# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# 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_Gd2
_database_code_depnum_ccdc_archive 'CCDC 2202463'
loop_
_audit_author_name
_audit_author_address
'Alexandros A. Kitos'
;University of Ottawa
Canada
;
_audit_update_record             
;
2022-08-19 deposited with the CCDC.	2022-11-17 downloaded from the CCDC.
;
#=============================================================
# CHEMICAL DATA

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H78 Gd2 N4 O2, C24 H20 B'
_chemical_formula_sum            'C74 H98 B Gd2 N4 O2'
_chemical_formula_weight         1400.87

#=============================================================
# CRYSTAL DATA

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'
B B 0.0013 0.0007 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, 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                   15.3219(5)
_cell_length_b                   20.3671(6)
_cell_length_c                   25.4887(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.429(2)
_cell_angle_gamma                90
_cell_volume                     7904.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    9789
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      33.83

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_F_000             2876
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.704
_shelx_estimated_absorpt_T_min   0.579
_shelx_estimated_absorpt_T_max   0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5051
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?

#=============================================================
# EXPERIMENTAL DATA

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω and φ scans'
_diffrn_ambient_temperature      203(2)
_diffrn_reflns_number            66087
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.608
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000

#=============================================================
# REFINEMENT DATA 

_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_number_total             7774
_reflns_number_gt                6514
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7774
_refine_ls_number_parameters     385
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0722
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+44.2809P] where P=(Fo²+2Fc²)/3'
_refine_diff_density_max         2.260
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.080

#=============================================================
# GENERAL COMPUTING 

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#=============================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
Gd Gd 0.54669(2) 0.67534(2) 0.77185(2) 0.03530(6) Uani 1 1 d . . . . .
C1 C 0.7479(2) 0.78324(18) 0.79281(16) 0.0405(8) Uani 1 1 d . . . . .
H1 H 0.746264 0.807403 0.824106 0.049 Uiso 1 1 calc R U . . .
C2 C 0.4684(3) 0.5534(2) 0.68419(18) 0.0609(13) Uani 1 1 d . . . . .
H2A H 0.407368 0.568123 0.682950 0.073 Uiso 1 1 calc R U . . .
H2B H 0.479500 0.520344 0.712119 0.073 Uiso 1 1 calc R U . . .
C3 C 0.4856(4) 0.5256(3) 0.6323(2) 0.0905(19) Uani 1 1 d D U . . .
H3A H 0.528770 0.489986 0.637196 0.109 Uiso 1 1 calc R U . . .
H3B H 0.431359 0.508480 0.613188 0.109 Uiso 1 1 calc R U . . .
C4 C 0.5193(4) 0.5796(3) 0.60399(19) 0.0782(16) Uani 1 1 d D . . . .
H4A H 0.471245 0.604069 0.584286 0.094 Uiso 1 1 calc R U . . .
H4B H 0.558945 0.563668 0.579152 0.094 Uiso 1 1 calc R U . . .
C5 C 0.5678(3) 0.6221(2) 0.64535(16) 0.0492(10) Uani 1 1 d . . . . .
H5A H 0.630499 0.611227 0.649766 0.059 Uiso 1 1 calc R U . . .
H5B H 0.561010 0.668574 0.635800 0.059 Uiso 1 1 calc R U . . .
C6 C 0.6149(3) 0.6422(2) 0.86939(17) 0.0521(10) Uani 1 1 d . . . . .
C7 C 0.5303(3) 0.6144(2) 0.86456(17) 0.0502(10) Uani 1 1 d . . . . .
C8 C 0.5278(3) 0.5626(2) 0.82765(17) 0.0477(10) Uani 1 1 d . . . . .
C9 C 0.6111(3) 0.55725(19) 0.81013(16) 0.0469(9) Uani 1 1 d . . . . .
C10 C 0.6652(3) 0.6066(2) 0.83554(17) 0.0485(10) Uani 1 1 d . . . . .
C11 C 0.6483(4) 0.6965(3) 0.9065(2) 0.0786(16) Uani 1 1 d . . . . .
H11A H 0.600272 0.725811 0.912067 0.118 Uiso 1 1 calc R U . . .
H11B H 0.693657 0.720907 0.891242 0.118 Uiso 1 1 calc R U . . .
H11C H 0.672466 0.677812 0.939976 0.118 Uiso 1 1 calc R U . . .
C12 C 0.4606(4) 0.6248(3) 0.9016(2) 0.0803(16) Uani 1 1 d . . . . .
H12A H 0.403296 0.627600 0.881189 0.120 Uiso 1 1 calc R U . . .
H12B H 0.472530 0.665147 0.921226 0.120 Uiso 1 1 calc R U . . .
H12C H 0.461272 0.588134 0.925934 0.120 Uiso 1 1 calc R U . . .
C13 C 0.4523(3) 0.5143(2) 0.8182(2) 0.0718(14) Uani 1 1 d . . . . .
H13A H 0.400873 0.536731 0.801071 0.108 Uiso 1 1 calc R U . . .
H13B H 0.439101 0.496448 0.851648 0.108 Uiso 1 1 calc R U . . .
H13C H 0.468557 0.478994 0.795683 0.108 Uiso 1 1 calc R U . . .
C14 C 0.6431(4) 0.5044(2) 0.7756(2) 0.0693(14) Uani 1 1 d . . . . .
H14A H 0.600119 0.469312 0.771160 0.104 Uiso 1 1 calc R U . . .
H14B H 0.698535 0.487102 0.792064 0.104 Uiso 1 1 calc R U . . .
H14C H 0.651335 0.522738 0.741388 0.104 Uiso 1 1 calc R U . . .
C15 C 0.7625(3) 0.6133(3) 0.8324(2) 0.0754(15) Uani 1 1 d . . . . .
H15A H 0.782239 0.655910 0.845892 0.113 Uiso 1 1 calc R U . . .
H15B H 0.774258 0.609075 0.795971 0.113 Uiso 1 1 calc R U . . .
H15C H 0.793573 0.579066 0.853431 0.113 Uiso 1 1 calc R U . . .
C16 C 0.4697(3) 0.7801(2) 0.7204(2) 0.0530(11) Uani 1 1 d . . . . .
C17 C 0.4791(3) 0.7966(2) 0.7738(2) 0.0570(12) Uani 1 1 d . . . . .
C18 C 0.4211(3) 0.7575(2) 0.79938(18) 0.0543(11) Uani 1 1 d . . . . .
C19 C 0.3769(2) 0.7150(2) 0.76078(17) 0.0476(10) Uani 1 1 d . . . . .
C20 C 0.4062(2) 0.7301(2) 0.71180(17) 0.0481(10) Uani 1 1 d . . . . .
C21 C 0.5137(3) 0.8145(3) 0.6772(3) 0.0861(18) Uani 1 1 d . . . . .
H21A H 0.520715 0.783637 0.648936 0.129 Uiso 1 1 calc R U . . .
H21B H 0.570864 0.830686 0.691697 0.129 Uiso 1 1 calc R U . . .
H21C H 0.477487 0.850983 0.663327 0.129 Uiso 1 1 calc R U . . .
C22 C 0.5317(4) 0.8533(2) 0.7991(3) 0.092(2) Uani 1 1 d . U . . .
H22A H 0.579792 0.863315 0.778757 0.139 Uiso 1 1 calc R U . . .
H22B H 0.554905 0.841457 0.834839 0.139 Uiso 1 1 calc R U . . .
H22C H 0.494069 0.891506 0.800052 0.139 Uiso 1 1 calc R U . . .
C23 C 0.3968(4) 0.7698(3) 0.8540(2) 0.091(2) Uani 1 1 d . . . . .
H23A H 0.449795 0.774111 0.878422 0.136 Uiso 1 1 calc R U . . .
H23B H 0.362273 0.733213 0.864737 0.136 Uiso 1 1 calc R U . . .
H23C H 0.362659 0.809851 0.854193 0.136 Uiso 1 1 calc R U . . .
C24 C 0.3032(3) 0.6683(2) 0.7693(2) 0.0651(13) Uani 1 1 d . . . . .
H24A H 0.303243 0.659902 0.806722 0.098 Uiso 1 1 calc R U . . .
H24B H 0.311467 0.627311 0.751064 0.098 Uiso 1 1 calc R U . . .
H24C H 0.247491 0.687674 0.755424 0.098 Uiso 1 1 calc R U . . .
C25 C 0.3663(3) 0.7062(3) 0.6588(2) 0.0801(17) Uani 1 1 d . . . . .
H25A H 0.319524 0.735753 0.645136 0.120 Uiso 1 1 calc R U . . .
H25B H 0.342605 0.662489 0.662334 0.120 Uiso 1 1 calc R U . . .
H25C H 0.410978 0.705030 0.634712 0.120 Uiso 1 1 calc R U . . .
C26 C 0.2497(2) 0.45152(18) 0.55362(14) 0.0363(8) Uani 1 1 d . . . . .
C27 C 0.2835(2) 0.42839(19) 0.60336(14) 0.0379(8) Uani 1 1 d . . . . .
H27 H 0.311593 0.387302 0.605597 0.046 Uiso 1 1 calc R U . . .
C28 C 0.2775(3) 0.4633(2) 0.64974(16) 0.0474(10) Uani 1 1 d . . . . .
H28 H 0.301040 0.445586 0.682360 0.057 Uiso 1 1 calc R U . . .
C29 C 0.2370(3) 0.5237(2) 0.64777(16) 0.0500(10) Uani 1 1 d . . . . .
H29 H 0.232792 0.547798 0.678856 0.060 Uiso 1 1 calc R U . . .
C30 C 0.2029(3) 0.5482(2) 0.59966(19) 0.0625(12) Uani 1 1 d . . . . .
H30 H 0.175399 0.589565 0.597781 0.075 Uiso 1 1 calc R U . . .
C31 C 0.2085(3) 0.5126(2) 0.55379(17) 0.0548(11) Uani 1 1 d . . . . .
H31 H 0.183464 0.530364 0.521507 0.066 Uiso 1 1 calc R U . . .
C32 C 0.1617(2) 0.36081(18) 0.50007(13) 0.0360(8) Uani 1 1 d . . . . .
C33 C 0.1635(3) 0.30307(19) 0.52980(16) 0.0446(9) Uani 1 1 d . . . . .
H33 H 0.217670 0.289075 0.547158 0.054 Uiso 1 1 calc R U . . .
C34 C 0.0899(3) 0.2654(2) 0.53507(19) 0.0596(12) Uani 1 1 d . . . . .
H34 H 0.094926 0.227005 0.555615 0.072 Uiso 1 1 calc R U . . .
C35 C 0.0097(3) 0.2840(3) 0.5104(2) 0.0687(14) Uani 1 1 d . . . . .
H35 H -0.040570 0.258444 0.513428 0.082 Uiso 1 1 calc R U . . .
C36 C 0.0040(3) 0.3403(3) 0.48133(18) 0.0662(14) Uani 1 1 d . . . . .
H36 H -0.050843 0.353752 0.464601 0.079 Uiso 1 1 calc R U . . .
C37 C 0.0789(2) 0.3785(2) 0.47597(16) 0.0503(10) Uani 1 1 d . . . . .
H37 H 0.072890 0.416979 0.455561 0.060 Uiso 1 1 calc R U . . .
B B 0.250000 0.4068(3) 0.500000 0.0336(12) Uani 1 2 d S T P . .
N1 N 0.67956(19) 0.74457(15) 0.77851(13) 0.0413(7) Uani 1 1 d . . . . .
N2 N 0.81777(19) 0.79127(15) 0.76776(13) 0.0406(7) Uani 1 1 d . . . . .
O O 0.52815(16) 0.60823(13) 0.69386(10) 0.0420(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd O 2.403(2) . ?
Gd N1 2.467(3) . ?
Gd N2 2.503(3) 7_666 ?
Gd C6 2.673(4) . ?
Gd C17 2.682(4) . ?
Gd C10 2.690(4) . ?
Gd C18 2.702(4) . ?
Gd C7 2.705(4) . ?
Gd C16 2.706(4) . ?
Gd C19 2.708(4) . ?
Gd C8 2.733(4) . ?
Gd C20 2.735(4) . ?
C1 N2 1.316(5) . ?
C1 N1 1.329(4) . ?
C1 H1 0.9400 . ?
C2 O 1.448(4) . ?
C2 C3 1.488(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 C4 1.443(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 C5 1.495(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O 1.465(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.407(6) . ?
C6 C10 1.420(6) . ?
C6 C11 1.507(6) . ?
C7 C8 1.411(6) . ?
C7 C12 1.517(6) . ?
C8 C9 1.404(6) . ?
C8 C13 1.517(6) . ?
C9 C10 1.413(6) . ?
C9 C14 1.507(6) . ?
C10 C15 1.508(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 C17 1.395(6) . ?
C16 C20 1.410(6) . ?
C16 C21 1.524(7) . ?
C17 C18 1.407(7) . ?
C17 C22 1.510(6) . ?
C18 C19 1.424(5) . ?
C18 C23 1.502(7) . ?
C19 C20 1.407(6) . ?
C19 C24 1.511(6) . ?
C20 C25 1.499(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.396(5) . ?
C26 C31 1.396(5) . ?
C26 B 1.643(5) . ?
C27 C28 1.391(5) . ?
C27 H27 0.9400 . ?
C28 C29 1.378(6) . ?
C28 H28 0.9400 . ?
C29 C30 1.372(6) . ?
C29 H29 0.9400 . ?
C30 C31 1.386(6) . ?
C30 H30 0.9400 . ?
C31 H31 0.9400 . ?
C32 C37 1.395(5) . ?
C32 C33 1.398(5) . ?
C32 B 1.645(5) . ?
C33 C34 1.382(6) . ?
C33 H33 0.9400 . ?
C34 C35 1.371(7) . ?
C34 H34 0.9400 . ?
C35 C36 1.361(7) . ?
C35 H35 0.9400 . ?
C36 C37 1.405(6) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
N1 N2 1.392(4) 7_666 ?

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
O Gd N1 113.72(9) . . ?
O Gd N2 81.22(9) . 7_666 ?
N1 Gd N2 32.51(10) . 7_666 ?
O Gd C6 128.58(12) . . ?
N1 Gd C6 81.18(12) . . ?
N2 Gd C6 100.86(12) 7_666 . ?
O Gd C17 121.96(12) . . ?
N1 Gd C17 77.86(12) . . ?
N2 Gd C17 95.57(13) 7_666 . ?
C6 Gd C17 109.07(14) . . ?
O Gd C10 102.26(11) . . ?
N1 Gd C10 76.11(12) . . ?
N2 Gd C10 81.39(12) 7_666 . ?
C6 Gd C10 30.71(13) . . ?
C17 Gd C10 134.80(13) . . ?
O Gd C18 123.06(11) . . ?
N1 Gd C18 103.55(12) . . ?
N2 Gd C18 125.71(13) 7_666 . ?
C6 Gd C18 97.48(14) . . ?
C17 Gd C18 30.29(15) . . ?
C10 Gd C18 128.19(13) . . ?
O Gd C7 116.60(11) . . ?
N1 Gd C7 111.02(12) . . ?
N2 Gd C7 129.74(12) 7_666 . ?
C6 Gd C7 30.31(13) . . ?
C17 Gd C7 109.41(15) . . ?
C10 Gd C7 49.94(13) . . ?
C18 Gd C7 85.34(14) . . ?
O Gd C16 92.45(12) . . ?
N1 Gd C16 83.91(11) . . ?
N2 Gd C16 85.76(12) 7_666 . ?
C6 Gd C16 138.92(14) . . ?
C17 Gd C16 30.01(14) . . ?
C10 Gd C16 158.68(13) . . ?
C18 Gd C16 49.68(15) . . ?
C7 Gd C16 135.02(13) . . ?
O Gd C19 93.46(10) . . ?
N1 Gd C19 127.76(11) . . ?
N2 Gd C19 135.04(12) 7_666 . ?
C6 Gd C19 116.29(14) . . ?
C17 Gd C19 50.09(12) . . ?
C10 Gd C19 142.56(13) . . ?
C18 Gd C19 30.51(12) . . ?
C7 Gd C19 92.63(13) . . ?
C16 Gd C19 49.67(13) . . ?
O Gd C8 86.74(11) . . ?
N1 Gd C8 125.39(12) . . ?
N2 Gd C8 125.40(11) 7_666 . ?
C6 Gd C8 50.00(13) . . ?
C17 Gd C8 134.46(15) . . ?
C10 Gd C8 49.63(12) . . ?
C18 Gd C8 105.37(14) . . ?
C7 Gd C8 30.08(12) . . ?
C16 Gd C8 148.12(13) . . ?
C19 Gd C8 98.53(13) . . ?
O Gd C20 75.89(11) . . ?
N1 Gd C20 113.41(12) . . ?
N2 Gd C20 107.46(12) 7_666 . ?
C6 Gd C20 145.52(13) . . ?
C17 Gd C20 49.72(12) . . ?
C10 Gd C20 170.34(13) . . ?
C18 Gd C20 49.76(13) . . ?
C7 Gd C20 122.10(13) . . ?
C16 Gd C20 30.03(12) . . ?
C19 Gd C20 29.95(13) . . ?
C8 Gd C20 120.72(13) . . ?
N2 C1 N1 126.8(4) . . ?
N2 C1 H1 116.6 . . ?
N1 C1 H1 116.6 . . ?
O C2 C3 105.8(3) . . ?
O C2 H2A 110.6 . . ?
C3 C2 H2A 110.6 . . ?
O C2 H2B 110.6 . . ?
C3 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
C4 C3 C2 105.3(4) . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3B 110.7 . . ?
C2 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
C3 C4 C5 105.4(4) . . ?
C3 C4 H4A 110.7 . . ?
C5 C4 H4A 110.7 . . ?
C3 C4 H4B 110.7 . . ?
C5 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
O C5 C4 105.3(3) . . ?
O C5 H5A 110.7 . . ?
C4 C5 H5A 110.7 . . ?
O C5 H5B 110.7 . . ?
C4 C5 H5B 110.7 . . ?
H5A C5 H5B 108.8 . . ?
C7 C6 C10 107.4(4) . . ?
C7 C6 C11 126.5(4) . . ?
C10 C6 C11 125.9(4) . . ?
C7 C6 Gd 76.1(2) . . ?
C10 C6 Gd 75.3(2) . . ?
C11 C6 Gd 117.9(3) . . ?
C6 C7 C8 108.4(4) . . ?
C6 C7 C12 126.6(4) . . ?
C8 C7 C12 123.3(4) . . ?
C6 C7 Gd 73.6(2) . . ?
C8 C7 Gd 76.0(2) . . ?
C12 C7 Gd 128.3(3) . . ?
C9 C8 C7 108.2(4) . . ?
C9 C8 C13 127.1(4) . . ?
C7 C8 C13 123.7(4) . . ?
C9 C8 Gd 75.3(2) . . ?
C7 C8 Gd 73.9(2) . . ?
C13 C8 Gd 125.8(3) . . ?
C8 C9 C10 107.9(3) . . ?
C8 C9 C14 127.5(4) . . ?
C10 C9 C14 124.3(4) . . ?
C8 C9 Gd 74.9(2) . . ?
C10 C9 Gd 73.0(2) . . ?
C14 C9 Gd 123.2(3) . . ?
C9 C10 C6 108.1(4) . . ?
C9 C10 C15 125.0(4) . . ?
C6 C10 C15 126.4(4) . . ?
C9 C10 Gd 76.8(2) . . ?
C6 C10 Gd 74.0(2) . . ?
C15 C10 Gd 121.7(3) . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C20 108.6(4) . . ?
C17 C16 C21 126.2(4) . . ?
C20 C16 C21 125.0(5) . . ?
C17 C16 Gd 74.0(2) . . ?
C20 C16 Gd 76.1(2) . . ?
C21 C16 Gd 120.6(3) . . ?
C16 C17 C18 108.4(4) . . ?
C16 C17 C22 126.4(5) . . ?
C18 C17 C22 124.7(5) . . ?
C16 C17 Gd 76.0(2) . . ?
C18 C17 Gd 75.7(2) . . ?
C22 C17 Gd 121.5(3) . . ?
C17 C18 C19 107.5(4) . . ?
C17 C18 C23 124.8(4) . . ?
C19 C18 C23 126.4(5) . . ?
C17 C18 Gd 74.1(2) . . ?
C19 C18 Gd 75.0(2) . . ?
C23 C18 Gd 126.9(3) . . ?
C20 C19 C18 107.9(4) . . ?
C20 C19 C24 125.6(4) . . ?
C18 C19 C24 126.1(4) . . ?
C20 C19 Gd 76.1(2) . . ?
C18 C19 Gd 74.5(2) . . ?
C24 C19 Gd 121.5(3) . . ?
C19 C20 C16 107.7(4) . . ?
C19 C20 C25 126.2(4) . . ?
C16 C20 C25 125.3(5) . . ?
C19 C20 Gd 73.9(2) . . ?
C16 C20 Gd 73.8(2) . . ?
C25 C20 Gd 126.0(3) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C31 114.8(3) . . ?
C27 C26 B 122.2(3) . . ?
C31 C26 B 122.7(3) . . ?
C28 C27 C26 123.1(4) . . ?
C28 C27 H27 118.4 . . ?
C26 C27 H27 118.4 . . ?
C29 C28 C27 119.8(4) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C30 C29 C28 118.9(4) . . ?
C30 C29 H29 120.6 . . ?
C28 C29 H29 120.6 . . ?
C29 C30 C31 120.7(4) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C30 C31 C26 122.6(4) . . ?
C30 C31 H31 118.7 . . ?
C26 C31 H31 118.7 . . ?
C37 C32 C33 114.7(4) . . ?
C37 C32 B 124.1(3) . . ?
C33 C32 B 120.9(3) . . ?
C34 C33 C32 123.6(4) . . ?
C34 C33 H33 118.2 . . ?
C32 C33 H33 118.2 . . ?
C35 C34 C33 120.1(5) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C36 C35 C34 118.8(4) . . ?
C36 C35 H35 120.6 . . ?
C34 C35 H35 120.6 . . ?
C35 C36 C37 121.1(4) . . ?
C35 C36 H36 119.5 . . ?
C37 C36 H36 119.5 . . ?
C32 C37 C36 121.8(4) . . ?
C32 C37 H37 119.1 . . ?
C36 C37 H37 119.1 . . ?
C26 B C26 112.7(4) 2_556 . ?
C26 B C32 113.28(17) 2_556 . ?
C26 B C32 103.66(17) . . ?
C26 B C32 103.66(17) 2_556 2_556 ?
C26 B C32 113.28(17) . 2_556 ?
C32 B C32 110.6(4) . 2_556 ?
C1 N1 N2 116.5(3) . 7_666 ?
C1 N1 Gd 167.7(3) . . ?
N2 N1 Gd 75.17(17) 7_666 . ?
C1 N2 N1 116.7(3) . 7_666 ?
C1 N2 Gd 170.3(3) . 7_666 ?
N1 N2 Gd 72.31(18) 7_666 7_666 ?
C2 O C5 108.6(3) . . ?
C2 O Gd 126.4(2) . . ?
C5 O Gd 124.5(2) . . ?

# start Validation Reply Form

_vrf_PLAT606_Gd2                 
;
RESPONSE: The structure contains an area of disordered 
solvent involving two diethyl ether (Et2O) molecules; 
attempts to model it with a chemically reasonable geometry were unsuccessful. 
Therefore, the SQUEEZE procedure of PLATON (A.L.Spek (2015) Acta Cryst. C71, 
9-18) was employed to remove the contribution of the electron 
density associated with those solvent molecules from the intensity 
data. The solvent-free model and intensity data were used for the 
final results reported here.  
;
_vrf_PLAT869_Gd2                 
; 
RESPONSE:See comment above.
;

# end Validation Reply Form



_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_Dy2
_database_code_depnum_ccdc_archive 'CCDC 2202465'
loop_
_audit_author_name
_audit_author_address
'Alexandros A. Kitos'
;University of Ottawa
Canada
;
_audit_update_record             
;
2022-08-19 deposited with the CCDC.	2022-11-17 downloaded from the CCDC.
;
#=============================================================
# CHEMICAL DATA

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H78 Dy2 N4 O2, C24 H20 B'
_chemical_formula_sum            'C74 H98 B Dy2 N4 O2'
_chemical_formula_weight         1411.37

#=============================================================
# CRYSTAL DATA

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'
B B 0.0013 0.0007 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, 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                   15.2675(6)
_cell_length_b                   20.2943(8)
_cell_length_c                   25.5113(12)
_cell_angle_alpha                90
_cell_angle_beta                 96.393(3)
_cell_angle_gamma                90
_cell_volume                     7855.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    9944
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.40

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             2892
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.928
_shelx_estimated_absorpt_T_min   0.676
_shelx_estimated_absorpt_T_max   0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?

#=============================================================
# EXPERIMENTAL DATA

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω and φ scans'
_diffrn_ambient_temperature      203(2)
_diffrn_reflns_number            52187
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.676
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999

#=============================================================
# REFINEMENT DATA 

_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_number_total             8592
_reflns_number_gt                6742
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8592
_refine_ls_number_parameters     385
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0642
_refine_ls_wR_factor_gt          0.0597
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0330P)²+3.7425P] where P=(Fo²+2Fc²)/3'
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.070

#=============================================================
# GENERAL COMPUTING 

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#=============================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
Dy Dy 0.54690(2) 0.67628(2) 0.77122(2) 0.03145(5) Uani 1 1 d . . . . .
C1 C 0.74773(18) 0.78328(14) 0.79267(12) 0.0382(6) Uani 1 1 d . . . . .
H1 H 0.745977 0.807464 0.823963 0.046 Uiso 1 1 calc R U . . .
C2 C 0.4681(2) 0.55475(17) 0.68425(14) 0.0563(9) Uani 1 1 d . . . . .
H2A H 0.406870 0.569955 0.682239 0.068 Uiso 1 1 calc R U . . .
H2B H 0.477976 0.521769 0.712337 0.068 Uiso 1 1 calc R U . . .
C3 C 0.4870(3) 0.5265(2) 0.63280(17) 0.0908(16) Uani 1 1 d . U . . .
H3A H 0.530412 0.490917 0.638232 0.109 Uiso 1 1 calc R U . . .
H3B H 0.433120 0.509154 0.613200 0.109 Uiso 1 1 calc R U . . .
C4 C 0.5214(3) 0.5804(2) 0.60490(14) 0.0684(11) Uani 1 1 d . . . . .
H4A H 0.473396 0.604670 0.584703 0.082 Uiso 1 1 calc R U . . .
H4B H 0.561755 0.564240 0.580506 0.082 Uiso 1 1 calc R U . . .
C5 C 0.5688(2) 0.62344(15) 0.64587(12) 0.0443(7) Uani 1 1 d . . . . .
H5A H 0.631847 0.612968 0.650557 0.053 Uiso 1 1 calc R U . . .
H5B H 0.561498 0.669954 0.636032 0.053 Uiso 1 1 calc R U . . .
C6 C 0.66456(19) 0.60804(16) 0.83366(13) 0.0448(7) Uani 1 1 d . . . . .
C7 C 0.6144(2) 0.64367(16) 0.86749(12) 0.0469(7) Uani 1 1 d . . . . .
C8 C 0.5293(2) 0.61561(16) 0.86291(13) 0.0466(7) Uani 1 1 d . . . . .
C9 C 0.5265(2) 0.56376(15) 0.82578(13) 0.0432(7) Uani 1 1 d . . . . .
C10 C 0.6105(2) 0.55879(14) 0.80855(12) 0.0427(7) Uani 1 1 d . . . . .
C11 C 0.7623(2) 0.6149(2) 0.83113(16) 0.0651(10) Uani 1 1 d . . . . .
H11A H 0.782699 0.656026 0.847572 0.098 Uiso 1 1 calc R U . . .
H11B H 0.774162 0.614725 0.794563 0.098 Uiso 1 1 calc R U . . .
H11C H 0.792815 0.578361 0.849614 0.098 Uiso 1 1 calc R U . . .
C12 C 0.6479(3) 0.6980(2) 0.90450(15) 0.0681(10) Uani 1 1 d . . . . .
H12A H 0.679163 0.679075 0.936144 0.102 Uiso 1 1 calc R U . . .
H12B H 0.598653 0.723979 0.913853 0.102 Uiso 1 1 calc R U . . .
H12C H 0.687656 0.726033 0.887371 0.102 Uiso 1 1 calc R U . . .
C13 C 0.4600(3) 0.6260(2) 0.90003(16) 0.0739(12) Uani 1 1 d . . . . .
H13A H 0.402583 0.630048 0.879833 0.111 Uiso 1 1 calc R U . . .
H13B H 0.473157 0.665916 0.920304 0.111 Uiso 1 1 calc R U . . .
H13C H 0.459887 0.588693 0.923794 0.111 Uiso 1 1 calc R U . . .
C14 C 0.4518(3) 0.51505(18) 0.81653(16) 0.0657(10) Uani 1 1 d . . . . .
H14A H 0.467181 0.481125 0.792372 0.098 Uiso 1 1 calc R U . . .
H14B H 0.398959 0.537659 0.801479 0.098 Uiso 1 1 calc R U . . .
H14C H 0.441369 0.495026 0.849790 0.098 Uiso 1 1 calc R U . . .
C15 C 0.6429(3) 0.50542(18) 0.77361(15) 0.0641(10) Uani 1 1 d . . . . .
H15A H 0.600030 0.469981 0.769454 0.096 Uiso 1 1 calc R U . . .
H15B H 0.698831 0.488366 0.789768 0.096 Uiso 1 1 calc R U . . .
H15C H 0.650420 0.523831 0.739316 0.096 Uiso 1 1 calc R U . . .
C16 C 0.47237(19) 0.78014(16) 0.71909(15) 0.0496(8) Uani 1 1 d . . . . .
C17 C 0.4808(2) 0.79747(15) 0.77260(16) 0.0526(9) Uani 1 1 d . . . . .
C18 C 0.4228(2) 0.75819(16) 0.79860(14) 0.0508(8) Uani 1 1 d . . . . .
C19 C 0.37852(18) 0.71525(15) 0.76051(13) 0.0429(7) Uani 1 1 d . . . . .
C20 C 0.40776(18) 0.73015(15) 0.71148(13) 0.0425(7) Uani 1 1 d . . . . .
C21 C 0.5151(3) 0.81379(19) 0.6758(2) 0.0768(13) Uani 1 1 d . . . . .
H21A H 0.514645 0.784376 0.645816 0.115 Uiso 1 1 calc R U . . .
H21B H 0.575489 0.825034 0.688596 0.115 Uiso 1 1 calc R U . . .
H21C H 0.482750 0.853605 0.665197 0.115 Uiso 1 1 calc R U . . .
C22 C 0.5337(3) 0.85398(18) 0.7978(2) 0.0834(14) Uani 1 1 d . . . . .
H22A H 0.495639 0.891966 0.799897 0.125 Uiso 1 1 calc R U . . .
H22B H 0.580804 0.864932 0.776810 0.125 Uiso 1 1 calc R U . . .
H22C H 0.558610 0.841473 0.833061 0.125 Uiso 1 1 calc R U . . .
C23 C 0.3991(3) 0.7712(2) 0.85315(16) 0.0820(14) Uani 1 1 d . . . . .
H23A H 0.452411 0.774615 0.877464 0.123 Uiso 1 1 calc R U . . .
H23B H 0.363184 0.735234 0.863923 0.123 Uiso 1 1 calc R U . . .
H23C H 0.366190 0.812064 0.853328 0.123 Uiso 1 1 calc R U . . .
C24 C 0.3042(2) 0.66886(18) 0.76897(16) 0.0587(9) Uani 1 1 d . . . . .
H24A H 0.315213 0.626221 0.753817 0.088 Uiso 1 1 calc R U . . .
H24B H 0.249160 0.686573 0.752064 0.088 Uiso 1 1 calc R U . . .
H24C H 0.300455 0.663944 0.806478 0.088 Uiso 1 1 calc R U . . .
C25 C 0.3664(2) 0.7067(2) 0.65891(15) 0.0633(10) Uani 1 1 d . . . . .
H25A H 0.319822 0.736845 0.645625 0.095 Uiso 1 1 calc R U . . .
H25B H 0.342004 0.663081 0.662525 0.095 Uiso 1 1 calc R U . . .
H25C H 0.410709 0.705135 0.634448 0.095 Uiso 1 1 calc R U . . .
C26 C 0.24990(18) 0.45215(13) 0.55353(11) 0.0343(6) Uani 1 1 d . . . . .
C27 C 0.28359(18) 0.42904(14) 0.60328(11) 0.0352(6) Uani 1 1 d . . . . .
H27 H 0.311958 0.387873 0.605670 0.042 Uiso 1 1 calc R U . . .
C28 C 0.27705(19) 0.46412(16) 0.64931(12) 0.0431(7) Uani 1 1 d . . . . .
H28 H 0.300255 0.446432 0.681989 0.052 Uiso 1 1 calc R U . . .
C29 C 0.2366(2) 0.52484(16) 0.64721(13) 0.0479(8) Uani 1 1 d . . . . .
H29 H 0.232687 0.549175 0.678213 0.057 Uiso 1 1 calc R U . . .
C30 C 0.2022(3) 0.54920(17) 0.59931(14) 0.0595(9) Uani 1 1 d . . . . .
H30 H 0.174380 0.590599 0.597449 0.071 Uiso 1 1 calc R U . . .
C31 C 0.2078(2) 0.51348(15) 0.55346(13) 0.0518(8) Uani 1 1 d . . . . .
H31 H 0.182451 0.531042 0.521191 0.062 Uiso 1 1 calc R U . . .
C32 C 0.16160(17) 0.36113(13) 0.50002(10) 0.0325(6) Uani 1 1 d . . . . .
C33 C 0.1633(2) 0.30309(15) 0.52955(12) 0.0426(7) Uani 1 1 d . . . . .
H33 H 0.217749 0.288973 0.546769 0.051 Uiso 1 1 calc R U . . .
C34 C 0.0898(2) 0.26536(17) 0.53486(14) 0.0572(9) Uani 1 1 d . . . . .
H34 H 0.094785 0.226706 0.555274 0.069 Uiso 1 1 calc R U . . .
C35 C 0.0098(3) 0.2843(2) 0.51044(15) 0.0661(11) Uani 1 1 d . . . . .
H35 H -0.040665 0.258763 0.513877 0.079 Uiso 1 1 calc R U . . .
C36 C 0.0036(2) 0.3403(2) 0.48107(14) 0.0662(11) Uani 1 1 d . . . . .
H36 H -0.051353 0.353402 0.463986 0.079 Uiso 1 1 calc R U . . .
C37 C 0.07864(19) 0.37866(18) 0.47606(12) 0.0482(8) Uani 1 1 d . . . . .
H37 H 0.072620 0.417462 0.455855 0.058 Uiso 1 1 calc R U . . .
B B 0.250000 0.4070(2) 0.500000 0.0313(9) Uani 1 2 d S T P . .
N1 N 0.67907(14) 0.74518(11) 0.77817(10) 0.0377(5) Uani 1 1 d . . . . .
N2 N 0.81842(15) 0.79101(11) 0.76794(10) 0.0376(5) Uani 1 1 d . . . . .
O O 0.52865(12) 0.60965(9) 0.69422(7) 0.0375(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy O 2.3755(18) . ?
Dy N1 2.445(2) . ?
Dy N2 2.475(2) 7_666 ?
Dy C7 2.640(3) . ?
Dy C6 2.654(3) . ?
Dy C17 2.660(3) . ?
Dy C18 2.671(3) . ?
Dy C19 2.674(3) . ?
Dy C16 2.677(3) . ?
Dy C8 2.683(3) . ?
Dy C20 2.704(3) . ?
Dy C10 2.708(3) . ?
C1 N2 1.319(3) . ?
C1 N1 1.322(3) . ?
C1 H1 0.9400 . ?
C2 O 1.452(3) . ?
C2 C3 1.489(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 C4 1.435(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 C5 1.487(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O 1.464(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C10 1.404(4) . ?
C6 C7 1.415(4) . ?
C6 C11 1.507(4) . ?
C7 C8 1.412(4) . ?
C7 C12 1.504(5) . ?
C8 C9 1.413(4) . ?
C8 C13 1.511(4) . ?
C9 C10 1.406(4) . ?
C9 C14 1.507(4) . ?
C10 C15 1.520(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 C17 1.402(5) . ?
C16 C20 1.413(4) . ?
C16 C21 1.507(5) . ?
C17 C18 1.411(5) . ?
C17 C22 1.505(5) . ?
C18 C19 1.419(4) . ?
C18 C23 1.500(5) . ?
C19 C20 1.407(4) . ?
C19 C24 1.508(4) . ?
C20 C25 1.495(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C27 1.396(4) . ?
C26 C31 1.401(4) . ?
C26 B 1.645(4) . ?
C27 C28 1.386(4) . ?
C27 H27 0.9400 . ?
C28 C29 1.377(4) . ?
C28 H28 0.9400 . ?
C29 C30 1.368(5) . ?
C29 H29 0.9400 . ?
C30 C31 1.387(4) . ?
C30 H30 0.9400 . ?
C31 H31 0.9400 . ?
C32 C37 1.390(4) . ?
C32 C33 1.397(4) . ?
C32 B 1.640(4) . ?
C33 C34 1.378(4) . ?
C33 H33 0.9400 . ?
C34 C35 1.363(6) . ?
C34 H34 0.9400 . ?
C35 C36 1.359(6) . ?
C35 H35 0.9400 . ?
C36 C37 1.403(5) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
N1 N2 1.391(3) 7_666 ?

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
O Dy N1 113.92(7) . . ?
O Dy N2 81.09(7) . 7_666 ?
N1 Dy N2 32.84(7) . 7_666 ?
O Dy C7 128.63(8) . . ?
N1 Dy C7 80.93(9) . . ?
N2 Dy C7 100.78(9) 7_666 . ?
O Dy C6 102.03(9) . . ?
N1 Dy C6 75.93(9) . . ?
N2 Dy C6 81.08(9) 7_666 . ?
C7 Dy C6 31.00(9) . . ?
O Dy C17 121.84(10) . . ?
N1 Dy C17 77.37(9) . . ?
N2 Dy C17 95.20(10) 7_666 . ?
C7 Dy C17 109.19(11) . . ?
C6 Dy C17 134.97(11) . . ?
O Dy C18 123.31(9) . . ?
N1 Dy C18 103.23(9) . . ?
N2 Dy C18 125.74(10) 7_666 . ?
C7 Dy C18 97.32(10) . . ?
C6 Dy C18 128.32(10) . . ?
C17 Dy C18 30.70(11) . . ?
O Dy C19 93.50(8) . . ?
N1 Dy C19 127.91(8) . . ?
N2 Dy C19 135.39(9) 7_666 . ?
C7 Dy C19 116.12(10) . . ?
C6 Dy C19 142.58(10) . . ?
C17 Dy C19 50.68(9) . . ?
C18 Dy C19 30.80(9) . . ?
O Dy C16 91.90(9) . . ?
N1 Dy C16 83.54(9) . . ?
N2 Dy C16 85.11(9) 7_666 . ?
C7 Dy C16 139.44(10) . . ?
C6 Dy C16 158.53(10) . . ?
C17 Dy C16 30.45(11) . . ?
C18 Dy C16 50.61(11) . . ?
C19 Dy C16 50.65(10) . . ?
O Dy C8 116.47(9) . . ?
N1 Dy C8 111.17(9) . . ?
N2 Dy C8 130.05(9) 7_666 . ?
C7 Dy C8 30.74(10) . . ?
C6 Dy C8 50.52(9) . . ?
C17 Dy C8 109.74(11) . . ?
C18 Dy C8 85.10(11) . . ?
C19 Dy C8 92.07(10) . . ?
C16 Dy C8 135.71(10) . . ?
O Dy C20 75.62(8) . . ?
N1 Dy C20 113.57(9) . . ?
N2 Dy C20 107.46(9) 7_666 . ?
C7 Dy C20 145.76(9) . . ?
C6 Dy C20 170.42(9) . . ?
C17 Dy C20 50.08(10) . . ?
C18 Dy C20 50.22(10) . . ?
C19 Dy C20 30.33(9) . . ?
C16 Dy C20 30.45(9) . . ?
C8 Dy C20 121.88(9) . . ?
O Dy C10 78.11(8) . . ?
N1 Dy C10 102.54(9) . . ?
N2 Dy C10 95.53(8) 7_666 . ?
C7 Dy C10 50.53(9) . . ?
C6 Dy C10 30.35(10) . . ?
C17 Dy C10 158.65(11) . . ?
C18 Dy C10 133.89(10) . . ?
C19 Dy C10 126.84(9) . . ?
C16 Dy C10 169.74(10) . . ?
C8 Dy C10 49.92(9) . . ?
C20 Dy C10 141.54(10) . . ?
N2 C1 N1 127.0(3) . . ?
N2 C1 H1 116.5 . . ?
N1 C1 H1 116.5 . . ?
O C2 C3 105.5(2) . . ?
O C2 H2A 110.6 . . ?
C3 C2 H2A 110.6 . . ?
O C2 H2B 110.6 . . ?
C3 C2 H2B 110.6 . . ?
H2A C2 H2B 108.8 . . ?
C4 C3 C2 105.2(3) . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3B 110.7 . . ?
C2 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
C3 C4 C5 106.0(3) . . ?
C3 C4 H4A 110.5 . . ?
C5 C4 H4A 110.5 . . ?
C3 C4 H4B 110.5 . . ?
C5 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
O C5 C4 105.2(2) . . ?
O C5 H5A 110.7 . . ?
C4 C5 H5A 110.7 . . ?
O C5 H5B 110.7 . . ?
C4 C5 H5B 110.7 . . ?
H5A C5 H5B 108.8 . . ?
C10 C6 C7 108.2(3) . . ?
C10 C6 C11 125.5(3) . . ?
C7 C6 C11 125.8(3) . . ?
C10 C6 Dy 76.92(18) . . ?
C7 C6 Dy 73.93(18) . . ?
C11 C6 Dy 122.2(2) . . ?
C8 C7 C6 107.4(3) . . ?
C8 C7 C12 126.4(3) . . ?
C6 C7 C12 126.0(3) . . ?
C8 C7 Dy 76.33(19) . . ?
C6 C7 Dy 75.07(18) . . ?
C12 C7 Dy 118.1(2) . . ?
C7 C8 C9 108.3(3) . . ?
C7 C8 C13 126.4(3) . . ?
C9 C8 C13 123.6(3) . . ?
C7 C8 Dy 72.92(18) . . ?
C9 C8 Dy 75.87(18) . . ?
C13 C8 Dy 128.9(2) . . ?
C10 C9 C8 107.6(3) . . ?
C10 C9 C14 127.2(3) . . ?
C8 C9 C14 124.0(3) . . ?
C10 C9 Dy 74.85(17) . . ?
C8 C9 Dy 73.76(18) . . ?
C14 C9 Dy 126.9(2) . . ?
C6 C10 C9 108.4(3) . . ?
C6 C10 C15 124.2(3) . . ?
C9 C10 C15 127.0(3) . . ?
C6 C10 Dy 72.73(17) . . ?
C9 C10 Dy 75.07(18) . . ?
C15 C10 Dy 123.3(2) . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C20 107.5(3) . . ?
C17 C16 C21 126.8(3) . . ?
C20 C16 C21 125.3(4) . . ?
C17 C16 Dy 74.09(19) . . ?
C20 C16 Dy 75.80(18) . . ?
C21 C16 Dy 121.7(2) . . ?
C16 C17 C18 108.7(3) . . ?
C16 C17 C22 126.5(4) . . ?
C18 C17 C22 124.3(4) . . ?
C16 C17 Dy 75.46(18) . . ?
C18 C17 Dy 75.09(17) . . ?
C22 C17 Dy 121.6(2) . . ?
C17 C18 C19 107.5(3) . . ?
C17 C18 C23 124.5(3) . . ?
C19 C18 C23 126.7(3) . . ?
C17 C18 Dy 74.21(16) . . ?
C19 C18 Dy 74.72(15) . . ?
C23 C18 Dy 127.1(2) . . ?
C20 C19 C18 107.6(3) . . ?
C20 C19 C24 125.4(3) . . ?
C18 C19 C24 126.4(3) . . ?
C20 C19 Dy 75.98(16) . . ?
C18 C19 Dy 74.48(16) . . ?
C24 C19 Dy 122.1(2) . . ?
C19 C20 C16 108.5(3) . . ?
C19 C20 C25 125.8(3) . . ?
C16 C20 C25 124.7(3) . . ?
C19 C20 Dy 73.69(18) . . ?
C16 C20 Dy 73.75(18) . . ?
C25 C20 Dy 127.2(2) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C31 115.0(3) . . ?
C27 C26 B 122.2(2) . . ?
C31 C26 B 122.5(3) . . ?
C28 C27 C26 122.9(3) . . ?
C28 C27 H27 118.5 . . ?
C26 C27 H27 118.5 . . ?
C29 C28 C27 120.1(3) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 119.0(3) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
C29 C30 C31 120.7(3) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 H30 119.6 . . ?
C30 C31 C26 122.3(3) . . ?
C30 C31 H31 118.8 . . ?
C26 C31 H31 118.8 . . ?
C37 C32 C33 114.5(3) . . ?
C37 C32 B 124.4(3) . . ?
C33 C32 B 120.8(2) . . ?
C34 C33 C32 123.7(3) . . ?
C34 C33 H33 118.2 . . ?
C32 C33 H33 118.2 . . ?
C35 C34 C33 119.8(3) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C36 C35 C34 119.4(3) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C35 C36 C37 120.5(3) . . ?
C35 C36 H36 119.7 . . ?
C37 C36 H36 119.8 . . ?
C32 C37 C36 122.1(3) . . ?
C32 C37 H37 119.0 . . ?
C36 C37 H37 119.0 . . ?
C32 B C32 110.8(3) 2_556 . ?
C32 B C26 113.16(14) 2_556 . ?
C32 B C26 103.84(12) . . ?
C32 B C26 103.84(12) 2_556 2_556 ?
C32 B C26 113.16(14) . 2_556 ?
C26 B C26 112.3(3) . 2_556 ?
C1 N1 N2 116.7(2) . 7_666 ?
C1 N1 Dy 167.7(2) . . ?
N2 N1 Dy 74.75(13) 7_666 . ?
C1 N2 N1 116.3(2) . 7_666 ?
C1 N2 Dy 170.43(19) . 7_666 ?
N1 N2 Dy 72.42(13) 7_666 7_666 ?
C2 O C5 108.5(2) . . ?
C2 O Dy 126.54(16) . . ?
C5 O Dy 124.49(16) . . ?

# start Validation Reply Form

_vrf_PLAT606_Dy2                 
;
RESPONSE: The structure contains an area of disordered 
solvent involving two diethyl ether (Et2O) molecules; 
attempts to model it with a chemically reasonable geometry were unsuccessful. 
Therefore, the SQUEEZE procedure of PLATON (A.L.Spek (2015) Acta Cryst. C71, 
9-18) was employed to remove the contribution of the electron 
density associated with those solvent molecules from the intensity 
data. The solvent-free model and intensity data were used for the 
final results reported here.  
;
_vrf_PLAT869_Dy2                 
; 
RESPONSE:See comment above.
;
_vrf_PLAT933_Dy2                 
;
RESPONSE: Those discordant reflections with error/esd > 10
 have been removed from the refinement.
;
# end Validation Reply Form



_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_Tb2
_database_code_depnum_ccdc_archive 'CCDC 2202464'
loop_
_audit_author_name
_audit_author_address
'Alexandros A. Kitos'
;University of Ottawa
Canada
;
_audit_update_record             
;
2022-08-19 deposited with the CCDC.	2022-11-17 downloaded from the CCDC.
;
#=============================================================
# CHEMICAL DATA

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H78 N4 O2 Tb2, C24 H20 B'
_chemical_formula_sum            'C74 H98 B N4 O2 Tb2'
_chemical_formula_weight         1404.21

#=============================================================
# CRYSTAL DATA

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'
B B 0.0013 0.0007 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, 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                   15.2603(8)
_cell_length_b                   20.2689(11)
_cell_length_c                   25.5427(14)
_cell_angle_alpha                90
_cell_angle_beta                 96.330(3)
_cell_angle_gamma                90
_cell_volume                     7852.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    9937
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      33.24

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_F_000             2884
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.827
_shelx_estimated_absorpt_T_min   0.536
_shelx_estimated_absorpt_T_max   0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5361
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?

#=============================================================
# EXPERIMENTAL DATA

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω and φ scans'
_diffrn_ambient_temperature      203(2)
_diffrn_reflns_number            70044
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.286
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000

#=============================================================
# REFINEMENT DATA 

_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_number_total             8587
_reflns_number_gt                7252
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8587
_refine_ls_number_parameters     385
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0634
_refine_ls_wR_factor_gt          0.0578
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0208P)²+24.0768P] where P=(Fo²+2Fc²)/3'
_refine_diff_density_max         1.514
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.068

#=============================================================
# GENERAL COMPUTING 

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#=============================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
Tb Tb 0.54672(2) 0.67586(2) 0.77149(2) 0.03051(5) Uani 1 1 d . . . . .
C1 C 0.74775(17) 0.78346(13) 0.79285(12) 0.0370(6) Uani 1 1 d . . . . .
H1 H 0.745976 0.807693 0.824094 0.044 Uiso 1 1 calc R U . . .
C2 C 0.4684(2) 0.55406(18) 0.68421(14) 0.0555(9) Uani 1 1 d . . . . .
H2A H 0.407149 0.569013 0.682748 0.067 Uiso 1 1 calc R U . . .
H2B H 0.479053 0.520827 0.712053 0.067 Uiso 1 1 calc R U . . .
C3 C 0.4863(3) 0.5262(2) 0.63248(17) 0.0877(15) Uani 1 1 d . U . . .
H3A H 0.529819 0.490512 0.637438 0.105 Uiso 1 1 calc R U . . .
H3B H 0.432106 0.508818 0.613266 0.105 Uiso 1 1 calc R U . . .
C4 C 0.5201(3) 0.5803(2) 0.60435(14) 0.0699(11) Uani 1 1 d . . . . .
H4A H 0.471813 0.604793 0.584632 0.084 Uiso 1 1 calc R U . . .
H4B H 0.560040 0.564362 0.579615 0.084 Uiso 1 1 calc R U . . .
C5 C 0.56825(19) 0.62303(16) 0.64547(12) 0.0446(7) Uani 1 1 d . . . . .
H5A H 0.631256 0.612323 0.649858 0.053 Uiso 1 1 calc R U . . .
H5B H 0.561167 0.669712 0.635942 0.053 Uiso 1 1 calc R U . . .
C6 C 0.6145(2) 0.64290(16) 0.86828(12) 0.0459(7) Uani 1 1 d . . . . .
C7 C 0.66469(19) 0.60748(15) 0.83443(13) 0.0438(7) Uani 1 1 d . . . . .
C8 C 0.6109(2) 0.55808(14) 0.80903(12) 0.0427(7) Uani 1 1 d . . . . .
C9 C 0.5271(2) 0.56321(15) 0.82639(12) 0.0422(7) Uani 1 1 d . . . . .
C10 C 0.5295(2) 0.61501(16) 0.86361(12) 0.0456(7) Uani 1 1 d . . . . .
C11 C 0.6478(3) 0.6972(2) 0.90541(15) 0.0711(11) Uani 1 1 d . . . . .
H11A H 0.676274 0.678051 0.937721 0.107 Uiso 1 1 calc R U . . .
H11B H 0.598691 0.724402 0.913359 0.107 Uiso 1 1 calc R U . . .
H11C H 0.689858 0.724014 0.889115 0.107 Uiso 1 1 calc R U . . .
C12 C 0.7624(2) 0.6140(2) 0.83173(17) 0.0667(11) Uani 1 1 d . . . . .
H12A H 0.782604 0.656148 0.846519 0.100 Uiso 1 1 calc R U . . .
H12B H 0.774503 0.611544 0.795292 0.100 Uiso 1 1 calc R U . . .
H12C H 0.793052 0.578593 0.851656 0.100 Uiso 1 1 calc R U . . .
C13 C 0.6431(3) 0.50511(18) 0.77439(15) 0.0634(10) Uani 1 1 d . . . . .
H13A H 0.599523 0.470151 0.769482 0.095 Uiso 1 1 calc R U . . .
H13B H 0.698263 0.487251 0.790950 0.095 Uiso 1 1 calc R U . . .
H13C H 0.652112 0.523841 0.740459 0.095 Uiso 1 1 calc R U . . .
C14 C 0.4521(3) 0.51474(18) 0.81699(16) 0.0657(10) Uani 1 1 d . . . . .
H14A H 0.467786 0.480335 0.793312 0.099 Uiso 1 1 calc R U . . .
H14B H 0.399707 0.537450 0.801373 0.099 Uiso 1 1 calc R U . . .
H14C H 0.440674 0.495225 0.850237 0.099 Uiso 1 1 calc R U . . .
C15 C 0.4601(3) 0.6254(2) 0.90053(16) 0.0713(11) Uani 1 1 d . . . . .
H15A H 0.402598 0.628497 0.880343 0.107 Uiso 1 1 calc R U . . .
H15B H 0.472443 0.665949 0.920191 0.107 Uiso 1 1 calc R U . . .
H15C H 0.460771 0.588584 0.924787 0.107 Uiso 1 1 calc R U . . .
C16 C 0.47102(19) 0.78015(15) 0.71958(15) 0.0492(8) Uani 1 1 d . . . . .
C17 C 0.4800(2) 0.79699(15) 0.77334(16) 0.0537(9) Uani 1 1 d . . . . .
C18 C 0.42209(19) 0.75784(16) 0.79896(14) 0.0491(8) Uani 1 1 d . . . . .
C19 C 0.37763(17) 0.71506(15) 0.76075(13) 0.0419(7) Uani 1 1 d . . . . .
C20 C 0.40696(17) 0.72992(15) 0.71159(13) 0.0421(7) Uani 1 1 d . . . . .
C21 C 0.5147(3) 0.8140(2) 0.6767(2) 0.0768(13) Uani 1 1 d . . . . .
H21A H 0.513048 0.785209 0.646274 0.115 Uiso 1 1 calc R U . . .
H21B H 0.575481 0.823960 0.689447 0.115 Uiso 1 1 calc R U . . .
H21C H 0.483598 0.854646 0.666782 0.115 Uiso 1 1 calc R U . . .
C22 C 0.5329(3) 0.85378(18) 0.7984(2) 0.0849(15) Uani 1 1 d . . . . .
H22A H 0.495045 0.892003 0.799944 0.127 Uiso 1 1 calc R U . . .
H22B H 0.580538 0.864247 0.777586 0.127 Uiso 1 1 calc R U . . .
H22C H 0.557218 0.841611 0.833768 0.127 Uiso 1 1 calc R U . . .
C23 C 0.3981(3) 0.7706(2) 0.85337(16) 0.0808(14) Uani 1 1 d . . . . .
H23A H 0.451354 0.775623 0.877489 0.121 Uiso 1 1 calc R U . . .
H23B H 0.363992 0.733778 0.864515 0.121 Uiso 1 1 calc R U . . .
H23C H 0.363267 0.810655 0.853328 0.121 Uiso 1 1 calc R U . . .
C24 C 0.3037(2) 0.66874(18) 0.76900(16) 0.0587(9) Uani 1 1 d . . . . .
H24A H 0.304985 0.658758 0.806220 0.088 Uiso 1 1 calc R U . . .
H24B H 0.310400 0.628273 0.749567 0.088 Uiso 1 1 calc R U . . .
H24C H 0.247800 0.689242 0.756546 0.088 Uiso 1 1 calc R U . . .
C25 C 0.3665(2) 0.7066(2) 0.65891(15) 0.0643(10) Uani 1 1 d . . . . .
H25A H 0.319347 0.736274 0.645708 0.097 Uiso 1 1 calc R U . . .
H25B H 0.342889 0.662513 0.662239 0.097 Uiso 1 1 calc R U . . .
H25C H 0.411023 0.705723 0.634584 0.097 Uiso 1 1 calc R U . . .
C26 C 0.24972(17) 0.45180(13) 0.55351(10) 0.0327(6) Uani 1 1 d . . . . .
C27 C 0.28367(17) 0.42859(14) 0.60316(10) 0.0337(6) Uani 1 1 d . . . . .
H27 H 0.312152 0.387401 0.605383 0.040 Uiso 1 1 calc R U . . .
C28 C 0.27731(19) 0.46353(16) 0.64939(11) 0.0421(7) Uani 1 1 d . . . . .
H28 H 0.300767 0.445797 0.681955 0.051 Uiso 1 1 calc R U . . .
C29 C 0.2365(2) 0.52425(16) 0.64733(12) 0.0463(7) Uani 1 1 d . . . . .
H29 H 0.232183 0.548460 0.678329 0.056 Uiso 1 1 calc R U . . .
C30 C 0.2024(3) 0.54880(17) 0.59945(14) 0.0577(9) Uani 1 1 d . . . . .
H30 H 0.174678 0.590292 0.597596 0.069 Uiso 1 1 calc R U . . .
C31 C 0.2082(2) 0.51306(16) 0.55362(13) 0.0509(8) Uani 1 1 d . . . . .
H31 H 0.183188 0.530853 0.521406 0.061 Uiso 1 1 calc R U . . .
C32 C 0.16168(17) 0.36088(14) 0.49998(10) 0.0323(6) Uani 1 1 d . . . . .
C33 C 0.1637(2) 0.30295(15) 0.52976(12) 0.0411(7) Uani 1 1 d . . . . .
H33 H 0.217962 0.288970 0.547182 0.049 Uiso 1 1 calc R U . . .
C34 C 0.0897(2) 0.26528(17) 0.53481(14) 0.0550(9) Uani 1 1 d . . . . .
H34 H 0.094479 0.226631 0.555264 0.066 Uiso 1 1 calc R U . . .
C35 C 0.0095(2) 0.2840(2) 0.51016(15) 0.0641(10) Uani 1 1 d . . . . .
H35 H -0.040944 0.258371 0.513297 0.077 Uiso 1 1 calc R U . . .
C36 C 0.0038(2) 0.3405(2) 0.48097(14) 0.0625(11) Uani 1 1 d . . . . .
H36 H -0.051141 0.354012 0.464124 0.075 Uiso 1 1 calc R U . . .
C37 C 0.07880(19) 0.37834(18) 0.47588(12) 0.0461(7) Uani 1 1 d . . . . .
H37 H 0.073062 0.416982 0.455437 0.055 Uiso 1 1 calc R U . . .
B B 0.250000 0.4069(2) 0.500000 0.0298(8) Uani 1 2 d S T P . .
N1 N 0.67942(14) 0.74495(11) 0.77835(10) 0.0368(5) Uani 1 1 d . . . . .
N2 N 0.81797(14) 0.79122(11) 0.76786(10) 0.0368(5) Uani 1 1 d . . . . .
O O 0.52827(12) 0.60888(9) 0.69412(8) 0.0370(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb O 2.3884(18) . ?
Tb N1 2.453(2) . ?
Tb N2 2.485(2) 7_666 ?
Tb C6 2.658(3) . ?
Tb C17 2.661(3) . ?
Tb C7 2.666(3) . ?
Tb C18 2.677(3) . ?
Tb C19 2.685(3) . ?
Tb C16 2.688(3) . ?
Tb C10 2.695(3) . ?
Tb C9 2.713(3) . ?
Tb C8 2.715(3) . ?
C1 N2 1.316(3) . ?
C1 N1 1.322(3) . ?
C1 H1 0.9400 . ?
C2 O 1.443(3) . ?
C2 C3 1.490(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 C4 1.438(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 C5 1.491(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O 1.472(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C10 1.408(4) . ?
C6 C7 1.413(4) . ?
C6 C11 1.504(5) . ?
C7 C8 1.407(4) . ?
C7 C12 1.506(4) . ?
C8 C9 1.403(4) . ?
C8 C13 1.507(4) . ?
C9 C10 1.414(4) . ?
C9 C14 1.507(4) . ?
C10 C15 1.508(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 C17 1.407(5) . ?
C16 C20 1.410(4) . ?
C16 C21 1.509(5) . ?
C17 C18 1.402(5) . ?
C17 C22 1.508(4) . ?
C18 C19 1.421(4) . ?
C18 C23 1.498(5) . ?
C19 C20 1.411(4) . ?
C19 C24 1.501(4) . ?
C20 C25 1.494(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 C31 1.394(4) . ?
C26 C27 1.398(4) . ?
C26 B 1.642(3) . ?
C27 C28 1.389(4) . ?
C27 H27 0.9400 . ?
C28 C29 1.378(5) . ?
C28 H28 0.9400 . ?
C29 C30 1.369(5) . ?
C29 H29 0.9400 . ?
C30 C31 1.388(4) . ?
C30 H30 0.9400 . ?
C31 H31 0.9400 . ?
C32 C37 1.390(4) . ?
C32 C33 1.398(4) . ?
C32 B 1.639(4) . ?
C33 C34 1.381(4) . ?
C33 H33 0.9400 . ?
C34 C35 1.367(5) . ?
C34 H34 0.9400 . ?
C35 C36 1.363(6) . ?
C35 H35 0.9400 . ?
C36 C37 1.396(5) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
N1 N2 1.394(3) 7_666 ?

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
O Tb N1 113.88(7) . . ?
O Tb N2 81.11(7) . 7_666 ?
N1 Tb N2 32.79(7) . 7_666 ?
O Tb C6 128.69(8) . . ?
N1 Tb C6 80.99(9) . . ?
N2 Tb C6 100.85(9) 7_666 . ?
O Tb C17 121.92(9) . . ?
N1 Tb C17 77.67(9) . . ?
N2 Tb C17 95.52(10) 7_666 . ?
C6 Tb C17 109.02(11) . . ?
O Tb C7 102.34(8) . . ?
N1 Tb C7 75.90(9) . . ?
N2 Tb C7 81.23(9) 7_666 . ?
C6 Tb C7 30.78(10) . . ?
C17 Tb C7 134.70(10) . . ?
O Tb C18 123.19(8) . . ?
N1 Tb C18 103.40(9) . . ?
N2 Tb C18 125.83(10) 7_666 . ?
C6 Tb C18 97.30(10) . . ?
C17 Tb C18 30.45(11) . . ?
C7 Tb C18 128.07(10) . . ?
O Tb C19 93.40(8) . . ?
N1 Tb C19 127.95(8) . . ?
N2 Tb C19 135.33(9) 7_666 . ?
C6 Tb C19 116.13(10) . . ?
C17 Tb C19 50.44(9) . . ?
C7 Tb C19 142.46(10) . . ?
C18 Tb C19 30.73(9) . . ?
O Tb C16 91.94(9) . . ?
N1 Tb C16 83.84(9) . . ?
N2 Tb C16 85.44(9) 7_666 . ?
C6 Tb C16 139.34(10) . . ?
C17 Tb C16 30.50(11) . . ?
C7 Tb C16 158.63(10) . . ?
C18 Tb C16 50.35(11) . . ?
C19 Tb C16 50.27(10) . . ?
O Tb C10 116.64(8) . . ?
N1 Tb C10 110.98(9) . . ?
N2 Tb C10 129.89(9) 7_666 . ?
C6 Tb C10 30.48(9) . . ?
C17 Tb C10 109.42(11) . . ?
C7 Tb C10 50.21(9) . . ?
C18 Tb C10 85.11(11) . . ?
C19 Tb C10 92.27(10) . . ?
C16 Tb C10 135.45(10) . . ?
O Tb C9 86.54(8) . . ?
N1 Tb C9 125.51(9) . . ?
N2 Tb C9 125.38(8) 7_666 . ?
C6 Tb C9 50.32(9) . . ?
C17 Tb C9 134.67(11) . . ?
C7 Tb C9 49.95(9) . . ?
C18 Tb C9 105.35(11) . . ?
C19 Tb C9 98.18(10) . . ?
C16 Tb C9 148.31(9) . . ?
C10 Tb C9 30.31(9) . . ?
O Tb C8 78.32(8) . . ?
N1 Tb C8 102.36(9) . . ?
N2 Tb C8 95.48(9) 7_666 . ?
C6 Tb C8 50.38(9) . . ?
C17 Tb C8 158.29(11) . . ?
C7 Tb C8 30.31(9) . . ?
C18 Tb C8 133.81(11) . . ?
C19 Tb C8 126.97(10) . . ?
C16 Tb C8 169.92(10) . . ?
C10 Tb C8 49.86(9) . . ?
C9 Tb C8 29.95(9) . . ?
N2 C1 N1 126.4(3) . . ?
N2 C1 H1 116.8 . . ?
N1 C1 H1 116.8 . . ?
O C2 C3 105.9(3) . . ?
O C2 H2A 110.6 . . ?
C3 C2 H2A 110.6 . . ?
O C2 H2B 110.6 . . ?
C3 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
C4 C3 C2 105.3(3) . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3B 110.7 . . ?
C2 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
C3 C4 C5 105.5(3) . . ?
C3 C4 H4A 110.6 . . ?
C5 C4 H4A 110.6 . . ?
C3 C4 H4B 110.6 . . ?
C5 C4 H4B 110.6 . . ?
H4A C4 H4B 108.8 . . ?
O C5 C4 105.3(2) . . ?
O C5 H5A 110.7 . . ?
C4 C5 H5A 110.7 . . ?
O C5 H5B 110.7 . . ?
C4 C5 H5B 110.7 . . ?
H5A C5 H5B 108.8 . . ?
C10 C6 C7 107.5(3) . . ?
C10 C6 C11 126.2(3) . . ?
C7 C6 C11 126.1(3) . . ?
C10 C6 Tb 76.22(18) . . ?
C7 C6 Tb 74.94(18) . . ?
C11 C6 Tb 118.2(2) . . ?
C8 C7 C6 108.4(3) . . ?
C8 C7 C12 124.9(3) . . ?
C6 C7 C12 126.1(3) . . ?
C8 C7 Tb 76.76(17) . . ?
C6 C7 Tb 74.29(18) . . ?
C12 C7 Tb 122.2(2) . . ?
C9 C8 C7 107.9(3) . . ?
C9 C8 C13 127.3(3) . . ?
C7 C8 C13 124.5(3) . . ?
C9 C8 Tb 74.97(17) . . ?
C7 C8 Tb 72.93(17) . . ?
C13 C8 Tb 123.2(2) . . ?
C8 C9 C10 108.1(3) . . ?
C8 C9 C14 127.1(3) . . ?
C10 C9 C14 123.7(3) . . ?
C8 C9 Tb 75.08(17) . . ?
C10 C9 Tb 74.12(18) . . ?
C14 C9 Tb 126.3(2) . . ?
C6 C10 C9 108.1(3) . . ?
C6 C10 C15 126.5(3) . . ?
C9 C10 C15 123.8(3) . . ?
C6 C10 Tb 73.30(18) . . ?
C9 C10 Tb 75.57(18) . . ?
C15 C10 Tb 128.6(2) . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C20 107.9(3) . . ?
C17 C16 C21 126.5(3) . . ?
C20 C16 C21 125.3(3) . . ?
C17 C16 Tb 73.69(18) . . ?
C20 C16 Tb 75.94(18) . . ?
C21 C16 Tb 121.1(2) . . ?
C18 C17 C16 108.7(3) . . ?
C18 C17 C22 124.7(4) . . ?
C16 C17 C22 126.1(4) . . ?
C18 C17 Tb 75.41(17) . . ?
C16 C17 Tb 75.81(17) . . ?
C22 C17 Tb 121.6(2) . . ?
C17 C18 C19 107.6(3) . . ?
C17 C18 C23 124.5(3) . . ?
C19 C18 C23 126.5(3) . . ?
C17 C18 Tb 74.13(17) . . ?
C19 C18 Tb 74.95(15) . . ?
C23 C18 Tb 127.2(2) . . ?
C20 C19 C18 107.9(3) . . ?
C20 C19 C24 125.1(3) . . ?
C18 C19 C24 126.5(3) . . ?
C20 C19 Tb 76.03(15) . . ?
C18 C19 Tb 74.32(15) . . ?
C24 C19 Tb 122.0(2) . . ?
C16 C20 C19 107.9(3) . . ?
C16 C20 C25 124.8(3) . . ?
C19 C20 C25 126.4(3) . . ?
C16 C20 Tb 73.79(16) . . ?
C19 C20 Tb 73.67(16) . . ?
C25 C20 Tb 126.9(2) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C31 C26 C27 114.9(3) . . ?
C31 C26 B 122.6(3) . . ?
C27 C26 B 122.3(2) . . ?
C28 C27 C26 123.1(3) . . ?
C28 C27 H27 118.5 . . ?
C26 C27 H27 118.5 . . ?
C29 C28 C27 119.8(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C30 C29 C28 119.0(3) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
C29 C30 C31 120.7(3) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C30 C31 C26 122.6(3) . . ?
C30 C31 H31 118.7 . . ?
C26 C31 H31 118.7 . . ?
C37 C32 C33 114.8(3) . . ?
C37 C32 B 124.3(3) . . ?
C33 C32 B 120.6(2) . . ?
C34 C33 C32 123.1(3) . . ?
C34 C33 H33 118.4 . . ?
C32 C33 H33 118.4 . . ?
C35 C34 C33 120.2(3) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C36 C35 C34 119.1(3) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C35 C36 C37 120.6(3) . . ?
C35 C36 H36 119.7 . . ?
C37 C36 H36 119.7 . . ?
C32 C37 C36 122.3(3) . . ?
C32 C37 H37 118.9 . . ?
C36 C37 H37 118.9 . . ?
C32 B C32 110.6(3) . 2_556 ?
C32 B C26 103.77(13) . . ?
C32 B C26 113.12(13) 2_556 . ?
C32 B C26 113.12(13) . 2_556 ?
C32 B C26 103.77(13) 2_556 2_556 ?
C26 B C26 112.7(3) . 2_556 ?
C1 N1 N2 116.9(2) . 7_666 ?
C1 N1 Tb 167.6(2) . . ?
N2 N1 Tb 74.91(13) 7_666 . ?
C1 N2 N1 116.7(2) . 7_666 ?
C1 N2 Tb 170.29(19) . 7_666 ?
N1 N2 Tb 72.30(13) 7_666 7_666 ?
C2 O C5 108.4(2) . . ?
C2 O Tb 126.70(17) . . ?
C5 O Tb 124.46(16) . . ?

# start Validation Reply Form

_vrf_PLAT606_Tb2                 
;
RESPONSE: The structure contains an area of disordered 
solvent involving two diethyl ether (Et2O) molecules; 
attempts to model it with a chemically reasonable geometry were unsuccessful. 
Therefore, the SQUEEZE procedure of PLATON (A.L.Spek (2015) Acta Cryst. C71, 
9-18) was employed to remove the contribution of the electron 
density associated with those solvent molecules from the intensity 
data. The solvent-free model and intensity data were used for the 
final results reported here.  
;
_vrf_PLAT869_Tb2                 
; 
RESPONSE:See comment above.
;
# end Validation Reply Form



_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
