# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1555475'
_audit_update_record             
;
2017-06-10 deposited with the CCDC.
2018-05-28 downloaded from the CCDC.
;
_audit_creation_date             2017-06-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C96 H60 N4 O32 Sm4), H2 O, 2(C2 H8 N)'
_chemical_formula_sum            'C52 H48 N4 O17 Sm2'
_chemical_formula_weight         1301.66
_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 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1890 4.4100 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   15.709(3)
_cell_length_b                   9.8734(16)
_cell_length_c                   21.052(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.544(4)
_cell_angle_gamma                90
_cell_volume                     3113.3(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8163
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.931
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38583
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         3.320
_diffrn_ambient_temperature      113.3
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_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                6151
_reflns_number_total             7186
_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       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         4.073
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7121
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0350
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1224
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-H9
 0.8 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C17(H17a,H17b), N2(H2a,H2b)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C16(H16), C23(H23), C15(H15), C24(H24), C3(H3), C11(H11), C19(H19),
 C12(H12), C6(H6), C20(H20)
4.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C26(H26a,H26b,H26c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
Sm1 Sm 0.39377(2) 0.04142(2) 0.53433(2) 0.01179(9) Uani 1 1 d . . . . .
O1 O 0.39133(16) 0.1697(3) 0.43773(12) 0.0146(5) Uani 1 1 d . . . . .
O8 O 0.50975(16) 0.7793(3) 0.40917(13) 0.0173(5) Uani 1 1 d . . . . .
O7 O 0.43062(17) 0.8842(3) 0.46447(13) 0.0173(5) Uani 1 1 d . . . . .
O2 O 0.49366(17) 0.0908(3) 0.39338(13) 0.0182(6) Uani 1 1 d . . . . .
O5 O -0.23817(18) 0.0305(3) 0.04247(15) 0.0185(6) Uani 1 1 d . . . . .
O3 O 0.37617(18) -0.0522(2) 0.14914(14) 0.0140(5) Uani 1 1 d . . . . .
O6 O -0.27484(16) 0.2083(3) -0.02356(13) 0.0193(6) Uani 1 1 d . . . . .
O4 O 0.31326(18) 0.1209(3) 0.08644(13) 0.0193(6) Uani 1 1 d . . . . .
N1 N 0.15648(19) 0.3666(3) 0.23603(15) 0.0130(6) Uani 1 1 d . . . . .
C9 C 0.1097(2) 0.4181(4) 0.16875(18) 0.0130(7) Uani 1 1 d . . . . .
H9A H 0.1505 0.4152 0.1421 0.016 Uiso 1 1 calc R . . . .
H9B H 0.0939 0.5121 0.1723 0.016 Uiso 1 1 calc R . . . .
C22 C 0.4378(2) 0.7979(4) 0.42173(18) 0.0139(7) Uani 1 1 d . . . . .
C8 C 0.2831(2) 0.2469(4) 0.30998(18) 0.0119(7) Uani 1 1 d . . . . .
H8 H 0.2708 0.2843 0.3468 0.014 Uiso 1 1 calc R . . . .
C5 C 0.3373(2) 0.0599(4) 0.14256(19) 0.0136(7) Uani 1 1 d . . . . .
C10 C 0.0262(2) 0.3405(4) 0.13272(18) 0.0135(7) Uani 1 1 d . . . . .
C1 C 0.4182(2) 0.1400(4) 0.38918(17) 0.0131(7) Uani 1 1 d . . . . .
C16 C -0.0293(3) 0.3970(4) 0.0735(2) 0.0200(8) Uani 1 1 d . . . . .
H16 H -0.0126 0.4775 0.0576 0.024 Uiso 1 1 calc R . . . .
C18 C 0.2173(2) 0.5439(3) 0.3217(2) 0.0112(7) Uani 1 1 d . . . . .
C17 C 0.1440(2) 0.4419(3) 0.29125(19) 0.0125(7) Uani 1 1 d . . . . .
H17A H 0.1405 0.3785 0.3256 0.015 Uiso 1 1 calc R . . . .
H17B H 0.0875 0.4894 0.2762 0.015 Uiso 1 1 calc R . . . .
C14 C -0.2203(2) 0.1460(4) 0.02516(18) 0.0159(7) Uani 1 1 d . . . . .
C7 C 0.2276(2) 0.2766(3) 0.24584(17) 0.0112(6) Uani 1 1 d . . . . .
C23 C 0.3517(3) 0.6642(4) 0.3237(2) 0.0211(8) Uani 1 1 d . . . . .
H23 H 0.3951 0.6850 0.3034 0.025 Uiso 1 1 calc R . . . .
C2 C 0.3564(2) 0.1622(4) 0.31931(17) 0.0121(7) Uani 1 1 d . . . . .
C13 C -0.1343(2) 0.2121(4) 0.06149(18) 0.0161(7) Uani 1 1 d . . . . .
C15 C -0.1086(2) 0.3344(5) 0.03845(18) 0.0213(9) Uani 1 1 d . . . . .
H15 H -0.1449 0.3735 -0.0005 0.026 Uiso 1 1 calc R . . . .
C21 C 0.3577(2) 0.7166(4) 0.38531(18) 0.0130(7) Uani 1 1 d . . . . .
C24 C 0.2812(3) 0.5804(4) 0.2917(2) 0.0212(8) Uani 1 1 d . . . . .
H24 H 0.2766 0.5481 0.2493 0.025 Uiso 1 1 calc R . . . .
C3 C 0.3754(2) 0.1006(4) 0.26553(17) 0.0138(7) Uani 1 1 d . . . . .
H3 H 0.4249 0.0447 0.2722 0.017 Uiso 1 1 calc R . . . .
C11 C 0.0011(2) 0.2197(4) 0.15568(19) 0.0158(7) Uani 1 1 d . . . . .
H11 H 0.0375 0.1808 0.1947 0.019 Uiso 1 1 calc R . . . .
C19 C 0.2226(3) 0.6006(5) 0.3827(2) 0.0295(10) Uani 1 1 d . . . . .
H19 H 0.1793 0.5795 0.4031 0.035 Uiso 1 1 calc R . . . .
C4 C 0.3183(2) 0.1247(4) 0.20136(17) 0.0125(6) Uani 1 1 d . . . . .
C12 C -0.0787(2) 0.1563(4) 0.12032(19) 0.0170(7) Uani 1 1 d . . . . .
H12 H -0.0950 0.0757 0.1363 0.020 Uiso 1 1 calc R . . . .
C6 C 0.2459(2) 0.2126(4) 0.19175(17) 0.0137(7) Uani 1 1 d . . . . .
H6 H 0.2090 0.2290 0.1488 0.016 Uiso 1 1 calc R . . . .
C20 C 0.2913(3) 0.6884(5) 0.4140(2) 0.0309(11) Uani 1 1 d . . . . .
H20 H 0.2927 0.7283 0.4543 0.037 Uiso 1 1 calc R . . . .
O9 O 0.5000 0.7761(4) 0.2500 0.0208(8) Uani 1 2 d DS TU P . .
H9 H 0.531(3) 0.817(5) 0.2815(18) 0.041(15) Uiso 1 1 d D . . . .
C25 C 0.5485(10) 0.4527(8) 0.4282(7) 0.129(6) Uani 1 1 d . . . . .
H25A H 0.5032 0.4909 0.3911 0.193 Uiso 1 1 calc GR . . . .
H25B H 0.5329 0.4674 0.4684 0.193 Uiso 1 1 calc GR . . . .
H25C H 0.5531 0.3572 0.4213 0.193 Uiso 1 1 calc GR . . . .
N2 N 0.6529(7) 0.5318(9) 0.4352(5) 0.112(3) Uani 1 1 d . U . . .
H2A H 0.6478 0.6107 0.4542 0.134 Uiso 1 1 calc R . . . .
H2B H 0.6907 0.4837 0.4673 0.134 Uiso 1 1 calc R . . . .
C26 C 0.7086(8) 0.5682(9) 0.3914(5) 0.098(3) Uani 1 1 d . U . . .
H26A H 0.6712 0.5750 0.3461 0.147 Uiso 1 1 calc GR . . . .
H26B H 0.7529 0.4994 0.3947 0.147 Uiso 1 1 calc GR . . . .
H26C H 0.7375 0.6535 0.4054 0.147 Uiso 1 1 calc GR . . . .


_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
Sm1 O1 2.386(2) . ?
Sm1 O8 2.400(3) 3_666 ?
Sm1 O7 2.328(3) 1_545 ?
Sm1 O7 2.848(3) 3_666 ?
Sm1 O2 2.351(3) 3_656 ?
Sm1 O5 2.494(3) 2 ?
Sm1 O3 2.516(3) 4_556 ?
Sm1 O6 2.450(3) 2 ?
Sm1 O4 2.492(3) 4_556 ?
Sm1 C5 2.863(4) 4_556 ?
Sm1 C14 2.829(4) 2 ?
O1 C1 1.253(4) . ?
O8 Sm1 2.400(3) 3_666 ?
O8 C22 1.250(4) . ?
O7 Sm1 2.329(3) 1_565 ?
O7 Sm1 2.848(3) 3_666 ?
O7 C22 1.268(4) . ?
O2 Sm1 2.351(3) 3_656 ?
O2 C1 1.259(4) . ?
O5 Sm1 2.494(3) 2 ?
O5 C14 1.255(5) . ?
O3 Sm1 2.516(3) 4 ?
O3 C5 1.252(4) . ?
O6 Sm1 2.450(3) 2 ?
O6 C14 1.279(5) . ?
O4 Sm1 2.491(3) 4 ?
O4 C5 1.277(5) . ?
N1 C9 1.475(5) . ?
N1 C17 1.442(5) . ?
N1 C7 1.393(4) . ?
C9 C10 1.511(5) . ?
C22 C21 1.494(5) . ?
C8 C7 1.400(5) . ?
C8 C2 1.387(5) . ?
C5 Sm1 2.863(4) 4 ?
C5 C4 1.501(5) . ?
C10 C16 1.403(5) . ?
C10 C11 1.388(5) . ?
C1 C2 1.515(5) . ?
C16 C15 1.388(5) . ?
C18 C17 1.518(5) . ?
C18 C24 1.385(5) . ?
C18 C19 1.381(5) . ?
C14 Sm1 2.829(4) 2 ?
C14 C13 1.488(5) . ?
C7 C6 1.406(5) . ?
C23 C21 1.374(5) . ?
C23 C24 1.384(5) . ?
C2 C3 1.394(5) . ?
C13 C15 1.405(6) . ?
C13 C12 1.396(5) . ?
C21 C20 1.383(5) . ?
C3 C4 1.398(5) . ?
C11 C12 1.398(5) . ?
C19 C20 1.386(6) . ?
C4 C6 1.397(5) . ?
C25 N2 1.783(16) . ?
N2 C26 1.493(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sm1 O8 82.89(9) . 3_666 ?
O1 Sm1 O7 68.73(8) . 3_666 ?
O1 Sm1 O5 73.12(9) . 2 ?
O1 Sm1 O3 144.87(8) . 4_556 ?
O1 Sm1 O6 75.41(9) . 2 ?
O1 Sm1 O4 146.80(9) . 4_556 ?
O1 Sm1 C5 159.14(9) . 4_556 ?
O1 Sm1 C14 70.31(9) . 2 ?
O8 Sm1 O7 48.69(8) 3_666 3_666 ?
O8 Sm1 O5 134.64(9) 3_666 2 ?
O8 Sm1 O3 74.25(8) 3_666 4_556 ?
O8 Sm1 O6 84.25(9) 3_666 2 ?
O8 Sm1 O4 125.79(9) 3_666 4_556 ?
O8 Sm1 C5 99.45(10) 3_666 4_556 ?
O8 Sm1 C14 109.29(10) 3_666 2 ?
O7 Sm1 O1 76.04(9) 1_545 . ?
O7 Sm1 O8 124.38(9) 1_545 3_666 ?
O7 Sm1 O7 75.69(9) 1_545 3_666 ?
O7 Sm1 O2 75.92(9) 1_545 3_656 ?
O7 Sm1 O5 86.74(9) 1_545 2 ?
O7 Sm1 O3 139.04(9) 1_545 4_556 ?
O7 Sm1 O6 135.88(9) 1_545 2 ?
O7 Sm1 O4 96.03(9) 1_545 4_556 ?
O7 Sm1 C5 117.73(10) 1_545 4_556 ?
O7 Sm1 C5 127.94(9) 3_666 4_556 ?
O7 Sm1 C14 110.70(10) 1_545 2 ?
O2 Sm1 O1 131.47(9) 3_656 . ?
O2 Sm1 O8 81.34(9) 3_656 3_666 ?
O2 Sm1 O7 66.41(9) 3_656 3_666 ?
O2 Sm1 O5 142.63(9) 3_656 2 ?
O2 Sm1 O3 71.38(9) 3_656 4_556 ?
O2 Sm1 O6 146.87(9) 3_656 2 ?
O2 Sm1 O4 74.94(9) 3_656 4_556 ?
O2 Sm1 C5 69.13(9) 3_656 4_556 ?
O2 Sm1 C14 157.76(10) 3_656 2 ?
O5 Sm1 O7 140.76(9) 2 3_666 ?
O5 Sm1 O3 104.75(9) 2 4_556 ?
O5 Sm1 C5 91.30(10) 2 4_556 ?
O5 Sm1 C14 26.32(10) 2 2 ?
O3 Sm1 O7 111.54(8) 4_556 3_666 ?
O3 Sm1 C5 25.89(9) 4_556 4_556 ?
O3 Sm1 C14 92.28(10) 4_556 2 ?
O6 Sm1 O7 122.48(9) 2 3_666 ?
O6 Sm1 O5 52.99(9) 2 2 ?
O6 Sm1 O3 76.05(8) 2 4_556 ?
O6 Sm1 O4 89.97(10) 2 4_556 ?
O6 Sm1 C5 84.16(10) 2 4_556 ?
O6 Sm1 C14 26.82(10) 2 2 ?
O4 Sm1 O7 141.35(8) 4_556 3_666 ?
O4 Sm1 O5 74.29(9) 4_556 2 ?
O4 Sm1 O3 52.20(8) 4_556 4_556 ?
O4 Sm1 C5 26.46(10) 4_556 4_556 ?
O4 Sm1 C14 83.15(10) 4_556 2 ?
C14 Sm1 O7 135.33(9) 2 3_666 ?
C14 Sm1 C5 89.53(10) 2 4_556 ?
C1 O1 Sm1 130.4(2) . . ?
C22 O8 Sm1 105.3(2) . 3_666 ?
Sm1 O7 Sm1 104.31(9) 1_565 3_666 ?
C22 O7 Sm1 171.1(2) . 1_565 ?
C22 O7 Sm1 83.5(2) . 3_666 ?
C1 O2 Sm1 140.2(2) . 3_656 ?
C14 O5 Sm1 91.9(2) . 2 ?
C5 O3 Sm1 92.7(2) . 4 ?
C14 O6 Sm1 93.3(2) . 2 ?
C5 O4 Sm1 93.2(2) . 4 ?
C17 N1 C9 116.6(3) . . ?
C7 N1 C9 120.5(3) . . ?
C7 N1 C17 120.4(3) . . ?
N1 C9 C10 114.4(3) . . ?
O8 C22 O7 121.9(3) . . ?
O8 C22 C21 119.2(3) . . ?
O7 C22 C21 119.0(3) . . ?
C2 C8 C7 120.8(3) . . ?
O3 C5 Sm1 61.39(19) . 4 ?
O3 C5 O4 121.2(3) . . ?
O3 C5 C4 119.8(3) . . ?
O4 C5 Sm1 60.32(19) . 4 ?
O4 C5 C4 119.0(3) . . ?
C4 C5 Sm1 172.5(2) . 4 ?
C16 C10 C9 117.2(3) . . ?
C11 C10 C9 123.7(3) . . ?
C11 C10 C16 119.1(3) . . ?
O1 C1 O2 125.1(3) . . ?
O1 C1 C2 118.9(3) . . ?
O2 C1 C2 116.0(3) . . ?
C15 C16 C10 120.9(4) . . ?
C24 C18 C17 122.8(3) . . ?
C19 C18 C17 119.1(3) . . ?
C19 C18 C24 118.1(3) . . ?
N1 C17 C18 114.4(3) . . ?
O5 C14 Sm1 61.76(19) . 2 ?
O5 C14 O6 121.1(3) . . ?
O5 C14 C13 119.8(3) . . ?
O6 C14 Sm1 59.83(18) . 2 ?
O6 C14 C13 119.1(3) . . ?
C13 C14 Sm1 172.8(2) . 2 ?
N1 C7 C8 121.1(3) . . ?
N1 C7 C6 121.2(3) . . ?
C8 C7 C6 117.8(3) . . ?
C21 C23 C24 120.2(3) . . ?
C8 C2 C1 119.1(3) . . ?
C8 C2 C3 121.3(3) . . ?
C3 C2 C1 119.6(3) . . ?
C15 C13 C14 120.7(3) . . ?
C12 C13 C14 120.8(3) . . ?
C12 C13 C15 118.5(3) . . ?
C16 C15 C13 120.3(4) . . ?
C23 C21 C22 119.7(3) . . ?
C23 C21 C20 119.4(3) . . ?
C20 C21 C22 120.9(3) . . ?
C23 C24 C18 121.1(4) . . ?
C2 C3 C4 118.6(3) . . ?
C10 C11 C12 120.1(3) . . ?
C18 C19 C20 121.0(3) . . ?
C3 C4 C5 119.7(3) . . ?
C6 C4 C5 120.1(3) . . ?
C6 C4 C3 120.1(3) . . ?
C13 C12 C11 121.1(4) . . ?
C4 C6 C7 121.3(3) . . ?
C21 C20 C19 120.0(4) . . ?
C26 N2 C25 138.6(10) . . ?

_platon_squeeze_details          
;

;
_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_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1555477'
_audit_update_record             
;
2017-06-10 deposited with the CCDC.
2018-05-28 downloaded from the CCDC.
;
_audit_creation_date             2017-06-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C96 H60 Dy4 N4 O32), H2 O, 2(C2 H8 N)'
_chemical_formula_sum            'C52 H48 Dy2 N4 O17'
_chemical_formula_weight         1325.94
_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 0.0030 0.0020 '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 -0.1890 4.4100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   15.7583(13)
_cell_length_b                   9.7867(10)
_cell_length_c                   20.9550(18)
_cell_angle_alpha                90
_cell_angle_beta                 108.100(3)
_cell_angle_gamma                90
_cell_volume                     3071.8(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8163
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32361
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_min         3.024
_diffrn_ambient_temperature      113.3
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_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                6370
_reflns_number_total             7094
_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       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         3.309
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7014
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0298
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+6.7100P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0896
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-H9
 0.8 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C17(H17a,H17b), N2(H2a,H2b)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C16(H16), C23(H23), C15(H15), C24(H24), C3(H3), C11(H11), C19(H19),
 C12(H12), C6(H6), C20(H20)
4.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C26(H26a,H26b,H26c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.39557(2) 0.04476(2) 0.53369(2) 0.01114(6) Uani 1 1 d . . . . .
O1 O 0.39089(15) 0.1670(3) 0.43606(12) 0.0187(5) Uani 1 1 d . . . . .
O8 O 0.50881(15) 0.7775(3) 0.41221(12) 0.0198(5) Uani 1 1 d . . . . .
O7 O 0.42873(16) 0.8828(2) 0.46696(12) 0.0202(5) Uani 1 1 d . . . . .
O2 O 0.49124(16) 0.0799(3) 0.39158(12) 0.0223(5) Uani 1 1 d . . . . .
O5 O -0.24174(16) 0.0343(2) 0.03995(14) 0.0228(5) Uani 1 1 d . . . . .
O3 O 0.37490(16) -0.0581(2) 0.14554(13) 0.0182(5) Uani 1 1 d . . . . .
O6 O -0.28234(15) 0.2180(3) -0.02324(12) 0.0225(5) Uani 1 1 d . . . . .
O4 O 0.31860(17) 0.1220(3) 0.08435(12) 0.0228(5) Uani 1 1 d . . . . .
N1 N 0.15661(17) 0.3654(3) 0.23145(14) 0.0157(5) Uani 1 1 d . . . . .
C9 C 0.1109(2) 0.4185(3) 0.16476(18) 0.0176(6) Uani 1 1 d . . . . .
H9A H 0.1507 0.4120 0.1377 0.021 Uiso 1 1 calc R . . . .
H9B H 0.0979 0.5145 0.1686 0.021 Uiso 1 1 calc R . . . .
C22 C 0.4359(2) 0.7977(3) 0.42348(16) 0.0165(6) Uani 1 1 d . . . . .
C8 C 0.2821(2) 0.2433(3) 0.30748(16) 0.0144(6) Uani 1 1 d . . . . .
H8 H 0.2698 0.2816 0.3442 0.017 Uiso 1 1 calc R . . . .
C5 C 0.3383(2) 0.0570(3) 0.13973(17) 0.0154(6) Uani 1 1 d . . . . .
C10 C 0.0241(2) 0.3447(3) 0.12863(17) 0.0162(6) Uani 1 1 d . . . . .
C1 C 0.4169(2) 0.1330(3) 0.38743(16) 0.0169(6) Uani 1 1 d . . . . .
C16 C -0.0335(2) 0.4039(4) 0.07108(18) 0.0215(7) Uani 1 1 d . . . . .
H16 H -0.0177 0.4857 0.0553 0.026 Uiso 1 1 calc R . . . .
C18 C 0.2158(2) 0.5440(3) 0.31850(19) 0.0164(7) Uani 1 1 d . . . . .
C17 C 0.1437(2) 0.4398(3) 0.28712(19) 0.0182(7) Uani 1 1 d . . . . .
H17A H 0.1409 0.3750 0.3214 0.022 Uiso 1 1 calc R . . . .
H17B H 0.0866 0.4865 0.2718 0.022 Uiso 1 1 calc R . . . .
C14 C -0.2254(2) 0.1526(4) 0.02369(17) 0.0191(7) Uani 1 1 d . . . . .
C7 C 0.22654(19) 0.2735(3) 0.24161(16) 0.0135(6) Uani 1 1 d . . . . .
C23 C 0.3545(2) 0.6567(3) 0.32510(18) 0.0198(7) Uani 1 1 d . . . . .
H23 H 0.4008 0.6724 0.3072 0.024 Uiso 1 1 calc R . . . .
C2 C 0.3550(2) 0.1564(3) 0.31737(16) 0.0151(6) Uani 1 1 d . . . . .
C13 C -0.1382(2) 0.2189(4) 0.05979(17) 0.0181(6) Uani 1 1 d . . . . .
C15 C -0.1140(2) 0.3428(4) 0.03703(18) 0.0241(8) Uani 1 1 d . . . . .
H15 H -0.1521 0.3842 -0.0011 0.029 Uiso 1 1 calc R . . . .
C21 C 0.3563(2) 0.7166(3) 0.38510(17) 0.0164(6) Uani 1 1 d . . . . .
C24 C 0.2838(2) 0.5731(4) 0.29141(19) 0.0220(7) Uani 1 1 d . . . . .
H24 H 0.2819 0.5359 0.2501 0.026 Uiso 1 1 calc R . . . .
C3 C 0.3732(2) 0.0937(3) 0.26334(16) 0.0159(6) Uani 1 1 d . . . . .
H3 H 0.4216 0.0347 0.2705 0.019 Uiso 1 1 calc R . . . .
C11 C 0.0001(2) 0.2218(3) 0.15148(17) 0.0187(6) Uani 1 1 d . . . . .
H11 H 0.0379 0.1814 0.1900 0.022 Uiso 1 1 calc R . . . .
C19 C 0.2157(2) 0.6100(4) 0.3769(2) 0.0276(8) Uani 1 1 d . . . . .
H19 H 0.1688 0.5956 0.3943 0.033 Uiso 1 1 calc R . . . .
C4 C 0.3179(2) 0.1206(3) 0.19838(16) 0.0151(6) Uani 1 1 d . . . . .
C12 C -0.0805(2) 0.1587(4) 0.11703(18) 0.0193(7) Uani 1 1 d . . . . .
H12 H -0.0957 0.0760 0.1324 0.023 Uiso 1 1 calc R . . . .
C6 C 0.2458(2) 0.2098(3) 0.18766(16) 0.0159(6) Uani 1 1 d . . . . .
H6 H 0.2099 0.2275 0.1440 0.019 Uiso 1 1 calc R . . . .
C20 C 0.2852(2) 0.6979(4) 0.4101(2) 0.0288(9) Uani 1 1 d . . . . .
H20 H 0.2838 0.7436 0.4486 0.035 Uiso 1 1 calc R . . . .
O9 O 0.5000 0.7698(4) 0.2500 0.0263(8) Uani 1 2 d DS T P . .
H9 H 0.527(3) 0.817(4) 0.2812(17) 0.040(14) Uiso 1 1 d D . . . .
C25 C 0.5596(6) 0.4416(6) 0.4366(5) 0.089(3) Uani 1 1 d . . . . .
H25A H 0.5090 0.4955 0.4123 0.134 Uiso 1 1 calc GR . . . .
H25B H 0.5602 0.4320 0.4824 0.134 Uiso 1 1 calc GR . . . .
H25C H 0.5558 0.3530 0.4164 0.134 Uiso 1 1 calc GR . . . .
N2 N 0.6511(7) 0.5171(10) 0.4348(5) 0.133(3) Uani 1 1 d . U . . .
H2A H 0.6943 0.4560 0.4507 0.159 Uiso 1 1 calc R . . . .
H2B H 0.6608 0.5830 0.4656 0.159 Uiso 1 1 calc R . . . .
C26 C 0.6720(9) 0.5878(15) 0.3690(5) 0.164(5) Uani 1 1 d . U . . .
H26A H 0.6307 0.5530 0.3283 0.246 Uiso 1 1 calc GR . . . .
H26B H 0.7319 0.5661 0.3701 0.246 Uiso 1 1 calc GR . . . .
H26C H 0.6655 0.6852 0.3706 0.246 Uiso 1 1 calc GR . . . .


_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 O1 2.352(2) . ?
Dy1 O8 2.350(2) 3_666 ?
Dy1 O7 2.279(2) 1_545 ?
Dy1 O7 2.862(2) 3_666 ?
Dy1 O2 2.321(2) 3_656 ?
Dy1 O5 2.438(2) 2 ?
Dy1 O3 2.468(2) 4_556 ?
Dy1 O6 2.422(2) 2 ?
Dy1 O4 2.462(2) 4_556 ?
Dy1 C5 2.827(3) 4_556 ?
Dy1 C14 2.783(3) 2 ?
O1 C1 1.256(4) . ?
O8 Dy1 2.350(2) 3_666 ?
O8 C22 1.258(4) . ?
O7 Dy1 2.279(2) 1_565 ?
O7 Dy1 2.862(2) 3_666 ?
O7 C22 1.265(4) . ?
O2 Dy1 2.321(2) 3_656 ?
O2 C1 1.259(4) . ?
O5 Dy1 2.438(2) 2 ?
O5 C14 1.256(4) . ?
O3 Dy1 2.468(2) 4 ?
O3 C5 1.255(4) . ?
O6 Dy1 2.422(2) 2 ?
O6 C14 1.278(4) . ?
O4 Dy1 2.462(2) 4 ?
O4 C5 1.274(4) . ?
N1 C9 1.455(4) . ?
N1 C17 1.442(4) . ?
N1 C7 1.386(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.523(4) . ?
C22 C21 1.491(4) . ?
C8 H8 0.9300 . ?
C8 C7 1.417(4) . ?
C8 C2 1.391(4) . ?
C5 Dy1 2.827(3) 4 ?
C5 C4 1.499(4) . ?
C10 C16 1.391(5) . ?
C10 C11 1.390(5) . ?
C1 C2 1.507(4) . ?
C16 H16 0.9300 . ?
C16 C15 1.383(5) . ?
C18 C17 1.517(4) . ?
C18 C24 1.389(5) . ?
C18 C19 1.385(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C14 Dy1 2.783(3) 2 ?
C14 C13 1.496(4) . ?
C7 C6 1.405(4) . ?
C23 H23 0.9300 . ?
C23 C21 1.380(5) . ?
C23 C24 1.386(5) . ?
C2 C3 1.395(4) . ?
C13 C15 1.399(5) . ?
C13 C12 1.391(5) . ?
C15 H15 0.9300 . ?
C21 C20 1.389(5) . ?
C24 H24 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.395(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.394(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.396(5) . ?
C4 C6 1.394(4) . ?
C12 H12 0.9300 . ?
C6 H6 0.9300 . ?
C20 H20 0.9300 . ?
O9 H9 0.807(10) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25 N2 1.631(12) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C26 1.664(14) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O7 68.82(7) . 3_666 ?
O1 Dy1 O5 73.40(8) . 2 ?
O1 Dy1 O3 145.25(8) . 4_556 ?
O1 Dy1 O6 75.04(8) . 2 ?
O1 Dy1 O4 145.69(8) . 4_556 ?
O1 Dy1 C5 158.72(8) . 4_556 ?
O1 Dy1 C14 70.46(9) . 2 ?
O8 Dy1 O1 83.40(9) 3_666 . ?
O8 Dy1 O7 48.90(7) 3_666 3_666 ?
O8 Dy1 O5 134.34(8) 3_666 2 ?
O8 Dy1 O3 75.92(8) 3_666 4_556 ?
O8 Dy1 O6 82.48(8) 3_666 2 ?
O8 Dy1 O4 127.65(8) 3_666 4_556 ?
O8 Dy1 C5 101.26(9) 3_666 4_556 ?
O8 Dy1 C14 108.36(10) 3_666 2 ?
O7 Dy1 O1 76.78(8) 1_545 . ?
O7 Dy1 O8 125.18(8) 1_545 3_666 ?
O7 Dy1 O7 76.29(8) 1_545 3_666 ?
O7 Dy1 O2 76.92(9) 1_545 3_656 ?
O7 Dy1 O5 87.41(9) 1_545 2 ?
O7 Dy1 O3 137.95(8) 1_545 4_556 ?
O7 Dy1 O6 137.25(8) 1_545 2 ?
O7 Dy1 O4 92.35(9) 1_545 4_556 ?
O7 Dy1 C5 115.29(9) 1_545 4_556 ?
O7 Dy1 C14 111.86(10) 1_545 2 ?
O2 Dy1 O1 131.63(8) 3_656 . ?
O2 Dy1 O8 79.67(9) 3_656 3_666 ?
O2 Dy1 O7 65.90(8) 3_656 3_666 ?
O2 Dy1 O5 144.06(9) 3_656 2 ?
O2 Dy1 O3 71.80(8) 3_656 4_556 ?
O2 Dy1 O6 145.02(8) 3_656 2 ?
O2 Dy1 O4 74.86(9) 3_656 4_556 ?
O2 Dy1 C5 69.55(9) 3_656 4_556 ?
O2 Dy1 C14 157.84(9) 3_656 2 ?
O5 Dy1 O7 141.30(8) 2 3_666 ?
O5 Dy1 O3 101.81(9) 2 4_556 ?
O5 Dy1 O4 73.68(9) 2 4_556 ?
O5 Dy1 C5 89.14(9) 2 4_556 ?
O5 Dy1 C14 26.80(9) 2 2 ?
O3 Dy1 O7 113.87(7) 4_556 3_666 ?
O3 Dy1 C5 26.31(8) 4_556 4_556 ?
O3 Dy1 C14 89.80(9) 4_556 2 ?
O6 Dy1 O7 120.85(8) 2 3_666 ?
O6 Dy1 O5 54.01(8) 2 2 ?
O6 Dy1 O3 74.81(8) 2 4_556 ?
O6 Dy1 O4 93.18(9) 2 4_556 ?
O6 Dy1 C5 84.93(9) 2 4_556 ?
O6 Dy1 C14 27.31(9) 2 2 ?
O4 Dy1 O7 140.64(8) 4_556 3_666 ?
O4 Dy1 O3 52.96(8) 4_556 4_556 ?
O4 Dy1 C5 26.75(9) 4_556 4_556 ?
O4 Dy1 C14 84.27(9) 4_556 2 ?
C5 Dy1 O7 129.55(8) 4_556 3_666 ?
C14 Dy1 O7 135.03(9) 2 3_666 ?
C14 Dy1 C5 88.46(9) 2 4_556 ?
C1 O1 Dy1 129.9(2) . . ?
C22 O8 Dy1 106.2(2) . 3_666 ?
Dy1 O7 Dy1 103.72(8) 1_565 3_666 ?
C22 O7 Dy1 171.3(2) . 1_565 ?
C22 O7 Dy1 81.74(18) . 3_666 ?
C1 O2 Dy1 140.1(2) . 3_656 ?
C14 O5 Dy1 92.1(2) . 2 ?
C5 O3 Dy1 93.0(2) . 4 ?
C14 O6 Dy1 92.3(2) . 2 ?
C5 O4 Dy1 92.80(19) . 4 ?
C17 N1 C9 116.4(3) . . ?
C7 N1 C9 120.8(3) . . ?
C7 N1 C17 120.6(3) . . ?
N1 C9 H9A 108.7 . . ?
N1 C9 H9B 108.7 . . ?
N1 C9 C10 114.1(3) . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
O8 C22 O7 122.0(3) . . ?
O8 C22 C21 118.6(3) . . ?
O7 C22 C21 119.3(3) . . ?
C7 C8 H8 119.9 . . ?
C2 C8 H8 119.9 . . ?
C2 C8 C7 120.3(3) . . ?
O3 C5 Dy1 60.66(18) . 4 ?
O3 C5 O4 120.7(3) . . ?
O3 C5 C4 120.2(3) . . ?
O4 C5 Dy1 60.44(17) . 4 ?
O4 C5 C4 119.1(3) . . ?
C4 C5 Dy1 173.2(2) . 4 ?
C16 C10 C9 118.5(3) . . ?
C11 C10 C9 122.5(3) . . ?
C11 C10 C16 119.0(3) . . ?
O1 C1 O2 125.8(3) . . ?
O1 C1 C2 118.3(3) . . ?
O2 C1 C2 115.9(3) . . ?
C10 C16 H16 119.5 . . ?
C15 C16 C10 121.0(3) . . ?
C15 C16 H16 119.5 . . ?
C24 C18 C17 122.0(3) . . ?
C19 C18 C17 119.3(3) . . ?
C19 C18 C24 118.7(3) . . ?
N1 C17 C18 114.6(3) . . ?
N1 C17 H17A 108.6 . . ?
N1 C17 H17B 108.6 . . ?
C18 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
O5 C14 Dy1 61.09(17) . 2 ?
O5 C14 O6 121.1(3) . . ?
O5 C14 C13 119.7(3) . . ?
O6 C14 Dy1 60.39(17) . 2 ?
O6 C14 C13 119.1(3) . . ?
C13 C14 Dy1 173.6(2) . 2 ?
N1 C7 C8 120.4(3) . . ?
N1 C7 C6 121.6(3) . . ?
C6 C7 C8 117.9(3) . . ?
C21 C23 H23 120.0 . . ?
C21 C23 C24 120.1(3) . . ?
C24 C23 H23 120.0 . . ?
C8 C2 C1 119.6(3) . . ?
C8 C2 C3 121.1(3) . . ?
C3 C2 C1 119.3(3) . . ?
C15 C13 C14 120.6(3) . . ?
C12 C13 C14 120.3(3) . . ?
C12 C13 C15 119.1(3) . . ?
C16 C15 C13 120.1(3) . . ?
C16 C15 H15 119.9 . . ?
C13 C15 H15 119.9 . . ?
C23 C21 C22 119.6(3) . . ?
C23 C21 C20 119.8(3) . . ?
C20 C21 C22 120.6(3) . . ?
C18 C24 H24 119.6 . . ?
C23 C24 C18 120.8(3) . . ?
C23 C24 H24 119.6 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.0(3) . . ?
C4 C3 H3 120.5 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.7(3) . . ?
C20 C19 H19 119.7 . . ?
C3 C4 C5 119.6(3) . . ?
C6 C4 C5 119.9(3) . . ?
C6 C4 C3 120.5(3) . . ?
C13 C12 C11 120.3(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C7 C6 H6 119.4 . . ?
C4 C6 C7 121.2(3) . . ?
C4 C6 H6 119.4 . . ?
C21 C20 C19 119.6(3) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C25 H25A 109.5 . . ?
N2 C25 H25B 109.5 . . ?
N2 C25 H25C 109.5 . . ?
C25 N2 H2A 105.4 . . ?
C25 N2 H2B 105.4 . . ?
C25 N2 C26 127.7(9) . . ?
H2A N2 H2B 106.0 . . ?
C26 N2 H2A 105.4 . . ?
C26 N2 H2B 105.4 . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C1 O2 -47.4(5) . . . . ?
Dy1 O1 C1 C2 132.5(3) . . . . ?
Dy1 O8 C22 O7 -12.5(4) 3_666 . . . ?
Dy1 O8 C22 C21 168.7(2) 3_666 . . . ?
Dy1 O7 C22 O8 9.9(3) 3_666 . . . ?
Dy1 O7 C22 C21 -171.3(3) 3_666 . . . ?
Dy1 O2 C1 O1 22.9(6) 3_656 . . . ?
Dy1 O2 C1 C2 -157.0(3) 3_656 . . . ?
Dy1 O5 C14 O6 -7.0(3) 2 . . . ?
Dy1 O5 C14 C13 172.8(3) 2 . . . ?
Dy1 O3 C5 O4 7.1(3) 4 . . . ?
Dy1 O3 C5 C4 -172.3(3) 4 . . . ?
Dy1 O6 C14 O5 7.1(3) 2 . . . ?
Dy1 O6 C14 C13 -172.7(3) 2 . . . ?
Dy1 O4 C5 O3 -7.1(3) 4 . . . ?
Dy1 O4 C5 C4 172.3(3) 4 . . . ?
O1 C1 C2 C8 15.7(5) . . . . ?
O1 C1 C2 C3 -166.1(3) . . . . ?
O8 C22 C21 C23 -21.0(5) . . . . ?
O8 C22 C21 C20 157.3(4) . . . . ?
O7 C22 C21 C23 160.2(3) . . . . ?
O7 C22 C21 C20 -21.5(5) . . . . ?
O2 C1 C2 C8 -164.4(3) . . . . ?
O2 C1 C2 C3 13.8(5) . . . . ?
O5 C14 C13 C15 171.9(3) . . . . ?
O5 C14 C13 C12 -9.0(5) . . . . ?
O3 C5 C4 C3 31.4(5) . . . . ?
O3 C5 C4 C6 -150.9(3) . . . . ?
O6 C14 C13 C15 -8.4(5) . . . . ?
O6 C14 C13 C12 170.8(3) . . . . ?
O4 C5 C4 C3 -148.0(3) . . . . ?
O4 C5 C4 C6 29.7(5) . . . . ?
N1 C9 C10 C16 167.1(3) . . . . ?
N1 C9 C10 C11 -12.0(5) . . . . ?
N1 C7 C6 C4 178.1(3) . . . . ?
C9 N1 C17 C18 -95.1(3) . . . . ?
C9 N1 C7 C8 167.3(3) . . . . ?
C9 N1 C7 C6 -11.4(4) . . . . ?
C9 C10 C16 C15 -178.7(3) . . . . ?
C9 C10 C11 C12 179.4(3) . . . . ?
C22 C21 C20 C19 -173.3(4) . . . . ?
C8 C7 C6 C4 -0.6(5) . . . . ?
C8 C2 C3 C4 0.9(5) . . . . ?
C5 C4 C6 C7 -178.4(3) . . . . ?
C10 C16 C15 C13 -0.8(6) . . . . ?
C10 C11 C12 C13 -0.7(5) . . . . ?
C1 C2 C3 C4 -177.2(3) . . . . ?
C16 C10 C11 C12 0.2(5) . . . . ?
C18 C19 C20 C21 -1.7(6) . . . . ?
C17 N1 C9 C10 -99.2(3) . . . . ?
C17 N1 C7 C8 5.1(4) . . . . ?
C17 N1 C7 C6 -173.7(3) . . . . ?
C17 C18 C24 C23 -172.5(3) . . . . ?
C17 C18 C19 C20 174.6(4) . . . . ?
C14 C13 C15 C16 179.4(3) . . . . ?
C14 C13 C12 C11 -178.7(3) . . . . ?
C7 N1 C9 C10 97.9(3) . . . . ?
C7 N1 C17 C18 67.9(4) . . . . ?
C7 C8 C2 C1 175.8(3) . . . . ?
C7 C8 C2 C3 -2.3(5) . . . . ?
C23 C21 C20 C19 5.0(6) . . . . ?
C2 C8 C7 N1 -176.7(3) . . . . ?
C2 C8 C7 C6 2.1(4) . . . . ?
C2 C3 C4 C5 178.2(3) . . . . ?
C2 C3 C4 C6 0.6(5) . . . . ?
C15 C13 C12 C11 0.5(5) . . . . ?
C21 C23 C24 C18 -2.5(6) . . . . ?
C24 C18 C17 N1 5.6(5) . . . . ?
C24 C18 C19 C20 -3.7(6) . . . . ?
C24 C23 C21 C22 175.4(3) . . . . ?
C24 C23 C21 C20 -2.9(5) . . . . ?
C3 C4 C6 C7 -0.7(5) . . . . ?
C11 C10 C16 C15 0.5(5) . . . . ?
C19 C18 C17 N1 -172.6(3) . . . . ?
C19 C18 C24 C23 5.8(6) . . . . ?
C12 C13 C15 C16 0.3(5) . . . . ?

_platon_squeeze_details          
;

;
_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_1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1555476'
_audit_update_record             
;
2017-06-10 deposited with the CCDC.
2018-05-28 downloaded from the CCDC.
;
_audit_creation_date             2017-06-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C96 H60 N4 O32 Tb4), H2 O, 2(C2 H8 N)'
_chemical_formula_sum            'C52 H48 N4 O17 Tb2'
_chemical_formula_weight         1318.80
_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 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1890 4.4100 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   15.7666(14)
_cell_length_b                   9.7926(8)
_cell_length_c                   20.9867(19)
_cell_angle_alpha                90
_cell_angle_beta                 107.985(2)
_cell_angle_gamma                90
_cell_volume                     3081.9(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8163
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.340
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32361
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         3.323
_diffrn_ambient_temperature      113.3
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_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                6370
_reflns_number_total             7108
_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       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         3.299
_refine_diff_density_min         -1.548
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7014
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0298
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0506P)²+6.7031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0896
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-H9
 0.8 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C17(H17a,H17b), N2(H2a,H2b)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C16(H16), C23(H23), C15(H15), C24(H24), C3(H3), C11(H11), C19(H19),
 C12(H12), C6(H6), C20(H20)
4.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C26(H26a,H26b,H26c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.39557(2) 0.04476(2) 0.53369(2) 0.01117(6) Uani 1 1 d . . . . .
O1 O 0.39089(15) 0.1670(3) 0.43606(12) 0.0188(5) Uani 1 1 d . . . . .
O8 O 0.50881(15) 0.7775(3) 0.41221(12) 0.0199(5) Uani 1 1 d . . . . .
O7 O 0.42873(16) 0.8828(2) 0.46696(12) 0.0203(5) Uani 1 1 d . . . . .
O2 O 0.49124(16) 0.0799(3) 0.39158(12) 0.0224(5) Uani 1 1 d . . . . .
O5 O -0.24174(16) 0.0343(2) 0.03995(14) 0.0228(5) Uani 1 1 d . . . . .
O3 O 0.37490(16) -0.0581(2) 0.14554(13) 0.0183(5) Uani 1 1 d . . . . .
O6 O -0.28234(15) 0.2180(3) -0.02324(12) 0.0226(5) Uani 1 1 d . . . . .
O4 O 0.31860(17) 0.1220(3) 0.08435(12) 0.0229(5) Uani 1 1 d . . . . .
N1 N 0.15661(17) 0.3654(3) 0.23145(14) 0.0157(5) Uani 1 1 d . . . . .
C9 C 0.1109(2) 0.4185(3) 0.16476(18) 0.0176(6) Uani 1 1 d . . . . .
H9A H 0.1507 0.4120 0.1377 0.021 Uiso 1 1 calc R . . . .
H9B H 0.0979 0.5145 0.1686 0.021 Uiso 1 1 calc R . . . .
C22 C 0.4359(2) 0.7977(3) 0.42347(16) 0.0165(6) Uani 1 1 d . . . . .
C8 C 0.2821(2) 0.2433(3) 0.30748(16) 0.0144(6) Uani 1 1 d . . . . .
H8 H 0.2697 0.2816 0.3442 0.017 Uiso 1 1 calc R . . . .
C5 C 0.3383(2) 0.0570(3) 0.13972(17) 0.0155(6) Uani 1 1 d . . . . .
C10 C 0.0241(2) 0.3447(3) 0.12863(17) 0.0163(6) Uani 1 1 d . . . . .
C1 C 0.4169(2) 0.1330(3) 0.38743(16) 0.0169(6) Uani 1 1 d . . . . .
C16 C -0.0335(2) 0.4039(4) 0.07108(18) 0.0215(7) Uani 1 1 d . . . . .
H16 H -0.0177 0.4857 0.0553 0.026 Uiso 1 1 calc R . . . .
C18 C 0.2158(2) 0.5440(3) 0.31850(18) 0.0165(7) Uani 1 1 d . . . . .
C17 C 0.1437(2) 0.4398(3) 0.28711(19) 0.0183(7) Uani 1 1 d . . . . .
H17A H 0.1408 0.3750 0.3213 0.022 Uiso 1 1 calc R . . . .
H17B H 0.0867 0.4865 0.2719 0.022 Uiso 1 1 calc R . . . .
C14 C -0.2254(2) 0.1526(4) 0.02369(17) 0.0192(7) Uani 1 1 d . . . . .
C7 C 0.22654(19) 0.2735(3) 0.24161(16) 0.0135(6) Uani 1 1 d . . . . .
C23 C 0.3545(2) 0.6567(3) 0.32510(18) 0.0199(7) Uani 1 1 d . . . . .
H23 H 0.4007 0.6724 0.3072 0.024 Uiso 1 1 calc R . . . .
C2 C 0.3550(2) 0.1564(3) 0.31738(16) 0.0151(6) Uani 1 1 d . . . . .
C13 C -0.1381(2) 0.2189(4) 0.05979(17) 0.0182(6) Uani 1 1 d . . . . .
C15 C -0.1140(2) 0.3428(4) 0.03703(18) 0.0241(8) Uani 1 1 d . . . . .
H15 H -0.1520 0.3842 -0.0010 0.029 Uiso 1 1 calc R . . . .
C21 C 0.3563(2) 0.7166(3) 0.38510(17) 0.0165(6) Uani 1 1 d . . . . .
C24 C 0.2838(2) 0.5731(4) 0.29141(19) 0.0220(7) Uani 1 1 d . . . . .
H24 H 0.2819 0.5360 0.2502 0.026 Uiso 1 1 calc R . . . .
C3 C 0.3732(2) 0.0937(3) 0.26334(16) 0.0159(6) Uani 1 1 d . . . . .
H3 H 0.4216 0.0348 0.2704 0.019 Uiso 1 1 calc R . . . .
C11 C 0.0001(2) 0.2218(3) 0.15148(17) 0.0188(7) Uani 1 1 d . . . . .
H11 H 0.0378 0.1814 0.1899 0.023 Uiso 1 1 calc R . . . .
C19 C 0.2157(2) 0.6100(4) 0.3769(2) 0.0277(8) Uani 1 1 d . . . . .
H19 H 0.1688 0.5956 0.3943 0.033 Uiso 1 1 calc R . . . .
C4 C 0.3179(2) 0.1206(3) 0.19838(16) 0.0152(6) Uani 1 1 d . . . . .
C12 C -0.0805(2) 0.1587(4) 0.11703(18) 0.0193(7) Uani 1 1 d . . . . .
H12 H -0.0957 0.0761 0.1324 0.023 Uiso 1 1 calc R . . . .
C6 C 0.2458(2) 0.2098(3) 0.18766(16) 0.0160(6) Uani 1 1 d . . . . .
H6 H 0.2100 0.2274 0.1441 0.019 Uiso 1 1 calc R . . . .
C20 C 0.2852(2) 0.6979(4) 0.4101(2) 0.0289(9) Uani 1 1 d . . . . .
H20 H 0.2838 0.7435 0.4486 0.035 Uiso 1 1 calc R . . . .
O9 O 0.5000 0.7698(4) 0.2500 0.0264(8) Uani 1 2 d DS T P . .
H9 H 0.527(3) 0.817(4) 0.2811(17) 0.040(14) Uiso 1 1 d D . . . .
C25 C 0.5596(6) 0.4416(6) 0.4367(5) 0.090(3) Uani 1 1 d . . . . .
H25A H 0.5091 0.4955 0.4124 0.135 Uiso 1 1 calc GR . . . .
H25B H 0.5601 0.4320 0.4823 0.135 Uiso 1 1 calc GR . . . .
H25C H 0.5558 0.3530 0.4164 0.135 Uiso 1 1 calc GR . . . .
N2 N 0.6511(7) 0.5171(10) 0.4348(5) 0.133(3) Uani 1 1 d . U . . .
H2A H 0.6943 0.4560 0.4507 0.160 Uiso 1 1 calc R . . . .
H2B H 0.6608 0.5829 0.4655 0.160 Uiso 1 1 calc R . . . .
C26 C 0.6720(9) 0.5878(15) 0.3690(5) 0.165(5) Uani 1 1 d . U . . .
H26A H 0.6308 0.5529 0.3285 0.247 Uiso 1 1 calc GR . . . .
H26B H 0.7318 0.5662 0.3701 0.247 Uiso 1 1 calc GR . . . .
H26C H 0.6655 0.6851 0.3706 0.247 Uiso 1 1 calc GR . . . .


_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 O1 2.355(2) . ?
Tb1 O8 2.353(2) 3_666 ?
Tb1 O7 2.281(2) 1_545 ?
Tb1 O7 2.864(2) 3_666 ?
Tb1 O2 2.325(2) 3_656 ?
Tb1 O5 2.443(2) 2 ?
Tb1 O3 2.471(2) 4_556 ?
Tb1 O6 2.423(2) 2 ?
Tb1 O4 2.463(2) 4_556 ?
Tb1 C5 2.829(3) 4_556 ?
Tb1 C14 2.787(3) 2 ?
O1 C1 1.257(4) . ?
O8 Tb1 2.353(2) 3_666 ?
O8 C22 1.258(4) . ?
O7 Tb1 2.281(2) 1_565 ?
O7 Tb1 2.864(2) 3_666 ?
O7 C22 1.266(4) . ?
O2 Tb1 2.325(2) 3_656 ?
O2 C1 1.260(4) . ?
O5 Tb1 2.443(2) 2 ?
O5 C14 1.256(4) . ?
O3 Tb1 2.471(2) 4 ?
O3 C5 1.256(4) . ?
O6 Tb1 2.423(2) 2 ?
O6 C14 1.280(4) . ?
O4 Tb1 2.463(2) 4 ?
O4 C5 1.276(4) . ?
N1 C9 1.458(4) . ?
N1 C17 1.444(4) . ?
N1 C7 1.387(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.526(4) . ?
C22 C21 1.494(4) . ?
C8 H8 0.9300 . ?
C8 C7 1.421(4) . ?
C8 C2 1.392(4) . ?
C5 Tb1 2.829(3) 4 ?
C5 C4 1.500(4) . ?
C10 C16 1.394(5) . ?
C10 C11 1.391(5) . ?
C1 C2 1.511(4) . ?
C16 H16 0.9300 . ?
C16 C15 1.385(5) . ?
C18 C17 1.519(4) . ?
C18 C24 1.389(5) . ?
C18 C19 1.387(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C14 Tb1 2.787(3) 2 ?
C14 C13 1.498(4) . ?
C7 C6 1.406(4) . ?
C23 H23 0.9300 . ?
C23 C21 1.382(5) . ?
C23 C24 1.388(5) . ?
C2 C3 1.396(4) . ?
C13 C15 1.399(5) . ?
C13 C12 1.394(5) . ?
C15 H15 0.9300 . ?
C21 C20 1.389(5) . ?
C24 H24 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.398(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.396(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.398(5) . ?
C4 C6 1.395(4) . ?
C12 H12 0.9300 . ?
C6 H6 0.9300 . ?
C20 H20 0.9300 . ?
O9 H9 0.807(10) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25 N2 1.632(12) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C26 1.666(14) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O7 68.92(7) . 3_666 ?
O1 Tb1 O5 73.29(8) . 2 ?
O1 Tb1 O3 145.27(8) . 4_556 ?
O1 Tb1 O6 74.98(8) . 2 ?
O1 Tb1 O4 145.64(8) . 4_556 ?
O1 Tb1 C5 158.73(8) . 4_556 ?
O1 Tb1 C14 70.36(9) . 2 ?
O8 Tb1 O1 83.51(9) 3_666 . ?
O8 Tb1 O7 48.88(7) 3_666 3_666 ?
O8 Tb1 O5 134.38(8) 3_666 2 ?
O8 Tb1 O3 75.83(8) 3_666 4_556 ?
O8 Tb1 O6 82.53(8) 3_666 2 ?
O8 Tb1 O4 127.59(8) 3_666 4_556 ?
O8 Tb1 C5 101.18(9) 3_666 4_556 ?
O8 Tb1 C14 108.42(10) 3_666 2 ?
O7 Tb1 O1 76.75(8) 1_545 . ?
O7 Tb1 O8 125.22(8) 1_545 3_666 ?
O7 Tb1 O7 76.35(8) 1_545 3_666 ?
O7 Tb1 O2 77.01(9) 1_545 3_656 ?
O7 Tb1 O5 87.33(9) 1_545 2 ?
O7 Tb1 O3 137.95(8) 1_545 4_556 ?
O7 Tb1 O6 137.17(8) 1_545 2 ?
O7 Tb1 O4 92.34(9) 1_545 4_556 ?
O7 Tb1 C5 115.30(9) 1_545 4_556 ?
O7 Tb1 C14 111.76(10) 1_545 2 ?
O2 Tb1 O1 131.70(8) 3_656 . ?
O2 Tb1 O8 79.58(9) 3_656 3_666 ?
O2 Tb1 O7 65.87(8) 3_656 3_666 ?
O2 Tb1 O5 144.10(9) 3_656 2 ?
O2 Tb1 O3 71.70(8) 3_656 4_556 ?
O2 Tb1 O6 145.01(8) 3_656 2 ?
O2 Tb1 O4 74.84(9) 3_656 4_556 ?
O2 Tb1 C5 69.48(9) 3_656 4_556 ?
O2 Tb1 C14 157.87(9) 3_656 2 ?
O5 Tb1 O7 141.29(8) 2 3_666 ?
O5 Tb1 O3 101.94(9) 2 4_556 ?
O5 Tb1 O4 73.74(9) 2 4_556 ?
O5 Tb1 C5 89.25(9) 2 4_556 ?
O5 Tb1 C14 26.78(9) 2 2 ?
O3 Tb1 O7 113.76(7) 4_556 3_666 ?
O3 Tb1 C5 26.31(8) 4_556 4_556 ?
O3 Tb1 C14 89.93(9) 4_556 2 ?
O6 Tb1 O7 120.85(8) 2 3_666 ?
O6 Tb1 O5 54.00(8) 2 2 ?
O6 Tb1 O3 74.90(8) 2 4_556 ?
O6 Tb1 O4 93.21(9) 2 4_556 ?
O6 Tb1 C5 84.99(9) 2 4_556 ?
O6 Tb1 C14 27.33(9) 2 2 ?
O4 Tb1 O7 140.59(8) 4_556 3_666 ?
O4 Tb1 O3 52.99(8) 4_556 4_556 ?
O4 Tb1 C5 26.78(9) 4_556 4_556 ?
O4 Tb1 C14 84.32(9) 4_556 2 ?
C5 Tb1 O7 129.45(8) 4_556 3_666 ?
C14 Tb1 O7 135.03(9) 2 3_666 ?
C14 Tb1 C5 88.55(9) 2 4_556 ?
C1 O1 Tb1 129.9(2) . . ?
C22 O8 Tb1 106.2(2) . 3_666 ?
Tb1 O7 Tb1 103.66(8) 1_565 3_666 ?
C22 O7 Tb1 171.3(2) . 1_565 ?
C22 O7 Tb1 81.81(18) . 3_666 ?
C1 O2 Tb1 140.1(2) . 3_656 ?
C14 O5 Tb1 92.1(2) . 2 ?
C5 O3 Tb1 93.0(2) . 4 ?
C14 O6 Tb1 92.4(2) . 2 ?
C5 O4 Tb1 92.81(19) . 4 ?
C17 N1 C9 116.4(3) . . ?
C7 N1 C9 120.9(3) . . ?
C7 N1 C17 120.4(3) . . ?
N1 C9 H9A 108.7 . . ?
N1 C9 H9B 108.7 . . ?
N1 C9 C10 114.2(3) . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
O8 C22 O7 122.0(3) . . ?
O8 C22 C21 118.6(3) . . ?
O7 C22 C21 119.4(3) . . ?
C7 C8 H8 119.8 . . ?
C2 C8 H8 119.8 . . ?
C2 C8 C7 120.3(3) . . ?
O3 C5 Tb1 60.71(18) . 4 ?
O3 C5 O4 120.7(3) . . ?
O3 C5 C4 120.1(3) . . ?
O4 C5 Tb1 60.41(17) . 4 ?
O4 C5 C4 119.2(3) . . ?
C4 C5 Tb1 173.2(2) . 4 ?
C16 C10 C9 118.6(3) . . ?
C11 C10 C9 122.5(3) . . ?
C11 C10 C16 118.9(3) . . ?
O1 C1 O2 125.7(3) . . ?
O1 C1 C2 118.3(3) . . ?
O2 C1 C2 116.0(3) . . ?
C10 C16 H16 119.5 . . ?
C15 C16 C10 121.1(3) . . ?
C15 C16 H16 119.5 . . ?
C24 C18 C17 121.9(3) . . ?
C19 C18 C17 119.4(3) . . ?
C19 C18 C24 118.6(3) . . ?
N1 C17 C18 114.6(3) . . ?
N1 C17 H17A 108.6 . . ?
N1 C17 H17B 108.6 . . ?
C18 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
O5 C14 Tb1 61.15(17) . 2 ?
O5 C14 O6 121.1(3) . . ?
O5 C14 C13 119.7(3) . . ?
O6 C14 Tb1 60.32(17) . 2 ?
O6 C14 C13 119.2(3) . . ?
C13 C14 Tb1 173.6(2) . 2 ?
N1 C7 C8 120.4(3) . . ?
N1 C7 C6 121.5(3) . . ?
C6 C7 C8 118.0(3) . . ?
C21 C23 H23 119.9 . . ?
C21 C23 C24 120.2(3) . . ?
C24 C23 H23 119.9 . . ?
C8 C2 C1 119.6(3) . . ?
C8 C2 C3 121.0(3) . . ?
C3 C2 C1 119.3(3) . . ?
C15 C13 C14 120.5(3) . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 C15 119.1(3) . . ?
C16 C15 C13 120.1(3) . . ?
C16 C15 H15 120.0 . . ?
C13 C15 H15 120.0 . . ?
C23 C21 C22 119.7(3) . . ?
C23 C21 C20 119.7(3) . . ?
C20 C21 C22 120.6(3) . . ?
C18 C24 H24 119.6 . . ?
C23 C24 C18 120.8(3) . . ?
C23 C24 H24 119.6 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.0(3) . . ?
C4 C3 H3 120.5 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C18 C19 H19 119.6 . . ?
C18 C19 C20 120.8(3) . . ?
C20 C19 H19 119.6 . . ?
C3 C4 C5 119.6(3) . . ?
C6 C4 C5 119.8(3) . . ?
C6 C4 C3 120.5(3) . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C7 C6 H6 119.5 . . ?
C4 C6 C7 121.1(3) . . ?
C4 C6 H6 119.5 . . ?
C21 C20 C19 119.6(3) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C25 H25A 109.5 . . ?
N2 C25 H25B 109.5 . . ?
N2 C25 H25C 109.5 . . ?
C25 N2 H2A 105.4 . . ?
C25 N2 H2B 105.4 . . ?
C25 N2 C26 127.6(9) . . ?
H2A N2 H2B 106.0 . . ?
C26 N2 H2A 105.4 . . ?
C26 N2 H2B 105.4 . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C1 O2 -47.3(5) . . . . ?
Tb1 O1 C1 C2 132.6(3) . . . . ?
Tb1 O8 C22 O7 -12.5(4) 3_666 . . . ?
Tb1 O8 C22 C21 168.7(2) 3_666 . . . ?
Tb1 O7 C22 O8 9.9(3) 3_666 . . . ?
Tb1 O7 C22 C21 -171.3(3) 3_666 . . . ?
Tb1 O2 C1 O1 22.8(6) 3_656 . . . ?
Tb1 O2 C1 C2 -157.1(3) 3_656 . . . ?
Tb1 O5 C14 O6 -7.0(3) 2 . . . ?
Tb1 O5 C14 C13 172.8(3) 2 . . . ?
Tb1 O3 C5 O4 7.1(3) 4 . . . ?
Tb1 O3 C5 C4 -172.3(3) 4 . . . ?
Tb1 O6 C14 O5 7.1(3) 2 . . . ?
Tb1 O6 C14 C13 -172.7(3) 2 . . . ?
Tb1 O4 C5 O3 -7.1(3) 4 . . . ?
Tb1 O4 C5 C4 172.3(3) 4 . . . ?
O1 C1 C2 C8 15.7(5) . . . . ?
O1 C1 C2 C3 -166.1(3) . . . . ?
O8 C22 C21 C23 -21.0(5) . . . . ?
O8 C22 C21 C20 157.3(4) . . . . ?
O7 C22 C21 C23 160.2(3) . . . . ?
O7 C22 C21 C20 -21.6(5) . . . . ?
O2 C1 C2 C8 -164.4(3) . . . . ?
O2 C1 C2 C3 13.8(5) . . . . ?
O5 C14 C13 C15 171.9(3) . . . . ?
O5 C14 C13 C12 -9.0(5) . . . . ?
O3 C5 C4 C3 31.4(5) . . . . ?
O3 C5 C4 C6 -150.9(3) . . . . ?
O6 C14 C13 C15 -8.3(5) . . . . ?
O6 C14 C13 C12 170.8(3) . . . . ?
O4 C5 C4 C3 -148.0(3) . . . . ?
O4 C5 C4 C6 29.7(5) . . . . ?
N1 C9 C10 C16 167.1(3) . . . . ?
N1 C9 C10 C11 -12.0(5) . . . . ?
N1 C7 C6 C4 178.2(3) . . . . ?
C9 N1 C17 C18 -95.2(3) . . . . ?
C9 N1 C7 C8 167.3(3) . . . . ?
C9 N1 C7 C6 -11.4(4) . . . . ?
C9 C10 C16 C15 -178.7(3) . . . . ?
C9 C10 C11 C12 179.4(3) . . . . ?
C22 C21 C20 C19 -173.3(4) . . . . ?
C8 C7 C6 C4 -0.6(5) . . . . ?
C8 C2 C3 C4 0.9(5) . . . . ?
C5 C4 C6 C7 -178.4(3) . . . . ?
C10 C16 C15 C13 -0.8(6) . . . . ?
C10 C11 C12 C13 -0.7(5) . . . . ?
C1 C2 C3 C4 -177.2(3) . . . . ?
C16 C10 C11 C12 0.2(5) . . . . ?
C18 C19 C20 C21 -1.7(6) . . . . ?
C17 N1 C9 C10 -99.2(3) . . . . ?
C17 N1 C7 C8 5.1(4) . . . . ?
C17 N1 C7 C6 -173.7(3) . . . . ?
C17 C18 C24 C23 -172.5(3) . . . . ?
C17 C18 C19 C20 174.6(4) . . . . ?
C14 C13 C15 C16 179.4(3) . . . . ?
C14 C13 C12 C11 -178.7(3) . . . . ?
C7 N1 C9 C10 97.8(3) . . . . ?
C7 N1 C17 C18 67.9(4) . . . . ?
C7 C8 C2 C1 175.8(3) . . . . ?
C7 C8 C2 C3 -2.3(5) . . . . ?
C23 C21 C20 C19 5.0(6) . . . . ?
C2 C8 C7 N1 -176.7(3) . . . . ?
C2 C8 C7 C6 2.1(4) . . . . ?
C2 C3 C4 C5 178.2(3) . . . . ?
C2 C3 C4 C6 0.6(5) . . . . ?
C15 C13 C12 C11 0.5(5) . . . . ?
C21 C23 C24 C18 -2.5(6) . . . . ?
C24 C18 C17 N1 5.6(5) . . . . ?
C24 C18 C19 C20 -3.7(6) . . . . ?
C24 C23 C21 C22 175.4(3) . . . . ?
C24 C23 C21 C20 -2.9(5) . . . . ?
C3 C4 C6 C7 -0.7(5) . . . . ?
C11 C10 C16 C15 0.5(5) . . . . ?
C19 C18 C17 N1 -172.6(3) . . . . ?
C19 C18 C24 C23 5.8(6) . . . . ?
C12 C13 C15 C16 0.3(5) . . . . ?

_platon_squeeze_details          
;

;
_olex2_submission_special_instructions 'No special instructions were received'
