# 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_Complex1
_database_code_depnum_ccdc_archive 'CCDC 2062614'
loop_
_audit_author_name
_audit_author_address
'Debashis Ray'
;IIT Kharagpur
India
;
_audit_update_record             
;
2021-02-11 deposited with the CCDC.	2021-07-26 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         'C64 H68 Gd2 N2 Ni2 O20, 2(CH3OH)'
_chemical_formula_sum            'C66 H76 Gd2 N2 Ni2 O22'
_chemical_formula_weight         1681.20

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   11.366(12)
_cell_length_b                   11.446(13)
_cell_length_c                   13.959(15)
_cell_angle_alpha                78.54(3)
_cell_angle_beta                 76.46(4)
_cell_angle_gamma                89.78(3)
_cell_volume                     1729(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5501
_cell_measurement_theta_min      1.533
_cell_measurement_theta_max      31.394

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_F_000             846
_exptl_transmission_factor_min   .676
_exptl_transmission_factor_max   .740
_exptl_crystal_size_max          .16
_exptl_crystal_size_mid          .14
_exptl_crystal_size_min          .12
_exptl_absorpt_coefficient_mu    2.505
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX-II'
_diffrn_measurement_method       'CCD area detector,ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22749
_diffrn_reflns_av_unetI/netI     0.1116
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.533
_diffrn_reflns_theta_max         31.394
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.812
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             9271
_reflns_number_gt                5501
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       SMART
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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)+(0.1044P)²] 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         9271
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1904
_refine_ls_wR_factor_gt          0.1568
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.978
_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
Gd1 Gd 0.31776(3) 0.55258(3) 0.68419(2) 0.03809(14) Uani 1 1 d . . . . .
N1 N 0.5902(6) 0.7864(5) 0.3730(4) 0.0425(14) Uani 1 1 d . . . . .
C8 C 0.6107(7) 0.8699(6) 0.4161(6) 0.0445(18) Uani 1 1 d . . . . .
H7 H 0.6455 0.9408 0.3739 0.053 Uiso 1 1 calc R U . . .
O11 O -0.0073(8) 0.3244(7) 0.9009(5) 0.091(2) Uani 1 1 d . . . . .
H38 H -0.0496 0.3621 0.9392 0.136 Uiso 1 1 calc R U . . .
Ni1 Ni 0.48798(8) 0.63143(7) 0.44443(6) 0.0348(2) Uani 1 1 d . . . . .
O4 O 0.6241(4) 0.5182(4) 0.4676(3) 0.0344(10) Uani 1 1 d . . . . .
O2 O 0.4693(4) 0.6804(4) 0.5775(3) 0.0380(11) Uani 1 1 d . . . . .
O3 O 0.5283(5) 0.5790(4) 0.3071(3) 0.0407(12) Uani 1 1 d . . . . .
O5 O 0.3361(5) 0.7177(4) 0.4203(4) 0.0448(12) Uani 1 1 d . . . . .
O7 O 0.2621(5) 0.4607(5) 0.8582(4) 0.0534(14) Uani 1 1 d . . . . .
O6 O 0.2143(5) 0.6732(4) 0.5740(4) 0.0504(14) Uani 1 1 d . . . . .
O10 O 0.1285(6) 0.4345(6) 0.7172(4) 0.0623(16) Uani 1 1 d . . . . .
H34 H 0.1172 0.3715 0.7724 0.075 Uiso 1 1 calc R U . . .
O1 O 0.4550(6) 0.6734(5) 0.7634(4) 0.0566(15) Uani 1 1 d . . . . .
O8 O 0.1580(7) 0.5722(6) 0.9564(4) 0.086(2) Uani 1 1 d . . . . .
O9 O 0.1958(6) 0.6917(5) 0.7736(4) 0.0664(18) Uani 1 1 d . . . . .
H30 H 0.1541 0.6542 0.8380 0.080 Uiso 1 1 calc R U . . .
C7 C 0.5211(7) 0.7720(6) 0.5969(5) 0.0370(16) Uani 1 1 d . . . . .
C17 C 0.2384(7) 0.7194(6) 0.4823(5) 0.0386(16) Uani 1 1 d . . . . .
C6 C 0.5864(7) 0.8671(6) 0.5222(5) 0.0407(16) Uani 1 1 d . . . . .
C25 C 0.2024(8) 0.3795(8) 1.0331(6) 0.059(2) Uani 1 1 d . . . . .
C2 C 0.5110(8) 0.7755(6) 0.6985(5) 0.0469(19) Uani 1 1 d . . . . .
C15 C 0.4904(7) 0.6567(6) 0.2365(5) 0.0447(19) Uani 1 1 d . . . . .
C10 C 0.5374(9) 0.7759(7) 0.2121(5) 0.054(2) Uani 1 1 d . . . . .
C16 C 0.7077(8) 0.5597(7) 0.5175(6) 0.053(2) Uani 1 1 d . . . . .
H15 H 0.7750 0.5084 0.5153 0.079 Uiso 1 1 calc R U . . .
H16 H 0.6676 0.5588 0.5863 0.079 Uiso 1 1 calc R U . . .
H14 H 0.7365 0.6396 0.4842 0.079 Uiso 1 1 calc R U . . .
C14 C 0.4054(9) 0.6247(8) 0.1891(6) 0.060(2) Uani 1 1 d . . . . .
H13 H 0.3733 0.5466 0.2056 0.072 Uiso 1 1 calc R U . . .
C18 C 0.1394(7) 0.7825(6) 0.4414(6) 0.0430(17) Uani 1 1 d . . . . .
C5 C 0.6271(7) 0.9656(6) 0.5544(6) 0.051(2) Uani 1 1 d . . . . .
H6 H 0.6664 1.0304 0.5062 0.061 Uiso 1 1 calc R U . . .
C9 C 0.6312(9) 0.8056(7) 0.2621(6) 0.060(2) Uani 1 1 d . . . . .
H9 H 0.7004 0.7574 0.2451 0.072 Uiso 1 1 calc R U . . .
H8 H 0.6580 0.8886 0.2359 0.072 Uiso 1 1 calc R U . . .
C24 C 0.2064(9) 0.4783(8) 0.9435(6) 0.060(2) Uani 1 1 d . . . . .
C3 C 0.5529(8) 0.8721(7) 0.7280(6) 0.056(2) Uani 1 1 d . . . . .
H4 H 0.5430 0.8729 0.7959 0.068 Uiso 1 1 calc R U . . .
C1 C 0.4603(10) 0.6582(9) 0.8672(6) 0.078(3) Uani 1 1 d . . . . .
H3 H 0.5402 0.6808 0.8707 0.117 Uiso 1 1 calc R U . . .
H1 H 0.4416 0.5762 0.8999 0.117 Uiso 1 1 calc R U . . .
H2 H 0.4025 0.7076 0.9002 0.117 Uiso 1 1 calc R U . . .
C4 C 0.6107(9) 0.9691(8) 0.6540(7) 0.062(2) Uani 1 1 d . . . . .
H5 H 0.6380 1.0358 0.6726 0.075 Uiso 1 1 calc R U . . .
C12 C 0.4117(11) 0.8227(9) 0.0934(7) 0.080(3) Uani 1 1 d . . . . .
H11 H 0.3851 0.8782 0.0455 0.096 Uiso 1 1 calc R U . . .
C11 C 0.4965(10) 0.8571(7) 0.1405(6) 0.068(3) Uani 1 1 d . . . . .
H10 H 0.5264 0.9359 0.1239 0.082 Uiso 1 1 calc R U . . .
C19 C 0.1510(9) 0.8228(7) 0.3420(7) 0.062(2) Uani 1 1 d . . . . .
H17 H 0.2221 0.8107 0.2969 0.074 Uiso 1 1 calc R U . . .
C26 C 0.2505(11) 0.2728(9) 1.0199(7) 0.079(3) Uani 1 1 d . . . . .
H26 H 0.2881 0.2609 0.9561 0.095 Uiso 1 1 calc R U . . .
C13 C 0.3675(10) 0.7074(10) 0.1173(6) 0.074(3) Uani 1 1 d . . . . .
H12 H 0.3113 0.6843 0.0850 0.089 Uiso 1 1 calc R U . . .
C30 C 0.1495(15) 0.3961(12) 1.1284(8) 0.126(6) Uani 1 1 d . . . . .
H22 H 0.1149 0.4682 1.1373 0.151 Uiso 1 1 calc R U . . .
C31 C 0.1727(12) 0.8116(8) 0.7533(8) 0.094(4) Uani 1 1 d . . . . .
H29 H 0.1009 0.8265 0.8005 0.141 Uiso 1 1 calc R U . . .
H27 H 0.1611 0.8336 0.6862 0.141 Uiso 1 1 calc R U . . .
H28 H 0.2400 0.8578 0.7591 0.141 Uiso 1 1 calc R U . . .
C23 C 0.0313(9) 0.8031(9) 0.5101(7) 0.072(3) Uani 1 1 d . . . . .
H21 H 0.0237 0.7788 0.5790 0.087 Uiso 1 1 calc R U . . .
C27 C 0.2423(13) 0.1831(11) 1.1035(9) 0.104(4) Uani 1 1 d . . . . .
H25 H 0.2754 0.1105 1.0946 0.125 Uiso 1 1 calc R U . . .
C21 C -0.0450(11) 0.8981(10) 0.3691(11) 0.095(4) Uani 1 1 d . . . . .
H19 H -0.1068 0.9358 0.3432 0.114 Uiso 1 1 calc R U . . .
C20 C 0.0591(11) 0.8817(9) 0.3059(9) 0.085(3) Uani 1 1 d . . . . .
H18 H 0.0697 0.9103 0.2371 0.102 Uiso 1 1 calc R U . . .
C33 C -0.0216(16) 0.2012(12) 0.9450(13) 0.139(6) Uani 1 1 d . . . . .
H37 H -0.0359 0.1909 1.0168 0.209 Uiso 1 1 calc R U . . .
H35 H 0.0505 0.1621 0.9198 0.209 Uiso 1 1 calc R U . . .
H36 H -0.0893 0.1671 0.9282 0.209 Uiso 1 1 calc R U . . .
C29 C 0.1477(16) 0.3057(14) 1.2111(9) 0.145(7) Uani 1 1 d . . . . .
H23 H 0.1188 0.3189 1.2759 0.174 Uiso 1 1 calc R U . . .
C32 C 0.0277(12) 0.4459(11) 0.6641(10) 0.107(4) Uani 1 1 d . . . . .
H33 H -0.0462 0.4125 0.7105 0.161 Uiso 1 1 calc R U . . .
H31 H 0.0463 0.4038 0.6097 0.161 Uiso 1 1 calc R U . . .
H32 H 0.0184 0.5286 0.6379 0.161 Uiso 1 1 calc R U . . .
C28 C 0.1892(11) 0.1955(12) 1.1960(9) 0.099(4) Uani 1 1 d . . . . .
H24 H 0.1802 0.1310 1.2500 0.119 Uiso 1 1 calc R U . . .
C22 C -0.0634(11) 0.8593(11) 0.4745(11) 0.103(4) Uani 1 1 d . . . . .
H20 H -0.1358 0.8709 0.5183 0.124 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O2 2.297(5) . ?
Gd1 O3 2.313(5) 2_666 ?
Gd1 O4 2.367(5) 2_666 ?
Gd1 O6 2.376(5) . ?
Gd1 O7 2.383(5) . ?
Gd1 O9 2.445(5) . ?
Gd1 O10 2.445(7) . ?
Gd1 O1 2.646(6) . ?
Gd1 Ni1 3.397(3) . ?
Gd1 Ni1 3.485(3) 2_666 ?
N1 C8 1.275(9) . ?
N1 C9 1.479(10) . ?
N1 Ni1 2.064(6) . ?
C8 C6 1.435(10) . ?
C8 H7 0.9300 . ?
O11 C33 1.415(14) . ?
O11 H38 0.8200 . ?
Ni1 O2 2.009(5) . ?
Ni1 O5 2.048(5) . ?
Ni1 O4 2.057(5) . ?
Ni1 O3 2.070(5) . ?
Ni1 O4 2.124(5) 2_666 ?
Ni1 Gd1 3.485(3) 2_666 ?
O4 C16 1.435(9) . ?
O4 Ni1 2.124(5) 2_666 ?
O4 Gd1 2.367(5) 2_666 ?
O2 C7 1.308(8) . ?
O3 C15 1.340(8) . ?
O3 Gd1 2.313(5) 2_666 ?
O5 C17 1.241(8) . ?
O7 C24 1.266(10) . ?
O6 C17 1.250(8) . ?
O10 C32 1.496(14) . ?
O10 H34 0.9300 . ?
O1 C2 1.380(9) . ?
O1 C1 1.440(9) . ?
O8 C24 1.231(10) . ?
O9 C31 1.382(9) . ?
O9 H30 0.9300 . ?
C7 C2 1.405(10) . ?
C7 C6 1.420(10) . ?
C17 C18 1.498(10) . ?
C6 C5 1.411(10) . ?
C25 C26 1.364(12) . ?
C25 C30 1.376(14) . ?
C25 C24 1.502(11) . ?
C2 C3 1.376(11) . ?
C15 C14 1.380(12) . ?
C15 C10 1.414(11) . ?
C10 C11 1.386(11) . ?
C10 C9 1.480(13) . ?
C16 H15 0.9600 . ?
C16 H16 0.9600 . ?
C16 H14 0.9600 . ?
C14 C13 1.382(11) . ?
C14 H13 0.9300 . ?
C18 C19 1.348(11) . ?
C18 C23 1.421(11) . ?
C5 C4 1.368(12) . ?
C5 H6 0.9300 . ?
C9 H9 0.9700 . ?
C9 H8 0.9700 . ?
C3 C4 1.401(12) . ?
C3 H4 0.9300 . ?
C1 H3 0.9600 . ?
C1 H1 0.9600 . ?
C1 H2 0.9600 . ?
C4 H5 0.9300 . ?
C12 C13 1.363(15) . ?
C12 C11 1.385(15) . ?
C12 H11 0.9300 . ?
C11 H10 0.9300 . ?
C19 C20 1.380(12) . ?
C19 H17 0.9300 . ?
C26 C27 1.377(13) . ?
C26 H26 0.9300 . ?
C13 H12 0.9300 . ?
C30 C29 1.386(15) . ?
C30 H22 0.9300 . ?
C31 H29 0.9600 . ?
C31 H27 0.9600 . ?
C31 H28 0.9600 . ?
C23 C22 1.391(13) . ?
C23 H21 0.9300 . ?
C27 C28 1.327(16) . ?
C27 H25 0.9300 . ?
C21 C20 1.337(16) . ?
C21 C22 1.415(17) . ?
C21 H19 0.9300 . ?
C20 H18 0.9300 . ?
C33 H37 0.9600 . ?
C33 H35 0.9600 . ?
C33 H36 0.9600 . ?
C29 C28 1.383(18) . ?
C29 H23 0.9300 . ?
C32 H33 0.9600 . ?
C32 H31 0.9600 . ?
C32 H32 0.9600 . ?
C28 H24 0.9300 . ?
C22 H20 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Gd1 O3 84.06(18) . 2_666 ?
O2 Gd1 O4 72.38(17) . 2_666 ?
O3 Gd1 O4 69.98(16) 2_666 2_666 ?
O2 Gd1 O6 77.1(2) . . ?
O3 Gd1 O6 144.55(17) 2_666 . ?
O4 Gd1 O6 75.78(17) 2_666 . ?
O2 Gd1 O7 137.55(19) . . ?
O3 Gd1 O7 79.60(18) 2_666 . ?
O4 Gd1 O7 134.76(18) 2_666 . ?
O6 Gd1 O7 133.50(19) . . ?
O2 Gd1 O9 100.6(2) . . ?
O3 Gd1 O9 143.01(19) 2_666 . ?
O4 Gd1 O9 146.59(17) 2_666 . ?
O6 Gd1 O9 70.83(19) . . ?
O7 Gd1 O9 72.32(19) . . ?
O2 Gd1 O10 151.16(19) . . ?
O3 Gd1 O10 107.6(2) 2_666 . ?
O4 Gd1 O10 86.68(19) 2_666 . ?
O6 Gd1 O10 78.7(2) . . ?
O7 Gd1 O10 71.3(2) . . ?
O9 Gd1 O10 85.9(2) . . ?
O2 Gd1 O1 61.56(18) . . ?
O3 Gd1 O1 80.79(19) 2_666 . ?
O4 Gd1 O1 127.32(18) 2_666 . ?
O6 Gd1 O1 114.50(19) . . ?
O7 Gd1 O1 77.2(2) . . ?
O9 Gd1 O1 70.0(2) . . ?
O10 Gd1 O1 144.93(19) . . ?
O2 Gd1 Ni1 35.03(11) . . ?
O3 Gd1 Ni1 80.31(13) 2_666 . ?
O4 Gd1 Ni1 38.24(12) 2_666 . ?
O6 Gd1 Ni1 66.98(14) . . ?
O7 Gd1 Ni1 159.49(14) . . ?
O9 Gd1 Ni1 123.62(14) . . ?
O10 Gd1 Ni1 119.30(15) . . ?
O1 Gd1 Ni1 95.50(14) . . ?
O2 Gd1 Ni1 75.52(13) . 2_666 ?
O3 Gd1 Ni1 34.98(12) 2_666 2_666 ?
O4 Gd1 Ni1 34.99(11) 2_666 2_666 ?
O6 Gd1 Ni1 110.30(14) . 2_666 ?
O7 Gd1 Ni1 108.71(14) . 2_666 ?
O9 Gd1 Ni1 175.41(17) . 2_666 ?
O10 Gd1 Ni1 98.72(17) . 2_666 ?
O1 Gd1 Ni1 105.70(15) . 2_666 ?
Ni1 Gd1 Ni1 54.31(6) . 2_666 ?
C8 N1 C9 118.4(6) . . ?
C8 N1 Ni1 124.8(5) . . ?
C9 N1 Ni1 116.5(5) . . ?
N1 C8 C6 127.5(7) . . ?
N1 C8 H7 116.3 . . ?
C6 C8 H7 116.3 . . ?
C33 O11 H38 109.5 . . ?
O2 Ni1 O5 91.7(2) . . ?
O2 Ni1 O4 93.3(2) . . ?
O5 Ni1 O4 169.9(2) . . ?
O2 Ni1 N1 90.1(2) . . ?
O5 Ni1 N1 89.0(2) . . ?
O4 Ni1 N1 99.8(2) . . ?
O2 Ni1 O3 173.4(2) . . ?
O5 Ni1 O3 94.4(2) . . ?
O4 Ni1 O3 81.13(18) . . ?
N1 Ni1 O3 87.4(2) . . ?
O2 Ni1 O4 83.53(19) . 2_666 ?
O5 Ni1 O4 89.2(2) . 2_666 ?
O4 Ni1 O4 82.6(2) . 2_666 ?
N1 Ni1 O4 173.3(2) . 2_666 ?
O3 Ni1 O4 99.18(19) . 2_666 ?
O2 Ni1 Gd1 41.02(14) . . ?
O5 Ni1 Gd1 83.11(15) . . ?
O4 Ni1 Gd1 94.86(14) . . ?
N1 Ni1 Gd1 129.74(17) . . ?
O3 Ni1 Gd1 142.56(15) . . ?
O4 Ni1 Gd1 43.61(12) 2_666 . ?
O2 Ni1 Gd1 134.46(14) . 2_666 ?
O5 Ni1 Gd1 133.59(15) . 2_666 ?
O4 Ni1 Gd1 41.28(13) . 2_666 ?
N1 Ni1 Gd1 94.74(18) . 2_666 ?
O3 Ni1 Gd1 39.84(12) . 2_666 ?
O4 Ni1 Gd1 91.16(14) 2_666 2_666 ?
Gd1 Ni1 Gd1 125.69(6) . 2_666 ?
C16 O4 Ni1 115.1(4) . . ?
C16 O4 Ni1 113.9(4) . 2_666 ?
Ni1 O4 Ni1 97.4(2) . 2_666 ?
C16 O4 Gd1 124.2(4) . 2_666 ?
Ni1 O4 Gd1 103.72(19) . 2_666 ?
Ni1 O4 Gd1 98.15(19) 2_666 2_666 ?
C7 O2 Ni1 128.2(4) . . ?
C7 O2 Gd1 127.4(4) . . ?
Ni1 O2 Gd1 103.9(2) . . ?
C15 O3 Ni1 111.7(4) . . ?
C15 O3 Gd1 138.0(4) . 2_666 ?
Ni1 O3 Gd1 105.2(2) . 2_666 ?
C17 O5 Ni1 127.5(4) . . ?
C24 O7 Gd1 142.6(5) . . ?
C17 O6 Gd1 135.5(5) . . ?
C32 O10 Gd1 131.3(6) . . ?
C32 O10 H34 114.4 . . ?
Gd1 O10 H34 114.4 . . ?
C2 O1 C1 117.1(7) . . ?
C2 O1 Gd1 113.6(4) . . ?
C1 O1 Gd1 128.2(5) . . ?
C31 O9 Gd1 136.5(6) . . ?
C31 O9 H30 111.7 . . ?
Gd1 O9 H30 111.7 . . ?
O2 C7 C2 117.4(6) . . ?
O2 C7 C6 124.3(6) . . ?
C2 C7 C6 118.4(7) . . ?
O5 C17 O6 126.8(7) . . ?
O5 C17 C18 115.8(6) . . ?
O6 C17 C18 117.4(7) . . ?
C5 C6 C7 117.8(7) . . ?
C5 C6 C8 118.3(7) . . ?
C7 C6 C8 123.8(7) . . ?
C26 C25 C30 119.9(9) . . ?
C26 C25 C24 120.0(8) . . ?
C30 C25 C24 120.0(9) . . ?
C3 C2 O1 124.8(7) . . ?
C3 C2 C7 122.4(7) . . ?
O1 C2 C7 112.9(7) . . ?
O3 C15 C14 122.2(7) . . ?
O3 C15 C10 118.4(7) . . ?
C14 C15 C10 119.3(7) . . ?
C11 C10 C15 118.6(9) . . ?
C11 C10 C9 123.7(8) . . ?
C15 C10 C9 117.6(7) . . ?
O4 C16 H15 109.5 . . ?
O4 C16 H16 109.5 . . ?
H15 C16 H16 109.5 . . ?
O4 C16 H14 109.5 . . ?
H15 C16 H14 109.5 . . ?
H16 C16 H14 109.5 . . ?
C15 C14 C13 120.6(9) . . ?
C15 C14 H13 119.7 . . ?
C13 C14 H13 119.7 . . ?
C19 C18 C23 119.2(7) . . ?
C19 C18 C17 122.0(7) . . ?
C23 C18 C17 118.7(7) . . ?
C4 C5 C6 122.2(8) . . ?
C4 C5 H6 118.9 . . ?
C6 C5 H6 118.9 . . ?
N1 C9 C10 114.1(7) . . ?
N1 C9 H9 108.7 . . ?
C10 C9 H9 108.7 . . ?
N1 C9 H8 108.7 . . ?
C10 C9 H8 108.7 . . ?
H9 C9 H8 107.6 . . ?
O8 C24 O7 123.4(8) . . ?
O8 C24 C25 119.1(8) . . ?
O7 C24 C25 117.5(8) . . ?
C2 C3 C4 118.9(8) . . ?
C2 C3 H4 120.5 . . ?
C4 C3 H4 120.5 . . ?
O1 C1 H3 109.5 . . ?
O1 C1 H1 109.5 . . ?
H3 C1 H1 109.5 . . ?
O1 C1 H2 109.5 . . ?
H3 C1 H2 109.5 . . ?
H1 C1 H2 109.5 . . ?
C5 C4 C3 120.0(8) . . ?
C5 C4 H5 120.0 . . ?
C3 C4 H5 120.0 . . ?
C13 C12 C11 119.8(8) . . ?
C13 C12 H11 120.1 . . ?
C11 C12 H11 120.1 . . ?
C12 C11 C10 121.0(9) . . ?
C12 C11 H10 119.5 . . ?
C10 C11 H10 119.5 . . ?
C18 C19 C20 121.1(9) . . ?
C18 C19 H17 119.4 . . ?
C20 C19 H17 119.4 . . ?
C25 C26 C27 118.4(10) . . ?
C25 C26 H26 120.8 . . ?
C27 C26 H26 120.8 . . ?
C12 C13 C14 120.6(10) . . ?
C12 C13 H12 119.7 . . ?
C14 C13 H12 119.7 . . ?
C25 C30 C29 120.0(12) . . ?
C25 C30 H22 120.0 . . ?
C29 C30 H22 120.0 . . ?
O9 C31 H29 109.5 . . ?
O9 C31 H27 109.5 . . ?
H29 C31 H27 109.5 . . ?
O9 C31 H28 109.5 . . ?
H29 C31 H28 109.5 . . ?
H27 C31 H28 109.5 . . ?
C22 C23 C18 120.1(10) . . ?
C22 C23 H21 119.9 . . ?
C18 C23 H21 119.9 . . ?
C28 C27 C26 123.1(12) . . ?
C28 C27 H25 118.5 . . ?
C26 C27 H25 118.5 . . ?
C20 C21 C22 121.5(9) . . ?
C20 C21 H19 119.2 . . ?
C22 C21 H19 119.2 . . ?
C21 C20 C19 120.5(10) . . ?
C21 C20 H18 119.7 . . ?
C19 C20 H18 119.7 . . ?
O11 C33 H37 109.5 . . ?
O11 C33 H35 109.5 . . ?
H37 C33 H35 109.5 . . ?
O11 C33 H36 109.5 . . ?
H37 C33 H36 109.5 . . ?
H35 C33 H36 109.5 . . ?
C28 C29 C30 119.2(12) . . ?
C28 C29 H23 120.4 . . ?
C30 C29 H23 120.4 . . ?
O10 C32 H33 109.5 . . ?
O10 C32 H31 109.5 . . ?
H33 C32 H31 109.5 . . ?
O10 C32 H32 109.5 . . ?
H33 C32 H32 109.5 . . ?
H31 C32 H32 109.5 . . ?
C27 C28 C29 119.0(10) . . ?
C27 C28 H24 120.5 . . ?
C29 C28 H24 120.5 . . ?
C23 C22 C21 117.4(11) . . ?
C23 C22 H20 121.3 . . ?
C21 C22 H20 121.3 . . ?

_refine_diff_density_max         2.245
_refine_diff_density_min         -2.513
_refine_diff_density_rms         0.252



####################################################################### 
# 
# 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_Complex3
_database_code_depnum_ccdc_archive 'CCDC 2062616'
loop_
_audit_author_name
_audit_author_address
'Debashis Ray'
;IIT Kharagpur
India
;
_audit_update_record             
;
2021-02-11 deposited with the CCDC.	2021-07-26 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         'C64 H68 Dy2 N2 Ni2 O20, 2(CH3OH)'
_chemical_formula_sum            'C66 H76 Dy2 N2 Ni2 O22'
_chemical_formula_weight         1691.70

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

_space_group_crystal_system      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                   11.108(18)
_cell_length_b                   11.279(18)
_cell_length_c                   13.69(2)
_cell_angle_alpha                101.289(19)
_cell_angle_beta                 103.51(2)
_cell_angle_gamma                90.45(2)
_cell_volume                     1633(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7051
_cell_measurement_theta_min      1.563
_cell_measurement_theta_max      28.757

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_F_000             850
_exptl_transmission_factor_min   .616
_exptl_transmission_factor_max   .748
_exptl_crystal_size_max          .17
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .10
_exptl_absorpt_coefficient_mu    2.910
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX-II'
_diffrn_measurement_method       'CCD area detector,ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22578
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.563
_diffrn_reflns_theta_max         28.757
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             7839
_reflns_number_gt                7051
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       SMART
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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)+(0.0560P)²+3.7943P] 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         7839
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.68269(2) 0.44785(2) 0.68414(2) 0.01649(7) Uani 1 1 d . . . . .
C8 C 0.3876(4) 0.1264(4) 0.4148(3) 0.0197(8) Uani 1 1 d . . . . .
H7 H 0.3520 0.0543 0.3714 0.024 Uiso 1 1 calc R U . . .
Ni1 Ni 0.51117(4) 0.36853(4) 0.44327(4) 0.01423(11) Uani 1 1 d . . . . .
O2 O 0.5300(3) 0.3192(2) 0.5773(2) 0.0182(6) Uani 1 1 d . . . . .
O4 O 0.6637(3) 0.2835(3) 0.4173(2) 0.0181(6) Uani 1 1 d . . . . .
O5 O 0.7867(3) 0.3282(3) 0.5750(2) 0.0217(6) Uani 1 1 d . . . . .
O6 O 0.7371(3) 0.5408(3) 0.8571(2) 0.0225(6) Uani 1 1 d . . . . .
O7 O 0.8413(3) 0.4249(3) 0.9578(2) 0.0359(8) Uani 1 1 d . . . . .
O1 O 0.5429(3) 0.3274(3) 0.7656(2) 0.0232(6) Uani 1 1 d . . . . .
O9 O 0.8699(3) 0.5676(3) 0.7152(2) 0.0267(7) Uani 1 1 d . . . . .
H34 H 0.8828 0.6306 0.7723 0.032 Uiso 1 1 calc R U . . .
O10 O 0.8031(3) 0.3096(3) 0.7712(2) 0.0298(7) Uani 1 1 d . . . . .
H30 H 0.8476 0.3471 0.8365 0.036 Uiso 1 1 calc R U . . .
O11 O 0.0072(3) 0.6732(3) 0.9002(3) 0.0361(8) Uani 1 1 d . . . . .
H38 H 0.0639 0.6372 0.9295 0.054 Uiso 1 1 calc R U . . .
N1 N 0.4080(3) 0.2112(3) 0.3716(3) 0.0185(7) Uani 1 1 d . . . . .
C7 C 0.4774(4) 0.2255(3) 0.5977(3) 0.0166(8) Uani 1 1 d . . . . .
C6 C 0.4130(4) 0.1282(4) 0.5231(3) 0.0172(8) Uani 1 1 d . . . . .
C23 C 0.7935(4) 0.5222(4) 0.9434(3) 0.0261(10) Uani 1 1 d . . . . .
C2 C 0.4879(4) 0.2228(4) 0.7006(3) 0.0194(8) Uani 1 1 d . . . . .
C5 C 0.3703(4) 0.0294(4) 0.5550(3) 0.0221(9) Uani 1 1 d . . . . .
H6 H 0.3282 -0.0359 0.5060 0.027 Uiso 1 1 calc R U . . .
C16 C 0.7626(4) 0.2812(4) 0.4810(3) 0.0181(8) Uani 1 1 d . . . . .
C17 C 0.8637(4) 0.2168(4) 0.4418(3) 0.0193(8) Uani 1 1 d . . . . .
C4 C 0.3886(4) 0.0259(4) 0.6556(4) 0.0244(9) Uani 1 1 d . . . . .
H5 H 0.3622 -0.0426 0.6748 0.029 Uiso 1 1 calc R U . . .
C18 C 0.8521(4) 0.1797(4) 0.3376(4) 0.0280(10) Uani 1 1 d . . . . .
H14 H 0.7808 0.1949 0.2916 0.034 Uiso 1 1 calc R U . . .
C3 C 0.4465(4) 0.1244(4) 0.7304(3) 0.0234(9) Uani 1 1 d . . . . .
H4 H 0.4570 0.1233 0.7996 0.028 Uiso 1 1 calc R U . . .
C22 C 0.9707(4) 0.1943(5) 0.5088(4) 0.0301(10) Uani 1 1 d . . . . .
H18 H 0.9796 0.2188 0.5792 0.036 Uiso 1 1 calc R U . . .
C24 C 0.7993(4) 0.6212(4) 1.0348(3) 0.0253(9) Uani 1 1 d . . . . .
C12 C 0.5930(5) 0.1766(5) 0.0919(3) 0.0321(11) Uani 1 1 d . . . . .
H11 H 0.6213 0.1200 0.0444 0.039 Uiso 1 1 calc R U . . .
C31 C 0.8238(6) 0.1871(5) 0.7492(4) 0.0397(13) Uani 1 1 d . . . . .
H28 H 0.7713 0.1430 0.7779 0.060 Uiso 1 1 calc R U . . .
H29 H 0.9090 0.1749 0.7783 0.060 Uiso 1 1 calc R U . . .
H27 H 0.8054 0.1588 0.6762 0.060 Uiso 1 1 calc R U . . .
C33 C 0.0219(6) 0.7975(5) 0.9465(5) 0.0440(13) Uani 1 1 d . . . . .
H35 H 0.1065 0.8256 0.9560 0.066 Uiso 1 1 calc R U . . .
H36 H 0.0012 0.8090 1.0119 0.066 Uiso 1 1 calc R U . . .
H37 H -0.0318 0.8423 0.9031 0.066 Uiso 1 1 calc R U . . .
C1 C 0.5374(5) 0.3406(5) 0.8699(3) 0.0334(11) Uani 1 1 d . . . . .
H3 H 0.4540 0.3221 0.8731 0.050 Uiso 1 1 calc R U . . .
H1 H 0.5624 0.4224 0.9053 0.050 Uiso 1 1 calc R U . . .
H2 H 0.5920 0.2861 0.9017 0.050 Uiso 1 1 calc R U . . .
C25 C 0.7565(5) 0.7316(5) 1.0231(4) 0.0335(11) Uani 1 1 d . . . . .
H19 H 0.7207 0.7445 0.9577 0.040 Uiso 1 1 calc R U . . .
C20 C 1.0515(5) 0.0994(5) 0.3684(5) 0.0408(13) Uani 1 1 d . . . . .
H16 H 1.1149 0.0603 0.3434 0.049 Uiso 1 1 calc R U . . .
C26 C 0.7657(5) 0.8250(5) 1.1075(4) 0.0389(12) Uani 1 1 d . . . . .
H20 H 0.7384 0.9008 1.0987 0.047 Uiso 1 1 calc R U . . .
C29 C 0.8431(7) 0.6002(6) 1.1319(5) 0.059(2) Uani 1 1 d . . . . .
H23 H 0.8688 0.5238 1.1405 0.071 Uiso 1 1 calc R U . . .
C19 C 0.9458(5) 0.1203(5) 0.3018(4) 0.0370(12) Uani 1 1 d . . . . .
H15 H 0.9369 0.0942 0.2316 0.044 Uiso 1 1 calc R U . . .
C21 C 1.0650(5) 0.1357(5) 0.4719(5) 0.0405(13) Uani 1 1 d . . . . .
H17 H 1.1371 0.1211 0.5173 0.049 Uiso 1 1 calc R U . . .
C27 C 0.8147(5) 0.8052(5) 1.2031(4) 0.0441(14) Uani 1 1 d . . . . .
H21 H 0.8250 0.8688 1.2596 0.053 Uiso 1 1 calc R U . . .
C32 C 0.9696(6) 0.5590(6) 0.6590(5) 0.0493(15) Uani 1 1 d . . . . .
H33 H 1.0485 0.5792 0.7071 0.074 Uiso 1 1 calc R U . . .
H31 H 0.9563 0.6143 0.6129 0.074 Uiso 1 1 calc R U . . .
H32 H 0.9686 0.4779 0.6207 0.074 Uiso 1 1 calc R U . . .
C28 C 0.8494(7) 0.6908(7) 1.2170(5) 0.064(2) Uani 1 1 d . . . . .
H22 H 0.8766 0.6754 1.2827 0.077 Uiso 1 1 calc R U . . .
O8 O 0.3737(2) 0.4807(2) 0.4675(2) 0.0159(5) Uani 1 1 d . . . . .
O3 O 0.4709(3) 0.4233(2) 0.3056(2) 0.0179(6) Uani 1 1 d . . . . .
C15 C 0.5098(4) 0.3447(4) 0.2339(3) 0.0196(8) Uani 1 1 d . . . . .
C14 C 0.5967(4) 0.3784(4) 0.1864(3) 0.0245(9) Uani 1 1 d . . . . .
H13 H 0.6276 0.4585 0.2023 0.029 Uiso 1 1 calc R U . . .
C10 C 0.4635(4) 0.2247(4) 0.2096(3) 0.0213(8) Uani 1 1 d . . . . .
C9 C 0.3662(4) 0.1895(4) 0.2593(3) 0.0240(9) Uani 1 1 d . . . . .
H9 H 0.2936 0.2351 0.2408 0.029 Uiso 1 1 calc R U . . .
H8 H 0.3420 0.1042 0.2332 0.029 Uiso 1 1 calc R U . . .
C11 C 0.5062(5) 0.1422(4) 0.1381(3) 0.0270(10) Uani 1 1 d . . . . .
H10 H 0.4752 0.0621 0.1215 0.032 Uiso 1 1 calc R U . . .
C13 C 0.6388(4) 0.2954(5) 0.1156(3) 0.0287(10) Uani 1 1 d . . . . .
H12 H 0.6977 0.3193 0.0839 0.034 Uiso 1 1 calc R U . . .
C30 C 0.2890(4) 0.4374(4) 0.5196(4) 0.0294(10) Uani 1 1 d . . . . .
H25 H 0.2580 0.3566 0.4851 0.044 Uiso 1 1 calc R U . . .
H24 H 0.2211 0.4895 0.5192 0.044 Uiso 1 1 calc R U . . .
H26 H 0.3315 0.4371 0.5892 0.044 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.256(3) . ?
Dy1 O3 2.261(4) 2_666 ?
Dy1 O8 2.325(4) 2_666 ?
Dy1 O6 2.327(4) . ?
Dy1 O5 2.330(4) . ?
Dy1 O9 2.377(4) . ?
Dy1 O10 2.378(4) . ?
Dy1 O1 2.621(4) . ?
Dy1 Ni1 3.344(4) . ?
Dy1 Ni1 3.420(3) 2_666 ?
C8 N1 1.263(6) . ?
C8 C6 1.440(6) . ?
C8 H7 0.9300 . ?
Ni1 O2 1.985(4) . ?
Ni1 O4 2.022(4) . ?
Ni1 O8 2.036(4) . ?
Ni1 N1 2.046(4) . ?
Ni1 O3 2.050(4) . ?
Ni1 O8 2.107(3) 2_666 ?
Ni1 Dy1 3.420(3) 2_666 ?
O2 C7 1.311(5) . ?
O4 C16 1.236(5) . ?
O5 C16 1.257(5) . ?
O6 C23 1.259(6) . ?
O7 C23 1.254(6) . ?
O1 C2 1.371(5) . ?
O1 C1 1.422(5) . ?
O9 C32 1.482(7) . ?
O9 H34 0.9300 . ?
O10 C31 1.388(6) . ?
O10 H30 0.9300 . ?
O11 C33 1.412(7) . ?
O11 H38 0.8200 . ?
N1 C9 1.468(6) . ?
C7 C2 1.393(6) . ?
C7 C6 1.402(5) . ?
C6 C5 1.392(6) . ?
C23 C24 1.493(6) . ?
C2 C3 1.366(6) . ?
C5 C4 1.352(7) . ?
C5 H6 0.9300 . ?
C16 C17 1.489(6) . ?
C17 C18 1.380(6) . ?
C17 C22 1.381(7) . ?
C4 C3 1.390(6) . ?
C4 H5 0.9300 . ?
C18 C19 1.376(7) . ?
C18 H14 0.9300 . ?
C3 H4 0.9300 . ?
C22 C21 1.384(7) . ?
C22 H18 0.9300 . ?
C24 C25 1.362(7) . ?
C24 C29 1.372(8) . ?
C12 C11 1.362(7) . ?
C12 C13 1.379(7) . ?
C12 H11 0.9300 . ?
C31 H28 0.9600 . ?
C31 H29 0.9600 . ?
C31 H27 0.9600 . ?
C33 H35 0.9600 . ?
C33 H36 0.9600 . ?
C33 H37 0.9600 . ?
C1 H3 0.9600 . ?
C1 H1 0.9600 . ?
C1 H2 0.9600 . ?
C25 C26 1.386(7) . ?
C25 H19 0.9300 . ?
C20 C19 1.361(8) . ?
C20 C21 1.367(8) . ?
C20 H16 0.9300 . ?
C26 C27 1.357(8) . ?
C26 H20 0.9300 . ?
C29 C28 1.379(8) . ?
C29 H23 0.9300 . ?
C19 H15 0.9300 . ?
C21 H17 0.9300 . ?
C27 C28 1.387(10) . ?
C27 H21 0.9300 . ?
C32 H33 0.9600 . ?
C32 H31 0.9600 . ?
C32 H32 0.9600 . ?
C28 H22 0.9300 . ?
O8 C30 1.441(6) . ?
O8 Ni1 2.107(3) 2_666 ?
O8 Dy1 2.325(4) 2_666 ?
O3 C15 1.341(5) . ?
O3 Dy1 2.261(4) 2_666 ?
C15 C14 1.371(7) . ?
C15 C10 1.393(6) . ?
C14 C13 1.379(6) . ?
C14 H13 0.9300 . ?
C10 C11 1.383(6) . ?
C10 C9 1.495(7) . ?
C9 H9 0.9700 . ?
C9 H8 0.9700 . ?
C11 H10 0.9300 . ?
C13 H12 0.9300 . ?
C30 H25 0.9600 . ?
C30 H24 0.9600 . ?
C30 H26 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O3 84.27(15) . 2_666 ?
O2 Dy1 O8 72.95(13) . 2_666 ?
O3 Dy1 O8 70.82(11) 2_666 2_666 ?
O2 Dy1 O6 137.46(11) . . ?
O3 Dy1 O6 78.46(11) 2_666 . ?
O8 Dy1 O6 133.94(14) 2_666 . ?
O2 Dy1 O5 77.12(15) . . ?
O3 Dy1 O5 145.56(11) 2_666 . ?
O8 Dy1 O5 76.08(14) 2_666 . ?
O6 Dy1 O5 133.77(12) . . ?
O2 Dy1 O9 150.79(11) . . ?
O3 Dy1 O9 107.20(17) 2_666 . ?
O8 Dy1 O9 85.35(11) 2_666 . ?
O6 Dy1 O9 71.74(11) . . ?
O5 Dy1 O9 78.85(15) . . ?
O2 Dy1 O10 100.00(16) . . ?
O3 Dy1 O10 142.76(12) 2_666 . ?
O8 Dy1 O10 145.97(11) 2_666 . ?
O6 Dy1 O10 73.62(14) . . ?
O5 Dy1 O10 69.91(15) . . ?
O9 Dy1 O10 87.00(16) . . ?
O2 Dy1 O1 61.97(14) . . ?
O3 Dy1 O1 79.83(15) 2_666 . ?
O8 Dy1 O1 127.98(12) 2_666 . ?
O6 Dy1 O1 76.77(13) . . ?
O5 Dy1 O1 114.91(14) . . ?
O9 Dy1 O1 145.31(11) . . ?
O10 Dy1 O1 70.24(16) . . ?
O2 Dy1 Ni1 35.19(8) . . ?
O3 Dy1 Ni1 80.81(10) 2_666 . ?
O8 Dy1 Ni1 38.62(9) 2_666 . ?
O6 Dy1 Ni1 158.94(8) . . ?
O5 Dy1 Ni1 67.26(12) . . ?
O9 Dy1 Ni1 118.57(9) . . ?
O10 Dy1 Ni1 123.00(10) . . ?
O1 Dy1 Ni1 95.98(12) . . ?
O2 Dy1 Ni1 75.97(14) . 2_666 ?
O3 Dy1 Ni1 35.39(9) 2_666 2_666 ?
O8 Dy1 Ni1 35.43(7) 2_666 2_666 ?
O6 Dy1 Ni1 107.67(11) . 2_666 ?
O5 Dy1 Ni1 111.00(13) . 2_666 ?
O9 Dy1 Ni1 97.66(14) . 2_666 ?
O10 Dy1 Ni1 175.34(9) . 2_666 ?
O1 Dy1 Ni1 105.54(13) . 2_666 ?
Ni1 Dy1 Ni1 54.68(7) . 2_666 ?
N1 C8 C6 127.6(4) . . ?
N1 C8 H7 116.2 . . ?
C6 C8 H7 116.2 . . ?
O2 Ni1 O4 92.24(13) . . ?
O2 Ni1 O8 92.89(13) . . ?
O4 Ni1 O8 169.96(11) . . ?
O2 Ni1 N1 89.79(15) . . ?
O4 Ni1 N1 88.48(16) . . ?
O8 Ni1 N1 100.16(17) . . ?
O2 Ni1 O3 173.36(12) . . ?
O4 Ni1 O3 94.08(13) . . ?
O8 Ni1 O3 81.17(13) . . ?
N1 Ni1 O3 88.37(15) . . ?
O2 Ni1 O8 83.41(14) . 2_666 ?
O4 Ni1 O8 89.22(15) . 2_666 ?
O8 Ni1 O8 82.81(16) . 2_666 ?
N1 Ni1 O8 172.73(13) . 2_666 ?
O3 Ni1 O8 98.68(14) . 2_666 ?
O2 Ni1 Dy1 40.91(10) . . ?
O4 Ni1 Dy1 83.75(11) . . ?
O8 Ni1 Dy1 94.52(11) . . ?
N1 Ni1 Dy1 129.30(11) . . ?
O3 Ni1 Dy1 142.03(10) . . ?
O8 Ni1 Dy1 43.53(8) 2_666 . ?
O2 Ni1 Dy1 134.28(10) . 2_666 ?
O4 Ni1 Dy1 133.17(11) . 2_666 ?
O8 Ni1 Dy1 41.46(10) . 2_666 ?
N1 Ni1 Dy1 95.56(15) . 2_666 ?
O3 Ni1 Dy1 39.71(8) . 2_666 ?
O8 Ni1 Dy1 91.05(14) 2_666 2_666 ?
Dy1 Ni1 Dy1 125.31(7) . 2_666 ?
C7 O2 Ni1 128.6(2) . . ?
C7 O2 Dy1 127.1(3) . . ?
Ni1 O2 Dy1 103.90(14) . . ?
C16 O4 Ni1 126.7(3) . . ?
C16 O5 Dy1 135.6(3) . . ?
C23 O6 Dy1 141.5(3) . . ?
C2 O1 C1 116.2(3) . . ?
C2 O1 Dy1 112.9(3) . . ?
C1 O1 Dy1 129.4(3) . . ?
C32 O9 Dy1 131.0(3) . . ?
C32 O9 H34 114.5 . . ?
Dy1 O9 H34 114.5 . . ?
C31 O10 Dy1 136.2(3) . . ?
C31 O10 H30 111.9 . . ?
Dy1 O10 H30 111.9 . . ?
C33 O11 H38 109.5 . . ?
C8 N1 C9 117.2(3) . . ?
C8 N1 Ni1 125.3(3) . . ?
C9 N1 Ni1 117.1(3) . . ?
O2 C7 C2 117.2(3) . . ?
O2 C7 C6 124.4(4) . . ?
C2 C7 C6 118.3(4) . . ?
C5 C6 C7 118.7(4) . . ?
C5 C6 C8 118.3(4) . . ?
C7 C6 C8 122.9(4) . . ?
O7 C23 O6 124.2(4) . . ?
O7 C23 C24 118.1(4) . . ?
O6 C23 C24 117.7(4) . . ?
C3 C2 O1 125.3(4) . . ?
C3 C2 C7 121.9(4) . . ?
O1 C2 C7 112.8(4) . . ?
C4 C5 C6 121.5(4) . . ?
C4 C5 H6 119.2 . . ?
C6 C5 H6 119.2 . . ?
O4 C16 O5 126.7(4) . . ?
O4 C16 C17 116.5(4) . . ?
O5 C16 C17 116.8(4) . . ?
C18 C17 C22 119.0(4) . . ?
C18 C17 C16 120.4(4) . . ?
C22 C17 C16 120.7(4) . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 H5 119.8 . . ?
C3 C4 H5 119.8 . . ?
C19 C18 C17 120.1(5) . . ?
C19 C18 H14 119.9 . . ?
C17 C18 H14 119.9 . . ?
C2 C3 C4 118.9(4) . . ?
C2 C3 H4 120.5 . . ?
C4 C3 H4 120.5 . . ?
C17 C22 C21 120.4(5) . . ?
C17 C22 H18 119.8 . . ?
C21 C22 H18 119.8 . . ?
C25 C24 C29 119.2(4) . . ?
C25 C24 C23 120.5(4) . . ?
C29 C24 C23 120.2(5) . . ?
C11 C12 C13 119.9(4) . . ?
C11 C12 H11 120.0 . . ?
C13 C12 H11 120.0 . . ?
O10 C31 H28 109.5 . . ?
O10 C31 H29 109.5 . . ?
H28 C31 H29 109.5 . . ?
O10 C31 H27 109.5 . . ?
H28 C31 H27 109.5 . . ?
H29 C31 H27 109.5 . . ?
O11 C33 H35 109.5 . . ?
O11 C33 H36 109.5 . . ?
H35 C33 H36 109.5 . . ?
O11 C33 H37 109.5 . . ?
H35 C33 H37 109.5 . . ?
H36 C33 H37 109.5 . . ?
O1 C1 H3 109.5 . . ?
O1 C1 H1 109.5 . . ?
H3 C1 H1 109.5 . . ?
O1 C1 H2 109.5 . . ?
H3 C1 H2 109.5 . . ?
H1 C1 H2 109.5 . . ?
C24 C25 C26 120.7(5) . . ?
C24 C25 H19 119.6 . . ?
C26 C25 H19 119.6 . . ?
C19 C20 C21 120.3(5) . . ?
C19 C20 H16 119.9 . . ?
C21 C20 H16 119.9 . . ?
C27 C26 C25 119.6(6) . . ?
C27 C26 H20 120.2 . . ?
C25 C26 H20 120.2 . . ?
C24 C29 C28 120.9(6) . . ?
C24 C29 H23 119.6 . . ?
C28 C29 H23 119.6 . . ?
C20 C19 C18 120.5(5) . . ?
C20 C19 H15 119.7 . . ?
C18 C19 H15 119.7 . . ?
C20 C21 C22 119.7(5) . . ?
C20 C21 H17 120.2 . . ?
C22 C21 H17 120.2 . . ?
C26 C27 C28 120.4(5) . . ?
C26 C27 H21 119.8 . . ?
C28 C27 H21 119.8 . . ?
O9 C32 H33 109.5 . . ?
O9 C32 H31 109.5 . . ?
H33 C32 H31 109.5 . . ?
O9 C32 H32 109.5 . . ?
H33 C32 H32 109.5 . . ?
H31 C32 H32 109.5 . . ?
C29 C28 C27 118.9(6) . . ?
C29 C28 H22 120.5 . . ?
C27 C28 H22 120.5 . . ?
C30 O8 Ni1 115.0(3) . . ?
C30 O8 Ni1 113.5(3) . 2_666 ?
Ni1 O8 Ni1 97.19(16) . 2_666 ?
C30 O8 Dy1 125.5(3) . 2_666 ?
Ni1 O8 Dy1 103.11(13) . 2_666 ?
Ni1 O8 Dy1 97.85(14) 2_666 2_666 ?
C15 O3 Ni1 110.9(3) . . ?
C15 O3 Dy1 138.8(2) . 2_666 ?
Ni1 O3 Dy1 104.90(13) . 2_666 ?
O3 C15 C14 121.8(4) . . ?
O3 C15 C10 119.0(4) . . ?
C14 C15 C10 119.2(4) . . ?
C15 C14 C13 121.0(4) . . ?
C15 C14 H13 119.5 . . ?
C13 C14 H13 119.5 . . ?
C11 C10 C15 119.3(4) . . ?
C11 C10 C9 121.8(4) . . ?
C15 C10 C9 118.9(4) . . ?
N1 C9 C10 112.8(3) . . ?
N1 C9 H9 109.0 . . ?
C10 C9 H9 109.0 . . ?
N1 C9 H8 109.0 . . ?
C10 C9 H8 109.0 . . ?
H9 C9 H8 107.8 . . ?
C12 C11 C10 121.0(4) . . ?
C12 C11 H10 119.5 . . ?
C10 C11 H10 119.5 . . ?
C14 C13 C12 119.6(5) . . ?
C14 C13 H12 120.2 . . ?
C12 C13 H12 120.2 . . ?
O8 C30 H25 109.5 . . ?
O8 C30 H24 109.5 . . ?
H25 C30 H24 109.5 . . ?
O8 C30 H26 109.5 . . ?
H25 C30 H26 109.5 . . ?
H24 C30 H26 109.5 . . ?

_refine_diff_density_max         3.634
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.155



####################################################################### 
# 
# 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_Complex2
_database_code_depnum_ccdc_archive 'CCDC 2062615'
loop_
_audit_author_name
_audit_author_address
'Debashis Ray'
;IIT Kharagpur
India
;
_audit_update_record             
;
2021-02-11 deposited with the CCDC.	2021-07-26 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         'C64 H68 N2 Ni2 O20 Tb2, (2CH3OH)'
_chemical_formula_sum            'C66 H76 N2 Ni2 O22 Tb2'
_chemical_formula_weight         1684.54

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

_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                   11.272(10)
_cell_length_b                   11.493(12)
_cell_length_c                   13.955(12)
_cell_angle_alpha                78.47(2)
_cell_angle_beta                 76.06(2)
_cell_angle_gamma                89.62(4)
_cell_volume                     1718(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    5786
_cell_measurement_theta_min      3.014
_cell_measurement_theta_max      26.586

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_F_000             848
_exptl_transmission_factor_min   .690
_exptl_transmission_factor_max   .767
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .10
_exptl_absorpt_coefficient_mu    2.649
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      290(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX-II'
_diffrn_measurement_method       'CCD area detector,ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21741
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.014
_diffrn_reflns_theta_max         26.586
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7022
_reflns_number_gt                5786
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       SMART
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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)+(0.0268P)²+0.4526P] 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         7022
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0587
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.31715(2) 0.55196(2) 0.68335(2) 0.03042(6) Uani 1 1 d . . . . .
Ni1 Ni 0.48856(4) 0.63122(3) 0.44450(3) 0.02735(10) Uani 1 1 d . . . . .
O10 O 0.6251(2) 0.51867(17) 0.46788(16) 0.0283(5) Uani 1 1 d . . . . .
O2 O 0.4697(2) 0.67903(18) 0.57833(16) 0.0319(5) Uani 1 1 d . . . . .
O3 O 0.5293(2) 0.57862(19) 0.30745(16) 0.0339(5) Uani 1 1 d . . . . .
O4 O 0.3377(2) 0.71787(19) 0.41922(17) 0.0347(5) Uani 1 1 d . . . . .
O6 O 0.2622(2) 0.4608(2) 0.85547(18) 0.0450(7) Uani 1 1 d . . . . .
O5 O 0.2154(2) 0.6718(2) 0.57467(18) 0.0410(6) Uani 1 1 d . . . . .
O1 O 0.4547(3) 0.6718(2) 0.76502(19) 0.0470(7) Uani 1 1 d . . . . .
O8 O 0.1277(3) 0.4355(2) 0.7162(2) 0.0517(7) Uani 1 1 d . . . . .
H8 H 0.1158 0.3739 0.7725 0.062 Uiso 1 1 calc R U . . .
N1 N 0.5905(3) 0.7859(2) 0.3743(2) 0.0347(7) Uani 1 1 d . . . . .
O9 O 0.1971(3) 0.6900(2) 0.7717(2) 0.0575(8) Uani 1 1 d . . . . .
H9 H 0.1534 0.6537 0.8361 0.069 Uiso 1 1 calc R U . . .
O7 O 0.1576(3) 0.5726(3) 0.9556(2) 0.0709(10) Uani 1 1 d . . . . .
C16 C 0.2387(3) 0.7191(3) 0.4821(3) 0.0330(7) Uani 1 1 d . . . . .
C7 C 0.5206(3) 0.7715(3) 0.5986(3) 0.0307(7) Uani 1 1 d . . . . .
C15 C 0.4926(3) 0.6570(3) 0.2364(2) 0.0375(8) Uani 1 1 d . . . . .
C6 C 0.5852(3) 0.8663(3) 0.5248(3) 0.0338(8) Uani 1 1 d . . . . .
C2 C 0.5098(3) 0.7739(3) 0.7003(3) 0.0381(8) Uani 1 1 d . . . . .
C8 C 0.6108(3) 0.8690(3) 0.4178(3) 0.0390(8) Uani 1 1 d . . . . .
H8A H 0.6462 0.9396 0.3756 0.047 Uiso 1 1 calc R U . . .
C17 C 0.1383(3) 0.7830(3) 0.4437(3) 0.0362(8) Uani 1 1 d . . . . .
C32 C 0.7085(4) 0.5600(3) 0.5203(3) 0.0475(10) Uani 1 1 d . . . . .
H32A H 0.7447 0.6362 0.4836 0.071 Uiso 1 1 calc R U . . .
H32B H 0.7717 0.5042 0.5251 0.071 Uiso 1 1 calc R U . . .
H32C H 0.6642 0.5667 0.5868 0.071 Uiso 1 1 calc R U . . .
O11 O -0.0091(4) 0.3276(3) 0.9013(3) 0.0819(11) Uani 1 1 d . . . . .
H11 H -0.0587 0.3634 0.9367 0.123 Uiso 1 1 calc R U . . .
C23 C 0.2073(4) 0.4782(4) 0.9409(3) 0.0494(10) Uani 1 1 d . . . . .
C14 C 0.4078(4) 0.6251(4) 0.1877(3) 0.0518(10) Uani 1 1 d . . . . .
H14 H 0.3772 0.5469 0.2025 0.062 Uiso 1 1 calc R U . . .
C5 C 0.6262(3) 0.9639(3) 0.5564(3) 0.0422(9) Uani 1 1 d . . . . .
H5 H 0.6670 1.0279 0.5081 0.051 Uiso 1 1 calc R U . . .
C10 C 0.5388(4) 0.7752(3) 0.2127(3) 0.0438(9) Uani 1 1 d . . . . .
C18 C 0.1513(4) 0.8249(3) 0.3415(3) 0.0498(10) Uani 1 1 d . . . . .
H18 H 0.2232 0.8136 0.2957 0.060 Uiso 1 1 calc R U . . .
C9 C 0.6330(4) 0.8066(3) 0.2632(3) 0.0487(10) Uani 1 1 d . . . . .
H9A H 0.7042 0.7601 0.2457 0.058 Uiso 1 1 calc R U . . .
H9B H 0.6581 0.8898 0.2375 0.058 Uiso 1 1 calc R U . . .
C3 C 0.5509(4) 0.8714(3) 0.7288(3) 0.0481(10) Uani 1 1 d . . . . .
H3 H 0.5406 0.8728 0.7967 0.058 Uiso 1 1 calc R U . . .
C4 C 0.6080(4) 0.9674(3) 0.6550(3) 0.0494(10) Uani 1 1 d . . . . .
H4 H 0.6337 1.0345 0.6736 0.059 Uiso 1 1 calc R U . . .
C24 C 0.2020(4) 0.3797(4) 1.0312(3) 0.0497(10) Uani 1 1 d . . . . .
C1 C 0.4612(5) 0.6564(4) 0.8679(3) 0.0694(14) Uani 1 1 d . . . . .
H1A H 0.5435 0.6737 0.8703 0.104 Uiso 1 1 calc R U . . .
H1B H 0.4375 0.5757 0.9019 0.104 Uiso 1 1 calc R U . . .
H1C H 0.4071 0.7093 0.9006 0.104 Uiso 1 1 calc R U . . .
C11 C 0.4973(5) 0.8570(4) 0.1410(3) 0.0607(13) Uani 1 1 d . . . . .
H11A H 0.5274 0.9354 0.1247 0.073 Uiso 1 1 calc R U . . .
C22 C 0.0303(4) 0.8008(4) 0.5094(4) 0.0627(13) Uani 1 1 d . . . . .
H22 H 0.0200 0.7734 0.5784 0.075 Uiso 1 1 calc R U . . .
C31 C 0.1776(5) 0.8108(4) 0.7492(4) 0.0799(17) Uani 1 1 d . . . . .
H31A H 0.2281 0.8531 0.7784 0.120 Uiso 1 1 calc R U . . .
H31B H 0.0931 0.8243 0.7764 0.120 Uiso 1 1 calc R U . . .
H31C H 0.1980 0.8385 0.6774 0.120 Uiso 1 1 calc R U . . .
C25 C 0.2496(5) 0.2732(4) 1.0194(3) 0.0676(13) Uani 1 1 d . . . . .
H25 H 0.2878 0.2619 0.9552 0.081 Uiso 1 1 calc R U . . .
C13 C 0.3686(5) 0.7085(5) 0.1177(3) 0.0677(14) Uani 1 1 d . . . . .
H13 H 0.3113 0.6861 0.0860 0.081 Uiso 1 1 calc R U . . .
C30 C 0.0309(5) 0.4433(5) 0.6658(4) 0.0744(15) Uani 1 1 d . . . . .
H30A H 0.0308 0.5225 0.6275 0.112 Uiso 1 1 calc R U . . .
H30B H -0.0459 0.4245 0.7147 0.112 Uiso 1 1 calc R U . . .
H30C H 0.0428 0.3881 0.6214 0.112 Uiso 1 1 calc R U . . .
C12 C 0.4129(5) 0.8239(5) 0.0942(3) 0.0740(16) Uani 1 1 d . . . . .
H12 H 0.3860 0.8796 0.0468 0.089 Uiso 1 1 calc R U . . .
C20 C -0.0472(5) 0.9004(5) 0.3732(5) 0.0861(18) Uani 1 1 d . . . . .
H20 H -0.1094 0.9409 0.3494 0.103 Uiso 1 1 calc R U . . .
C26 C 0.2417(5) 0.1808(5) 1.1020(4) 0.0812(16) Uani 1 1 d . . . . .
H26 H 0.2722 0.1074 1.0927 0.097 Uiso 1 1 calc R U . . .
C29 C 0.1533(6) 0.3961(5) 1.1261(4) 0.108(2) Uani 1 1 d . . . . .
H29 H 0.1232 0.4695 1.1356 0.129 Uiso 1 1 calc R U . . .
C19 C 0.0578(5) 0.8833(4) 0.3079(4) 0.0729(15) Uani 1 1 d . . . . .
H19 H 0.0669 0.9114 0.2391 0.087 Uiso 1 1 calc R U . . .
C21 C -0.0622(5) 0.8586(5) 0.4737(5) 0.0907(19) Uani 1 1 d . . . . .
H21 H -0.1353 0.8691 0.5185 0.109 Uiso 1 1 calc R U . . .
C27 C 0.1900(5) 0.1974(5) 1.1959(4) 0.0869(19) Uani 1 1 d . . . . .
H27 H 0.1835 0.1352 1.2513 0.104 Uiso 1 1 calc R U . . .
C28 C 0.1476(7) 0.3049(6) 1.2090(4) 0.137(3) Uani 1 1 d . . . . .
H28 H 0.1146 0.3177 1.2737 0.164 Uiso 1 1 calc R U . . .
C33 C -0.0234(6) 0.2040(5) 0.9437(5) 0.112(2) Uani 1 1 d . . . . .
H33A H -0.0041 0.1895 1.0083 0.167 Uiso 1 1 calc R U . . .
H33B H 0.0306 0.1615 0.8998 0.167 Uiso 1 1 calc R U . . .
H33C H -0.1065 0.1775 0.9517 0.167 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O2 2.281(3) . ?
Tb1 O3 2.293(3) 2_666 ?
Tb1 O5 2.344(3) . ?
Tb1 O6 2.353(3) . ?
Tb1 O10 2.356(3) 2_666 ?
Tb1 O9 2.412(3) . ?
Tb1 O8 2.426(3) . ?
Tb1 O1 2.665(3) . ?
Tb1 Ni1 3.373(2) . ?
Tb1 Ni1 3.460(2) 2_666 ?
Ni1 O2 2.013(3) . ?
Ni1 O4 2.033(3) . ?
Ni1 O10 2.048(3) . ?
Ni1 N1 2.057(3) . ?
Ni1 O3 2.066(3) . ?
Ni1 O10 2.130(3) 2_666 ?
Ni1 Tb1 3.460(2) 2_666 ?
O10 C32 1.457(4) . ?
O10 Ni1 2.130(3) 2_666 ?
O10 Tb1 2.356(3) 2_666 ?
O2 C7 1.321(4) . ?
O3 C15 1.342(4) . ?
O3 Tb1 2.294(3) 2_666 ?
O4 C16 1.245(4) . ?
O6 C23 1.258(4) . ?
O5 C16 1.261(4) . ?
O1 C2 1.377(4) . ?
O1 C1 1.431(4) . ?
O8 C30 1.427(5) . ?
O8 H8 0.9300 . ?
N1 C8 1.278(4) . ?
N1 C9 1.478(4) . ?
O9 C31 1.389(5) . ?
O9 H9 0.9300 . ?
O7 C23 1.248(5) . ?
C16 C17 1.494(5) . ?
C7 C2 1.402(5) . ?
C7 C6 1.406(5) . ?
C15 C14 1.389(5) . ?
C15 C10 1.405(5) . ?
C6 C5 1.402(5) . ?
C6 C8 1.445(5) . ?
C2 C3 1.379(5) . ?
C8 H8A 0.9300 . ?
C17 C22 1.377(5) . ?
C17 C18 1.382(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O11 C33 1.419(6) . ?
O11 H11 0.8200 . ?
C23 C24 1.506(5) . ?
C14 C13 1.377(6) . ?
C14 H14 0.9300 . ?
C5 C4 1.350(5) . ?
C5 H5 0.9300 . ?
C10 C11 1.396(5) . ?
C10 C9 1.490(6) . ?
C18 C19 1.373(6) . ?
C18 H18 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C3 C4 1.388(5) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C24 C25 1.358(6) . ?
C24 C29 1.356(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C11 C12 1.370(7) . ?
C11 H11A 0.9300 . ?
C22 C21 1.373(6) . ?
C22 H22 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C25 C26 1.388(6) . ?
C25 H25 0.9300 . ?
C13 C12 1.369(7) . ?
C13 H13 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C12 H12 0.9300 . ?
C20 C19 1.348(7) . ?
C20 C21 1.359(7) . ?
C20 H20 0.9300 . ?
C26 C27 1.351(7) . ?
C26 H26 0.9300 . ?
C29 C28 1.387(7) . ?
C29 H29 0.9300 . ?
C19 H19 0.9300 . ?
C21 H21 0.9300 . ?
C27 C28 1.353(8) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Tb1 O3 84.34(11) . 2_666 ?
O2 Tb1 O5 77.06(10) . . ?
O3 Tb1 O5 144.87(9) 2_666 . ?
O2 Tb1 O6 136.80(9) . . ?
O3 Tb1 O6 78.92(9) 2_666 . ?
O5 Tb1 O6 134.01(10) . . ?
O2 Tb1 O10 73.33(9) . 2_666 ?
O3 Tb1 O10 70.41(9) 2_666 2_666 ?
O5 Tb1 O10 75.77(10) . 2_666 ?
O6 Tb1 O10 134.39(10) . 2_666 ?
O2 Tb1 O9 99.71(11) . . ?
O3 Tb1 O9 142.54(10) 2_666 . ?
O5 Tb1 O9 70.83(11) . . ?
O6 Tb1 O9 72.83(10) . . ?
O10 Tb1 O9 146.58(9) 2_666 . ?
O2 Tb1 O8 151.59(9) . . ?
O3 Tb1 O8 107.46(12) 2_666 . ?
O5 Tb1 O8 78.99(11) . . ?
O6 Tb1 O8 71.56(10) . . ?
O10 Tb1 O8 86.17(9) 2_666 . ?
O9 Tb1 O8 86.54(12) . . ?
O2 Tb1 O1 61.60(10) . . ?
O3 Tb1 O1 80.78(11) 2_666 . ?
O5 Tb1 O1 114.50(11) . . ?
O6 Tb1 O1 76.47(10) . . ?
O10 Tb1 O1 128.28(9) 2_666 . ?
O9 Tb1 O1 69.18(11) . . ?
O8 Tb1 O1 144.42(9) . . ?
O2 Tb1 Ni1 35.49(6) . . ?
O3 Tb1 Ni1 80.82(7) 2_666 . ?
O5 Tb1 Ni1 66.71(8) . . ?
O6 Tb1 Ni1 159.28(7) . . ?
O10 Tb1 Ni1 38.76(6) 2_666 . ?
O9 Tb1 Ni1 123.05(8) . . ?
O8 Tb1 Ni1 119.27(7) . . ?
O1 Tb1 Ni1 96.04(8) . . ?
O2 Tb1 Ni1 76.16(9) . 2_666 ?
O3 Tb1 Ni1 35.25(7) 2_666 2_666 ?
O5 Tb1 Ni1 110.42(8) . 2_666 ?
O6 Tb1 Ni1 108.23(8) . 2_666 ?
O10 Tb1 Ni1 35.17(6) 2_666 2_666 ?
O9 Tb1 Ni1 175.06(8) . 2_666 ?
O8 Tb1 Ni1 98.38(10) . 2_666 ?
O1 Tb1 Ni1 106.21(9) . 2_666 ?
Ni1 Tb1 Ni1 54.75(5) . 2_666 ?
O2 Ni1 O4 92.41(10) . . ?
O2 Ni1 O10 92.67(10) . . ?
O4 Ni1 O10 170.22(9) . . ?
O2 Ni1 N1 89.60(11) . . ?
O4 Ni1 N1 88.19(12) . . ?
O10 Ni1 N1 100.20(12) . . ?
O2 Ni1 O3 173.19(10) . . ?
O4 Ni1 O3 93.99(10) . . ?
O10 Ni1 O3 81.34(10) . . ?
N1 Ni1 O3 88.28(11) . . ?
O2 Ni1 O10 83.86(10) . 2_666 ?
O4 Ni1 O10 89.81(11) . 2_666 ?
O10 Ni1 O10 82.44(11) . 2_666 ?
N1 Ni1 O10 173.07(10) . 2_666 ?
O3 Ni1 O10 98.48(10) . 2_666 ?
O2 Ni1 Tb1 41.13(7) . . ?
O4 Ni1 Tb1 83.92(8) . . ?
O10 Ni1 Tb1 94.46(7) . . ?
N1 Ni1 Tb1 129.29(9) . . ?
O3 Ni1 Tb1 142.12(8) . . ?
O10 Ni1 Tb1 43.85(6) 2_666 . ?
O2 Ni1 Tb1 134.11(7) . 2_666 ?
O4 Ni1 Tb1 133.20(8) . 2_666 ?
O10 Ni1 Tb1 41.51(7) . 2_666 ?
N1 Ni1 Tb1 95.65(11) . 2_666 ?
O3 Ni1 Tb1 39.83(7) . 2_666 ?
O10 Ni1 Tb1 90.56(9) 2_666 2_666 ?
Tb1 Ni1 Tb1 125.25(5) . 2_666 ?
C32 O10 Ni1 114.9(2) . . ?
C32 O10 Ni1 113.3(2) . 2_666 ?
Ni1 O10 Ni1 97.56(11) . 2_666 ?
C32 O10 Tb1 125.7(2) . 2_666 ?
Ni1 O10 Tb1 103.32(10) . 2_666 ?
Ni1 O10 Tb1 97.39(10) 2_666 2_666 ?
C7 O2 Ni1 128.7(2) . . ?
C7 O2 Tb1 127.4(2) . . ?
Ni1 O2 Tb1 103.38(10) . . ?
C15 O3 Ni1 111.6(2) . . ?
C15 O3 Tb1 138.0(2) . 2_666 ?
Ni1 O3 Tb1 104.92(10) . 2_666 ?
C16 O4 Ni1 126.5(2) . . ?
C23 O6 Tb1 142.6(3) . . ?
C16 O5 Tb1 136.6(2) . . ?
C2 O1 C1 116.9(3) . . ?
C2 O1 Tb1 112.8(2) . . ?
C1 O1 Tb1 129.3(2) . . ?
C30 O8 Tb1 132.4(3) . . ?
C30 O8 H8 113.8 . . ?
Tb1 O8 H8 113.8 . . ?
C8 N1 C9 117.9(3) . . ?
C8 N1 Ni1 125.3(2) . . ?
C9 N1 Ni1 116.5(2) . . ?
C31 O9 Tb1 135.3(3) . . ?
C31 O9 H9 112.4 . . ?
Tb1 O9 H9 112.4 . . ?
O4 C16 O5 126.2(3) . . ?
O4 C16 C17 116.5(3) . . ?
O5 C16 C17 117.3(3) . . ?
O2 C7 C2 117.4(3) . . ?
O2 C7 C6 124.2(3) . . ?
C2 C7 C6 118.4(3) . . ?
O3 C15 C14 121.7(3) . . ?
O3 C15 C10 119.1(3) . . ?
C14 C15 C10 119.2(3) . . ?
C7 C6 C5 118.5(3) . . ?
C7 C6 C8 123.3(3) . . ?
C5 C6 C8 118.1(3) . . ?
O1 C2 C3 125.5(3) . . ?
O1 C2 C7 113.1(3) . . ?
C3 C2 C7 121.3(3) . . ?
N1 C8 C6 127.8(3) . . ?
N1 C8 H8A 116.1 . . ?
C6 C8 H8A 116.1 . . ?
C22 C17 C18 118.5(4) . . ?
C22 C17 C16 120.6(4) . . ?
C18 C17 C16 120.8(3) . . ?
O10 C32 H32A 109.5 . . ?
O10 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O10 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C33 O11 H11 109.5 . . ?
O7 C23 O6 124.0(4) . . ?
O7 C23 C24 117.8(4) . . ?
O6 C23 C24 118.1(4) . . ?
C13 C14 C15 120.4(4) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C4 C5 C6 121.8(3) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C11 C10 C15 118.7(4) . . ?
C11 C10 C9 123.0(4) . . ?
C15 C10 C9 118.3(3) . . ?
C19 C18 C17 119.9(4) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
N1 C9 C10 113.8(3) . . ?
N1 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N1 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C2 C3 C4 119.3(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C25 C24 C29 118.4(4) . . ?
C25 C24 C23 120.5(4) . . ?
C29 C24 C23 121.1(4) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C12 C11 C10 121.3(4) . . ?
C12 C11 H11A 119.4 . . ?
C10 C11 H11A 119.4 . . ?
C21 C22 C17 120.5(5) . . ?
C21 C22 H22 119.8 . . ?
C17 C22 H22 119.8 . . ?
O9 C31 H31A 109.5 . . ?
O9 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O9 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C24 C25 C26 120.8(5) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C12 C13 C14 120.8(5) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
O8 C30 H30A 109.5 . . ?
O8 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O8 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C11 C12 C13 119.6(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C19 C20 C21 120.1(5) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C27 C26 C25 120.1(5) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C24 C29 C28 120.9(6) . . ?
C24 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C20 C19 C18 120.9(5) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C20 C21 C22 120.1(5) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C26 C27 C28 119.6(5) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C27 C28 C29 120.0(6) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
O11 C33 H33A 109.5 . . ?
O11 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O11 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_refine_diff_density_max         0.611
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.100



####################################################################### 
# 
# 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_Complex4
_database_code_depnum_ccdc_archive 'CCDC 2062617'
loop_
_audit_author_name
_audit_author_address
'Debashis Ray'
;IIT Kharagpur
India
;
_audit_update_record             
;
2021-02-11 deposited with the CCDC.	2021-07-26 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         'C64 H68 Ho2 N2 Ni2 O20, 2(CH3OH)'
_chemical_formula_sum            'C66 H76 Ho2 N2 Ni2 O22'
_chemical_formula_weight         1696.56

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   11.072(9)
_cell_length_b                   11.326(10)
_cell_length_c                   13.677(11)
_cell_angle_alpha                101.34(3)
_cell_angle_beta                 103.396(12)
_cell_angle_gamma                90.601(11)
_cell_volume                     1633(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6068
_cell_measurement_theta_min      1.564
_cell_measurement_theta_max      26.408

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_F_000             852
_exptl_transmission_factor_min   .584
_exptl_transmission_factor_max   .694
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    3.043
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX-II'
_diffrn_measurement_method       'CCD area detector,ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20893
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.564
_diffrn_reflns_theta_max         26.408
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             6480
_reflns_number_gt                6068
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       SMART
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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)+(0.0352P)²+2.6939P] 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         6480
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0724
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ho1 Ho 0.68392(2) 0.44883(2) 0.68298(2) 0.01261(6) Uani 1 1 d . . . . .
Ni1 Ni 0.51064(4) 0.36883(3) 0.44324(3) 0.01133(10) Uani 1 1 d . . . . .
O3 O 0.4690(2) 0.4224(2) 0.30517(18) 0.0149(5) Uani 1 1 d . . . . .
O2 O 0.5303(2) 0.3207(2) 0.57825(17) 0.0138(5) Uani 1 1 d . . . . .
O8 O 0.3728(2) 0.48045(19) 0.46859(17) 0.0123(5) Uani 1 1 d . . . . .
O4 O 0.6627(2) 0.2826(2) 0.41597(18) 0.0155(5) Uani 1 1 d . . . . .
O6 O 0.7391(2) 0.5411(2) 0.85574(18) 0.0182(5) Uani 1 1 d . . . . .
O5 O 0.7872(2) 0.3301(2) 0.57335(18) 0.0177(5) Uani 1 1 d . . . . .
O1 O 0.5442(2) 0.3304(2) 0.76723(19) 0.0204(5) Uani 1 1 d . . . . .
O10 O 0.8722(2) 0.5673(2) 0.71422(19) 0.0213(5) Uani 1 1 d . . . . .
H10 H 0.8847 0.6296 0.7717 0.026 Uiso 1 1 calc R U . . .
O7 O 0.8414(3) 0.4261(2) 0.9561(2) 0.0303(6) Uani 1 1 d . . . . .
O9 O 0.8032(3) 0.3121(2) 0.7696(2) 0.0264(6) Uani 1 1 d . . . . .
H9 H 0.8469 0.3493 0.8353 0.032 Uiso 1 1 calc R U . . .
N1 N 0.4065(3) 0.2120(2) 0.3728(2) 0.0145(6) Uani 1 1 d . . . . .
O11 O 1.0081(3) 0.6724(3) 0.9013(2) 0.0324(7) Uani 1 1 d . . . . .
H11A H 1.0577 0.6345 0.9357 0.049 Uiso 1 1 calc R U . . .
C6 C 0.4138(3) 0.1297(3) 0.5248(3) 0.0144(7) Uani 1 1 d . . . . .
C8 C 0.3877(3) 0.1266(3) 0.4164(3) 0.0166(7) Uani 1 1 d . . . . .
H8 H 0.3533 0.0541 0.3734 0.020 Uiso 1 1 calc R U . . .
C16 C 0.7623(3) 0.2814(3) 0.4799(3) 0.0145(7) Uani 1 1 d . . . . .
C7 C 0.4791(3) 0.2273(3) 0.5993(3) 0.0143(7) Uani 1 1 d . . . . .
C4 C 0.3923(3) 0.0274(3) 0.6589(3) 0.0197(7) Uani 1 1 d . . . . .
H4 H 0.3665 -0.0410 0.6785 0.024 Uiso 1 1 calc R U . . .
C17 C 0.8638(3) 0.2160(3) 0.4397(3) 0.0160(7) Uani 1 1 d . . . . .
C14 C 0.5958(4) 0.3783(3) 0.1858(3) 0.0214(8) Uani 1 1 d . . . . .
H14 H 0.6268 0.4582 0.2015 0.026 Uiso 1 1 calc R U . . .
C2 C 0.4901(3) 0.2252(3) 0.7031(3) 0.0172(7) Uani 1 1 d . . . . .
C18 C 0.8503(4) 0.1760(3) 0.3361(3) 0.0226(8) Uani 1 1 d . . . . .
H18 H 0.7783 0.1898 0.2900 0.027 Uiso 1 1 calc R U . . .
C9 C 0.3641(3) 0.1903(3) 0.2601(3) 0.0203(7) Uani 1 1 d . . . . .
H9A H 0.2914 0.2359 0.2421 0.024 Uiso 1 1 calc R U . . .
H9B H 0.3392 0.1055 0.2341 0.024 Uiso 1 1 calc R U . . .
C32 C 0.2890(3) 0.4372(3) 0.5208(3) 0.0213(8) Uani 1 1 d . . . . .
H32A H 0.2551 0.3581 0.4847 0.032 Uiso 1 1 calc R U . . .
H32B H 0.2228 0.4909 0.5235 0.032 Uiso 1 1 calc R U . . .
H32C H 0.3329 0.4337 0.5894 0.032 Uiso 1 1 calc R U . . .
C10 C 0.4603(3) 0.2246(3) 0.2089(3) 0.0170(7) Uani 1 1 d . . . . .
C23 C 0.7932(4) 0.5228(3) 0.9419(3) 0.0231(8) Uani 1 1 d . . . . .
C24 C 0.7982(3) 0.6201(3) 1.0342(3) 0.0226(8) Uani 1 1 d . . . . .
C5 C 0.3730(3) 0.0306(3) 0.5579(3) 0.0185(7) Uani 1 1 d . . . . .
H5 H 0.3313 -0.0351 0.5093 0.022 Uiso 1 1 calc R U . . .
C12 C 0.5923(4) 0.1761(4) 0.0912(3) 0.0276(9) Uani 1 1 d . . . . .
H12 H 0.6214 0.1194 0.0444 0.033 Uiso 1 1 calc R U . . .
C3 C 0.4508(3) 0.1261(3) 0.7332(3) 0.0206(8) Uani 1 1 d . . . . .
H3 H 0.4630 0.1248 0.8026 0.025 Uiso 1 1 calc R U . . .
C15 C 0.5074(3) 0.3444(3) 0.2337(3) 0.0168(7) Uani 1 1 d . . . . .
C13 C 0.6383(4) 0.2954(4) 0.1152(3) 0.0253(8) Uani 1 1 d . . . . .
H13 H 0.6977 0.3193 0.0838 0.030 Uiso 1 1 calc R U . . .
C11 C 0.5028(4) 0.1427(3) 0.1376(3) 0.0244(8) Uani 1 1 d . . . . .
H11 H 0.4705 0.0632 0.1203 0.029 Uiso 1 1 calc R U . . .
C20 C 1.0501(4) 0.0955(4) 0.3674(4) 0.0347(10) Uani 1 1 d . . . . .
H20 H 1.1133 0.0554 0.3428 0.042 Uiso 1 1 calc R U . . .
C22 C 0.9706(4) 0.1951(3) 0.5080(3) 0.0262(8) Uani 1 1 d . . . . .
H22 H 0.9795 0.2215 0.5782 0.031 Uiso 1 1 calc R U . . .
C26 C 0.7679(4) 0.8238(4) 1.1077(3) 0.0322(9) Uani 1 1 d . . . . .
H26 H 0.7440 0.9003 1.0990 0.039 Uiso 1 1 calc R U . . .
C30 C 0.8246(4) 0.1888(3) 0.7468(3) 0.0291(9) Uani 1 1 d . . . . .
H30A H 0.7735 0.1445 0.7768 0.044 Uiso 1 1 calc R U . . .
H30B H 0.9106 0.1772 0.7743 0.044 Uiso 1 1 calc R U . . .
H30C H 0.8043 0.1604 0.6737 0.044 Uiso 1 1 calc R U . . .
C25 C 0.7584(4) 0.7321(4) 1.0234(3) 0.0293(9) Uani 1 1 d . . . . .
H25 H 0.7244 0.7461 0.9582 0.035 Uiso 1 1 calc R U . . .
C1 C 0.5383(4) 0.3445(4) 0.8716(3) 0.0287(9) Uani 1 1 d . . . . .
H1A H 0.4550 0.3246 0.8747 0.043 Uiso 1 1 calc R U . . .
H1B H 0.5618 0.4266 0.9063 0.043 Uiso 1 1 calc R U . . .
H1C H 0.5941 0.2918 0.9042 0.043 Uiso 1 1 calc R U . . .
C29 C 0.8397(5) 0.5980(4) 1.1314(3) 0.0413(12) Uani 1 1 d . . . . .
H29 H 0.8642 0.5216 1.1398 0.050 Uiso 1 1 calc R U . . .
C31 C 0.9708(4) 0.5612(4) 0.6611(3) 0.0311(9) Uani 1 1 d . . . . .
H31A H 0.9667 0.4828 0.6177 0.047 Uiso 1 1 calc R U . . .
H31B H 1.0496 0.5750 0.7102 0.047 Uiso 1 1 calc R U . . .
H31C H 0.9619 0.6216 0.6199 0.047 Uiso 1 1 calc R U . . .
C21 C 1.0642(4) 0.1348(4) 0.4714(4) 0.0347(10) Uani 1 1 d . . . . .
H21 H 1.1365 0.1209 0.5170 0.042 Uiso 1 1 calc R U . . .
C28 C 0.8452(5) 0.6883(5) 1.2167(4) 0.0441(12) Uani 1 1 d . . . . .
H28 H 0.8709 0.6724 1.2823 0.053 Uiso 1 1 calc R U . . .
C19 C 0.9444(4) 0.1151(4) 0.3005(3) 0.0306(9) Uani 1 1 d . . . . .
H19 H 0.9352 0.0874 0.2304 0.037 Uiso 1 1 calc R U . . .
C33 C 1.0260(5) 0.7959(4) 0.9468(4) 0.0414(11) Uani 1 1 d . . . . .
H33A H 1.0143 0.8078 1.0153 0.062 Uiso 1 1 calc R U . . .
H33B H 0.9670 0.8401 0.9071 0.062 Uiso 1 1 calc R U . . .
H33C H 1.1089 0.8240 0.9489 0.062 Uiso 1 1 calc R U . . .
C27 C 0.8123(4) 0.8027(4) 1.2036(4) 0.0371(10) Uani 1 1 d . . . . .
H27 H 0.8205 0.8652 1.2606 0.045 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O2 2.248(3) . ?
Ho1 O3 2.260(3) 2_666 ?
Ho1 O8 2.322(3) 2_666 ?
Ho1 O6 2.323(3) . ?
Ho1 O5 2.323(3) . ?
Ho1 O9 2.363(3) . ?
Ho1 O10 2.373(3) . ?
Ho1 O1 2.629(3) . ?
Ho1 Ni1 3.337(2) . ?
Ho1 Ni1 3.4143(19) 2_666 ?
Ni1 O2 1.991(3) . ?
Ni1 O4 2.028(3) . ?
Ni1 O8 2.039(3) . ?
Ni1 N1 2.046(3) . ?
Ni1 O3 2.049(3) . ?
Ni1 O8 2.111(3) 2_666 ?
Ni1 Ho1 3.4143(19) 2_666 ?
O3 C15 1.333(4) . ?
O3 Ho1 2.260(3) 2_666 ?
O2 C7 1.306(4) . ?
O8 C32 1.431(4) . ?
O8 Ni1 2.111(3) 2_666 ?
O8 Ho1 2.322(3) 2_666 ?
O4 C16 1.240(4) . ?
O6 C23 1.250(5) . ?
O5 C16 1.253(4) . ?
O1 C2 1.370(4) . ?
O1 C1 1.422(4) . ?
O10 C31 1.441(5) . ?
O10 H10 0.9300 . ?
O7 C23 1.252(5) . ?
O9 C30 1.405(4) . ?
O9 H9 0.9300 . ?
N1 C8 1.270(4) . ?
N1 C9 1.473(5) . ?
O11 C33 1.406(5) . ?
O11 H11A 0.8200 . ?
C6 C5 1.398(5) . ?
C6 C7 1.408(5) . ?
C6 C8 1.437(5) . ?
C8 H8 0.9300 . ?
C16 C17 1.503(5) . ?
C7 C2 1.401(5) . ?
C4 C5 1.355(5) . ?
C4 C3 1.391(5) . ?
C4 H4 0.9300 . ?
C17 C18 1.373(5) . ?
C17 C22 1.381(5) . ?
C14 C13 1.377(5) . ?
C14 C15 1.388(5) . ?
C14 H14 0.9300 . ?
C2 C3 1.369(5) . ?
C18 C19 1.385(6) . ?
C18 H18 0.9300 . ?
C9 C10 1.490(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C10 C11 1.378(5) . ?
C10 C15 1.397(5) . ?
C23 C24 1.494(5) . ?
C24 C25 1.371(6) . ?
C24 C29 1.375(6) . ?
C5 H5 0.9300 . ?
C12 C11 1.380(6) . ?
C12 C13 1.388(6) . ?
C12 H12 0.9300 . ?
C3 H3 0.9300 . ?
C13 H13 0.9300 . ?
C11 H11 0.9300 . ?
C20 C19 1.359(6) . ?
C20 C21 1.376(7) . ?
C20 H20 0.9300 . ?
C22 C21 1.382(6) . ?
C22 H22 0.9300 . ?
C26 C27 1.359(6) . ?
C26 C25 1.374(6) . ?
C26 H26 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C25 H25 0.9300 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C29 C28 1.381(6) . ?
C29 H29 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C21 H21 0.9300 . ?
C28 C27 1.383(7) . ?
C28 H28 0.9300 . ?
C19 H19 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C27 H27 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ho1 O3 84.44(10) . 2_666 ?
O2 Ho1 O8 73.41(9) . 2_666 ?
O3 Ho1 O8 71.11(9) 2_666 2_666 ?
O2 Ho1 O6 136.87(9) . . ?
O3 Ho1 O6 78.19(9) 2_666 . ?
O8 Ho1 O6 134.07(9) 2_666 . ?
O2 Ho1 O5 77.51(10) . . ?
O3 Ho1 O5 145.75(9) 2_666 . ?
O8 Ho1 O5 75.90(10) 2_666 . ?
O6 Ho1 O5 133.79(9) . . ?
O2 Ho1 O9 99.73(11) . . ?
O3 Ho1 O9 142.29(9) 2_666 . ?
O8 Ho1 O9 146.16(9) 2_666 . ?
O6 Ho1 O9 73.39(10) . . ?
O5 Ho1 O9 70.27(10) . . ?
O2 Ho1 O10 151.53(9) . . ?
O3 Ho1 O10 107.23(11) 2_666 . ?
O8 Ho1 O10 85.70(9) 2_666 . ?
O6 Ho1 O10 71.58(9) . . ?
O5 Ho1 O10 78.80(10) . . ?
O9 Ho1 O10 86.83(11) . . ?
O2 Ho1 O1 62.03(9) . . ?
O3 Ho1 O1 79.60(10) 2_666 . ?
O8 Ho1 O1 128.38(9) 2_666 . ?
O6 Ho1 O1 76.06(9) . . ?
O5 Ho1 O1 115.53(10) . . ?
O9 Ho1 O1 69.95(11) . . ?
O10 Ho1 O1 144.46(9) . . ?
O2 Ho1 Ni1 35.44(6) . . ?
O3 Ho1 Ni1 81.11(7) 2_666 . ?
O8 Ho1 Ni1 38.84(7) 2_666 . ?
O6 Ho1 Ni1 158.91(7) . . ?
O5 Ho1 Ni1 67.28(8) . . ?
O9 Ho1 Ni1 122.97(8) . . ?
O10 Ho1 Ni1 119.13(7) . . ?
O1 Ho1 Ni1 96.28(8) . . ?
O2 Ho1 Ni1 76.13(8) . 2_666 ?
O3 Ho1 Ni1 35.49(7) 2_666 2_666 ?
O8 Ho1 Ni1 35.62(6) 2_666 2_666 ?
O6 Ho1 Ni1 107.68(8) . 2_666 ?
O5 Ho1 Ni1 111.01(8) . 2_666 ?
O9 Ho1 Ni1 175.05(7) . 2_666 ?
O10 Ho1 Ni1 98.10(8) . 2_666 ?
O1 Ho1 Ni1 105.46(8) . 2_666 ?
Ni1 Ho1 Ni1 54.82(4) . 2_666 ?
O2 Ni1 O4 92.34(10) . . ?
O2 Ni1 O8 92.53(10) . . ?
O4 Ni1 O8 170.56(9) . . ?
O2 Ni1 N1 89.75(11) . . ?
O4 Ni1 N1 88.15(12) . . ?
O8 Ni1 N1 99.95(12) . . ?
O2 Ni1 O3 173.18(10) . . ?
O4 Ni1 O3 94.15(10) . . ?
O8 Ni1 O3 81.35(10) . . ?
N1 Ni1 O3 88.36(11) . . ?
O2 Ni1 O8 83.47(10) . 2_666 ?
O4 Ni1 O8 89.52(11) . 2_666 ?
O8 Ni1 O8 83.00(11) . 2_666 ?
N1 Ni1 O8 172.73(10) . 2_666 ?
O3 Ni1 O8 98.67(10) . 2_666 ?
O2 Ni1 Ho1 40.88(7) . . ?
O4 Ni1 Ho1 83.98(8) . . ?
O8 Ni1 Ho1 94.45(8) . . ?
N1 Ni1 Ho1 129.21(8) . . ?
O3 Ni1 Ho1 142.14(8) . . ?
O8 Ni1 Ho1 43.63(7) 2_666 . ?
O2 Ni1 Ho1 134.02(7) . 2_666 ?
O4 Ni1 Ho1 133.35(8) . 2_666 ?
O8 Ni1 Ho1 41.54(7) . 2_666 ?
N1 Ni1 Ho1 95.67(10) . 2_666 ?
O3 Ni1 Ho1 39.81(7) . 2_666 ?
O8 Ni1 Ho1 90.94(9) 2_666 2_666 ?
Ho1 Ni1 Ho1 125.18(4) . 2_666 ?
C15 O3 Ni1 110.9(2) . . ?
C15 O3 Ho1 139.2(2) . 2_666 ?
Ni1 O3 Ho1 104.70(10) . 2_666 ?
C7 O2 Ni1 128.7(2) . . ?
C7 O2 Ho1 127.0(2) . . ?
Ni1 O2 Ho1 103.68(10) . . ?
C32 O8 Ni1 115.0(2) . . ?
C32 O8 Ni1 114.0(2) . 2_666 ?
Ni1 O8 Ni1 96.99(11) . 2_666 ?
C32 O8 Ho1 125.7(2) . 2_666 ?
Ni1 O8 Ho1 102.84(10) . 2_666 ?
Ni1 O8 Ho1 97.53(10) 2_666 2_666 ?
C16 O4 Ni1 125.9(2) . . ?
C23 O6 Ho1 142.0(2) . . ?
C16 O5 Ho1 135.8(2) . . ?
C2 O1 C1 116.1(3) . . ?
C2 O1 Ho1 112.4(2) . . ?
C1 O1 Ho1 130.0(2) . . ?
C31 O10 Ho1 132.3(2) . . ?
C31 O10 H10 113.9 . . ?
Ho1 O10 H10 113.9 . . ?
C30 O9 Ho1 136.1(2) . . ?
C30 O9 H9 112.0 . . ?
Ho1 O9 H9 112.0 . . ?
C8 N1 C9 117.5(3) . . ?
C8 N1 Ni1 125.4(3) . . ?
C9 N1 Ni1 116.6(2) . . ?
C33 O11 H11A 109.5 . . ?
C5 C6 C7 118.4(3) . . ?
C5 C6 C8 118.4(3) . . ?
C7 C6 C8 123.2(3) . . ?
N1 C8 C6 127.2(3) . . ?
N1 C8 H8 116.4 . . ?
C6 C8 H8 116.4 . . ?
O4 C16 O5 126.9(3) . . ?
O4 C16 C17 115.9(3) . . ?
O5 C16 C17 117.1(3) . . ?
O2 C7 C2 117.3(3) . . ?
O2 C7 C6 124.3(3) . . ?
C2 C7 C6 118.3(3) . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C18 C17 C22 120.1(3) . . ?
C18 C17 C16 120.4(3) . . ?
C22 C17 C16 119.5(3) . . ?
C13 C14 C15 120.9(4) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C3 C2 O1 125.7(3) . . ?
C3 C2 C7 121.7(3) . . ?
O1 C2 C7 112.6(3) . . ?
C17 C18 C19 119.6(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
N1 C9 C10 113.6(3) . . ?
N1 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N1 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
O8 C32 H32A 109.5 . . ?
O8 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O8 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C11 C10 C15 119.4(3) . . ?
C11 C10 C9 122.3(3) . . ?
C15 C10 C9 118.3(3) . . ?
O6 C23 O7 123.8(4) . . ?
O6 C23 C24 118.5(3) . . ?
O7 C23 C24 117.6(3) . . ?
C25 C24 C29 118.9(4) . . ?
C25 C24 C23 120.5(4) . . ?
C29 C24 C23 120.6(4) . . ?
C4 C5 C6 121.9(3) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C11 C12 C13 119.2(3) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C2 C3 C4 119.2(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
O3 C15 C14 121.6(3) . . ?
O3 C15 C10 119.2(3) . . ?
C14 C15 C10 119.2(3) . . ?
C14 C13 C12 119.9(4) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C10 C11 C12 121.4(4) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C19 C20 C21 120.3(4) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C17 C22 C21 119.7(4) . . ?
C17 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C27 C26 C25 120.0(4) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
O9 C30 H30A 109.5 . . ?
O9 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O9 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C24 C25 C26 120.9(4) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C24 C29 C28 120.5(4) . . ?
C24 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
O10 C31 H31A 109.5 . . ?
O10 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O10 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C20 C21 C22 119.8(4) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C29 C28 C27 119.4(5) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C20 C19 C18 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
O11 C33 H33A 109.5 . . ?
O11 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O11 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C27 C28 120.0(4) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?

_refine_diff_density_max         1.064
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.122



