Uiso 1 1 calc R U . . .
C64 C 0.5295(2) 0.0744(2) 0.4769(3) 0.0202(10) Uani 1 1 d . . . . .
H64A H 0.5602 0.0476 0.5197 0.030 Uiso 1 1 calc R U . . .
H64B H 0.4866 0.0553 0.4399 0.030 Uiso 1 1 calc R U . . .
H64C H 0.5216 0.1070 0.5038 0.030 Uiso 1 1 calc R U . . .
N71 N 0.5000 0.4657(3) -0.2500 0.027(3) Uiso 0.4453 2 d DS U P A 1
O71 O 0.5000 0.4119(3) -0.2500 0.055(4) Uiso 0.4453 2 d DS U P A 1
O72 O 0.5156(5) 0.4908(3) -0.18242(19) 0.045(2) Uiso 0.4453 1 d D U P A 1
O1 O 0.5436(6) 0.2527(5) -0.1672(7) 0.023(3) Uiso 0.2774 1 d . . P B 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
Ni1 O31 2.041(3) . ?
Ni1 O11 2.047(3) . ?
Ni1 O51 2.052(3) . ?
Ni1 N31 2.116(4) . ?
Ni1 N51 2.118(4) . ?
Ni1 N11 2.122(4) . ?
Ni1 La1 3.4361(7) . ?
La1 O11 2.517(3) 2_655 ?
La1 O11 2.517(3) . ?
La1 O51 2.525(3) 2_655 ?
La1 O51 2.525(3) . ?
La1 O31 2.525(3) 2_655 ?
La1 O31 2.525(3) . ?
La1 O52 2.892(3) . ?
La1 O52 2.892(3) 2_655 ?
La1 O32 2.919(3) . ?
La1 O32 2.919(3) 2_655 ?
La1 O12 2.937(3) 2_655 ?
La1 O12 2.937(3) . ?
N11 C17 1.299(6) . ?
N11 C18 1.449(6) . ?
O11 C16 1.319(5) . ?
C11 C16 1.406(7) . ?
C11 C12 1.423(7) . ?
C11 C17 1.434(7) . ?
O12 C15 1.386(6) . ?
O12 C24 1.450(6) . ?
C12 C13 1.373(8) . ?
C12 H12A 0.9500 . ?
C13 C14 1.393(8) . ?
C13 H13A 0.9500 . ?
C14 C15 1.369(7) . ?
C14 H14A 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C15 C16 1.402(7) . ?
C17 H17A 0.9500 . ?
C18 C23 1.382(7) . ?
C18 C19 1.393(7) . ?
C19 C20 1.375(8) . ?
C19 H19A 0.9500 . ?
C20 C21 1.377(8) . ?
C20 H20A 0.9500 . ?
C21 C22 1.409(8) . ?
C21 H21A 0.9500 . ?
C22 C23 1.383(7) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
N31 C37 1.285(6) . ?
N31 C38 1.446(6) . ?
O31 C36 1.310(5) . ?
C31 C36 1.406(6) . ?
C31 C32 1.413(6) . ?
C31 C37 1.452(6) . ?
O32 C35 1.373(5) . ?
O32 C44 1.438(5) . ?
C32 C33 1.384(7) . ?
C32 H32A 0.9500 . ?
C33 C34 1.407(7) . ?
C33 H33A 0.9500 . ?
C34 C35 1.381(6) . ?
C34 H34A 0.9500 . ?
C35 C36 1.420(6) . ?
C37 H37A 0.9500 . ?
C38 C43 1.383(7) . ?
C38 C39 1.399(7) . ?
C39 C40 1.384(7) . ?
C39 H39A 0.9500 . ?
C40 C41 1.386(8) . ?
C40 H40A 0.9500 . ?
C41 C42 1.404(8) . ?
C41 H41A 0.9500 . ?
C42 C43 1.388(7) . ?
C42 H42A 0.9500 . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
N51 C57 1.285(6) . ?
N51 C58 1.450(6) . ?
O51 C56 1.310(5) . ?
C51 C56 1.417(6) . ?
C51 C52 1.417(6) . ?
C51 C57 1.434(7) . ?
O52 C55 1.392(5) . ?
O52 C64 1.427(6) . ?
C52 C53 1.365(7) . ?
C52 H52A 0.9500 . ?
C53 C54 1.411(7) . ?
C53 H53A 0.9500 . ?
C54 C55 1.373(6) . ?
C54 H54A 0.9500 . ?
C55 C56 1.401(7) . ?
C57 H57A 0.9500 . ?
C58 C63 1.381(7) . ?
C58 C59 1.384(7) . ?
C59 C60 1.398(8) . ?
C59 H59A 0.9500 . ?
C60 C61 1.381(9) . ?
C60 H60A 0.9500 . ?
C61 C62 1.371(9) . ?
C61 H61A 0.9500 . ?
C62 C63 1.394(8) . ?
C62 H62A 0.9500 . ?
C63 H63A 0.9500 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
N71 O72 1.2635(10) 2_654 ?
N71 O72 1.2636(10) . ?
N71 O71 1.2643(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O31 Ni1 O11 78.21(12) . . ?
O31 Ni1 O51 78.12(12) . . ?
O11 Ni1 O51 78.41(12) . . ?
O31 Ni1 N31 87.46(13) . . ?
O11 Ni1 N31 165.64(14) . . ?
O51 Ni1 N31 98.08(14) . . ?
O31 Ni1 N51 164.30(15) . . ?
O11 Ni1 N51 97.47(14) . . ?
O51 Ni1 N51 86.24(14) . . ?
N31 Ni1 N51 96.17(15) . . ?
O31 Ni1 N11 98.51(14) . . ?
O11 Ni1 N11 87.25(14) . . ?
O51 Ni1 N11 165.65(14) . . ?
N31 Ni1 N11 95.68(15) . . ?
N51 Ni1 N11 96.33(15) . . ?
O31 Ni1 La1 46.83(9) . . ?
O11 Ni1 La1 46.63(9) . . ?
O51 Ni1 La1 46.85(8) . . ?
N31 Ni1 La1 121.45(11) . . ?
N51 Ni1 La1 119.85(11) . . ?
N11 Ni1 La1 121.25(10) . . ?
O11 La1 O11 121.89(14) 2_655 . ?
O11 La1 O51 61.85(10) 2_655 2_655 ?
O11 La1 O51 115.51(10) . 2_655 ?
O11 La1 O51 115.52(10) 2_655 . ?
O11 La1 O51 61.85(10) . . ?
O51 La1 O51 175.16(14) 2_655 . ?
O11 La1 O31 61.51(10) 2_655 2_655 ?
O11 La1 O31 174.47(10) . 2_655 ?
O51 La1 O31 61.44(10) 2_655 2_655 ?
O51 La1 O31 121.55(10) . 2_655 ?
O11 La1 O31 174.48(10) 2_655 . ?
O11 La1 O31 61.51(10) . . ?
O51 La1 O31 121.55(10) 2_655 . ?
O51 La1 O31 61.43(10) . . ?
O31 La1 O31 115.48(14) 2_655 . ?
O11 La1 O52 68.67(9) 2_655 . ?
O11 La1 O52 112.01(9) . . ?
O51 La1 O52 123.90(9) 2_655 . ?
O51 La1 O52 56.17(9) . . ?
O31 La1 O52 73.03(9) 2_655 . ?
O31 La1 O52 106.25(9) . . ?
O11 La1 O52 112.01(9) 2_655 2_655 ?
O11 La1 O52 68.67(9) . 2_655 ?
O51 La1 O52 56.17(9) 2_655 2_655 ?
O51 La1 O52 123.89(9) . 2_655 ?
O31 La1 O52 106.25(9) 2_655 2_655 ?
O31 La1 O52 73.03(9) . 2_655 ?
O52 La1 O52 178.70(13) . 2_655 ?
O11 La1 O32 124.53(9) 2_655 . ?
O11 La1 O32 105.24(10) . . ?
O51 La1 O32 72.95(9) 2_655 . ?
O51 La1 O32 111.43(9) . . ?
O31 La1 O32 69.68(10) 2_655 . ?
O31 La1 O32 55.62(9) . . ?
O52 La1 O32 120.52(9) . . ?
O52 La1 O32 58.19(9) 2_655 . ?
O11 La1 O32 105.24(10) 2_655 2_655 ?
O11 La1 O32 124.53(9) . 2_655 ?
O51 La1 O32 111.43(9) 2_655 2_655 ?
O51 La1 O32 72.95(9) . 2_655 ?
O31 La1 O32 55.62(9) 2_655 2_655 ?
O31 La1 O32 69.68(10) . 2_655 ?
O52 La1 O32 58.19(9) . 2_655 ?
O52 La1 O32 120.52(9) 2_655 2_655 ?
O32 La1 O32 62.64(12) . 2_655 ?
O11 La1 O12 55.55(9) 2_655 2_655 ?
O11 La1 O12 73.16(10) . 2_655 ?
O51 La1 O12 105.26(9) 2_655 2_655 ?
O51 La1 O12 70.27(9) . 2_655 ?
O31 La1 O12 111.81(10) 2_655 2_655 ?
O31 La1 O12 124.66(9) . 2_655 ?
O52 La1 O12 62.52(9) . 2_655 ?
O52 La1 O12 118.77(9) 2_655 2_655 ?
O32 La1 O12 176.94(9) . 2_655 ?
O32 La1 O12 120.41(9) 2_655 2_655 ?
O11 La1 O12 73.16(10) 2_655 . ?
O11 La1 O12 55.54(9) . . ?
O51 La1 O12 70.27(9) 2_655 . ?
O51 La1 O12 105.26(9) . . ?
O31 La1 O12 124.66(9) 2_655 . ?
O31 La1 O12 111.81(10) . . ?
O52 La1 O12 118.77(9) . . ?
O52 La1 O12 62.53(9) 2_655 . ?
O32 La1 O12 120.41(9) . . ?
O32 La1 O12 176.94(9) 2_655 . ?
O12 La1 O12 56.53(13) 2_655 . ?
C17 N11 C18 113.0(4) . . ?
C17 N11 Ni1 123.5(3) . . ?
C18 N11 Ni1 122.5(3) . . ?
C16 O11 Ni1 130.2(3) . . ?
C16 O11 La1 127.5(3) . . ?
Ni1 O11 La1 97.14(12) . . ?
C16 C11 C12 119.1(5) . . ?
C16 C11 C17 124.2(4) . . ?
C12 C11 C17 116.6(5) . . ?
C15 O12 C24 117.8(4) . . ?
C15 O12 La1 114.4(3) . . ?
C24 O12 La1 127.5(3) . . ?
C13 C12 C11 120.0(5) . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C12 C13 C14 120.8(5) . . ?
C12 C13 H13A 119.6 . . ?
C14 C13 H13A 119.6 . . ?
C15 C14 C13 119.3(5) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
O12 C24 H24A 109.5 . . ?
O12 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O12 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C14 C15 O12 125.3(5) . . ?
C14 C15 C16 122.0(5) . . ?
O12 C15 C16 112.7(4) . . ?
O11 C16 C15 118.3(4) . . ?
O11 C16 C11 123.3(4) . . ?
C15 C16 C11 118.4(4) . . ?
N11 C17 C11 128.5(5) . . ?
N11 C17 H17A 115.8 . . ?
C11 C17 H17A 115.8 . . ?
C23 C18 C19 119.9(5) . . ?
C23 C18 N11 120.0(4) . . ?
C19 C18 N11 120.0(5) . . ?
C20 C19 C18 120.3(5) . . ?
C20 C19 H19A 119.8 . . ?
C18 C19 H19A 119.8 . . ?
C19 C20 C21 120.3(5) . . ?
C19 C20 H20A 119.9 . . ?
C21 C20 H20A 119.9 . . ?
C20 C21 C22 119.8(5) . . ?
C20 C21 H21A 120.1 . . ?
C22 C21 H21A 120.1 . . ?
C23 C22 C21 119.6(5) . . ?
C23 C22 H22A 120.2 . . ?
C21 C22 H22A 120.2 . . ?
C18 C23 C22 120.1(5) . . ?
C18 C23 H23A 120.0 . . ?
C22 C23 H23A 120.0 . . ?
C37 N31 C38 115.0(4) . . ?
C37 N31 Ni1 124.1(3) . . ?
C38 N31 Ni1 120.4(3) . . ?
C36 O31 Ni1 129.9(3) . . ?
C36 O31 La1 127.2(3) . . ?
Ni1 O31 La1 97.04(12) . . ?
C36 C31 C32 119.4(4) . . ?
C36 C31 C37 123.1(4) . . ?
C32 C31 C37 117.3(4) . . ?
C35 O32 C44 116.7(3) . . ?
C35 O32 La1 114.3(2) . . ?
C44 O32 La1 128.7(3) . . ?
C33 C32 C31 120.9(4) . . ?
C33 C32 H32A 119.5 . . ?
C31 C32 H32A 119.5 . . ?
C32 C33 C34 120.2(4) . . ?
C32 C33 H33A 119.9 . . ?
C34 C33 H33A 119.9 . . ?
C35 C34 C33 119.1(4) . . ?
C35 C34 H34A 120.5 . . ?
C33 C34 H34A 120.5 . . ?
O32 C35 C34 124.9(4) . . ?
O32 C35 C36 113.1(4) . . ?
C34 C35 C36 121.9(4) . . ?
O31 C36 C31 124.4(4) . . ?
O31 C36 C35 117.3(4) . . ?
C31 C36 C35 118.3(4) . . ?
N31 C37 C31 128.4(4) . . ?
N31 C37 H37A 115.8 . . ?
C31 C37 H37A 115.8 . . ?
C43 C38 C39 119.8(4) . . ?
C43 C38 N31 121.5(4) . . ?
C39 C38 N31 118.7(4) . . ?
C40 C39 C38 119.5(5) . . ?
C40 C39 H39A 120.2 . . ?
C38 C39 H39A 120.2 . . ?
C39 C40 C41 121.0(5) . . ?
C39 C40 H40A 119.5 . . ?
C41 C40 H40A 119.5 . . ?
C40 C41 C42 119.2(5) . . ?
C40 C41 H41A 120.4 . . ?
C42 C41 H41A 120.4 . . ?
C43 C42 C41 119.8(5) . . ?
C43 C42 H42A 120.1 . . ?
C41 C42 H42A 120.1 . . ?
C38 C43 C42 120.5(5) . . ?
C38 C43 H43A 119.7 . . ?
C42 C43 H43A 119.7 . . ?
O32 C44 H44A 109.5 . . ?
O32 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O32 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C57 N51 C58 114.3(4) . . ?
C57 N51 Ni1 124.8(3) . . ?
C58 N51 Ni1 120.4(3) . . ?
C56 O51 Ni1 130.7(3) . . ?
C56 O51 La1 125.7(3) . . ?
Ni1 O51 La1 96.78(11) . . ?
C56 C51 C52 118.8(4) . . ?
C56 C51 C57 122.7(4) . . ?
C52 C51 C57 118.1(4) . . ?
C55 O52 C64 117.3(3) . . ?
C55 O52 La1 113.8(3) . . ?
C64 O52 La1 128.7(2) . . ?
C53 C52 C51 121.8(4) . . ?
C53 C52 H52A 119.1 . . ?
C51 C52 H52A 119.1 . . ?
C52 C53 C54 119.7(5) . . ?
C52 C53 H53A 120.2 . . ?
C54 C53 H53A 120.2 . . ?
C55 C54 C53 118.8(5) . . ?
C55 C54 H54A 120.6 . . ?
C53 C54 H54A 120.6 . . ?
C54 C55 O52 124.0(4) . . ?
C54 C55 C56 123.2(4) . . ?
O52 C55 C56 112.7(4) . . ?
O51 C56 C55 118.6(4) . . ?
O51 C56 C51 123.9(4) . . ?
C55 C56 C51 117.5(4) . . ?
N51 C57 C51 128.3(4) . . ?
N51 C57 H57A 115.8 . . ?
C51 C57 H57A 115.8 . . ?
C63 C58 C59 119.7(5) . . ?
C63 C58 N51 122.0(5) . . ?
C59 C58 N51 118.3(5) . . ?
C58 C59 C60 120.8(6) . . ?
C58 C59 H59A 119.6 . . ?
C60 C59 H59A 119.6 . . ?
C61 C60 C59 118.5(6) . . ?
C61 C60 H60A 120.7 . . ?
C59 C60 H60A 120.7 . . ?
C62 C61 C60 121.2(6) . . ?
C62 C61 H61A 119.4 . . ?
C60 C61 H61A 119.4 . . ?
C61 C62 C63 120.0(6) . . ?
C61 C62 H62A 120.0 . . ?
C63 C62 H62A 120.0 . . ?
C58 C63 C62 119.8(6) . . ?
C58 C63 H63A 120.1 . . ?
C62 C63 H63A 120.1 . . ?
O52 C64 H64A 109.5 . . ?
O52 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
O52 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O72 N71 O72 124.2(3) 2_654 . ?
O72 N71 O71 117.88(14) 2_654 . ?
O72 N71 O71 117.88(14) . . ?

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
C16 C11 C12 C13 -0.5(8) . . . . ?
C17 C11 C12 C13 175.5(5) . . . . ?
C11 C12 C13 C14 -2.8(9) . . . . ?
C12 C13 C14 C15 1.4(9) . . . . ?
C13 C14 C15 O12 -175.4(5) . . . . ?
C13 C14 C15 C16 3.3(8) . . . . ?
C24 O12 C15 C14 -13.4(7) . . . . ?
La1 O12 C15 C14 160.4(4) . . . . ?
C24 O12 C15 C16 167.9(4) . . . . ?
La1 O12 C15 C16 -18.3(5) . . . . ?
Ni1 O11 C16 C15 -175.1(3) . . . . ?
La1 O11 C16 C15 36.4(6) . . . . ?
Ni1 O11 C16 C11 6.7(6) . . . . ?
La1 O11 C16 C11 -141.8(4) . . . . ?
C14 C15 C16 O11 175.3(4) . . . . ?
O12 C15 C16 O11 -5.9(6) . . . . ?
C14 C15 C16 C11 -6.4(7) . . . . ?
O12 C15 C16 C11 172.3(4) . . . . ?
C12 C11 C16 O11 -176.8(4) . . . . ?
C17 C11 C16 O11 7.4(7) . . . . ?
C12 C11 C16 C15 5.0(7) . . . . ?
C17 C11 C16 C15 -170.8(4) . . . . ?
C18 N11 C17 C11 179.0(5) . . . . ?
Ni1 N11 C17 C11 -12.4(7) . . . . ?
C16 C11 C17 N11 -3.8(8) . . . . ?
C12 C11 C17 N11 -179.6(5) . . . . ?
C17 N11 C18 C23 -119.0(5) . . . . ?
Ni1 N11 C18 C23 72.2(5) . . . . ?
C17 N11 C18 C19 61.0(6) . . . . ?
Ni1 N11 C18 C19 -107.7(5) . . . . ?
C23 C18 C19 C20 -1.6(8) . . . . ?
N11 C18 C19 C20 178.4(5) . . . . ?
C18 C19 C20 C21 1.9(9) . . . . ?
C19 C20 C21 C22 -0.9(9) . . . . ?
C20 C21 C22 C23 -0.5(8) . . . . ?
C19 C18 C23 C22 0.2(7) . . . . ?
N11 C18 C23 C22 -179.7(4) . . . . ?
C21 C22 C23 C18 0.8(8) . . . . ?
C36 C31 C32 C33 -1.1(7) . . . . ?
C37 C31 C32 C33 173.2(5) . . . . ?
C31 C32 C33 C34 -2.2(8) . . . . ?
C32 C33 C34 C35 1.9(7) . . . . ?
C44 O32 C35 C34 -17.2(6) . . . . ?
La1 O32 C35 C34 157.4(4) . . . . ?
C44 O32 C35 C36 165.0(4) . . . . ?
La1 O32 C35 C36 -20.5(5) . . . . ?
C33 C34 C35 O32 -176.0(4) . . . . ?
C33 C34 C35 C36 1.7(7) . . . . ?
Ni1 O31 C36 C31 5.5(7) . . . . ?
La1 O31 C36 C31 -141.1(4) . . . . ?
Ni1 O31 C36 C35 -177.2(3) . . . . ?
La1 O31 C36 C35 36.2(5) . . . . ?
C32 C31 C36 O31 -178.2(4) . . . . ?
C37 C31 C36 O31 7.9(7) . . . . ?
C32 C31 C36 C35 4.5(7) . . . . ?
C37 C31 C36 C35 -169.4(4) . . . . ?
O32 C35 C36 O31 -4.5(6) . . . . ?
C34 C35 C36 O31 177.6(4) . . . . ?
O32 C35 C36 C31 173.0(4) . . . . ?
C34 C35 C36 C31 -4.9(7) . . . . ?
C38 N31 C37 C31 177.4(5) . . . . ?
Ni1 N31 C37 C31 -11.1(7) . . . . ?
C36 C31 C37 N31 -4.4(8) . . . . ?
C32 C31 C37 N31 -178.4(5) . . . . ?
C37 N31 C38 C43 65.8(6) . . . . ?
Ni1 N31 C38 C43 -106.0(5) . . . . ?
C37 N31 C38 C39 -112.7(5) . . . . ?
Ni1 N31 C38 C39 75.5(5) . . . . ?
C43 C38 C39 C40 2.4(8) . . . . ?
N31 C38 C39 C40 -179.0(5) . . . . ?
C38 C39 C40 C41 -0.9(9) . . . . ?
C39 C40 C41 C42 -0.6(10) . . . . ?
C40 C41 C42 C43 0.6(10) . . . . ?
C39 C38 C43 C42 -2.4(8) . . . . ?
N31 C38 C43 C42 179.1(5) . . . . ?
C41 C42 C43 C38 0.9(9) . . . . ?
C56 C51 C52 C53 -2.7(7) . . . . ?
C57 C51 C52 C53 169.8(5) . . . . ?
C51 C52 C53 C54 -0.6(8) . . . . ?
C52 C53 C54 C55 1.8(7) . . . . ?
C53 C54 C55 O52 -177.6(4) . . . . ?
C53 C54 C55 C56 0.4(7) . . . . ?
C64 O52 C55 C54 -18.3(6) . . . . ?
La1 O52 C55 C54 155.9(4) . . . . ?
C64 O52 C55 C56 163.6(4) . . . . ?
La1 O52 C55 C56 -22.3(4) . . . . ?
Ni1 O51 C56 C55 179.7(3) . . . . ?
La1 O51 C56 C55 35.8(5) . . . . ?
Ni1 O51 C56 C51 1.8(6) . . . . ?
La1 O51 C56 C51 -142.1(4) . . . . ?
C54 C55 C56 O51 178.4(4) . . . . ?
O52 C55 C56 O51 -3.5(6) . . . . ?
C54 C55 C56 C51 -3.6(7) . . . . ?
O52 C55 C56 C51 174.6(4) . . . . ?
C52 C51 C56 O51 -177.5(4) . . . . ?
C57 C51 C56 O51 10.4(7) . . . . ?
C52 C51 C56 C55 4.6(7) . . . . ?
C57 C51 C56 C55 -167.5(4) . . . . ?
C58 N51 C57 C51 172.6(5) . . . . ?
Ni1 N51 C57 C51 -14.9(7) . . . . ?
C56 C51 C57 N51 -3.0(8) . . . . ?
C52 C51 C57 N51 -175.1(5) . . . . ?
C57 N51 C58 C63 66.6(6) . . . . ?
Ni1 N51 C58 C63 -106.2(5) . . . . ?
C57 N51 C58 C59 -114.6(5) . . . . ?
Ni1 N51 C58 C59 72.6(5) . . . . ?
C63 C58 C59 C60 1.3(8) . . . . ?
N51 C58 C59 C60 -177.6(5) . . . . ?
C58 C59 C60 C61 -0.4(8) . . . . ?
C59 C60 C61 C62 -1.1(9) . . . . ?
C60 C61 C62 C63 1.6(9) . . . . ?
C59 C58 C63 C62 -0.8(8) . . . . ?
N51 C58 C63 C62 178.0(5) . . . . ?
C61 C62 C63 C58 -0.6(9) . . . . ?

_refine_diff_density_max         1.886
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.138



####################################################################### 
# 
# 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_ni2dy2_sq
_database_code_depnum_ccdc_archive 'CCDC 1424758'
_audit_update_record             
;
2016-01-02 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'Ni2Dy2C48 H46N4O24'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H46 Dy2 N4 Ni2 O24'
_chemical_formula_weight         1505.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   12.530(5)
_cell_length_b                   12.446(4)
_cell_length_c                   20.918(8)
_cell_angle_alpha                90
_cell_angle_beta                 102.904(5)
_cell_angle_gamma                90
_cell_volume                     3180(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6903
_cell_measurement_theta_min      3.088
_cell_measurement_theta_max      27.998

_exptl_crystal_description       Needle
_exptl_crystal_colour            'Pale Green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_F_000             1484
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.980
_shelx_estimated_absorpt_T_min   0.647
_shelx_estimated_absorpt_T_max   0.796
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.6463
_exptl_absorpt_correction_T_max  0.7960
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38888
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.088
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7673
_reflns_number_gt                7015
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

;

_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
All non-hydrogen atoms were refined anisotropically except disorded benzene ring of ligands which is refined iostropically.Hydrogen atoms are
added in its calculated geometric position which are refined as riding model. Several restrains/constrains have used like SIMU,
DELU, DFIX, AFIX etc.

 Due to the diffused electron density, the solvent molecules could not be
modelled, hence SQUZZEE routine was employed.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+22.3531P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7673
_refine_ls_number_parameters     323
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0726
_refine_ls_wR_factor_ref         0.1591
_refine_ls_wR_factor_gt          0.1518
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_restrained_S_all      1.218
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.52601(3) 0.13271(3) 0.05520(2) 0.02678(12) Uani 1 1 d . . . . .
Ni2 Ni 0.70038(8) 0.24370(8) -0.03089(5) 0.0322(2) Uani 1 1 d . . . . .
O11 O 0.7069(4) 0.1537(4) 0.0507(3) 0.0332(12) Uani 1 1 d . . . . .
O12 O 0.6624(5) 0.0235(4) 0.1376(2) 0.0335(12) Uani 1 1 d . . . . .
O31 O 0.5412(4) 0.2604(4) -0.0246(2) 0.0318(11) Uani 1 1 d . . . . .
O32 O 0.3480(4) 0.1867(4) -0.0182(2) 0.0324(11) Uani 1 1 d . . . . .
O33 O 0.6688(6) 0.3477(5) -0.1095(3) 0.0485(16) Uani 1 1 d . . . . .
O41 O 0.7432(5) 0.3784(4) 0.0294(3) 0.0410(14) Uani 1 1 d . . . . .
H41 H 0.8169 0.3849 0.0533 0.049 Uiso 1 1 calc R U . . .
O51 O 0.4040(5) 0.0522(4) 0.1166(2) 0.0362(12) Uani 1 1 d D . . . .
O52 O 0.4503(4) -0.0393(4) 0.0388(2) 0.0340(12) Uani 1 1 d D . . . .
O53 O 0.6661(5) 0.1106(4) -0.0929(3) 0.0447(15) Uani 1 1 d . . . . .
O61 O 0.4469(4) 0.2937(4) 0.0964(3) 0.0359(12) Uani 1 1 d . . . . .
O62 O 0.5936(5) 0.2317(4) 0.1591(3) 0.0398(13) Uani 1 1 d . . . . .
O63 O 0.5122(6) 0.3710(5) 0.1906(3) 0.0569(19) Uani 1 1 d . . . . .
N11 N 0.8640(5) 0.2214(5) -0.0236(4) 0.0380(15) Uani 1 1 d . . . . .
N61 N 0.5174(5) 0.3017(4) 0.1504(3) 0.0380(16) Uani 1 1 d . . . . .
C11 C 0.8942(7) 0.0954(7) 0.0683(4) 0.042(2) Uani 1 1 d . . . . .
C12 C 0.9778(8) 0.0286(8) 0.1064(5) 0.053(2) Uani 1 1 d . . . . .
H12A H 1.0489 0.0284 0.0975 0.064 Uiso 1 1 calc R U . . .
C13 C 0.9567(8) -0.0351(7) 0.1558(5) 0.048(2) Uani 1 1 d . . . . .
H13A H 1.0137 -0.0770 0.1818 0.058 Uiso 1 1 calc R U . . .
C14 C 0.8510(8) -0.0383(7) 0.1678(4) 0.043(2) Uani 1 1 d . . . . .
H14A H 0.8361 -0.0831 0.2015 0.052 Uiso 1 1 calc R U . . .
C15 C 0.7698(7) 0.0227(6) 0.1312(4) 0.0336(17) Uani 1 1 d . . . . .
C16 C 0.7883(6) 0.0939(6) 0.0813(4) 0.0337(17) Uani 1 1 d . . . . .
C17 C 0.9256(8) 0.1620(7) 0.0176(5) 0.045(2) Uani 1 1 d . . . . .
H17A H 1.0006 0.1602 0.0156 0.053 Uiso 1 1 calc R U . . .
C18 C 0.9152(6) 0.2866(6) -0.0680(3) 0.058(2) Uiso 1 1 d G U . . .
C19 C 0.8882(6) 0.2708(6) -0.1355(4) 0.077(3) Uiso 1 1 d G U . . .
H19 H 0.8356 0.2179 -0.1539 0.093 Uiso 1 1 calc R U . . .
C20 C 0.9381(7) 0.3324(7) -0.1760(3) 0.083(3) Uiso 1 1 d G U . . .
H20 H 0.9196 0.3216 -0.2221 0.100 Uiso 1 1 calc R U . . .
C21 C 1.0150(7) 0.4097(7) -0.1490(4) 0.085(3) Uiso 1 1 d G U . . .
H21 H 1.0491 0.4518 -0.1767 0.102 Uiso 1 1 calc R U . . .
C22 C 1.0421(6) 0.4256(6) -0.0816(4) 0.087(4) Uiso 1 1 d G U . . .
H22 H 1.0947 0.4784 -0.0631 0.104 Uiso 1 1 calc R U . . .
C23 C 0.9922(7) 0.3640(6) -0.0411(3) 0.072(3) Uiso 1 1 d G U . . .
H23 H 1.0107 0.3748 0.0051 0.087 Uiso 1 1 calc R U . . .
C24 C 0.6383(7) -0.0332(6) 0.1926(4) 0.0372(18) Uani 1 1 d . . . . .
H24A H 0.6377 -0.1107 0.1841 0.056 Uiso 1 1 calc R U . . .
H24B H 0.5663 -0.0109 0.1989 0.056 Uiso 1 1 calc R U . . .
H24C H 0.6943 -0.0167 0.2321 0.056 Uiso 1 1 calc R U . . .
C31 C 0.4718(8) 0.3374(6) -0.1321(4) 0.0376(19) Uani 1 1 d . . . . .
C32 C 0.3798(9) 0.3607(7) -0.1824(4) 0.048(2) Uani 1 1 d . . . . .
H32A H 0.3890 0.3995 -0.2199 0.058 Uiso 1 1 calc R U . . .
C33 C 0.2767(7) 0.3283(7) -0.1782(4) 0.041(2) Uani 1 1 d . . . . .
H33A H 0.2149 0.3441 -0.2124 0.049 Uiso 1 1 calc R U . . .
C34 C 0.2648(7) 0.2718(6) -0.1226(4) 0.0374(18) Uani 1 1 d . . . . .
H34A H 0.1938 0.2500 -0.1189 0.045 Uiso 1 1 calc R U . . .
C35 C 0.3527(6) 0.2470(5) -0.0737(3) 0.0262(14) Uani 1 1 d . . . . .
C36 C 0.4595(7) 0.2812(6) -0.0754(4) 0.0324(16) Uani 1 1 d . . . . .
C37 C 0.5776(8) 0.3731(7) -0.1417(5) 0.043(2) Uani 1 1 d . . . . .
H37A H 0.5762 0.4217 -0.1769 0.051 Uiso 1 1 calc R U . . .
C38 C 0.2413(7) 0.1772(7) -0.0027(4) 0.0396(19) Uani 1 1 d . . . . .
H38A H 0.2091 0.2488 -0.0019 0.059 Uiso 1 1 calc R U . . .
H38B H 0.2491 0.1433 0.0404 0.059 Uiso 1 1 calc R U . . .
H38C H 0.1936 0.1331 -0.0361 0.059 Uiso 1 1 calc R U . . .
C41 C 0.6680(9) 0.4604(8) 0.0365(6) 0.063(3) Uani 1 1 d . . . . .
H41A H 0.7058 0.5152 0.0670 0.095 Uiso 1 1 calc R U . . .
H41B H 0.6381 0.4934 -0.0063 0.095 Uiso 1 1 calc R U . . .
H41C H 0.6083 0.4293 0.0537 0.095 Uiso 1 1 calc R U . . .
C51 C 0.3945(4) -0.0342(4) 0.0832(2) 0.0362(18) Uani 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O11 2.305(5) . ?
Dy1 O52 2.336(5) . ?
Dy1 O31 2.343(5) . ?
Dy1 O52 2.359(4) 3_655 ?
Dy1 O51 2.422(5) . ?
Dy1 O61 2.474(5) . ?
Dy1 O62 2.478(5) . ?
Dy1 O32 2.500(5) . ?
Dy1 O12 2.535(5) . ?
Dy1 C51 2.794(6) . ?
Dy1 N61 2.915(6) . ?
Dy1 Ni2 3.4180(13) . ?
Ni2 O11 2.027(5) . ?
Ni2 O31 2.038(5) . ?
Ni2 N11 2.041(7) . ?
Ni2 O33 2.060(6) . ?
Ni2 O53 2.088(5) . ?
Ni2 O41 2.094(5) . ?
O11 C16 1.308(9) . ?
O12 C15 1.383(10) . ?
O12 C24 1.437(9) . ?
O31 C36 1.325(9) . ?
O32 C35 1.394(8) . ?
O32 C38 1.449(9) . ?
O33 C37 1.231(11) . ?
O41 C41 1.419(11) . ?
O41 H41 0.9500 . ?
O51 C51 1.273(6) . ?
O52 C51 1.283(6) . ?
O52 Dy1 2.359(4) 3_655 ?
O53 C51 1.261(6) 3_655 ?
O61 N61 1.274(8) . ?
O62 N61 1.276(8) . ?
O63 N61 1.217(8) . ?
N11 C17 1.259(12) . ?
N11 C18 1.484(9) . ?
C11 C16 1.412(11) . ?
C11 C12 1.432(13) . ?
C11 C17 1.469(12) . ?
C12 C13 1.374(14) . ?
C12 H12A 0.9500 . ?
C13 C14 1.402(13) . ?
C13 H13A 0.9500 . ?
C14 C15 1.360(12) . ?
C14 H14A 0.9500 . ?
C15 C16 1.427(11) . ?
C17 H17A 0.9500 . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9500 . ?
C20 C21 1.3900 . ?
C20 H20 0.9500 . ?
C21 C22 1.3900 . ?
C21 H21 0.9500 . ?
C22 C23 1.3900 . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C32 1.407(12) . ?
C31 C36 1.416(11) . ?
C31 C37 1.453(12) . ?
C32 C33 1.375(13) . ?
C32 H32A 0.9500 . ?
C33 C34 1.395(12) . ?
C33 H33A 0.9500 . ?
C34 C35 1.362(10) . ?
C34 H34A 0.9500 . ?
C35 C36 1.412(10) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C51 O53 1.261(6) 3_655 ?

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
O11 Dy1 O52 117.96(18) . . ?
O11 Dy1 O31 69.91(19) . . ?
O52 Dy1 O31 127.74(17) . . ?
O11 Dy1 O52 73.33(18) . 3_655 ?
O52 Dy1 O52 63.18(18) . 3_655 ?
O31 Dy1 O52 72.24(17) . 3_655 ?
O11 Dy1 O51 144.26(19) . . ?
O52 Dy1 O51 54.21(14) . . ?
O31 Dy1 O51 145.05(19) . . ?
O52 Dy1 O51 116.76(15) 3_655 . ?
O11 Dy1 O61 113.39(18) . . ?
O52 Dy1 O61 127.74(17) . . ?
O31 Dy1 O61 78.53(18) . . ?
O52 Dy1 O61 145.47(18) 3_655 . ?
O51 Dy1 O61 78.51(17) . . ?
O11 Dy1 O62 80.40(19) . . ?
O52 Dy1 O62 129.25(18) . . ?
O31 Dy1 O62 102.79(19) . . ?
O52 Dy1 O62 153.40(19) 3_655 . ?
O51 Dy1 O62 82.70(17) . . ?
O61 Dy1 O62 51.47(18) . . ?
O11 Dy1 O32 134.01(18) . . ?
O52 Dy1 O32 83.04(18) . . ?
O31 Dy1 O32 65.40(18) . . ?
O52 Dy1 O32 83.22(18) 3_655 . ?
O51 Dy1 O32 81.65(18) . . ?
O61 Dy1 O32 67.91(17) . . ?
O62 Dy1 O32 119.23(18) . . ?
O11 Dy1 O12 64.46(18) . . ?
O52 Dy1 O12 78.36(18) . . ?
O31 Dy1 O12 134.31(18) . . ?
O52 Dy1 O12 96.38(18) 3_655 . ?
O51 Dy1 O12 80.04(18) . . ?
O61 Dy1 O12 117.37(17) . . ?
O62 Dy1 O12 67.89(18) . . ?
O32 Dy1 O12 159.24(17) . . ?
O11 Dy1 C51 136.44(16) . . ?
O52 Dy1 C51 27.14(14) . . ?
O31 Dy1 C51 143.06(15) . . ?
O52 Dy1 C51 89.92(17) 3_655 . ?
O51 Dy1 C51 27.08(14) . . ?
O61 Dy1 C51 103.18(17) . . ?
O62 Dy1 C51 106.73(17) . . ?
O32 Dy1 C51 80.88(14) . . ?
O12 Dy1 C51 78.36(14) . . ?
O11 Dy1 N61 97.66(16) . . ?
O52 Dy1 N61 133.30(12) . . ?
O31 Dy1 N61 91.06(16) . . ?
O52 Dy1 N61 162.85(13) 3_655 . ?
O51 Dy1 N61 79.16(12) . . ?
O61 Dy1 N61 25.71(17) . . ?
O62 Dy1 N61 25.76(17) . . ?
O32 Dy1 N61 93.52(18) . . ?
O12 Dy1 N61 92.57(17) . . ?
C51 Dy1 N61 106.23(14) . . ?
O11 Dy1 Ni2 35.13(13) . . ?
O52 Dy1 Ni2 125.42(11) . . ?
O31 Dy1 Ni2 35.64(13) . . ?
O52 Dy1 Ni2 62.97(11) 3_655 . ?
O51 Dy1 Ni2 179.29(13) . . ?
O61 Dy1 Ni2 102.07(13) . . ?
O62 Dy1 Ni2 97.34(14) . . ?
O32 Dy1 Ni2 98.94(12) . . ?
O12 Dy1 Ni2 99.32(13) . . ?
C51 Dy1 Ni2 152.55(12) . . ?
N61 Dy1 Ni2 101.18(7) . . ?
O11 Ni2 O31 81.9(2) . . ?
O11 Ni2 N11 90.6(3) . . ?
O31 Ni2 N11 172.0(3) . . ?
O11 Ni2 O33 169.5(3) . . ?
O31 Ni2 O33 88.3(2) . . ?
N11 Ni2 O33 99.0(3) . . ?
O11 Ni2 O53 92.8(2) . . ?
O31 Ni2 O53 93.0(2) . . ?
N11 Ni2 O53 90.1(3) . . ?
O33 Ni2 O53 91.5(2) . . ?
O11 Ni2 O41 88.8(2) . . ?
O31 Ni2 O41 90.1(2) . . ?
N11 Ni2 O41 86.9(3) . . ?
O33 Ni2 O41 87.4(2) . . ?
O53 Ni2 O41 176.7(2) . . ?
O11 Ni2 Dy1 40.87(15) . . ?
O31 Ni2 Dy1 42.05(14) . . ?
N11 Ni2 Dy1 130.9(2) . . ?
O33 Ni2 Dy1 130.01(19) . . ?
O53 Ni2 Dy1 86.53(13) . . ?
O41 Ni2 Dy1 96.55(16) . . ?
C16 O11 Ni2 127.4(5) . . ?
C16 O11 Dy1 125.6(5) . . ?
Ni2 O11 Dy1 104.0(2) . . ?
C15 O12 C24 117.2(6) . . ?
C15 O12 Dy1 117.4(4) . . ?
C24 O12 Dy1 125.2(5) . . ?
C36 O31 Ni2 124.1(5) . . ?
C36 O31 Dy1 122.1(5) . . ?
Ni2 O31 Dy1 102.3(2) . . ?
C35 O32 C38 116.2(6) . . ?
C35 O32 Dy1 117.3(4) . . ?
C38 O32 Dy1 125.6(4) . . ?
C37 O33 Ni2 126.0(6) . . ?
C41 O41 Ni2 123.5(6) . . ?
C41 O41 H41 118.2 . . ?
Ni2 O41 H41 118.2 . . ?
C51 O51 Dy1 92.9(4) . . ?
C51 O52 Dy1 96.7(4) . . ?
C51 O52 Dy1 145.0(4) . 3_655 ?
Dy1 O52 Dy1 116.82(18) . 3_655 ?
C51 O53 Ni2 123.1(4) 3_655 . ?
N61 O61 Dy1 96.9(4) . . ?
N61 O62 Dy1 96.6(4) . . ?
C17 N11 C18 117.7(7) . . ?
C17 N11 Ni2 125.7(6) . . ?
C18 N11 Ni2 116.5(5) . . ?
O63 N61 O61 122.4(7) . . ?
O63 N61 O62 122.6(7) . . ?
O61 N61 O62 115.0(6) . . ?
O63 N61 Dy1 178.7(3) . . ?
O61 N61 Dy1 57.4(3) . . ?
O62 N61 Dy1 57.6(3) . . ?
C16 C11 C12 119.2(8) . . ?
C16 C11 C17 124.1(8) . . ?
C12 C11 C17 116.7(8) . . ?
C13 C12 C11 120.9(9) . . ?
C13 C12 H12A 119.5 . . ?
C11 C12 H12A 119.5 . . ?
C12 C13 C14 119.9(8) . . ?
C12 C13 H13A 120.1 . . ?
C14 C13 H13A 120.1 . . ?
C15 C14 C13 120.1(8) . . ?
C15 C14 H14A 120.0 . . ?
C13 C14 H14A 120.0 . . ?
C14 C15 O12 124.8(7) . . ?
C14 C15 C16 122.4(8) . . ?
O12 C15 C16 112.8(7) . . ?
O11 C16 C11 124.2(7) . . ?
O11 C16 C15 118.4(7) . . ?
C11 C16 C15 117.4(7) . . ?
N11 C17 C11 127.1(8) . . ?
N11 C17 H17A 116.4 . . ?
C11 C17 H17A 116.4 . . ?
C19 C18 C23 120.0 . . ?
C19 C18 N11 121.1(6) . . ?
C23 C18 N11 118.9(6) . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
O12 C24 H24A 109.5 . . ?
O12 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O12 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C32 C31 C36 120.3(8) . . ?
C32 C31 C37 117.1(8) . . ?
C36 C31 C37 122.7(8) . . ?
C33 C32 C31 121.2(8) . . ?
C33 C32 H32A 119.4 . . ?
C31 C32 H32A 119.4 . . ?
C32 C33 C34 118.5(8) . . ?
C32 C33 H33A 120.7 . . ?
C34 C33 H33A 120.7 . . ?
C35 C34 C33 121.5(8) . . ?
C35 C34 H34A 119.2 . . ?
C33 C34 H34A 119.2 . . ?
C34 C35 O32 124.8(7) . . ?
C34 C35 C36 121.6(7) . . ?
O32 C35 C36 113.5(6) . . ?
O31 C36 C35 119.2(7) . . ?
O31 C36 C31 124.0(8) . . ?
C35 C36 C31 116.8(7) . . ?
O33 C37 C31 127.6(8) . . ?
O33 C37 H37A 116.2 . . ?
C31 C37 H37A 116.2 . . ?
O32 C38 H38A 109.5 . . ?
O32 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O32 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O41 C41 H41A 109.5 . . ?
O41 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O41 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O53 C51 O51 122.4(6) 3_655 . ?
O53 C51 O52 121.5(5) 3_655 . ?
O51 C51 O52 116.1(5) . . ?
O53 C51 Dy1 177.2(4) 3_655 . ?
O51 C51 Dy1 60.0(3) . . ?
O52 C51 Dy1 56.2(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O61 N61 O63 -178.4(3) . . . . ?
Dy1 O61 N61 O62 1.6(3) . . . . ?
Dy1 O62 N61 O63 178.4(3) . . . . ?
Dy1 O62 N61 O61 -1.6(3) . . . . ?
C16 C11 C12 C13 -1.1(14) . . . . ?
C17 C11 C12 C13 178.9(9) . . . . ?
C11 C12 C13 C14 2.4(14) . . . . ?
C12 C13 C14 C15 -0.8(13) . . . . ?
C13 C14 C15 O12 178.2(7) . . . . ?
C13 C14 C15 C16 -2.0(12) . . . . ?
C24 O12 C15 C14 8.7(11) . . . . ?
Dy1 O12 C15 C14 -174.5(6) . . . . ?
C24 O12 C15 C16 -171.1(6) . . . . ?
Dy1 O12 C15 C16 5.7(8) . . . . ?
Ni2 O11 C16 C11 10.7(11) . . . . ?
Dy1 O11 C16 C11 167.7(6) . . . . ?
Ni2 O11 C16 C15 -169.5(5) . . . . ?
Dy1 O11 C16 C15 -12.6(10) . . . . ?
C12 C11 C16 O11 178.1(8) . . . . ?
C17 C11 C16 O11 -1.8(14) . . . . ?
C12 C11 C16 C15 -1.7(12) . . . . ?
C17 C11 C16 C15 178.4(8) . . . . ?
C14 C15 C16 O11 -176.5(7) . . . . ?
O12 C15 C16 O11 3.3(10) . . . . ?
C14 C15 C16 C11 3.3(12) . . . . ?
O12 C15 C16 C11 -176.9(7) . . . . ?
C18 N11 C17 C11 176.5(8) . . . . ?
Ni2 N11 C17 C11 0.8(13) . . . . ?
C16 C11 C17 N11 -4.4(15) . . . . ?
C12 C11 C17 N11 175.6(9) . . . . ?
C17 N11 C18 C19 117.0(8) . . . . ?
Ni2 N11 C18 C19 -66.9(7) . . . . ?
C17 N11 C18 C23 -62.4(9) . . . . ?
Ni2 N11 C18 C23 113.7(5) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
N11 C18 C19 C20 -179.4(7) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
N11 C18 C23 C22 179.4(7) . . . . ?
C36 C31 C32 C33 -1.0(13) . . . . ?
C37 C31 C32 C33 178.8(8) . . . . ?
C31 C32 C33 C34 0.2(13) . . . . ?
C32 C33 C34 C35 -1.0(12) . . . . ?
C33 C34 C35 O32 -177.0(7) . . . . ?
C33 C34 C35 C36 2.7(12) . . . . ?
C38 O32 C35 C34 -18.7(10) . . . . ?
Dy1 O32 C35 C34 171.6(6) . . . . ?
C38 O32 C35 C36 161.6(6) . . . . ?
Dy1 O32 C35 C36 -8.1(7) . . . . ?
Ni2 O31 C36 C35 152.9(5) . . . . ?
Dy1 O31 C36 C35 16.2(9) . . . . ?
Ni2 O31 C36 C31 -27.8(10) . . . . ?
Dy1 O31 C36 C31 -164.5(6) . . . . ?
C34 C35 C36 O31 176.0(7) . . . . ?
O32 C35 C36 O31 -4.3(9) . . . . ?
C34 C35 C36 C31 -3.4(11) . . . . ?
O32 C35 C36 C31 176.3(6) . . . . ?
C32 C31 C36 O31 -176.8(7) . . . . ?
C37 C31 C36 O31 3.4(12) . . . . ?
C32 C31 C36 C35 2.5(11) . . . . ?
C37 C31 C36 C35 -177.3(7) . . . . ?
Ni2 O33 C37 C31 0.6(14) . . . . ?
C32 C31 C37 O33 -168.1(9) . . . . ?
C36 C31 C37 O33 11.7(15) . . . . ?
Dy1 O51 C51 O53 -178.1(3) . . . 3_655 ?
Dy1 O51 C51 O52 1.9(3) . . . . ?
Dy1 O52 C51 O53 178.1(3) . . . 3_655 ?
Dy1 O52 C51 O53 14.6(6) 3_655 . . 3_655 ?
Dy1 O52 C51 O51 -1.9(3) . . . . ?
Dy1 O52 C51 O51 -165.4(6) 3_655 . . . ?
Dy1 O52 C51 Dy1 -163.5(7) 3_655 . . . ?

_refine_diff_density_max         2.271
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.170



