# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2023

####################################################################### 
# 
# 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. 
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data_complex_1
_database_code_depnum_ccdc_archive 'CCDC 2095746'
loop_
_audit_author_name
_audit_author_address
'Mousumi Biswas'
;IIT Kharagpur
India
;
_audit_update_record             
;
2023-07-07 deposited with the CCDC.	2023-07-11 downloaded from the CCDC.
;
_audit_creation_date             2023-07-05
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C78 H99 Dy4 N3 Ni3 O31, 2H, 11[H2O]'
_chemical_formula_sum            'C78 H123 Dy4 N3 Ni3 O42'
_chemical_formula_weight         2600.90
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   20.009(4)
_cell_length_b                   20.009(4)
_cell_length_c                   15.363(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5327(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.074
_cell_measurement_theta_min      2.429
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.368
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55281
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.080
_diffrn_reflns_theta_max         25.080
_diffrn_reflns_theta_min         2.351
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5512
_reflns_number_total             6307
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6307
_refine_ls_number_restraints     118
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0227
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0195P)²+5.7744P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0553
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C20 \\sim C17-C20A
 with sigma of 0.02
 C17-C18 \\sim C17-C18A
 with sigma of 0.02
 C18-C19 \\sim C18-C20 \\sim C19-C20 \\sim C20A-C18A \\sim C20A-C19A \\sim
C18A-C19A
 with sigma of 0.04
 C17-C19 \\sim C17-C19A
 with sigma of 0.02
 C17-C16 \\sim C17-C18 \\sim C17-C19 \\sim C17-C20 \\sim C17-C20A \\sim
C17-C18A \\sim C17-C19A
 with sigma of 0.02
 O11-C26 \\sim O11-C26A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26A) = Uanis(C26)
4. Rigid body (RIGU) restrains
 C18, C20, C19, C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20A, C19A, C18A, C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Fixed Sof: C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C20A(0.5) H20D(0.5)
 H20E(0.5) H20F(0.5) C18A(0.5) H18D(0.5) H18E(0.5) H18F(0.5) C19A(0.5)
 H19D(0.5) H19E(0.5) H19F(0.5)
6.a Ternary CH refined with riding coordinates:
 O9(H9)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C3(H3), C10(H10), C12(H12), C5(H5), C11(H11), C4(H4)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C23(H23A,H23B,
 H23C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C20A(H20D,H20E,H20F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C26(H26A,
 H26B,H26C), C26A(H26D,H26E,H26F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.79008(2) 0.36202(2) 0.39028(2) 0.03276(5) Uani 1 1 d . . . . .
Dy2 Dy 0.666667 0.333333 0.19965(2) 0.03420(7) Uani 1 3 d S T P . .
Ni1 Ni 0.77066(2) 0.22518(2) 0.24642(3) 0.03668(10) Uani 1 1 d . . . . .
O10 O 0.666667 0.333333 0.3522(2) 0.0334(8) Uani 1 3 d S T P . .
O9 O 0.77568(12) 0.32919(12) 0.24145(13) 0.0337(5) Uani 1 1 d . . . . .
H9 H 0.820861 0.366546 0.208252 0.040 Uiso 1 1 calc R U . . .
O1 O 0.82007(12) 0.26553(13) 0.36347(14) 0.0401(5) Uani 1 1 d . . . . .
O2 O 0.91215(14) 0.35938(14) 0.47760(16) 0.0491(6) Uani 1 1 d . . . . .
O4 O 0.54441(13) 0.08650(13) 0.32813(16) 0.0434(5) Uani 1 1 d . . . . .
O3 O 0.66290(12) 0.17885(12) 0.30417(14) 0.0371(5) Uani 1 1 d . . . . .
O5 O 0.73177(15) 0.18843(14) 0.12499(16) 0.0506(6) Uani 1 1 d . . . . .
O6 O 0.65443(15) 0.23709(15) 0.10564(16) 0.0523(6) Uani 1 1 d . . . . .
O7 O 0.72653(17) 0.28038(16) 0.50164(18) 0.0650(8) Uani 1 1 d . . . . .
O8 O 0.62074(15) 0.16675(16) 0.50086(16) 0.0560(7) Uani 1 1 d . . . . .
N1 N 0.76192(16) 0.12338(16) 0.27869(19) 0.0419(7) Uani 1 1 d . . . . .
O11 O 0.88119(16) 0.27058(18) 0.1884(2) 0.0704(8) Uani 1 1 d D . . . .
C15 C 0.60993(19) 0.10785(18) 0.2974(2) 0.0374(7) Uani 1 1 d . . . . .
C14 C 0.62395(19) 0.04948(18) 0.2521(2) 0.0407(8) Uani 1 1 d . . . . .
C1 C 0.86895(19) 0.2470(2) 0.3975(2) 0.0413(8) Uani 1 1 d . . . . .
C9 C 0.6973(2) 0.05650(19) 0.2442(2) 0.0456(8) Uani 1 1 d . . . . .
C21 C 0.6826(2) 0.2151(2) 0.5356(2) 0.0478(9) Uani 1 1 d . . . . .
C7 C 0.8100(2) 0.1167(2) 0.3277(2) 0.0474(9) Uani 1 1 d . . . . .
H7 H 0.806017 0.068415 0.331062 0.057 Uiso 1 1 calc R U . . .
C13 C 0.5608(2) -0.0167(2) 0.2195(2) 0.0498(9) Uani 1 1 d . . . . .
H13 H 0.511814 -0.022620 0.224757 0.060 Uiso 1 1 calc R U . . .
C2 C 0.9222(2) 0.2978(2) 0.4593(2) 0.0482(9) Uani 1 1 d . . . . .
C16 C 0.6852(2) 0.1991(2) 0.0810(2) 0.0436(8) Uani 1 1 d D . . . .
C6 C 0.8698(2) 0.1783(2) 0.3782(2) 0.0466(8) Uani 1 1 d . . . . .
C22 C 0.7075(2) 0.1968(2) 0.6221(2) 0.0487(9) Uani 1 1 d . . . . .
C8 C 0.9582(2) 0.4082(3) 0.5480(3) 0.0697(12) Uani 1 1 d . . . . .
H8A H 0.948691 0.377781 0.599665 0.105 Uiso 1 1 calc R U . . .
H8B H 0.944769 0.447387 0.558372 0.105 Uiso 1 1 calc R U . . .
H8C H 1.011864 0.432147 0.532917 0.105 Uiso 1 1 calc R U . . .
C3 C 0.9762(2) 0.2835(3) 0.4964(3) 0.0671(12) Uani 1 1 d . . . . .
H3 H 1.011398 0.318337 0.536239 0.081 Uiso 1 1 calc R U . . .
C10 C 0.7050(2) -0.0013(2) 0.2036(3) 0.0640(11) Uani 1 1 d . . . . .
H10 H 0.753466 0.003451 0.198020 0.077 Uiso 1 1 calc R U . . .
C12 C 0.5691(2) -0.0738(2) 0.1792(3) 0.0640(11) Uani 1 1 d . . . . .
H12 H 0.526152 -0.117606 0.157559 0.077 Uiso 1 1 calc R U . . .
C5 C 0.9260(2) 0.1656(3) 0.4184(3) 0.0669(12) Uani 1 1 d . . . . .
H5 H 0.927204 0.120715 0.405737 0.080 Uiso 1 1 calc R U . . .
C17 C 0.6639(2) 0.1617(2) -0.0088(2) 0.0637(11) Uani 1 1 d D . . . .
C11 C 0.6408(3) -0.0657(2) 0.1715(3) 0.0736(13) Uani 1 1 d . . . . .
H11 H 0.646351 -0.104064 0.144136 0.088 Uiso 1 1 calc R U . . .
C24 C 0.7700(3) 0.1773(4) 0.6037(4) 0.107(2) Uani 1 1 d . . . . .
H24A H 0.787127 0.166516 0.657515 0.160 Uiso 1 1 calc R U . . .
H24B H 0.812592 0.220265 0.575455 0.160 Uiso 1 1 calc R U . . .
H24C H 0.749872 0.132849 0.566613 0.160 Uiso 1 1 calc R U . . .
C25 C 0.6402(3) 0.1301(3) 0.6677(3) 0.0832(16) Uani 1 1 d . . . . .
H25A H 0.620168 0.084881 0.631668 0.125 Uiso 1 1 calc R U . . .
H25B H 0.600532 0.142677 0.678223 0.125 Uiso 1 1 calc R U . . .
H25C H 0.657338 0.120250 0.722095 0.125 Uiso 1 1 calc R U . . .
C23 C 0.7395(4) 0.2670(3) 0.6816(4) 0.1039(19) Uani 1 1 d . . . . .
H23A H 0.756154 0.255611 0.735358 0.156 Uiso 1 1 calc R U . . .
H23B H 0.700042 0.279773 0.693146 0.156 Uiso 1 1 calc R U . . .
H23C H 0.782516 0.309930 0.653762 0.156 Uiso 1 1 calc R U . . .
C4 C 0.9783(3) 0.2174(3) 0.4749(4) 0.0791(15) Uani 1 1 d . . . . .
H4 H 1.015761 0.208509 0.499245 0.095 Uiso 1 1 calc R U . . .
C18 C 0.6259(8) 0.1949(9) -0.0650(9) 0.100(4) Uani 0.5 1 d D U P A 1
H18A H 0.656251 0.250188 -0.064179 0.150 Uiso 0.5 1 calc R U P A 1
H18B H 0.575193 0.178874 -0.043053 0.150 Uiso 0.5 1 calc R U P A 1
H18C H 0.622135 0.176738 -0.123658 0.150 Uiso 0.5 1 calc R U P A 1
C19 C 0.7399(6) 0.1825(9) -0.0562(7) 0.106(4) Uani 0.5 1 d D . P A 1
H19A H 0.728493 0.160899 -0.113766 0.159 Uiso 0.5 1 calc R U P A 1
H19B H 0.766881 0.161979 -0.024429 0.159 Uiso 0.5 1 calc R U P A 1
H19C H 0.771493 0.237609 -0.060009 0.159 Uiso 0.5 1 calc R U P A 1
C20 C 0.6172(11) 0.0766(5) -0.0006(9) 0.145(8) Uani 0.5 1 d D . P A 1
H20A H 0.570026 0.062956 0.029520 0.217 Uiso 0.5 1 calc R U P A 1
H20B H 0.645783 0.058035 0.031554 0.217 Uiso 0.5 1 calc R U P A 1
H20C H 0.605564 0.053752 -0.057496 0.217 Uiso 0.5 1 calc R U P A 1
C20A C 0.5766(6) 0.1026(8) -0.0009(10) 0.131(6) Uani 0.5 1 d D U P A 2
H20D H 0.550256 0.127840 0.022045 0.196 Uiso 0.5 1 calc R U P A 2
H20E H 0.569151 0.061585 0.037460 0.196 Uiso 0.5 1 calc R U P A 2
H20F H 0.556139 0.081809 -0.057330 0.196 Uiso 0.5 1 calc R U P A 2
C18A C 0.6707(10) 0.2180(8) -0.0753(9) 0.119(5) Uani 0.5 1 d D U P A 2
H18D H 0.653643 0.192512 -0.130531 0.179 Uiso 0.5 1 calc R U P A 2
H18E H 0.723612 0.258316 -0.079804 0.179 Uiso 0.5 1 calc R U P A 2
H18F H 0.639361 0.239830 -0.058960 0.179 Uiso 0.5 1 calc R U P A 2
C19A C 0.7031(11) 0.1167(11) -0.0275(11) 0.152(6) Uani 0.5 1 d D U P A 2
H19D H 0.686094 0.091451 -0.082784 0.228 Uiso 0.5 1 calc R U P A 2
H19E H 0.690693 0.078778 0.017243 0.228 Uiso 0.5 1 calc R U P A 2
H19F H 0.757959 0.150976 -0.028949 0.228 Uiso 0.5 1 calc R U P A 2
C26 C 0.9527(4) 0.3291(5) 0.2131(6) 0.134(4) Uani 0.850(9) 1 d D . P B 1
H26A H 0.976116 0.364398 0.165584 0.202 Uiso 0.850(9) 1 calc R U P B 1
H26B H 0.984624 0.307760 0.229075 0.202 Uiso 0.850(9) 1 calc R U P B 1
H26C H 0.947376 0.355901 0.262037 0.202 Uiso 0.850(9) 1 calc R U P B 1
C26A C 0.904(3) 0.316(2) 0.116(2) 0.134(4) Uani 0.150(9) 1 d D . P B 2
H26D H 0.934043 0.368848 0.132668 0.202 Uiso 0.150(9) 1 calc R U P B 2
H26E H 0.858811 0.308085 0.084673 0.202 Uiso 0.150(9) 1 calc R U P B 2
H26F H 0.933745 0.301831 0.079489 0.202 Uiso 0.150(9) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O10 2.3133(10) . ?
Dy1 O9 2.357(2) . ?
Dy1 O1 2.327(2) . ?
Dy1 O2 2.810(2) . ?
Dy1 O4 2.440(2) 2_655 ?
Dy1 O3 2.565(2) 2_655 ?
Dy1 O7 2.266(3) . ?
Dy1 O8 2.330(2) 2_655 ?
Dy2 O10 2.344(4) . ?
Dy2 O9 2.315(2) 2_655 ?
Dy2 O9 2.315(2) . ?
Dy2 O9 2.315(2) 3_665 ?
Dy2 O6 2.320(2) 2_655 ?
Dy2 O6 2.320(2) 3_665 ?
Dy2 O6 2.320(2) . ?
Ni1 O9 2.034(2) . ?
Ni1 O1 2.016(2) . ?
Ni1 O3 2.073(2) . ?
Ni1 O5 2.013(2) . ?
Ni1 N1 2.017(3) . ?
Ni1 O11 2.122(3) . ?
O9 H9 0.9800 . ?
O1 C1 1.316(4) . ?
O2 C2 1.373(4) . ?
O2 C8 1.440(4) . ?
O4 C15 1.250(4) . ?
O3 C15 1.283(4) . ?
O5 C16 1.252(4) . ?
O6 C16 1.253(4) . ?
O7 C21 1.267(4) . ?
O8 C21 1.247(5) . ?
N1 C9 1.419(4) . ?
N1 C7 1.280(4) . ?
O11 C26 1.374(8) . ?
O11 C26A 1.36(2) . ?
C15 C14 1.501(4) . ?
C14 C9 1.408(5) . ?
C14 C13 1.388(5) . ?
C1 C2 1.409(5) . ?
C1 C6 1.414(5) . ?
C9 C10 1.389(5) . ?
C21 C22 1.526(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.441(5) . ?
C13 H13 0.9300 . ?
C13 C12 1.381(5) . ?
C2 C3 1.372(5) . ?
C16 C17 1.525(5) . ?
C6 C5 1.415(5) . ?
C22 C24 1.511(6) . ?
C22 C25 1.513(5) . ?
C22 C23 1.523(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C3 H3 0.9300 . ?
C3 C4 1.386(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.377(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.365(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.356(6) . ?
C17 C18 1.506(10) . ?
C17 C19 1.544(9) . ?
C17 C20 1.481(9) . ?
C17 C20A 1.549(10) . ?
C17 C18A 1.477(10) . ?
C17 C19A 1.488(10) . ?
C11 H11 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C4 H4 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18A H18F 0.9600 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C26A H26D 0.9600 . ?
C26A H26E 0.9600 . ?
C26A H26F 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
O10 Dy1 O9 73.69(9) . . ?
O10 Dy1 O1 115.81(6) . . ?
O10 Dy1 O2 161.07(8) . . ?
O10 Dy1 O4 129.15(8) . 2_655 ?
O10 Dy1 O3 80.01(6) . 2_655 ?
O10 Dy1 O8 107.97(9) . 2_655 ?
O9 Dy1 O2 116.37(7) . . ?
O9 Dy1 O4 76.95(8) . 2_655 ?
O9 Dy1 O3 72.70(7) . 2_655 ?
O1 Dy1 O9 69.10(7) . . ?
O1 Dy1 O2 58.79(7) . . ?
O1 Dy1 O4 90.21(8) . 2_655 ?
O1 Dy1 O3 131.15(7) . 2_655 ?
O1 Dy1 O8 129.54(9) . 2_655 ?
O4 Dy1 O2 69.76(8) 2_655 . ?
O4 Dy1 O3 51.78(7) 2_655 2_655 ?
O3 Dy1 O2 117.70(7) 2_655 . ?
O7 Dy1 O10 82.37(10) . . ?
O7 Dy1 O9 125.82(9) . . ?
O7 Dy1 O1 79.64(9) . . ?
O7 Dy1 O2 78.80(9) . . ?
O7 Dy1 O4 147.65(10) . 2_655 ?
O7 Dy1 O3 148.99(8) . 2_655 ?
O7 Dy1 O8 82.63(10) . 2_655 ?
O8 Dy1 O9 150.81(8) 2_655 . ?
O8 Dy1 O2 71.60(8) 2_655 . ?
O8 Dy1 O4 80.47(9) 2_655 2_655 ?
O8 Dy1 O3 78.85(8) 2_655 2_655 ?
O10 Dy2 Dy1 37.388(8) . . ?
O9 Dy2 Dy1 100.94(5) 3_665 . ?
O9 Dy2 Dy1 38.30(5) . . ?
O9 Dy2 Dy1 86.20(5) 2_655 . ?
O9 Dy2 O10 73.89(5) 2_655 . ?
O9 Dy2 O10 73.89(5) . . ?
O9 Dy2 O10 73.89(5) 3_665 . ?
O9 Dy2 O9 112.62(4) 3_665 2_655 ?
O9 Dy2 O9 112.62(4) . 2_655 ?
O9 Dy2 O9 112.61(4) . 3_665 ?
O9 Dy2 O6 81.56(8) . . ?
O9 Dy2 O6 81.56(8) 3_665 3_665 ?
O9 Dy2 O6 81.56(8) 2_655 2_655 ?
O9 Dy2 O6 75.11(8) 3_665 . ?
O9 Dy2 O6 157.20(8) 2_655 . ?
O9 Dy2 O6 157.20(8) 3_665 2_655 ?
O9 Dy2 O6 75.11(8) . 2_655 ?
O9 Dy2 O6 157.20(8) . 3_665 ?
O9 Dy2 O6 75.10(8) 2_655 3_665 ?
O6 Dy2 Dy1 114.10(6) . . ?
O6 Dy2 Dy1 97.65(7) 2_655 . ?
O6 Dy2 Dy1 160.47(7) 3_665 . ?
O6 Dy2 O10 128.50(7) 3_665 . ?
O6 Dy2 O10 128.50(7) 2_655 . ?
O6 Dy2 O10 128.50(7) . . ?
O6 Dy2 O6 85.34(10) . 3_665 ?
O6 Dy2 O6 85.34(10) . 2_655 ?
O6 Dy2 O6 85.33(10) 2_655 3_665 ?
O9 Ni1 O3 88.96(8) . . ?
O9 Ni1 O11 92.20(11) . . ?
O1 Ni1 O9 81.97(8) . . ?
O1 Ni1 O3 89.39(9) . . ?
O1 Ni1 N1 87.86(10) . . ?
O1 Ni1 O11 90.35(11) . . ?
O3 Ni1 O11 178.76(11) . . ?
O5 Ni1 O9 98.70(9) . . ?
O5 Ni1 O1 174.39(10) . . ?
O5 Ni1 O3 96.18(10) . . ?
O5 Ni1 N1 92.09(11) . . ?
O5 Ni1 O11 84.07(11) . . ?
N1 Ni1 O9 167.76(10) . . ?
N1 Ni1 O3 84.12(10) . . ?
N1 Ni1 O11 94.66(12) . . ?
Dy1 O10 Dy1 113.84(7) 3_665 2_655 ?
Dy1 O10 Dy1 113.84(7) . 3_665 ?
Dy1 O10 Dy1 113.84(7) . 2_655 ?
Dy1 O10 Dy2 104.64(8) 3_665 . ?
Dy1 O10 Dy2 104.64(8) . . ?
Dy1 O10 Dy2 104.64(8) 2_655 . ?
Dy1 O9 H9 110.8 . . ?
Dy2 O9 Dy1 104.20(8) . . ?
Dy2 O9 H9 110.8 . . ?
Ni1 O9 Dy1 100.69(8) . . ?
Ni1 O9 Dy2 118.79(9) . . ?
Ni1 O9 H9 110.8 . . ?
Ni1 O1 Dy1 102.23(9) . . ?
C1 O1 Dy1 134.4(2) . . ?
C1 O1 Ni1 121.8(2) . . ?
C2 O2 Dy1 115.94(19) . . ?
C2 O2 C8 115.6(3) . . ?
C8 O2 Dy1 127.8(2) . . ?
C15 O4 Dy1 97.72(19) . 3_665 ?
Ni1 O3 Dy1 144.86(10) . 3_665 ?
C15 O3 Dy1 90.96(18) . 3_665 ?
C15 O3 Ni1 124.0(2) . . ?
C16 O5 Ni1 128.5(2) . . ?
C16 O6 Dy2 144.3(2) . . ?
C21 O7 Dy1 154.8(3) . . ?
C21 O8 Dy1 117.5(2) . 3_665 ?
C9 N1 Ni1 116.0(2) . . ?
C7 N1 Ni1 124.1(2) . . ?
C7 N1 C9 119.9(3) . . ?
C26 O11 Ni1 131.8(4) . . ?
C26A O11 Ni1 123.7(19) . . ?
O4 C15 Dy1 56.87(16) . 3_665 ?
O4 C15 O3 119.5(3) . . ?
O4 C15 C14 118.7(3) . . ?
O3 C15 Dy1 62.66(16) . 3_665 ?
O3 C15 C14 121.8(3) . . ?
C14 C15 Dy1 175.4(2) . 3_665 ?
C9 C14 C15 123.6(3) . . ?
C13 C14 C15 118.3(3) . . ?
C13 C14 C9 118.0(3) . . ?
O1 C1 C2 117.7(3) . . ?
O1 C1 C6 124.2(3) . . ?
C2 C1 C6 118.1(3) . . ?
C14 C9 N1 118.3(3) . . ?
C10 C9 N1 121.7(3) . . ?
C10 C9 C14 120.0(3) . . ?
O7 C21 C22 117.7(4) . . ?
O8 C21 O7 122.1(3) . . ?
O8 C21 C22 120.2(3) . . ?
N1 C7 H7 117.5 . . ?
N1 C7 C6 124.9(3) . . ?
C6 C7 H7 117.5 . . ?
C14 C13 H13 119.3 . . ?
C12 C13 C14 121.5(4) . . ?
C12 C13 H13 119.3 . . ?
O2 C2 C1 112.9(3) . . ?
C3 C2 O2 125.8(3) . . ?
C3 C2 C1 121.3(4) . . ?
O5 C16 O6 125.0(3) . . ?
O5 C16 C17 117.0(3) . . ?
O6 C16 C17 118.0(3) . . ?
C1 C6 C7 122.5(3) . . ?
C1 C6 C5 118.7(3) . . ?
C5 C6 C7 118.4(3) . . ?
C24 C22 C21 108.1(3) . . ?
C24 C22 C25 110.1(4) . . ?
C24 C22 C23 109.2(4) . . ?
C25 C22 C21 111.2(3) . . ?
C25 C22 C23 108.4(4) . . ?
C23 C22 C21 109.8(3) . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.2(4) . . ?
C4 C3 H3 119.9 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0(4) . . ?
C11 C10 H10 120.0 . . ?
C13 C12 H12 120.2 . . ?
C11 C12 C13 119.6(4) . . ?
C11 C12 H12 120.2 . . ?
C6 C5 H5 119.3 . . ?
C4 C5 C6 121.4(4) . . ?
C4 C5 H5 119.3 . . ?
C16 C17 C19 107.3(5) . . ?
C16 C17 C20A 103.7(6) . . ?
C18 C17 C16 112.4(7) . . ?
C18 C17 C19 104.8(8) . . ?
C20 C17 C16 110.4(6) . . ?
C20 C17 C18 112.9(9) . . ?
C20 C17 C19 108.7(9) . . ?
C18A C17 C16 110.8(7) . . ?
C18A C17 C20A 106.0(9) . . ?
C18A C17 C19A 116.9(10) . . ?
C19A C17 C16 111.6(7) . . ?
C19A C17 C20A 106.8(9) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.9(4) . . ?
C12 C11 H11 119.6 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 119.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C20A H20D 109.5 . . ?
C17 C20A H20E 109.5 . . ?
C17 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C17 C18A H18D 109.5 . . ?
C17 C18A H18E 109.5 . . ?
C17 C18A H18F 109.5 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C17 C19A H19D 109.5 . . ?
C17 C19A H19E 109.5 . . ?
C17 C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
O11 C26 H26A 109.5 . . ?
O11 C26 H26B 109.5 . . ?
O11 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O11 C26A H26D 109.5 . . ?
O11 C26A H26E 109.5 . . ?
O11 C26A H26F 109.5 . . ?
H26D C26A H26E 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C1 C2 -7.1(5) . . . . ?
Dy1 O1 C1 C6 170.8(2) . . . . ?
Dy1 O2 C2 C1 1.1(4) . . . . ?
Dy1 O2 C2 C3 -177.6(3) . . . . ?
Dy1 O4 C15 O3 -2.5(3) 3_665 . . . ?
Dy1 O4 C15 C14 178.5(2) 3_665 . . . ?
Dy1 O3 C15 O4 2.3(3) 3_665 . . . ?
Dy1 O3 C15 C14 -178.7(3) 3_665 . . . ?
Dy1 O7 C21 O8 -43.1(8) . . . . ?
Dy1 O7 C21 C22 137.3(5) . . . . ?
Dy1 O8 C21 O7 -15.1(5) 3_665 . . . ?
Dy1 O8 C21 C22 164.5(3) 3_665 . . . ?
Dy2 O6 C16 O5 23.2(7) . . . . ?
Dy2 O6 C16 C17 -157.7(3) . . . . ?
Ni1 O1 C1 C2 155.9(2) . . . . ?
Ni1 O1 C1 C6 -26.2(4) . . . . ?
Ni1 O3 C15 Dy1 -176.1(2) . . . 3_665 ?
Ni1 O3 C15 O4 -173.8(2) . . . . ?
Ni1 O3 C15 C14 5.2(4) . . . . ?
Ni1 O5 C16 O6 1.2(5) . . . . ?
Ni1 O5 C16 C17 -177.9(2) . . . . ?
Ni1 N1 C9 C14 -48.3(4) . . . . ?
Ni1 N1 C9 C10 131.9(3) . . . . ?
Ni1 N1 C7 C6 10.5(5) . . . . ?
O1 C1 C2 O2 2.7(5) . . . . ?
O1 C1 C2 C3 -178.6(4) . . . . ?
O1 C1 C6 C7 -8.6(6) . . . . ?
O1 C1 C6 C5 179.2(4) . . . . ?
O2 C2 C3 C4 177.3(4) . . . . ?
O4 C15 C14 C9 -155.2(3) . . . . ?
O4 C15 C14 C13 22.0(5) . . . . ?
O3 C15 C14 C9 25.8(5) . . . . ?
O3 C15 C14 C13 -157.0(3) . . . . ?
O5 C16 C17 C18 -164.4(7) . . . . ?
O5 C16 C17 C19 -49.6(8) . . . . ?
O5 C16 C17 C20 68.6(10) . . . . ?
O5 C16 C17 C20A 115.4(7) . . . . ?
O5 C16 C17 C18A -131.3(8) . . . . ?
O5 C16 C17 C19A 0.9(11) . . . . ?
O6 C16 C17 C18 16.5(8) . . . . ?
O6 C16 C17 C19 131.2(7) . . . . ?
O6 C16 C17 C20 -110.5(10) . . . . ?
O6 C16 C17 C20A -63.7(8) . . . . ?
O6 C16 C17 C18A 49.6(9) . . . . ?
O6 C16 C17 C19A -178.3(10) . . . . ?
O7 C21 C22 C24 -76.8(5) . . . . ?
O7 C21 C22 C25 162.2(4) . . . . ?
O7 C21 C22 C23 42.2(5) . . . . ?
O8 C21 C22 C24 103.6(5) . . . . ?
O8 C21 C22 C25 -17.4(5) . . . . ?
O8 C21 C22 C23 -137.4(4) . . . . ?
N1 C9 C10 C11 179.5(4) . . . . ?
N1 C7 C6 C1 17.6(6) . . . . ?
N1 C7 C6 C5 -170.1(4) . . . . ?
C15 C14 C9 N1 -1.8(5) . . . . ?
C15 C14 C9 C10 178.0(4) . . . . ?
C15 C14 C13 C12 -178.1(4) . . . . ?
C14 C9 C10 C11 -0.3(6) . . . . ?
C14 C13 C12 C11 0.2(7) . . . . ?
C1 C2 C3 C4 -1.2(7) . . . . ?
C1 C6 C5 C4 0.4(7) . . . . ?
C9 N1 C7 C6 -168.9(3) . . . . ?
C9 C14 C13 C12 -0.8(6) . . . . ?
C9 C10 C11 C12 -0.2(8) . . . . ?
C7 N1 C9 C14 131.1(4) . . . . ?
C7 N1 C9 C10 -48.7(5) . . . . ?
C7 C6 C5 C4 -172.1(4) . . . . ?
C13 C14 C9 N1 -179.0(3) . . . . ?
C13 C14 C9 C10 0.8(5) . . . . ?
C13 C12 C11 C10 0.3(8) . . . . ?
C2 C1 C6 C7 169.3(3) . . . . ?
C2 C1 C6 C5 -2.9(5) . . . . ?
C2 C3 C4 C5 -1.4(8) . . . . ?
C6 C1 C2 O2 -175.3(3) . . . . ?
C6 C1 C2 C3 3.4(6) . . . . ?
C6 C5 C4 C3 1.9(8) . . . . ?
C8 O2 C2 C1 172.5(3) . . . . ?
C8 O2 C2 C3 -6.2(6) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 222 electrons were 
found in a volume of 1214Å³ in 1 void per unit cell. 
This is consistent with the presence of 11[H2O] 
per Formula Unit which account for 220 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.721 1213.6 221.5 '22 H2O'
2 0.333 0.667 0.187 7.3 0.0 ?
3 0.667 0.333 0.813 7.3 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex_2
_database_code_depnum_ccdc_archive 'CCDC 2095747'
loop_
_audit_author_name
_audit_author_address
'Mousumi Biswas'
;IIT Kharagpur
India
;
_audit_update_record             
;
2023-07-07 deposited with the CCDC.	2023-07-11 downloaded from the CCDC.
;
_audit_creation_date             2023-07-05
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C77.494 H97.482 N3 Ni3 O30.494 Tb4, 0.506(C1 H3 O1), 2H, 9[H2O]'
_chemical_formula_sum            'C78 H119 N3 Ni3 O40 Tb4'
_chemical_formula_weight         2550.55
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   20.046(4)
_cell_length_b                   20.046(4)
_cell_length_c                   15.420(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5366(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.047
_cell_measurement_theta_min      2.421
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.192
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57521
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.095
_diffrn_reflns_theta_max         25.095
_diffrn_reflns_theta_min         2.346
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5605
_reflns_number_total             6343
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5-beta (Bourhis et al., 2015)'
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0236
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0082P)²+7.9932P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0544
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C18 \\sim C17-C18A
 with sigma of 0.02
 C18-C20 \\sim C18-C19 \\sim C20-C19 \\sim C20A-C18A \\sim C20A-C19A \\sim
C18A-C19A
 with sigma of 0.04
 C17-C20 \\sim C17-C20A
 with sigma of 0.02
 C17-C19 \\sim C17-C19A
 with sigma of 0.02
 C17-C16 \\sim C17-C18 \\sim C17-C20 \\sim C17-C19 \\sim C17-C20A \\sim
C17-C18A \\sim C17-C19A
 with sigma of 0.02
 Ni1-O11 \\sim Ni1-O11A
 with sigma of 0.02
 O11-C26 \\sim O11A-C26A
 with sigma of 0.02
 Ni1-C26 \\sim Ni1-C26A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) = Uanis(C26A)
Uanis(O11) = Uanis(O11A)
4. Rigid body (RIGU) restrains
 C18, C19, C20, C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20A, C19A, C18A, C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(O11A)=1-FVAR(1)
 Sof(O11)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Fixed Sof: C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C20(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20A(0.5) H20D(0.5)
 H20E(0.5) H20F(0.5) C18A(0.5) H18D(0.5) H18E(0.5) H18F(0.5) C19A(0.5)
 H19D(0.5) H19E(0.5) H19F(0.5)
6.a Ternary CH refined with riding coordinates:
 O9(H9)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C10(H10), C3(H3), C12(H12), C5(H5), C11(H11), C4(H4)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C23(H23A,H23B,
 H23C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C),
 C20A(H20D,H20E,H20F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C26(H26A,
 H26B,H26C), C26A(H26D,H26E,H26F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.63794(2) 0.20973(2) 0.60899(2) 0.03205(5) Uani 1 1 d . . . . .
Tb2 Tb 0.666667 0.333333 0.80059(2) 0.03334(7) Uani 1 3 d S T P . .
Ni1 Ni 0.77505(2) 0.22928(2) 0.75329(3) 0.03599(10) Uani 1 1 d D . . . .
O10 O 0.666667 0.333333 0.6477(2) 0.0324(8) Uani 1 3 d S T P . .
O9 O 0.67105(12) 0.22375(12) 0.75863(14) 0.0336(5) Uani 1 1 d . . . . .
H9 H 0.633865 0.178562 0.791670 0.040 Uiso 1 1 calc R U . . .
O1 O 0.73507(13) 0.18007(13) 0.63601(15) 0.0396(5) Uani 1 1 d . . . . .
O2 O 0.64125(14) 0.08791(14) 0.52243(17) 0.0487(6) Uani 1 1 d . . . . .
O4 O 0.91391(13) 0.45546(13) 0.67176(16) 0.0433(6) Uani 1 1 d . . . . .
O3 O 0.82140(12) 0.33714(12) 0.69574(14) 0.0360(5) Uani 1 1 d . . . . .
O5 O 0.81184(15) 0.26820(15) 0.87465(16) 0.0509(6) Uani 1 1 d . . . . .
O6 O 0.76369(15) 0.34579(15) 0.89399(16) 0.0514(6) Uani 1 1 d . . . . .
O7 O 0.72109(17) 0.27536(18) 0.49825(19) 0.0672(8) Uani 1 1 d . . . . .
O8 O 0.83484(17) 0.38026(17) 0.49780(18) 0.0590(7) Uani 1 1 d . . . . .
N1 N 0.87689(16) 0.23806(16) 0.72106(19) 0.0418(7) Uani 1 1 d . . . . .
C15 C 0.89224(19) 0.3899(2) 0.7028(2) 0.0370(7) Uani 1 1 d . . . . .
C14 C 0.95053(19) 0.3759(2) 0.7482(2) 0.0406(8) Uani 1 1 d . . . . .
C1 C 0.7538(2) 0.13116(19) 0.6023(2) 0.0406(8) Uani 1 1 d . . . . .
C9 C 0.94363(19) 0.3028(2) 0.7559(2) 0.0444(8) Uani 1 1 d . . . . .
C7 C 0.8836(2) 0.1900(2) 0.6726(3) 0.0476(9) Uani 1 1 d . . . . .
H7 H 0.931637 0.193709 0.669714 0.057 Uiso 1 1 calc R U . . .
C2 C 0.7027(2) 0.0781(2) 0.5407(2) 0.0462(9) Uani 1 1 d . . . . .
C16 C 0.8012(2) 0.3144(2) 0.9188(2) 0.0431(8) Uani 1 1 d D . . . .
C13 C 1.0164(2) 0.4389(2) 0.7811(3) 0.0494(9) Uani 1 1 d . . . . .
H13 H 1.022326 0.487823 0.775704 0.059 Uiso 1 1 calc R U . . .
C21 C 0.7862(2) 0.3184(2) 0.4637(2) 0.0476(9) Uani 1 1 d . . . . .
C6 C 0.8219(2) 0.1302(2) 0.6218(3) 0.0471(9) Uani 1 1 d . . . . .
C22 C 0.8034(2) 0.2926(2) 0.3774(2) 0.0486(9) Uani 1 1 d . . . . .
C10 C 1.0008(2) 0.2948(2) 0.7969(3) 0.0621(11) Uani 1 1 d . . . . .
H10 H 0.995737 0.246319 0.802761 0.074 Uiso 1 1 calc R U . . .
C8 C 0.5922(3) 0.0414(3) 0.4527(3) 0.0683(12) Uani 1 1 d . . . . .
H8A H 0.622216 0.051547 0.400783 0.102 Uiso 1 1 calc R U . . .
H8B H 0.552270 0.053674 0.443307 0.102 Uiso 1 1 calc R U . . .
H8C H 0.569583 -0.012106 0.467631 0.102 Uiso 1 1 calc R U . . .
C3 C 0.7176(3) 0.0245(3) 0.5037(3) 0.0677(12) Uani 1 1 d . . . . .
H3 H 0.683065 -0.010372 0.463687 0.081 Uiso 1 1 calc R U . . .
C12 C 1.0735(2) 0.4308(3) 0.8216(3) 0.0632(12) Uani 1 1 d . . . . .
H12 H 1.117073 0.473652 0.843371 0.076 Uiso 1 1 calc R U . . .
C5 C 0.8348(3) 0.0743(2) 0.5818(3) 0.0669(12) Uani 1 1 d . . . . .
H5 H 0.879680 0.073428 0.594496 0.080 Uiso 1 1 calc R U . . .
C17 C 0.8383(3) 0.3355(3) 1.0090(3) 0.0639(11) Uani 1 1 d D . . . .
C11 C 1.0652(3) 0.3591(3) 0.8292(3) 0.0744(14) Uani 1 1 d . . . . .
H11 H 1.103498 0.353418 0.856553 0.089 Uiso 1 1 calc R U . . .
C24 C 0.8231(4) 0.2307(4) 0.3959(4) 0.109(2) Uani 1 1 d . . . . .
H24A H 0.867645 0.250985 0.432720 0.164 Uiso 1 1 calc R U . . .
H24B H 0.833872 0.213403 0.342352 0.164 Uiso 1 1 calc R U . . .
H24C H 0.780447 0.188122 0.424295 0.164 Uiso 1 1 calc R U . . .
C25 C 0.8697(3) 0.3596(3) 0.3314(3) 0.0852(17) Uani 1 1 d . . . . .
H25A H 0.915610 0.378069 0.365585 0.128 Uiso 1 1 calc R U . . .
H25B H 0.858056 0.400192 0.323646 0.128 Uiso 1 1 calc R U . . .
H25C H 0.877411 0.342909 0.275860 0.128 Uiso 1 1 calc R U . . .
C23 C 0.7327(3) 0.2602(4) 0.3188(4) 0.108(2) Uani 1 1 d . . . . .
H23A H 0.744033 0.244252 0.264697 0.162 Uiso 1 1 calc R U . . .
H23B H 0.719230 0.299183 0.308218 0.162 Uiso 1 1 calc R U . . .
H23C H 0.690422 0.216764 0.346503 0.162 Uiso 1 1 calc R U . . .
C4 C 0.7835(3) 0.0219(3) 0.5253(4) 0.0790(15) Uani 1 1 d . . . . .
H4 H 0.792435 -0.015537 0.501214 0.095 Uiso 1 1 calc R U . . .
C18 C 0.8036(10) 0.3727(8) 1.0645(9) 0.103(5) Uani 0.5 1 d D U P A 1
H18A H 0.809030 0.417535 1.035573 0.154 Uiso 0.5 1 calc R U P A 1
H18B H 0.829854 0.387414 1.119298 0.154 Uiso 0.5 1 calc R U P A 1
H18C H 0.749990 0.336733 1.073954 0.154 Uiso 0.5 1 calc R U P A 1
C20 C 0.9233(5) 0.3839(11) 1.0007(10) 0.149(8) Uani 0.5 1 d D . P A 1
H20A H 0.942769 0.356511 0.967995 0.223 Uiso 0.5 1 calc R U P A 1
H20B H 0.946197 0.395386 1.057366 0.223 Uiso 0.5 1 calc R U P A 1
H20C H 0.935837 0.430974 0.971395 0.223 Uiso 0.5 1 calc R U P A 1
C19 C 0.8184(9) 0.2602(6) 1.0558(7) 0.105(5) Uani 0.5 1 d D . P A 1
H19A H 0.763412 0.228434 1.060277 0.158 Uiso 0.5 1 calc R U P A 1
H19B H 0.840502 0.271647 1.112873 0.158 Uiso 0.5 1 calc R U P A 1
H19C H 0.838667 0.233291 1.023638 0.158 Uiso 0.5 1 calc R U P A 1
C20A C 0.8974(8) 0.4220(7) 1.0012(11) 0.130(6) Uani 0.5 1 d D U P A 2
H20D H 0.925083 0.431537 0.947603 0.195 Uiso 0.5 1 calc R U P A 2
H20E H 0.932833 0.437578 1.048855 0.195 Uiso 0.5 1 calc R U P A 2
H20F H 0.870994 0.450935 1.002212 0.195 Uiso 0.5 1 calc R U P A 2
C18A C 0.7813(8) 0.3270(10) 1.0757(10) 0.124(6) Uani 0.5 1 d D U P A 2
H18D H 0.750531 0.347732 1.054016 0.186 Uiso 0.5 1 calc R U P A 2
H18E H 0.807806 0.354306 1.127196 0.186 Uiso 0.5 1 calc R U P A 2
H18F H 0.748640 0.273413 1.089127 0.186 Uiso 0.5 1 calc R U P A 2
C19A C 0.8848(11) 0.2970(12) 1.0276(11) 0.152(6) Uani 0.5 1 d D U P A 2
H19D H 0.919127 0.322551 1.075222 0.228 Uiso 0.5 1 calc R U P A 2
H19E H 0.914243 0.299838 0.977184 0.228 Uiso 0.5 1 calc R U P A 2
H19F H 0.850812 0.243936 1.042356 0.228 Uiso 0.5 1 calc R U P A 2
O11 O 0.7280(3) 0.1172(2) 0.8083(3) 0.0621(13) Uani 0.831(9) 1 d D . P B 1
C26 C 0.6702(5) 0.0476(4) 0.7868(6) 0.119(3) Uani 0.831(9) 1 d D . P B 1
H26A H 0.644425 0.051773 0.736417 0.178 Uiso 0.831(9) 1 calc R U P B 1
H26B H 0.634439 0.026866 0.834087 0.178 Uiso 0.831(9) 1 calc R U P B 1
H26C H 0.690354 0.014066 0.774376 0.178 Uiso 0.831(9) 1 calc R U P B 1
C26A C 0.680(2) 0.089(2) 0.876(3) 0.119(3) Uani 0.169(9) 1 d D . P B 2
H26D H 0.635602 0.080295 0.843063 0.178 Uiso 0.169(9) 1 calc R U P B 2
H26E H 0.683770 0.117613 0.927319 0.178 Uiso 0.169(9) 1 calc R U P B 2
H26F H 0.674226 0.039902 0.892261 0.178 Uiso 0.169(9) 1 calc R U P B 2
O11A O 0.7434(18) 0.1279(14) 0.828(2) 0.0621(13) Uani 0.169(9) 1 d D . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O10 2.3240(10) . ?
Tb1 O9 2.378(2) . ?
Tb1 O1 2.340(2) . ?
Tb1 O2 2.813(2) . ?
Tb1 O4 2.455(2) 3_665 ?
Tb1 O3 2.579(2) 3_665 ?
Tb1 O7 2.287(3) . ?
Tb1 O8 2.350(3) 3_665 ?
Tb2 O10 2.357(4) . ?
Tb2 O9 2.333(2) 2_655 ?
Tb2 O9 2.333(2) 3_665 ?
Tb2 O9 2.333(2) . ?
Tb2 O6 2.331(2) . ?
Tb2 O6 2.331(2) 2_655 ?
Tb2 O6 2.331(2) 3_665 ?
Ni1 O9 2.033(2) . ?
Ni1 O1 2.024(2) . ?
Ni1 O3 2.078(2) . ?
Ni1 O5 2.020(2) . ?
Ni1 N1 2.022(3) . ?
Ni1 O11 2.130(4) . ?
O9 H9 0.9800 . ?
O1 C1 1.319(4) . ?
O2 C2 1.370(4) . ?
O2 C8 1.440(4) . ?
O4 C15 1.255(4) . ?
O3 C15 1.283(4) . ?
O5 C16 1.250(4) . ?
O6 C16 1.258(4) . ?
O7 C21 1.267(5) . ?
O8 C21 1.247(5) . ?
N1 C9 1.423(4) . ?
N1 C7 1.278(5) . ?
C15 C14 1.504(5) . ?
C14 C9 1.407(5) . ?
C14 C13 1.389(5) . ?
C1 C2 1.412(5) . ?
C1 C6 1.409(5) . ?
C9 C10 1.386(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.447(5) . ?
C2 C3 1.373(5) . ?
C16 C17 1.533(5) . ?
C13 H13 0.9300 . ?
C13 C12 1.383(5) . ?
C21 C22 1.528(5) . ?
C6 C5 1.411(5) . ?
C22 C24 1.507(6) . ?
C22 C25 1.512(6) . ?
C22 C23 1.525(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.383(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C3 H3 0.9300 . ?
C3 C4 1.391(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.368(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.356(6) . ?
C17 C18 1.514(10) . ?
C17 C20 1.486(10) . ?
C17 C19 1.536(9) . ?
C17 C20A 1.540(11) . ?
C17 C18A 1.483(11) . ?
C17 C19A 1.507(10) . ?
C11 H11 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C4 H4 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18A H18F 0.9600 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
O11 C26 1.335(8) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C26A H26D 0.9600 . ?
C26A H26E 0.9600 . ?
C26A H26F 0.9600 . ?
C26A O11A 1.34(2) . ?

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
O10 Tb1 O9 73.68(10) . . ?
O10 Tb1 O1 115.54(6) . . ?
O10 Tb1 O2 161.23(8) . . ?
O10 Tb1 O4 128.72(8) . 3_665 ?
O10 Tb1 O3 79.84(6) . 3_665 ?
O10 Tb1 O8 108.70(9) . 3_665 ?
O9 Tb1 O2 115.89(7) . . ?
O9 Tb1 O4 76.65(8) . 3_665 ?
O9 Tb1 O3 72.58(7) . 3_665 ?
O1 Tb1 O9 68.83(7) . . ?
O1 Tb1 O2 58.67(7) . . ?
O1 Tb1 O4 90.47(8) . 3_665 ?
O1 Tb1 O3 131.04(8) . 3_665 ?
O1 Tb1 O8 129.21(9) . 3_665 ?
O4 Tb1 O2 70.05(8) 3_665 . ?
O4 Tb1 O3 51.55(7) 3_665 3_665 ?
O3 Tb1 O2 117.90(7) 3_665 . ?
O7 Tb1 O10 81.83(11) . . ?
O7 Tb1 O9 125.19(10) . . ?
O7 Tb1 O1 79.60(9) . . ?
O7 Tb1 O2 79.53(10) . . ?
O7 Tb1 O4 148.70(10) . 3_665 ?
O7 Tb1 O3 149.01(9) . 3_665 ?
O7 Tb1 O8 83.32(11) . 3_665 ?
O8 Tb1 O9 150.85(9) 3_665 . ?
O8 Tb1 O2 71.36(9) 3_665 . ?
O8 Tb1 O4 80.24(9) 3_665 3_665 ?
O8 Tb1 O3 79.20(9) 3_665 3_665 ?
O10 Tb2 Tb1 37.242(8) . 2_655 ?
O9 Tb2 Tb1 100.88(5) 3_665 2_655 ?
O9 Tb2 Tb1 38.47(5) 2_655 2_655 ?
O9 Tb2 Tb1 86.10(5) . 2_655 ?
O9 Tb2 O10 73.90(5) . . ?
O9 Tb2 O10 73.90(5) 3_665 . ?
O9 Tb2 O10 73.90(5) 2_655 . ?
O9 Tb2 O9 112.63(5) 2_655 3_665 ?
O9 Tb2 O9 112.62(5) . 2_655 ?
O9 Tb2 O9 112.62(5) . 3_665 ?
O6 Tb2 Tb1 97.44(7) . 2_655 ?
O6 Tb2 Tb1 160.07(7) 3_665 2_655 ?
O6 Tb2 Tb1 113.95(6) 2_655 2_655 ?
O6 Tb2 O10 128.16(7) 2_655 . ?
O6 Tb2 O10 128.16(7) . . ?
O6 Tb2 O10 128.16(7) 3_665 . ?
O6 Tb2 O9 74.92(8) 2_655 3_665 ?
O6 Tb2 O9 157.53(8) 3_665 2_655 ?
O6 Tb2 O9 81.37(8) 3_665 3_665 ?
O6 Tb2 O9 157.53(8) . 3_665 ?
O6 Tb2 O9 74.92(8) 3_665 . ?
O6 Tb2 O9 81.38(8) 2_655 2_655 ?
O6 Tb2 O9 74.91(9) . 2_655 ?
O6 Tb2 O9 81.37(8) . . ?
O6 Tb2 O9 157.53(8) 2_655 . ?
O6 Tb2 O6 85.84(10) 3_665 2_655 ?
O6 Tb2 O6 85.84(10) . 3_665 ?
O6 Tb2 O6 85.84(10) . 2_655 ?
O9 Ni1 O3 89.25(8) . . ?
O9 Ni1 O11 91.43(19) . . ?
O1 Ni1 O9 82.20(9) . . ?
O1 Ni1 O3 89.29(9) . . ?
O1 Ni1 O11 89.03(16) . . ?
O3 Ni1 O11 178.09(18) . . ?
O5 Ni1 O9 98.62(10) . . ?
O5 Ni1 O1 174.52(10) . . ?
O5 Ni1 O3 96.13(10) . . ?
O5 Ni1 N1 92.09(11) . . ?
O5 Ni1 O11 85.54(16) . . ?
N1 Ni1 O9 167.96(10) . . ?
N1 Ni1 O1 87.66(11) . . ?
N1 Ni1 O3 84.13(10) . . ?
N1 Ni1 O11 94.9(2) . . ?
Tb1 O10 Tb1 113.64(7) 2_655 3_665 ?
Tb1 O10 Tb1 113.64(7) . 2_655 ?
Tb1 O10 Tb1 113.64(7) . 3_665 ?
Tb1 O10 Tb2 104.89(8) 3_665 . ?
Tb1 O10 Tb2 104.89(8) 2_655 . ?
Tb1 O10 Tb2 104.89(8) . . ?
Tb1 O9 H9 110.9 . . ?
Tb2 O9 Tb1 103.92(8) . . ?
Tb2 O9 H9 110.9 . . ?
Ni1 O9 Tb1 100.67(9) . . ?
Ni1 O9 Tb2 118.69(10) . . ?
Ni1 O9 H9 110.9 . . ?
Ni1 O1 Tb1 102.26(9) . . ?
C1 O1 Tb1 134.5(2) . . ?
C1 O1 Ni1 121.6(2) . . ?
C2 O2 Tb1 116.2(2) . . ?
C2 O2 C8 115.5(3) . . ?
C8 O2 Tb1 127.7(2) . . ?
C15 O4 Tb1 97.8(2) . 2_655 ?
Ni1 O3 Tb1 144.85(10) . 2_655 ?
C15 O3 Tb1 91.18(19) . 2_655 ?
C15 O3 Ni1 123.8(2) . . ?
C16 O5 Ni1 128.8(2) . . ?
C16 O6 Tb2 144.1(2) . . ?
C21 O7 Tb1 155.8(3) . . ?
C21 O8 Tb1 116.5(2) . 2_655 ?
C9 N1 Ni1 115.8(2) . . ?
C7 N1 Ni1 124.0(3) . . ?
C7 N1 C9 120.2(3) . . ?
O4 C15 Tb1 56.89(17) . 2_655 ?
O4 C15 O3 119.5(3) . . ?
O4 C15 C14 118.6(3) . . ?
O3 C15 Tb1 62.62(16) . 2_655 ?
O3 C15 C14 122.0(3) . . ?
C14 C15 Tb1 175.3(2) . 2_655 ?
C9 C14 C15 123.5(3) . . ?
C13 C14 C15 118.3(3) . . ?
C13 C14 C9 118.1(3) . . ?
O1 C1 C2 117.2(3) . . ?
O1 C1 C6 124.3(3) . . ?
C6 C1 C2 118.4(3) . . ?
C14 C9 N1 118.4(3) . . ?
C10 C9 N1 121.4(3) . . ?
C10 C9 C14 120.1(3) . . ?
N1 C7 H7 117.5 . . ?
N1 C7 C6 125.0(3) . . ?
C6 C7 H7 117.5 . . ?
O2 C2 C1 113.2(3) . . ?
O2 C2 C3 126.1(4) . . ?
C3 C2 C1 120.6(4) . . ?
O5 C16 O6 124.8(3) . . ?
O5 C16 C17 117.4(3) . . ?
O6 C16 C17 117.8(3) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 C14 121.6(4) . . ?
C12 C13 H13 119.2 . . ?
O7 C21 C22 117.7(4) . . ?
O8 C21 O7 121.8(4) . . ?
O8 C21 C22 120.4(3) . . ?
C1 C6 C7 122.5(3) . . ?
C1 C6 C5 118.7(4) . . ?
C5 C6 C7 118.4(4) . . ?
C24 C22 C21 108.1(4) . . ?
C24 C22 C25 110.1(4) . . ?
C24 C22 C23 109.4(5) . . ?
C25 C22 C21 110.8(3) . . ?
C25 C22 C23 108.5(4) . . ?
C23 C22 C21 110.0(4) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 H10 120.0 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 120.9(4) . . ?
C4 C3 H3 119.5 . . ?
C13 C12 H12 120.3 . . ?
C11 C12 C13 119.4(4) . . ?
C11 C12 H12 120.3 . . ?
C6 C5 H5 119.0 . . ?
C4 C5 C6 121.9(4) . . ?
C4 C5 H5 119.0 . . ?
C16 C17 C19 107.6(5) . . ?
C16 C17 C20A 103.5(7) . . ?
C18 C17 C16 111.8(7) . . ?
C18 C17 C19 105.1(8) . . ?
C20 C17 C16 110.0(7) . . ?
C20 C17 C18 112.7(10) . . ?
C20 C17 C19 109.4(9) . . ?
C18A C17 C16 111.0(7) . . ?
C18A C17 C20A 107.3(9) . . ?
C18A C17 C19A 116.6(10) . . ?
C19A C17 C16 111.8(7) . . ?
C19A C17 C20A 105.5(9) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.9(4) . . ?
C12 C11 H11 119.6 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.3(4) . . ?
C5 C4 H4 120.3 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20A H20D 109.5 . . ?
C17 C20A H20E 109.5 . . ?
C17 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C17 C18A H18D 109.5 . . ?
C17 C18A H18E 109.5 . . ?
C17 C18A H18F 109.5 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C17 C19A H19D 109.5 . . ?
C17 C19A H19E 109.5 . . ?
C17 C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C26 O11 Ni1 134.3(4) . . ?
O11 C26 H26A 109.5 . . ?
O11 C26 H26B 109.5 . . ?
O11 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
H26D C26A H26E 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
O11A C26A H26D 109.5 . . ?
O11A C26A H26E 109.5 . . ?
O11A C26A H26F 109.5 . . ?
C26A O11A Ni1 127(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C1 C2 -6.8(5) . . . . ?
Tb1 O1 C1 C6 171.2(3) . . . . ?
Tb1 O2 C2 C1 1.1(4) . . . . ?
Tb1 O2 C2 C3 -177.3(4) . . . . ?
Tb1 O4 C15 O3 -2.2(3) 2_655 . . . ?
Tb1 O4 C15 C14 178.5(2) 2_655 . . . ?
Tb1 O3 C15 O4 2.1(3) 2_655 . . . ?
Tb1 O3 C15 C14 -178.6(3) 2_655 . . . ?
Tb1 O7 C21 O8 -46.3(9) . . . . ?
Tb1 O7 C21 C22 134.3(6) . . . . ?
Tb1 O8 C21 O7 -14.7(5) 2_655 . . . ?
Tb1 O8 C21 C22 164.7(3) 2_655 . . . ?
Tb2 O6 C16 O5 25.0(7) . . . . ?
Tb2 O6 C16 C17 -156.5(3) . . . . ?
Ni1 O1 C1 C2 155.7(3) . . . . ?
Ni1 O1 C1 C6 -26.4(5) . . . . ?
Ni1 O3 C15 Tb1 -176.3(2) . . . 2_655 ?
Ni1 O3 C15 O4 -174.2(2) . . . . ?
Ni1 O3 C15 C14 5.1(4) . . . . ?
Ni1 O5 C16 O6 0.2(6) . . . . ?
Ni1 O5 C16 C17 -178.3(3) . . . . ?
Ni1 N1 C9 C14 -48.3(4) . . . . ?
Ni1 N1 C9 C10 131.3(3) . . . . ?
Ni1 N1 C7 C6 11.1(5) . . . . ?
O1 C1 C2 O2 2.5(5) . . . . ?
O1 C1 C2 C3 -179.0(4) . . . . ?
O1 C1 C6 C7 -8.4(6) . . . . ?
O1 C1 C6 C5 179.4(4) . . . . ?
O2 C2 C3 C4 177.6(4) . . . . ?
O4 C15 C14 C9 -154.6(3) . . . . ?
O4 C15 C14 C13 22.4(5) . . . . ?
O3 C15 C14 C9 26.0(5) . . . . ?
O3 C15 C14 C13 -156.9(3) . . . . ?
O5 C16 C17 C18 -164.0(7) . . . . ?
O5 C16 C17 C20 70.0(10) . . . . ?
O5 C16 C17 C19 -49.1(8) . . . . ?
O5 C16 C17 C20A 114.9(8) . . . . ?
O5 C16 C17 C18A -130.2(8) . . . . ?
O5 C16 C17 C19A 1.8(11) . . . . ?
O6 C16 C17 C18 17.4(8) . . . . ?
O6 C16 C17 C20 -108.6(10) . . . . ?
O6 C16 C17 C19 132.3(7) . . . . ?
O6 C16 C17 C20A -63.7(8) . . . . ?
O6 C16 C17 C18A 51.2(9) . . . . ?
O6 C16 C17 C19A -176.8(10) . . . . ?
O7 C21 C22 C24 -77.6(5) . . . . ?
O7 C21 C22 C25 161.7(4) . . . . ?
O7 C21 C22 C23 41.8(5) . . . . ?
O8 C21 C22 C24 103.0(5) . . . . ?
O8 C21 C22 C25 -17.7(6) . . . . ?
O8 C21 C22 C23 -137.6(4) . . . . ?
N1 C9 C10 C11 179.3(4) . . . . ?
N1 C7 C6 C1 17.3(6) . . . . ?
N1 C7 C6 C5 -170.6(4) . . . . ?
C15 C14 C9 N1 -1.9(5) . . . . ?
C15 C14 C9 C10 178.4(4) . . . . ?
C15 C14 C13 C12 -178.2(4) . . . . ?
C14 C9 C10 C11 -1.0(7) . . . . ?
C14 C13 C12 C11 0.3(7) . . . . ?
C1 C2 C3 C4 -0.7(7) . . . . ?
C1 C6 C5 C4 0.1(7) . . . . ?
C9 N1 C7 C6 -168.8(4) . . . . ?
C9 C14 C13 C12 -1.1(6) . . . . ?
C9 C10 C11 C12 0.2(8) . . . . ?
C7 N1 C9 C14 131.5(4) . . . . ?
C7 N1 C9 C10 -48.8(5) . . . . ?
C7 C6 C5 C4 -172.3(5) . . . . ?
C2 C1 C6 C7 169.5(4) . . . . ?
C2 C1 C6 C5 -2.6(6) . . . . ?
C2 C3 C4 C5 -1.9(8) . . . . ?
C13 C14 C9 N1 -178.9(3) . . . . ?
C13 C14 C9 C10 1.4(6) . . . . ?
C13 C12 C11 C10 0.1(8) . . . . ?
C6 C1 C2 O2 -175.6(3) . . . . ?
C6 C1 C2 C3 2.9(6) . . . . ?
C6 C5 C4 C3 2.2(8) . . . . ?
C8 O2 C2 C1 173.0(3) . . . . ?
C8 O2 C2 C3 -5.4(6) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 187 electrons were 
found in a volume of 1220Å³ in 1 void per unit cell. 
This is consistent with the presence of 9[H2O] per 
Formula Unit which account for 180 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.512 1219.9 187.2 '18 H2O'
2 0.333 0.667 0.813 7.3 0.0 ?
3 0.667 0.333 0.187 7.3 0.5 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT242_complex_2           
;
PROBLEM:Low    'MainMol' Ueq as Compared to Neighbors of        C17 Check 
RESPONSE:This is due to disorder in the terminal t-butyl group.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_complex_3
_database_code_depnum_ccdc_archive 'CCDC 2095748'
loop_
_audit_author_name
_audit_author_address
'Mousumi Biswas'
;IIT Kharagpur
India
;
_audit_update_record             
;
2023-07-07 deposited with the CCDC.	2023-07-11 downloaded from the CCDC.
;
_audit_creation_date             2023-07-05
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C78 H99 Ho4 N3 Ni3 O31, 2H, 11[H2O]'
_chemical_formula_sum            'C78 H123 Ho4 N3 Ni3 O42'
_chemical_formula_weight         2610.62
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   20.033(4)
_cell_length_b                   20.033(4)
_cell_length_c                   15.367(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5341(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9272
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.075
_cell_measurement_theta_min      2.347
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.524
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            97643
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.162
_diffrn_reflns_theta_max         25.162
_diffrn_reflns_theta_min         2.348
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5740
_reflns_number_total             6347
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5-beta (Bourhis et al., 2015)'
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6347
_refine_ls_number_restraints     113
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0219
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0152P)²+8.4272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0525
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C17-C20 \\sim C17-C20A
 with sigma of 0.02
 C17-C19 \\sim C17-C19A
 with sigma of 0.02
 C17-C18 \\sim C17-C18A
 with sigma of 0.02
 C17-C19 \\sim C17-C20 \\sim C17-C18 \\sim C17-C18A \\sim C17-C20A \\sim
C17-C19A \\sim C17-C16
 with sigma of 0.02
 C19-C20 \\sim C19-C18 \\sim C20-C18 \\sim C18A-C20A \\sim C18A-C19A
 with sigma of 0.04
 O11-C26 \\sim O11-C26A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C20A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C18A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) = Uanis(C26A)
4. Rigid body (RIGU) restrains
 C18A, C19A, C20A, C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C18, C20, C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Fixed Sof: C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C18A(0.5) H18D(0.5)
 H18E(0.5) H18F(0.5) C20A(0.5) H20D(0.5) H20E(0.5) H20F(0.5) C19A(0.5)
 H19D(0.5) H19E(0.5) H19F(0.5)
6.a Ternary CH refined with riding coordinates:
 O9(H9)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C7(H7), C10(H10), C5(H5), C11(H11), C3(H3), C13(H13), C4(H4)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C),
 C18A(H18D,H18E,H18F), C20A(H20D,H20E,H20F), C19A(H19D,H19E,H19F), C26(H26A,
 H26B,H26C), C26A(H26D,H26E,H26F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.63814(2) 0.21030(2) 0.38975(2) 0.03259(5) Uani 1 1 d . . . . .
Ho2 Ho 0.666667 0.333333 0.19997(2) 0.03409(7) Uani 1 3 d S T P . .
Ni1 Ni 0.77473(2) 0.22987(2) 0.24639(3) 0.03686(10) Uani 1 1 d . . . . .
O10 O 0.666667 0.333333 0.3524(2) 0.0330(8) Uani 1 3 d S T P . .
O9 O 0.67104(12) 0.22506(12) 0.24141(13) 0.0343(5) Uani 1 1 d . . . . .
H9 H 0.633746 0.179966 0.208154 0.051 Uiso 1 1 calc R U . . .
O1 O 0.73399(13) 0.18018(13) 0.36326(14) 0.0414(5) Uani 1 1 d . . . . .
O2 O 0.64007(14) 0.08794(14) 0.47726(16) 0.0498(6) Uani 1 1 d . . . . .
O3 O 0.82089(12) 0.33745(12) 0.30439(13) 0.0367(5) Uani 1 1 d . . . . .
O5 O 0.81168(15) 0.26895(15) 0.12477(15) 0.0516(6) Uani 1 1 d . . . . .
O4 O 0.91279(13) 0.45583(13) 0.32819(15) 0.0441(5) Uani 1 1 d . . . . .
O6 O 0.76205(15) 0.34524(15) 0.10575(16) 0.0528(6) Uani 1 1 d . . . . .
O8 O 0.83193(16) 0.37855(15) 0.49954(16) 0.0555(6) Uani 1 1 d . . . . .
O7 O 0.71881(16) 0.27210(17) 0.50173(18) 0.0640(7) Uani 1 1 d . . . . .
N1 N 0.87651(16) 0.23861(16) 0.27889(18) 0.0424(6) Uani 1 1 d . . . . .
C15 C 0.89179(18) 0.39036(19) 0.2974(2) 0.0365(7) Uani 1 1 d . . . . .
O11 O 0.72870(19) 0.11949(16) 0.1881(2) 0.0725(8) Uani 1 1 d D . . . .
C1 C 0.75245(19) 0.13137(19) 0.3975(2) 0.0413(7) Uani 1 1 d . . . . .
C21 C 0.7840(2) 0.3168(2) 0.5349(2) 0.0471(8) Uani 1 1 d . . . . .
C14 C 0.95030(19) 0.3764(2) 0.2524(2) 0.0410(7) Uani 1 1 d . . . . .
C16 C 0.8005(2) 0.3152(2) 0.0811(2) 0.0446(8) Uani 1 1 d D . . . .
C9 C 0.94365(19) 0.3035(2) 0.2449(2) 0.0449(8) Uani 1 1 d . . . . .
C12 C 1.0162(2) 0.4398(2) 0.2204(2) 0.0485(8) Uani 1 1 d . . . . .
H12 H 1.021982 0.488640 0.225822 0.058 Uiso 1 1 calc R U . . .
C7 C 0.8831(2) 0.1905(2) 0.3280(2) 0.0478(8) Uani 1 1 d . . . . .
H7 H 0.931277 0.194437 0.331677 0.057 Uiso 1 1 calc R U . . .
C2 C 0.7015(2) 0.0779(2) 0.4594(2) 0.0470(8) Uani 1 1 d . . . . .
C6 C 0.8212(2) 0.1308(2) 0.3780(2) 0.0470(8) Uani 1 1 d . . . . .
C22 C 0.8030(2) 0.2926(2) 0.6216(2) 0.0487(8) Uani 1 1 d . . . . .
C8 C 0.5915(3) 0.0423(3) 0.5481(3) 0.0698(12) Uani 1 1 d . . . . .
H8A H 0.621858 0.053186 0.599996 0.105 Uiso 1 1 calc R U . . .
H8B H 0.568733 -0.011421 0.534041 0.105 Uiso 1 1 calc R U . . .
H8C H 0.551554 0.054712 0.557323 0.105 Uiso 1 1 calc R U . . .
C10 C 1.0014(2) 0.2956(2) 0.2048(3) 0.0635(11) Uani 1 1 d . . . . .
H10 H 0.996475 0.247122 0.199397 0.076 Uiso 1 1 calc R U . . .
C5 C 0.8338(3) 0.0745(2) 0.4186(3) 0.0680(12) Uani 1 1 d . . . . .
H5 H 0.878872 0.073663 0.406356 0.082 Uiso 1 1 calc R U . . .
C25 C 0.8222(4) 0.2298(3) 0.6037(4) 0.106(2) Uani 1 1 d . . . . .
H25A H 0.778843 0.186854 0.576446 0.159 Uiso 1 1 calc R U . . .
H25B H 0.833727 0.213352 0.657479 0.159 Uiso 1 1 calc R U . . .
H25C H 0.866034 0.249289 0.565764 0.159 Uiso 1 1 calc R U . . .
C11 C 1.0738(2) 0.4316(3) 0.1805(3) 0.0640(11) Uani 1 1 d . . . . .
H11 H 1.117496 0.474636 0.159020 0.077 Uiso 1 1 calc R U . . .
C3 C 0.7157(3) 0.0241(2) 0.4967(3) 0.0672(12) Uani 1 1 d . . . . .
H3 H 0.681006 -0.010921 0.536663 0.081 Uiso 1 1 calc R U . . .
C13 C 1.0659(2) 0.3597(3) 0.1729(3) 0.0729(13) Uani 1 1 d . . . . .
H13 H 1.104527 0.354212 0.146044 0.087 Uiso 1 1 calc R U . . .
C23 C 0.8702(3) 0.3599(3) 0.6663(3) 0.0835(15) Uani 1 1 d . . . . .
H23A H 0.914881 0.379824 0.629562 0.125 Uiso 1 1 calc R U . . .
H23B H 0.880707 0.342971 0.720417 0.125 Uiso 1 1 calc R U . . .
H23C H 0.857684 0.399506 0.677264 0.125 Uiso 1 1 calc R U . . .
C17 C 0.8384(3) 0.3374(3) -0.0086(2) 0.0669(11) Uani 1 1 d D . . . .
C4 C 0.7820(3) 0.0217(3) 0.4749(4) 0.0799(15) Uani 1 1 d . . . . .
H4 H 0.790769 -0.015887 0.498827 0.096 Uiso 1 1 calc R U . . .
C24 C 0.7332(3) 0.2610(4) 0.6817(3) 0.1023(19) Uani 1 1 d . . . . .
H24A H 0.721849 0.301182 0.694941 0.153 Uiso 1 1 calc R U . . .
H24B H 0.744113 0.242853 0.734636 0.153 Uiso 1 1 calc R U . . .
H24C H 0.689560 0.219244 0.653450 0.153 Uiso 1 1 calc R U . . .
C19 C 0.8042(11) 0.3748(10) -0.0633(11) 0.117(6) Uani 0.5 1 d D . P A 1
H19A H 0.817162 0.423893 -0.038707 0.176 Uiso 0.5 1 calc R U P A 1
H19B H 0.749125 0.342424 -0.064794 0.176 Uiso 0.5 1 calc R U P A 1
H19C H 0.824271 0.382019 -0.121383 0.176 Uiso 0.5 1 calc R U P A 1
C20 C 0.8177(9) 0.2613(6) -0.0567(6) 0.104(4) Uani 0.5 1 d D . P A 1
H20A H 0.762646 0.229550 -0.060275 0.156 Uiso 0.5 1 calc R U P A 1
H20B H 0.838472 0.234439 -0.025271 0.156 Uiso 0.5 1 calc R U P A 1
H20C H 0.839058 0.272924 -0.114308 0.156 Uiso 0.5 1 calc R U P A 1
C18 C 0.9230(5) 0.3840(11) -0.0012(8) 0.126(5) Uani 0.5 1 d D U P A 1
H18A H 0.936653 0.431265 0.028655 0.190 Uiso 0.5 1 calc R U P A 1
H18B H 0.945399 0.395449 -0.058319 0.190 Uiso 0.5 1 calc R U P A 1
H18C H 0.941875 0.355770 0.030833 0.190 Uiso 0.5 1 calc R U P A 1
C18A C 0.8903(11) 0.3053(13) -0.0248(11) 0.158(6) Uani 0.5 1 d D U P A 2
H18D H 0.910307 0.317823 -0.082918 0.236 Uiso 0.5 1 calc R U P A 2
H18E H 0.861738 0.250333 -0.017894 0.236 Uiso 0.5 1 calc R U P A 2
H18F H 0.932112 0.327125 0.016061 0.236 Uiso 0.5 1 calc R U P A 2
C20A C 0.7850(10) 0.3341(12) -0.0754(11) 0.117(6) Uani 0.5 1 d D U P A 2
H20D H 0.746204 0.281346 -0.085263 0.176 Uiso 0.5 1 calc R U P A 2
H20E H 0.812732 0.355887 -0.128508 0.176 Uiso 0.5 1 calc R U P A 2
H20F H 0.761062 0.362738 -0.056478 0.176 Uiso 0.5 1 calc R U P A 2
C19A C 0.8957(9) 0.4263(6) 0.0017(9) 0.126(5) Uani 0.5 1 d D U P A 2
H19D H 0.932417 0.434713 0.046638 0.190 Uiso 0.5 1 calc R U P A 2
H19E H 0.867410 0.451591 0.017032 0.190 Uiso 0.5 1 calc R U P A 2
H19F H 0.922342 0.446852 -0.052237 0.190 Uiso 0.5 1 calc R U P A 2
C26 C 0.6710(5) 0.0482(5) 0.2127(7) 0.160(4) Uani 0.837(9) 1 d D . P B 1
H26A H 0.643884 0.053176 0.261479 0.240 Uiso 0.837(9) 1 calc R U P B 1
H26B H 0.692744 0.016726 0.228839 0.240 Uiso 0.837(9) 1 calc R U P B 1
H26C H 0.635902 0.024495 0.165096 0.240 Uiso 0.837(9) 1 calc R U P B 1
C26A C 0.708(3) 0.114(3) 0.1040(16) 0.160(4) Uani 0.163(9) 1 d D . P B 2
H26D H 0.724203 0.082025 0.073949 0.240 Uiso 0.163(9) 1 calc R U P B 2
H26E H 0.733188 0.164313 0.078298 0.240 Uiso 0.163(9) 1 calc R U P B 2
H26F H 0.653565 0.091337 0.099680 0.240 Uiso 0.163(9) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O10 2.3069(9) . ?
Ho1 O9 2.350(2) . ?
Ho1 O1 2.319(2) . ?
Ho1 O2 2.813(2) . ?
Ho1 O3 2.554(2) 3_665 ?
Ho1 O4 2.431(2) 3_665 ?
Ho1 O8 2.318(2) 3_665 ?
Ho1 O7 2.259(2) . ?
Ho2 O10 2.342(3) . ?
Ho2 O9 2.304(2) 3_665 ?
Ho2 O9 2.304(2) . ?
Ho2 O9 2.304(2) 2_655 ?
Ho2 O6 2.313(2) 2_655 ?
Ho2 O6 2.313(2) . ?
Ho2 O6 2.313(2) 3_665 ?
Ni1 O9 2.032(2) . ?
Ni1 O1 2.018(2) . ?
Ni1 O3 2.074(2) . ?
Ni1 O5 2.018(2) . ?
Ni1 N1 2.020(3) . ?
Ni1 O11 2.122(3) . ?
O9 H9 0.9800 . ?
O1 C1 1.316(4) . ?
O2 C2 1.369(4) . ?
O2 C8 1.441(4) . ?
O3 C15 1.283(4) . ?
O5 C16 1.252(4) . ?
O4 C15 1.253(4) . ?
O6 C16 1.251(4) . ?
O8 C21 1.250(4) . ?
O7 C21 1.263(4) . ?
N1 C9 1.423(4) . ?
N1 C7 1.282(4) . ?
C15 C14 1.503(4) . ?
O11 C26 1.367(9) . ?
O11 C26A 1.34(2) . ?
C1 C2 1.415(5) . ?
C1 C6 1.416(5) . ?
C21 C22 1.531(5) . ?
C14 C9 1.403(5) . ?
C14 C12 1.386(5) . ?
C16 C17 1.529(5) . ?
C9 C10 1.387(5) . ?
C12 H12 0.9300 . ?
C12 C11 1.385(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.441(5) . ?
C2 C3 1.371(5) . ?
C6 C5 1.417(5) . ?
C22 C25 1.512(6) . ?
C22 C23 1.512(5) . ?
C22 C24 1.526(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10 0.9300 . ?
C10 C13 1.379(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.359(6) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C11 H11 0.9300 . ?
C11 C13 1.374(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.394(6) . ?
C13 H13 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C17 C19 1.501(11) . ?
C17 C20 1.552(9) . ?
C17 C18 1.474(10) . ?
C17 C18A 1.490(10) . ?
C17 C20A 1.459(11) . ?
C17 C19A 1.571(10) . ?
C4 H4 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18A H18F 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C26A H26D 0.9600 . ?
C26A H26E 0.9600 . ?
C26A H26F 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
O10 Ho1 O9 73.76(9) . . ?
O10 Ho1 O1 116.07(6) . . ?
O10 Ho1 O2 161.06(8) . . ?
O10 Ho1 O3 80.22(6) . 3_665 ?
O10 Ho1 O4 129.56(8) . 3_665 ?
O10 Ho1 O8 107.42(9) . 3_665 ?
O9 Ho1 O2 116.62(7) . . ?
O9 Ho1 O3 72.89(7) . 3_665 ?
O9 Ho1 O4 77.19(8) . 3_665 ?
O1 Ho1 O9 69.26(7) . . ?
O1 Ho1 O2 58.87(7) . . ?
O1 Ho1 O3 131.21(7) . 3_665 ?
O1 Ho1 O4 89.92(8) . 3_665 ?
O3 Ho1 O2 117.35(7) 3_665 . ?
O4 Ho1 O2 69.35(8) 3_665 . ?
O4 Ho1 O3 51.97(7) 3_665 3_665 ?
O8 Ho1 O9 150.79(8) 3_665 . ?
O8 Ho1 O1 129.76(8) 3_665 . ?
O8 Ho1 O2 71.75(8) 3_665 . ?
O8 Ho1 O3 78.53(8) 3_665 3_665 ?
O8 Ho1 O4 80.64(9) 3_665 3_665 ?
O7 Ho1 O10 82.93(10) . . ?
O7 Ho1 O9 126.23(9) . . ?
O7 Ho1 O1 79.50(9) . . ?
O7 Ho1 O2 78.21(9) . . ?
O7 Ho1 O3 149.17(8) . 3_665 ?
O7 Ho1 O4 146.66(9) . 3_665 ?
O7 Ho1 O8 82.19(10) . 3_665 ?
O10 Ho2 Ho1 37.459(8) . . ?
O9 Ho2 Ho1 101.08(5) 2_655 . ?
O9 Ho2 Ho1 38.31(5) . . ?
O9 Ho2 Ho1 86.23(5) 3_665 . ?
O9 Ho2 O10 73.96(5) 3_665 . ?
O9 Ho2 O10 73.95(5) . . ?
O9 Ho2 O10 73.96(5) 2_655 . ?
O9 Ho2 O9 112.67(4) 2_655 3_665 ?
O9 Ho2 O9 112.67(4) . 3_665 ?
O9 Ho2 O9 112.67(4) . 2_655 ?
O9 Ho2 O6 75.37(8) 3_665 2_655 ?
O9 Ho2 O6 81.47(8) 3_665 3_665 ?
O9 Ho2 O6 156.93(8) 3_665 . ?
O9 Ho2 O6 156.93(8) 2_655 3_665 ?
O9 Ho2 O6 75.37(8) 2_655 . ?
O9 Ho2 O6 81.47(8) 2_655 2_655 ?
O9 Ho2 O6 156.93(8) . 2_655 ?
O9 Ho2 O6 75.37(8) . 3_665 ?
O9 Ho2 O6 81.48(8) . . ?
O6 Ho2 Ho1 97.88(7) 3_665 . ?
O6 Ho2 Ho1 114.17(6) . . ?
O6 Ho2 Ho1 160.80(7) 2_655 . ?
O6 Ho2 O10 128.76(7) 2_655 . ?
O6 Ho2 O10 128.76(7) 3_665 . ?
O6 Ho2 O10 128.76(7) . . ?
O6 Ho2 O6 84.96(10) 3_665 2_655 ?
O6 Ho2 O6 84.96(10) . 3_665 ?
O6 Ho2 O6 84.96(10) . 2_655 ?
O9 Ni1 O3 88.82(8) . . ?
O9 Ni1 O11 91.91(11) . . ?
O1 Ni1 O9 81.85(8) . . ?
O1 Ni1 O3 89.44(9) . . ?
O1 Ni1 O5 174.31(10) . . ?
O1 Ni1 N1 87.97(10) . . ?
O1 Ni1 O11 90.20(11) . . ?
O3 Ni1 O11 179.13(12) . . ?
O5 Ni1 O9 98.71(9) . . ?
O5 Ni1 O3 96.22(10) . . ?
O5 Ni1 N1 92.11(11) . . ?
O5 Ni1 O11 84.12(12) . . ?
N1 Ni1 O9 167.67(10) . . ?
N1 Ni1 O3 84.11(10) . . ?
N1 Ni1 O11 95.08(12) . . ?
Ho1 O10 Ho1 114.03(6) 2_655 3_665 ?
Ho1 O10 Ho1 114.03(6) . 2_655 ?
Ho1 O10 Ho1 114.03(6) . 3_665 ?
Ho1 O10 Ho2 104.40(8) 2_655 . ?
Ho1 O10 Ho2 104.40(8) . . ?
Ho1 O10 Ho2 104.40(8) 3_665 . ?
Ho1 O9 H9 110.7 . . ?
Ho2 O9 Ho1 104.25(8) . . ?
Ho2 O9 H9 110.7 . . ?
Ni1 O9 Ho1 100.67(8) . . ?
Ni1 O9 Ho2 119.00(9) . . ?
Ni1 O9 H9 110.7 . . ?
Ni1 O1 Ho1 102.20(9) . . ?
C1 O1 Ho1 134.5(2) . . ?
C1 O1 Ni1 121.8(2) . . ?
C2 O2 Ho1 115.88(19) . . ?
C2 O2 C8 115.4(3) . . ?
C8 O2 Ho1 127.9(2) . . ?
Ni1 O3 Ho1 144.84(10) . 2_655 ?
C15 O3 Ho1 91.10(18) . 2_655 ?
C15 O3 Ni1 123.83(19) . . ?
C16 O5 Ni1 128.1(2) . . ?
C15 O4 Ho1 97.72(19) . 2_655 ?
C16 O6 Ho2 144.7(2) . . ?
C21 O8 Ho1 118.3(2) . 2_655 ?
C21 O7 Ho1 153.9(3) . . ?
C9 N1 Ni1 116.1(2) . . ?
C7 N1 Ni1 124.0(2) . . ?
C7 N1 C9 119.9(3) . . ?
O3 C15 Ho1 62.44(15) . 2_655 ?
O3 C15 C14 121.9(3) . . ?
O4 C15 Ho1 56.75(16) . 2_655 ?
O4 C15 O3 119.1(3) . . ?
O4 C15 C14 118.9(3) . . ?
C14 C15 Ho1 175.5(2) . 2_655 ?
C26 O11 Ni1 132.3(4) . . ?
C26A O11 Ni1 117(2) . . ?
O1 C1 C2 117.8(3) . . ?
O1 C1 C6 124.0(3) . . ?
C2 C1 C6 118.2(3) . . ?
O8 C21 O7 122.5(3) . . ?
O8 C21 C22 120.1(3) . . ?
O7 C21 C22 117.4(3) . . ?
C9 C14 C15 123.6(3) . . ?
C12 C14 C15 117.9(3) . . ?
C12 C14 C9 118.4(3) . . ?
O5 C16 C17 116.9(3) . . ?
O6 C16 O5 125.1(3) . . ?
O6 C16 C17 118.0(3) . . ?
C14 C9 N1 118.4(3) . . ?
C10 C9 N1 121.3(3) . . ?
C10 C9 C14 120.3(3) . . ?
C14 C12 H12 119.4 . . ?
C11 C12 C14 121.1(4) . . ?
C11 C12 H12 119.4 . . ?
N1 C7 H7 117.6 . . ?
N1 C7 C6 124.7(3) . . ?
C6 C7 H7 117.6 . . ?
O2 C2 C1 112.7(3) . . ?
O2 C2 C3 125.9(3) . . ?
C3 C2 C1 121.4(4) . . ?
C1 C6 C7 122.8(3) . . ?
C1 C6 C5 118.4(3) . . ?
C5 C6 C7 118.3(3) . . ?
C25 C22 C21 108.2(3) . . ?
C25 C22 C24 109.1(4) . . ?
C23 C22 C21 111.4(3) . . ?
C23 C22 C25 110.0(4) . . ?
C23 C22 C24 108.5(4) . . ?
C24 C22 C21 109.6(3) . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C10 H10 120.0 . . ?
C13 C10 C9 119.9(4) . . ?
C13 C10 H10 120.0 . . ?
C6 C5 H5 119.0 . . ?
C4 C5 C6 121.9(4) . . ?
C4 C5 H5 119.0 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C12 C11 H11 120.1 . . ?
C13 C11 C12 119.8(4) . . ?
C13 C11 H11 120.1 . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.2(4) . . ?
C4 C3 H3 119.9 . . ?
C10 C13 H13 119.7 . . ?
C11 C13 C10 120.5(4) . . ?
C11 C13 H13 119.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C16 C17 C20 107.1(5) . . ?
C16 C17 C19A 102.3(6) . . ?
C19 C17 C16 111.5(9) . . ?
C19 C17 C20 105.0(8) . . ?
C18 C17 C16 111.1(6) . . ?
C18 C17 C19 113.2(10) . . ?
C18 C17 C20 108.5(8) . . ?
C18A C17 C16 112.1(6) . . ?
C18A C17 C19A 103.5(9) . . ?
C20A C17 C16 112.0(9) . . ?
C20A C17 C18A 121.0(10) . . ?
C20A C17 C19A 103.1(10) . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C18A H18D 109.5 . . ?
C17 C18A H18E 109.5 . . ?
C17 C18A H18F 109.5 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C17 C20A H20D 109.5 . . ?
C17 C20A H20E 109.5 . . ?
C17 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C17 C19A H19D 109.5 . . ?
C17 C19A H19E 109.5 . . ?
C17 C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
O11 C26 H26A 109.5 . . ?
O11 C26 H26B 109.5 . . ?
O11 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O11 C26A H26D 109.5 . . ?
O11 C26A H26E 109.5 . . ?
O11 C26A H26F 109.5 . . ?
H26D C26A H26E 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O1 C1 C2 7.2(5) . . . . ?
Ho1 O1 C1 C6 -170.7(2) . . . . ?
Ho1 O2 C2 C1 -1.3(4) . . . . ?
Ho1 O2 C2 C3 177.5(3) . . . . ?
Ho1 O3 C15 O4 -2.2(3) 2_655 . . . ?
Ho1 O3 C15 C14 178.6(3) 2_655 . . . ?
Ho1 O4 C15 O3 2.4(3) 2_655 . . . ?
Ho1 O4 C15 C14 -178.4(2) 2_655 . . . ?
Ho1 O8 C21 O7 15.8(5) 2_655 . . . ?
Ho1 O8 C21 C22 -164.2(2) 2_655 . . . ?
Ho1 O7 C21 O8 39.8(8) . . . . ?
Ho1 O7 C21 C22 -140.2(5) . . . . ?
Ho2 O6 C16 O5 -22.2(7) . . . . ?
Ho2 O6 C16 C17 159.0(3) . . . . ?
Ni1 O1 C1 C2 -156.1(2) . . . . ?
Ni1 O1 C1 C6 25.9(4) . . . . ?
Ni1 O3 C15 Ho1 175.8(2) . . . 2_655 ?
Ni1 O3 C15 O4 173.6(2) . . . . ?
Ni1 O3 C15 C14 -5.6(4) . . . . ?
Ni1 O5 C16 O6 -1.3(5) . . . . ?
Ni1 O5 C16 C17 177.5(3) . . . . ?
Ni1 N1 C9 C14 47.6(4) . . . . ?
Ni1 N1 C9 C10 -132.1(3) . . . . ?
Ni1 N1 C7 C6 -10.3(5) . . . . ?
O1 C1 C2 O2 -2.5(5) . . . . ?
O1 C1 C2 C3 178.6(4) . . . . ?
O1 C1 C6 C7 9.0(6) . . . . ?
O1 C1 C6 C5 -179.3(4) . . . . ?
O2 C2 C3 C4 -177.8(4) . . . . ?
O3 C15 C14 C9 -25.9(5) . . . . ?
O3 C15 C14 C12 157.5(3) . . . . ?
O5 C16 C17 C19 164.5(8) . . . . ?
O5 C16 C17 C20 50.2(7) . . . . ?
O5 C16 C17 C18 -68.2(10) . . . . ?
O5 C16 C17 C18A -6.2(11) . . . . ?
O5 C16 C17 C20A 133.7(9) . . . . ?
O5 C16 C17 C19A -116.5(8) . . . . ?
O4 C15 C14 C9 155.0(3) . . . . ?
O4 C15 C14 C12 -21.6(5) . . . . ?
O6 C16 C17 C19 -16.6(9) . . . . ?
O6 C16 C17 C20 -130.9(7) . . . . ?
O6 C16 C17 C18 110.8(10) . . . . ?
O6 C16 C17 C18A 172.7(11) . . . . ?
O6 C16 C17 C20A -47.4(10) . . . . ?
O6 C16 C17 C19A 62.4(8) . . . . ?
O8 C21 C22 C25 -104.0(5) . . . . ?
O8 C21 C22 C23 17.0(5) . . . . ?
O8 C21 C22 C24 137.1(4) . . . . ?
O7 C21 C22 C25 76.0(5) . . . . ?
O7 C21 C22 C23 -163.0(4) . . . . ?
O7 C21 C22 C24 -42.9(5) . . . . ?
N1 C9 C10 C13 -179.6(4) . . . . ?
N1 C7 C6 C1 -17.9(6) . . . . ?
N1 C7 C6 C5 170.3(4) . . . . ?
C15 C14 C9 N1 2.4(5) . . . . ?
C15 C14 C9 C10 -177.9(3) . . . . ?
C15 C14 C12 C11 178.0(3) . . . . ?
C1 C2 C3 C4 0.9(7) . . . . ?
C1 C6 C5 C4 0.1(7) . . . . ?
C14 C9 C10 C13 0.7(6) . . . . ?
C14 C12 C11 C13 -0.5(6) . . . . ?
C9 N1 C7 C6 168.7(3) . . . . ?
C9 C14 C12 C11 1.2(5) . . . . ?
C9 C10 C13 C11 0.0(7) . . . . ?
C12 C14 C9 N1 179.0(3) . . . . ?
C12 C14 C9 C10 -1.3(5) . . . . ?
C12 C11 C13 C10 -0.1(7) . . . . ?
C7 N1 C9 C14 -131.5(4) . . . . ?
C7 N1 C9 C10 48.8(5) . . . . ?
C7 C6 C5 C4 172.2(5) . . . . ?
C2 C1 C6 C7 -168.9(3) . . . . ?
C2 C1 C6 C5 2.8(5) . . . . ?
C2 C3 C4 C5 2.1(8) . . . . ?
C6 C1 C2 O2 175.5(3) . . . . ?
C6 C1 C2 C3 -3.4(6) . . . . ?
C6 C5 C4 C3 -2.6(8) . . . . ?
C8 O2 C2 C1 -172.1(3) . . . . ?
C8 O2 C2 C3 6.7(6) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 236 electrons were 
found in a volume of 1247Å³ in 1 void per unit cell. 
This is consistent with the presence of 11[H2O] 
per Formula Unit which account for 220 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.957 1246.7 235.5 '22 H2O'
2 0.333 0.667 0.187 7.2 0.0 ?
3 0.667 0.333 0.813 7.2 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
