# Supplementary Information (SI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2025

####################################################################### 
# 
# 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_op1_a
_database_code_depnum_ccdc_archive 'CCDC 2472483'
loop_
_audit_author_name
_audit_author_address
'Maxim Shmelev'
;Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2025-07-14 deposited with the CCDC.	2025-11-06 downloaded from the CCDC.
;
_audit_creation_date             2024-10-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Gd H16 O8, 2(C10 H10 O10 V), 0.667(H2 O), C16 H36 N'
_chemical_formula_sum            'C36 H74 Gd N O29 V2'
_chemical_formula_weight         1244.09
_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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   15.8568(8)
_cell_length_b                   21.4138(11)
_cell_length_c                   15.4243(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5237.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.64
_shelx_estimated_absorpt_T_max   0.920
_shelx_estimated_absorpt_T_min   0.786
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1307 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.7578.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31266
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.627
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3560
_reflns_number_total             4465
_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 V8.35A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.955
_refine_diff_density_min         -2.030
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         4465
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0233P)²+33.4521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1137
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C17B-C18B = C17A-C18A = C17A-C16B = C17B-C16A = C16B-C15 = C16A-C15
 1.5 with sigma of 0.02
 C14A-C13 = C14B-C13
 1.55 with sigma of 0.02
 Gd1-HF \\sim Gd1-HG
 with sigma of 0.02
 Gd1-HD \\sim Gd1-HE
 with sigma of 0.02
 Gd1-HB \\sim Gd1-HC
 with sigma of 0.02
 Gd1-H \\sim Gd1-HA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18A) \\sim Ueq, Uanis(C18B) \\sim Ueq: with sigma of 0.015 and sigma for
terminal atoms of 0.03
Uanis(C12) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
Uanis(C16B) = Uanis(C16A)
4. Others
 Sof(O4A)=1-FVAR(1)
 Sof(O4B)=FVAR(1)
 Sof(HR)=Sof(HS)=Sof(C14B)=Sof(H6)=Sof(H7)=Sof(H8)=1-FVAR(2)
 Sof(HP)=Sof(HQ)=Sof(C14A)=Sof(HV)=Sof(HW)=Sof(HX)=FVAR(2)
 Sof(HJ)=Sof(HK)=Sof(C16B)=Sof(HY)=Sof(HZ)=Sof(C17A)=Sof(H1)=Sof(H2)=Sof(C18A)=
 Sof(H3)=Sof(H4)=Sof(H5)=1-FVAR(3)
 Sof(HL)=Sof(HM)=Sof(C16A)=Sof(H9)=Sof(H10)=Sof(C17B)=Sof(H11)=Sof(H12)=
 Sof(C18B)=Sof(H13)=Sof(H14)=Sof(H15)=FVAR(3)
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(4)
 Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=FVAR(4)
 Fixed Sof: O1S(0.333333) HH(0.333333) HI(0.333333) V1B(0.666667)
 H2A(0.333333) H2B(0.333333) V1A(0.333333) H1A(0.66666) H1B(0.66666)
5.a Riding coordinates:
 O11(H,HA), O14(HB,HC), O13(HD,HE), O12(HF,HG), O2(H2A,H2B), O1(H1A,H1B)
5.b Rotating group:
 O1S(HH,HI)
5.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C15(HJ,HK), C15(HL,HM), C11(HN,HO), C10A(H10A,H10B),
  C9A(H9AA,H9AB), C13(HP,HQ), C13(HR,HS), C12(HT,HU), C16B(HY,HZ), C17A(H1,H2),
 C16A(H9,H10), C17B(H11,H12), C10B(H10C,H10D), C9B(H9BA,H9BB)
5.d Me refined with riding coordinates:
 C18A(H3,H4,H5)
5.e Idealised Me refined as rotating group:
 C14A(HV,HW,HX), C14B(H6,H7,H8), C18B(H13,H14,H15)
;
_atom_sites_solution_hydrogens   mixed
_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
Gd1 Gd 0.19704(2) 0.7500 0.2500 0.02111(13) Uani 1 2 d DS T P . .
O11 O 0.2511(3) 0.80238(19) 0.3741(3) 0.0314(10) Uani 1 1 d . . . . .
H H 0.2230 0.8170 0.4164 0.047 Uiso 1 1 d DR U . . .
HA H 0.3021 0.8107 0.3863 0.047 Uiso 1 1 d DR U . . .
O14 O 0.3097(2) 0.68466(19) 0.2960(3) 0.0310(10) Uani 1 1 d . . . . .
HB H 0.3510 0.6703 0.2670 0.047 Uiso 1 1 d DR U . . .
HC H 0.3170 0.6703 0.3469 0.047 Uiso 1 1 d DR U . . .
O13 O 0.0830(3) 0.81041(19) 0.3057(3) 0.0318(10) Uani 1 1 d . . . . .
HD H 0.0430 0.8261 0.2762 0.048 Uiso 1 1 d DR U . . .
HE H 0.0725 0.8212 0.3576 0.048 Uiso 1 1 d DR U . . .
O12 O 0.1485(3) 0.8159(2) 0.1351(3) 0.0342(10) Uani 1 1 d . . . . .
HF H 0.0968 0.8151 0.1204 0.051 Uiso 1 1 d DR U . . .
HG H 0.1707 0.8428 0.1016 0.051 Uiso 1 1 d DR U . . .
O10 O 0.4541(3) 0.6387(2) 0.7109(3) 0.0528(14) Uani 1 1 d . . . . .
O6 O 0.6628(3) 0.8484(2) 0.4919(3) 0.0501(14) Uani 1 1 d . . . . .
O8 O 0.2488(3) 0.6287(3) 0.4916(4) 0.0731(19) Uani 1 1 d . . . . .
C3 C 0.5955(4) 0.8261(3) 0.4685(4) 0.0318(14) Uani 1 1 d . . . . .
C8 C 0.4329(4) 0.6546(3) 0.6368(4) 0.0358(15) Uani 1 1 d . . . . .
O4A O 0.4657(19) 0.8349(19) 0.2676(15) 0.054(9) Uani 0.67(8) 1 d . . P A 2
C6 C 0.3164(4) 0.6515(3) 0.5157(5) 0.0433(18) Uani 1 1 d . . . . .
C1 C 0.4795(5) 0.8243(4) 0.3463(5) 0.048(2) Uani 1 1 d . . . . .
C7 C 0.3484(4) 0.6353(3) 0.6043(4) 0.0368(16) Uani 1 1 d . . . . .
C5 C 0.6117(5) 0.8900(4) 0.3299(5) 0.051(2) Uani 1 1 d . . . . .
H5A H 0.5801 0.9128 0.2864 0.061 Uiso 1 1 calc R U . . .
H5B H 0.6516 0.9150 0.3626 0.061 Uiso 1 1 calc R U . . .
C2 C 0.5667(4) 0.8371(3) 0.3775(4) 0.0327(15) Uani 1 1 d . . . . .
C4 C 0.6352(5) 0.8253(4) 0.3102(5) 0.059(2) Uani 1 1 d . . . . .
H4A H 0.6895 0.8107 0.3307 0.071 Uiso 1 1 calc R U . . .
H4B H 0.6180 0.8085 0.2545 0.071 Uiso 1 1 calc R U . . .
O1S O 0.6025(7) 0.9179(5) 0.0531(8) 0.030(3) Uani 0.3333 1 d . . P . .
HH H 0.6513 0.9110 0.0323 0.045 Uiso 0.3333 1 d R U P . .
HI H 0.6118 0.9376 0.0999 0.045 Uiso 0.3333 1 d R U P . .
V1B V 0.44305(11) 0.74685(9) 0.50323(12) 0.0285(4) Uani 0.6667 1 d . . P B 2
O2 O 0.3813(4) 0.7855(3) 0.5677(5) 0.088(2) Uani 1 1 d . . . . .
H2A H 0.4214 0.8021 0.6106 0.132 Uiso 0.3333 1 d R U P B .
H2B H 0.3228 0.8004 0.5710 0.132 Uiso 0.3333 1 d R U P . .
V1A V 0.4754(3) 0.72257(17) 0.4740(2) 0.0311(8) Uani 0.3333 1 d . . P B 1
O1 O 0.5295(3) 0.6879(3) 0.4115(3) 0.0561(14) Uani 1 1 d . . . . .
H1A H 0.5604 0.6491 0.4241 0.084 Uiso 0.6667 1 d R U P B 2
H1B H 0.4901 0.6619 0.3783 0.084 Uiso 0.6667 1 d R U P B 2
O9 O 0.4833(3) 0.6858(2) 0.5877(3) 0.0434(12) Uani 1 1 d . . . . .
O7 O 0.3590(3) 0.6864(2) 0.4653(3) 0.0410(12) Uani 1 1 d . . . . .
O5 O 0.5496(3) 0.7930(2) 0.5198(3) 0.0338(10) Uani 1 1 d . . . . .
O3 O 0.4275(3) 0.7935(2) 0.3943(3) 0.0395(11) Uani 1 1 d . . . . .
O4B O 0.440(2) 0.8604(18) 0.294(3) 0.029(9) Uani 0.33(8) 1 d . . P A 1
N1 N 0.2500 1.0000 0.3486(6) 0.052(2) Uani 1 2 d S T P C .
C15 C 0.3098(6) 1.0382(5) 0.2931(7) 0.084(3) Uani 1 1 d D . . . .
HJ H 0.2745 1.0577 0.2495 0.101 Uiso 0.41(2) 1 calc R U P C 2
HK H 0.3291 1.0718 0.3304 0.101 Uiso 0.41(2) 1 calc R U P C 2
HL H 0.3508 1.0597 0.3291 0.101 Uiso 0.59(2) 1 calc R U P C 1
HM H 0.2790 1.0690 0.2596 0.101 Uiso 0.59(2) 1 calc R U P C 1
C11 C 0.2976(5) 0.9535(3) 0.4043(6) 0.057(2) Uani 1 1 d . . . . .
HN H 0.2571 0.9293 0.4373 0.069 Uiso 1 1 calc R U . C .
HO H 0.3276 0.9249 0.3665 0.069 Uiso 1 1 calc R U . . .
C10A C 0.2833(7) 0.6183(16) 0.6715(7) 0.052(8) Uani 0.74(5) 1 d . . P D 2
H10A H 0.2971 0.6267 0.7316 0.062 Uiso 0.74(5) 1 calc R U P D 2
H10B H 0.2246 0.6250 0.6566 0.062 Uiso 0.74(5) 1 calc R U P D 2
C9A C 0.3255(13) 0.5675(9) 0.6306(18) 0.060(6) Uani 0.74(5) 1 d . . P D 2
H9AA H 0.2936 0.5426 0.5895 0.072 Uiso 0.74(5) 1 calc R U P D 2
H9AB H 0.3663 0.5443 0.6647 0.072 Uiso 0.74(5) 1 calc R U P D 2
C13 C 0.4046(9) 0.9346(5) 0.5224(8) 0.112(4) Uani 1 1 d D . . . .
HP H 0.4102 0.8954 0.4914 0.135 Uiso 0.56(3) 1 calc R U P E 2
HQ H 0.4606 0.9495 0.5369 0.135 Uiso 0.56(3) 1 calc R U P E 2
HR H 0.3682 0.8984 0.5270 0.135 Uiso 0.44(3) 1 calc R U P E 1
HS H 0.4548 0.9215 0.4915 0.135 Uiso 0.44(3) 1 calc R U P E 1
C12 C 0.3595(8) 0.9822(5) 0.4659(8) 0.108(4) Uani 1 1 d . U . . .
HT H 0.3300 1.0116 0.5030 0.130 Uiso 1 1 calc R U . . .
HU H 0.4011 1.0055 0.4330 0.130 Uiso 1 1 calc R U . . .
C14A C 0.3558(15) 0.9255(10) 0.6005(12) 0.092(9) Uani 0.56(3) 1 d D . P E 2
HV H 0.3415 0.9654 0.6250 0.138 Uiso 0.56(3) 1 calc R U P E 2
HW H 0.3883 0.9020 0.6416 0.138 Uiso 0.56(3) 1 calc R U P E 2
HX H 0.3050 0.9031 0.5868 0.138 Uiso 0.56(3) 1 calc R U P E 2
C16B C 0.3862(14) 1.0169(18) 0.246(2) 0.102(7) Uani 0.41(2) 1 d D . P C 2
HY H 0.4117 0.9815 0.2750 0.122 Uiso 0.41(2) 1 calc R U P C 2
HZ H 0.4275 1.0502 0.2420 0.122 Uiso 0.41(2) 1 calc R U P C 2
C17A C 0.3552(19) 0.9991(16) 0.159(2) 0.16(3) Uani 0.41(2) 1 d D . P C 2
H1 H 0.3319 0.9572 0.1611 0.198 Uiso 0.41(2) 1 calc R U P C 2
H2 H 0.3103 1.0273 0.1416 0.198 Uiso 0.41(2) 1 calc R U P C 2
C18A C 0.422(2) 1.001(2) 0.092(3) 0.126(15) Uani 0.41(2) 1 d D U P C 2
H3 H 0.3990 0.9890 0.0371 0.189 Uiso 0.41(2) 1 calc R U P C 2
H4 H 0.4446 1.0424 0.0884 0.189 Uiso 0.41(2) 1 calc R U P C 2
H5 H 0.4663 0.9723 0.1079 0.189 Uiso 0.41(2) 1 calc R U P C 2
C14B C 0.430(2) 0.9518(12) 0.6097(14) 0.112(14) Uani 0.44(3) 1 d D . P E 1
H6 H 0.4731 0.9834 0.6069 0.168 Uiso 0.44(3) 1 calc R U P E 1
H7 H 0.4519 0.9157 0.6391 0.168 Uiso 0.44(3) 1 calc R U P E 1
H8 H 0.3824 0.9678 0.6409 0.168 Uiso 0.44(3) 1 calc R U P E 1
C16A C 0.3534(15) 0.9918(10) 0.2337(15) 0.102(7) Uani 0.59(2) 1 d D . P C 1
H9 H 0.3880 0.9642 0.2687 0.122 Uiso 0.59(2) 1 calc R U P C 1
H10 H 0.3108 0.9664 0.2055 0.122 Uiso 0.59(2) 1 calc R U P C 1
C17B C 0.4073(18) 1.0209(9) 0.1660(13) 0.122(11) Uani 0.59(2) 1 d D . P C 1
H11 H 0.3711 1.0433 0.1260 0.147 Uiso 0.59(2) 1 calc R U P C 1
H12 H 0.4436 1.0514 0.1938 0.147 Uiso 0.59(2) 1 calc R U P C 1
C18B C 0.4605(17) 0.9781(10) 0.1158(16) 0.102(8) Uani 0.59(2) 1 d D U P C 1
H13 H 0.4990 1.0018 0.0808 0.152 Uiso 0.59(2) 1 calc R U P C 1
H14 H 0.4256 0.9528 0.0791 0.152 Uiso 0.59(2) 1 calc R U P C 1
H15 H 0.4917 0.9518 0.1546 0.152 Uiso 0.59(2) 1 calc R U P C 1
C10B C 0.278(3) 0.652(3) 0.676(3) 0.051(12) Uiso 0.26(5) 1 d . . P D 1
H10C H 0.2975 0.6694 0.7309 0.062 Uiso 0.26(5) 1 calc R U P D 1
H10D H 0.2240 0.6672 0.6562 0.062 Uiso 0.26(5) 1 calc R U P D 1
C9B C 0.304(3) 0.587(3) 0.653(3) 0.029(10) Uiso 0.26(5) 1 d . . P D 1
H9BA H 0.3363 0.5643 0.6959 0.035 Uiso 0.26(5) 1 calc R U P D 1
H9BB H 0.2633 0.5621 0.6217 0.035 Uiso 0.26(5) 1 calc R U P D 1


_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 O11 2.378(4) . ?
Gd1 O11 2.378(4) 4_565 ?
Gd1 O14 2.378(4) . ?
Gd1 O14 2.378(4) 4_565 ?
Gd1 O13 2.384(4) . ?
Gd1 O13 2.384(4) 4_565 ?
Gd1 O12 2.393(4) 4_565 ?
Gd1 O12 2.393(4) . ?
O11 H 0.8502 . ?
O11 HA 0.8495 . ?
O14 HB 0.8502 . ?
O14 HC 0.8501 . ?
O13 HD 0.8499 . ?
O13 HE 0.8499 . ?
O12 HF 0.8500 . ?
O12 HG 0.8502 . ?
O10 C8 1.240(7) . ?
O6 C3 1.223(7) . ?
O8 C6 1.236(8) . ?
C3 C2 1.496(8) . ?
C3 O5 1.288(7) . ?
C8 C7 1.489(9) . ?
C8 O9 1.288(7) . ?
O4A C1 1.254(14) . ?
C6 C7 1.498(9) . ?
C6 O7 1.272(8) . ?
C1 C2 1.490(9) . ?
C1 O3 1.290(8) . ?
C1 O4B 1.29(2) . ?
C7 C10A 1.507(11) . ?
C7 C9A 1.551(14) . ?
C7 C10B 1.61(4) . ?
C7 C9B 1.46(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C2 1.526(8) . ?
C5 C4 1.465(11) . ?
C2 C4 1.524(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O1S HH 0.8500 . ?
O1S HI 0.8499 . ?
V1B H2A 2.0633 . ?
V1B O1 2.341(5) . ?
V1B O9 1.952(5) . ?
V1B O7 1.948(5) . ?
V1B O5 1.973(4) . ?
V1B O3 1.970(4) . ?
O2 H2A 0.9832 . ?
O2 H2B 0.9831 . ?
O2 V1A 2.476(8) . ?
V1A O9 1.927(5) . ?
V1A O7 2.006(6) . ?
V1A O5 2.039(5) . ?
V1A O3 2.096(6) . ?
O1 H1A 0.9827 . ?
O1 H1B 0.9826 . ?
N1 C15 1.518(9) . ?
N1 C15 1.517(9) 2_575 ?
N1 C11 1.515(9) 2_575 ?
N1 C11 1.516(9) . ?
C15 HJ 0.9700 . ?
C15 HK 0.9700 . ?
C15 HL 0.9700 . ?
C15 HM 0.9700 . ?
C15 C16B 1.484(18) . ?
C15 C16A 1.519(17) . ?
C11 HN 0.9700 . ?
C11 HO 0.9700 . ?
C11 C12 1.499(13) . ?
C10A H10A 0.9700 . ?
C10A H10B 0.9700 . ?
C10A C9A 1.42(2) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C13 HP 0.9700 . ?
C13 HQ 0.9700 . ?
C13 HR 0.9700 . ?
C13 HS 0.9700 . ?
C13 C12 1.520(14) . ?
C13 C14A 1.446(15) . ?
C13 C14B 1.455(18) . ?
C12 HT 0.9700 . ?
C12 HU 0.9700 . ?
C14A HV 0.9600 . ?
C14A HW 0.9600 . ?
C14A HX 0.9600 . ?
C16B HY 0.9700 . ?
C16B HZ 0.9700 . ?
C16B C17A 1.485(19) . ?
C17A H1 0.9700 . ?
C17A H2 0.9700 . ?
C17A C18A 1.475(19) . ?
C18A H3 0.9600 . ?
C18A H4 0.9600 . ?
C18A H5 0.9600 . ?
C14B H6 0.9600 . ?
C14B H7 0.9600 . ?
C14B H8 0.9600 . ?
C16A H9 0.9700 . ?
C16A H10 0.9700 . ?
C16A C17B 1.487(17) . ?
C17B H11 0.9700 . ?
C17B H12 0.9700 . ?
C17B C18B 1.466(17) . ?
C18B H13 0.9600 . ?
C18B H14 0.9600 . ?
C18B H15 0.9600 . ?
C10B H10C 0.9700 . ?
C10B H10D 0.9700 . ?
C10B C9B 1.50(4) . ?
C9B H9BA 0.9700 . ?
C9B H9BB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Gd1 O11 137.8(2) . 4_565 ?
O11 Gd1 O14 76.50(14) 4_565 4_565 ?
O11 Gd1 O14 72.06(14) . 4_565 ?
O11 Gd1 O14 72.06(14) 4_565 . ?
O11 Gd1 O14 76.50(14) . . ?
O11 Gd1 O13 74.17(14) . . ?
O11 Gd1 O13 145.03(14) 4_565 . ?
O11 Gd1 O13 145.03(14) . 4_565 ?
O11 Gd1 O13 74.17(14) 4_565 4_565 ?
O11 Gd1 O12 115.69(14) 4_565 4_565 ?
O11 Gd1 O12 78.37(14) 4_565 . ?
O11 Gd1 O12 115.69(14) . . ?
O11 Gd1 O12 78.37(14) . 4_565 ?
O14 Gd1 O14 82.6(2) . 4_565 ?
O14 Gd1 O13 111.01(14) 4_565 . ?
O14 Gd1 O13 141.41(14) . . ?
O14 Gd1 O13 111.00(14) . 4_565 ?
O14 Gd1 O13 141.41(14) 4_565 4_565 ?
O14 Gd1 O12 144.11(14) 4_565 4_565 ?
O14 Gd1 O12 70.95(14) . 4_565 ?
O14 Gd1 O12 144.12(14) . . ?
O14 Gd1 O12 70.95(14) 4_565 . ?
O13 Gd1 O13 81.3(2) . 4_565 ?
O13 Gd1 O12 78.98(14) . 4_565 ?
O13 Gd1 O12 72.70(14) . . ?
O13 Gd1 O12 72.70(14) 4_565 4_565 ?
O13 Gd1 O12 78.98(14) 4_565 . ?
O12 Gd1 O12 142.4(2) 4_565 . ?
Gd1 O11 H 127.1 . . ?
Gd1 O11 HA 128.4 . . ?
H O11 HA 104.5 . . ?
Gd1 O14 HB 129.4 . . ?
Gd1 O14 HC 126.2 . . ?
HB O14 HC 104.5 . . ?
Gd1 O13 HD 125.9 . . ?
Gd1 O13 HE 129.5 . . ?
HD O13 HE 104.5 . . ?
Gd1 O12 HF 119.7 . . ?
Gd1 O12 HG 135.8 . . ?
HF O12 HG 104.5 . . ?
O6 C3 C2 118.8(5) . . ?
O6 C3 O5 121.8(6) . . ?
O5 C3 C2 119.4(5) . . ?
O10 C8 C7 118.5(6) . . ?
O10 C8 O9 121.1(6) . . ?
O9 C8 C7 120.3(5) . . ?
O8 C6 C7 118.5(6) . . ?
O8 C6 O7 120.6(6) . . ?
O7 C6 C7 120.8(6) . . ?
O4A C1 C2 116.1(11) . . ?
O4A C1 O3 122.5(8) . . ?
O3 C1 C2 120.2(6) . . ?
O4B C1 C2 123.3(10) . . ?
O4B C1 O3 110.8(17) . . ?
C8 C7 C6 123.2(5) . . ?
C8 C7 C10A 116.8(7) . . ?
C8 C7 C9A 112.5(7) . . ?
C8 C7 C10B 109.0(17) . . ?
C6 C7 C10A 116.8(7) . . ?
C6 C7 C9A 112.1(9) . . ?
C6 C7 C10B 109.9(17) . . ?
C10A C7 C9A 55.5(8) . . ?
C9B C7 C8 117.2(18) . . ?
C9B C7 C6 118.1(17) . . ?
C9B C7 C10B 58.1(16) . . ?
H5A C5 H5B 114.8 . . ?
C2 C5 H5A 117.6 . . ?
C2 C5 H5B 117.6 . . ?
C4 C5 H5A 117.6 . . ?
C4 C5 H5B 117.6 . . ?
C4 C5 C2 61.2(5) . . ?
C3 C2 C5 115.2(5) . . ?
C3 C2 C4 113.3(6) . . ?
C1 C2 C3 123.9(5) . . ?
C1 C2 C5 114.6(5) . . ?
C1 C2 C4 114.3(6) . . ?
C4 C2 C5 57.4(5) . . ?
C5 C4 C2 61.4(5) . . ?
C5 C4 H4A 117.6 . . ?
C5 C4 H4B 117.6 . . ?
C2 C4 H4A 117.6 . . ?
C2 C4 H4B 117.6 . . ?
H4A C4 H4B 114.7 . . ?
HH O1S HI 104.5 . . ?
O1 V1B H2A 153.1 . . ?
O9 V1B H2A 84.4 . . ?
O9 V1B O1 81.4(2) . . ?
O9 V1B O5 88.18(18) . . ?
O9 V1B O3 161.7(2) . . ?
O7 V1B H2A 120.5 . . ?
O7 V1B O1 82.0(2) . . ?
O7 V1B O9 88.81(19) . . ?
O7 V1B O5 163.1(2) . . ?
O7 V1B O3 89.70(18) . . ?
O5 V1B H2A 75.6 . . ?
O5 V1B O1 81.18(19) . . ?
O3 V1B H2A 111.9 . . ?
O3 V1B O1 80.3(2) . . ?
O3 V1B O5 87.96(17) . . ?
H2A O2 H2B 117.2 . . ?
V1A O2 H2A 101.6 . . ?
V1A O2 H2B 140.9 . . ?
O9 V1A O2 74.3(3) . . ?
O9 V1A O7 87.9(2) . . ?
O9 V1A O5 87.0(2) . . ?
O9 V1A O3 148.5(3) . . ?
O7 V1A O2 72.2(2) . . ?
O7 V1A O5 147.1(3) . . ?
O7 V1A O3 84.7(2) . . ?
O5 V1A O2 75.1(2) . . ?
O5 V1A O3 82.9(2) . . ?
O3 V1A O2 74.3(2) . . ?
V1B O1 H1A 128.8 . . ?
V1B O1 H1B 104.4 . . ?
H1A O1 H1B 86.6 . . ?
C8 O9 V1B 122.4(4) . . ?
C8 O9 V1A 134.9(4) . . ?
C6 O7 V1B 124.7(4) . . ?
C6 O7 V1A 132.5(4) . . ?
C3 O5 V1B 132.8(4) . . ?
C3 O5 V1A 121.3(4) . . ?
C1 O3 V1B 132.0(4) . . ?
C1 O3 V1A 118.4(5) . . ?
C15 N1 C15 111.4(11) 2_575 . ?
C11 N1 C15 106.1(5) 2_575 . ?
C11 N1 C15 111.2(5) 2_575 2_575 ?
C11 N1 C15 111.2(5) . . ?
C11 N1 C15 106.1(5) . 2_575 ?
C11 N1 C11 111.0(9) 2_575 . ?
N1 C15 HJ 105.2 . . ?
N1 C15 HK 105.2 . . ?
N1 C15 HL 110.6 . . ?
N1 C15 HM 110.6 . . ?
N1 C15 C16A 105.7(9) . . ?
HJ C15 HK 105.9 . . ?
HL C15 HM 108.7 . . ?
C16B C15 N1 128.3(16) . . ?
C16B C15 HJ 105.2 . . ?
C16B C15 HK 105.2 . . ?
C16A C15 HL 110.6 . . ?
C16A C15 HM 110.6 . . ?
N1 C11 HN 108.6 . . ?
N1 C11 HO 108.6 . . ?
HN C11 HO 107.6 . . ?
C12 C11 N1 114.6(6) . . ?
C12 C11 HN 108.6 . . ?
C12 C11 HO 108.6 . . ?
C7 C10A H10A 117.4 . . ?
C7 C10A H10B 117.4 . . ?
H10A C10A H10B 114.4 . . ?
C9A C10A C7 63.8(7) . . ?
C9A C10A H10A 117.4 . . ?
C9A C10A H10B 117.4 . . ?
C7 C9A H9AA 117.7 . . ?
C7 C9A H9AB 117.7 . . ?
C10A C9A C7 60.7(7) . . ?
C10A C9A H9AA 117.7 . . ?
C10A C9A H9AB 117.7 . . ?
H9AA C9A H9AB 114.8 . . ?
HP C13 HQ 108.4 . . ?
HR C13 HS 107.0 . . ?
C12 C13 HP 110.0 . . ?
C12 C13 HQ 110.0 . . ?
C12 C13 HR 107.5 . . ?
C12 C13 HS 107.5 . . ?
C14A C13 HP 110.0 . . ?
C14A C13 HQ 110.0 . . ?
C14A C13 C12 108.4(13) . . ?
C14B C13 HR 107.5 . . ?
C14B C13 HS 107.5 . . ?
C14B C13 C12 119.5(13) . . ?
C11 C12 C13 113.4(9) . . ?
C11 C12 HT 108.9 . . ?
C11 C12 HU 108.9 . . ?
C13 C12 HT 108.9 . . ?
C13 C12 HU 108.9 . . ?
HT C12 HU 107.7 . . ?
C13 C14A HV 109.5 . . ?
C13 C14A HW 109.5 . . ?
C13 C14A HX 109.5 . . ?
HV C14A HW 109.5 . . ?
HV C14A HX 109.5 . . ?
HW C14A HX 109.5 . . ?
C15 C16B HY 110.8 . . ?
C15 C16B HZ 110.8 . . ?
C15 C16B C17A 104.8(19) . . ?
HY C16B HZ 108.9 . . ?
C17A C16B HY 110.8 . . ?
C17A C16B HZ 110.8 . . ?
C16B C17A H1 109.1 . . ?
C16B C17A H2 109.1 . . ?
H1 C17A H2 107.8 . . ?
C18A C17A C16B 113(3) . . ?
C18A C17A H1 109.1 . . ?
C18A C17A H2 109.0 . . ?
C17A C18A H3 109.5 . . ?
C17A C18A H4 109.5 . . ?
C17A C18A H5 109.5 . . ?
H3 C18A H4 109.5 . . ?
H3 C18A H5 109.5 . . ?
H4 C18A H5 109.5 . . ?
C13 C14B H6 109.5 . . ?
C13 C14B H7 109.5 . . ?
C13 C14B H8 109.5 . . ?
H6 C14B H7 109.5 . . ?
H6 C14B H8 109.5 . . ?
H7 C14B H8 109.5 . . ?
C15 C16A H9 108.7 . . ?
C15 C16A H10 108.7 . . ?
H9 C16A H10 107.6 . . ?
C17B C16A C15 114.3(16) . . ?
C17B C16A H9 108.7 . . ?
C17B C16A H10 108.7 . . ?
C16A C17B H11 108.3 . . ?
C16A C17B H12 108.3 . . ?
H11 C17B H12 107.4 . . ?
C18B C17B C16A 116.1(17) . . ?
C18B C17B H11 108.3 . . ?
C18B C17B H12 108.3 . . ?
C17B C18B H13 109.5 . . ?
C17B C18B H14 109.5 . . ?
C17B C18B H15 109.5 . . ?
H13 C18B H14 109.5 . . ?
H13 C18B H15 109.5 . . ?
H14 C18B H15 109.5 . . ?
C7 C10B H10C 118.2 . . ?
C7 C10B H10D 118.2 . . ?
H10C C10B H10D 115.4 . . ?
C9B C10B C7 56(2) . . ?
C9B C10B H10C 118.2 . . ?
C9B C10B H10D 118.2 . . ?
C7 C9B C10B 66(3) . . ?
C7 C9B H9BA 117.1 . . ?
C7 C9B H9BB 117.1 . . ?
C10B C9B H9BA 117.1 . . ?
C10B C9B H9BB 117.1 . . ?
H9BA C9B H9BB 114.1 . . ?

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
O10 C8 C7 C6 -179.6(7) . . . . ?
O10 C8 C7 C10A 21.2(18) . . . . ?
O10 C8 C7 C9A -40.2(17) . . . . ?
O10 C8 C7 C10B 49(2) . . . . ?
O10 C8 C7 C9B -14(3) . . . . ?
O10 C8 O9 V1B -147.8(6) . . . . ?
O10 C8 O9 V1A -176.7(5) . . . . ?
O6 C3 C2 C1 -166.8(7) . . . . ?
O6 C3 C2 C5 -16.3(10) . . . . ?
O6 C3 C2 C4 47.2(9) . . . . ?
O6 C3 O5 V1B -176.2(5) . . . . ?
O6 C3 O5 V1A -148.7(6) . . . . ?
O8 C6 C7 C8 173.5(7) . . . . ?
O8 C6 C7 C10A -27.3(18) . . . . ?
O8 C6 C7 C9A 34.0(16) . . . . ?
O8 C6 C7 C10B -56(2) . . . . ?
O8 C6 C7 C9B 8(3) . . . . ?
O8 C6 O7 V1B 158.2(6) . . . . ?
O8 C6 O7 V1A -171.1(6) . . . . ?
C3 C2 C4 C5 -106.0(6) . . . . ?
C8 C7 C10A C9A -100.0(10) . . . . ?
C8 C7 C9A C10A 107.9(9) . . . . ?
C8 C7 C10B C9B -111(3) . . . . ?
C8 C7 C9B C10B 96(3) . . . . ?
O4A C1 C2 C3 -179(3) . . . . ?
O4A C1 C2 C5 31(3) . . . . ?
O4A C1 C2 C4 -33(3) . . . . ?
O4A C1 O3 V1B 158(3) . . . . ?
C6 C7 C10A C9A 99.5(12) . . . . ?
C6 C7 C9A C10A -108.1(10) . . . . ?
C6 C7 C10B C9B 111(2) . . . . ?
C6 C7 C9B C10B -97(3) . . . . ?
C1 C2 C4 C5 104.7(6) . . . . ?
C7 C8 O9 V1B 34.1(9) . . . . ?
C7 C8 O9 V1A 5.2(11) . . . . ?
C7 C6 O7 V1B -24.2(10) . . . . ?
C7 C6 O7 V1A 6.5(11) . . . . ?
C2 C3 O5 V1B 3.1(9) . . . . ?
C2 C3 O5 V1A 30.7(8) . . . . ?
C2 C1 O3 V1B -9.3(11) . . . . ?
C2 C1 O3 V1A -33.9(9) . . . . ?
C4 C5 C2 C3 102.6(7) . . . . ?
C4 C5 C2 C1 -104.2(7) . . . . ?
O9 C8 C7 C6 -1.5(11) . . . . ?
O9 C8 C7 C10A -160.6(16) . . . . ?
O9 C8 C7 C9A 137.9(16) . . . . ?
O9 C8 C7 C10B -132(2) . . . . ?
O9 C8 C7 C9B 164(2) . . . . ?
O7 C6 C7 C8 -4.1(11) . . . . ?
O7 C6 C7 C10A 155.0(16) . . . . ?
O7 C6 C7 C9A -143.7(15) . . . . ?
O7 C6 C7 C10B 126(2) . . . . ?
O7 C6 C7 C9B -170(2) . . . . ?
O5 C3 C2 C1 13.9(10) . . . . ?
O5 C3 C2 C5 164.3(6) . . . . ?
O5 C3 C2 C4 -132.1(6) . . . . ?
O3 C1 C2 C3 -10.9(12) . . . . ?
O3 C1 C2 C5 -161.5(7) . . . . ?
O3 C1 C2 C4 134.8(8) . . . . ?
O4B C1 C2 C3 140(3) . . . . ?
O4B C1 C2 C5 -11(4) . . . . ?
O4B C1 C2 C4 -74(4) . . . . ?
O4B C1 O3 V1A 172(3) . . . . ?
N1 C15 C16B C17A 91(3) . . . . ?
N1 C15 C16A C17B 173(2) . . . . ?
N1 C11 C12 C13 178.6(9) . . . . ?
C15 N1 C15 C16B -77.5(18) 2_575 . . . ?
C15 N1 C15 C16A -55.5(12) 2_575 . . . ?
C15 N1 C11 C12 -178.8(9) 2_575 . . . ?
C15 N1 C11 C12 60.0(11) . . . . ?
C15 C16B C17A C18A 157(3) . . . . ?
C15 C16A C17B C18B 171(2) . . . . ?
C11 N1 C15 C16B 161.4(18) 2_575 . . . ?
C11 N1 C15 C16B 41(2) . . . . ?
C11 N1 C15 C16A -176.6(13) 2_575 . . . ?
C11 N1 C15 C16A 62.6(14) . . . . ?
C11 N1 C11 C12 -57.9(8) 2_575 . . . ?
C14A C13 C12 C11 -89.8(17) . . . . ?
C14B C13 C12 C11 -148(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.101 0.250 0.750 12.6 1.0 ?
2 -0.101 0.750 0.250 12.6 1.0 ?
3 0.195 0.734 0.541 10.1 0.4 ?
4 0.195 0.766 -0.041 10.1 0.3 ?
5 0.250 0.500 0.762 17.4 0.2 ?
6 0.250 0.000 0.738 17.4 0.3 ?
7 0.250 0.000 0.019 6.5 0.5 ?
8 0.250 0.500 0.481 6.5 0.5 ?
9 0.305 0.234 0.959 10.1 0.6 ?
10 0.305 0.266 0.541 10.1 0.5 ?
11 0.399 0.750 0.750 12.6 1.1 ?
12 0.601 0.250 0.250 12.6 1.0 ?
13 0.695 0.734 0.459 10.1 0.3 ?
14 0.695 0.766 0.041 10.1 0.3 ?
15 0.750 0.500 0.238 17.4 0.2 ?
16 0.750 1.000 0.262 17.4 0.1 ?
17 0.750 0.000 -0.019 6.5 0.5 ?
18 0.750 0.500 0.519 6.5 0.5 ?
19 0.805 0.234 0.041 10.1 0.3 ?
20 0.805 0.266 0.459 10.1 0.3 ?

_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_104
_database_code_depnum_ccdc_archive 'CCDC 2472485'
loop_
_audit_author_name
_audit_author_address
'Maxim Shmelev'
;Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2025-07-14 deposited with the CCDC.	2025-11-06 downloaded from the CCDC.
;
_audit_creation_date             2024-10-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Dy H16 O8, 2(C10 H10 O10 V), C16 H36 N, 0.667(H2 O)'
_chemical_formula_sum            'C36 H73.33 Dy N O28.67 V2'
_chemical_formula_weight         1243.34
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   15.7781(12)
_cell_length_b                   21.2907(15)
_cell_length_c                   15.4105(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5176.8(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6316
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.66
_shelx_estimated_absorpt_T_max   0.896
_shelx_estimated_absorpt_T_min   0.807
_exptl_absorpt_coefficient_mu    1.871
_exptl_absorpt_correction_T_max  0.2657
_exptl_absorpt_correction_T_min  0.1877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1046 before and 0.0893 after correction.
The Ratio of minimum to maximum transmission is 0.7064.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2551
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36809
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.631
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3099
_reflns_number_total             4418
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.874
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4418
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0537
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0259P)²+40.2510P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1275
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Dy1-H12E_$1 \\sim Dy1-H12F_$1
 with sigma of 0.02
 Dy1-H14G_$1 \\sim Dy1-H14H_$1
 with sigma of 0.02
 Dy1-H11E_$1 \\sim Dy1-H11F_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13A) = Uanis(C13B)
Uanis(C12A) = Uanis(C12B)
Uanis(C14A) = Uanis(C13A)
Uanis(C10A) = Uanis(C9A)
Uiso(C9B) = Uiso(C10B)
Uanis(C18) = Uanis(C19B)
Uanis(C19A) = Uanis(C18)
4. Others
 Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(C14B)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C13B)=Sof(H13A)=Sof(H13B)=1-FVAR(1)
 Sof(H11A)=Sof(H11B)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C12A)=Sof(H12C)=
 Sof(H12D)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=FVAR(1)
 Sof(H2A)=Sof(H2B)=Sof(V1A)=1-FVAR(2)
 Sof(V1B)=Sof(H1A)=Sof(H1B)=FVAR(2)
 Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=1-FVAR(3)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=FVAR(3)
 Sof(O6A)=1-FVAR(4)
 Sof(O6B)=FVAR(4)
 Fixed Sof: H18C(0.5) H18D(0.5) H18A(0.5) H18B(0.5) O1S(0.333333)
 H1SA(0.333333) H1SB(0.333333) C19B(0.5) H19A(0.5) H19B(0.5) H19C(0.5)
 C19A(0.5) H19D(0.5) H19E(0.5) H19F(0.5)
5.a Riding coordinates:
 O12(H12E,H12F), O13(H13E,H13F), O14(H14G,H14H), O11(H11E,H11F), O1S(H1SA,H1SB)
5.b Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
5.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C16(H16A,H16B), C10B(H10A,H10B), C4(H4A,H4B), C9B(H9BA,H9BB),
 C18(H18C,H18D), C18(H18A,H18B), C17(H17A,H17B), C11(H11C,H11D), C11(H11A,H11B),
  C12B(H12A,H12B), C13B(H13A,H13B), C13A(H13C,H13D), C12A(H12C,H12D), C9A(H9AA,
 H9AB), C10A(H10C,H10D)
5.d Idealised Me refined as rotating group:
 C19B(H19A,H19B,H19C), C14B(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C19A(H19D,
 H19E,H19F)
;
_atom_sites_solution_hydrogens   mixed
_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 0.19669(3) 0.2500 0.7500 0.02484(15) Uani 1 2 d DS T P . .
V1B V 0.4421(3) 0.2475(3) 0.4964(3) 0.0265(14) Uani 0.628(16) 1 d . . P A 1
O5 O 0.4279(3) 0.2934(3) 0.6061(3) 0.0404(13) Uani 1 1 d . . . . .
O12 O 0.2505(3) 0.3025(2) 0.6270(3) 0.0323(12) Uani 1 1 d . . . . .
H12E H 0.2230 0.3172 0.5842 0.048 Uiso 1 1 d R U . . .
H12F H 0.3020 0.3110 0.6157 0.048 Uiso 1 1 d R U . . .
O3 O 0.5492(3) 0.2931(2) 0.4800(3) 0.0364(13) Uani 1 1 d . . . . .
O13 O 0.3089(3) 0.3158(2) 0.7962(3) 0.0322(12) Uani 1 1 d . . . . .
H13E H 0.3415 0.3232 0.7535 0.048 Uiso 1 1 d R U . . .
H13F H 0.3397 0.2960 0.8322 0.048 Uiso 1 1 d R U . . .
O14 O 0.1478(3) 0.3157(2) 0.8633(3) 0.0339(12) Uani 1 1 d . . . . .
H14G H 0.0960 0.3150 0.8785 0.051 Uiso 1 1 d R U . . .
H14H H 0.1704 0.3429 0.8965 0.051 Uiso 1 1 d R U . . .
O9 O 0.3584(3) 0.1860(3) 0.5349(3) 0.0425(14) Uani 1 1 d . . . . .
O7 O 0.4825(3) 0.1863(3) 0.4116(3) 0.0425(14) Uani 1 1 d . . . . .
O11 O 0.0829(3) 0.1898(2) 0.8053(3) 0.0308(12) Uani 1 1 d . . . . .
H11E H 0.0425 0.1739 0.7761 0.046 Uiso 1 1 d R U . . .
H11F H 0.0728 0.1790 0.8573 0.046 Uiso 1 1 d R U . . .
O4 O 0.6638(4) 0.3486(3) 0.5082(4) 0.0507(16) Uani 1 1 d . . . . .
O8 O 0.4528(4) 0.1385(3) 0.2885(3) 0.0516(16) Uani 1 1 d . . . . .
O1 O 0.5300(4) 0.1873(3) 0.5883(4) 0.0562(17) Uani 1 1 d . . . . .
H1A H 0.5419 0.1522 0.5641 0.084 Uiso 0.628(16) 1 d R U P A 1
H1B H 0.5025 0.1768 0.6341 0.084 Uiso 0.628(16) 1 d R U P A 1
O10 O 0.2467(4) 0.1285(4) 0.5087(4) 0.082(3) Uani 1 1 d . . . . .
C1 C 0.5958(5) 0.3264(4) 0.5324(5) 0.0365(19) Uani 1 1 d . . . . .
N1 N 0.2500 0.5000 0.6511(7) 0.053(3) Uani 1 2 d S T P G .
C6 C 0.4315(5) 0.1546(4) 0.3623(5) 0.0383(19) Uani 1 1 d . . . . .
O6A O 0.467(2) 0.3349(18) 0.7336(16) 0.053(9) Uani 0.65(7) 1 d . . P B 2
O2 O 0.3803(5) 0.2855(4) 0.4336(5) 0.089(2) Uani 1 1 d . . . . .
H2A H 0.3514 0.3203 0.4459 0.134 Uiso 0.372(16) 1 d R U P A 2
H2B H 0.3662 0.2785 0.3779 0.134 Uiso 0.372(16) 1 d R U P A 2
C7 C 0.3468(5) 0.1351(4) 0.3961(5) 0.0355(18) Uani 1 1 d . . . . .
C5 C 0.6130(5) 0.3904(4) 0.6700(5) 0.043(2) Uani 1 1 d . . . . .
H5A H 0.6532 0.4153 0.6369 0.051 Uiso 1 1 calc R U . . .
H5B H 0.5815 0.4138 0.7134 0.051 Uiso 1 1 calc R U . . .
C8 C 0.3139(5) 0.1515(4) 0.4832(5) 0.049(2) Uani 1 1 d . . . . .
C3 C 0.4803(6) 0.3240(4) 0.6548(5) 0.050(2) Uani 1 1 d . . . . .
C2 C 0.5673(5) 0.3375(4) 0.6232(5) 0.0361(19) Uani 1 1 d . . . . .
C16 C 0.2993(6) 0.4540(4) 0.5950(6) 0.056(2) Uani 1 1 d . . . . .
H16A H 0.3313 0.4263 0.6326 0.067 Uiso 1 1 calc R U . . .
H16B H 0.2594 0.4285 0.5627 0.067 Uiso 1 1 calc R U . . .
C10B C 0.2773(14) 0.1432(16) 0.3252(14) 0.029(5) Uiso 0.38(4) 1 d . . P C 2
H10A H 0.2214 0.1565 0.3439 0.034 Uiso 0.38(4) 1 calc R U P C 2
H10B H 0.2948 0.1595 0.2692 0.034 Uiso 0.38(4) 1 calc R U P C 2
C4 C 0.6363(6) 0.3253(5) 0.6905(6) 0.060(3) Uani 1 1 d . . . . .
H4A H 0.6190 0.3087 0.7464 0.071 Uiso 1 1 calc R U . . .
H4B H 0.6907 0.3101 0.6699 0.071 Uiso 1 1 calc R U . . .
C9B C 0.3032(19) 0.0821(13) 0.3472(19) 0.029(5) Uiso 0.38(4) 1 d . . P C 2
H9BA H 0.3367 0.0593 0.3048 0.034 Uiso 0.38(4) 1 calc R U P C 2
H9BB H 0.2635 0.0564 0.3793 0.034 Uiso 0.38(4) 1 calc R U P C 2
C18 C 0.4049(9) 0.4378(6) 0.4755(8) 0.102(4) Uani 1 1 d . . . . .
H18C H 0.4594 0.4550 0.4588 0.122 Uiso 0.5 1 calc R U P D 2
H18D H 0.4145 0.3989 0.5066 0.122 Uiso 0.5 1 calc R U P D 2
H18A H 0.4568 0.4274 0.5060 0.122 Uiso 0.5 1 calc R U P E 1
H18B H 0.3708 0.3999 0.4751 0.122 Uiso 0.5 1 calc R U P E 1
O1S O 0.1009(9) 0.4194(7) 1.0522(10) 0.036(4) Uani 0.3333 1 d . . P . .
H1SA H 0.1498 0.4129 1.0309 0.054 Uiso 0.3333 1 d R U P . .
H1SB H 0.1103 0.4391 1.0992 0.054 Uiso 0.3333 1 d R U P . .
C19B C 0.3555(19) 0.4264(13) 0.4010(16) 0.102(4) Uani 0.5 1 d . . P F 2
H19A H 0.3090 0.3994 0.4158 0.152 Uiso 0.5 1 calc R U P F 2
H19B H 0.3899 0.4065 0.3575 0.152 Uiso 0.5 1 calc R U P F 2
H19C H 0.3341 0.4654 0.3790 0.152 Uiso 0.5 1 calc R U P F 2
C17 C 0.3584(9) 0.4838(6) 0.5329(9) 0.114(5) Uani 1 1 d . . . . .
H17A H 0.3997 0.5082 0.5652 0.137 Uiso 1 1 calc R U . . .
H17B H 0.3268 0.5127 0.4965 0.137 Uiso 1 1 calc R U . . .
C11 C 0.1912(7) 0.4608(6) 0.7056(8) 0.090(4) Uani 1 1 d . . . . .
H11C H 0.1693 0.4287 0.6670 0.108 Uiso 0.539(17) 1 calc R U P G 2
H11D H 0.2272 0.4392 0.7470 0.108 Uiso 0.539(17) 1 calc R U P G 2
H11A H 0.2223 0.4287 0.7369 0.108 Uiso 0.461(17) 1 calc R U P G 1
H11B H 0.1483 0.4408 0.6699 0.108 Uiso 0.461(17) 1 calc R U P G 1
C12B C 0.1231(17) 0.4816(11) 0.7521(17) 0.077(5) Uani 0.539(17) 1 d . . P G 2
H12A H 0.0754 0.4666 0.7181 0.092 Uiso 0.539(17) 1 calc R U P G 2
H12B H 0.1245 0.5266 0.7424 0.092 Uiso 0.539(17) 1 calc R U P G 2
C14B C 0.040(2) 0.5214(13) 0.8836(18) 0.096(10) Uani 0.539(17) 1 d . . P G 2
H14A H 0.0746 0.5477 0.9197 0.144 Uiso 0.539(17) 1 calc R U P G 2
H14B H -0.0010 0.4999 0.9189 0.144 Uiso 0.539(17) 1 calc R U P G 2
H14C H 0.0112 0.5468 0.8414 0.144 Uiso 0.539(17) 1 calc R U P G 2
C13B C 0.092(3) 0.4769(16) 0.841(2) 0.137(10) Uani 0.539(17) 1 d . . P G 2
H13A H 0.0610 0.4375 0.8438 0.165 Uiso 0.539(17) 1 calc R U P G 2
H13B H 0.1414 0.4719 0.8771 0.165 Uiso 0.539(17) 1 calc R U P G 2
C13A C 0.142(3) 0.4965(19) 0.838(3) 0.137(10) Uani 0.461(17) 1 d . . P G 1
H13C H 0.1928 0.5107 0.8664 0.165 Uiso 0.461(17) 1 calc R U P G 1
H13D H 0.1496 0.4519 0.8277 0.165 Uiso 0.461(17) 1 calc R U P G 1
C12A C 0.145(2) 0.5156(13) 0.7781(19) 0.077(5) Uani 0.461(17) 1 d . . P G 1
H12C H 0.1790 0.5535 0.7800 0.092 Uiso 0.461(17) 1 calc R U P G 1
H12D H 0.0886 0.5267 0.7581 0.092 Uiso 0.461(17) 1 calc R U P G 1
C14A C 0.074(3) 0.499(2) 0.908(3) 0.137(10) Uani 0.461(17) 1 d . . P G 1
H14D H 0.0700 0.5416 0.9292 0.206 Uiso 0.461(17) 1 calc R U P G 1
H14E H 0.0897 0.4718 0.9546 0.206 Uiso 0.461(17) 1 calc R U P G 1
H14F H 0.0207 0.4866 0.8842 0.206 Uiso 0.461(17) 1 calc R U P G 1
C19A C 0.4253(19) 0.4470(13) 0.4001(16) 0.102(4) Uani 0.5 1 d . . P F 1
H19D H 0.4569 0.4116 0.3791 0.152 Uiso 0.5 1 calc R U P F 1
H19E H 0.4598 0.4841 0.3967 0.152 Uiso 0.5 1 calc R U P F 1
H19F H 0.3754 0.4525 0.3654 0.152 Uiso 0.5 1 calc R U P F 1
V1A V 0.4735(7) 0.2229(5) 0.5254(6) 0.039(3) Uani 0.372(16) 1 d . . P A 2
C9A C 0.3296(12) 0.0645(9) 0.3745(13) 0.044(4) Uani 0.62(4) 1 d . . P C 1
H9AA H 0.3726 0.0418 0.3422 0.053 Uiso 0.62(4) 1 calc R U P C 1
H9AB H 0.2994 0.0396 0.4173 0.053 Uiso 0.62(4) 1 calc R U P C 1
C10A C 0.2833(10) 0.1125(12) 0.3298(10) 0.044(4) Uani 0.62(4) 1 d . . P C 1
H10C H 0.2237 0.1171 0.3440 0.053 Uiso 0.62(4) 1 calc R U P C 1
H10D H 0.2967 0.1193 0.2691 0.053 Uiso 0.62(4) 1 calc R U P C 1
O6B O 0.4391(19) 0.3619(19) 0.708(2) 0.026(8) Uani 0.35(7) 1 d . . P B 1


_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 O12 2.359(4) . ?
Dy1 O12 2.359(4) 4_556 ?
Dy1 O13 2.367(5) . ?
Dy1 O13 2.367(5) 4_556 ?
Dy1 O14 2.367(5) . ?
Dy1 O14 2.367(5) 4_556 ?
Dy1 O11 2.365(5) 4_556 ?
Dy1 O11 2.365(5) . ?
V1B O5 1.964(5) . ?
V1B O3 1.966(5) . ?
V1B O9 1.951(6) . ?
V1B O7 1.953(6) . ?
V1B O1 2.360(11) . ?
V1B O2 1.595(13) . ?
O5 C3 1.295(9) . ?
O5 V1A 2.078(9) . ?
O12 H12E 0.8501 . ?
O12 H12F 0.8500 . ?
O3 C1 1.301(8) . ?
O3 V1A 2.038(7) . ?
O13 H13E 0.8500 . ?
O13 H13F 0.8498 . ?
O14 H14G 0.8500 . ?
O14 H14H 0.8498 . ?
O9 C8 1.292(9) . ?
O9 V1A 1.983(9) . ?
O7 C6 1.296(9) . ?
O7 V1A 1.924(7) . ?
O11 H11E 0.8502 . ?
O11 H11F 0.8499 . ?
O4 C1 1.230(9) . ?
O8 C6 1.234(9) . ?
O1 H1A 0.8552 . ?
O1 H1B 0.8588 . ?
O1 V1A 1.519(18) . ?
O10 C8 1.233(9) . ?
C1 C2 1.488(10) . ?
N1 C16 1.520(10) . ?
N1 C16 1.520(10) 2_565 ?
N1 C11 1.503(11) . ?
N1 C11 1.503(11) 2_565 ?
C6 C7 1.493(10) . ?
O6A C3 1.252(16) . ?
O2 H2A 0.8908 . ?
O2 H2B 0.8984 . ?
O2 V1A 2.44(2) . ?
C7 C8 1.482(10) . ?
C7 C10B 1.56(2) . ?
C7 C9B 1.52(3) . ?
C7 C9A 1.564(17) . ?
C7 C10A 1.510(17) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C2 1.522(10) . ?
C5 C4 1.470(12) . ?
C3 C2 1.483(10) . ?
C3 O6B 1.32(3) . ?
C2 C4 1.527(12) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.479(14) . ?
C10B H10A 0.9700 . ?
C10B H10B 0.9700 . ?
C10B C9B 1.40(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C9B H9BA 0.9700 . ?
C9B H9BB 0.9700 . ?
C18 H18C 0.9700 . ?
C18 H18D 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19B 1.41(3) . ?
C18 C17 1.510(15) . ?
C18 C19A 1.22(3) . ?
O1S H1SA 0.8500 . ?
O1S H1SB 0.8501 . ?
C19B H19A 0.9600 . ?
C19B H19B 0.9600 . ?
C19B H19C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12B 1.37(3) . ?
C11 C12A 1.77(3) . ?
C12B H12A 0.9700 . ?
C12B H12B 0.9700 . ?
C12B C13B 1.46(4) . ?
C14B H14A 0.9600 . ?
C14B H14B 0.9600 . ?
C14B H14C 0.9600 . ?
C14B C13B 1.41(4) . ?
C13B H13A 0.9700 . ?
C13B H13B 0.9700 . ?
C13A H13C 0.9700 . ?
C13A H13D 0.9700 . ?
C13A C12A 1.01(5) . ?
C13A C14A 1.52(5) . ?
C12A H12C 0.9700 . ?
C12A H12D 0.9700 . ?
C14A H14D 0.9600 . ?
C14A H14E 0.9600 . ?
C14A H14F 0.9600 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C10A 1.43(2) . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 Dy1 O12 137.8(2) . 4_556 ?
O12 Dy1 O13 76.68(17) . 4_556 ?
O12 Dy1 O13 72.05(16) 4_556 4_556 ?
O12 Dy1 O13 76.68(17) 4_556 . ?
O12 Dy1 O13 72.05(16) . . ?
O12 Dy1 O14 78.76(16) 4_556 . ?
O12 Dy1 O14 78.76(16) . 4_556 ?
O12 Dy1 O14 115.45(17) 4_556 4_556 ?
O12 Dy1 O14 115.45(17) . . ?
O12 Dy1 O11 145.07(16) 4_556 4_556 ?
O12 Dy1 O11 145.07(16) . . ?
O12 Dy1 O11 74.16(16) . 4_556 ?
O12 Dy1 O11 74.17(16) 4_556 . ?
O13 Dy1 O13 83.2(2) . 4_556 ?
O13 Dy1 O14 70.85(16) . . ?
O13 Dy1 O14 144.65(16) 4_556 . ?
O13 Dy1 O14 144.65(16) . 4_556 ?
O13 Dy1 O14 70.85(16) 4_556 4_556 ?
O14 Dy1 O14 141.9(2) . 4_556 ?
O11 Dy1 O13 141.28(15) . . ?
O11 Dy1 O13 110.82(16) 4_556 . ?
O11 Dy1 O13 110.83(16) . 4_556 ?
O11 Dy1 O13 141.28(15) 4_556 4_556 ?
O11 Dy1 O14 78.88(17) . . ?
O11 Dy1 O14 72.41(16) . 4_556 ?
O11 Dy1 O14 72.41(16) 4_556 . ?
O11 Dy1 O14 78.88(17) 4_556 4_556 ?
O11 Dy1 O11 81.2(2) . 4_556 ?
O5 V1B O3 87.9(2) . . ?
O5 V1B O1 79.7(3) . . ?
O3 V1B O1 80.8(3) . . ?
O9 V1B O5 89.7(2) . . ?
O9 V1B O3 162.2(5) . . ?
O9 V1B O7 88.7(3) . . ?
O9 V1B O1 81.5(4) . . ?
O7 V1B O5 160.9(5) . . ?
O7 V1B O3 87.9(2) . . ?
O7 V1B O1 81.2(3) . . ?
O2 V1B O5 101.6(4) . . ?
O2 V1B O3 101.4(4) . . ?
O2 V1B O9 96.4(4) . . ?
O2 V1B O7 97.5(4) . . ?
O2 V1B O1 177.5(3) . . ?
C3 O5 V1B 132.6(5) . . ?
C3 O5 V1A 119.3(6) . . ?
Dy1 O12 H12E 127.9 . . ?
Dy1 O12 H12F 127.6 . . ?
H12E O12 H12F 104.5 . . ?
C1 O3 V1B 132.4(5) . . ?
C1 O3 V1A 121.2(5) . . ?
Dy1 O13 H13E 109.2 . . ?
Dy1 O13 H13F 109.4 . . ?
H13E O13 H13F 104.5 . . ?
Dy1 O14 H14G 120.4 . . ?
Dy1 O14 H14H 135.1 . . ?
H14G O14 H14H 104.5 . . ?
C8 O9 V1B 124.2(5) . . ?
C8 O9 V1A 132.6(5) . . ?
C6 O7 V1B 122.5(5) . . ?
C6 O7 V1A 134.4(5) . . ?
Dy1 O11 H11E 126.5 . . ?
Dy1 O11 H11F 129.0 . . ?
H11E O11 H11F 104.5 . . ?
V1B O1 H1A 109.9 . . ?
V1B O1 H1B 109.7 . . ?
H1A O1 H1B 104.0 . . ?
O3 C1 C2 119.9(6) . . ?
O4 C1 O3 120.9(7) . . ?
O4 C1 C2 119.2(7) . . ?
C16 N1 C16 110.7(10) . 2_565 ?
C11 N1 C16 106.0(6) 2_565 2_565 ?
C11 N1 C16 106.0(6) . . ?
C11 N1 C16 111.0(5) . 2_565 ?
C11 N1 C16 111.0(5) 2_565 . ?
C11 N1 C11 112.1(13) 2_565 . ?
O7 C6 C7 119.8(6) . . ?
O8 C6 O7 121.1(7) . . ?
O8 C6 C7 119.1(7) . . ?
H2A O2 H2B 102.5 . . ?
V1A O2 H2A 129.7 . . ?
V1A O2 H2B 127.8 . . ?
C6 C7 C10B 110.8(10) . . ?
C6 C7 C9B 116.0(10) . . ?
C6 C7 C9A 110.4(8) . . ?
C6 C7 C10A 116.6(8) . . ?
C8 C7 C6 124.3(7) . . ?
C8 C7 C10B 111.3(11) . . ?
C8 C7 C9B 117.8(10) . . ?
C8 C7 C9A 111.0(9) . . ?
C8 C7 C10A 117.1(9) . . ?
C9B C7 C10B 54.3(10) . . ?
C10A C7 C9A 55.5(7) . . ?
H5A C5 H5B 114.7 . . ?
C2 C5 H5A 117.6 . . ?
C2 C5 H5B 117.6 . . ?
C4 C5 H5A 117.6 . . ?
C4 C5 H5B 117.6 . . ?
C4 C5 C2 61.4(6) . . ?
O9 C8 C7 120.2(7) . . ?
O10 C8 O9 119.9(7) . . ?
O10 C8 C7 119.7(7) . . ?
O5 C3 C2 119.8(6) . . ?
O5 C3 O6B 110.7(14) . . ?
O6A C3 O5 123.5(10) . . ?
O6A C3 C2 115.7(12) . . ?
O6B C3 C2 122.8(10) . . ?
C1 C2 C5 114.8(6) . . ?
C1 C2 C4 113.3(7) . . ?
C5 C2 C4 57.6(5) . . ?
C3 C2 C1 124.0(6) . . ?
C3 C2 C5 115.2(6) . . ?
C3 C2 C4 113.8(7) . . ?
N1 C16 H16A 108.6 . . ?
N1 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C17 C16 N1 114.5(8) . . ?
C17 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
C7 C10B H10A 117.6 . . ?
C7 C10B H10B 117.6 . . ?
H10A C10B H10B 114.7 . . ?
C9B C10B C7 61.5(13) . . ?
C9B C10B H10A 117.6 . . ?
C9B C10B H10B 117.6 . . ?
C5 C4 C2 61.0(6) . . ?
C5 C4 H4A 117.7 . . ?
C5 C4 H4B 117.7 . . ?
C2 C4 H4A 117.7 . . ?
C2 C4 H4B 117.7 . . ?
H4A C4 H4B 114.8 . . ?
C7 C9B H9BA 117.3 . . ?
C7 C9B H9BB 117.3 . . ?
C10B C9B C7 64.2(13) . . ?
C10B C9B H9BA 117.3 . . ?
C10B C9B H9BB 117.3 . . ?
H9BA C9B H9BB 114.4 . . ?
H18C C18 H18D 108.3 . . ?
H18A C18 H18B 106.2 . . ?
C19B C18 H18C 109.9 . . ?
C19B C18 H18D 109.9 . . ?
C19B C18 C17 108.8(16) . . ?
C17 C18 H18C 109.9 . . ?
C17 C18 H18D 109.9 . . ?
C17 C18 H18A 105.9 . . ?
C17 C18 H18B 105.9 . . ?
C19A C18 H18A 105.9 . . ?
C19A C18 H18B 105.9 . . ?
C19A C18 C17 125.6(19) . . ?
H1SA O1S H1SB 104.5 . . ?
C18 C19B H19A 109.5 . . ?
C18 C19B H19B 109.5 . . ?
C18 C19B H19C 109.5 . . ?
H19A C19B H19B 109.5 . . ?
H19A C19B H19C 109.5 . . ?
H19B C19B H19C 109.5 . . ?
C16 C17 C18 114.0(11) . . ?
C16 C17 H17A 108.7 . . ?
C16 C17 H17B 108.7 . . ?
C18 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
N1 C11 H11C 105.6 . . ?
N1 C11 H11D 105.6 . . ?
N1 C11 H11A 111.0 . . ?
N1 C11 H11B 111.0 . . ?
N1 C11 C12A 104.0(12) . . ?
H11C C11 H11D 106.1 . . ?
H11A C11 H11B 109.0 . . ?
C12B C11 N1 126.8(13) . . ?
C12B C11 H11C 105.6 . . ?
C12B C11 H11D 105.6 . . ?
C12A C11 H11A 111.0 . . ?
C12A C11 H11B 111.0 . . ?
C11 C12B H12A 102.7 . . ?
C11 C12B H12B 102.7 . . ?
C11 C12B C13B 138(3) . . ?
H12A C12B H12B 105.0 . . ?
C13B C12B H12A 102.7 . . ?
C13B C12B H12B 102.7 . . ?
H14A C14B H14B 109.5 . . ?
H14A C14B H14C 109.5 . . ?
H14B C14B H14C 109.5 . . ?
C13B C14B H14A 109.5 . . ?
C13B C14B H14B 109.5 . . ?
C13B C14B H14C 109.5 . . ?
C12B C13B H13A 105.8 . . ?
C12B C13B H13B 105.8 . . ?
C14B C13B C12B 126(3) . . ?
C14B C13B H13A 105.8 . . ?
C14B C13B H13B 105.8 . . ?
H13A C13B H13B 106.2 . . ?
H13C C13A H13D 105.5 . . ?
C12A C13A H13C 104.2 . . ?
C12A C13A H13D 104.2 . . ?
C12A C13A C14A 132(5) . . ?
C14A C13A H13C 104.2 . . ?
C14A C13A H13D 104.2 . . ?
C11 C12A H12C 109.8 . . ?
C11 C12A H12D 109.8 . . ?
C13A C12A C11 109(3) . . ?
C13A C12A H12C 109.8 . . ?
C13A C12A H12D 109.8 . . ?
H12C C12A H12D 108.2 . . ?
C13A C14A H14D 109.5 . . ?
C13A C14A H14E 109.5 . . ?
C13A C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C18 C19A H19D 109.5 . . ?
C18 C19A H19E 109.5 . . ?
C18 C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
O5 V1A O2 75.1(5) . . ?
O3 V1A O5 83.0(3) . . ?
O3 V1A O2 75.7(5) . . ?
O9 V1A O5 85.6(4) . . ?
O9 V1A O3 148.5(10) . . ?
O9 V1A O2 72.9(5) . . ?
O7 V1A O5 149.7(10) . . ?
O7 V1A O3 86.6(3) . . ?
O7 V1A O9 88.6(4) . . ?
O7 V1A O2 74.7(5) . . ?
O1 V1A O5 100.5(5) . . ?
O1 V1A O3 103.9(6) . . ?
O1 V1A O9 107.1(6) . . ?
O1 V1A O7 109.7(7) . . ?
O1 V1A O2 175.6(4) . . ?
C7 C9A H9AA 117.7 . . ?
C7 C9A H9AB 117.7 . . ?
H9AA C9A H9AB 114.9 . . ?
C10A C9A C7 60.3(8) . . ?
C10A C9A H9AA 117.7 . . ?
C10A C9A H9AB 117.7 . . ?
C7 C10A H10C 117.3 . . ?
C7 C10A H10D 117.3 . . ?
C9A C10A C7 64.2(9) . . ?
C9A C10A H10C 117.3 . . ?
C9A C10A H10D 117.3 . . ?
H10C C10A H10D 114.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O12 H12E O4 0.85 1.83 2.680(7) 179.9 6_556
O12 H12F O5 0.85 2.03 2.823(7) 155.7 .
O13 H13E O6A 0.85 2.03 2.713(18) 137.2 .
O13 H13E O6B 0.85 1.88 2.65(2) 149.8 .
O13 H13F O9 0.85 2.10 2.717(7) 128.7 4_556
O14 H14G O7 0.85 1.86 2.712(7) 179.9 7_566
O14 H14H O10 0.85 1.99 2.782(8) 154.8 4_556
O11 H11E O8 0.85 1.89 2.738(7) 179.9 6_556
O11 H11F O3 0.85 2.02 2.768(6) 147.1 7_566
O1 H1A O1S 0.86 1.80 2.592(16) 154.0 7_665
O1S H1SA O10 0.85 1.87 2.685(15) 161.1 4_556
C14A H14E O1S 0.96 1.88 2.83(4) 170.4 .

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
V1B O5 C3 C2 9.7(14) . . . . ?
V1B O5 C3 O6B 162(2) . . . . ?
V1B O3 C1 O4 176.6(6) . . . . ?
V1B O3 C1 C2 -2.9(12) . . . . ?
V1B O9 C8 O10 -158.2(8) . . . . ?
V1B O9 C8 C7 27.0(12) . . . . ?
V1B O7 C6 O8 148.2(7) . . . . ?
V1B O7 C6 C7 -34.0(10) . . . . ?
O5 C3 C2 C1 9.6(14) . . . . ?
O5 C3 C2 C5 160.8(8) . . . . ?
O5 C3 C2 C4 -135.3(9) . . . . ?
O3 C1 C2 C5 -164.1(7) . . . . ?
O3 C1 C2 C3 -12.8(13) . . . . ?
O3 C1 C2 C4 132.2(8) . . . . ?
O7 C6 C7 C8 2.3(13) . . . . ?
O7 C6 C7 C10B 139.2(15) . . . . ?
O7 C6 C7 C9B -161.5(17) . . . . ?
O7 C6 C7 C9A -133.5(12) . . . . ?
O7 C6 C7 C10A 165.7(13) . . . . ?
O4 C1 C2 C5 16.4(12) . . . . ?
O4 C1 C2 C3 167.6(8) . . . . ?
O4 C1 C2 C4 -47.3(11) . . . . ?
O8 C6 C7 C8 -179.8(9) . . . . ?
O8 C6 C7 C10B -42.9(16) . . . . ?
O8 C6 C7 C9B 16.4(19) . . . . ?
O8 C6 C7 C9A 44.4(14) . . . . ?
O8 C6 C7 C10A -16.4(16) . . . . ?
C1 C2 C4 C5 105.6(8) . . . . ?
N1 C16 C17 C18 -178.0(11) . . . . ?
N1 C11 C12B C13B -128(3) . . . . ?
N1 C11 C12A C13A -139(4) . . . . ?
C6 C7 C8 O9 1.6(14) . . . . ?
C6 C7 C8 O10 -173.1(9) . . . . ?
C6 C7 C10B C9B 107.7(13) . . . . ?
C6 C7 C9B C10B -97.8(15) . . . . ?
C6 C7 C9A C10A -108.9(10) . . . . ?
C6 C7 C10A C9A 97.4(11) . . . . ?
O6A C3 C2 C1 179(3) . . . . ?
O6A C3 C2 C5 -30(3) . . . . ?
O6A C3 C2 C4 34(3) . . . . ?
C8 C7 C10B C9B -109.6(13) . . . . ?
C8 C7 C9B C10B 97.3(15) . . . . ?
C8 C7 C9A C10A 109.1(11) . . . . ?
C8 C7 C10A C9A -97.9(12) . . . . ?
C3 C2 C4 C5 -105.7(8) . . . . ?
C16 N1 C16 C17 56.7(9) 2_565 . . . ?
C16 N1 C11 C12B -165.3(18) . . . . ?
C16 N1 C11 C12B -45(2) 2_565 . . . ?
C16 N1 C11 C12A -66.4(15) 2_565 . . . ?
C16 N1 C11 C12A 173.3(13) . . . . ?
C10B C7 C8 O9 -135.1(15) . . . . ?
C10B C7 C8 O10 50.2(17) . . . . ?
C4 C5 C2 C1 -102.9(8) . . . . ?
C4 C5 C2 C3 103.3(9) . . . . ?
C9B C7 C8 O9 165.1(17) . . . . ?
C9B C7 C8 O10 -10(2) . . . . ?
C19B C18 C17 C16 88(2) . . . . ?
C11 N1 C16 C17 177.2(10) . . . . ?
C11 N1 C16 C17 -60.8(13) 2_565 . . . ?
C11 N1 C11 C12B 73.3(19) 2_565 . . . ?
C11 N1 C11 C12A 52.0(12) 2_565 . . . ?
C11 C12B C13B C14B 152(4) . . . . ?
C14A C13A C12A C11 -141(5) . . . . ?
C19A C18 C17 C16 146(2) . . . . ?
V1A O5 C3 O6A -133(3) . . . . ?
V1A O5 C3 C2 34.7(12) . . . . ?
V1A O3 C1 O4 149.4(8) . . . . ?
V1A O3 C1 C2 -30.1(11) . . . . ?
V1A O9 C8 O10 171.7(9) . . . . ?
V1A O9 C8 C7 -3.0(15) . . . . ?
V1A O7 C6 O8 176.9(9) . . . . ?
V1A O7 C6 C7 -5.2(14) . . . . ?
C9A C7 C8 O9 137.2(12) . . . . ?
C9A C7 C8 O10 -37.5(15) . . . . ?
C10A C7 C8 O9 -161.8(13) . . . . ?
C10A C7 C8 O10 23.5(17) . . . . ?
O6B C3 C2 C1 -139(3) . . . . ?
O6B C3 C2 C5 12(3) . . . . ?
O6B C3 C2 C4 76(3) . . . . ?

_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_001
_database_code_depnum_ccdc_archive 'CCDC 2472484'
loop_
_audit_author_name
_audit_author_address
'Maxim Shmelev'
;Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2025-07-14 deposited with the CCDC.	2025-11-06 downloaded from the CCDC.
;
_audit_creation_date             2024-08-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_PLAT972_001                 
;
PROBLEM: Check Calcd Resid. Dens.  2.00Ang From O4A            -2.77 eA-3  
RESPONSE: This alert is related to crystal defects.
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'H16 O8 Tb, 2(C10 H10 O10 V), C16 H36 N, 0.667(H2 O)'
_chemical_formula_sum            'C36 H73.33 N O28.67 Tb V2'
_chemical_formula_weight         1239.76
_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'
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'
V V 0.3005 0.5294 '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      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   15.7396(9)
_cell_length_b                   21.3320(10)
_cell_length_c                   15.4082(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5173.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.81
_cell_measurement_theta_min      2.64
_shelx_estimated_absorpt_T_max   0.900
_shelx_estimated_absorpt_T_min   0.775
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  0.2681
_exptl_absorpt_correction_T_min  0.1915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0703 after correction.
The Ratio of minimum to maximum transmission is 0.7143.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2547
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37267
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.630
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3881
_reflns_number_total             4419
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_refine_diff_density_max         1.348
_refine_diff_density_min         -2.350
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4419
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0506
_refine_ls_restrained_S_all      1.191
_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)+34.7288P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1018
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Tb1-H11E \\sim Tb1-H11F
 with sigma of 0.02
 C14B-C13B \\sim C14A-C13A
 with sigma of 0.02
 Tb1-H12E \\sim Tb1-H12F
 with sigma of 0.02
 Tb1-H13E \\sim Tb1-H13F
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13A) = Uanis(C14A)
Uanis(C13B) = Uanis(C14B)
Uanis(C9B) = Uanis(C10B)
Uanis(C10A) = Uanis(C9A)
Uanis(O4A) = Uanis(O4B)
Uanis(C17A) = Uanis(C17B)
Uanis(C17B) = Uanis(C18B)
Uanis(C17A) = Uanis(C18A)
Uanis(O8A) = Uanis(O8B)
Uanis(O4B) = Uanis(O4A)
4. Others
 Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=1-FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(H1A)=Sof(H1B)=Sof(O4A)=Sof(V1B)=1-FVAR(2)
 Sof(H2A)=Sof(H2B)=Sof(V1A)=Sof(O4B)=FVAR(2)
 Sof(O8A)=1-FVAR(3)
 Sof(O8B)=FVAR(3)
 Fixed Sof: C11A(0.5) H11A(0.5) H11B(0.5) C17B(0.5) H17A(0.5) H17B(0.5)
 C16B(0.5) H16A(0.5) H16B(0.5) C18B(0.5) H18A(0.5) H18B(0.5) H18C(0.5)
 C14B(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C12B(0.5) H12A(0.5) H12B(0.5)
 C13B(0.5) H13A(0.5) H13B(0.5) O1S(0.333333) H1SA(0.333333) H1SB(0.333333)
 C11B(0.5) H11C(0.5) H11D(0.5) H15A(0.5) H15B(0.5) H15C(0.5) H15D(0.5)
 C16A(0.5) H16C(0.5) H16D(0.5) C12A(0.5) H12C(0.5) H12D(0.5) C17A(0.5)
 H17C(0.5) H17D(0.5) C13A(0.5) H13C(0.5) H13D(0.5) C18A(0.5) H18D(0.5)
 H18E(0.5) H18F(0.5) C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5)
5.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O1S(H1SA,H1SB)
5.b Free rotating group:
 O11(H11E,H11F), O12(H12E,H12F), O13(H13E,H13F)
5.c Rotating group:
 O14(H14G,H14H)
5.d Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C9A(H9AA,H9AB), C11A(H11A,H11B), C10A(H10A,H10B),
 C17B(H17A,H17B), C16B(H16A,H16B), C12B(H12A,H12B), C13B(H13A,H13B), C10B(H10C,
 H10D), C9B(H9BA,H9BB), C11B(H11C,H11D), C15(H15A,H15B), C15(H15C,H15D),
 C16A(H16C,H16D), C12A(H12C,H12D), C17A(H17C,H17D), C13A(H13C,H13D)
5.e Idealised Me refined as rotating group:
 C18B(H18A,H18B,H18C), C14B(H14A,H14B,H14C), C18A(H18D,H18E,H18F), C14A(H14D,
 H14E,H14F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.19643(2) 0.7500 0.2500 0.02011(12) Uani 1 2 d DS T P . .
O11 O 0.2501(2) 0.8026(2) 0.3722(2) 0.0309(9) Uani 1 1 d G . . . .
H11E H 0.2204 0.8170 0.4138 0.046 Uiso 1 1 d DG U . . .
H11F H 0.2989 0.7965 0.3942 0.046 Uiso 1 1 d DG U . . .
O3 O 0.4271(3) 0.7935(2) 0.3938(3) 0.0372(11) Uani 1 1 d . . . . .
O5 O 0.5492(3) 0.7933(2) 0.5202(2) 0.0332(10) Uani 1 1 d . . . . .
O12 O 0.1480(2) 0.8157(2) 0.1369(2) 0.0316(10) Uani 1 1 d G . . . .
H12E H 0.0968 0.8208 0.1211 0.047 Uiso 1 1 d DG U . . .
H12F H 0.1773 0.8301 0.0950 0.047 Uiso 1 1 d DG U . . .
O13 O 0.0831(2) 0.8101(2) 0.3053(2) 0.0287(9) Uani 1 1 d G . . . .
H13E H 0.0426 0.8253 0.2753 0.043 Uiso 1 1 d DG U . . .
H13F H 0.0629 0.8074 0.3564 0.043 Uiso 1 1 d DG U . . .
O14 O 0.3088(2) 0.68405(18) 0.2954(2) 0.0287(9) Uani 1 1 d . . . . .
H14G H 0.3561 0.6976 0.2750 0.043 Uiso 1 1 d R U . . .
H14H H 0.3149 0.6868 0.3507 0.043 Uiso 1 1 d R U . . .
O7 O 0.3577(3) 0.6861(2) 0.4654(3) 0.0397(11) Uani 1 1 d . . . . .
O9 O 0.4820(3) 0.6864(2) 0.5888(3) 0.0420(12) Uani 1 1 d . . . . .
O8 O 0.4524(3) 0.6386(2) 0.7115(3) 0.0480(13) Uani 1 1 d . . . . .
O6 O 0.6632(3) 0.8493(2) 0.4924(3) 0.0465(13) Uani 1 1 d . . . . .
O1 O 0.5300(3) 0.6876(3) 0.4119(3) 0.0541(13) Uani 1 1 d . . . . .
H1A H 0.5453 0.6544 0.4382 0.081 Uiso 0.587(10) 1 d R U P A 2
H1B H 0.5013 0.6745 0.3688 0.081 Uiso 0.587(10) 1 d R U P A 2
O8A O 0.2488(4) 0.6246(4) 0.4887(4) 0.047(2) Uani 0.792(11) 1 d . . P B 2
C3 C 0.5953(4) 0.8264(3) 0.4684(4) 0.0311(14) Uani 1 1 d . . . . .
C7 C 0.3466(4) 0.6343(3) 0.6041(4) 0.0345(15) Uani 1 1 d . . . . .
O4A O 0.4674(6) 0.8330(5) 0.2642(6) 0.041(2) Uani 0.587(10) 1 d . . P A 2
C8 C 0.4314(4) 0.6544(3) 0.6378(4) 0.0336(14) Uani 1 1 d . . . . .
C6 C 0.3144(5) 0.6509(4) 0.5153(4) 0.0466(18) Uani 1 1 d . . . . .
C1 C 0.4798(5) 0.8240(4) 0.3455(4) 0.048(2) Uani 1 1 d . . . . .
C5 C 0.6132(4) 0.8899(3) 0.3296(4) 0.0411(18) Uani 1 1 d . . . . .
H5A H 0.5815 0.9130 0.2861 0.049 Uiso 1 1 calc R U . . .
H5B H 0.6534 0.9148 0.3626 0.049 Uiso 1 1 calc R U . . .
O2 O 0.3798(4) 0.7859(3) 0.5671(4) 0.0833(19) Uani 1 1 d . . . . .
H2A H 0.3824 0.8165 0.6147 0.125 Uiso 0.413(10) 1 d R U P A 1
H2B H 0.3246 0.7654 0.5580 0.125 Uiso 0.413(10) 1 d R U P A 1
C2 C 0.5674(4) 0.8371(3) 0.3768(4) 0.0322(14) Uani 1 1 d . . . . .
C4 C 0.6365(5) 0.8254(4) 0.3096(5) 0.056(2) Uani 1 1 d . . . . .
H4A H 0.6911 0.8104 0.3302 0.067 Uiso 1 1 calc R U . . .
H4B H 0.6193 0.8087 0.2537 0.067 Uiso 1 1 calc R U . . .
C9A C 0.2801(14) 0.6086(14) 0.6721(15) 0.042(4) Uani 0.50(5) 1 d . . P C 1
H9AA H 0.2935 0.6129 0.7333 0.050 Uiso 0.50(5) 1 calc R U P C 1
H9AB H 0.2202 0.6122 0.6580 0.050 Uiso 0.50(5) 1 calc R U P C 1
C11A C 0.1862(15) 0.9509(11) 0.3040(16) 0.047(6) Uani 0.5 1 d . . P D 1
H11A H 0.2188 0.9211 0.2702 0.056 Uiso 0.5 1 calc R U P D 1
H11B H 0.1576 0.9279 0.3497 0.056 Uiso 0.5 1 calc R U P D 1
C10A C 0.3313(14) 0.5655(10) 0.6210(17) 0.042(4) Uani 0.50(5) 1 d . . P C 1
H10A H 0.3026 0.5418 0.5760 0.050 Uiso 0.50(5) 1 calc R U P C 1
H10B H 0.3756 0.5425 0.6510 0.050 Uiso 0.50(5) 1 calc R U P C 1
C17B C 0.394(2) 0.933(2) 0.529(3) 0.087(4) Uani 0.5 1 d . . P E 2
H17A H 0.3397 0.9132 0.5426 0.104 Uiso 0.5 1 calc R U P E 2
H17B H 0.4291 0.9001 0.5034 0.104 Uiso 0.5 1 calc R U P E 2
C16B C 0.3756(13) 0.9843(13) 0.4523(16) 0.073(9) Uani 0.5 1 d . . P E 2
H16A H 0.3608 1.0249 0.4765 0.087 Uiso 0.5 1 calc R U P E 2
H16B H 0.4242 0.9890 0.4142 0.087 Uiso 0.5 1 calc R U P E 2
C18B C 0.4283(15) 0.9475(10) 0.6015(13) 0.087(4) Uani 0.5 1 d . . P E 2
H18A H 0.4618 0.9847 0.5940 0.130 Uiso 0.5 1 calc R U P E 2
H18B H 0.4642 0.9139 0.6209 0.130 Uiso 0.5 1 calc R U P E 2
H18C H 0.3849 0.9551 0.6439 0.130 Uiso 0.5 1 calc R U P E 2
C14B C 0.080(2) 1.0001(17) 0.0921(19) 0.159(13) Uani 0.5 1 d D . P D 2
H14A H 0.0616 0.9587 0.0757 0.239 Uiso 0.5 1 calc R U P D 2
H14B H 0.1027 1.0212 0.0424 0.239 Uiso 0.5 1 calc R U P D 2
H14C H 0.0317 1.0233 0.1137 0.239 Uiso 0.5 1 calc R U P D 2
C12B C 0.1426(16) 1.0157(10) 0.2236(15) 0.081(7) Uani 0.5 1 d . . P D 2
H12A H 0.0850 1.0198 0.2453 0.097 Uiso 0.5 1 calc R U P D 2
H12B H 0.1687 1.0569 0.2233 0.097 Uiso 0.5 1 calc R U P D 2
C13B C 0.142(2) 0.9959(17) 0.157(2) 0.159(13) Uani 0.5 1 d D . P D 2
H13A H 0.1511 0.9513 0.1653 0.191 Uiso 0.5 1 calc R U P D 2
H13B H 0.1935 1.0116 0.1303 0.191 Uiso 0.5 1 calc R U P D 2
V1B V 0.44077(18) 0.74800(17) 0.5047(2) 0.0233(8) Uani 0.587(10) 1 d . . P A 2
V1A V 0.4710(5) 0.7250(3) 0.4766(4) 0.0419(18) Uani 0.413(10) 1 d . . P A 1
O1S O 0.1002(7) 0.5813(6) 0.5525(8) 0.036(3) Uani 0.3333 1 d . . P . .
H1SA H 0.1492 0.5876 0.5311 0.054 Uiso 0.3333 1 d R U P . .
H1SB H 0.1095 0.5616 0.5995 0.054 Uiso 0.3333 1 d R U P . .
O4B O 0.4418(10) 0.8600(8) 0.2908(9) 0.041(2) Uani 0.413(10) 1 d . . P A 1
C10B C 0.3066(16) 0.5776(16) 0.6493(16) 0.054(7) Uani 0.50(5) 1 d . . P C 2
H10C H 0.2680 0.5518 0.6158 0.065 Uiso 0.50(5) 1 calc R U P C 2
H10D H 0.3411 0.5549 0.6910 0.065 Uiso 0.50(5) 1 calc R U P C 2
C9B C 0.2793(13) 0.6392(19) 0.6721(14) 0.054(7) Uani 0.50(5) 1 d . . P C 2
H9BA H 0.2960 0.6551 0.7285 0.065 Uiso 0.50(5) 1 calc R U P C 2
H9BB H 0.2230 0.6519 0.6534 0.065 Uiso 0.50(5) 1 calc R U P C 2
C11B C 0.192(2) 0.9720(10) 0.2801(17) 0.063(9) Uani 0.5 1 d . . P D 2
H11C H 0.2266 0.9456 0.2426 0.075 Uiso 0.5 1 calc R U P D 2
H11D H 0.1524 0.9448 0.3097 0.075 Uiso 0.5 1 calc R U P D 2
C15 C 0.2987(6) 0.9541(3) 0.4040(5) 0.059(2) Uani 1 1 d . . . . .
H15A H 0.2591 0.9226 0.4246 0.071 Uiso 0.5 1 calc R U P E 1
H15B H 0.3402 0.9329 0.3679 0.071 Uiso 0.5 1 calc R U P E 1
H15C H 0.3194 0.9200 0.3681 0.071 Uiso 0.5 1 calc R U P E 2
H15D H 0.2602 0.9365 0.4466 0.071 Uiso 0.5 1 calc R U P E 2
C16A C 0.3434(15) 0.9801(10) 0.4796(16) 0.060(6) Uani 0.5 1 d . . P E 1
H16C H 0.3019 0.9874 0.5251 0.072 Uiso 0.5 1 calc R U P E 1
H16D H 0.3666 1.0206 0.4634 0.072 Uiso 0.5 1 calc R U P E 1
C12A C 0.1209(13) 0.9802(10) 0.2467(14) 0.071(5) Uani 0.5 1 d . . P D 1
H12C H 0.0709 0.9767 0.2832 0.086 Uiso 0.5 1 calc R U P D 1
H12D H 0.1370 1.0240 0.2510 0.086 Uiso 0.5 1 calc R U P D 1
C17A C 0.417(2) 0.940(2) 0.518(3) 0.087(4) Uani 0.5 1 d . . P E 1
H17C H 0.4681 0.9631 0.5317 0.104 Uiso 0.5 1 calc R U P E 1
H17D H 0.4298 0.9021 0.4852 0.104 Uiso 0.5 1 calc R U P E 1
C13A C 0.0841(18) 0.9794(10) 0.1653(16) 0.097(6) Uani 0.5 1 d D . P D 1
H13C H 0.0505 0.9413 0.1663 0.116 Uiso 0.5 1 calc R U P D 1
H13D H 0.1317 0.9702 0.1274 0.116 Uiso 0.5 1 calc R U P D 1
C18A C 0.3565(14) 0.9279(10) 0.5999(14) 0.087(4) Uani 0.5 1 d . . P E 1
H18D H 0.3206 0.9637 0.6083 0.130 Uiso 0.5 1 calc R U P E 1
H18E H 0.3905 0.9213 0.6508 0.130 Uiso 0.5 1 calc R U P E 1
H18F H 0.3220 0.8915 0.5896 0.130 Uiso 0.5 1 calc R U P E 1
C14A C 0.0341(19) 1.0204(13) 0.1150(18) 0.097(6) Uani 0.5 1 d D . P D 1
H14D H -0.0002 1.0459 0.1525 0.145 Uiso 0.5 1 calc R U P D 1
H14E H -0.0019 0.9965 0.0772 0.145 Uiso 0.5 1 calc R U P D 1
H14F H 0.0705 1.0469 0.0809 0.145 Uiso 0.5 1 calc R U P D 1
N1 N 0.2500 1.0000 0.3473(6) 0.054(2) Uani 1 2 d S T P D .
O8B O 0.2235(16) 0.6634(15) 0.5172(17) 0.047(2) Uani 0.208(11) 1 d . . P B 1


_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 O11 2.349(4) . ?
Tb1 O11 2.349(4) 4_565 ?
Tb1 O12 2.363(4) 4_565 ?
Tb1 O12 2.363(4) . ?
Tb1 O13 2.357(4) 4_565 ?
Tb1 O13 2.357(4) . ?
Tb1 O14 2.365(4) 4_565 ?
Tb1 O14 2.365(4) . ?
O11 H11E 0.8505 . ?
O11 H11F 0.8493 . ?
O3 C1 1.291(7) . ?
O3 V1B 1.976(4) . ?
O3 V1A 2.059(6) . ?
O5 C3 1.290(7) . ?
O5 V1B 1.975(4) . ?
O5 V1A 2.021(5) . ?
O12 H12E 0.8490 . ?
O12 H12F 0.8505 . ?
O13 H13E 0.8504 . ?
O13 H13F 0.8509 . ?
O14 H14G 0.8590 . ?
O14 H14H 0.8597 . ?
O7 C6 1.273(7) . ?
O7 V1B 1.954(5) . ?
O7 V1A 1.974(6) . ?
O9 C8 1.291(7) . ?
O9 V1B 1.956(5) . ?
O9 V1A 1.923(5) . ?
O8 C8 1.231(7) . ?
O6 C3 1.231(7) . ?
O1 H1A 0.8497 . ?
O1 H1B 0.8500 . ?
O1 V1B 2.382(7) . ?
O1 V1A 1.579(12) . ?
O8A C6 1.246(8) . ?
C3 C2 1.495(8) . ?
C7 C8 1.494(8) . ?
C7 C6 1.502(9) . ?
C7 C9A 1.58(3) . ?
C7 C10A 1.51(2) . ?
C7 C10B 1.53(2) . ?
C7 C9B 1.49(3) . ?
O4A C1 1.282(11) . ?
C6 O8B 1.46(3) . ?
C1 C2 1.487(8) . ?
C1 O4B 1.288(16) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C2 1.521(8) . ?
C5 C4 1.457(10) . ?
O2 H2A 0.9838 . ?
O2 H2B 0.9830 . ?
O2 V1B 1.581(9) . ?
O2 V1A 2.385(13) . ?
C2 C4 1.523(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C10A 1.45(3) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C11A C12A 1.49(3) . ?
C11A N1 1.60(2) . ?
C10A H10A 0.9700 . ?
C10A H10B 0.9700 . ?
C17B H17A 0.9700 . ?
C17B H17B 0.9700 . ?
C17B C16B 1.64(4) . ?
C17B C18B 1.28(5) . ?
C16B H16A 0.9700 . ?
C16B H16B 0.9700 . ?
C16B C15 1.56(2) . ?
C18B H18A 0.9600 . ?
C18B H18B 0.9600 . ?
C18B H18C 0.9600 . ?
C14B H14A 0.9600 . ?
C14B H14B 0.9600 . ?
C14B H14C 0.9600 . ?
C14B C13B 1.41(2) . ?
C12B H12A 0.9700 . ?
C12B H12B 0.9700 . ?
C12B C13B 1.11(4) . ?
C12B C11B 1.50(4) . ?
C13B H13A 0.9700 . ?
C13B H13B 0.9700 . ?
O1S H1SA 0.8500 . ?
O1S H1SB 0.8499 . ?
C10B H10C 0.9700 . ?
C10B H10D 0.9700 . ?
C10B C9B 1.43(3) . ?
C9B H9BA 0.9700 . ?
C9B H9BB 0.9700 . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C11B N1 1.50(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C15 H15D 0.9700 . ?
C15 C16A 1.47(3) . ?
C15 N1 1.520(9) . ?
C16A H16C 0.9700 . ?
C16A H16D 0.9700 . ?
C16A C17A 1.56(5) . ?
C12A H12C 0.9700 . ?
C12A H12D 0.9700 . ?
C12A C13A 1.38(3) . ?
C17A H17C 0.9700 . ?
C17A H17D 0.9700 . ?
C17A C18A 1.60(4) . ?
C13A H13C 0.9700 . ?
C13A H13D 0.9700 . ?
C13A C14A 1.41(2) . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18A H18F 0.9600 . ?
C14A H14D 0.9600 . ?
C14A H14E 0.9600 . ?
C14A H14F 0.9600 . ?
N1 C11A 1.60(2) 2_575 ?
N1 C11B 1.50(3) 2_575 ?
N1 C15 1.520(9) 2_575 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Tb1 O11 137.85(19) . 4_565 ?
O11 Tb1 O12 78.94(14) 4_565 . ?
O11 Tb1 O12 115.08(16) . . ?
O11 Tb1 O12 115.08(16) 4_565 4_565 ?
O11 Tb1 O12 78.94(14) . 4_565 ?
O11 Tb1 O13 145.26(13) . 4_565 ?
O11 Tb1 O13 145.26(13) 4_565 . ?
O11 Tb1 O13 73.91(14) 4_565 4_565 ?
O11 Tb1 O13 73.91(14) . . ?
O11 Tb1 O14 71.61(14) . 4_565 ?
O11 Tb1 O14 77.17(14) . . ?
O11 Tb1 O14 71.61(14) 4_565 . ?
O11 Tb1 O14 77.17(14) 4_565 4_565 ?
O12 Tb1 O12 142.35(19) . 4_565 ?
O12 Tb1 O14 70.74(14) . 4_565 ?
O12 Tb1 O14 70.74(14) 4_565 . ?
O12 Tb1 O14 144.32(13) . . ?
O12 Tb1 O14 144.32(13) 4_565 4_565 ?
O13 Tb1 O12 72.49(13) 4_565 4_565 ?
O13 Tb1 O12 72.49(13) . . ?
O13 Tb1 O12 79.18(15) . 4_565 ?
O13 Tb1 O12 79.17(15) 4_565 . ?
O13 Tb1 O13 81.6(2) 4_565 . ?
O13 Tb1 O14 141.52(13) . . ?
O13 Tb1 O14 110.44(14) . 4_565 ?
O13 Tb1 O14 110.44(14) 4_565 . ?
O13 Tb1 O14 141.52(13) 4_565 4_565 ?
O14 Tb1 O14 83.25(19) 4_565 . ?
Tb1 O11 H11E 125.4 . . ?
Tb1 O11 H11F 124.9 . . ?
H11E O11 H11F 104.5 . . ?
C1 O3 V1B 132.6(4) . . ?
C1 O3 V1A 120.0(5) . . ?
C3 O5 V1B 132.7(4) . . ?
C3 O5 V1A 122.1(4) . . ?
Tb1 O12 H12E 126.4 . . ?
Tb1 O12 H12F 126.8 . . ?
H12E O12 H12F 104.6 . . ?
Tb1 O13 H13E 125.3 . . ?
Tb1 O13 H13F 125.4 . . ?
H13E O13 H13F 104.5 . . ?
Tb1 O14 H14G 109.9 . . ?
Tb1 O14 H14H 109.7 . . ?
H14G O14 H14H 104.1 . . ?
C6 O7 V1B 124.7(4) . . ?
C6 O7 V1A 132.8(4) . . ?
C8 O9 V1B 122.5(4) . . ?
C8 O9 V1A 134.1(4) . . ?
H1A O1 H1B 104.5 . . ?
V1B O1 H1A 109.3 . . ?
V1B O1 H1B 109.5 . . ?
O5 C3 C2 120.2(5) . . ?
O6 C3 O5 121.2(5) . . ?
O6 C3 C2 118.6(5) . . ?
C8 C7 C6 123.3(5) . . ?
C8 C7 C9A 117.5(8) . . ?
C8 C7 C10A 111.3(8) . . ?
C8 C7 C10B 115.9(8) . . ?
C6 C7 C9A 117.5(8) . . ?
C6 C7 C10A 109.4(9) . . ?
C6 C7 C10B 117.5(8) . . ?
C10A C7 C9A 56.1(9) . . ?
C9B C7 C8 111.8(10) . . ?
C9B C7 C6 112.5(9) . . ?
C9B C7 C10B 56.3(10) . . ?
O9 C8 C7 120.0(5) . . ?
O8 C8 O9 121.2(6) . . ?
O8 C8 C7 118.7(5) . . ?
O7 C6 C7 120.6(6) . . ?
O7 C6 O8B 115.5(11) . . ?
O8A C6 O7 120.8(6) . . ?
O8A C6 C7 118.2(6) . . ?
O8B C6 C7 110.9(11) . . ?
O3 C1 C2 120.2(5) . . ?
O4A C1 O3 122.7(7) . . ?
O4A C1 C2 115.5(7) . . ?
O4B C1 O3 112.3(9) . . ?
O4B C1 C2 122.1(8) . . ?
H5A C5 H5B 114.7 . . ?
C2 C5 H5A 117.6 . . ?
C2 C5 H5B 117.6 . . ?
C4 C5 H5A 117.6 . . ?
C4 C5 H5B 117.6 . . ?
C4 C5 C2 61.5(5) . . ?
H2A O2 H2B 116.0 . . ?
V1A O2 H2A 140.7 . . ?
V1A O2 H2B 101.9 . . ?
C3 C2 C5 115.2(5) . . ?
C3 C2 C4 114.0(6) . . ?
C1 C2 C3 123.3(5) . . ?
C1 C2 C5 115.0(5) . . ?
C1 C2 C4 114.2(6) . . ?
C5 C2 C4 57.2(4) . . ?
C5 C4 C2 61.3(5) . . ?
C5 C4 H4A 117.6 . . ?
C5 C4 H4B 117.6 . . ?
C2 C4 H4A 117.6 . . ?
C2 C4 H4B 117.6 . . ?
H4A C4 H4B 114.7 . . ?
C7 C9A H9AA 117.8 . . ?
C7 C9A H9AB 117.8 . . ?
H9AA C9A H9AB 115.0 . . ?
C10A C9A C7 59.5(17) . . ?
C10A C9A H9AA 117.8 . . ?
C10A C9A H9AB 117.8 . . ?
H11A C11A H11B 107.7 . . ?
C12A C11A H11A 108.8 . . ?
C12A C11A H11B 108.8 . . ?
C12A C11A N1 113.9(17) . . ?
N1 C11A H11A 108.8 . . ?
N1 C11A H11B 108.8 . . ?
C7 C10A H10A 117.3 . . ?
C7 C10A H10B 117.3 . . ?
C9A C10A C7 64.4(14) . . ?
C9A C10A H10A 117.3 . . ?
C9A C10A H10B 117.3 . . ?
H10A C10A H10B 114.4 . . ?
H17A C17B H17B 106.6 . . ?
C16B C17B H17A 106.8 . . ?
C16B C17B H17B 106.8 . . ?
C18B C17B H17A 106.8 . . ?
C18B C17B H17B 106.8 . . ?
C18B C17B C16B 122(3) . . ?
C17B C16B H16A 111.5 . . ?
C17B C16B H16B 111.5 . . ?
H16A C16B H16B 109.3 . . ?
C15 C16B C17B 101.6(19) . . ?
C15 C16B H16A 111.5 . . ?
C15 C16B H16B 111.5 . . ?
C17B C18B H18A 109.5 . . ?
C17B C18B H18B 109.5 . . ?
C17B C18B H18C 109.5 . . ?
H18A C18B H18B 109.5 . . ?
H18A C18B H18C 109.5 . . ?
H18B C18B H18C 109.5 . . ?
H14A C14B H14B 109.5 . . ?
H14A C14B H14C 109.5 . . ?
H14B C14B H14C 109.5 . . ?
C13B C14B H14A 109.5 . . ?
C13B C14B H14B 109.5 . . ?
C13B C14B H14C 109.5 . . ?
H12A C12B H12B 108.5 . . ?
C13B C12B H12A 110.2 . . ?
C13B C12B H12B 110.2 . . ?
C13B C12B C11B 108(3) . . ?
C11B C12B H12A 110.2 . . ?
C11B C12B H12B 110.2 . . ?
C14B C13B H13A 104.9 . . ?
C14B C13B H13B 104.9 . . ?
C12B C13B C14B 130(4) . . ?
C12B C13B H13A 104.8 . . ?
C12B C13B H13B 104.9 . . ?
H13A C13B H13B 105.8 . . ?
O3 V1B O1 79.1(2) . . ?
O5 V1B O3 87.63(18) . . ?
O5 V1B O1 80.1(2) . . ?
O7 V1B O3 89.52(19) . . ?
O7 V1B O5 161.1(3) . . ?
O7 V1B O9 88.5(2) . . ?
O7 V1B O1 81.0(3) . . ?
O9 V1B O3 159.8(3) . . ?
O9 V1B O5 87.80(18) . . ?
O9 V1B O1 80.7(2) . . ?
O2 V1B O3 102.1(3) . . ?
O2 V1B O5 101.6(3) . . ?
O2 V1B O7 97.3(3) . . ?
O2 V1B O9 98.1(3) . . ?
O2 V1B O1 177.9(3) . . ?
O3 V1A O2 77.0(4) . . ?
O5 V1A O3 84.2(2) . . ?
O5 V1A O2 77.3(3) . . ?
O7 V1A O3 86.6(3) . . ?
O7 V1A O5 151.8(6) . . ?
O7 V1A O2 74.7(4) . . ?
O9 V1A O3 153.0(6) . . ?
O9 V1A O5 87.4(2) . . ?
O9 V1A O7 88.8(2) . . ?
O9 V1A O2 76.2(4) . . ?
O1 V1A O3 99.5(3) . . ?
O1 V1A O5 102.5(4) . . ?
O1 V1A O7 105.3(4) . . ?
O1 V1A O9 107.4(5) . . ?
O1 V1A O2 176.5(3) . . ?
H1SA O1S H1SB 104.5 . . ?
C7 C10B H10C 117.7 . . ?
C7 C10B H10D 117.7 . . ?
H10C C10B H10D 114.8 . . ?
C9B C10B C7 60.6(15) . . ?
C9B C10B H10C 117.7 . . ?
C9B C10B H10D 117.7 . . ?
C7 C9B H9BA 117.4 . . ?
C7 C9B H9BB 117.4 . . ?
C10B C9B C7 63.2(14) . . ?
C10B C9B H9BA 117.4 . . ?
C10B C9B H9BB 117.4 . . ?
H9BA C9B H9BB 114.5 . . ?
C12B C11B H11C 107.8 . . ?
C12B C11B H11D 107.8 . . ?
C12B C11B N1 118.0(16) . . ?
H11C C11B H11D 107.2 . . ?
N1 C11B H11C 107.8 . . ?
N1 C11B H11D 107.8 . . ?
C16B C15 H15C 108.9 . . ?
C16B C15 H15D 108.9 . . ?
H15A C15 H15B 107.3 . . ?
H15C C15 H15D 107.7 . . ?
C16A C15 H15A 108.0 . . ?
C16A C15 H15B 108.0 . . ?
C16A C15 N1 117.0(11) . . ?
N1 C15 C16B 113.6(10) . . ?
N1 C15 H15A 108.0 . . ?
N1 C15 H15B 108.0 . . ?
N1 C15 H15C 108.9 . . ?
N1 C15 H15D 108.9 . . ?
C15 C16A H16C 108.1 . . ?
C15 C16A H16D 108.1 . . ?
C15 C16A C17A 117(2) . . ?
H16C C16A H16D 107.3 . . ?
C17A C16A H16C 108.1 . . ?
C17A C16A H16D 108.1 . . ?
C11A C12A H12C 100.6 . . ?
C11A C12A H12D 100.6 . . ?
H12C C12A H12D 104.3 . . ?
C13A C12A C11A 145(2) . . ?
C13A C12A H12C 100.6 . . ?
C13A C12A H12D 100.6 . . ?
C16A C17A H17C 114.2 . . ?
C16A C17A H17D 114.2 . . ?
C16A C17A C18A 87(2) . . ?
H17C C17A H17D 111.3 . . ?
C18A C17A H17C 114.2 . . ?
C18A C17A H17D 114.2 . . ?
C12A C13A H13C 103.0 . . ?
C12A C13A H13D 103.0 . . ?
C12A C13A C14A 137(2) . . ?
H13C C13A H13D 105.1 . . ?
C14A C13A H13C 103.0 . . ?
C14A C13A H13D 103.0 . . ?
C17A C18A H18D 109.5 . . ?
C17A C18A H18E 109.5 . . ?
C17A C18A H18F 109.5 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C13A C14A H14D 109.5 . . ?
C13A C14A H14E 109.5 . . ?
C13A C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C11A N1 C11A 130.7(18) . 2_575 ?
C11B N1 C11B 92.8(17) . 2_575 ?
C11B N1 C15 116.4(10) 2_575 2_575 ?
C11B N1 C15 110.4(12) . 2_575 ?
C11B N1 C15 110.4(12) 2_575 . ?
C11B N1 C15 116.5(10) . . ?
C15 N1 C11A 110.2(11) 2_575 . ?
C15 N1 C11A 97.8(9) . . ?
C15 N1 C11A 97.8(9) 2_575 2_575 ?
C15 N1 C11A 110.2(11) . 2_575 ?
C15 N1 C15 109.8(9) 2_575 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C1 C2 C3 -10.7(11) . . . . ?
O3 C1 C2 C5 -161.0(7) . . . . ?
O3 C1 C2 C4 135.5(7) . . . . ?
O5 C3 C2 C1 14.2(10) . . . . ?
O5 C3 C2 C5 164.5(6) . . . . ?
O5 C3 C2 C4 -132.0(6) . . . . ?
O6 C3 C2 C1 -166.5(7) . . . . ?
O6 C3 C2 C5 -16.3(9) . . . . ?
O6 C3 C2 C4 47.3(9) . . . . ?
C3 C2 C4 C5 -105.5(6) . . . . ?
O4A C1 C2 C3 -176.9(8) . . . . ?
O4A C1 C2 C5 32.8(11) . . . . ?
O4A C1 C2 C4 -30.8(11) . . . . ?
C8 C7 C6 O7 -3.3(11) . . . . ?
C8 C7 C6 O8A 169.8(8) . . . . ?
C8 C7 C6 O8B -142.9(15) . . . . ?
C8 C7 C9A C10A -98.2(11) . . . . ?
C8 C7 C10A C9A 109.6(10) . . . . ?
C8 C7 C10B C9B 99.9(13) . . . . ?
C8 C7 C9B C10B -107.4(12) . . . . ?
C6 C7 C8 O9 -1.8(10) . . . . ?
C6 C7 C8 O8 179.9(7) . . . . ?
C6 C7 C9A C10A 95.8(12) . . . . ?
C6 C7 C10A C9A -110.7(11) . . . . ?
C6 C7 C10B C9B -99.8(13) . . . . ?
C6 C7 C9B C10B 109.0(12) . . . . ?
C1 C2 C4 C5 105.2(6) . . . . ?
C4 C5 C2 C3 103.4(7) . . . . ?
C4 C5 C2 C1 -103.8(7) . . . . ?
C9A C7 C8 O9 -166.9(12) . . . . ?
C9A C7 C8 O8 14.7(14) . . . . ?
C9A C7 C6 O7 161.9(13) . . . . ?
C9A C7 C6 O8B 22.2(19) . . . . ?
C11A C12A C13A C14A -162(3) . . . . ?
C10A C7 C8 O9 131.2(13) . . . . ?
C10A C7 C8 O8 -47.1(15) . . . . ?
C10A C7 C6 O7 -137.0(13) . . . . ?
C10A C7 C6 O8B 83.4(18) . . . . ?
C17B C16B C15 N1 162.1(19) . . . . ?
C16B C15 N1 C11B 58.9(16) . . . 2_575 ?
C16B C15 N1 C11B 163.0(16) . . . . ?
C16B C15 N1 C15 -70.7(12) . . . 2_575 ?
C18B C17B C16B C15 -153(3) . . . . ?
C12B C11B N1 C11B -66.2(16) . . . 2_575 ?
C12B C11B N1 C15 179.3(16) . . . . ?
C12B C11B N1 C15 53(2) . . . 2_575 ?
C13B C12B C11B N1 141(2) . . . . ?
V1B O3 C1 O4A 156.6(7) . . . . ?
V1B O3 C1 C2 -8.6(11) . . . . ?
V1B O5 C3 O6 -178.0(5) . . . . ?
V1B O5 C3 C2 1.2(10) . . . . ?
V1B O7 C6 O8A 161.6(7) . . . . ?
V1B O7 C6 C7 -25.5(10) . . . . ?
V1B O9 C8 O8 -147.2(6) . . . . ?
V1B O9 C8 C7 34.5(9) . . . . ?
V1A O3 C1 C2 -32.7(9) . . . . ?
V1A O3 C1 O4B 172.8(8) . . . . ?
V1A O5 C3 O6 -151.7(6) . . . . ?
V1A O5 C3 C2 27.5(9) . . . . ?
V1A O7 C6 C7 3.4(12) . . . . ?
V1A O7 C6 O8B 141.2(15) . . . . ?
V1A O9 C8 O8 -174.3(6) . . . . ?
V1A O9 C8 C7 7.4(11) . . . . ?
O4B C1 C2 C3 141.4(11) . . . . ?
O4B C1 C2 C5 -8.9(13) . . . . ?
O4B C1 C2 C4 -72.5(12) . . . . ?
C10B C7 C8 O9 157.2(18) . . . . ?
C10B C7 C8 O8 -21.1(19) . . . . ?
C10B C7 C6 O7 -162.0(18) . . . . ?
C10B C7 C6 O8A 11(2) . . . . ?
C9B C7 C8 O9 -140.9(17) . . . . ?
C9B C7 C8 O8 40.8(18) . . . . ?
C9B C7 C6 O7 135.6(17) . . . . ?
C9B C7 C6 O8A -51.4(19) . . . . ?
C11B C12B C13B C14B 149(3) . . . . ?
C15 C16A C17A C18A -110(2) . . . . ?
C16A C15 N1 C11A 63.4(15) . . . 2_575 ?
C16A C15 N1 C11A -157.9(14) . . . . ?
C16A C15 N1 C15 -43.1(10) . . . 2_575 ?
C12A C11A N1 C11A -59.4(17) . . . 2_575 ?
C12A C11A N1 C15 175.4(18) . . . . ?
C12A C11A N1 C15 61(2) . . . 2_575 ?
N1 C11A C12A C13A 128(4) . . . . ?
N1 C15 C16A C17A -159.4(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
