# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_2na
_database_code_depnum_ccdc_archive 'CCDC 2057598'
loop_
_audit_author_name
_audit_author_address
'Christian Nather'
;Institute of Inorganic Chemistry University of Kiel
Germany
;
_audit_update_record             
;
2021-03-26 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H116 N28 Na2 Nb2 Ni3 O22'
_chemical_formula_weight         1821.59

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.1568(7)
_cell_length_b                   15.3486(10)
_cell_length_c                   15.3374(9)
_cell_angle_alpha                60.695(5)
_cell_angle_beta                 84.540(5)
_cell_angle_gamma                84.295(6)
_cell_volume                     2071.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    21966
_cell_measurement_theta_min      1.524
_cell_measurement_theta_max      26.004

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.027
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7697
_exptl_absorpt_correction_T_max  0.9282
_exptl_absorpt_process_details   'X-red and X-Shape(STOE, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21966
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.524
_diffrn_reflns_theta_max         26.004
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8130
_reflns_number_gt                6730
_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       'X-Area (STOE, 2008)'
_computing_cell_refinement       'X-Area (STOE, 2008)'
_computing_data_reduction        'X-Area (STOE, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0782P)²+8.4289P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0048(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8130
_refine_ls_number_parameters     508
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.1792
_refine_ls_wR_factor_gt          0.1581
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.003
_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
Nb1 Nb 0.22111(7) 0.66510(6) 0.67489(6) 0.03399(19) Uani 1 1 d . . . . .
N1 N 0.3688(9) 0.4477(7) 0.6964(6) 0.048(2) Uani 1 1 d . . . . .
C1 C 0.3233(11) 0.5234(7) 0.6882(7) 0.042(2) Uani 1 1 d . . . . .
N2 N 0.4029(9) 0.8683(6) 0.6035(6) 0.0425(18) Uani 1 1 d . . . . .
C2 C 0.3426(11) 0.7987(6) 0.6306(7) 0.040(2) Uani 1 1 d . . . . .
N3 N 0.3707(10) 0.7224(6) 0.4449(7) 0.052(2) Uani 1 1 d . . . . .
C3 C 0.3240(12) 0.7008(7) 0.5240(7) 0.045(2) Uani 1 1 d . . . . .
N4 N 0.0135(6) 0.5735(7) 0.5832(7) 0.0428(15) Uani 1 1 d . . . . .
C4 C 0.0752(7) 0.6064(7) 0.6183(7) 0.0384(16) Uani 1 1 d . . . . .
N5 N 0.0599(9) 0.7693(5) 0.8110(6) 0.053(2) Uani 1 1 d . . . . .
C5 C 0.1109(9) 0.7345(6) 0.7639(6) 0.044(2) Uani 1 1 d . . . . .
N6 N 0.0583(9) 0.8705(6) 0.4957(6) 0.052(2) Uani 1 1 d . . . . .
C6 C 0.1096(11) 0.7996(8) 0.5621(7) 0.046(2) Uani 1 1 d . . . . .
N7 N 0.4330(9) 0.5889(6) 0.8561(6) 0.0420(19) Uani 1 1 d . . . . .
C7 C 0.3649(10) 0.6186(7) 0.7925(7) 0.037(2) Uani 1 1 d . . . . .
N8 N 0.0958(9) 0.4639(7) 0.8838(6) 0.053(2) Uani 1 1 d . . . . .
C8 C 0.1289(10) 0.5345(6) 0.8141(6) 0.037(2) Uani 1 1 d . . . . .
Ni1 Ni 0.500000 1.000000 0.500000 0.0389(4) Uani 1 2 d S . P . .
N11 N 0.5747(8) 1.0138(6) 0.6139(5) 0.0437(17) Uani 1 1 d . . . . .
H11 H 0.638019 1.068373 0.582106 0.052 Uiso 1 1 calc R U . . .
C11 C 0.4596(11) 1.0488(7) 0.6592(8) 0.054(2) Uani 1 1 d . . . . .
H11A H 0.491348 1.077756 0.698036 0.065 Uiso 1 1 calc R U . . .
H11B H 0.405789 0.991793 0.705144 0.065 Uiso 1 1 calc R U . . .
C12 C 0.3769(14) 1.1268(9) 0.5764(9) 0.059(3) Uani 1 1 d . . . . .
H12A H 0.297537 1.148629 0.605185 0.071 Uiso 1 1 calc R U . . .
H12B H 0.428835 1.185880 0.533303 0.071 Uiso 1 1 calc R U . . .
N12 N 0.3363(7) 1.0836(5) 0.5165(6) 0.0458(17) Uani 1 1 d . . . . .
H12 H 0.265931 1.036300 0.556920 0.055 Uiso 1 1 calc R U . . .
C13 C 0.2806(11) 1.1587(7) 0.4218(9) 0.055(3) Uani 1 1 d . . . . .
H13A H 0.346554 1.208935 0.381934 0.066 Uiso 1 1 calc R U . . .
H13B H 0.201297 1.193833 0.435939 0.066 Uiso 1 1 calc R U . . .
C14 C 0.2424(11) 1.1120(7) 0.3615(8) 0.063(3) Uani 1 1 d . . . . .
H14A H 0.184115 1.161551 0.308935 0.075 Uiso 1 1 calc R U . . .
H14B H 0.189177 1.054177 0.406473 0.075 Uiso 1 1 calc R U . . .
C15 C 0.3542(13) 1.0761(9) 0.3113(8) 0.056(3) Uani 1 1 d . . . . .
H15A H 0.317406 1.061009 0.262988 0.068 Uiso 1 1 calc R U . . .
H15B H 0.416512 1.129767 0.273809 0.068 Uiso 1 1 calc R U . . .
Ni2 Ni 0.000000 0.500000 0.500000 0.0367(3) Uani 1 2 d S . P . .
N21 N 0.1470(9) 0.3981(6) 0.5824(6) 0.0431(19) Uani 1 1 d . . . . .
H21 H 0.183057 0.423671 0.623466 0.052 Uiso 1 1 calc R U . . .
C21 C 0.0737(15) 0.3049(8) 0.6538(9) 0.062(3) Uani 1 1 d . . . . .
H21A H 0.055990 0.268292 0.618416 0.075 Uiso 1 1 calc R U . . .
H21B H 0.129328 0.259947 0.710537 0.075 Uiso 1 1 calc R U . . .
C22 C -0.0549(14) 0.3342(8) 0.6926(8) 0.059(3) Uani 1 1 d . . . . .
H22A H -0.104029 0.273858 0.737152 0.071 Uiso 1 1 calc R U . . .
H22B H -0.037365 0.367061 0.731696 0.071 Uiso 1 1 calc R U . . .
N22 N -0.1322(9) 0.4016(7) 0.6092(6) 0.047(2) Uani 1 1 d . . . . .
H22 H -0.164429 0.360995 0.581630 0.057 Uiso 1 1 calc R U . . .
C23 C -0.2502(15) 0.4476(10) 0.6377(9) 0.064(3) Uani 1 1 d . . . . .
H23A H -0.222856 0.481108 0.673640 0.077 Uiso 1 1 calc R U . . .
H23B H -0.309548 0.394598 0.684026 0.077 Uiso 1 1 calc R U . . .
C24 C -0.3256(9) 0.5235(10) 0.5474(9) 0.058(3) Uani 1 1 d . . . . .
H24A H -0.411653 0.542147 0.571904 0.070 Uiso 1 1 calc R U . . .
H24B H -0.344731 0.490476 0.508885 0.070 Uiso 1 1 calc R U . . .
C25 C -0.2578(10) 0.6192(8) 0.4761(8) 0.049(3) Uani 1 1 d . . . . .
H25A H -0.323186 0.668766 0.430148 0.059 Uiso 1 1 calc R U . . .
H25B H -0.225254 0.647731 0.515109 0.059 Uiso 1 1 calc R U . . .
Ni3 Ni 0.500000 0.500000 1.000000 0.0375(4) Uani 1 2 d S . P . .
N31 N 0.4471(9) 0.6177(7) 1.0298(6) 0.059(2) Uani 1 1 d . . . . .
H31 H 0.397103 0.669510 0.971476 0.071 Uiso 1 1 calc R U . . .
C31 C 0.5703(12) 0.6613(8) 1.0257(8) 0.057(3) Uani 1 1 d . . . . .
H31A H 0.615259 0.620163 1.089133 0.068 Uiso 1 1 calc R U . . .
H31B H 0.551092 0.729651 1.016680 0.068 Uiso 1 1 calc R U . . .
C32 C 0.6607(14) 0.6653(9) 0.9372(9) 0.061(3) Uani 1 1 d . . . . .
H32A H 0.617146 0.708095 0.873370 0.073 Uiso 1 1 calc R U . . .
H32B H 0.745481 0.693876 0.933772 0.073 Uiso 1 1 calc R U . . .
N32 N 0.6851(9) 0.5635(7) 0.9531(6) 0.056(2) Uani 1 1 d . . . . .
H32 H 0.744318 0.526531 1.010377 0.068 Uiso 1 1 calc R U . . .
C33 C 0.7543(12) 0.5603(9) 0.8643(8) 0.061(3) Uani 1 1 d . . . . .
H33A H 0.842963 0.587007 0.851928 0.073 Uiso 1 1 calc R U . . .
H33B H 0.702940 0.602652 0.804311 0.073 Uiso 1 1 calc R U . . .
C34 C 0.7686(12) 0.4533(10) 0.8827(10) 0.071(3) Uani 1 1 d . . . . .
H34A H 0.807784 0.410837 0.948440 0.085 Uiso 1 1 calc R U . . .
H34B H 0.832992 0.450868 0.831167 0.085 Uiso 1 1 calc R U . . .
C35 C 0.6398(13) 0.4047(10) 0.8822(8) 0.060(3) Uani 1 1 d . . . . .
H35A H 0.591678 0.451201 0.821606 0.073 Uiso 1 1 calc R U . . .
H35B H 0.665047 0.342269 0.879168 0.073 Uiso 1 1 calc R U . . .
Na1 Na 0.8404(4) 0.0728(3) 0.8675(3) 0.0578(10) Uani 1 1 d D . . . .
O1 O 1.0665(9) 0.0403(6) 0.8228(6) 0.068(2) Uani 1 1 d . . . . .
H1A H 1.081413 0.029077 0.770994 0.102 Uiso 1 1 d DR U . . .
H1B H 1.113580 -0.010120 0.867657 0.102 Uiso 1 1 d DR U . . .
O2 O 0.6361(10) 0.1426(8) 0.8805(7) 0.094(4) Uani 1 1 d . . . . .
H2A H 0.574369 0.096582 0.906076 0.141 Uiso 1 1 d R U . . .
H2B H 0.607284 0.186138 0.819252 0.141 Uiso 1 1 d R U . . .
O3 O 0.9017(9) 0.1242(7) 0.9831(7) 0.073(2) Uani 1 1 d D . . . .
H3A H 0.982(3) 0.134(11) 0.992(10) 0.109 Uiso 1 1 d D U . . .
H3B H 0.854(7) 0.166(9) 1.000(10) 0.109 Uiso 1 1 d D U . . .
O4 O 0.8095(9) 0.1271(7) 0.7006(6) 0.069(2) Uani 1 1 d D . . . .
H4A H 0.732(4) 0.129(12) 0.679(6) 0.104 Uiso 1 1 d D U . . .
H4B H 0.866(7) 0.110(10) 0.664(6) 0.104 Uiso 1 1 d D U . . .
O5 O 0.7571(9) -0.0903(5) 0.9632(5) 0.064(2) Uani 1 1 d D . . . .
H5A H 0.726(12) -0.103(6) 1.023(4) 0.097 Uiso 1 1 d D U . . .
H5B H 0.817(8) -0.138(5) 0.972(7) 0.097 Uiso 1 1 d D U . . .
O6 O 0.4867(7) 0.9247(7) 0.9222(7) 0.0652(17) Uani 1 1 d G . . . .
H6A H 0.438178 0.979351 0.908790 0.098 Uiso 1 1 d G U . . .
H6B H 0.433815 0.886035 0.917648 0.098 Uiso 1 1 d G U . . .
O7 O 0.3058(9) 0.1024(6) 0.8489(5) 0.062(2) Uani 1 1 d G . . . .
H7A H 0.340876 0.159151 0.809228 0.093 Uiso 1 1 d R U . . .
H7B H 0.244278 0.099556 0.814791 0.093 Uiso 1 1 d R U . . .
O8 O 0.0890(8) 0.9928(5) 0.6677(5) 0.0555(17) Uani 1 1 d G . . . .
H8A H 0.059180 0.933333 0.695705 0.083 Uiso 1 1 d G U . . .
H8B H 0.047763 1.026310 0.612383 0.083 Uiso 1 1 d G U . . .
O9 O 0.0606(8) 0.2513(5) 1.0031(5) 0.0573(18) Uani 1 1 d G . . . .
H9A H 0.034757 0.260665 1.053784 0.086 Uiso 1 1 d G U . . .
H9B H 0.069988 0.311335 0.953097 0.086 Uiso 1 1 d G U . . .
O10 O 0.2991(10) 0.8177(7) 0.8957(8) 0.083(3) Uani 1 1 d G . . . .
H10A H 0.219944 0.813652 0.881236 0.125 Uiso 1 1 d G U . . .
H10B H 0.350408 0.819104 0.846356 0.125 Uiso 1 1 d G U . . .
O11 O 0.4713(8) 0.2603(5) 0.7288(4) 0.0505(19) Uani 1 1 d G . . . .
H11C H 0.462972 0.271768 0.668098 0.076 Uiso 1 1 d G U . . .
H11D H 0.450468 0.317727 0.726444 0.076 Uiso 1 1 d G U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 C7 2.220(9) . ?
Nb1 C6 2.225(10) . ?
Nb1 C1 2.237(9) . ?
Nb1 C4 2.244(7) . ?
Nb1 C5 2.269(8) . ?
Nb1 C3 2.271(11) . ?
Nb1 C2 2.274(10) . ?
Nb1 C8 2.293(9) . ?
N1 C1 1.158(12) . ?
N2 C2 1.155(13) . ?
N2 Ni1 2.130(9) . ?
N3 C3 1.156(13) . ?
N4 C4 1.153(9) . ?
N4 Ni2 2.097(6) . ?
N5 C5 1.152(11) . ?
N6 C6 1.182(13) . ?
N7 C7 1.126(11) . ?
N7 Ni3 2.086(7) . ?
N8 C8 1.141(12) . ?
Ni1 N12 2.071(7) 2_676 ?
Ni1 N12 2.071(7) . ?
Ni1 N11 2.078(7) . ?
Ni1 N11 2.078(7) 2_676 ?
N11 C15 1.468(12) 2_676 ?
N11 C11 1.491(13) . ?
N11 H11 1.0000 . ?
C11 C12 1.505(16) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N12 1.476(13) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N12 C13 1.465(12) . ?
N12 H12 1.0000 . ?
C13 C14 1.515(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.520(17) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
Ni2 N21 2.057(8) 2_566 ?
Ni2 N21 2.057(8) . ?
Ni2 N22 2.095(10) 2_566 ?
Ni2 N22 2.095(10) . ?
N21 C25 1.458(13) 2_566 ?
N21 C21 1.524(15) . ?
N21 H21 1.0000 . ?
C21 C22 1.503(15) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N22 1.434(14) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
N22 C23 1.470(16) . ?
N22 H22 1.0000 . ?
C23 C24 1.519(17) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.520(17) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
Ni3 N31 2.082(9) . ?
Ni3 N31 2.082(9) 2_667 ?
Ni3 N32 2.103(9) 2_667 ?
Ni3 N32 2.103(9) . ?
N31 C35 1.448(15) 2_667 ?
N31 C31 1.458(15) . ?
N31 H31 1.0000 . ?
C31 C32 1.544(18) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 N32 1.457(14) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
N32 C33 1.493(14) . ?
N32 H32 1.0000 . ?
C33 C34 1.518(18) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.571(19) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
Na1 O2 2.276(10) . ?
Na1 O4 2.315(8) . ?
Na1 O5 2.394(9) . ?
Na1 O1 2.408(10) . ?
Na1 O3 2.414(9) . ?
O1 H1A 0.8892 . ?
O1 H1B 0.8767 . ?
O2 H2A 0.9037 . ?
O2 H2B 0.9023 . ?
O3 H3A 0.88(2) . ?
O3 H3B 0.89(2) . ?
O4 H4A 0.87(2) . ?
O4 H4B 0.87(2) . ?
O5 H5A 0.88(2) . ?
O5 H5B 0.87(2) . ?
O6 H6A 0.8701 . ?
O6 H6B 0.8701 . ?
O7 H7A 0.8700 . ?
O7 H7B 0.8699 . ?
O8 H8A 0.8700 . ?
O8 H8B 0.8701 . ?
O9 H9A 0.8701 . ?
O9 H9B 0.8702 . ?
O10 H10A 0.8700 . ?
O10 H10B 0.8700 . ?
O11 H11C 0.8703 . ?
O11 H11D 0.8698 . ?

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
C7 Nb1 C6 141.7(3) . . ?
C7 Nb1 C1 75.3(3) . . ?
C6 Nb1 C1 138.1(3) . . ?
C7 Nb1 C4 143.0(3) . . ?
C6 Nb1 C4 74.4(3) . . ?
C1 Nb1 C4 76.3(3) . . ?
C7 Nb1 C5 81.3(3) . . ?
C6 Nb1 C5 75.4(3) . . ?
C1 Nb1 C5 143.5(3) . . ?
C4 Nb1 C5 109.5(3) . . ?
C7 Nb1 C3 111.9(4) . . ?
C6 Nb1 C3 74.2(4) . . ?
C1 Nb1 C3 72.1(3) . . ?
C4 Nb1 C3 80.8(4) . . ?
C5 Nb1 C3 143.7(3) . . ?
C7 Nb1 C2 72.9(3) . . ?
C6 Nb1 C2 73.0(4) . . ?
C1 Nb1 C2 119.3(4) . . ?
C4 Nb1 C2 143.0(3) . . ?
C5 Nb1 C2 78.5(4) . . ?
C3 Nb1 C2 74.0(4) . . ?
C7 Nb1 C8 75.1(3) . . ?
C6 Nb1 C8 125.5(3) . . ?
C1 Nb1 C8 72.6(4) . . ?
C4 Nb1 C8 74.1(3) . . ?
C5 Nb1 C8 74.7(3) . . ?
C3 Nb1 C8 140.5(3) . . ?
C2 Nb1 C8 140.7(3) . . ?
N1 C1 Nb1 175.9(10) . . ?
C2 N2 Ni1 157.7(7) . . ?
N2 C2 Nb1 176.8(8) . . ?
N3 C3 Nb1 176.4(9) . . ?
C4 N4 Ni2 151.0(6) . . ?
N4 C4 Nb1 171.6(7) . . ?
N5 C5 Nb1 177.1(8) . . ?
N6 C6 Nb1 174.0(9) . . ?
C7 N7 Ni3 158.5(8) . . ?
N7 C7 Nb1 175.0(9) . . ?
N8 C8 Nb1 172.6(8) . . ?
N12 Ni1 N12 180.0(3) 2_676 . ?
N12 Ni1 N11 95.1(3) 2_676 . ?
N12 Ni1 N11 84.9(3) . . ?
N12 Ni1 N11 84.9(3) 2_676 2_676 ?
N12 Ni1 N11 95.1(3) . 2_676 ?
N11 Ni1 N11 180.0 . 2_676 ?
N12 Ni1 N2 91.7(3) 2_676 . ?
N12 Ni1 N2 88.3(3) . . ?
N11 Ni1 N2 92.5(3) . . ?
N11 Ni1 N2 87.5(3) 2_676 . ?
N12 Ni1 N2 88.3(3) 2_676 2_676 ?
N12 Ni1 N2 91.7(3) . 2_676 ?
N11 Ni1 N2 87.5(3) . 2_676 ?
N11 Ni1 N2 92.5(3) 2_676 2_676 ?
N2 Ni1 N2 180.0(4) . 2_676 ?
C15 N11 C11 112.5(8) 2_676 . ?
C15 N11 Ni1 115.5(6) 2_676 . ?
C11 N11 Ni1 105.8(6) . . ?
C15 N11 H11 107.6 2_676 . ?
C11 N11 H11 107.6 . . ?
Ni1 N11 H11 107.6 . . ?
N11 C11 C12 108.7(8) . . ?
N11 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
N11 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
N12 C12 C11 109.0(8) . . ?
N12 C12 H12A 109.9 . . ?
C11 C12 H12A 109.9 . . ?
N12 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C13 N12 C12 113.2(8) . . ?
C13 N12 Ni1 114.1(7) . . ?
C12 N12 Ni1 106.4(7) . . ?
C13 N12 H12 107.6 . . ?
C12 N12 H12 107.6 . . ?
Ni1 N12 H12 107.6 . . ?
N12 C13 C14 111.7(8) . . ?
N12 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
N12 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 C15 117.3(9) . . ?
C13 C14 H14A 108.0 . . ?
C15 C14 H14A 108.0 . . ?
C13 C14 H14B 108.0 . . ?
C15 C14 H14B 108.0 . . ?
H14A C14 H14B 107.2 . . ?
N11 C15 C14 110.6(9) 2_676 . ?
N11 C15 H15A 109.5 2_676 . ?
C14 C15 H15A 109.5 . . ?
N11 C15 H15B 109.5 2_676 . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
N21 Ni2 N21 180.0 2_566 . ?
N21 Ni2 N4 88.4(3) 2_566 2_566 ?
N21 Ni2 N4 91.5(3) . 2_566 ?
N21 Ni2 N4 91.6(3) 2_566 . ?
N21 Ni2 N4 88.5(3) . . ?
N4 Ni2 N4 180.0 2_566 . ?
N21 Ni2 N22 85.7(3) 2_566 2_566 ?
N21 Ni2 N22 94.3(3) . 2_566 ?
N4 Ni2 N22 91.0(4) 2_566 2_566 ?
N4 Ni2 N22 89.0(4) . 2_566 ?
N21 Ni2 N22 94.2(3) 2_566 . ?
N21 Ni2 N22 85.8(3) . . ?
N4 Ni2 N22 89.0(4) 2_566 . ?
N4 Ni2 N22 91.0(4) . . ?
N22 Ni2 N22 180.0(4) 2_566 . ?
C25 N21 C21 114.3(9) 2_566 . ?
C25 N21 Ni2 115.2(6) 2_566 . ?
C21 N21 Ni2 104.0(7) . . ?
C25 N21 H21 107.7 2_566 . ?
C21 N21 H21 107.6 . . ?
Ni2 N21 H21 107.7 . . ?
C22 C21 N21 109.9(9) . . ?
C22 C21 H21A 109.7 . . ?
N21 C21 H21A 109.7 . . ?
C22 C21 H21B 109.7 . . ?
N21 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
N22 C22 C21 108.8(10) . . ?
N22 C22 H22A 109.9 . . ?
C21 C22 H22A 109.9 . . ?
N22 C22 H22B 109.9 . . ?
C21 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C22 N22 C23 113.1(10) . . ?
C22 N22 Ni2 106.2(8) . . ?
C23 N22 Ni2 116.4(7) . . ?
C22 N22 H22 106.9 . . ?
C23 N22 H22 106.9 . . ?
Ni2 N22 H22 106.9 . . ?
N22 C23 C24 112.1(9) . . ?
N22 C23 H23A 109.2 . . ?
C24 C23 H23A 109.2 . . ?
N22 C23 H23B 109.2 . . ?
C24 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 C25 116.7(8) . . ?
C23 C24 H24A 108.1 . . ?
C25 C24 H24A 108.1 . . ?
C23 C24 H24B 108.1 . . ?
C25 C24 H24B 108.1 . . ?
H24A C24 H24B 107.3 . . ?
N21 C25 C24 112.1(8) 2_566 . ?
N21 C25 H25A 109.2 2_566 . ?
C24 C25 H25A 109.2 . . ?
N21 C25 H25B 109.2 2_566 . ?
C24 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
N31 Ni3 N31 180.0 . 2_667 ?
N31 Ni3 N7 89.2(3) . . ?
N31 Ni3 N7 90.8(3) 2_667 . ?
N31 Ni3 N7 90.8(3) . 2_667 ?
N31 Ni3 N7 89.2(3) 2_667 2_667 ?
N7 Ni3 N7 180.0 . 2_667 ?
N31 Ni3 N32 95.4(4) . 2_667 ?
N31 Ni3 N32 84.6(4) 2_667 2_667 ?
N7 Ni3 N32 89.3(3) . 2_667 ?
N7 Ni3 N32 90.7(3) 2_667 2_667 ?
N31 Ni3 N32 84.6(4) . . ?
N31 Ni3 N32 95.4(4) 2_667 . ?
N7 Ni3 N32 90.7(3) . . ?
N7 Ni3 N32 89.3(3) 2_667 . ?
N32 Ni3 N32 180.0 2_667 . ?
C35 N31 C31 115.4(9) 2_667 . ?
C35 N31 Ni3 116.3(8) 2_667 . ?
C31 N31 Ni3 106.2(6) . . ?
C35 N31 H31 106.0 2_667 . ?
C31 N31 H31 106.0 . . ?
Ni3 N31 H31 106.0 . . ?
N31 C31 C32 109.0(9) . . ?
N31 C31 H31A 109.9 . . ?
C32 C31 H31A 109.9 . . ?
N31 C31 H31B 109.9 . . ?
C32 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
N32 C32 C31 107.9(10) . . ?
N32 C32 H32A 110.1 . . ?
C31 C32 H32A 110.1 . . ?
N32 C32 H32B 110.1 . . ?
C31 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
C32 N32 C33 112.4(9) . . ?
C32 N32 Ni3 105.3(7) . . ?
C33 N32 Ni3 116.2(8) . . ?
C32 N32 H32 107.5 . . ?
C33 N32 H32 107.5 . . ?
Ni3 N32 H32 107.5 . . ?
N32 C33 C34 109.9(10) . . ?
N32 C33 H33A 109.7 . . ?
C34 C33 H33A 109.7 . . ?
N32 C33 H33B 109.7 . . ?
C34 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
C33 C34 C35 117.5(10) . . ?
C33 C34 H34A 107.9 . . ?
C35 C34 H34A 107.9 . . ?
C33 C34 H34B 107.9 . . ?
C35 C34 H34B 107.9 . . ?
H34A C34 H34B 107.2 . . ?
N31 C35 C34 112.0(9) 2_667 . ?
N31 C35 H35A 109.2 2_667 . ?
C34 C35 H35A 109.2 . . ?
N31 C35 H35B 109.2 2_667 . ?
C34 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
O2 Na1 O4 89.3(3) . . ?
O2 Na1 O5 89.9(4) . . ?
O4 Na1 O5 107.6(3) . . ?
O2 Na1 O1 166.0(4) . . ?
O4 Na1 O1 83.5(3) . . ?
O5 Na1 O1 103.7(3) . . ?
O2 Na1 O3 85.0(4) . . ?
O4 Na1 O3 144.0(4) . . ?
O5 Na1 O3 108.0(3) . . ?
O1 Na1 O3 93.8(3) . . ?
Na1 O1 H1A 117.9 . . ?
Na1 O1 H1B 119.0 . . ?
H1A O1 H1B 100.6 . . ?
Na1 O2 H2A 111.3 . . ?
Na1 O2 H2B 110.5 . . ?
H2A O2 H2B 102.7 . . ?
Na1 O3 H3A 126(4) . . ?
Na1 O3 H3B 126(4) . . ?
H3A O3 H3B 101(5) . . ?
Na1 O4 H4A 122(5) . . ?
Na1 O4 H4B 122(5) . . ?
H4A O4 H4B 104(5) . . ?
Na1 O5 H5A 113(6) . . ?
Na1 O5 H5B 113(6) . . ?
H5A O5 H5B 106(5) . . ?
H6A O6 H6B 104.5 . . ?
H7A O7 H7B 104.5 . . ?
H8A O8 H8B 104.5 . . ?
H9A O9 H9B 104.4 . . ?
H10A O10 H10B 104.5 . . ?
H11C O11 H11D 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 N11 C11 C12 -168.3(9) 2_676 . . . ?
Ni1 N11 C11 C12 -41.3(9) . . . . ?
N11 C11 C12 N12 56.8(11) . . . . ?
C11 C12 N12 C13 -167.4(9) . . . . ?
C11 C12 N12 Ni1 -41.3(10) . . . . ?
C12 N12 C13 C14 179.0(9) . . . . ?
Ni1 N12 C13 C14 57.0(10) . . . . ?
N12 C13 C14 C15 -73.1(12) . . . . ?
C13 C14 C15 N11 71.4(12) . . . 2_676 ?
C25 N21 C21 C22 -167.3(8) 2_566 . . . ?
Ni2 N21 C21 C22 -40.8(9) . . . . ?
N21 C21 C22 N22 57.6(10) . . . . ?
C21 C22 N22 C23 -170.6(9) . . . . ?
C21 C22 N22 Ni2 -41.7(9) . . . . ?
C22 N22 C23 C24 176.4(10) . . . . ?
Ni2 N22 C23 C24 52.9(12) . . . . ?
N22 C23 C24 C25 -68.4(12) . . . . ?
C23 C24 C25 N21 72.0(11) . . . 2_566 ?
C35 N31 C31 C32 171.2(8) 2_667 . . . ?
Ni3 N31 C31 C32 40.7(9) . . . . ?
N31 C31 C32 N32 -59.0(11) . . . . ?
C31 C32 N32 C33 171.2(9) . . . . ?
C31 C32 N32 Ni3 43.7(10) . . . . ?
C32 N32 C33 C34 -176.2(10) . . . . ?
Ni3 N32 C33 C34 -54.8(10) . . . . ?
N32 C33 C34 C35 71.5(13) . . . . ?
C33 C34 C35 N31 -72.0(13) . . . 2_667 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N12 H12 O8 1.00 2.26 3.170(11) 150.7 .
C13 H13A N2 0.99 2.68 3.211(14) 114.0 2_676
N21 H21 N1 1.00 2.43 3.333(12) 150.3 .
C25 H25B N4 0.99 2.65 3.183(12) 113.7 .
N31 H31 O10 1.00 2.17 3.066(12) 148.7 .
C31 H31B O6 0.99 2.65 3.588(14) 157.8 .
C32 H32B O9 0.99 2.65 3.584(17) 157.8 2_667
N32 H32 N8 1.00 2.47 3.351(12) 147.4 2_667
O1 H1A O8 0.89 1.91 2.794(11) 170.8 1_645
O1 H1B O3 0.88 2.10 2.829(12) 140.6 2_757
O2 H2B O11 0.90 1.91 2.739(10) 152.7 .
O3 H3A O9 0.88(2) 2.13(8) 2.795(12) 132(8) 1_655
O3 H3B O10 0.89(2) 2.21(9) 2.992(15) 146(14) 2_667
O4 H4A N3 0.87(2) 2.37(13) 2.925(12) 122(12) 2_666
O4 H4B N6 0.87(2) 2.38(5) 3.163(12) 149(8) 2_666
O5 H5A O7 0.88(2) 1.96(4) 2.810(11) 163(11) 2_657
O5 H5B O9 0.87(2) 1.93(2) 2.797(10) 176(8) 2_657
O7 H7A O11 0.87 1.98 2.817(11) 162.1 .
O7 H7B O1 0.87 2.07 2.828(12) 145.4 1_455

_refine_diff_density_max         2.088
_refine_diff_density_min         -2.374
_refine_diff_density_rms         0.141



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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2057600'
loop_
_audit_author_name
_audit_author_address
'Christian Nather'
;Institute of Inorganic Chemistry University of Kiel
Germany
;
_audit_update_record             
;
2021-01-20 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H122 Ca N28 Nb2 Ni3 O25'
_chemical_formula_weight         1869.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ca Ca 0.2262 0.3064 '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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

_cell_length_a                   26.199(5)
_cell_length_b                   15.628(3)
_cell_length_c                   10.235(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.39(3)
_cell_angle_gamma                90
_cell_volume                     4172.0(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    21074
_cell_measurement_theta_min      1.519
_cell_measurement_theta_max      25.001

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_F_000             1960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.075
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'IPDS-2 from STOE'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21074
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.519
_diffrn_reflns_theta_max         25.001
_diffrn_reflns_theta_full        25.001
_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             3821
_reflns_number_gt                3402
_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       'X-AREA (STOE, 2008)'
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0779P)²+14.5174P] 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         3821
_refine_ls_number_parameters     302
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1339
_refine_ls_wR_factor_gt          0.1291
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.003
_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
Nb1 Nb 0.32806(2) 0.500000 0.72005(4) 0.02720(16) Uani 1 2 d S T P . .
Ni2 Ni 0.250000 0.750000 1.000000 0.0325(2) Uani 1 2 d S . P . .
Ni1 Ni 0.500000 0.500000 0.500000 0.0328(3) Uani 1 4 d S T P . .
C1 C 0.28529(15) 0.5852(2) 0.8484(4) 0.0322(8) Uani 1 1 d . . . . .
N1 N 0.26548(14) 0.6331(2) 0.9116(3) 0.0393(8) Uani 1 1 d . . . . .
C2 C 0.3872(2) 0.500000 0.5780(5) 0.0336(12) Uani 1 2 d S T P . .
N2 N 0.4215(2) 0.500000 0.5157(5) 0.0398(11) Uani 1 2 d S T P . .
C3 C 0.38895(16) 0.5853(3) 0.8212(4) 0.0384(9) Uani 1 1 d . . . . .
N3 N 0.42037(16) 0.6304(3) 0.8670(4) 0.0532(10) Uani 1 1 d . . . . .
C4 C 0.32218(17) 0.3720(3) 0.6173(4) 0.0402(10) Uani 1 1 d . . . . .
N4 N 0.3224(2) 0.3056(3) 0.5701(4) 0.0626(12) Uani 1 1 d . . . . .
C5 C 0.2502(2) 0.500000 0.6053(6) 0.0413(14) Uani 1 2 d S T P . .
N5 N 0.2104(2) 0.500000 0.5497(6) 0.0551(15) Uani 1 2 d S T P . .
N21 N 0.18993(18) 0.6991(3) 1.0925(5) 0.0594(12) Uani 1 1 d . . . . .
H21 H 0.179080 0.743607 1.154469 0.071 Uiso 1 1 calc R U . . .
C21 C 0.1477(2) 0.6882(4) 0.9896(8) 0.083(2) Uani 1 1 d . . . . .
H21A H 0.114883 0.682721 1.029650 0.100 Uiso 1 1 calc R U . . .
H21B H 0.152980 0.635387 0.939151 0.100 Uiso 1 1 calc R U . . .
C22 C 0.1457(2) 0.7648(5) 0.8994(7) 0.083(2) Uani 1 1 d . . . . .
H22A H 0.118651 0.756167 0.826277 0.099 Uiso 1 1 calc R U . . .
H22B H 0.137006 0.816626 0.948274 0.099 Uiso 1 1 calc R U . . .
N22 N 0.19557(18) 0.7769(3) 0.8463(4) 0.0587(12) Uani 1 1 d . . . . .
H22 H 0.198429 0.731161 0.779001 0.070 Uiso 1 1 calc R U . . .
C23 C 0.2010(3) 0.8584(4) 0.7802(6) 0.087(2) Uani 1 1 d . . . . .
H23A H 0.196395 0.905622 0.842592 0.104 Uiso 1 1 calc R U . . .
H23B H 0.173771 0.863558 0.706677 0.104 Uiso 1 1 calc R U . . .
C24 C 0.2518(4) 0.8668(4) 0.7289(7) 0.092(3) Uani 1 1 d . . . . .
H24A H 0.250501 0.916000 0.667812 0.111 Uiso 1 1 calc R U . . .
H24B H 0.257921 0.814806 0.677222 0.111 Uiso 1 1 calc R U . . .
C25 C 0.2973(3) 0.8790(4) 0.8298(9) 0.096(3) Uani 1 1 d . . . . .
H25A H 0.327507 0.896131 0.784507 0.116 Uiso 1 1 calc R U . . .
H25B H 0.289766 0.925939 0.889950 0.116 Uiso 1 1 calc R U . . .
C11 C 0.5174(2) 0.6749(4) 0.5622(7) 0.0746(18) Uani 1 1 d . . . . .
H11A H 0.553616 0.675640 0.541733 0.090 Uiso 1 1 calc R U . . .
H11B H 0.511180 0.726525 0.614349 0.090 Uiso 1 1 calc R U . . .
N11 N 0.50755(16) 0.5975(3) 0.6377(4) 0.0525(10) Uani 1 1 d . . . . .
H11 H 0.473497 0.605005 0.672975 0.063 Uiso 1 1 calc R U . . .
C12 C 0.5459(2) 0.5811(5) 0.7511(5) 0.0726(19) Uani 1 1 d . . . . .
H12A H 0.545931 0.629874 0.812730 0.087 Uiso 1 1 calc R U . . .
H12B H 0.580407 0.577699 0.719282 0.087 Uiso 1 1 calc R U . . .
C13 C 0.5359(3) 0.500000 0.8235(7) 0.081(3) Uani 1 2 d S T P . .
H13A H 0.557635 0.500000 0.908046 0.098 Uiso 1 2 calc R U P . .
H13B H 0.499680 0.500001 0.843734 0.098 Uiso 1 2 calc R U P . .
Ca1 Ca 0.4653(2) 0.0813(3) 0.6314(5) 0.0673(12) Uani 0.25 1 d . . P A 1
O1 O 0.3871(3) 0.000000 0.6185(9) 0.136(4) Uani 1 2 d S T P A 1
O2 O 0.4131(4) 0.2045(8) 0.6784(14) 0.089(3) Uani 0.5 1 d . . P A 1
O3 O 0.4327(13) 0.110(2) 0.405(2) 0.139(13) Uani 0.25 1 d . . P A 1
O4 O 0.5214(5) 0.1441(8) 0.8045(13) 0.073(4) Uani 0.4 1 d . . P A 1
O4' O 0.4956(5) 0.1546(7) 0.8233(14) 0.073(3) Uani 0.4 1 d . . P A 1
O5 O 0.4783(10) -0.0746(16) 0.533(2) 0.115(9) Uani 0.25 1 d . . P A 1
O6 O 0.4498(3) 0.000000 0.8520(9) 0.113(3) Uani 1 2 d S T P A 1
O7 O 0.3315(2) 0.1685(3) 0.3950(4) 0.0820(13) Uani 1 1 d . . . B 1
O8 O 0.500000 0.2713(3) 1.000000 0.0566(12) Uani 1 2 d S T P C 1
O9 O 0.4208(13) 0.000000 1.027(3) 0.078(8) Uiso 0.2 2 d S . P D 1
O10 O 0.4100(6) 0.000000 1.1163(17) 0.053(4) Uiso 0.3 2 d S . P E 2
O11 O 0.3815(4) 0.0529(6) 0.4593(9) 0.078(2) Uani 0.5 1 d . . P F 2
O12 O 0.4063(12) 0.1721(17) 0.644(3) 0.088(9) Uiso 0.25 1 d . . P G 2
O13 O 0.5238(8) 0.1066(14) 0.909(2) 0.072(5) Uiso 0.2 1 d . . P H 2
O14 O 0.4239(4) 0.1024(7) 0.3165(12) 0.087(3) Uiso 0.5 1 d . . P I 2
O15 O 0.4549(8) 0.0930(14) 0.433(3) 0.071(5) Uiso 0.25 1 d . . P I 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
Nb1 C2 2.222(6) . ?
Nb1 C1 2.243(4) 6_565 ?
Nb1 C1 2.243(4) . ?
Nb1 C3 2.255(4) . ?
Nb1 C3 2.255(4) 6_565 ?
Nb1 C5 2.257(6) . ?
Nb1 C4 2.258(4) 6_565 ?
Nb1 C4 2.259(4) . ?
Ni2 N22 2.065(4) . ?
Ni2 N22 2.065(4) 7_567 ?
Ni2 N21 2.070(4) 7_567 ?
Ni2 N21 2.070(4) . ?
Ni2 N1 2.096(3) . ?
Ni2 N1 2.096(3) 7_567 ?
Ni1 N11 2.073(4) . ?
Ni1 N11 2.073(4) 5_666 ?
Ni1 N11 2.073(4) 6_565 ?
Ni1 N11 2.073(4) 2_656 ?
Ni1 N2 2.078(5) . ?
Ni1 N2 2.078(5) 5_666 ?
C1 N1 1.144(5) . ?
C2 N2 1.150(7) . ?
C3 N3 1.149(6) . ?
C4 N4 1.145(6) . ?
C5 N5 1.138(8) . ?
N21 C21 1.464(9) . ?
N21 C25 1.477(8) 7_567 ?
C21 C22 1.511(11) . ?
C22 N22 1.474(8) . ?
N22 C23 1.456(8) . ?
C23 C24 1.484(11) . ?
C24 C25 1.514(12) . ?
C11 N11 1.471(8) . ?
C11 C11 1.495(14) 2_656 ?
N11 C12 1.484(7) . ?
C12 C13 1.503(8) . ?
Ca1 O5 1.098(18) 6 ?
Ca1 O5 2.34(2) 5_656 ?
Ca1 O4' 2.347(16) . ?
Ca1 O4 2.404(13) . ?
Ca1 O1 2.403(9) . ?
Ca1 O3 2.44(2) . ?
Ca1 O2 2.435(13) . ?
Ca1 Ca1 2.540(10) 6 ?
Ca1 O6 2.655(10) . ?
Ca1 O5 2.67(3) . ?
Ca1 O3 2.77(4) 2_656 ?
Ca1 Ca1 3.385(11) 2_656 ?
O3 O5 1.78(4) 6 ?
O4 O4' 0.740(12) . ?
O5 O5 1.38(4) 2_656 ?
O11 O11 1.654(17) 6 ?
O14 O15 1.38(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Nb1 C1 143.19(10) . 6_565 ?
C2 Nb1 C1 143.19(10) . . ?
C1 Nb1 C1 72.8(2) 6_565 . ?
C2 Nb1 C3 78.09(16) . . ?
C1 Nb1 C3 116.93(15) 6_565 . ?
C1 Nb1 C3 75.56(15) . . ?
C2 Nb1 C3 78.09(16) . 6_565 ?
C1 Nb1 C3 75.56(15) 6_565 6_565 ?
C1 Nb1 C3 116.92(15) . 6_565 ?
C3 Nb1 C3 72.5(2) . 6_565 ?
C2 Nb1 C5 108.2(2) . . ?
C1 Nb1 C5 80.08(17) 6_565 . ?
C1 Nb1 C5 80.08(17) . . ?
C3 Nb1 C5 143.61(11) . . ?
C3 Nb1 C5 143.61(11) 6_565 . ?
C2 Nb1 C4 73.53(12) . 6_565 ?
C1 Nb1 C4 141.50(15) 6_565 6_565 ?
C1 Nb1 C4 74.40(14) . 6_565 ?
C3 Nb1 C4 72.81(17) . 6_565 ?
C3 Nb1 C4 138.77(16) 6_565 6_565 ?
C5 Nb1 C4 74.86(14) . 6_565 ?
C2 Nb1 C4 73.54(12) . . ?
C1 Nb1 C4 74.40(14) 6_565 . ?
C1 Nb1 C4 141.50(15) . . ?
C3 Nb1 C4 138.77(16) . . ?
C3 Nb1 C4 72.82(17) 6_565 . ?
C5 Nb1 C4 74.86(14) . . ?
C4 Nb1 C4 124.7(2) 6_565 . ?
N22 Ni2 N22 180.0 . 7_567 ?
N22 Ni2 N21 94.2(2) . 7_567 ?
N22 Ni2 N21 85.8(2) 7_567 7_567 ?
N22 Ni2 N21 85.8(2) . . ?
N22 Ni2 N21 94.2(2) 7_567 . ?
N21 Ni2 N21 180.0 7_567 . ?
N22 Ni2 N1 89.77(15) . . ?
N22 Ni2 N1 90.23(15) 7_567 . ?
N21 Ni2 N1 87.20(15) 7_567 . ?
N21 Ni2 N1 92.81(15) . . ?
N22 Ni2 N1 90.23(15) . 7_567 ?
N22 Ni2 N1 89.77(15) 7_567 7_567 ?
N21 Ni2 N1 92.80(15) 7_567 7_567 ?
N21 Ni2 N1 87.19(15) . 7_567 ?
N1 Ni2 N1 180.0 . 7_567 ?
N11 Ni1 N11 180.0 . 5_666 ?
N11 Ni1 N11 94.6(3) . 6_565 ?
N11 Ni1 N11 85.4(3) 5_666 6_565 ?
N11 Ni1 N11 85.4(3) . 2_656 ?
N11 Ni1 N11 94.6(3) 5_666 2_656 ?
N11 Ni1 N11 180.0 6_565 2_656 ?
N11 Ni1 N2 88.82(15) . . ?
N11 Ni1 N2 91.18(15) 5_666 . ?
N11 Ni1 N2 88.82(15) 6_565 . ?
N11 Ni1 N2 91.18(15) 2_656 . ?
N11 Ni1 N2 91.18(15) . 5_666 ?
N11 Ni1 N2 88.82(15) 5_666 5_666 ?
N11 Ni1 N2 91.18(15) 6_565 5_666 ?
N11 Ni1 N2 88.82(15) 2_656 5_666 ?
N2 Ni1 N2 180.0 . 5_666 ?
N1 C1 Nb1 175.4(3) . . ?
C1 N1 Ni2 158.5(3) . . ?
N2 C2 Nb1 172.9(5) . . ?
C2 N2 Ni1 150.9(5) . . ?
N3 C3 Nb1 176.7(4) . . ?
N4 C4 Nb1 175.2(5) . . ?
N5 C5 Nb1 178.7(6) . . ?
C21 N21 C25 114.1(6) . 7_567 ?
C21 N21 Ni2 105.8(4) . . ?
C25 N21 Ni2 114.9(4) 7_567 . ?
N21 C21 C22 109.1(5) . . ?
N22 C22 C21 110.2(5) . . ?
C23 N22 C22 114.3(5) . . ?
C23 N22 Ni2 116.2(4) . . ?
C22 N22 Ni2 105.4(4) . . ?
N22 C23 C24 111.8(5) . . ?
C23 C24 C25 116.4(6) . . ?
N21 C25 C24 112.7(5) 7_567 . ?
N11 C11 C11 108.9(4) . 2_656 ?
C11 N11 C12 114.4(5) . . ?
C11 N11 Ni1 104.9(3) . . ?
C12 N11 Ni1 114.8(4) . . ?
N11 C12 C13 113.2(5) . . ?
C12 C13 C12 114.8(6) 6_565 . ?
O5 Ca1 O5 21(2) 6 5_656 ?
O5 Ca1 O4' 134.8(14) 6 . ?
O5 Ca1 O4' 115.9(9) 5_656 . ?
O5 Ca1 O4 119.6(15) 6 . ?
O5 Ca1 O4 99.5(9) 5_656 . ?
O4' Ca1 O4 17.9(3) . . ?
O5 Ca1 O1 103.6(13) 6 . ?
O5 Ca1 O1 121.9(8) 5_656 . ?
O4' Ca1 O1 121.6(4) . . ?
O4 Ca1 O1 135.7(5) . . ?
O5 Ca1 O3 42.0(17) 6 . ?
O5 Ca1 O3 60.9(12) 5_656 . ?
O4' Ca1 O3 140.0(9) . . ?
O4 Ca1 O3 139.6(9) . . ?
O1 Ca1 O3 79.9(8) . . ?
O5 Ca1 O2 119.0(16) 6 . ?
O5 Ca1 O2 125.5(7) 5_656 . ?
O4' Ca1 O2 66.4(5) . . ?
O4 Ca1 O2 81.2(5) . . ?
O1 Ca1 O2 86.4(4) . . ?
O3 Ca1 O2 83.6(9) . . ?
O5 Ca1 Ca1 84.5(14) 6 6 ?
O5 Ca1 Ca1 87.4(6) 5_656 6 ?
O4' Ca1 Ca1 119.2(3) . 6 ?
O4 Ca1 Ca1 114.1(3) . 6 ?
O1 Ca1 Ca1 58.10(17) . 6 ?
O3 Ca1 Ca1 100.7(8) . 6 ?
O2 Ca1 Ca1 142.3(3) . 6 ?
O5 Ca1 O6 145.0(15) 6 . ?
O5 Ca1 O6 138.2(6) 5_656 . ?
O4' Ca1 O6 65.7(3) . . ?
O4 Ca1 O6 72.5(4) . . ?
O1 Ca1 O6 66.2(3) . . ?
O3 Ca1 O6 146.1(8) . . ?
O2 Ca1 O6 94.4(4) . . ?
Ca1 Ca1 O6 61.42(15) 6 . ?
O5 Ca1 O5 60.3(15) 6 . ?
O5 Ca1 O5 65.0(9) 5_656 . ?
O4' Ca1 O5 135.7(7) . . ?
O4 Ca1 O5 124.0(7) . . ?
O1 Ca1 O5 68.6(6) . . ?
O3 Ca1 O5 81.7(9) . . ?
O2 Ca1 O5 152.9(8) . . ?
Ca1 Ca1 O5 24.2(4) 6 . ?
O6 Ca1 O5 85.4(4) . . ?
O5 Ca1 O3 60.4(15) 6 2_656 ?
O5 Ca1 O3 39.6(8) 5_656 2_656 ?
O4' Ca1 O3 77.2(5) . 2_656 ?
O4 Ca1 O3 60.1(5) . 2_656 ?
O1 Ca1 O3 155.1(6) . 2_656 ?
O3 Ca1 O3 95.7(11) . 2_656 ?
O2 Ca1 O3 117.6(7) . 2_656 ?
Ca1 Ca1 O3 99.4(7) 6 2_656 ?
O6 Ca1 O3 114.7(7) . 2_656 ?
O5 Ca1 O3 86.5(8) . 2_656 ?
O5 Ca1 Ca1 15.2(14) 6 2_656 ?
O5 Ca1 Ca1 7.1(6) 5_656 2_656 ?
O4' Ca1 Ca1 120.0(4) . 2_656 ?
O4 Ca1 Ca1 104.4(4) . 2_656 ?
O1 Ca1 Ca1 118.4(3) . 2_656 ?
O3 Ca1 Ca1 53.9(8) . 2_656 ?
O2 Ca1 Ca1 120.7(3) . 2_656 ?
Ca1 Ca1 Ca1 90.0 6 2_656 ?
O6 Ca1 Ca1 144.3(2) . 2_656 ?
O5 Ca1 Ca1 66.6(4) . 2_656 ?
O3 Ca1 Ca1 45.3(4) 2_656 2_656 ?
Ca1 O1 Ca1 63.8(3) . 6 ?
O5 O3 Ca1 24.4(7) 6 . ?
O5 O3 Ca1 57.1(12) 6 2_656 ?
Ca1 O3 Ca1 80.8(9) . 2_656 ?
O4' O4 Ca1 76.7(17) . . ?
O4 O4' Ca1 85.4(17) . . ?
Ca1 O5 O5 142(4) 6 2_656 ?
Ca1 O5 O3 114(2) 6 6 ?
O5 O5 O3 100(3) 2_656 6 ?
Ca1 O5 Ca1 158(2) 6 5_656 ?
O5 O5 Ca1 16.6(16) 2_656 5_656 ?
O3 O5 Ca1 83.3(14) 6 5_656 ?
Ca1 O5 Ca1 71.3(14) 6 . ?
O5 O5 Ca1 109.0(10) 2_656 . ?
O3 O5 Ca1 117.6(15) 6 . ?
Ca1 O5 Ca1 115.0(9) 5_656 . ?
Ca1 O6 Ca1 57.2(3) 6 . ?

_refine_diff_density_max         0.761
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.092



####################################################################### 
# 
# 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_5Sr
_database_code_depnum_ccdc_archive 'CCDC 2058272'
loop_
_audit_author_name
_audit_author_address
'Michal Heczko'
;Jagiellonian University in Cracow
Poland
;
_audit_update_record             
;
2021-03-24 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H118 N28 Nb2 Ni3 O23 Sr'
_chemical_formula_weight         1881.25

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'
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

_cell_length_a                   26.1052(7)
_cell_length_b                   15.6770(4)
_cell_length_c                   10.3076(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.1260(10)
_cell_angle_gamma                90
_cell_volume                     4201.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    13041
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.58

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_F_000             1956
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    1.631
_shelx_estimated_absorpt_T_min   0.780
_shelx_estimated_absorpt_T_max   0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25693
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.212
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5028
_reflns_number_gt                4245
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1009P)²+69.7015P] 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         5028
_refine_ls_number_parameters     279
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0709
_refine_ls_wR_factor_ref         0.2055
_refine_ls_wR_factor_gt          0.1956
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.090
_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
Nb1 Nb 0.17258(2) 0.500000 0.78054(6) 0.01032(18) Uani 1 2 d S T P . .
Ni2 Ni 0.250000 0.750000 0.500000 0.0140(2) Uani 1 2 d S . P . .
Ni1 Ni 0.000000 0.500000 1.000000 0.0158(3) Uani 1 4 d S T P . .
Sr1 Sr 0.03309(14) 0.0816(2) -0.1321(3) 0.0493(8) Uani 0.25 1 d . . P . .
N2 N 0.23528(18) 0.6337(3) 0.5891(4) 0.0198(9) Uani 1 1 d . . . . .
N1 N 0.0787(3) 0.500000 0.9848(6) 0.0222(14) Uani 1 2 d S T P . .
C1 C 0.1132(3) 0.500000 0.9224(7) 0.0164(14) Uani 1 2 d S T P . .
N4 N 0.2899(3) 0.500000 0.9523(7) 0.0282(16) Uani 1 2 d S T P . .
N3 N 0.0801(2) 0.3704(4) 0.6338(5) 0.0318(12) Uani 1 1 d . . . . .
N5 N 0.1784(2) 0.6930(4) 0.9324(5) 0.0344(13) Uani 1 1 d . . . . .
N11 N -0.0073(2) 0.4024(4) 0.8637(5) 0.0327(13) Uani 1 1 d . . . . .
H11 H 0.026987 0.395111 0.828876 0.039 Uiso 1 1 calc R U . . .
N22 N 0.1880(2) 0.7994(3) 0.5883(6) 0.0345(13) Uani 1 1 d . . . . .
H22 H 0.177073 0.755319 0.650261 0.041 Uiso 1 1 calc R U . . .
C4 C 0.2503(3) 0.500000 0.8947(7) 0.0200(15) Uani 1 2 d S T P . .
C3 C 0.11163(19) 0.4151(4) 0.6795(5) 0.0182(10) Uani 1 1 d . . . . .
C2 C 0.21531(19) 0.5854(3) 0.6529(5) 0.0158(10) Uani 1 1 d . . . . .
N21 N 0.1970(2) 0.7213(4) 0.3456(5) 0.0342(13) Uani 1 1 d . . . . .
H21 H 0.199649 0.766899 0.278701 0.041 Uiso 1 1 calc R U . . .
C5 C 0.1780(2) 0.6275(4) 0.8832(5) 0.0203(11) Uani 1 1 d . . . . .
C23 C 0.1458(3) 0.7314(6) 0.3980(8) 0.054(2) Uani 1 1 d . . . . .
H23A H 0.137815 0.680004 0.448135 0.065 Uiso 1 1 calc R U . . .
H23B H 0.118698 0.738140 0.325143 0.065 Uiso 1 1 calc R U . . .
C12 C -0.0455(3) 0.4181(6) 0.7507(7) 0.051(2) Uani 1 1 d . . . . .
H12A H -0.080305 0.421395 0.781621 0.061 Uiso 1 1 calc R U . . .
H12B H -0.045152 0.369422 0.689582 0.061 Uiso 1 1 calc R U . . .
C24 C 0.1468(3) 0.8082(6) 0.4842(10) 0.053(2) Uani 1 1 d . . . . .
H24A H 0.152348 0.860156 0.432686 0.064 Uiso 1 1 calc R U . . .
H24B H 0.113368 0.813995 0.521979 0.064 Uiso 1 1 calc R U . . .
C13 C -0.0170(3) 0.3259(5) 0.9378(9) 0.051(2) Uani 1 1 d . . . . .
H13A H -0.010035 0.274644 0.886185 0.062 Uiso 1 1 calc R U . . .
H13B H -0.053481 0.324473 0.956789 0.062 Uiso 1 1 calc R U . . .
C25 C 0.2006(4) 0.8791(4) 0.6648(10) 0.062(3) Uani 1 1 d . . . . .
H25A H 0.169780 0.897462 0.706942 0.074 Uiso 1 1 calc R U . . .
H25B H 0.209310 0.924893 0.604510 0.074 Uiso 1 1 calc R U . . .
C22 C 0.2041(4) 0.6390(5) 0.2805(7) 0.058(3) Uani 1 1 d . . . . .
H22A H 0.199952 0.591993 0.342917 0.070 Uiso 1 1 calc R U . . .
H22B H 0.177322 0.632364 0.207032 0.070 Uiso 1 1 calc R U . . .
C21 C 0.2450(4) 0.8674(5) 0.7685(8) 0.062(3) Uani 1 1 d . . . . .
H21A H 0.245242 0.916133 0.829690 0.075 Uiso 1 1 calc R U . . .
H21B H 0.238821 0.815035 0.818493 0.075 Uiso 1 1 calc R U . . .
C11 C -0.0347(4) 0.500000 0.6790(9) 0.056(4) Uani 1 2 d S T P . .
H11A H -0.055682 0.499999 0.594117 0.067 Uiso 1 2 calc R U P . .
H11B H 0.001932 0.500001 0.660781 0.067 Uiso 1 2 calc R U P . .
O1 O 0.1108(2) 0.0525(3) 0.0560(5) 0.0419(12) Uani 1 1 d . . . . .
O2 O 0.0502(4) 0.000000 -0.3536(12) 0.080(3) Uani 1 2 d S T P . .
O3 O -0.0042(7) 0.1532(7) -0.3168(11) 0.077(5) Uani 0.5 1 d . . P . .
O5 O 0.0892(3) 0.1985(9) -0.1605(13) 0.059(4) Uani 0.5 1 d . . P . .
O6 O 0.1137(5) 0.000000 -0.1109(11) 0.107(5) Uani 1 2 d S T P . .
O7 O 0.0765(4) 0.0999(8) 0.1840(14) 0.055(3) Uani 0.5 1 d . . P . .
O8 O 0.1696(2) 0.1704(3) 0.1100(5) 0.0435(13) Uani 1 1 d . . . . .
O9 O 0.000000 0.2745(4) 0.500000 0.0391(17) Uani 1 2 d S T P . .
O10 O -0.0894(8) 0.000000 -0.402(2) 0.084(7) Uani 0.5 2 d S TU P . .
O4 O 0.000000 0.064(2) 0.000000 0.120(10) Uani 0.5 2 d S TU P . .
O11 O -0.162(2) 0.000000 -0.260(6) 0.23(3) Uani 0.5 2 d S TU 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
Nb1 C1 2.223(7) . ?
Nb1 C2 2.243(5) 6_565 ?
Nb1 C2 2.243(5) . ?
Nb1 C4 2.252(8) . ?
Nb1 C3 2.256(5) 6_565 ?
Nb1 C3 2.256(5) . ?
Nb1 C5 2.260(5) . ?
Nb1 C5 2.260(5) 6_565 ?
Ni2 N21 2.063(5) . ?
Ni2 N21 2.063(5) 7_566 ?
Ni2 N22 2.075(5) . ?
Ni2 N22 2.075(5) 7_566 ?
Ni2 N2 2.093(5) 7_566 ?
Ni2 N2 2.093(5) . ?
Ni1 N1 2.074(7) . ?
Ni1 N1 2.074(7) 5_567 ?
Ni1 N11 2.074(5) . ?
Ni1 N11 2.074(5) 5_567 ?
Ni1 N11 2.074(5) 6_565 ?
Ni1 N11 2.074(5) 2_557 ?
Sr1 O4 1.699(7) . ?
Sr1 O3 2.346(11) . ?
Sr1 O5 2.381(13) . ?
Sr1 O6 2.455(11) . ?
Sr1 Sr1 2.557(7) 6 ?
Sr1 O2 2.688(12) . ?
Sr1 O1 2.717(6) . ?
Sr1 O4 2.83(3) 5 ?
Sr1 O7 2.878(10) 2 ?
Sr1 Sr1 3.352(7) 2 ?
Sr1 Sr1 4.216(7) 5 ?
N2 C2 1.157(7) . ?
N1 C1 1.154(10) . ?
N4 C4 1.147(11) . ?
N3 C3 1.149(7) . ?
N5 C5 1.146(8) . ?
N11 C13 1.456(10) . ?
N11 C12 1.485(10) . ?
N11 H11 1.0000 . ?
N22 C24 1.457(11) . ?
N22 C25 1.498(10) . ?
N22 H22 1.0000 . ?
N21 C22 1.474(11) . ?
N21 C23 1.494(10) . ?
N21 H21 1.0000 . ?
C23 C24 1.495(14) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C12 C11 1.521(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C13 C13 1.492(19) 2_557 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C25 C21 1.516(15) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C22 C21 1.466(14) 7_566 ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
O1 O1 1.646(10) 6 ?
O1 O7 1.817(13) . ?

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
C1 Nb1 C2 142.96(13) . 6_565 ?
C1 Nb1 C2 142.96(13) . . ?
C2 Nb1 C2 73.3(3) 6_565 . ?
C1 Nb1 C4 107.7(3) . . ?
C2 Nb1 C4 80.5(2) 6_565 . ?
C2 Nb1 C4 80.5(2) . . ?
C1 Nb1 C3 78.4(2) . 6_565 ?
C2 Nb1 C3 116.64(19) 6_565 6_565 ?
C2 Nb1 C3 75.20(18) . 6_565 ?
C4 Nb1 C3 143.73(14) . 6_565 ?
C1 Nb1 C3 78.4(2) . . ?
C2 Nb1 C3 75.20(19) 6_565 . ?
C2 Nb1 C3 116.64(19) . . ?
C4 Nb1 C3 143.73(14) . . ?
C3 Nb1 C3 72.3(3) 6_565 . ?
C1 Nb1 C5 73.18(15) . . ?
C2 Nb1 C5 142.05(19) 6_565 . ?
C2 Nb1 C5 74.51(19) . . ?
C4 Nb1 C5 74.87(17) . . ?
C3 Nb1 C5 73.0(2) 6_565 . ?
C3 Nb1 C5 138.6(2) . . ?
C1 Nb1 C5 73.18(15) . 6_565 ?
C2 Nb1 C5 74.51(19) 6_565 6_565 ?
C2 Nb1 C5 142.05(19) . 6_565 ?
C4 Nb1 C5 74.87(17) . 6_565 ?
C3 Nb1 C5 138.6(2) 6_565 6_565 ?
C3 Nb1 C5 73.0(2) . 6_565 ?
C5 Nb1 C5 124.4(3) . 6_565 ?
N21 Ni2 N21 180.0 . 7_566 ?
N21 Ni2 N22 85.6(3) . . ?
N21 Ni2 N22 94.4(3) 7_566 . ?
N21 Ni2 N22 94.4(3) . 7_566 ?
N21 Ni2 N22 85.6(3) 7_566 7_566 ?
N22 Ni2 N22 180.0 . 7_566 ?
N21 Ni2 N2 89.33(19) . 7_566 ?
N21 Ni2 N2 90.67(19) 7_566 7_566 ?
N22 Ni2 N2 92.76(19) . 7_566 ?
N22 Ni2 N2 87.24(19) 7_566 7_566 ?
N21 Ni2 N2 90.67(19) . . ?
N21 Ni2 N2 89.33(19) 7_566 . ?
N22 Ni2 N2 87.24(19) . . ?
N22 Ni2 N2 92.76(19) 7_566 . ?
N2 Ni2 N2 180.0 7_566 . ?
N1 Ni1 N1 180.0 . 5_567 ?
N1 Ni1 N11 88.87(19) . . ?
N1 Ni1 N11 91.13(19) 5_567 . ?
N1 Ni1 N11 91.13(19) . 5_567 ?
N1 Ni1 N11 88.87(19) 5_567 5_567 ?
N11 Ni1 N11 180.0 . 5_567 ?
N1 Ni1 N11 88.87(19) . 6_565 ?
N1 Ni1 N11 91.13(19) 5_567 6_565 ?
N11 Ni1 N11 95.1(4) . 6_565 ?
N11 Ni1 N11 84.9(4) 5_567 6_565 ?
N1 Ni1 N11 91.13(19) . 2_557 ?
N1 Ni1 N11 88.87(19) 5_567 2_557 ?
N11 Ni1 N11 84.9(4) . 2_557 ?
N11 Ni1 N11 95.1(4) 5_567 2_557 ?
N11 Ni1 N11 180.0 6_565 2_557 ?
O4 Sr1 O3 121.7(7) . . ?
O4 Sr1 O5 126.0(10) . . ?
O3 Sr1 O5 75.3(5) . . ?
O4 Sr1 O6 109.7(8) . . ?
O3 Sr1 O6 127.7(5) . . ?
O5 Sr1 O6 83.1(3) . . ?
O4 Sr1 Sr1 80.6(11) . 6 ?
O3 Sr1 Sr1 118.6(3) . 6 ?
O5 Sr1 Sr1 140.4(3) . 6 ?
O6 Sr1 Sr1 58.62(17) . 6 ?
O4 Sr1 O2 137.5(10) . . ?
O3 Sr1 O2 68.1(4) . . ?
O5 Sr1 O2 96.4(4) . . ?
O6 Sr1 O2 67.8(3) . . ?
Sr1 Sr1 O2 61.61(15) 6 . ?
O4 Sr1 O1 78.5(2) . . ?
O3 Sr1 O1 152.7(5) . . ?
O5 Sr1 O1 77.8(3) . . ?
O6 Sr1 O1 43.1(3) . . ?
Sr1 Sr1 O1 80.35(13) 6 . ?
O2 Sr1 O1 110.9(3) . . ?
O4 Sr1 O4 44.2(15) . 5 ?
O3 Sr1 O4 130.8(4) . 5 ?
O5 Sr1 O4 153.8(3) . 5 ?
O6 Sr1 O4 80.4(3) . 5 ?
Sr1 Sr1 O4 36.3(4) 6 5 ?
O2 Sr1 O4 96.1(4) . 5 ?
O1 Sr1 O4 76.23(14) . 5 ?
O4 Sr1 O7 66.3(4) . 2 ?
O3 Sr1 O7 57.8(5) . 2 ?
O5 Sr1 O7 120.8(4) . 2 ?
O6 Sr1 O7 153.9(3) . 2 ?
Sr1 Sr1 O7 95.7(2) 6 2 ?
O2 Sr1 O7 97.3(4) . 2 ?
O1 Sr1 O7 144.7(3) . 2 ?
O4 Sr1 O7 80.1(3) 5 2 ?
O4 Sr1 Sr1 9.4(11) . 2 ?
O3 Sr1 Sr1 116.9(4) . 2 ?
O5 Sr1 Sr1 117.8(3) . 2 ?
O6 Sr1 Sr1 115.3(3) . 2 ?
Sr1 Sr1 Sr1 90.0 6 2 ?
O2 Sr1 Sr1 145.7(2) . 2 ?
O1 Sr1 Sr1 80.00(17) . 2 ?
O4 Sr1 Sr1 53.7(4) 5 2 ?
O7 Sr1 Sr1 64.9(3) 2 2 ?
O4 Sr1 Sr1 27.9(11) . 5 ?
O3 Sr1 Sr1 130.5(5) . 5 ?
O5 Sr1 Sr1 147.0(3) . 5 ?
O6 Sr1 Sr1 91.4(3) . 5 ?
Sr1 Sr1 Sr1 52.67(9) 6 5 ?
O2 Sr1 Sr1 111.6(2) . 5 ?
O1 Sr1 Sr1 76.13(15) . 5 ?
O4 Sr1 Sr1 16.3(4) 5 5 ?
O7 Sr1 Sr1 73.9(3) 2 5 ?
Sr1 Sr1 Sr1 37.33(9) 2 5 ?
C2 N2 Ni2 158.3(4) . . ?
C1 N1 Ni1 150.6(6) . . ?
N1 C1 Nb1 172.8(7) . . ?
C13 N11 C12 114.3(6) . . ?
C13 N11 Ni1 105.2(4) . . ?
C12 N11 Ni1 115.1(5) . . ?
C13 N11 H11 107.3 . . ?
C12 N11 H11 107.3 . . ?
Ni1 N11 H11 107.3 . . ?
C24 N22 C25 114.9(7) . . ?
C24 N22 Ni2 105.5(5) . . ?
C25 N22 Ni2 113.6(5) . . ?
C24 N22 H22 107.5 . . ?
C25 N22 H22 107.5 . . ?
Ni2 N22 H22 107.5 . . ?
N4 C4 Nb1 179.7(7) . . ?
N3 C3 Nb1 176.7(5) . . ?
N2 C2 Nb1 175.6(4) . . ?
C22 N21 C23 114.3(6) . . ?
C22 N21 Ni2 116.0(5) . . ?
C23 N21 Ni2 105.0(4) . . ?
C22 N21 H21 107.0 . . ?
C23 N21 H21 107.0 . . ?
Ni2 N21 H21 107.0 . . ?
N5 C5 Nb1 176.5(6) . . ?
N21 C23 C24 109.4(6) . . ?
N21 C23 H23A 109.8 . . ?
C24 C23 H23A 109.8 . . ?
N21 C23 H23B 109.8 . . ?
C24 C23 H23B 109.8 . . ?
H23A C23 H23B 108.2 . . ?
N11 C12 C11 112.3(6) . . ?
N11 C12 H12A 109.1 . . ?
C11 C12 H12A 109.1 . . ?
N11 C12 H12B 109.1 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
N22 C24 C23 109.5(6) . . ?
N22 C24 H24A 109.8 . . ?
C23 C24 H24A 109.8 . . ?
N22 C24 H24B 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.2 . . ?
N11 C13 C13 109.4(5) . 2_557 ?
N11 C13 H13A 109.8 . . ?
C13 C13 H13A 109.8 2_557 . ?
N11 C13 H13B 109.8 . . ?
C13 C13 H13B 109.8 2_557 . ?
H13A C13 H13B 108.2 . . ?
N22 C25 C21 112.8(6) . . ?
N22 C25 H25A 109.0 . . ?
C21 C25 H25A 109.0 . . ?
N22 C25 H25B 109.0 . . ?
C21 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C21 C22 N21 111.8(6) 7_566 . ?
C21 C22 H22A 109.2 7_566 . ?
N21 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 7_566 . ?
N21 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C22 C21 C25 115.1(6) 7_566 . ?
C22 C21 H21A 108.5 7_566 . ?
C25 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 7_566 . ?
C25 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C12 C11 C12 115.2(8) . 6_565 ?
C12 C11 H11A 108.5 . . ?
C12 C11 H11A 108.5 6_565 . ?
C12 C11 H11B 108.5 . . ?
C12 C11 H11B 108.5 6_565 . ?
H11A C11 H11B 107.5 . . ?
O1 O1 O7 114.1(4) 6 . ?
O1 O1 Sr1 99.65(13) 6 . ?
O7 O1 Sr1 93.7(4) . . ?
Sr1 O2 Sr1 56.8(3) . 6 ?
Sr1 O6 Sr1 62.8(3) 6 . ?
O1 O7 Sr1 111.7(6) . 2 ?
Sr1 O4 Sr1 161(2) 2 . ?
Sr1 O4 Sr1 135.8(15) 2 6 ?
Sr1 O4 Sr1 63.1(7) . 6 ?
Sr1 O4 Sr1 63.1(7) 2 5 ?
Sr1 O4 Sr1 135.8(15) . 5 ?
Sr1 O4 Sr1 72.7(8) 6 5 ?

_refine_diff_density_max         1.735
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.191



####################################################################### 
# 
# 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_3mg
_database_code_depnum_ccdc_archive 'CCDC 2057599'
loop_
_audit_author_name
_audit_author_address
'Christian Nather'
;Institute of Inorganic Chemistry University of Kiel
Germany
;
_audit_update_record             
;
2021-03-26 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H120 Mg N28 Nb2 Ni3 O24'
_chemical_formula_weight         1835.95

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'
Mg Mg 0.0486 0.0363 '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'
Nb Nb -2.0727 0.6215 '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/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   10.2154(3)
_cell_length_b                   15.6242(4)
_cell_length_c                   26.2257(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.930(3)
_cell_angle_gamma                90
_cell_volume                     4163.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    21150
_cell_measurement_theta_min      1.56
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_F_000             1924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    1.022
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'IPDS-2 from STOE'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21150
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.561
_diffrn_reflns_theta_max         26.002
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             7927
_reflns_number_gt                6029
_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       'X-AREA (STOE, 2008)'
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²+0.6405P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7927
_refine_ls_number_parameters     595
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1018
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.006
_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
Nb1 Nb 0.28133(2) 0.48958(2) 0.17230(2) 0.01909(9) Uani 1 1 d . . . . .
C1 C 0.1505(3) 0.4018(2) 0.21203(13) 0.0244(7) Uani 1 1 d . . . . .
N1 N 0.0858(3) 0.35327(19) 0.23032(12) 0.0277(6) Uani 1 1 d . . . . .
C2 C 0.4233(3) 0.4938(2) 0.11295(13) 0.0240(6) Uani 1 1 d . . . . .
N2 N 0.4841(3) 0.4964(2) 0.07865(11) 0.0287(6) Uani 1 1 d . . . . .
C3 C 0.1762(3) 0.5764(2) 0.11255(14) 0.0270(7) Uani 1 1 d . . . . .
N3 N 0.1308(3) 0.6240(2) 0.08213(13) 0.0380(8) Uani 1 1 d . . . . .
C4 C 0.3980(3) 0.4878(2) 0.24953(13) 0.0253(7) Uani 1 1 d . . . . .
N4 N 0.4594(3) 0.4877(2) 0.28922(12) 0.0326(7) Uani 1 1 d . . . . .
C5 C 0.3842(3) 0.6179(2) 0.18033(14) 0.0258(7) Uani 1 1 d . . . . .
N5 N 0.4327(3) 0.6838(2) 0.18177(14) 0.0382(8) Uani 1 1 d . . . . .
C6 C 0.3856(3) 0.3620(2) 0.17726(15) 0.0285(7) Uani 1 1 d . . . . .
N6 N 0.4330(3) 0.2958(2) 0.17698(16) 0.0458(9) Uani 1 1 d . . . . .
C7 C 0.1538(3) 0.5722(2) 0.21693(13) 0.0237(7) Uani 1 1 d . . . . .
N7 N 0.0913(3) 0.61870(19) 0.23794(12) 0.0286(6) Uani 1 1 d . . . . .
C8 C 0.1844(3) 0.4049(2) 0.10927(14) 0.0273(7) Uani 1 1 d . . . . .
N8 N 0.1421(3) 0.3596(2) 0.07730(13) 0.0391(8) Uani 1 1 d . . . . .
Ni1 Ni -0.00224(4) 0.23587(3) 0.24546(2) 0.02325(11) Uani 1 1 d . . . . .
N11 N 0.1530(3) 0.2106(2) 0.30063(14) 0.0398(8) Uani 1 1 d . . . . .
H11 H 0.220074 0.256477 0.297563 0.048 Uiso 1 1 calc R U . . .
C11 C 0.0992(4) 0.2240(3) 0.35044(16) 0.0485(12) Uani 1 1 d . . . . .
H11A H 0.172332 0.233290 0.377709 0.058 Uiso 1 1 calc R U . . .
H11B H 0.050079 0.172452 0.359351 0.058 Uiso 1 1 calc R U . . .
C12 C 0.0087(5) 0.3007(3) 0.34728(18) 0.0481(11) Uani 1 1 d . . . . .
H12A H -0.031206 0.307254 0.379895 0.058 Uiso 1 1 calc R U . . .
H12B H 0.059285 0.353209 0.341528 0.058 Uiso 1 1 calc R U . . .
N12 N -0.0942(3) 0.2886(2) 0.30520(13) 0.0360(7) Uani 1 1 d . . . . .
H12 H -0.156596 0.244735 0.316328 0.043 Uiso 1 1 calc R U . . .
C13 C -0.1720(5) 0.3674(3) 0.2910(2) 0.0499(11) Uani 1 1 d . . . . .
H13A H -0.111467 0.413358 0.282277 0.060 Uiso 1 1 calc R U . . .
H13B H -0.215789 0.386736 0.320935 0.060 Uiso 1 1 calc R U . . .
C14 C -0.2751(4) 0.3535(3) 0.2461(2) 0.0494(11) Uani 1 1 d . . . . .
H14A H -0.326211 0.301672 0.253003 0.059 Uiso 1 1 calc R U . . .
H14B H -0.336566 0.402627 0.244275 0.059 Uiso 1 1 calc R U . . .
C15 C -0.2242(4) 0.3433(3) 0.1946(2) 0.0466(11) Uani 1 1 d . . . . .
H15A H -0.298679 0.347239 0.167355 0.056 Uiso 1 1 calc R U . . .
H15B H -0.162238 0.390400 0.189358 0.056 Uiso 1 1 calc R U . . .
N13 N -0.1570(3) 0.2610(2) 0.19028(13) 0.0357(7) Uani 1 1 d . . . . .
H13 H -0.224222 0.215230 0.193349 0.043 Uiso 1 1 calc R U . . .
C16 C -0.1040(4) 0.2480(3) 0.14036(16) 0.0452(10) Uani 1 1 d . . . . .
H16A H -0.054905 0.299582 0.131484 0.054 Uiso 1 1 calc R U . . .
H16B H -0.177463 0.238937 0.113193 0.054 Uiso 1 1 calc R U . . .
C17 C -0.0137(5) 0.1712(3) 0.14322(18) 0.0493(11) Uani 1 1 d . . . . .
H17A H -0.064257 0.118648 0.148864 0.059 Uiso 1 1 calc R U . . .
H17B H 0.026291 0.164921 0.110612 0.059 Uiso 1 1 calc R U . . .
N14 N 0.0896(3) 0.1835(2) 0.18570(13) 0.0368(7) Uani 1 1 d . . . . .
H14 H 0.151588 0.227695 0.174604 0.044 Uiso 1 1 calc R U . . .
C18 C 0.1686(5) 0.1049(3) 0.1996(2) 0.0539(13) Uani 1 1 d . . . . .
H18A H 0.212957 0.086292 0.169693 0.065 Uiso 1 1 calc R U . . .
H18B H 0.108650 0.058399 0.208090 0.065 Uiso 1 1 calc R U . . .
C19 C 0.2707(4) 0.1192(3) 0.2446(2) 0.0569(14) Uani 1 1 d . . . . .
H19A H 0.333012 0.070543 0.246393 0.068 Uiso 1 1 calc R U . . .
H19B H 0.321026 0.171445 0.237850 0.068 Uiso 1 1 calc R U . . .
C20 C 0.2202(4) 0.1287(3) 0.2960(2) 0.0503(13) Uani 1 1 d . . . . .
H20A H 0.158401 0.081422 0.301051 0.060 Uiso 1 1 calc R U . . .
H20B H 0.294788 0.124542 0.323159 0.060 Uiso 1 1 calc R U . . .
Ni2 Ni 0.500000 0.500000 0.000000 0.02283(14) Uani 1 2 d S . P . .
N22 N 0.3732(3) 0.6045(2) -0.00560(13) 0.0381(8) Uani 1 1 d . . . . .
H22 H 0.339674 0.612201 0.028607 0.046 Uiso 1 1 calc R U . . .
C21 C 0.4592(6) 0.6786(3) -0.0138(2) 0.0562(13) Uani 1 1 d . . . . .
H21A H 0.413631 0.732524 -0.006594 0.067 Uiso 1 1 calc R U . . .
H21B H 0.479260 0.679906 -0.049939 0.067 Uiso 1 1 calc R U . . .
C22 C 0.5841(5) 0.6708(3) 0.0211(2) 0.0527(12) Uani 1 1 d . . . . .
H22A H 0.642536 0.719902 0.015865 0.063 Uiso 1 1 calc R U . . .
H22B H 0.564262 0.671331 0.057292 0.063 Uiso 1 1 calc R U . . .
N21 N 0.6498(3) 0.5906(2) 0.01008(13) 0.0370(8) Uani 1 1 d . . . . .
H21 H 0.686469 0.597753 -0.023573 0.044 Uiso 1 1 calc R U . . .
C23 C 0.7599(4) 0.5673(4) 0.04846(17) 0.0520(13) Uani 1 1 d . . . . .
H23A H 0.727317 0.563176 0.082632 0.062 Uiso 1 1 calc R U . . .
H23B H 0.827515 0.612862 0.050018 0.062 Uiso 1 1 calc R U . . .
C24 C 0.8228(4) 0.4821(4) 0.03578(18) 0.0590(15) Uani 1 1 d . . . . .
H24A H 0.841333 0.483520 -0.000517 0.071 Uiso 1 1 calc R U . . .
H24B H 0.908140 0.476719 0.057118 0.071 Uiso 1 1 calc R U . . .
C25 C 0.7416(4) 0.4034(4) 0.04387(18) 0.0525(13) Uani 1 1 d . . . . .
H25A H 0.797650 0.351971 0.042243 0.063 Uiso 1 1 calc R U . . .
H25B H 0.711349 0.405743 0.078499 0.063 Uiso 1 1 calc R U . . .
Mg1 Mg 0.4877(2) 0.48590(15) 0.45498(9) 0.0274(5) Uani 0.5 1 d D . P A -1
O18 O 0.3434(10) 0.5675(8) 0.4238(5) 0.041(2) Uani 0.5 1 d D . P A -1
H18C H 0.348(8) 0.601(7) 0.397(4) 0.061 Uiso 0.5 1 d D U P B -1
H18D H 0.276(7) 0.587(6) 0.438(3) 0.061 Uiso 0.5 1 d D U P C -1
O2 O 0.6500(5) 0.4052(3) 0.4794(2) 0.0319(11) Uani 0.5 1 d D . P A -1
H2A H 0.619(6) 0.377(4) 0.504(2) 0.048 Uiso 0.5 1 d D U P D -1
H2B H 0.645(8) 0.366(3) 0.4553(19) 0.048 Uiso 0.5 1 d D U P E -1
O3 O 0.5825(5) 0.5017(6) 0.3898(2) 0.0345(13) Uani 0.5 1 d D . P A -1
H3A H 0.666(3) 0.490(9) 0.389(2) 0.052 Uiso 0.5 1 d D U P F -1
H3B H 0.546(5) 0.490(7) 0.3593(14) 0.052 Uiso 0.5 1 d D U P G -1
O4 O 0.3800(6) 0.3812(4) 0.4276(2) 0.0358(12) Uani 0.5 1 d D . P A -1
H4A H 0.405(8) 0.371(7) 0.3977(17) 0.054 Uiso 0.5 1 d D U P H -1
H4B H 0.300(4) 0.400(7) 0.421(4) 0.054 Uiso 0.5 1 d D U P I -1
O5 O 0.4044(6) 0.4644(5) 0.5214(2) 0.0395(13) Uani 0.5 1 d D . P A -1
H5A H 0.402(9) 0.499(4) 0.547(2) 0.059 Uiso 0.5 1 d D U P J -1
H5B H 0.347(9) 0.425(5) 0.527(2) 0.059 Uiso 0.5 1 d D U P K -1
O6 O 0.5920(6) 0.5874(4) 0.4869(2) 0.0346(12) Uani 0.5 1 d D . P A -1
H6A H 0.619(9) 0.594(4) 0.5192(10) 0.052 Uiso 0.5 1 d D U P L -1
H6B H 0.624(8) 0.629(4) 0.4704(15) 0.052 Uiso 0.5 1 d D U P M -1
O7 O 0.6277(9) 0.4558(5) 0.3888(2) 0.0404(14) Uani 0.5 1 d G . P N 2
H7A H 0.653722 0.508180 0.394989 0.061 Uiso 0.5 1 d G U P N 2
H7B H 0.580323 0.458547 0.359334 0.061 Uiso 0.5 1 d G U P N 2
O8 O 0.2943(6) 0.4018(5) 0.4155(3) 0.0390(13) Uani 0.5 1 d . . P O 2
H8A H 0.307769 0.359274 0.396509 0.047 Uiso 0.5 1 d R U P O 2
H8B H 0.220589 0.426964 0.409349 0.047 Uiso 0.5 1 d R U P O 2
O9 O 0.8062(7) 0.3502(5) 0.5067(3) 0.069(2) Uani 0.5 1 d . . P P 2
H9A H 0.789981 0.387153 0.482098 0.103 Uiso 0.5 1 d R U P P 2
H9B H 0.850791 0.378763 0.531138 0.103 Uiso 0.5 1 d R U P P 2
O10 O 0.2988(11) 0.5766(8) 0.4117(4) 0.042(2) Uani 0.5 1 d G . P Q 2
H10A H 0.370048 0.591439 0.398463 0.063 Uiso 0.5 1 d G U P Q 2
H10B H 0.299086 0.607745 0.439234 0.063 Uiso 0.5 1 d G U P Q 2
O11 O 0.0021(3) 0.26654(18) -0.00507(11) 0.0414(7) Uani 1 1 d G . . . .
H11C H 0.040346 0.297267 0.019767 0.062 Uiso 1 1 d G U . . .
H11D H -0.032068 0.303835 -0.027287 0.062 Uiso 1 1 d G U . . .
O12 O 0.6109(3) 0.81909(18) 0.16915(12) 0.0367(6) Uani 1 1 d G . . . .
H12C H 0.551267 0.780422 0.172769 0.055 Uiso 1 1 d G U . . .
H12D H 0.590221 0.861337 0.188424 0.055 Uiso 1 1 d G U . . .
O13 O 0.8653(4) 0.4913(2) 0.44466(14) 0.0571(8) Uani 1 1 d G . . . .
H13C H 0.941364 0.486490 0.432733 0.086 Uiso 1 1 d G U . . .
H13D H 0.874145 0.535178 0.465128 0.086 Uiso 1 1 d G U . . .
O14 O 0.3234(5) 0.7760(3) 0.08649(18) 0.0884(14) Uani 1 1 d G . . . .
H14C H 0.261631 0.809909 0.094972 0.133 Uiso 1 1 d G U . . .
H14D H 0.364560 0.759814 0.115577 0.133 Uiso 1 1 d G U . . .
O15 O 0.3047(4) 0.1909(3) 0.07843(16) 0.0743(11) Uani 1 1 d G . . . .
H15C H 0.365051 0.204518 0.102985 0.111 Uiso 1 1 d G U . . .
H15D H 0.253918 0.235699 0.074960 0.111 Uiso 1 1 d G U . . .
O16 O 0.1000(6) 0.3909(3) 0.46942(18) 0.0863(15) Uani 1 1 d G . . . .
H16C H 0.172727 0.363166 0.466671 0.129 Uiso 1 1 d G U . . .
H16D H 0.041667 0.351182 0.472527 0.129 Uiso 1 1 d G U . . .
O17 O 0.6036(6) 0.1553(4) 0.1656(2) 0.0389(12) Uani 0.7 1 d G . P R 1
H17C H 0.551988 0.197242 0.172199 0.058 Uiso 0.7 1 d G U P R 1
H17D H 0.574898 0.111721 0.181882 0.058 Uiso 0.7 1 d G U P R 1
O17' O 0.532(2) 0.1498(12) 0.1531(7) 0.076(5) Uani 0.3 1 d G . P S 2
H17E H 0.467229 0.166411 0.169725 0.114 Uiso 0.3 1 d G U P S 2
H17F H 0.596175 0.184539 0.163074 0.114 Uiso 0.3 1 d G U P S 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
Nb1 C2 2.236(3) . ?
Nb1 C4 2.241(3) . ?
Nb1 C1 2.245(3) . ?
Nb1 C7 2.247(3) . ?
Nb1 C6 2.258(3) . ?
Nb1 C3 2.258(3) . ?
Nb1 C5 2.263(3) . ?
Nb1 C8 2.263(3) . ?
C1 N1 1.144(5) . ?
N1 Ni1 2.099(3) . ?
C2 N2 1.146(4) . ?
N2 Ni2 2.086(3) . ?
C3 N3 1.152(5) . ?
C4 N4 1.159(4) . ?
C5 N5 1.142(5) . ?
C6 N6 1.142(5) . ?
C7 N7 1.145(5) . ?
N7 Ni1 2.110(3) 2 ?
C8 N8 1.147(5) . ?
Ni1 N13 2.068(3) . ?
Ni1 N11 2.071(3) . ?
Ni1 N14 2.076(3) . ?
Ni1 N12 2.079(3) . ?
N11 C20 1.463(6) . ?
N11 C11 1.484(6) . ?
N11 H11 1.0000 . ?
C11 C12 1.510(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N12 1.455(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N12 C13 1.492(6) . ?
N12 H12 1.0000 . ?
C13 C14 1.511(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.506(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N13 1.467(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N13 C16 1.482(6) . ?
N13 H13 1.0000 . ?
C16 C17 1.510(7) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 N14 1.466(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
N14 C18 1.494(6) . ?
N14 H14 1.0000 . ?
C18 C19 1.508(8) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.499(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
Ni2 N22 2.080(3) 3_665 ?
Ni2 N22 2.080(3) . ?
Ni2 N21 2.082(3) . ?
Ni2 N21 2.082(3) 3_665 ?
N22 C25 1.468(5) 3_665 ?
N22 C21 1.482(6) . ?
N22 H22 1.0000 . ?
C21 C22 1.497(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N21 1.464(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
N21 C23 1.476(6) . ?
N21 H21 1.0000 . ?
C23 C24 1.529(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.510(8) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
Mg1 O6 2.041(7) . ?
Mg1 O5 2.044(6) . ?
Mg1 O18 2.053(9) . ?
Mg1 O4 2.058(6) . ?
Mg1 O3 2.065(6) . ?
Mg1 O2 2.129(6) . ?
O18 H18C 0.87(2) . ?
O18 H18D 0.87(2) . ?
O2 H2A 0.88(2) . ?
O2 H2B 0.87(2) . ?
O3 H3A 0.87(2) . ?
O3 H3B 0.87(2) . ?
O4 H4A 0.87(2) . ?
O4 H4B 0.87(2) . ?
O5 H5A 0.87(2) . ?
O5 H5B 0.87(2) . ?
O6 H6A 0.87(2) . ?
O6 H6B 0.87(2) . ?
O7 H7A 0.8700 . ?
O7 H7B 0.8700 . ?
O8 H8A 0.8501 . ?
O8 H8B 0.8500 . ?
O9 H9A 0.8699 . ?
O9 H9B 0.8697 . ?
O10 H10A 0.8698 . ?
O10 H10B 0.8704 . ?
O11 H11C 0.8689 . ?
O11 H11D 0.8710 . ?
O12 H12C 0.8700 . ?
O12 H12D 0.8706 . ?
O13 H13C 0.8698 . ?
O13 H13D 0.8701 . ?
O14 H14C 0.8701 . ?
O14 H14D 0.8699 . ?
O15 H15C 0.8705 . ?
O15 H15D 0.8699 . ?
O16 H16C 0.8699 . ?
O16 H16D 0.8702 . ?
O17 H17C 0.8699 . ?
O17 H17D 0.8704 . ?
O17' H17E 0.8700 . ?
O17' H17F 0.8700 . ?

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
C2 Nb1 C4 107.87(11) . . ?
C2 Nb1 C1 143.26(12) . . ?
C4 Nb1 C1 81.92(12) . . ?
C2 Nb1 C7 142.98(12) . . ?
C4 Nb1 C7 79.56(12) . . ?
C1 Nb1 C7 72.81(12) . . ?
C2 Nb1 C6 74.33(13) . . ?
C4 Nb1 C6 74.55(13) . . ?
C1 Nb1 C6 74.56(13) . . ?
C7 Nb1 C6 140.62(13) . . ?
C2 Nb1 C3 78.19(12) . . ?
C4 Nb1 C3 143.55(13) . . ?
C1 Nb1 C3 115.21(12) . . ?
C7 Nb1 C3 75.91(13) . . ?
C6 Nb1 C3 139.29(13) . . ?
C2 Nb1 C5 73.15(13) . . ?
C4 Nb1 C5 74.23(13) . . ?
C1 Nb1 C5 142.26(13) . . ?
C7 Nb1 C5 74.40(12) . . ?
C6 Nb1 C5 124.40(12) . . ?
C3 Nb1 C5 73.46(12) . . ?
C2 Nb1 C8 77.02(12) . . ?
C4 Nb1 C8 143.55(13) . . ?
C1 Nb1 C8 75.26(13) . . ?
C7 Nb1 C8 118.86(12) . . ?
C6 Nb1 C8 72.21(13) . . ?
C3 Nb1 C8 72.76(13) . . ?
C5 Nb1 C8 138.54(13) . . ?
N1 C1 Nb1 175.9(3) . . ?
C1 N1 Ni1 159.5(3) . . ?
N2 C2 Nb1 172.4(3) . . ?
C2 N2 Ni2 151.8(2) . . ?
N3 C3 Nb1 175.1(3) . . ?
N4 C4 Nb1 179.1(3) . . ?
N5 C5 Nb1 176.2(3) . . ?
N6 C6 Nb1 175.5(4) . . ?
N7 C7 Nb1 175.7(3) . . ?
C7 N7 Ni1 157.4(3) . 2 ?
N8 C8 Nb1 176.0(3) . . ?
N13 Ni1 N11 179.89(18) . . ?
N13 Ni1 N14 85.36(14) . . ?
N11 Ni1 N14 94.53(15) . . ?
N13 Ni1 N12 94.57(14) . . ?
N11 Ni1 N12 85.54(14) . . ?
N14 Ni1 N12 179.84(14) . . ?
N13 Ni1 N1 90.78(12) . . ?
N11 Ni1 N1 89.21(12) . . ?
N14 Ni1 N1 88.03(13) . . ?
N12 Ni1 N1 91.83(13) . . ?
N13 Ni1 N7 89.67(12) . 2_545 ?
N11 Ni1 N7 90.35(12) . 2_545 ?
N14 Ni1 N7 92.98(13) . 2_545 ?
N12 Ni1 N7 87.16(13) . 2_545 ?
N1 Ni1 N7 178.93(13) . 2_545 ?
C20 N11 C11 114.6(4) . . ?
C20 N11 Ni1 116.1(3) . . ?
C11 N11 Ni1 105.2(2) . . ?
C20 N11 H11 106.8 . . ?
C11 N11 H11 106.8 . . ?
Ni1 N11 H11 106.8 . . ?
N11 C11 C12 110.1(3) . . ?
N11 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N11 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N12 C12 C11 109.2(4) . . ?
N12 C12 H12A 109.8 . . ?
C11 C12 H12A 109.8 . . ?
N12 C12 H12B 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
C12 N12 C13 114.0(3) . . ?
C12 N12 Ni1 106.0(3) . . ?
C13 N12 Ni1 114.2(3) . . ?
C12 N12 H12 107.4 . . ?
C13 N12 H12 107.4 . . ?
Ni1 N12 H12 107.4 . . ?
N12 C13 C14 112.7(4) . . ?
N12 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
N12 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C15 C14 C13 115.9(4) . . ?
C15 C14 H14A 108.3 . . ?
C13 C14 H14A 108.3 . . ?
C15 C14 H14B 108.3 . . ?
C13 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
N13 C15 C14 111.7(3) . . ?
N13 C15 H15A 109.3 . . ?
C14 C15 H15A 109.3 . . ?
N13 C15 H15B 109.3 . . ?
C14 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
C15 N13 C16 113.9(3) . . ?
C15 N13 Ni1 116.3(3) . . ?
C16 N13 Ni1 105.6(2) . . ?
C15 N13 H13 106.8 . . ?
C16 N13 H13 106.8 . . ?
Ni1 N13 H13 106.8 . . ?
N13 C16 C17 110.0(4) . . ?
N13 C16 H16A 109.7 . . ?
C17 C16 H16A 109.7 . . ?
N13 C16 H16B 109.7 . . ?
C17 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
N14 C17 C16 108.8(4) . . ?
N14 C17 H17A 109.9 . . ?
C16 C17 H17A 109.9 . . ?
N14 C17 H17B 109.9 . . ?
C16 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
C17 N14 C18 114.0(4) . . ?
C17 N14 Ni1 106.2(3) . . ?
C18 N14 Ni1 114.5(3) . . ?
C17 N14 H14 107.3 . . ?
C18 N14 H14 107.3 . . ?
Ni1 N14 H14 107.3 . . ?
N14 C18 C19 112.4(4) . . ?
N14 C18 H18A 109.1 . . ?
C19 C18 H18A 109.1 . . ?
N14 C18 H18B 109.1 . . ?
C19 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C18 116.3(4) . . ?
C20 C19 H19A 108.2 . . ?
C18 C19 H19A 108.2 . . ?
C20 C19 H19B 108.2 . . ?
C18 C19 H19B 108.2 . . ?
H19A C19 H19B 107.4 . . ?
N11 C20 C19 111.7(4) . . ?
N11 C20 H20A 109.3 . . ?
C19 C20 H20A 109.3 . . ?
N11 C20 H20B 109.3 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
N22 Ni2 N22 180.0 3_665 . ?
N22 Ni2 N21 94.64(14) 3_665 . ?
N22 Ni2 N21 85.36(14) . . ?
N22 Ni2 N21 85.36(14) 3_665 3_665 ?
N22 Ni2 N21 94.64(14) . 3_665 ?
N21 Ni2 N21 180.00(12) . 3_665 ?
N22 Ni2 N2 88.82(12) 3_665 3_665 ?
N22 Ni2 N2 91.18(12) . 3_665 ?
N21 Ni2 N2 88.63(12) . 3_665 ?
N21 Ni2 N2 91.37(12) 3_665 3_665 ?
N22 Ni2 N2 91.18(12) 3_665 . ?
N22 Ni2 N2 88.82(12) . . ?
N21 Ni2 N2 91.37(12) . . ?
N21 Ni2 N2 88.63(12) 3_665 . ?
N2 Ni2 N2 180.0 3_665 . ?
C25 N22 C21 114.2(4) 3_665 . ?
C25 N22 Ni2 115.5(3) 3_665 . ?
C21 N22 Ni2 104.4(3) . . ?
C25 N22 H22 107.4 3_665 . ?
C21 N22 H22 107.4 . . ?
Ni2 N22 H22 107.4 . . ?
N22 C21 C22 109.1(4) . . ?
N22 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
N22 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
N21 C22 C21 109.1(4) . . ?
N21 C22 H22A 109.9 . . ?
C21 C22 H22A 109.9 . . ?
N21 C22 H22B 109.9 . . ?
C21 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C22 N21 C23 114.2(4) . . ?
C22 N21 Ni2 105.1(3) . . ?
C23 N21 Ni2 114.6(3) . . ?
C22 N21 H21 107.5 . . ?
C23 N21 H21 107.5 . . ?
Ni2 N21 H21 107.5 . . ?
N21 C23 C24 112.0(3) . . ?
N21 C23 H23A 109.2 . . ?
C24 C23 H23A 109.2 . . ?
N21 C23 H23B 109.2 . . ?
C24 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C25 C24 C23 115.4(4) . . ?
C25 C24 H24A 108.4 . . ?
C23 C24 H24A 108.4 . . ?
C25 C24 H24B 108.4 . . ?
C23 C24 H24B 108.4 . . ?
H24A C24 H24B 107.5 . . ?
N22 C25 C24 112.6(4) 3_665 . ?
N22 C25 H25A 109.1 3_665 . ?
C24 C25 H25A 109.1 . . ?
N22 C25 H25B 109.1 3_665 . ?
C24 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
O6 Mg1 O5 91.4(3) . . ?
O6 Mg1 O18 90.2(4) . . ?
O5 Mg1 O18 95.6(4) . . ?
O6 Mg1 O4 176.2(3) . . ?
O5 Mg1 O4 84.9(3) . . ?
O18 Mg1 O4 91.1(4) . . ?
O6 Mg1 O3 88.7(3) . . ?
O5 Mg1 O3 175.9(3) . . ?
O18 Mg1 O3 88.5(4) . . ?
O4 Mg1 O3 94.9(3) . . ?
O6 Mg1 O2 88.8(2) . . ?
O5 Mg1 O2 91.5(3) . . ?
O18 Mg1 O2 172.9(4) . . ?
O4 Mg1 O2 90.3(2) . . ?
O3 Mg1 O2 84.4(3) . . ?
Mg1 O18 H18C 127(3) . . ?
Mg1 O18 H18D 127(3) . . ?
H18C O18 H18D 104(5) . . ?
Mg1 O2 H2A 102(4) . . ?
Mg1 O2 H2B 102(4) . . ?
H2A O2 H2B 101(4) . . ?
Mg1 O3 H3A 123(4) . . ?
Mg1 O3 H3B 123(4) . . ?
H3A O3 H3B 105(5) . . ?
Mg1 O4 H4A 105(6) . . ?
Mg1 O4 H4B 105(7) . . ?
H4A O4 H4B 104(5) . . ?
Mg1 O5 H5A 127(3) . . ?
Mg1 O5 H5B 127(3) . . ?
H5A O5 H5B 104(5) . . ?
Mg1 O6 H6A 126(3) . . ?
Mg1 O6 H6B 126(3) . . ?
H6A O6 H6B 107(5) . . ?
H7A O7 H7B 104.5 . . ?
H8A O8 H8B 116.4 . . ?
H9A O9 H9B 104.5 . . ?
H10A O10 H10B 104.5 . . ?
H11C O11 H11D 104.5 . . ?
H12C O12 H12D 104.4 . . ?
H13C O13 H13D 104.5 . . ?
H14C O14 H14D 104.5 . . ?
H15C O15 H15D 104.5 . . ?
H16C O16 H16D 104.5 . . ?
H17C O17 H17D 104.5 . . ?
H17E O17' H17F 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 N11 C11 C12 -168.2(3) . . . . ?
Ni1 N11 C11 C12 -39.5(4) . . . . ?
N11 C11 C12 N12 56.1(4) . . . . ?
C11 C12 N12 C13 -167.4(4) . . . . ?
C11 C12 N12 Ni1 -40.9(4) . . . . ?
C12 N12 C13 C14 178.2(4) . . . . ?
Ni1 N12 C13 C14 56.1(4) . . . . ?
N12 C13 C14 C15 -72.0(5) . . . . ?
C13 C14 C15 N13 71.2(5) . . . . ?
C14 C15 N13 C16 -179.5(3) . . . . ?
C14 C15 N13 Ni1 -56.3(4) . . . . ?
C15 N13 C16 C17 168.4(3) . . . . ?
Ni1 N13 C16 C17 39.6(4) . . . . ?
N13 C16 C17 N14 -55.8(5) . . . . ?
C16 C17 N14 C18 167.9(4) . . . . ?
C16 C17 N14 Ni1 40.9(4) . . . . ?
C17 N14 C18 C19 -178.0(4) . . . . ?
Ni1 N14 C18 C19 -55.5(4) . . . . ?
N14 C18 C19 C20 71.9(5) . . . . ?
C11 N11 C20 C19 179.4(3) . . . . ?
Ni1 N11 C20 C19 56.4(4) . . . . ?
C18 C19 C20 N11 -71.7(5) . . . . ?
C25 N22 C21 C22 -169.6(4) 3_665 . . . ?
Ni2 N22 C21 C22 -42.6(4) . . . . ?
N22 C21 C22 N21 59.3(5) . . . . ?
C21 C22 N21 C23 -168.6(4) . . . . ?
C21 C22 N21 Ni2 -42.1(4) . . . . ?
C22 N21 C23 C24 178.6(4) . . . . ?
Ni2 N21 C23 C24 57.2(4) . . . . ?
N21 C23 C24 C25 -72.3(5) . . . . ?
C23 C24 C25 N22 71.3(5) . . . 3_665 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N11 H11 O12 1.00 2.10 2.987(4) 147.4 2_645
C11 H11B N3 0.99 2.63 3.457(6) 140.8 2_545
N13 H13 O17 1.00 2.06 2.966(7) 149.9 1_455
N22 H22 N3 1.00 2.68 3.563(5) 147.5 .
N21 H21 N8 1.00 2.45 3.373(5) 153.2 3_665
C23 H23A N2 0.99 2.69 3.202(5) 112.7 .
O2 H2B O14 0.87(2) 1.84(3) 2.688(7) 165(6) 2_645
O3 H3A O13 0.87(2) 2.38(4) 3.097(6) 139(5) .
O3 H3B N4 0.87(2) 1.96(3) 2.811(6) 169(10) .
O4 H4A O12 0.87(2) 1.92(4) 2.728(6) 154(8) 2_645
O4 H4B O16 0.87(2) 2.51(9) 3.171(9) 133(11) .
O5 H5B O15 0.87(2) 2.33(7) 3.078(9) 144(10) 4_566
O6 H6B O15 0.87(2) 1.81(3) 2.654(8) 162(7) 2_655
O9 H9A O13 0.87 2.09 2.842(8) 144.7 .

_refine_diff_density_max         0.599
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.073



####################################################################### 
# 
# 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_lineu
_database_code_depnum_ccdc_archive 'CCDC 2058271'
loop_
_audit_author_name
_audit_author_address
'Michal Heczko'
;Jagiellonian University in Cracow
Poland
;
_audit_update_record             
;
2021-03-24 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H112 Li2 N28 Nb2 Ni3 O20'
_chemical_formula_weight         1753.46

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'
Li Li -0.0003 0.0001 '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'
Nb Nb -2.0727 0.6215 '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           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

_cell_length_a                   26.4583(10)
_cell_length_b                   15.5934(6)
_cell_length_c                   10.1748(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.078(2)
_cell_angle_gamma                90
_cell_volume                     4174.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9910
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      25.21

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_F_000             1832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.005
_shelx_estimated_absorpt_T_min   0.832
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_T_max  0.7452
_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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18953
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.586
_diffrn_reflns_theta_max         25.209
_diffrn_reflns_theta_full        25.209
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3919
_reflns_number_gt                3492
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0178P)²+31.4552P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3919
_refine_ls_number_parameters     311
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0948
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.130
_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
Nb1 Nb 0.32963(2) 0.500000 0.22212(4) 0.01068(12) Uani 1 2 d S T P . .
C1 C 0.38815(19) 0.500000 0.0789(5) 0.0164(10) Uani 1 2 d S T P . .
N1 N 0.42209(16) 0.500000 0.0165(4) 0.0185(9) Uani 1 2 d S T P . .
C2 C 0.28688(14) 0.5853(2) 0.3499(4) 0.0192(8) Uani 1 1 d . . . . .
N2 N 0.26689(13) 0.6332(2) 0.4134(3) 0.0250(7) Uani 1 1 d . . . . .
C3 C 0.38998(15) 0.5862(3) 0.3253(4) 0.0236(8) Uani 1 1 d . . . . .
N3 N 0.42068(15) 0.6323(3) 0.3717(4) 0.0396(10) Uani 1 1 d . . . . .
C4 C 0.2536(2) 0.500000 0.1016(6) 0.0309(14) Uani 1 2 d S T P . .
N4 N 0.2148(2) 0.500000 0.0401(6) 0.0492(16) Uani 1 2 d S T P . .
C5 C 0.32268(16) 0.3718(3) 0.1187(4) 0.0278(9) Uani 1 1 d . . . . .
N5 N 0.3205(2) 0.3053(3) 0.0694(4) 0.0546(13) Uani 1 1 d . . . . .
Ni1 Ni 0.500000 0.500000 0.000000 0.0125(2) Uani 1 4 d S T P . .
C11 C 0.5176(2) 0.6748(3) 0.0631(7) 0.0648(19) Uani 1 1 d . . . . .
H11A H 0.553396 0.675653 0.042718 0.078 Uiso 1 1 calc R U . . .
H11B H 0.511625 0.726514 0.115724 0.078 Uiso 1 1 calc R U . . .
N11 N 0.50826(13) 0.5976(3) 0.1386(4) 0.0400(10) Uani 1 1 d . . . . .
H11 H 0.474632 0.605262 0.173653 0.048 Uiso 1 1 calc R U . . .
C12 C 0.54655(17) 0.5815(4) 0.2539(5) 0.0552(17) Uani 1 1 d . . . . .
H12A H 0.546336 0.630167 0.316224 0.066 Uiso 1 1 calc R U . . .
H12B H 0.580745 0.578680 0.222874 0.066 Uiso 1 1 calc R U . . .
C13 C 0.5370(3) 0.500000 0.3255(6) 0.063(3) Uani 1 2 d S T P . .
H13A H 0.501126 0.499998 0.345444 0.076 Uiso 1 2 calc R U P . .
H13B H 0.558661 0.500001 0.410995 0.076 Uiso 1 2 calc R U P . .
Ni2 Ni 0.250000 0.750000 0.500000 0.01662(16) Uani 1 2 d S . P . .
C21 C 0.2498(5) 0.8660(6) 0.2256(9) 0.057(3) Uani 0.705(12) 1 d D . P A 1
H21A H 0.247785 0.915370 0.164013 0.068 Uiso 0.705(12) 1 calc R U P A 1
H21B H 0.257314 0.814485 0.174271 0.068 Uiso 0.705(12) 1 calc R U P A 1
C22 C 0.2947(6) 0.8811(7) 0.3314(11) 0.051(3) Uani 0.705(12) 1 d D . P A 1
H22A H 0.324401 0.900962 0.288187 0.062 Uiso 0.705(12) 1 calc R U P A 1
H22B H 0.285653 0.926891 0.392114 0.062 Uiso 0.705(12) 1 calc R U P A 1
N21 N 0.3084(3) 0.8043(4) 0.4068(7) 0.0372(18) Uani 0.705(12) 1 d D . P A 1
H21 H 0.319582 0.760623 0.344096 0.045 Uiso 0.705(12) 1 calc R U P A 1
C23 C 0.3503(3) 0.8176(6) 0.5095(11) 0.053(2) Uani 0.705(12) 1 d D . P A 1
H23A H 0.344538 0.870935 0.558524 0.063 Uiso 0.705(12) 1 calc R U P A 1
H23B H 0.382378 0.824256 0.468375 0.063 Uiso 0.705(12) 1 calc R U P A 1
C24 C 0.3552(3) 0.7421(7) 0.6054(9) 0.042(2) Uani 0.705(12) 1 d D . P A 1
H24A H 0.365604 0.689991 0.559556 0.051 Uiso 0.705(12) 1 calc R U P A 1
H24B H 0.381411 0.754592 0.679709 0.051 Uiso 0.705(12) 1 calc R U P A 1
N22 N 0.3051(3) 0.7274(5) 0.6566(7) 0.0379(18) Uani 0.705(12) 1 d D . P A 1
H22 H 0.301267 0.773462 0.723100 0.045 Uiso 0.705(12) 1 calc R U P A 1
C25 C 0.3018(4) 0.6458(6) 0.7258(7) 0.047(2) Uani 0.705(12) 1 d D . P A 1
H25A H 0.328374 0.643865 0.802021 0.057 Uiso 0.705(12) 1 calc R U P A 1
H25B H 0.308236 0.598185 0.665465 0.057 Uiso 0.705(12) 1 calc R U P A 1
C21' C 0.2934(16) 0.875(2) 0.277(3) 0.075(9) Uani 0.295(12) 1 d D . P A 2
H21C H 0.303707 0.926525 0.228425 0.090 Uiso 0.295(12) 1 calc R U P A 2
H21D H 0.300490 0.824568 0.223288 0.090 Uiso 0.295(12) 1 calc R U P A 2
C22' C 0.3277(12) 0.8702(14) 0.407(2) 0.085(8) Uani 0.295(12) 1 d D . P A 2
H22C H 0.363490 0.877994 0.389551 0.102 Uiso 0.295(12) 1 calc R U P A 2
H22D H 0.318877 0.917190 0.465841 0.102 Uiso 0.295(12) 1 calc R U P A 2
N21' N 0.3225(8) 0.7886(11) 0.473(3) 0.065(6) Uani 0.295(12) 1 d D . P A 2
H21' H 0.336372 0.744166 0.415680 0.078 Uiso 0.295(12) 1 calc R U P A 2
C23' C 0.3517(10) 0.7819(15) 0.600(3) 0.071(8) Uani 0.295(12) 1 d D . P A 2
H23C H 0.344943 0.832336 0.654826 0.085 Uiso 0.295(12) 1 calc R U P A 2
H23D H 0.388374 0.781104 0.589010 0.085 Uiso 0.295(12) 1 calc R U P A 2
C24' C 0.3376(9) 0.7004(14) 0.670(3) 0.086(8) Uani 0.295(12) 1 d D . P A 2
H24C H 0.347070 0.649312 0.620200 0.103 Uiso 0.295(12) 1 calc R U P A 2
H24D H 0.355870 0.697851 0.760052 0.103 Uiso 0.295(12) 1 calc R U P A 2
N22' N 0.2806(9) 0.7020(10) 0.6774(19) 0.060(6) Uani 0.295(12) 1 d D . P A 2
H22' H 0.273822 0.744599 0.746905 0.071 Uiso 0.295(12) 1 calc R U P A 2
C25' C 0.2631(13) 0.6199(13) 0.718(3) 0.074(9) Uani 0.295(12) 1 d D . P A 2
H25C H 0.280176 0.605019 0.806657 0.089 Uiso 0.295(12) 1 calc R U P A 2
H25D H 0.271201 0.575043 0.655026 0.089 Uiso 0.295(12) 1 calc R U P A 2
Li1 Li 0.3960(9) 0.8776(10) 1.0032(17) 0.057(5) Uani 0.5 1 d . . P B 2
O1 O 0.4164(2) 0.7983(5) 1.1378(7) 0.142(3) Uani 1 1 d . . . B 2
H1C H 0.439988 0.813910 1.194574 0.213 Uiso 1 1 d R U . B 2
H1D H 0.390888 0.786604 1.176806 0.213 Uiso 1 1 d R U . B 2
O2 O 0.3837(2) 1.000000 1.0865(6) 0.0752(19) Uani 1 2 d S T P B 2
H2A H 0.401023 1.000000 1.160463 0.113 Uiso 1 2 d R U P B 2
H2B H 0.353114 1.000000 1.102023 0.113 Uiso 1 2 d R U P B 2
O3 O 0.33361(16) 0.8360(2) 0.9093(4) 0.0625(11) Uani 1 1 d . . . B 2
H3C H 0.309602 0.870881 0.912976 0.094 Uiso 1 1 d R U . B 2
H3D H 0.329862 0.791701 0.954196 0.094 Uiso 1 1 d R U . B 2
O4 O 0.4453(3) 0.9081(3) 0.8895(7) 0.165(4) Uani 1 1 d . . . B 2
H4C H 0.458381 0.890613 0.823084 0.247 Uiso 1 1 d R U . B 2
H4D H 0.445451 0.961893 0.889385 0.247 Uiso 1 1 d R U . B 2
O5 O 0.500000 0.7316(2) 0.500000 0.0263(9) Uani 1 2 d S T P C 2
H5C H 0.521180 0.696349 0.535700 0.039 Uiso 1 1 d R U . C 2
O6 O 0.49776(18) 0.8536(3) 0.6916(4) 0.0772(14) Uani 1 1 d . . . D 2
H6C H 0.497640 0.816071 0.632365 0.116 Uiso 1 1 d R U . D 2
H6D H 0.513384 0.882323 0.638876 0.116 Uiso 1 1 d R U . D 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
Nb1 C1 2.235(5) . ?
Nb1 C4 2.243(6) . ?
Nb1 C2 2.248(4) 6_565 ?
Nb1 C2 2.248(4) . ?
Nb1 C5 2.257(4) 6_565 ?
Nb1 C5 2.257(4) . ?
Nb1 C3 2.259(4) . ?
Nb1 C3 2.259(4) 6_565 ?
C1 N1 1.154(6) . ?
N1 Ni1 2.086(4) . ?
C2 N2 1.152(5) . ?
N2 Ni2 2.092(3) . ?
C3 N3 1.148(5) . ?
C4 N4 1.143(8) . ?
C5 N5 1.151(6) . ?
Ni1 N11 2.071(4) . ?
Ni1 N11 2.071(4) 5_665 ?
Ni1 N11 2.071(4) 6_565 ?
Ni1 N11 2.071(4) 2_655 ?
C11 N11 1.462(7) . ?
C11 C11 1.506(12) 2_655 ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N11 C12 1.488(6) . ?
N11 H11 1.0000 . ?
C12 C13 1.500(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
Ni2 N22' 2.040(19) 7_566 ?
Ni2 N22' 2.040(19) . ?
Ni2 N21' 2.057(19) 7_566 ?
Ni2 N21' 2.057(19) . ?
Ni2 N22 2.073(7) 7_566 ?
Ni2 N22 2.073(7) . ?
Ni2 N21 2.076(6) . ?
Ni2 N21 2.076(6) 7_566 ?
C21 C25 1.513(14) 7_566 ?
C21 C22 1.53(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N21 1.448(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
N21 C23 1.457(11) . ?
N21 H21 1.0000 . ?
C23 C24 1.526(14) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N22 1.491(11) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
N22 C25 1.460(10) . ?
N22 H22 1.0000 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C21' C25' 1.50(5) 7_566 ?
C21' C22' 1.53(3) . ?
C21' H21C 0.9900 . ?
C21' H21D 0.9900 . ?
C22' N21' 1.45(2) . ?
C22' H22C 0.9900 . ?
C22' H22D 0.9900 . ?
N21' C23' 1.44(2) . ?
N21' H21' 1.0000 . ?
C23' C24' 1.52(2) . ?
C23' H23C 0.9900 . ?
C23' H23D 0.9900 . ?
C24' N22' 1.52(2) . ?
C24' H24C 0.9900 . ?
C24' H24D 0.9900 . ?
N22' C25' 1.438(19) . ?
N22' H22' 1.0000 . ?
C25' H25C 0.9900 . ?
C25' H25D 0.9900 . ?
Li1 O1 1.881(17) . ?
Li1 O4 1.89(2) . ?
Li1 O3 1.93(2) . ?
Li1 O2 2.128(16) . ?
Li1 H1D 2.2804 . ?
Li1 H3D 2.2183 . ?
Li1 H4D 2.2587 . ?
O1 H1C 0.8400 . ?
O1 H1D 0.8392 . ?
O2 H2A 0.8396 . ?
O2 H2B 0.8398 . ?
O3 H3C 0.8399 . ?
O3 H3D 0.8400 . ?
O4 H4C 0.8371 . ?
O4 H4D 0.8391 . ?
O5 H5C 0.8400 . ?
O5 H5C 0.8399 2_656 ?
O6 H6C 0.8400 . ?
O6 H6D 0.8404 . ?

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
C1 Nb1 C4 106.7(2) . . ?
C1 Nb1 C2 143.39(9) . 6_565 ?
C4 Nb1 C2 80.73(16) . 6_565 ?
C1 Nb1 C2 143.39(9) . . ?
C4 Nb1 C2 80.74(16) . . ?
C2 Nb1 C2 72.59(18) 6_565 . ?
C1 Nb1 C5 73.99(11) . 6_565 ?
C4 Nb1 C5 73.80(13) . 6_565 ?
C2 Nb1 C5 140.59(14) 6_565 6_565 ?
C2 Nb1 C5 73.99(13) . 6_565 ?
C1 Nb1 C5 73.99(11) . . ?
C4 Nb1 C5 73.80(13) . . ?
C2 Nb1 C5 73.99(13) 6_565 . ?
C2 Nb1 C5 140.59(14) . . ?
C5 Nb1 C5 124.6(2) 6_565 . ?
C1 Nb1 C3 78.38(14) . . ?
C4 Nb1 C3 143.42(11) . . ?
C2 Nb1 C3 117.24(13) 6_565 . ?
C2 Nb1 C3 75.70(14) . . ?
C5 Nb1 C3 73.03(15) 6_565 . ?
C5 Nb1 C3 139.67(15) . . ?
C1 Nb1 C3 78.38(14) . 6_565 ?
C4 Nb1 C3 143.42(11) . 6_565 ?
C2 Nb1 C3 75.71(14) 6_565 6_565 ?
C2 Nb1 C3 117.24(13) . 6_565 ?
C5 Nb1 C3 139.67(15) 6_565 6_565 ?
C5 Nb1 C3 73.03(15) . 6_565 ?
C3 Nb1 C3 73.1(2) . 6_565 ?
N1 C1 Nb1 172.8(4) . . ?
C1 N1 Ni1 151.4(4) . . ?
N2 C2 Nb1 175.7(3) . . ?
C2 N2 Ni2 158.7(3) . . ?
N3 C3 Nb1 176.5(4) . . ?
N4 C4 Nb1 180.0(6) . . ?
N5 C5 Nb1 177.5(5) . . ?
N11 Ni1 N11 180.0 . 5_665 ?
N11 Ni1 N11 94.6(3) . 6_565 ?
N11 Ni1 N11 85.4(3) 5_665 6_565 ?
N11 Ni1 N11 85.4(3) . 2_655 ?
N11 Ni1 N11 94.6(3) 5_665 2_655 ?
N11 Ni1 N11 180.00(16) 6_565 2_655 ?
N11 Ni1 N1 88.80(12) . . ?
N11 Ni1 N1 91.20(12) 5_665 . ?
N11 Ni1 N1 88.80(12) 6_565 . ?
N11 Ni1 N1 91.20(12) 2_655 . ?
N11 Ni1 N1 91.20(12) . 5_665 ?
N11 Ni1 N1 88.80(12) 5_665 5_665 ?
N11 Ni1 N1 91.20(12) 6_565 5_665 ?
N11 Ni1 N1 88.80(12) 2_655 5_665 ?
N1 Ni1 N1 180.0 . 5_665 ?
N11 C11 C11 108.9(4) . 2_655 ?
N11 C11 H11A 109.9 . . ?
C11 C11 H11A 109.9 2_655 . ?
N11 C11 H11B 109.9 . . ?
C11 C11 H11B 109.9 2_655 . ?
H11A C11 H11B 108.3 . . ?
C11 N11 C12 114.5(4) . . ?
C11 N11 Ni1 105.0(3) . . ?
C12 N11 Ni1 115.2(3) . . ?
C11 N11 H11 107.2 . . ?
C12 N11 H11 107.2 . . ?
Ni1 N11 H11 107.2 . . ?
N11 C12 C13 113.0(5) . . ?
N11 C12 H12A 109.0 . . ?
C13 C12 H12A 109.0 . . ?
N11 C12 H12B 109.0 . . ?
C13 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C12 C13 C12 115.8(6) . 6_565 ?
C12 C13 H13A 108.3 . . ?
C12 C13 H13A 108.3 6_565 . ?
C12 C13 H13B 108.3 . . ?
C12 C13 H13B 108.3 6_565 . ?
H13A C13 H13B 107.4 . . ?
N22' Ni2 N22' 180.0 7_566 . ?
N22' Ni2 N21' 93.6(8) 7_566 . ?
N22' Ni2 N21' 86.4(8) . . ?
N21' Ni2 N21' 180.0(4) 7_566 . ?
N22 Ni2 N22 180.0 7_566 . ?
N22 Ni2 N21 94.4(3) 7_566 . ?
N22 Ni2 N21 85.6(3) . . ?
N22 Ni2 N21 85.6(3) 7_566 7_566 ?
N22 Ni2 N21 94.4(3) . 7_566 ?
N21 Ni2 N21 180.0(3) . 7_566 ?
N22 Ni2 N2 90.6(2) 7_566 7_566 ?
N22 Ni2 N2 89.4(2) . 7_566 ?
N21 Ni2 N2 92.3(2) . 7_566 ?
N21 Ni2 N2 87.7(2) 7_566 7_566 ?
N22' Ni2 N2 91.7(5) 7_566 . ?
N22' Ni2 N2 88.3(5) . . ?
N21' Ni2 N2 92.6(5) 7_566 . ?
N21' Ni2 N2 87.4(5) . . ?
N22 Ni2 N2 89.4(2) 7_566 . ?
N22 Ni2 N2 90.6(2) . . ?
N21 Ni2 N2 87.7(2) . . ?
N21 Ni2 N2 92.3(2) 7_566 . ?
N2 Ni2 N2 180.0 7_566 . ?
C25 C21 C22 116.6(7) 7_566 . ?
C25 C21 H21A 108.1 7_566 . ?
C22 C21 H21A 108.1 . . ?
C25 C21 H21B 108.1 7_566 . ?
C22 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
N21 C22 C21 112.1(10) . . ?
N21 C22 H22A 109.2 . . ?
C21 C22 H22A 109.2 . . ?
N21 C22 H22B 109.2 . . ?
C21 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C22 N21 C23 113.0(8) . . ?
C22 N21 Ni2 115.1(7) . . ?
C23 N21 Ni2 106.1(5) . . ?
C22 N21 H21 107.4 . . ?
C23 N21 H21 107.4 . . ?
Ni2 N21 H21 107.4 . . ?
N21 C23 C24 110.8(7) . . ?
N21 C23 H23A 109.5 . . ?
C24 C23 H23A 109.5 . . ?
N21 C23 H23B 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
N22 C24 C23 108.9(6) . . ?
N22 C24 H24A 109.9 . . ?
C23 C24 H24A 109.9 . . ?
N22 C24 H24B 109.9 . . ?
C23 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
C25 N22 C24 113.8(7) . . ?
C25 N22 Ni2 116.5(6) . . ?
C24 N22 Ni2 106.5(5) . . ?
C25 N22 H22 106.5 . . ?
C24 N22 H22 106.5 . . ?
Ni2 N22 H22 106.5 . . ?
N22 C25 C21 111.5(6) . 7_566 ?
N22 C25 H25A 109.3 . . ?
C21 C25 H25A 109.3 7_566 . ?
N22 C25 H25B 109.3 . . ?
C21 C25 H25B 109.3 7_566 . ?
H25A C25 H25B 108.0 . . ?
C25' C21' C22' 118(2) 7_566 . ?
C25' C21' H21C 107.7 7_566 . ?
C22' C21' H21C 107.7 . . ?
C25' C21' H21D 107.7 7_566 . ?
C22' C21' H21D 107.7 . . ?
H21C C21' H21D 107.1 . . ?
N21' C22' C21' 112(2) . . ?
N21' C22' H22C 109.2 . . ?
C21' C22' H22C 109.2 . . ?
N21' C22' H22D 109.2 . . ?
C21' C22' H22D 109.2 . . ?
H22C C22' H22D 107.9 . . ?
C23' N21' C22' 114.4(17) . . ?
C23' N21' Ni2 106.1(15) . . ?
C22' N21' Ni2 116.9(16) . . ?
C23' N21' H21' 106.2 . . ?
C22' N21' H21' 106.2 . . ?
Ni2 N21' H21' 106.2 . . ?
N21' C23' C24' 110.3(18) . . ?
N21' C23' H23C 109.6 . . ?
C24' C23' H23C 109.6 . . ?
N21' C23' H23D 109.6 . . ?
C24' C23' H23D 109.6 . . ?
H23C C23' H23D 108.1 . . ?
N22' C24' C23' 107.6(17) . . ?
N22' C24' H24C 110.2 . . ?
C23' C24' H24C 110.2 . . ?
N22' C24' H24D 110.2 . . ?
C23' C24' H24D 110.2 . . ?
H24C C24' H24D 108.5 . . ?
C25' N22' C24' 110.5(18) . . ?
C25' N22' Ni2 118.2(16) . . ?
C24' N22' Ni2 105.4(14) . . ?
C25' N22' H22' 107.4 . . ?
C24' N22' H22' 107.4 . . ?
Ni2 N22' H22' 107.4 . . ?
N22' C25' H25C 110.0 . . ?
C21' C25' H25C 110.0 7_566 . ?
N22' C25' H25D 110.0 . . ?
C21' C25' H25D 110.0 7_566 . ?
H25C C25' H25D 108.4 . . ?
O1 Li1 O4 116.6(11) . . ?
O1 Li1 O3 107.7(10) . . ?
O4 Li1 O3 113.0(9) . . ?
O1 Li1 O2 110.1(9) . . ?
O4 Li1 O2 99.4(9) . . ?
O3 Li1 O2 109.8(10) . . ?
O1 Li1 H1D 20.5 . . ?
O4 Li1 H1D 137.0 . . ?
O3 Li1 H1D 93.2 . . ?
O2 Li1 H1D 103.0 . . ?
O1 Li1 H3D 85.7 . . ?
O4 Li1 H3D 126.3 . . ?
O3 Li1 H3D 22.0 . . ?
O2 Li1 H3D 118.7 . . ?
H1D Li1 H3D 71.8 . . ?
O1 Li1 H4D 128.2 . . ?
O4 Li1 H4D 21.0 . . ?
O3 Li1 H4D 116.9 . . ?
O2 Li1 H4D 78.7 . . ?
H1D Li1 H4D 147.6 . . ?
H3D Li1 H4D 136.2 . . ?
Li1 O1 H1C 116.5 . . ?
Li1 O1 H1D 107.7 . . ?
H1C O1 H1D 108.3 . . ?
Li1 O2 Li1 127.6(12) 6_575 . ?
Li1 O2 H2A 105.3 6_575 . ?
Li1 O2 H2A 105.3 . . ?
Li1 O2 H2B 105.5 6_575 . ?
Li1 O2 H2B 105.5 . . ?
H2A O2 H2B 106.1 . . ?
Li1 O3 H3C 111.9 . . ?
Li1 O3 H3D 98.7 . . ?
H3C O3 H3D 112.0 . . ?
Li1 O4 H4C 141.5 . . ?
Li1 O4 H4D 104.9 . . ?
H4C O4 H4D 108.8 . . ?
H5C O5 H5C 98.2 . 2_656 ?
H6C O6 H6D 83.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N11 H11 N3 1.00 2.62 3.528(5) 150.4 .
C24 H24A N3 0.99 2.68 3.530(9) 144.2 .
C21' H21D N5 0.99 2.65 3.64(3) 176.7 6_565
C23' H23C O3 0.99 2.64 3.34(3) 127.8 .
N22' H22' O3 1.00 2.59 3.347(18) 132.4 .
C25' H25D N2 0.99 2.61 3.12(3) 112.1 .
O1 H1C O6 0.84 2.01 2.842(8) 171.8 2_657
O2 H2B N4 0.84 2.18 2.781(8) 128.0 7_566
O3 H3C N4 0.84 2.18 2.929(5) 148.1 7_566
O4 H4C O6 0.84 1.87 2.701(6) 170.7 .
O5 H5C N3 0.84 1.99 2.816(4) 169.2 2_656
O6 H6C O5 0.84 1.89 2.729(5) 177.9 .

_refine_diff_density_max         0.748
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.090




####################################################################### 
# 
# 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_6Ba
_database_code_depnum_ccdc_archive 'CCDC 2058273'
loop_
_audit_author_name
_audit_author_address
'Michal Heczko'
;Jagiellonian University in Cracow
Poland
;
_audit_update_record             
;
2021-03-24 deposited with the CCDC.	2021-04-15 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            'C46 H121 Ba N28 Nb2 Ni3 O24.50'
_chemical_formula_weight         1957.99

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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   20.1987(6)
_cell_length_b                   15.7904(4)
_cell_length_c                   26.4099(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.1660(10)
_cell_angle_gamma                90
_cell_volume                     8389.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    12292
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      25.11

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_F_000             4044
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.467
_shelx_estimated_absorpt_T_min   0.758
_shelx_estimated_absorpt_T_max   0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6595
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            81022
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.317
_diffrn_reflns_theta_max         25.108
_diffrn_reflns_theta_full        25.108
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             14788
_reflns_number_gt                10278
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0236P)²+101.6155P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14788
_refine_ls_number_parameters     950
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.1497
_refine_ls_wR_factor_gt          0.1355
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.006
_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 0.75072(5) 0.25477(7) 0.25153(4) 0.0137(2) Uani 1 1 d . . . . .
Ni2 Ni 1.0000 0.5000 0.0000 0.0143(3) Uani 1 2 d S . P . .
Ni3 Ni 1.0000 0.0000 0.0000 0.0118(3) Uani 1 2 d S . P . .
Ni4 Ni 0.5000 0.5000 0.5000 0.0119(3) Uani 1 2 d S . P . .
Ni5 Ni 0.5000 0.0000 0.5000 0.0121(3) Uani 1 2 d S . P . .
Nb1 Nb 0.86342(3) 0.25109(5) 0.08005(3) 0.01111(17) Uani 1 1 d . . . . .
Nb2 Nb 0.64095(4) 0.25012(5) 0.42249(3) 0.01095(17) Uani 1 1 d . . . . .
Ba1 Ba 0.71774(3) 0.30062(3) 0.63974(2) 0.01563(13) Uani 1 1 d . . . . .
C1 C 0.7915(4) 0.2517(5) 0.1396(3) 0.0176(18) Uani 1 1 d . . . . .
C1A C 0.7135(4) 0.2525(5) 0.3639(3) 0.0136(17) Uani 1 1 d . . . . .
C2 C 0.9254(4) 0.3381(6) 0.0366(3) 0.019(2) Uani 1 1 d . . . . .
C2A C 0.5973(4) 0.3431(5) 0.3641(3) 0.0141(18) Uani 1 1 d . . . . .
C3 C 0.9316(4) 0.1676(5) 0.0395(3) 0.0121(18) Uani 1 1 d . . . . .
C3A C 0.6984(4) 0.3730(5) 0.4343(3) 0.0155(19) Uani 1 1 d . . . . .
C4 C 0.9114(4) 0.1637(6) 0.1415(3) 0.0169(19) Uani 1 1 d . . . . .
C4A C 0.5763(4) 0.3356(5) 0.4663(3) 0.0131(18) Uani 1 1 d . . . . .
C5 C 0.8096(4) 0.1265(6) 0.0706(3) 0.018(2) Uani 1 1 d . . . . .
C5A C 0.5774(4) 0.1661(5) 0.4667(3) 0.0106(17) Uani 1 1 d . . . . .
C6 C 0.8107(4) 0.3763(6) 0.0759(3) 0.020(2) Uani 1 1 d . . . . .
C6A C 0.7012(4) 0.2405(5) 0.4973(3) 0.0140(17) Uani 1 1 d . U . . .
C7 C 0.8082(4) 0.2562(6) 0.0024(4) 0.025(2) Uani 1 1 d . . . . .
C7A C 0.6850(5) 0.1189(6) 0.4211(3) 0.021(2) Uani 1 1 d . . . . .
C8 C 0.9180(4) 0.3346(6) 0.1388(3) 0.019(2) Uani 1 1 d . . . . .
C8A C 0.5825(4) 0.1755(5) 0.3593(3) 0.017(2) Uani 1 1 d . . . . .
C11 C 0.8751(5) 0.1681(7) 0.2969(4) 0.032(3) Uani 1 1 d . . . . .
H11A H 0.9054 0.1189 0.2961 0.039 Uiso 1 1 calc R U . . .
H11B H 0.8597 0.1715 0.3314 0.039 Uiso 1 1 calc R U . . .
C12 C 0.9139(5) 0.2503(7) 0.2861(4) 0.034(2) Uani 1 1 d . . . . .
H12A H 0.9573 0.2492 0.3068 0.041 Uiso 1 1 calc R U . . .
H12B H 0.9229 0.2505 0.2499 0.041 Uiso 1 1 calc R U . . .
C13 C 0.8789(5) 0.3303(7) 0.2972(4) 0.030(2) Uani 1 1 d . . . . .
H13A H 0.8624 0.3261 0.3313 0.036 Uiso 1 1 calc R U . . .
H13B H 0.9109 0.3779 0.2980 0.036 Uiso 1 1 calc R U . . .
C14 C 0.7863(5) 0.4264(6) 0.2702(4) 0.032(3) Uani 1 1 d . . . . .
H14A H 0.8140 0.4767 0.2647 0.038 Uiso 1 1 calc R U . . .
H14B H 0.7758 0.4263 0.3061 0.038 Uiso 1 1 calc R U . . .
C15 C 0.7224(5) 0.4298(6) 0.2351(4) 0.033(3) Uani 1 1 d . . . . .
H15A H 0.6973 0.4819 0.2416 0.040 Uiso 1 1 calc R U . . .
H15B H 0.7329 0.4303 0.1992 0.040 Uiso 1 1 calc R U . . .
C16 C 0.6246(5) 0.3420(6) 0.2069(3) 0.028(2) Uani 1 1 d . . . . .
H16A H 0.6403 0.3395 0.1725 0.033 Uiso 1 1 calc R U . . .
H16B H 0.5945 0.3913 0.2080 0.033 Uiso 1 1 calc R U . . .
C17 C 0.5866(4) 0.2631(6) 0.2159(3) 0.024(2) Uani 1 1 d . . . . .
H17A H 0.5442 0.2650 0.1940 0.029 Uiso 1 1 calc R U . . .
H17B H 0.5753 0.2635 0.2516 0.029 Uiso 1 1 calc R U . . .
C18 C 0.6210(4) 0.1788(6) 0.2063(3) 0.027(2) Uani 1 1 d . . . . .
H18A H 0.5883 0.1322 0.2071 0.032 Uiso 1 1 calc R U . . .
H18B H 0.6372 0.1798 0.1720 0.032 Uiso 1 1 calc R U . . .
C19 C 0.7130(5) 0.0817(6) 0.2371(4) 0.028(2) Uani 1 1 d . . . . .
H19A H 0.7226 0.0766 0.2011 0.034 Uiso 1 1 calc R U . . .
H19B H 0.6847 0.0333 0.2452 0.034 Uiso 1 1 calc R U . . .
C20 C 0.7762(5) 0.0797(6) 0.2705(4) 0.034(3) Uani 1 1 d . . . . .
H20A H 0.8009 0.0270 0.2644 0.041 Uiso 1 1 calc R U . . .
H20B H 0.7666 0.0805 0.3066 0.041 Uiso 1 1 calc R U . . .
C21 C 1.0854(8) 0.4562(12) 0.0876(6) 0.108(8) Uani 1 1 d . . . . .
H21A H 1.0602 0.4061 0.0976 0.129 Uiso 1 1 calc R U . . .
H21B H 1.1303 0.4540 0.1059 0.129 Uiso 1 1 calc R U . . .
C22 C 1.1107(7) 0.3707(9) 0.0094(6) 0.066(4) Uani 1 1 d . U . . .
H22A H 1.1556 0.3550 0.0246 0.079 Uiso 1 1 calc R U . . .
H22B H 1.0795 0.3261 0.0187 0.079 Uiso 1 1 calc R U . . .
C23 C 1.1110(8) 0.3727(11) -0.0449(6) 0.080(5) Uani 1 1 d . U . . .
H23A H 1.1346 0.3214 -0.0551 0.096 Uiso 1 1 calc R U . . .
H23B H 1.1379 0.4221 -0.0536 0.096 Uiso 1 1 calc R U . . .
C24 C 1.0484(10) 0.3770(8) -0.0761(6) 0.099(7) Uani 1 1 d . . . . .
H24A H 1.0564 0.3657 -0.1119 0.119 Uiso 1 1 calc R U . . .
H24B H 1.0185 0.3321 -0.0652 0.119 Uiso 1 1 calc R U . . .
C25 C 0.9485(8) 0.4667(11) -0.1011(5) 0.075(4) Uani 1 1 d . U . . .
H25A H 0.9532 0.4664 -0.1381 0.090 Uiso 1 1 calc R U . . .
H25B H 0.9215 0.4169 -0.0931 0.090 Uiso 1 1 calc R U . . .
C31 C 1.0376(6) -0.0152(8) 0.1046(4) 0.052(3) Uani 1 1 d . . . . .
H31A H 1.0168 0.0377 0.1157 0.062 Uiso 1 1 calc R U . . .
H31B H 1.0700 -0.0342 0.1326 0.062 Uiso 1 1 calc R U . . .
C32 C 1.1149(6) 0.0733(9) 0.0649(5) 0.055(4) Uani 1 1 d . . . . .
H32A H 1.1513 0.0625 0.0918 0.066 Uiso 1 1 calc R U . . .
H32B H 1.0901 0.1235 0.0754 0.066 Uiso 1 1 calc R U . . .
C33 C 1.1448(7) 0.0942(8) 0.0169(5) 0.059(4) Uani 1 1 d . . . . .
H33A H 1.1698 0.0434 0.0077 0.071 Uiso 1 1 calc R U . . .
H33B H 1.1781 0.1392 0.0254 0.071 Uiso 1 1 calc R U . . .
C34 C 1.1033(6) 0.1229(7) -0.0319(6) 0.064(4) Uani 1 1 d . . . . .
H34A H 1.0759 0.1727 -0.0247 0.077 Uiso 1 1 calc R U . . .
H34B H 1.1330 0.1389 -0.0582 0.077 Uiso 1 1 calc R U . . .
C35 C 1.0170(6) 0.0837(8) -0.0950(4) 0.048(3) Uani 1 1 d . . . . .
H35A H 1.0426 0.0894 -0.1251 0.058 Uiso 1 1 calc R U . . .
H35B H 0.9968 0.1392 -0.0883 0.058 Uiso 1 1 calc R U . . .
C41 C 0.5475(4) 0.5212(6) 0.6042(3) 0.022(2) Uani 1 1 d . . . . .
H41A H 0.5213 0.5724 0.6109 0.026 Uiso 1 1 calc R U . . .
H41B H 0.5836 0.5154 0.6319 0.026 Uiso 1 1 calc R U . . .
C42 C 0.5030(5) 0.4435(6) 0.6026(3) 0.026(2) Uani 1 1 d . . . . .
H42A H 0.5300 0.3920 0.5985 0.031 Uiso 1 1 calc R U . . .
H42B H 0.4819 0.4386 0.6348 0.031 Uiso 1 1 calc R U . . .
C43 C 0.4145(5) 0.3720(6) 0.5482(4) 0.026(2) Uani 1 1 d . . . . .
H43A H 0.3922 0.3547 0.5784 0.031 Uiso 1 1 calc R U . . .
H43B H 0.4462 0.3267 0.5409 0.031 Uiso 1 1 calc R U . . .
C44 C 0.3624(4) 0.3812(6) 0.5028(4) 0.027(2) Uani 1 1 d . . . . .
H44A H 0.3350 0.4318 0.5082 0.032 Uiso 1 1 calc R U . . .
H44B H 0.3327 0.3312 0.5018 0.032 Uiso 1 1 calc R U . . .
C45 C 0.3907(5) 0.3895(6) 0.4509(4) 0.025(2) Uani 1 1 d . . . . .
H45A H 0.4228 0.3431 0.4469 0.030 Uiso 1 1 calc R U . . .
H45B H 0.3541 0.3838 0.4235 0.030 Uiso 1 1 calc R U . . .
C51 C 0.5052(5) 0.0436(6) 0.6049(3) 0.027(2) Uani 1 1 d . . . . .
H51A H 0.4844 0.0427 0.6375 0.032 Uiso 1 1 calc R U . . .
H51B H 0.5312 0.0965 0.6036 0.032 Uiso 1 1 calc R U . . .
C52 C 0.4161(5) 0.1214(6) 0.5536(4) 0.031(3) Uani 1 1 d . . . . .
H52A H 0.4478 0.1671 0.5471 0.038 Uiso 1 1 calc R U . . .
H52B H 0.3950 0.1361 0.5849 0.038 Uiso 1 1 calc R U . . .
C53 C 0.3630(5) 0.1168(6) 0.5095(4) 0.031(3) Uani 1 1 d . . . . .
H53A H 0.3332 0.1663 0.5114 0.037 Uiso 1 1 calc R U . . .
H53B H 0.3361 0.0653 0.5134 0.037 Uiso 1 1 calc R U . . .
C54 C 0.3888(5) 0.1152(6) 0.4566(4) 0.029(2) Uani 1 1 d . . . . .
H54A H 0.3510 0.1230 0.4304 0.034 Uiso 1 1 calc R U . . .
H54B H 0.4202 0.1627 0.4536 0.034 Uiso 1 1 calc R U . . .
C55 C 0.4497(5) 0.0313(6) 0.3978(3) 0.025(2) Uani 1 1 d . . . . .
H55A H 0.4748 0.0840 0.3925 0.030 Uiso 1 1 calc R U . . .
H55B H 0.4129 0.0273 0.3705 0.030 Uiso 1 1 calc R U . . .
N1 N 0.7596(3) 0.2528(5) 0.1736(3) 0.0214(16) Uani 1 1 d . . . . .
N1A N 0.7443(3) 0.2544(5) 0.3297(3) 0.0174(16) Uani 1 1 d . . . . .
N2 N 0.9550(4) 0.3870(5) 0.0156(3) 0.0198(17) Uani 1 1 d . . . . .
N2A N 0.5795(4) 0.3918(5) 0.3325(3) 0.0232(18) Uani 1 1 d . . . . .
N3 N 0.9639(3) 0.1190(4) 0.0211(3) 0.0161(16) Uani 1 1 d . . . . .
N3A N 0.7253(4) 0.4370(5) 0.4403(3) 0.0236(18) Uani 1 1 d . . . . .
N4 N 0.9326(4) 0.1173(5) 0.1718(3) 0.0224(18) Uani 1 1 d . . . . .
N4A N 0.5454(3) 0.3831(4) 0.4873(2) 0.0142(16) Uani 1 1 d . . . . .
N5 N 0.7854(4) 0.0610(5) 0.0684(3) 0.0278(19) Uani 1 1 d . . . . .
N5A N 0.5466(3) 0.1197(4) 0.4890(3) 0.0162(16) Uani 1 1 d . . . . .
N6 N 0.7855(4) 0.4416(5) 0.0759(4) 0.035(2) Uani 1 1 d . . . . .
N6A N 0.7296(3) 0.2355(4) 0.5379(3) 0.0203(17) Uani 1 1 d . . . . .
N7 N 0.7808(4) 0.2631(7) -0.0374(3) 0.045(3) Uani 1 1 d . . . . .
N7A N 0.7053(4) 0.0510(5) 0.4162(3) 0.0275(19) Uani 1 1 d . . . . .
N8 N 0.9441(4) 0.3810(5) 0.1688(3) 0.031(2) Uani 1 1 d . . . . .
N8A N 0.5584(4) 0.1345(5) 0.3275(3) 0.0223(17) Uani 1 1 d . . . . .
N11 N 0.8175(4) 0.1552(5) 0.2594(3) 0.0241(18) Uani 1 1 d . . . . .
H11 H 0.8348 0.1457 0.2255 0.029 Uiso 1 1 calc R U . . .
N12 N 0.8225(4) 0.3487(5) 0.2593(3) 0.0206(17) Uani 1 1 d . . . . .
H12 H 0.8406 0.3562 0.2255 0.025 Uiso 1 1 calc R U . . .
N13 N 0.6824(4) 0.3544(4) 0.2449(3) 0.0195(17) Uani 1 1 d . . . . .
H13 H 0.6649 0.3622 0.2788 0.023 Uiso 1 1 calc R U . . .
N14 N 0.6777(3) 0.1621(5) 0.2447(3) 0.0200(17) Uani 1 1 d . . . . .
H14 H 0.6590 0.1580 0.2784 0.024 Uiso 1 1 calc R U . . .
N21 N 1.0906(4) 0.4550(6) 0.0324(4) 0.053(3) Uani 1 1 d . . . . .
H21 H 1.1251 0.4976 0.0252 0.064 Uiso 1 1 calc R U . . .
N22 N 1.0149(5) 0.4607(6) -0.0729(3) 0.047(2) Uani 1 1 d . U . . .
H22 H 1.0439 0.5038 -0.0877 0.057 Uiso 1 1 calc R U . . .
N31 N 1.0711(5) 0.0023(6) 0.0624(4) 0.049(3) Uani 1 1 d . . . . .
H31 H 1.1001 -0.0482 0.0581 0.058 Uiso 1 1 calc R U . . .
N32 N 1.0622(5) 0.0553(6) -0.0492(4) 0.057(3) Uani 1 1 d . . . . .
H32 H 1.0916 0.0097 -0.0609 0.069 Uiso 1 1 calc R U . . .
N41 N 0.5760(3) 0.5291(4) 0.5545(3) 0.0165(16) Uani 1 1 d . . . . .
H41 H 0.6105 0.4840 0.5533 0.020 Uiso 1 1 calc R U . . .
N42 N 0.4510(4) 0.4504(4) 0.5595(3) 0.0172(16) Uani 1 1 d . . . . .
H42 H 0.4182 0.4939 0.5688 0.021 Uiso 1 1 calc R U . . .
N51 N 0.4528(4) 0.0414(4) 0.5619(3) 0.0187(17) Uani 1 1 d . . . . .
H51 H 0.4200 -0.0031 0.5696 0.022 Uiso 1 1 calc R U . . .
N52 N 0.4227(4) 0.0343(5) 0.4474(3) 0.0201(17) Uani 1 1 d . . . . .
H52 H 0.3884 -0.0114 0.4474 0.024 Uiso 1 1 calc R U . . .
O1 O 0.6110(3) 0.3631(4) 0.6896(2) 0.0227(14) Uani 1 1 d . . . . .
O2 O 0.5971(3) 0.2464(4) 0.5927(2) 0.0219(13) Uani 1 1 d . . . . .
O3 O 0.7472(4) -0.2972(5) 0.2447(2) 0.049(2) Uani 1 1 d . . . . .
O4 O 0.6897(3) 0.1308(4) 0.6742(3) 0.0353(17) Uani 1 1 d . . . . .
O5 O 0.8312(4) 0.2082(5) 0.6502(3) 0.048(2) Uani 1 1 d . . . . .
O6 O 0.8067(3) 0.4308(4) 0.6594(3) 0.0364(18) Uani 1 1 d . . . . .
O7 O 0.7014(3) 0.4217(3) 0.5633(2) 0.0157(13) Uani 1 1 d . . . . .
O10 O 0.0000 0.4753(6) 0.2500 0.034(2) Uani 1 2 d S T P . .
O11 O 0.9066(3) 0.4007(4) 0.7368(3) 0.0366(18) Uani 1 1 d . . . . .
O12 O 0.7557(3) 0.4045(4) 0.8959(2) 0.0299(16) Uani 1 1 d . . . . .
O13 O 0.6636(4) 0.6428(4) 0.3164(3) 0.0427(19) Uani 1 1 d . . . . .
O14 O 0.6229(3) 0.8067(5) 0.3222(2) 0.0355(17) Uani 1 1 d . . . . .
O15 O 0.5668(3) 0.5370(4) 0.2704(2) 0.0310(16) Uani 1 1 d . . . . .
O16 O 1.0000 -0.0174(5) 0.7500 0.026(2) Uani 1 2 d S T P . .
O17 O 0.8278(4) 0.0313(5) 0.6642(3) 0.052(2) Uani 1 1 d . . . . .
O18 O 0.6975(3) 0.0704(4) 0.5788(3) 0.0274(16) Uani 1 1 d . . . . .
O19 O 0.5129(3) 0.2370(4) 0.6695(2) 0.0292(16) Uani 1 1 d . . . . .
O20 O 0.4199(3) -0.1148(4) 0.2702(2) 0.0308(16) Uani 1 1 d . . . . .
O21 O 0.5000 0.0239(5) 0.2500 0.0199(19) Uani 1 2 d S T P . .
O22 O 0.9509(4) 0.2518(5) 0.6960(3) 0.055(2) Uani 1 1 d . . . . .
O23 O 0.9119(4) 0.1156(6) 0.7581(4) 0.071(3) Uani 1 1 d . . . . .
O24 O 0.7763(5) -0.1339(5) 0.2656(4) 0.067(3) Uani 1 1 d . . . . .
O26 O 0.9246(5) 0.2341(6) 0.8409(4) 0.083(3) Uani 1 1 d . . . . .
O27 O 0.8435(5) -0.1495(6) 0.4037(4) 0.077(3) Uani 1 1 d . . . . .
O28 O 0.8394(5) 0.3636(6) 0.8200(4) 0.074(3) Uani 1 1 d . . . . .
O30 O 0.7297(4) -0.0972(6) 0.3616(4) 0.076(3) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N11 2.069(8) . ?
Ni1 N12 2.071(7) . ?
Ni1 N14 2.074(7) . ?
Ni1 N1A 2.081(7) . ?
Ni1 N1 2.081(7) . ?
Ni1 N13 2.089(7) . ?
Ni2 N2 2.062(7) 3_765 ?
Ni2 N2 2.062(7) . ?
Ni2 N22 2.071(9) 3_765 ?
Ni2 N22 2.071(9) . ?
Ni2 N21 2.074(8) . ?
Ni2 N21 2.074(8) 3_765 ?
Ni3 N32 2.080(10) 3_755 ?
Ni3 N32 2.080(10) . ?
Ni3 N31 2.087(10) . ?
Ni3 N31 2.087(10) 3_755 ?
Ni3 N3 2.109(7) 3_755 ?
Ni3 N3 2.109(7) . ?
Ni4 N41 2.060(7) 3_666 ?
Ni4 N41 2.060(7) . ?
Ni4 N42 2.083(7) . ?
Ni4 N42 2.083(7) 3_666 ?
Ni4 N4A 2.101(7) 3_666 ?
Ni4 N4A 2.101(7) . ?
Ni5 N52 2.067(7) . ?
Ni5 N52 2.067(7) 3_656 ?
Ni5 N51 2.071(7) 3_656 ?
Ni5 N51 2.071(7) . ?
Ni5 N5A 2.142(7) 3_656 ?
Ni5 N5A 2.142(7) . ?
Nb1 C1 2.235(8) . ?
Nb1 C2 2.243(9) . ?
Nb1 C6 2.244(9) . ?
Nb1 C3 2.247(8) . ?
Nb1 C7 2.246(10) . ?
Nb1 C8 2.249(9) . ?
Nb1 C5 2.252(9) . ?
Nb1 C4 2.279(9) . ?
Nb2 C1A 2.225(8) . ?
Nb2 C6A 2.231(9) . ?
Nb2 C5A 2.244(8) . ?
Nb2 C2A 2.252(9) . ?
Nb2 C7A 2.256(9) . ?
Nb2 C4A 2.267(9) . ?
Nb2 C3A 2.268(9) . ?
Nb2 C8A 2.282(9) . ?
Ba1 O5 2.710(7) . ?
Ba1 O6 2.749(7) . ?
Ba1 O2 2.769(6) . ?
Ba1 O7 2.779(5) . ?
Ba1 O3 2.783(7) 4_556 ?
Ba1 O1 2.805(6) . ?
Ba1 O4 2.903(7) . ?
Ba1 N6A 2.908(7) . ?
C1 N1 1.153(10) . ?
C1A N1A 1.142(10) . ?
C2 N2 1.148(11) . ?
C2A N2A 1.166(11) . ?
C3 N3 1.143(10) . ?
C3A N3A 1.152(11) . ?
C4 N4 1.139(11) . ?
C4A N4A 1.151(10) . ?
C5 N5 1.143(11) . ?
C5A N5A 1.158(10) . ?
C6 N6 1.149(11) . ?
C6A N6A 1.173(10) . ?
C7 N7 1.149(12) . ?
C7A N7A 1.161(11) . ?
C8 N8 1.168(11) . ?
C8A N8A 1.136(11) . ?
C11 N11 1.474(12) . ?
C11 C12 1.555(14) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.490(14) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N12 1.478(12) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N12 1.470(12) . ?
C14 C15 1.520(14) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N13 1.474(11) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N13 1.483(12) . ?
C16 C17 1.493(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.533(13) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 N14 1.484(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 N14 1.479(11) . ?
C19 C20 1.484(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 N11 1.499(12) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C25 1.46(2) 3_765 ?
C21 N21 1.47(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.435(19) . ?
C22 N21 1.533(16) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.45(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N22 1.491(17) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C21 1.46(2) 3_765 ?
C25 N22 1.478(17) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C31 N31 1.384(14) . ?
C31 C35 1.550(17) 3_755 ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 N31 1.426(15) . ?
C32 C33 1.490(17) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.541(18) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 N32 1.402(15) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 N32 1.515(15) . ?
C35 C31 1.550(17) 3_755 ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C41 N41 1.486(10) . ?
C41 C42 1.518(13) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 N42 1.482(11) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 N42 1.458(11) . ?
C43 C44 1.529(13) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.538(13) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 N41 1.462(11) 3_666 ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C51 N51 1.481(11) . ?
C51 C55 1.499(14) 3_656 ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 N51 1.471(11) . ?
C52 C53 1.512(14) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.534(13) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 N52 1.480(12) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 N52 1.464(11) . ?
C55 C51 1.499(14) 3_656 ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
N11 H11 1.0000 . ?
N12 H12 1.0000 . ?
N13 H13 1.0000 . ?
N14 H14 1.0000 . ?
N21 H21 1.0000 . ?
N22 H22 1.0000 . ?
N31 H31 1.0000 . ?
N32 H32 1.0000 . ?
N41 C45 1.463(11) 3_666 ?
N41 H41 1.0000 . ?
N42 H42 1.0000 . ?
N51 H51 1.0000 . ?
N52 H52 1.0000 . ?
O3 Ba1 2.783(7) 4 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N11 Ni1 N12 95.2(3) . . ?
N11 Ni1 N14 85.7(3) . . ?
N12 Ni1 N14 178.8(3) . . ?
N11 Ni1 N1A 89.8(3) . . ?
N12 Ni1 N1A 90.6(3) . . ?
N14 Ni1 N1A 88.7(3) . . ?
N11 Ni1 N1 88.5(3) . . ?
N12 Ni1 N1 89.2(3) . . ?
N14 Ni1 N1 91.6(3) . . ?
N1A Ni1 N1 178.3(3) . . ?
N11 Ni1 N13 178.9(3) . . ?
N12 Ni1 N13 85.4(3) . . ?
N14 Ni1 N13 93.7(3) . . ?
N1A Ni1 N13 89.2(3) . . ?
N1 Ni1 N13 92.5(3) . . ?
N2 Ni2 N2 180.0 3_765 . ?
N2 Ni2 N22 91.7(3) 3_765 3_765 ?
N2 Ni2 N22 88.3(3) . 3_765 ?
N2 Ni2 N22 88.3(3) 3_765 . ?
N2 Ni2 N22 91.7(3) . . ?
N22 Ni2 N22 180.0 3_765 . ?
N2 Ni2 N21 89.5(3) 3_765 . ?
N2 Ni2 N21 90.5(3) . . ?
N22 Ni2 N21 85.2(4) 3_765 . ?
N22 Ni2 N21 94.8(4) . . ?
N2 Ni2 N21 90.5(3) 3_765 3_765 ?
N2 Ni2 N21 89.5(3) . 3_765 ?
N22 Ni2 N21 94.8(4) 3_765 3_765 ?
N22 Ni2 N21 85.2(4) . 3_765 ?
N21 Ni2 N21 180.0 . 3_765 ?
N32 Ni3 N32 180.0 3_755 . ?
N32 Ni3 N31 85.7(4) 3_755 . ?
N32 Ni3 N31 94.3(4) . . ?
N32 Ni3 N31 94.3(4) 3_755 3_755 ?
N32 Ni3 N31 85.7(4) . 3_755 ?
N31 Ni3 N31 180.0 . 3_755 ?
N32 Ni3 N3 91.9(3) 3_755 3_755 ?
N32 Ni3 N3 88.1(3) . 3_755 ?
N31 Ni3 N3 89.7(3) . 3_755 ?
N31 Ni3 N3 90.3(3) 3_755 3_755 ?
N32 Ni3 N3 88.1(3) 3_755 . ?
N32 Ni3 N3 91.9(3) . . ?
N31 Ni3 N3 90.3(3) . . ?
N31 Ni3 N3 89.7(3) 3_755 . ?
N3 Ni3 N3 180.0 3_755 . ?
N41 Ni4 N41 180.0 3_666 . ?
N41 Ni4 N42 93.9(3) 3_666 . ?
N41 Ni4 N42 86.1(3) . . ?
N41 Ni4 N42 86.1(3) 3_666 3_666 ?
N41 Ni4 N42 93.9(3) . 3_666 ?
N42 Ni4 N42 180.0 . 3_666 ?
N41 Ni4 N4A 90.0(3) 3_666 3_666 ?
N41 Ni4 N4A 90.0(3) . 3_666 ?
N42 Ni4 N4A 88.1(3) . 3_666 ?
N42 Ni4 N4A 91.9(3) 3_666 3_666 ?
N41 Ni4 N4A 90.0(3) 3_666 . ?
N41 Ni4 N4A 90.0(3) . . ?
N42 Ni4 N4A 91.9(3) . . ?
N42 Ni4 N4A 88.1(3) 3_666 . ?
N4A Ni4 N4A 180.00(17) 3_666 . ?
N52 Ni5 N52 180.0 . 3_656 ?
N52 Ni5 N51 85.7(3) . 3_656 ?
N52 Ni5 N51 94.3(3) 3_656 3_656 ?
N52 Ni5 N51 94.3(3) . . ?
N52 Ni5 N51 85.7(3) 3_656 . ?
N51 Ni5 N51 180.0 3_656 . ?
N52 Ni5 N5A 90.5(3) . 3_656 ?
N52 Ni5 N5A 89.5(3) 3_656 3_656 ?
N51 Ni5 N5A 93.9(3) 3_656 3_656 ?
N51 Ni5 N5A 86.1(3) . 3_656 ?
N52 Ni5 N5A 89.5(3) . . ?
N52 Ni5 N5A 90.5(3) 3_656 . ?
N51 Ni5 N5A 86.1(3) 3_656 . ?
N51 Ni5 N5A 93.9(3) . . ?
N5A Ni5 N5A 180.00(17) 3_656 . ?
C1 Nb1 C2 141.8(3) . . ?
C1 Nb1 C6 72.2(3) . . ?
C2 Nb1 C6 73.7(3) . . ?
C1 Nb1 C3 143.5(3) . . ?
C2 Nb1 C3 73.8(3) . . ?
C6 Nb1 C3 143.4(3) . . ?
C1 Nb1 C7 110.0(3) . . ?
C2 Nb1 C7 76.4(3) . . ?
C6 Nb1 C7 74.3(3) . . ?
C3 Nb1 C7 82.0(3) . . ?
C1 Nb1 C8 79.7(3) . . ?
C2 Nb1 C8 74.5(3) . . ?
C6 Nb1 C8 73.6(3) . . ?
C3 Nb1 C8 112.9(3) . . ?
C7 Nb1 C8 141.4(3) . . ?
C1 Nb1 C5 75.2(3) . . ?
C2 Nb1 C5 139.8(3) . . ?
C6 Nb1 C5 122.8(3) . . ?
C3 Nb1 C5 75.2(3) . . ?
C7 Nb1 C5 74.6(3) . . ?
C8 Nb1 C5 142.3(3) . . ?
C1 Nb1 C4 76.3(3) . . ?
C2 Nb1 C4 121.0(3) . . ?
C6 Nb1 C4 137.5(3) . . ?
C3 Nb1 C4 75.2(3) . . ?
C7 Nb1 C4 144.7(3) . . ?
C8 Nb1 C4 73.3(3) . . ?
C5 Nb1 C4 73.7(3) . . ?
C1A Nb2 C6A 106.1(3) . . ?
C1A Nb2 C5A 144.6(3) . . ?
C6A Nb2 C5A 77.9(3) . . ?
C1A Nb2 C2A 75.8(3) . . ?
C6A Nb2 C2A 143.1(3) . . ?
C5A Nb2 C2A 122.3(3) . . ?
C1A Nb2 C7A 73.7(3) . . ?
C6A Nb2 C7A 76.5(3) . . ?
C5A Nb2 C7A 73.2(3) . . ?
C2A Nb2 C7A 135.9(3) . . ?
C1A Nb2 C4A 142.2(3) . . ?
C6A Nb2 C4A 83.2(3) . . ?
C5A Nb2 C4A 72.8(3) . . ?
C2A Nb2 C4A 75.7(3) . . ?
C7A Nb2 C4A 143.2(3) . . ?
C1A Nb2 C3A 73.7(3) . . ?
C6A Nb2 C3A 72.9(3) . . ?
C5A Nb2 C3A 138.1(3) . . ?
C2A Nb2 C3A 72.5(3) . . ?
C7A Nb2 C3A 126.2(3) . . ?
C4A Nb2 C3A 74.5(3) . . ?
C1A Nb2 C8A 80.2(3) . . ?
C6A Nb2 C8A 144.8(3) . . ?
C5A Nb2 C8A 78.0(3) . . ?
C2A Nb2 C8A 72.0(3) . . ?
C7A Nb2 C8A 72.1(3) . . ?
C4A Nb2 C8A 113.4(3) . . ?
C3A Nb2 C8A 140.0(3) . . ?
O5 Ba1 O6 81.4(2) . . ?
O5 Ba1 O2 125.5(2) . . ?
O6 Ba1 O2 148.2(2) . . ?
O5 Ba1 O7 119.27(19) . . ?
O6 Ba1 O7 69.86(19) . . ?
O2 Ba1 O7 81.05(17) . . ?
O5 Ba1 O3 77.6(2) . 4_556 ?
O6 Ba1 O3 75.5(2) . 4_556 ?
O2 Ba1 O3 122.8(2) . 4_556 ?
O7 Ba1 O3 137.5(2) . 4_556 ?
O5 Ba1 O1 145.1(2) . . ?
O6 Ba1 O1 99.5(2) . . ?
O2 Ba1 O1 68.71(17) . . ?
O7 Ba1 O1 93.05(17) . . ?
O3 Ba1 O1 69.1(2) 4_556 . ?
O5 Ba1 O4 70.0(2) . . ?
O6 Ba1 O4 140.7(2) . . ?
O2 Ba1 O4 70.51(19) . . ?
O7 Ba1 O4 148.12(18) . . ?
O3 Ba1 O4 72.6(2) 4_556 . ?
O1 Ba1 O4 89.86(18) . . ?
O5 Ba1 N6A 76.4(2) . . ?
O6 Ba1 N6A 109.4(2) . . ?
O2 Ba1 N6A 67.59(18) . . ?
O7 Ba1 N6A 65.54(18) . . ?
O3 Ba1 N6A 152.4(2) 4_556 . ?
O1 Ba1 N6A 133.59(19) . . ?
O4 Ba1 N6A 89.9(2) . . ?
N1 C1 Nb1 173.5(7) . . ?
N1A C1A Nb2 171.9(7) . . ?
N2 C2 Nb1 175.5(7) . . ?
N2A C2A Nb2 174.7(7) . . ?
N3 C3 Nb1 173.7(7) . . ?
N3A C3A Nb2 177.4(8) . . ?
N4 C4 Nb1 176.5(8) . . ?
N4A C4A Nb2 175.8(7) . . ?
N5 C5 Nb1 175.2(8) . . ?
N5A C5A Nb2 176.8(7) . . ?
N6 C6 Nb1 176.7(9) . . ?
N6A C6A Nb2 176.3(7) . . ?
N7 C7 Nb1 176.6(9) . . ?
N7A C7A Nb2 174.2(8) . . ?
N8 C8 Nb1 176.7(8) . . ?
N8A C8A Nb2 174.1(8) . . ?
N11 C11 C12 111.9(8) . . ?
N11 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
N11 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C13 C12 C11 114.6(8) . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12B 108.6 . . ?
C11 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
N12 C13 C12 112.6(8) . . ?
N12 C13 H13A 109.1 . . ?
C12 C13 H13A 109.1 . . ?
N12 C13 H13B 109.1 . . ?
C12 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
N12 C14 C15 108.6(8) . . ?
N12 C14 H14A 110.0 . . ?
C15 C14 H14A 110.0 . . ?
N12 C14 H14B 110.0 . . ?
C15 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
N13 C15 C14 108.2(8) . . ?
N13 C15 H15A 110.1 . . ?
C14 C15 H15A 110.1 . . ?
N13 C15 H15B 110.1 . . ?
C14 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
N13 C16 C17 112.8(7) . . ?
N13 C16 H16A 109.0 . . ?
C17 C16 H16A 109.0 . . ?
N13 C16 H16B 109.0 . . ?
C17 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C16 C17 C18 116.8(7) . . ?
C16 C17 H17A 108.1 . . ?
C18 C17 H17A 108.1 . . ?
C16 C17 H17B 108.1 . . ?
C18 C17 H17B 108.1 . . ?
H17A C17 H17B 107.3 . . ?
N14 C18 C17 112.0(7) . . ?
N14 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
N14 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
N14 C19 C20 109.7(8) . . ?
N14 C19 H19A 109.7 . . ?
C20 C19 H19A 109.7 . . ?
N14 C19 H19B 109.7 . . ?
C20 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
C19 C20 N11 109.3(8) . . ?
C19 C20 H20A 109.8 . . ?
N11 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
N11 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
C25 C21 N21 109.3(11) 3_765 . ?
C25 C21 H21A 109.8 3_765 . ?
N21 C21 H21A 109.8 . . ?
C25 C21 H21B 109.8 3_765 . ?
N21 C21 H21B 109.8 . . ?
H21A C21 H21B 108.3 . . ?
C23 C22 N21 113.7(12) . . ?
C23 C22 H22A 108.8 . . ?
N21 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
N21 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C22 C23 C24 119.1(14) . . ?
C22 C23 H23A 107.5 . . ?
C24 C23 H23A 107.5 . . ?
C22 C23 H23B 107.5 . . ?
C24 C23 H23B 107.5 . . ?
H23A C23 H23B 107.0 . . ?
N22 C24 C23 112.8(12) . . ?
N22 C24 H24A 109.0 . . ?
C23 C24 H24A 109.0 . . ?
N22 C24 H24B 109.0 . . ?
C23 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C21 C25 N22 110.8(12) 3_765 . ?
C21 C25 H25A 109.5 3_765 . ?
N22 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 3_765 . ?
N22 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
N31 C31 C35 113.6(10) . 3_755 ?
N31 C31 H31A 108.8 . . ?
C35 C31 H31A 108.8 3_755 . ?
N31 C31 H31B 108.8 . . ?
C35 C31 H31B 108.8 3_755 . ?
H31A C31 H31B 107.7 . . ?
N31 C32 C33 115.5(10) . . ?
N31 C32 H32A 108.4 . . ?
C33 C32 H32A 108.4 . . ?
N31 C32 H32B 108.4 . . ?
C33 C32 H32B 108.4 . . ?
H32A C32 H32B 107.5 . . ?
C32 C33 C34 123.1(12) . . ?
C32 C33 H33A 106.6 . . ?
C34 C33 H33A 106.6 . . ?
C32 C33 H33B 106.6 . . ?
C34 C33 H33B 106.6 . . ?
H33A C33 H33B 106.5 . . ?
N32 C34 C33 108.1(10) . . ?
N32 C34 H34A 110.1 . . ?
C33 C34 H34A 110.1 . . ?
N32 C34 H34B 110.1 . . ?
C33 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
N32 C35 C31 107.0(10) . 3_755 ?
N32 C35 H35A 110.3 . . ?
C31 C35 H35A 110.3 3_755 . ?
N32 C35 H35B 110.3 . . ?
C31 C35 H35B 110.3 3_755 . ?
H35A C35 H35B 108.6 . . ?
N41 C41 C42 108.5(7) . . ?
N41 C41 H41A 110.0 . . ?
C42 C41 H41A 110.0 . . ?
N41 C41 H41B 110.0 . . ?
C42 C41 H41B 110.0 . . ?
H41A C41 H41B 108.4 . . ?
N42 C42 C41 109.8(7) . . ?
N42 C42 H42A 109.7 . . ?
C41 C42 H42A 109.7 . . ?
N42 C42 H42B 109.7 . . ?
C41 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
N42 C43 C44 112.2(7) . . ?
N42 C43 H43A 109.2 . . ?
C44 C43 H43A 109.2 . . ?
N42 C43 H43B 109.2 . . ?
C44 C43 H43B 109.2 . . ?
H43A C43 H43B 107.9 . . ?
C43 C44 C45 115.0(8) . . ?
C43 C44 H44A 108.5 . . ?
C45 C44 H44A 108.5 . . ?
C43 C44 H44B 108.5 . . ?
C45 C44 H44B 108.5 . . ?
H44A C44 H44B 107.5 . . ?
N41 C45 C44 111.9(7) 3_666 . ?
N41 C45 H45A 109.2 3_666 . ?
C44 C45 H45A 109.2 . . ?
N41 C45 H45B 109.2 3_666 . ?
C44 C45 H45B 109.2 . . ?
H45A C45 H45B 107.9 . . ?
N51 C51 C55 109.8(7) . 3_656 ?
N51 C51 H51A 109.7 . . ?
C55 C51 H51A 109.7 3_656 . ?
N51 C51 H51B 109.7 . . ?
C55 C51 H51B 109.7 3_656 . ?
H51A C51 H51B 108.2 . . ?
N51 C52 C53 112.8(8) . . ?
N51 C52 H52A 109.0 . . ?
C53 C52 H52A 109.0 . . ?
N51 C52 H52B 109.0 . . ?
C53 C52 H52B 109.0 . . ?
H52A C52 H52B 107.8 . . ?
C52 C53 C54 115.3(8) . . ?
C52 C53 H53A 108.4 . . ?
C54 C53 H53A 108.4 . . ?
C52 C53 H53B 108.4 . . ?
C54 C53 H53B 108.4 . . ?
H53A C53 H53B 107.5 . . ?
N52 C54 C53 111.4(7) . . ?
N52 C54 H54A 109.4 . . ?
C53 C54 H54A 109.4 . . ?
N52 C54 H54B 109.4 . . ?
C53 C54 H54B 109.4 . . ?
H54A C54 H54B 108.0 . . ?
N52 C55 C51 110.3(7) . 3_656 ?
N52 C55 H55A 109.6 . . ?
C51 C55 H55A 109.6 3_656 . ?
N52 C55 H55B 109.6 . . ?
C51 C55 H55B 109.6 3_656 . ?
H55A C55 H55B 108.1 . . ?
C1 N1 Ni1 151.0(7) . . ?
C1A N1A Ni1 150.6(7) . . ?
C2 N2 Ni2 159.4(7) . . ?
C3 N3 Ni3 159.1(6) . . ?
C4A N4A Ni4 156.0(6) . . ?
C5A N5A Ni5 153.0(6) . . ?
C6A N6A Ba1 138.3(6) . . ?
C11 N11 C20 113.4(8) . . ?
C11 N11 Ni1 115.5(6) . . ?
C20 N11 Ni1 104.8(6) . . ?
C11 N11 H11 107.6 . . ?
C20 N11 H11 107.6 . . ?
Ni1 N11 H11 107.6 . . ?
C14 N12 C13 113.4(7) . . ?
C14 N12 Ni1 105.1(5) . . ?
C13 N12 Ni1 114.6(6) . . ?
C14 N12 H12 107.8 . . ?
C13 N12 H12 107.8 . . ?
Ni1 N12 H12 107.8 . . ?
C15 N13 C16 113.5(7) . . ?
C15 N13 Ni1 104.7(5) . . ?
C16 N13 Ni1 115.6(6) . . ?
C15 N13 H13 107.5 . . ?
C16 N13 H13 107.5 . . ?
Ni1 N13 H13 107.5 . . ?
C19 N14 C18 114.3(7) . . ?
C19 N14 Ni1 105.6(5) . . ?
C18 N14 Ni1 115.7(6) . . ?
C19 N14 H14 106.9 . . ?
C18 N14 H14 106.9 . . ?
Ni1 N14 H14 106.9 . . ?
C21 N21 C22 116.7(11) . . ?
C21 N21 Ni2 105.4(9) . . ?
C22 N21 Ni2 112.9(8) . . ?
C21 N21 H21 107.1 . . ?
C22 N21 H21 107.1 . . ?
Ni2 N21 H21 107.1 . . ?
C24 N22 C25 115.1(12) . . ?
C24 N22 Ni2 115.0(9) . . ?
C25 N22 Ni2 104.3(8) . . ?
C24 N22 H22 107.3 . . ?
C25 N22 H22 107.3 . . ?
Ni2 N22 H22 107.3 . . ?
C31 N31 C32 117.7(10) . . ?
C31 N31 Ni3 106.3(8) . . ?
C32 N31 Ni3 115.5(8) . . ?
C31 N31 H31 105.4 . . ?
C32 N31 H31 105.4 . . ?
Ni3 N31 H31 105.4 . . ?
C34 N32 C35 109.4(10) . . ?
C34 N32 Ni3 119.2(9) . . ?
C35 N32 Ni3 105.6(7) . . ?
C34 N32 H32 107.4 . . ?
C35 N32 H32 107.4 . . ?
Ni3 N32 H32 107.4 . . ?
C45 N41 C41 112.2(7) 3_666 . ?
C45 N41 Ni4 116.7(6) 3_666 . ?
C41 N41 Ni4 106.0(5) . . ?
C45 N41 H41 107.2 3_666 . ?
C41 N41 H41 107.2 . . ?
Ni4 N41 H41 107.2 . . ?
C43 N42 C42 113.9(7) . . ?
C43 N42 Ni4 115.5(5) . . ?
C42 N42 Ni4 104.7(5) . . ?
C43 N42 H42 107.4 . . ?
C42 N42 H42 107.4 . . ?
Ni4 N42 H42 107.4 . . ?
C52 N51 C51 114.2(7) . . ?
C52 N51 Ni5 114.5(5) . . ?
C51 N51 Ni5 105.4(5) . . ?
C52 N51 H51 107.4 . . ?
C51 N51 H51 107.4 . . ?
Ni5 N51 H51 107.4 . . ?
C55 N52 C54 113.0(7) . . ?
C55 N52 Ni5 105.8(5) . . ?
C54 N52 Ni5 116.6(6) . . ?
C55 N52 H52 107.0 . . ?
C54 N52 H52 107.0 . . ?
Ni5 N52 H52 107.0 . . ?

_refine_diff_density_max         1.460
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.150



