# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1554927'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;

_audit_creation_date             2017-05-20T08:30:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C38 H50 Dy2 N4 O24'
_chemical_formula_sum            'C38 H50 Dy2 N4 O24'
_chemical_formula_weight         1271.82

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2404(14)
_cell_length_b                   12.026(2)
_cell_length_c                   13.259(2)
_cell_angle_alpha                69.446(6)
_cell_angle_beta                 89.417(6)
_cell_angle_gamma                74.285(6)
_cell_volume                     1179.1(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1901
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      20.83

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             630

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_correction_T_min  0.5481
_exptl_absorpt_correction_T_max  0.7454

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.1112
_diffrn_reflns_number            9572
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.579
_diffrn_reflns_theta_max         26.324
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_reflns_Friedel_coverage         0
_reflns_number_total             4726
_reflns_number_gt                3424
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4726
_refine_ls_number_parameters     344
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1068
_refine_ls_wR_factor_gt          0.0955
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.229
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.19

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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 0.27401(4) -0.12977(4) 0.45430(3) 0.02505(13) Uani 1 1 d . . . . .
O1 O 0.0823(7) 0.0554(5) 0.3440(4) 0.0388(15) Uani 1 1 d . . . . .
O2 O -0.1677(6) 0.1575(5) 0.3772(4) 0.0338(14) Uani 1 1 d . . . . .
O3 O 0.177(5) 0.154(4) -0.043(3) 0.062(9) Uani 0.58 1 d . U P A 1
O4 O 0.131(5) 0.345(2) -0.135(3) 0.054(6) Uani 0.58 1 d . U P A 1
O32 O 0.215(7) 0.179(6) -0.039(5) 0.077(16) Uani 0.42 1 d . U P A 2
O42 O 0.102(7) 0.386(3) -0.142(4) 0.055(9) Uani 0.42 1 d . U P A 2
O5 O -0.4716(8) 0.5551(6) 0.0988(6) 0.063(2) Uani 1 1 d . . . . .
O6 O -0.3492(9) 0.6297(6) -0.0442(5) 0.071(2) Uani 1 1 d . . . . .
O7 O 0.5349(6) -0.2108(5) 0.5613(4) 0.0311(13) Uani 1 1 d . . . . .
O8 O 0.3304(6) -0.3415(5) 0.5232(4) 0.0348(14) Uani 1 1 d . . . . .
O9 O 0.4593(6) -0.0330(5) 0.3428(4) 0.0328(13) Uani 1 1 d . . . . .
O10 O 0.2762(7) -0.1753(5) 0.3004(4) 0.0387(14) Uani 1 1 d . . . . .
N1 N 0.1137(11) 0.2713(9) -0.0581(7) 0.055(2) Uani 1 1 d . . . . .
N2 N -0.3590(10) 0.5462(7) 0.0397(6) 0.052(2) Uani 1 1 d . . . . .
C1 C -0.0521(9) 0.1395(7) 0.3182(6) 0.0258(18) Uani 1 1 d . . . . .
C2 C -0.0813(8) 0.2321(6) 0.2027(6) 0.0210(16) Uani 1 1 d . . . . .
C3 C 0.0252(9) 0.2076(7) 0.1285(6) 0.0285(18) Uani 1 1 d . . . . .
H3A H 0.112847 0.131775 0.147456 0.034 Uiso 1 1 calc R U . . .
C4 C 0.0020(10) 0.2963(8) 0.0247(6) 0.036(2) Uani 1 1 d . . . . .
C5 C -0.1207(10) 0.4071(8) -0.0053(6) 0.038(2) Uani 1 1 d . . . . .
H5A H -0.132254 0.468045 -0.075747 0.046 Uiso 1 1 calc R U . . .
C6 C -0.2256(10) 0.4258(7) 0.0705(6) 0.034(2) Uani 1 1 d . . . . .
C7 C -0.2100(9) 0.3417(7) 0.1744(6) 0.0269(18) Uani 1 1 d . . . . .
H7A H -0.285769 0.358443 0.225189 0.032 Uiso 1 1 calc R U . . .
C8 C 0.7750(11) -0.3245(8) 0.6874(7) 0.049(2) Uani 1 1 d . . . . .
H8A H 0.746994 -0.277543 0.735579 0.073 Uiso 1 1 calc R U . . .
H8B H 0.847986 -0.288881 0.634238 0.073 Uiso 1 1 calc R U . . .
H8C H 0.834322 -0.411125 0.729948 0.073 Uiso 1 1 calc R U . . .
C9 C 0.6176(9) -0.3182(7) 0.6305(6) 0.0312(19) Uani 1 1 d . . . . .
C10 C 0.5661(10) -0.4239(7) 0.6510(6) 0.033(2) Uani 1 1 d . . . . .
H10A H 0.633033 -0.497745 0.705062 0.04 Uiso 1 1 calc R U . . .
C11 C 0.4265(10) -0.4320(7) 0.6002(6) 0.033(2) Uani 1 1 d . . . . .
C12 C 0.3829(11) -0.5526(7) 0.6336(8) 0.046(2) Uani 1 1 d . . . . .
H12A H 0.29864 -0.547974 0.579517 0.069 Uiso 1 1 calc R U . . .
H12B H 0.336407 -0.568703 0.70396 0.069 Uiso 1 1 calc R U . . .
H12C H 0.485197 -0.619885 0.639173 0.069 Uiso 1 1 calc R U . . .
C13 C 0.5959(11) 0.0764(9) 0.1979(7) 0.053(3) Uani 1 1 d . . . . .
H13A H 0.59476 0.09889 0.119267 0.08 Uiso 1 1 calc R U . . .
H13B H 0.711966 0.033392 0.231478 0.08 Uiso 1 1 calc R U . . .
H13C H 0.553064 0.151598 0.214795 0.08 Uiso 1 1 calc R U . . .
C14 C 0.4843(10) -0.0080(8) 0.2412(7) 0.041(2) Uani 1 1 d . . . . .
C15 C 0.4196(11) -0.0535(8) 0.1742(7) 0.041(2) Uani 1 1 d . . . . .
H15A H 0.444917 -0.027951 0.100913 0.049 Uiso 1 1 calc R U . . .
C16 C 0.3200(10) -0.1340(8) 0.2055(7) 0.042(2) Uani 1 1 d . . . . .
C17 C 0.2586(12) -0.1791(9) 0.1229(7) 0.056(3) Uani 1 1 d . . . . .
H17A H 0.225067 -0.254338 0.160779 0.083 Uiso 1 1 calc R U . . .
H17B H 0.349985 -0.197354 0.07817 0.083 Uiso 1 1 calc R U . . .
H17C H 0.161126 -0.114595 0.076725 0.083 Uiso 1 1 calc R U . . .
O11 O 0.3056(6) 0.0335(4) 0.5153(4) 0.0262(12) Uani 1 1 d . . . . .
H1 H 0.323134 0.094853 0.481675 0.031 Uiso 1 1 d R U . . .
H2 H 0.369534 0.017153 0.576974 0.031 Uiso 1 1 d R U . . .
O12 O 0.0020(6) -0.1722(5) 0.4409(4) 0.0379(14) Uani 1 1 d D . . . .
H3 H -0.092196 -0.121582 0.455795 0.045 Uiso 1 1 d R U . B .
C18 C -0.071(2) -0.2212(14) 0.3626(14) 0.044(5) Uani 0.5 1 d D . P B 1
H18A H -0.194718 -0.206577 0.366361 0.053 Uiso 0.5 1 calc R U P B 1
H18B H -0.050418 -0.177287 0.2873 0.053 Uiso 0.5 1 calc R U P B 1
C19 C 0.017(3) -0.3597(16) 0.3965(17) 0.068(7) Uani 0.5 1 d D . P B 1
H19A H -0.02631 -0.392195 0.347366 0.102 Uiso 0.5 1 calc R U P B 1
H19B H -0.006535 -0.402623 0.470564 0.102 Uiso 0.5 1 calc R U P B 1
H19C H 0.139032 -0.373352 0.393373 0.102 Uiso 0.5 1 calc R U P B 1
C182 C -0.025(7) -0.287(3) 0.417(4) 0.051(9) Uiso 0.24 1 d D U P B 2
H18C H 0.084578 -0.343754 0.41174 0.061 Uiso 0.24 1 calc R U P B 2
H18D H -0.084613 -0.334616 0.474072 0.061 Uiso 0.24 1 calc R U P B 2
C192 C -0.133(5) -0.229(4) 0.309(3) 0.051(9) Uiso 0.24 1 d D U P B 2
H19D H -0.155732 -0.294082 0.287594 0.076 Uiso 0.24 1 calc R U P B 2
H19E H -0.240331 -0.172942 0.315186 0.076 Uiso 0.24 1 calc R U P B 2
H19F H -0.07229 -0.182019 0.253278 0.076 Uiso 0.24 1 calc R U P B 2
C183 C -0.048(6) -0.274(3) 0.437(3) 0.052(9) Uiso 0.26 1 d D U P B 3
H18E H -0.172661 -0.253498 0.435564 0.063 Uiso 0.26 1 calc R U P B 3
H18F H 0.000339 -0.345709 0.504212 0.063 Uiso 0.26 1 calc R U P B 3
C193 C 0.006(6) -0.311(4) 0.341(3) 0.052(9) Uiso 0.26 1 d D U P B 3
H19G H -0.033422 -0.381764 0.344302 0.078 Uiso 0.26 1 calc R U P B 3
H19H H -0.043563 -0.240986 0.273764 0.078 Uiso 0.26 1 calc R U P B 3
H19I H 0.129751 -0.333365 0.342537 0.078 Uiso 0.26 1 calc R U P B 3



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O10 2.290(6) . ?
Dy1 O8 2.296(5) . ?
Dy1 O1 2.334(5) . ?
Dy1 O2 2.337(5) 2_556 ?
Dy1 O7 2.354(5) . ?
Dy1 O9 2.362(5) . ?
Dy1 O11 2.443(5) . ?
Dy1 O12 2.452(5) . ?
Dy1 Dy1 5.1490(10) 2_556 ?
O1 C1 1.235(8) . ?
O2 C1 1.248(8) . ?
O3 N1 1.30(5) . ?
O4 N1 1.13(3) . ?
O32 N1 1.14(6) . ?
O42 N1 1.42(4) . ?
O5 N2 1.216(9) . ?
O6 N2 1.229(9) . ?
O7 C9 1.296(8) . ?
O8 C11 1.274(9) . ?
O9 C14 1.300(9) . ?
O10 C16 1.269(10) . ?
N1 C4 1.484(10) . ?
N2 C6 1.484(10) . ?
C1 C2 1.519(10) . ?
C2 C3 1.368(10) . ?
C2 C7 1.380(9) . ?
C3 C4 1.390(10) . ?
C3 H3A 0.95 . ?
C4 C5 1.365(11) . ?
C5 C6 1.358(11) . ?
C5 H5A 0.95 . ?
C6 C7 1.375(10) . ?
C7 H7A 0.95 . ?
C8 C9 1.477(11) . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 C10 1.384(11) . ?
C10 C11 1.383(11) . ?
C10 H10A 0.95 . ?
C11 C12 1.502(10) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C14 1.514(11) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C15 1.372(12) . ?
C15 C16 1.387(12) . ?
C15 H15A 0.95 . ?
C16 C17 1.525(12) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
O11 H1 0.7682 . ?
O11 H2 0.9086 . ?
O12 C183 1.405(19) . ?
O12 C18 1.555(14) . ?
O12 C182 1.598(18) . ?
O12 H3 0.9152 . ?
C18 C19 1.526(16) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C182 C192 1.52(2) . ?
C182 H18C 0.99 . ?
C182 H18D 0.99 . ?
C192 H19D 0.98 . ?
C192 H19E 0.98 . ?
C192 H19F 0.98 . ?
C183 C193 1.516(19) . ?
C183 H18E 0.99 . ?
C183 H18F 0.99 . ?
C193 H19G 0.98 . ?
C193 H19H 0.98 . ?
C193 H19I 0.98 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Dy1 O8 77.94(19) . . ?
O10 Dy1 O1 82.49(19) . . ?
O8 Dy1 O1 144.67(19) . . ?
O10 Dy1 O2 145.94(19) . 2_556 ?
O8 Dy1 O2 79.87(18) . 2_556 ?
O1 Dy1 O2 101.81(18) . 2_556 ?
O10 Dy1 O7 114.84(18) . . ?
O8 Dy1 O7 72.58(18) . . ?
O1 Dy1 O7 142.75(19) . . ?
O2 Dy1 O7 82.14(17) 2_556 . ?
O10 Dy1 O9 72.75(19) . . ?
O8 Dy1 O9 121.19(18) . . ?
O1 Dy1 O9 79.42(18) . . ?
O2 Dy1 O9 141.30(19) 2_556 . ?
O7 Dy1 O9 75.41(17) . . ?
O10 Dy1 O11 140.49(18) . . ?
O8 Dy1 O11 137.86(17) . . ?
O1 Dy1 O11 72.63(18) . . ?
O2 Dy1 O11 70.82(17) 2_556 . ?
O7 Dy1 O11 73.96(17) . . ?
O9 Dy1 O11 72.86(17) . . ?
O10 Dy1 O12 75.78(19) . . ?
O8 Dy1 O12 74.00(18) . . ?
O1 Dy1 O12 72.82(18) . . ?
O2 Dy1 O12 73.45(18) 2_556 . ?
O7 Dy1 O12 141.40(18) . . ?
O9 Dy1 O12 140.19(18) . . ?
O11 Dy1 O12 122.79(16) . . ?
O10 Dy1 Dy1 120.34(13) . 2_556 ?
O8 Dy1 Dy1 118.02(12) . 2_556 ?
O1 Dy1 Dy1 50.49(13) . 2_556 ?
O2 Dy1 Dy1 51.57(12) 2_556 2_556 ?
O7 Dy1 Dy1 124.82(13) . 2_556 ?
O9 Dy1 Dy1 120.79(13) . 2_556 ?
O11 Dy1 Dy1 64.39(10) . 2_556 ?
O12 Dy1 Dy1 58.41(13) . 2_556 ?
C1 O1 Dy1 156.2(5) . . ?
C1 O2 Dy1 152.8(5) . 2_556 ?
C9 O7 Dy1 135.3(5) . . ?
C11 O8 Dy1 137.0(5) . . ?
C14 O9 Dy1 133.5(5) . . ?
C16 O10 Dy1 137.1(6) . . ?
O4 N1 O3 120(3) . . ?
O32 N1 O42 129(4) . . ?
O4 N1 C4 124.7(16) . . ?
O32 N1 C4 121(3) . . ?
O3 N1 C4 115(2) . . ?
O42 N1 C4 107.6(18) . . ?
O5 N2 O6 124.4(8) . . ?
O5 N2 C6 117.6(7) . . ?
O6 N2 C6 118.0(8) . . ?
O1 C1 O2 126.9(7) . . ?
O1 C1 C2 117.2(7) . . ?
O2 C1 C2 115.9(7) . . ?
C3 C2 C7 120.6(7) . . ?
C3 C2 C1 119.2(6) . . ?
C7 C2 C1 120.2(7) . . ?
C2 C3 C4 118.4(7) . . ?
C2 C3 H3A 120.8 . . ?
C4 C3 H3A 120.8 . . ?
C5 C4 C3 122.6(7) . . ?
C5 C4 N1 117.8(7) . . ?
C3 C4 N1 119.6(8) . . ?
C6 C5 C4 116.7(7) . . ?
C6 C5 H5A 121.6 . . ?
C4 C5 H5A 121.6 . . ?
C5 C6 C7 123.5(7) . . ?
C5 C6 N2 117.5(7) . . ?
C7 C6 N2 119.0(7) . . ?
C6 C7 C2 118.1(7) . . ?
C6 C7 H7A 120.9 . . ?
C2 C7 H7A 120.9 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O7 C9 C10 123.2(7) . . ?
O7 C9 C8 116.6(7) . . ?
C10 C9 C8 120.3(7) . . ?
C11 C10 C9 126.1(7) . . ?
C11 C10 H10A 116.9 . . ?
C9 C10 H10A 116.9 . . ?
O8 C11 C10 123.4(7) . . ?
O8 C11 C12 116.5(8) . . ?
C10 C11 C12 120.1(7) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O9 C14 C15 124.9(8) . . ?
O9 C14 C13 115.5(8) . . ?
C15 C14 C13 119.7(8) . . ?
C14 C15 C16 124.8(8) . . ?
C14 C15 H15A 117.6 . . ?
C16 C15 H15A 117.6 . . ?
O10 C16 C15 124.3(9) . . ?
O10 C16 C17 116.2(8) . . ?
C15 C16 C17 119.5(8) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Dy1 O11 H1 128.1 . . ?
Dy1 O11 H2 122.5 . . ?
H1 O11 H2 97.7 . . ?
C183 O12 Dy1 135.0(19) . . ?
C18 O12 Dy1 131.4(7) . . ?
C182 O12 Dy1 126(2) . . ?
C183 O12 H3 105.5 . . ?
C18 O12 H3 103.3 . . ?
C182 O12 H3 116 . . ?
Dy1 O12 H3 118 . . ?
C19 C18 O12 108.2(15) . . ?
C19 C18 H18A 110.1 . . ?
O12 C18 H18A 110.1 . . ?
C19 C18 H18B 110.1 . . ?
O12 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C192 C182 O12 104(3) . . ?
C192 C182 H18C 110.9 . . ?
O12 C182 H18C 110.9 . . ?
C192 C182 H18D 110.9 . . ?
O12 C182 H18D 110.9 . . ?
H18C C182 H18D 108.9 . . ?
C182 C192 H19D 109.5 . . ?
C182 C192 H19E 109.5 . . ?
H19D C192 H19E 109.5 . . ?
C182 C192 H19F 109.5 . . ?
H19D C192 H19F 109.5 . . ?
H19E C192 H19F 109.5 . . ?
O12 C183 C193 115(2) . . ?
O12 C183 H18E 108.6 . . ?
C193 C183 H18E 108.6 . . ?
O12 C183 H18F 108.6 . . ?
C193 C183 H18F 108.6 . . ?
H18E C183 H18F 107.6 . . ?
C183 C193 H19G 109.5 . . ?
C183 C193 H19H 109.5 . . ?
H19G C193 H19H 109.5 . . ?
C183 C193 H19I 109.5 . . ?
H19G C193 H19I 109.5 . . ?
H19H C193 H19I 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H1 O7 0.77 1.99 2.698(7) 153.8 2_656
O11 H2 O9 0.91 1.86 2.712(7) 154.4 2_656
O12 H3 O11 0.92 1.9 2.812(7) 171.2 2_556


# END of CIF
_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_5
_database_code_depnum_ccdc_archive 'CCDC 1554928'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;

_audit_creation_date             2017-05-20T08:48:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C38 H50 Ho2 N4 O24'
_chemical_formula_sum            'C38 H50 Ho2 N4 O24'
_chemical_formula_weight         1276.68

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2284(4)
_cell_length_b                   12.0412(5)
_cell_length_c                   13.2437(6)
_cell_angle_alpha                69.4450(10)
_cell_angle_beta                 89.3480(10)
_cell_angle_gamma                74.1940(10)
_cell_volume                     1177.01(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5908
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      27.46

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             632

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_T_min  0.5127
_exptl_absorpt_correction_T_max  0.7463

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_number            16878
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.584
_diffrn_reflns_theta_max         32.051
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.89
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.89
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.89
_reflns_Friedel_coverage         0
_reflns_number_total             7308
_reflns_number_gt                6266
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7308
_refine_ls_number_parameters     327
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.069
_refine_ls_wR_factor_gt          0.0658
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.865
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.131

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.27398(2) -0.12948(2) 0.45434(2) 0.02199(5) Uani 1 1 d . . . . .
O1 O 0.0834(3) 0.05498(19) 0.34405(17) 0.0329(5) Uani 1 1 d . . . . .
O2 O -0.1684(3) 0.1567(2) 0.37778(17) 0.0330(5) Uani 1 1 d . . . . .
O3 O 0.1927(4) 0.1646(3) -0.0424(2) 0.0812(12) Uani 1 1 d . . . . .
O4 O 0.1210(5) 0.3605(3) -0.1387(2) 0.0739(10) Uani 1 1 d . . . . .
O5 O -0.4720(4) 0.5551(3) 0.0984(2) 0.0613(8) Uani 1 1 d . . . . .
O6 O -0.3488(4) 0.6297(3) -0.0436(2) 0.0682(9) Uani 1 1 d . . . . .
O7 O 0.5346(2) -0.20999(18) 0.56103(16) 0.0283(5) Uani 1 1 d . . . . .
O8 O 0.3292(3) -0.33971(19) 0.52346(18) 0.0333(5) Uani 1 1 d . . . . .
O9 O 0.4592(3) -0.0325(2) 0.34261(16) 0.0293(5) Uani 1 1 d . . . . .
O10 O 0.2771(3) -0.1761(2) 0.30130(18) 0.0343(5) Uani 1 1 d . . . . .
N1 N 0.1143(4) 0.2706(4) -0.0585(3) 0.0547(9) Uani 1 1 d . . . . .
N2 N -0.3597(4) 0.5463(3) 0.0400(3) 0.0475(8) Uani 1 1 d . . . . .
C1 C -0.0532(4) 0.1391(3) 0.3184(2) 0.0234(6) Uani 1 1 d . . . . .
C2 C -0.0813(3) 0.2309(3) 0.2031(2) 0.0220(5) Uani 1 1 d . . . . .
C3 C 0.0255(4) 0.2072(3) 0.1265(2) 0.0281(6) Uani 1 1 d . . . . .
H3A H 0.113541 0.131555 0.14483 0.034 Uiso 1 1 calc R U . . .
C4 C 0.0016(4) 0.2956(3) 0.0232(3) 0.0359(7) Uani 1 1 d . . . . .
C5 C -0.1207(4) 0.4074(3) -0.0068(3) 0.0379(8) Uani 1 1 d . . . . .
H5A H -0.13224 0.468155 -0.077461 0.045 Uiso 1 1 calc R U . . .
C6 C -0.2258(4) 0.4272(3) 0.0702(3) 0.0331(7) Uani 1 1 d . . . . .
C7 C -0.2110(4) 0.3410(3) 0.1743(2) 0.0263(6) Uani 1 1 d . . . . .
H7A H -0.288136 0.357009 0.224871 0.032 Uiso 1 1 calc R U . . .
C8 C 0.7752(4) -0.3218(3) 0.6878(3) 0.0440(9) Uani 1 1 d . . . . .
H8A H 0.745553 -0.27136 0.733044 0.066 Uiso 1 1 calc R U . . .
H8B H 0.850836 -0.289548 0.634838 0.066 Uiso 1 1 calc R U . . .
H8C H 0.832699 -0.407718 0.733552 0.066 Uiso 1 1 calc R U . . .
C9 C 0.6161(4) -0.3171(3) 0.6291(2) 0.0311(7) Uani 1 1 d . . . . .
C10 C 0.5672(4) -0.4231(3) 0.6513(3) 0.0349(7) Uani 1 1 d . . . . .
H10A H 0.633985 -0.496641 0.70582 0.042 Uiso 1 1 calc R U . . .
C11 C 0.4251(4) -0.4298(3) 0.5984(3) 0.0301(7) Uani 1 1 d . . . . .
C12 C 0.3820(5) -0.5507(3) 0.6333(3) 0.0409(8) Uani 1 1 d . . . . .
H12A H 0.33111 -0.55877 0.570599 0.061 Uiso 1 1 calc R U . . .
H12B H 0.301285 -0.552836 0.688442 0.061 Uiso 1 1 calc R U . . .
H12C H 0.485525 -0.619307 0.663511 0.061 Uiso 1 1 calc R U . . .
C13 C 0.5966(5) 0.0758(4) 0.1982(3) 0.0530(11) Uani 1 1 d . . . . .
H13A H 0.584222 0.105434 0.118842 0.079 Uiso 1 1 calc R U . . .
H13B H 0.715336 0.029899 0.224699 0.079 Uiso 1 1 calc R U . . .
H13C H 0.562291 0.146543 0.221912 0.079 Uiso 1 1 calc R U . . .
C14 C 0.4850(4) -0.0089(3) 0.2431(3) 0.0358(8) Uani 1 1 d . . . . .
C15 C 0.4193(5) -0.0534(4) 0.1745(3) 0.0412(8) Uani 1 1 d . . . . .
H15A H 0.443278 -0.026756 0.100898 0.049 Uiso 1 1 calc R U . . .
C16 C 0.3197(4) -0.1352(3) 0.2069(3) 0.0342(7) Uani 1 1 d . . . . .
C17 C 0.2594(6) -0.1799(4) 0.1249(3) 0.0559(11) Uani 1 1 d . . . . .
H17A H 0.216728 -0.250815 0.162444 0.084 Uiso 1 1 calc R U . . .
H17B H 0.354143 -0.205026 0.084518 0.084 Uiso 1 1 calc R U . . .
H17C H 0.168391 -0.112993 0.074592 0.084 Uiso 1 1 calc R U . . .
O11 O 0.3045(2) 0.03309(18) 0.51507(15) 0.0235(4) Uani 1 1 d . . . . .
H1 H 0.366401 0.014982 0.573403 0.028 Uiso 1 1 d R U . . .
H2 H 0.346381 0.084532 0.473022 0.028 Uiso 1 1 d R U . . .
O12 O 0.0019(3) -0.1725(2) 0.44087(19) 0.0347(5) Uani 1 1 d D . . . .
H3 H -0.084219 -0.114213 0.46158 0.042 Uiso 1 1 d R U . A .
C18 C -0.0692(9) -0.2174(6) 0.3688(6) 0.0383(15) Uani 0.53 1 d D . P A 1
H18A H -0.053619 -0.170486 0.29307 0.046 Uiso 0.53 1 calc R U P A 1
H18B H -0.192504 -0.203109 0.375436 0.046 Uiso 0.53 1 calc R U P A 1
C19 C 0.0141(10) -0.3537(7) 0.3946(8) 0.0498(19) Uani 0.53 1 d D . P A 1
H19A H -0.036596 -0.381339 0.344549 0.075 Uiso 0.53 1 calc R U P A 1
H19B H 0.135862 -0.367861 0.386837 0.075 Uiso 0.53 1 calc R U P A 1
H19C H -0.002903 -0.400456 0.469132 0.075 Uiso 0.53 1 calc R U P A 1
C182 C -0.0189(18) -0.2772(12) 0.4198(12) 0.030(3) Uiso 0.28 1 d D . P A 2
H18C H -0.070989 -0.327308 0.48012 0.035 Uiso 0.28 1 calc R U P A 2
H18D H 0.092488 -0.330158 0.412454 0.035 Uiso 0.28 1 calc R U P A 2
C192 C -0.132(2) -0.2281(15) 0.3164(12) 0.057(4) Uiso 0.28 1 d D . P A 2
H19D H -0.14893 -0.297436 0.299553 0.086 Uiso 0.28 1 calc R U P A 2
H19E H -0.241889 -0.176003 0.324708 0.086 Uiso 0.28 1 calc R U P A 2
H19F H -0.079099 -0.178841 0.257326 0.086 Uiso 0.28 1 calc R U P A 2
C183 C -0.047(3) -0.2788(16) 0.4468(16) 0.035(5) Uiso 0.19 1 d D . P A 3
H18E H -0.170667 -0.263142 0.453858 0.041 Uiso 0.19 1 calc R U P A 3
H18F H 0.013227 -0.350055 0.511507 0.041 Uiso 0.19 1 calc R U P A 3
C193 C -0.006(4) -0.310(2) 0.3444(18) 0.056(7) Uiso 0.19 1 d D . P A 3
H19G H -0.040117 -0.382937 0.349382 0.084 Uiso 0.19 1 calc R U P A 3
H19H H -0.066863 -0.239314 0.280472 0.084 Uiso 0.19 1 calc R U P A 3
H19I H 0.1167 -0.32607 0.338018 0.084 Uiso 0.19 1 calc R U P A 3



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O8 2.282(2) . ?
Ho1 O10 2.283(2) . ?
Ho1 O1 2.324(2) . ?
Ho1 O2 2.325(2) 2_556 ?
Ho1 O7 2.3473(19) . ?
Ho1 O9 2.363(2) . ?
Ho1 O11 2.433(2) . ?
Ho1 O12 2.454(2) . ?
Ho1 Ho1 5.1362(3) 2_556 ?
O1 C1 1.246(3) . ?
O2 C1 1.245(3) . ?
O3 N1 1.206(5) . ?
O4 N1 1.235(4) . ?
O5 N2 1.206(4) . ?
O6 N2 1.228(4) . ?
O7 C9 1.285(3) . ?
O8 C11 1.257(4) . ?
O9 C14 1.275(4) . ?
O10 C16 1.256(4) . ?
N1 C4 1.475(4) . ?
N2 C6 1.475(4) . ?
C1 C2 1.515(4) . ?
C2 C7 1.388(4) . ?
C2 C3 1.388(4) . ?
C3 C4 1.383(4) . ?
C3 H3A 0.95 . ?
C4 C5 1.371(5) . ?
C5 C6 1.373(5) . ?
C5 H5A 0.95 . ?
C6 C7 1.386(4) . ?
C7 H7A 0.95 . ?
C8 C9 1.507(5) . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 C10 1.375(5) . ?
C10 C11 1.405(5) . ?
C10 H10A 0.95 . ?
C11 C12 1.504(4) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C14 1.520(5) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C15 1.384(5) . ?
C15 C16 1.401(5) . ?
C15 H15A 0.95 . ?
C16 C17 1.511(5) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
O11 H1 0.8565 . ?
O11 H2 0.8258 . ?
O12 C183 1.420(14) . ?
O12 C182 1.435(11) . ?
O12 C18 1.446(7) . ?
O12 H3 0.9644 . ?
C18 C19 1.510(9) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C182 C192 1.501(14) . ?
C182 H18C 0.99 . ?
C182 H18D 0.99 . ?
C192 H19D 0.98 . ?
C192 H19E 0.98 . ?
C192 H19F 0.98 . ?
C183 C193 1.539(17) . ?
C183 H18E 0.99 . ?
C183 H18F 0.99 . ?
C193 H19G 0.98 . ?
C193 H19H 0.98 . ?
C193 H19I 0.98 . ?

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
O8 Ho1 O10 77.81(8) . . ?
O8 Ho1 O1 144.68(8) . . ?
O10 Ho1 O1 82.72(8) . . ?
O8 Ho1 O2 79.70(8) . 2_556 ?
O10 Ho1 O2 145.96(8) . 2_556 ?
O1 Ho1 O2 101.98(8) . 2_556 ?
O8 Ho1 O7 72.78(7) . . ?
O10 Ho1 O7 114.67(8) . . ?
O1 Ho1 O7 142.53(7) . . ?
O2 Ho1 O7 82.05(7) 2_556 . ?
O8 Ho1 O9 121.62(8) . . ?
O10 Ho1 O9 72.94(8) . . ?
O1 Ho1 O9 79.11(7) . . ?
O2 Ho1 O9 141.08(8) 2_556 . ?
O7 Ho1 O9 75.42(7) . . ?
O8 Ho1 O11 137.82(7) . . ?
O10 Ho1 O11 140.78(7) . . ?
O1 Ho1 O11 72.51(7) . . ?
O2 Ho1 O11 70.62(7) 2_556 . ?
O7 Ho1 O11 73.98(7) . . ?
O9 Ho1 O11 72.85(7) . . ?
O8 Ho1 O12 73.62(8) . . ?
O10 Ho1 O12 75.64(8) . . ?
O1 Ho1 O12 73.14(8) . . ?
O2 Ho1 O12 73.69(8) 2_556 . ?
O7 Ho1 O12 141.37(7) . . ?
O9 Ho1 O12 140.16(7) . . ?
O11 Ho1 O12 122.88(7) . . ?
O8 Ho1 Ho1 117.73(6) . 2_556 ?
O10 Ho1 Ho1 120.54(6) . 2_556 ?
O1 Ho1 Ho1 50.67(6) . 2_556 ?
O2 Ho1 Ho1 51.59(5) 2_556 2_556 ?
O7 Ho1 Ho1 124.79(5) . 2_556 ?
O9 Ho1 Ho1 120.65(5) . 2_556 ?
O11 Ho1 Ho1 64.27(4) . 2_556 ?
O12 Ho1 Ho1 58.63(5) . 2_556 ?
C1 O1 Ho1 155.5(2) . . ?
C1 O2 Ho1 153.0(2) . 2_556 ?
C9 O7 Ho1 134.6(2) . . ?
C11 O8 Ho1 137.6(2) . . ?
C14 O9 Ho1 133.5(2) . . ?
C16 O10 Ho1 137.2(2) . . ?
O3 N1 O4 124.9(4) . . ?
O3 N1 C4 117.9(3) . . ?
O4 N1 C4 117.2(4) . . ?
O5 N2 O6 124.5(3) . . ?
O5 N2 C6 118.1(3) . . ?
O6 N2 C6 117.4(3) . . ?
O2 C1 O1 127.1(3) . . ?
O2 C1 C2 116.5(2) . . ?
O1 C1 C2 116.5(3) . . ?
C7 C2 C3 119.7(3) . . ?
C7 C2 C1 120.0(3) . . ?
C3 C2 C1 120.3(3) . . ?
C4 C3 C2 118.9(3) . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
C5 C4 C3 123.0(3) . . ?
C5 C4 N1 117.9(3) . . ?
C3 C4 N1 119.1(3) . . ?
C4 C5 C6 116.6(3) . . ?
C4 C5 H5A 121.7 . . ?
C6 C5 H5A 121.7 . . ?
C5 C6 C7 123.1(3) . . ?
C5 C6 N2 117.9(3) . . ?
C7 C6 N2 119.0(3) . . ?
C6 C7 C2 118.6(3) . . ?
C6 C7 H7A 120.7 . . ?
C2 C7 H7A 120.7 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O7 C9 C10 124.9(3) . . ?
O7 C9 C8 115.4(3) . . ?
C10 C9 C8 119.7(3) . . ?
C9 C10 C11 124.3(3) . . ?
C9 C10 H10A 117.9 . . ?
C11 C10 H10A 117.9 . . ?
O8 C11 C10 123.8(3) . . ?
O8 C11 C12 117.3(3) . . ?
C10 C11 C12 118.9(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O9 C14 C15 125.4(3) . . ?
O9 C14 C13 116.1(3) . . ?
C15 C14 C13 118.5(3) . . ?
C14 C15 C16 124.0(3) . . ?
C14 C15 H15A 118 . . ?
C16 C15 H15A 118 . . ?
O10 C16 C15 124.3(3) . . ?
O10 C16 C17 116.7(3) . . ?
C15 C16 C17 119.0(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Ho1 O11 H1 120.4 . . ?
Ho1 O11 H2 115.7 . . ?
H1 O11 H2 99.3 . . ?
C183 O12 Ho1 134.9(9) . . ?
C182 O12 Ho1 124.9(6) . . ?
C18 O12 Ho1 132.7(3) . . ?
C183 O12 H3 112.6 . . ?
C182 O12 H3 126.2 . . ?
C18 O12 H3 111.7 . . ?
Ho1 O12 H3 108.4 . . ?
O12 C18 C19 111.4(6) . . ?
O12 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
O12 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O12 C182 C192 107.4(11) . . ?
O12 C182 H18C 110.2 . . ?
C192 C182 H18C 110.2 . . ?
O12 C182 H18D 110.2 . . ?
C192 C182 H18D 110.2 . . ?
H18C C182 H18D 108.5 . . ?
C182 C192 H19D 109.5 . . ?
C182 C192 H19E 109.5 . . ?
H19D C192 H19E 109.5 . . ?
C182 C192 H19F 109.5 . . ?
H19D C192 H19F 109.5 . . ?
H19E C192 H19F 109.5 . . ?
O12 C183 C193 110.2(15) . . ?
O12 C183 H18E 109.6 . . ?
C193 C183 H18E 109.6 . . ?
O12 C183 H18F 109.6 . . ?
C193 C183 H18F 109.6 . . ?
H18E C183 H18F 108.1 . . ?
C183 C193 H19G 109.5 . . ?
C183 C193 H19H 109.5 . . ?
H19G C193 H19H 109.5 . . ?
C183 C193 H19I 109.5 . . ?
H19G C193 H19I 109.5 . . ?
H19H C193 H19I 109.5 . . ?


# END of CIF
_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_6
_database_code_depnum_ccdc_archive 'CCDC 1554929'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;

_audit_creation_date             2017-05-20T08:08:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C38 H50 Er2 N4 O24'
_chemical_formula_sum            'C38 H50 Er2 N4 O24'
_chemical_formula_weight         1281.34

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1860(3)
_cell_length_b                   12.0866(5)
_cell_length_c                   13.1847(5)
_cell_angle_alpha                69.4010(10)
_cell_angle_beta                 89.6460(10)
_cell_angle_gamma                74.2250(10)
_cell_volume                     1169.30(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5099
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.49

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.82
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             634

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_T_max  0.746

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_number            16381
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.598
_diffrn_reflns_theta_max         30.113
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_reflns_Friedel_coverage         0
_reflns_number_total             6832
_reflns_number_gt                5733
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6832
_refine_ls_number_parameters     346
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.046
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0656
_refine_ls_wR_factor_gt          0.0614
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.14

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Er1 Er 0.27406(2) -0.12977(2) 0.45478(2) 0.01723(5) Uani 1 1 d . . . . .
O1 O 0.0820(3) 0.0532(2) 0.34326(19) 0.0285(5) Uani 1 1 d . . . . .
O2 O -0.1687(3) 0.1560(2) 0.37792(18) 0.0261(5) Uani 1 1 d . . . . .
O3 O 0.186(3) 0.1543(19) -0.047(2) 0.046(4) Uani 0.58 1 d . U P A 1
O4 O 0.119(4) 0.350(3) -0.141(2) 0.061(7) Uani 0.58 1 d . U P A 1
O32 O 0.204(5) 0.181(3) -0.042(3) 0.050(6) Uani 0.42 1 d . U P A 2
O42 O 0.123(4) 0.374(3) -0.141(2) 0.035(4) Uani 0.42 1 d . U P A 2
O5 O -0.4723(4) 0.5566(3) 0.0985(2) 0.0449(7) Uani 1 1 d . . . . .
O6 O -0.3483(4) 0.6308(3) -0.0447(2) 0.0513(8) Uani 1 1 d . . . . .
O7 O 0.5354(3) -0.2092(2) 0.56193(18) 0.0218(5) Uani 1 1 d . . . . .
O8 O 0.3296(3) -0.3387(2) 0.5242(2) 0.0261(5) Uani 1 1 d . . . . .
O9 O 0.4577(3) -0.0331(2) 0.34270(18) 0.0237(5) Uani 1 1 d . . . . .
O10 O 0.2750(3) -0.1761(2) 0.30227(19) 0.0280(5) Uani 1 1 d . . . . .
N1 N 0.1152(5) 0.2720(4) -0.0606(3) 0.0416(9) Uani 1 1 d . . . . .
N2 N -0.3599(4) 0.5474(3) 0.0395(3) 0.0344(7) Uani 1 1 d . . . . .
C1 C -0.0546(4) 0.1379(3) 0.3176(2) 0.0184(6) Uani 1 1 d . . . . .
C2 C -0.0825(4) 0.2311(3) 0.2015(2) 0.0181(6) Uani 1 1 d . . . . .
C3 C 0.0241(4) 0.2070(3) 0.1252(3) 0.0230(7) Uani 1 1 d . . . . .
H3A H 0.11149 0.131015 0.143369 0.028 Uiso 1 1 calc R U . . .
C4 C 0.0006(4) 0.2959(4) 0.0220(3) 0.0273(8) Uani 1 1 d . . . . .
C5 C -0.1206(4) 0.4083(3) -0.0083(3) 0.0273(8) Uani 1 1 d . . . . .
H5A H -0.131373 0.469513 -0.078906 0.033 Uiso 1 1 calc R U . . .
C6 C -0.2259(4) 0.4274(3) 0.0695(3) 0.0247(7) Uani 1 1 d . . . . .
C7 C -0.2116(4) 0.3413(3) 0.1739(3) 0.0202(6) Uani 1 1 d . . . . .
H7A H -0.287881 0.357296 0.224972 0.024 Uiso 1 1 calc R U . . .
C8 C 0.7803(5) -0.3209(4) 0.6880(3) 0.0343(9) Uani 1 1 d . . . . .
H8A H 0.750535 -0.272368 0.734905 0.052 Uiso 1 1 calc R U . . .
H8B H 0.854601 -0.286592 0.634865 0.052 Uiso 1 1 calc R U . . .
H8C H 0.83998 -0.406733 0.732683 0.052 Uiso 1 1 calc R U . . .
C9 C 0.6199(4) -0.3161(3) 0.6290(3) 0.0238(7) Uani 1 1 d . . . . .
C10 C 0.5725(4) -0.4226(3) 0.6510(3) 0.0264(7) Uani 1 1 d . . . . .
H10A H 0.642152 -0.496244 0.704457 0.032 Uiso 1 1 calc R U . . .
C11 C 0.4273(4) -0.4293(3) 0.5992(3) 0.0232(7) Uani 1 1 d . . . . .
C12 C 0.3851(5) -0.5495(3) 0.6327(3) 0.0308(8) Uani 1 1 d . . . . .
H12A H 0.318389 -0.551204 0.572118 0.046 Uiso 1 1 calc R U . . .
H12B H 0.318478 -0.558178 0.695598 0.046 Uiso 1 1 calc R U . . .
H12C H 0.490871 -0.61766 0.652319 0.046 Uiso 1 1 calc R U . . .
C13 C 0.5946(5) 0.0747(4) 0.1982(3) 0.0436(11) Uani 1 1 d . . . . .
H13A H 0.576089 0.108555 0.118483 0.065 Uiso 1 1 calc R U . . .
H13B H 0.714806 0.027754 0.221139 0.065 Uiso 1 1 calc R U . . .
H13C H 0.564964 0.142318 0.225792 0.065 Uiso 1 1 calc R U . . .
C14 C 0.4845(4) -0.0089(3) 0.2428(3) 0.0281(8) Uani 1 1 d . . . . .
C15 C 0.4161(5) -0.0542(4) 0.1742(3) 0.0336(9) Uani 1 1 d . . . . .
H15A H 0.438046 -0.027202 0.099902 0.04 Uiso 1 1 calc R U . . .
C16 C 0.3183(4) -0.1360(3) 0.2071(3) 0.0278(8) Uani 1 1 d . . . . .
C17 C 0.2551(6) -0.1792(4) 0.1249(3) 0.0421(10) Uani 1 1 d . . . . .
H17A H 0.204256 -0.245597 0.162164 0.063 Uiso 1 1 calc R U . . .
H17B H 0.350801 -0.2099 0.087556 0.063 Uiso 1 1 calc R U . . .
H17C H 0.16905 -0.110168 0.071575 0.063 Uiso 1 1 calc R U . . .
O11 O 0.3040(3) 0.0320(2) 0.51458(17) 0.0190(5) Uani 1 1 d . . . . .
H1 H 0.324878 0.096308 0.482023 0.023 Uiso 1 1 d R U . . .
H2 H 0.373788 0.015808 0.562523 0.023 Uiso 1 1 d R U . . .
O12 O 0.0009(3) -0.1719(2) 0.4417(2) 0.0277(5) Uani 1 1 d D . . . .
H3 H -0.087394 -0.118322 0.451942 0.033 Uiso 1 1 d R U . B .
C18 C -0.0710(8) -0.2171(6) 0.3666(6) 0.0252(14) Uani 0.52 1 d D . P B 1
H18A H -0.050917 -0.172726 0.290944 0.03 Uiso 0.52 1 calc R U P B 1
H18B H -0.195616 -0.20112 0.370476 0.03 Uiso 0.52 1 calc R U P B 1
C19 C 0.0127(11) -0.3544(7) 0.3979(7) 0.0335(18) Uani 0.52 1 d D . P B 1
H19A H -0.036641 -0.384386 0.34882 0.05 Uiso 0.52 1 calc R U P B 1
H19B H -0.006835 -0.397909 0.472981 0.05 Uiso 0.52 1 calc R U P B 1
H19C H 0.135554 -0.369589 0.391964 0.05 Uiso 0.52 1 calc R U P B 1
C182 C -0.014(3) -0.2868(17) 0.4157(18) 0.044(6) Uiso 0.24 1 d D . P B 2
H18C H 0.09699 -0.332213 0.399277 0.053 Uiso 0.24 1 calc R U P B 2
H18D H -0.056045 -0.344114 0.476639 0.053 Uiso 0.24 1 calc R U P B 2
C192 C -0.141(2) -0.2258(17) 0.3174(14) 0.042(4) Uiso 0.24 1 d D . P B 2
H19D H -0.161912 -0.288583 0.292516 0.063 Uiso 0.24 1 calc R U P B 2
H19E H -0.248025 -0.180225 0.335956 0.063 Uiso 0.24 1 calc R U P B 2
H19F H -0.096414 -0.168435 0.259314 0.063 Uiso 0.24 1 calc R U P B 2
C183 C -0.046(2) -0.2709(15) 0.4375(14) 0.031(4) Uiso 0.24 1 d D . P B 3
H18E H -0.171554 -0.25083 0.439151 0.037 Uiso 0.24 1 calc R U P B 3
H18F H 0.00447 -0.341361 0.505707 0.037 Uiso 0.24 1 calc R U P B 3
C193 C -0.005(4) -0.316(2) 0.3459(18) 0.061(8) Uiso 0.24 1 d D . P B 3
H19G H -0.047965 -0.38676 0.356559 0.092 Uiso 0.24 1 calc R U P B 3
H19H H -0.057806 -0.24959 0.276931 0.092 Uiso 0.24 1 calc R U P B 3
H19I H 0.119423 -0.340742 0.343943 0.092 Uiso 0.24 1 calc R U P B 3



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Er1 O10 2.269(2) . ?
Er1 O8 2.275(2) . ?
Er1 O2 2.312(2) 2_556 ?
Er1 O1 2.318(2) . ?
Er1 O7 2.337(2) . ?
Er1 O9 2.350(2) . ?
Er1 O11 2.419(2) . ?
Er1 O12 2.444(2) . ?
Er1 Er1 5.1291(3) 2_556 ?
O1 C1 1.246(4) . ?
O2 C1 1.247(4) . ?
O3 N1 1.33(2) . ?
O4 N1 1.15(3) . ?
O32 N1 1.08(3) . ?
O42 N1 1.33(3) . ?
O5 N2 1.209(4) . ?
O6 N2 1.233(4) . ?
O7 C9 1.284(4) . ?
O8 C11 1.260(4) . ?
O9 C14 1.276(4) . ?
O10 C16 1.263(4) . ?
N1 C4 1.487(5) . ?
N2 C6 1.483(4) . ?
C1 C2 1.521(4) . ?
C2 C3 1.385(4) . ?
C2 C7 1.387(4) . ?
C3 C4 1.380(5) . ?
C3 H3A 0.95 . ?
C4 C5 1.371(5) . ?
C5 C6 1.377(5) . ?
C5 H5A 0.95 . ?
C6 C7 1.385(4) . ?
C7 H7A 0.95 . ?
C8 C9 1.508(5) . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 C10 1.378(5) . ?
C10 C11 1.409(5) . ?
C10 H10A 0.95 . ?
C11 C12 1.498(5) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C14 1.500(5) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C15 1.397(5) . ?
C15 C16 1.390(5) . ?
C15 H15A 0.95 . ?
C16 C17 1.505(5) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
O11 H1 0.8089 . ?
O11 H2 0.788 . ?
O12 C183 1.372(13) . ?
O12 C18 1.479(6) . ?
O12 C182 1.577(15) . ?
O12 H3 0.8756 . ?
C18 C19 1.515(9) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C182 C192 1.495(17) . ?
C182 H18C 0.99 . ?
C182 H18D 0.99 . ?
C192 H19D 0.98 . ?
C192 H19E 0.98 . ?
C192 H19F 0.98 . ?
C183 C193 1.492(17) . ?
C183 H18E 0.99 . ?
C183 H18F 0.99 . ?
C193 H19G 0.98 . ?
C193 H19H 0.98 . ?
C193 H19I 0.98 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Er1 O8 77.66(9) . . ?
O10 Er1 O2 145.73(9) . 2_556 ?
O8 Er1 O2 79.92(9) . 2_556 ?
O10 Er1 O1 82.41(9) . . ?
O8 Er1 O1 144.38(9) . . ?
O2 Er1 O1 101.89(9) 2_556 . ?
O10 Er1 O7 114.99(8) . . ?
O8 Er1 O7 73.00(8) . . ?
O2 Er1 O7 82.18(8) 2_556 . ?
O1 Er1 O7 142.61(8) . . ?
O10 Er1 O9 73.11(8) . . ?
O8 Er1 O9 121.75(8) . . ?
O2 Er1 O9 141.16(8) 2_556 . ?
O1 Er1 O9 78.95(8) . . ?
O7 Er1 O9 75.58(8) . . ?
O10 Er1 O11 140.80(8) . . ?
O8 Er1 O11 138.12(8) . . ?
O2 Er1 O11 70.60(8) 2_556 . ?
O1 Er1 O11 72.53(8) . . ?
O7 Er1 O11 74.06(7) . . ?
O9 Er1 O11 72.85(8) . . ?
O10 Er1 O12 75.62(8) . . ?
O8 Er1 O12 73.72(8) . . ?
O2 Er1 O12 73.39(8) 2_556 . ?
O1 Er1 O12 72.88(9) . . ?
O7 Er1 O12 141.47(8) . . ?
O9 Er1 O12 140.10(8) . . ?
O11 Er1 O12 122.46(7) . . ?
O10 Er1 Er1 120.46(6) . 2_556 ?
O8 Er1 Er1 117.97(6) . 2_556 ?
O2 Er1 Er1 51.43(6) 2_556 2_556 ?
O1 Er1 Er1 50.68(6) . 2_556 ?
O7 Er1 Er1 124.55(6) . 2_556 ?
O9 Er1 Er1 120.27(6) . 2_556 ?
O11 Er1 Er1 63.85(5) . 2_556 ?
O12 Er1 Er1 58.63(5) . 2_556 ?
C1 O1 Er1 155.6(2) . . ?
C1 O2 Er1 153.7(2) . 2_556 ?
C9 O7 Er1 134.8(2) . . ?
C11 O8 Er1 137.8(2) . . ?
C14 O9 Er1 134.4(2) . . ?
C16 O10 Er1 137.2(2) . . ?
O4 N1 O3 121.3(19) . . ?
O32 N1 O42 125(2) . . ?
O32 N1 C4 119.7(18) . . ?
O4 N1 C4 121.1(15) . . ?
O3 N1 C4 116.3(12) . . ?
O42 N1 C4 113.6(16) . . ?
O5 N2 O6 124.7(3) . . ?
O5 N2 C6 118.1(3) . . ?
O6 N2 C6 117.2(3) . . ?
O1 C1 O2 126.7(3) . . ?
O1 C1 C2 116.5(3) . . ?
O2 C1 C2 116.7(3) . . ?
C3 C2 C7 120.4(3) . . ?
C3 C2 C1 119.9(3) . . ?
C7 C2 C1 119.6(3) . . ?
C4 C3 C2 118.5(3) . . ?
C4 C3 H3A 120.7 . . ?
C2 C3 H3A 120.7 . . ?
C5 C4 C3 123.4(3) . . ?
C5 C4 N1 117.5(3) . . ?
C3 C4 N1 119.1(3) . . ?
C4 C5 C6 116.2(3) . . ?
C4 C5 H5A 121.9 . . ?
C6 C5 H5A 121.9 . . ?
C5 C6 C7 123.5(3) . . ?
C5 C6 N2 117.8(3) . . ?
C7 C6 N2 118.8(3) . . ?
C6 C7 C2 118.0(3) . . ?
C6 C7 H7A 121 . . ?
C2 C7 H7A 121 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O7 C9 C10 124.9(3) . . ?
O7 C9 C8 115.6(3) . . ?
C10 C9 C8 119.4(3) . . ?
C9 C10 C11 124.2(3) . . ?
C9 C10 H10A 117.9 . . ?
C11 C10 H10A 117.9 . . ?
O8 C11 C10 123.4(3) . . ?
O8 C11 C12 117.2(3) . . ?
C10 C11 C12 119.5(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O9 C14 C15 123.9(3) . . ?
O9 C14 C13 116.8(3) . . ?
C15 C14 C13 119.3(3) . . ?
C16 C15 C14 124.5(3) . . ?
C16 C15 H15A 117.7 . . ?
C14 C15 H15A 117.7 . . ?
O10 C16 C15 124.3(3) . . ?
O10 C16 C17 116.6(4) . . ?
C15 C16 C17 119.0(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Er1 O11 H1 131.1 . . ?
Er1 O11 H2 119.2 . . ?
H1 O11 H2 91.1 . . ?
C183 O12 Er1 134.4(8) . . ?
C18 O12 Er1 131.7(3) . . ?
C182 O12 Er1 122.1(9) . . ?
C183 O12 H3 109.7 . . ?
C18 O12 H3 103.7 . . ?
C182 O12 H3 122.9 . . ?
Er1 O12 H3 115 . . ?
O12 C18 C19 109.6(6) . . ?
O12 C18 H18A 109.7 . . ?
C19 C18 H18A 109.7 . . ?
O12 C18 H18B 109.7 . . ?
C19 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C192 C182 O12 101.2(14) . . ?
C192 C182 H18C 111.5 . . ?
O12 C182 H18C 111.5 . . ?
C192 C182 H18D 111.5 . . ?
O12 C182 H18D 111.5 . . ?
H18C C182 H18D 109.3 . . ?
C182 C192 H19D 109.5 . . ?
C182 C192 H19E 109.5 . . ?
H19D C192 H19E 109.5 . . ?
C182 C192 H19F 109.5 . . ?
H19D C192 H19F 109.5 . . ?
H19E C192 H19F 109.5 . . ?
O12 C183 C193 121.0(15) . . ?
O12 C183 H18E 107.1 . . ?
C193 C183 H18E 107.1 . . ?
O12 C183 H18F 107.1 . . ?
C193 C183 H18F 107.1 . . ?
H18E C183 H18F 106.8 . . ?
C183 C193 H19G 109.5 . . ?
C183 C193 H19H 109.5 . . ?
H19G C193 H19H 109.5 . . ?
C183 C193 H19I 109.5 . . ?
H19G C193 H19I 109.5 . . ?
H19H C193 H19I 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H1 O7 0.81 1.95 2.707(3) 156.3 2_656
O11 H2 O9 0.79 1.97 2.725(3) 161.1 2_656
O12 H3 O11 0.88 1.93 2.792(3) 166.8 2_556


# END of CIF
_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_7
_database_code_depnum_ccdc_archive 'CCDC 1554930'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;

_audit_creation_date             2017-05-20T08:42:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C38 H50 N4 O24 Tm2'
_chemical_formula_sum            'C38 H50 N4 O24 Tm2'
_chemical_formula_weight         1284.68

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1770(4)
_cell_length_b                   12.1187(6)
_cell_length_c                   13.2254(6)
_cell_angle_alpha                69.2020(10)
_cell_angle_beta                 89.3350(10)
_cell_angle_gamma                74.1100(10)
_cell_volume                     1173.00(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9919
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      31.4

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             636

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_T_min  0.5948
_exptl_absorpt_correction_T_max  0.7465

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_number            31341
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.602
_diffrn_reflns_theta_max         33.163
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.954
_reflns_Friedel_coverage         0
_reflns_number_total             8546
_reflns_number_gt                7578
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8546
_refine_ls_number_parameters     327
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.023
_refine_ls_wR_factor_ref         0.0539
_refine_ls_wR_factor_gt          0.0509
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.279
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.112

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Tm1 Tm 0.27430(2) -0.12914(2) 0.45487(2) 0.01845(3) Uani 1 1 d . . . . .
O1 O 0.08354(19) 0.05267(13) 0.34370(12) 0.0293(3) Uani 1 1 d . . . . .
O2 O -0.16783(19) 0.15583(14) 0.37862(12) 0.0286(3) Uani 1 1 d . . . . .
O3 O 0.1924(3) 0.1637(2) -0.04393(17) 0.0727(8) Uani 1 1 d . . . . .
O4 O 0.1213(3) 0.3603(3) -0.14008(16) 0.0662(7) Uani 1 1 d . . . . .
O5 O -0.4715(3) 0.55558(18) 0.09894(17) 0.0535(5) Uani 1 1 d . . . . .
O6 O -0.3476(3) 0.62927(18) -0.04409(17) 0.0597(6) Uani 1 1 d . . . . .
O7 O 0.53393(17) -0.20766(13) 0.56179(11) 0.0241(3) Uani 1 1 d . . . . .
O8 O 0.32870(19) -0.33667(13) 0.52425(13) 0.0291(3) Uani 1 1 d . . . . .
O9 O 0.45709(18) -0.03176(14) 0.34337(11) 0.0257(3) Uani 1 1 d . . . . .
O10 O 0.2764(2) -0.17555(15) 0.30394(12) 0.0302(3) Uani 1 1 d . . . . .
N1 N 0.1147(3) 0.2705(3) -0.05961(17) 0.0480(6) Uani 1 1 d . . . . .
N2 N -0.3589(3) 0.54628(19) 0.03973(17) 0.0402(5) Uani 1 1 d . . . . .
C1 C -0.0530(2) 0.13756(17) 0.31880(15) 0.0194(3) Uani 1 1 d . . . . .
C2 C -0.0814(2) 0.22996(17) 0.20249(14) 0.0183(3) Uani 1 1 d . . . . .
C3 C 0.0253(3) 0.20558(19) 0.12592(16) 0.0235(4) Uani 1 1 d . . . . .
H3A H 0.112347 0.129466 0.143981 0.028 Uiso 1 1 calc R U . . .
C4 C 0.0019(3) 0.2949(2) 0.02238(16) 0.0295(5) Uani 1 1 d . . . . .
C5 C -0.1202(3) 0.4074(2) -0.00766(17) 0.0317(5) Uani 1 1 d . . . . .
H5A H -0.1313 0.468384 -0.078302 0.038 Uiso 1 1 calc R U . . .
C6 C -0.2253(3) 0.42669(19) 0.07000(17) 0.0280(4) Uani 1 1 d . . . . .
C7 C -0.2109(2) 0.34081(18) 0.17437(15) 0.0219(4) Uani 1 1 d . . . . .
H7A H -0.287346 0.357085 0.225411 0.026 Uiso 1 1 calc R U . . .
C8 C 0.7784(3) -0.3197(2) 0.6876(2) 0.0388(6) Uani 1 1 d . . . . .
H8A H 0.749676 -0.265822 0.729616 0.058 Uiso 1 1 calc R U . . .
H8B H 0.857196 -0.292072 0.634526 0.058 Uiso 1 1 calc R U . . .
H8C H 0.832723 -0.404578 0.736759 0.058 Uiso 1 1 calc R U . . .
C9 C 0.6175(3) -0.31429(19) 0.62885(16) 0.0250(4) Uani 1 1 d . . . . .
C10 C 0.5698(3) -0.4209(2) 0.65110(18) 0.0302(5) Uani 1 1 d . . . . .
H10A H 0.638055 -0.494418 0.70532 0.036 Uiso 1 1 calc R U . . .
C11 C 0.4264(3) -0.42701(18) 0.59829(17) 0.0252(4) Uani 1 1 d . . . . .
C12 C 0.3849(3) -0.5477(2) 0.6319(2) 0.0347(5) Uani 1 1 d . . . . .
H12A H 0.318516 -0.549397 0.571555 0.052 Uiso 1 1 calc R U . . .
H12B H 0.318058 -0.5568 0.6948 0.052 Uiso 1 1 calc R U . . .
H12C H 0.491137 -0.615486 0.651263 0.052 Uiso 1 1 calc R U . . .
C13 C 0.5951(4) 0.0764(3) 0.1987(2) 0.0470(7) Uani 1 1 d . . . . .
H13A H 0.577263 0.110696 0.119202 0.071 Uiso 1 1 calc R U . . .
H13B H 0.71534 0.029529 0.221725 0.071 Uiso 1 1 calc R U . . .
H13C H 0.564722 0.143639 0.226522 0.071 Uiso 1 1 calc R U . . .
C14 C 0.4834(3) -0.0084(2) 0.24334(17) 0.0299(5) Uani 1 1 d . . . . .
C15 C 0.4185(3) -0.0542(2) 0.17554(18) 0.0360(5) Uani 1 1 d . . . . .
H15A H 0.44252 -0.028181 0.101691 0.043 Uiso 1 1 calc R U . . .
C16 C 0.3205(3) -0.1360(2) 0.20884(18) 0.0310(5) Uani 1 1 d . . . . .
C17 C 0.2600(4) -0.1812(3) 0.1277(2) 0.0478(7) Uani 1 1 d . . . . .
H17A H 0.231626 -0.258033 0.166425 0.072 Uiso 1 1 calc R U . . .
H17B H 0.350571 -0.196006 0.080915 0.072 Uiso 1 1 calc R U . . .
H17C H 0.158317 -0.118793 0.08317 0.072 Uiso 1 1 calc R U . . .
O11 O 0.30398(16) 0.03187(12) 0.51475(11) 0.0200(3) Uani 1 1 d . . . . .
H1 H 0.365841 0.013761 0.573082 0.024 Uiso 1 1 d R U . . .
H2 H 0.345821 0.083311 0.472705 0.024 Uiso 1 1 d R U . . .
O12 O 0.00209(19) -0.17120(14) 0.44130(13) 0.0291(3) Uani 1 1 d D . . . .
H3 H -0.084001 -0.112866 0.462012 0.035 Uiso 1 1 d R U . A .
C18 C -0.0687(5) -0.2159(4) 0.3691(4) 0.0333(9) Uani 0.57 1 d D . P A 1
H18A H -0.051045 -0.169832 0.293349 0.04 Uiso 0.57 1 calc R U P A 1
H18B H -0.193269 -0.199945 0.374467 0.04 Uiso 0.57 1 calc R U P A 1
C19 C 0.0109(7) -0.3504(5) 0.3952(5) 0.0466(13) Uani 0.57 1 d D . P A 1
H19A H -0.040648 -0.376676 0.344526 0.07 Uiso 0.57 1 calc R U P A 1
H19B H 0.133915 -0.366381 0.388589 0.07 Uiso 0.57 1 calc R U P A 1
H19C H -0.008283 -0.396488 0.469692 0.07 Uiso 0.57 1 calc R U P A 1
C182 C -0.0181(14) -0.2757(10) 0.4188(10) 0.029(2) Uiso 0.25 1 d D . P A 2
H18C H -0.063691 -0.329147 0.480935 0.035 Uiso 0.25 1 calc R U P A 2
H18D H 0.093516 -0.325119 0.40703 0.035 Uiso 0.25 1 calc R U P A 2
C192 C -0.1383(15) -0.2271(11) 0.3202(9) 0.048(3) Uiso 0.25 1 d D . P A 2
H19D H -0.154459 -0.29589 0.302962 0.072 Uiso 0.25 1 calc R U P A 2
H19E H -0.248307 -0.178594 0.332879 0.072 Uiso 0.25 1 calc R U P A 2
H19F H -0.091724 -0.174582 0.259267 0.072 Uiso 0.25 1 calc R U P A 2
C183 C -0.0465(19) -0.2740(11) 0.4454(11) 0.026(3) Uiso 0.18 1 d D . P A 3
H18E H -0.1706 -0.257939 0.45277 0.031 Uiso 0.18 1 calc R U P A 3
H18F H 0.013994 -0.345289 0.510505 0.031 Uiso 0.18 1 calc R U P A 3
C193 C -0.008(4) -0.307(2) 0.3447(17) 0.073(8) Uiso 0.18 1 d D . P A 3
H19G H -0.044129 -0.379615 0.351583 0.11 Uiso 0.18 1 calc R U P A 3
H19H H -0.069192 -0.237393 0.280017 0.11 Uiso 0.18 1 calc R U P A 3
H19I H 0.115449 -0.324765 0.337767 0.11 Uiso 0.18 1 calc R U P A 3



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Tm1 O10 2.2565(15) . ?
Tm1 O8 2.2634(15) . ?
Tm1 O2 2.3057(14) 2_556 ?
Tm1 O1 2.3065(14) . ?
Tm1 O7 2.3281(14) . ?
Tm1 O9 2.3409(14) . ?
Tm1 O11 2.4196(14) . ?
Tm1 O12 2.4376(15) . ?
Tm1 Tm1 5.1171(2) 2_556 ?
O1 C1 1.246(2) . ?
O2 C1 1.245(2) . ?
O3 N1 1.219(3) . ?
O4 N1 1.236(3) . ?
O5 N2 1.209(3) . ?
O6 N2 1.227(3) . ?
O7 C9 1.281(2) . ?
O8 C11 1.254(2) . ?
O9 C14 1.280(2) . ?
O10 C16 1.264(3) . ?
N1 C4 1.473(3) . ?
N2 C6 1.478(3) . ?
C1 C2 1.522(2) . ?
C2 C3 1.387(3) . ?
C2 C7 1.393(3) . ?
C3 C4 1.387(3) . ?
C3 H3A 0.95 . ?
C4 C5 1.375(3) . ?
C5 C6 1.374(3) . ?
C5 H5A 0.95 . ?
C6 C7 1.385(3) . ?
C7 H7A 0.95 . ?
C8 C9 1.510(3) . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 C10 1.383(3) . ?
C10 C11 1.404(3) . ?
C10 H10A 0.95 . ?
C11 C12 1.502(3) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C14 1.519(3) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C15 1.386(4) . ?
C15 C16 1.391(4) . ?
C15 H15A 0.95 . ?
C16 C17 1.508(4) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
O11 H1 0.8527 . ?
O11 H2 0.8253 . ?
O12 C183 1.392(11) . ?
O12 C18 1.446(4) . ?
O12 C182 1.450(9) . ?
O12 H3 0.9648 . ?
C18 C19 1.492(6) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C182 C192 1.477(13) . ?
C182 H18C 0.99 . ?
C182 H18D 0.99 . ?
C192 H19D 0.98 . ?
C192 H19E 0.98 . ?
C192 H19F 0.98 . ?
C183 C193 1.527(16) . ?
C183 H18E 0.99 . ?
C183 H18F 0.99 . ?
C193 H19G 0.98 . ?
C193 H19H 0.98 . ?
C193 H19I 0.98 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Tm1 O8 77.57(6) . . ?
O10 Tm1 O2 145.47(6) . 2_556 ?
O8 Tm1 O2 79.66(6) . 2_556 ?
O10 Tm1 O1 82.42(6) . . ?
O8 Tm1 O1 144.22(6) . . ?
O2 Tm1 O1 102.08(5) 2_556 . ?
O10 Tm1 O7 115.22(5) . . ?
O8 Tm1 O7 73.30(5) . . ?
O2 Tm1 O7 82.01(5) 2_556 . ?
O1 Tm1 O7 142.48(5) . . ?
O10 Tm1 O9 73.45(5) . . ?
O8 Tm1 O9 122.31(5) . . ?
O2 Tm1 O9 141.07(5) 2_556 . ?
O1 Tm1 O9 78.62(5) . . ?
O7 Tm1 O9 75.76(5) . . ?
O10 Tm1 O11 141.09(5) . . ?
O8 Tm1 O11 137.96(5) . . ?
O2 Tm1 O11 70.66(5) 2_556 . ?
O1 Tm1 O11 72.79(5) . . ?
O7 Tm1 O11 73.66(5) . . ?
O9 Tm1 O11 72.60(5) . . ?
O10 Tm1 O12 75.31(5) . . ?
O8 Tm1 O12 73.50(5) . . ?
O2 Tm1 O12 73.53(5) 2_556 . ?
O1 Tm1 O12 72.89(5) . . ?
O7 Tm1 O12 141.59(5) . . ?
O9 Tm1 O12 139.90(5) . . ?
O11 Tm1 O12 122.72(5) . . ?
O10 Tm1 Tm1 120.54(4) . 2_556 ?
O8 Tm1 Tm1 117.73(4) . 2_556 ?
O2 Tm1 Tm1 51.43(4) 2_556 2_556 ?
O1 Tm1 Tm1 50.86(4) . 2_556 ?
O7 Tm1 Tm1 124.23(4) . 2_556 ?
O9 Tm1 Tm1 119.96(4) . 2_556 ?
O11 Tm1 Tm1 63.91(3) . 2_556 ?
O12 Tm1 Tm1 58.83(4) . 2_556 ?
C1 O1 Tm1 155.25(14) . . ?
C1 O2 Tm1 153.50(14) . 2_556 ?
C9 O7 Tm1 134.52(14) . . ?
C11 O8 Tm1 137.90(15) . . ?
C14 O9 Tm1 133.52(14) . . ?
C16 O10 Tm1 137.30(16) . . ?
O3 N1 O4 125.0(2) . . ?
O3 N1 C4 117.8(2) . . ?
O4 N1 C4 117.2(2) . . ?
O5 N2 O6 124.6(2) . . ?
O5 N2 C6 118.0(2) . . ?
O6 N2 C6 117.4(2) . . ?
O2 C1 O1 127.29(18) . . ?
O2 C1 C2 116.50(17) . . ?
O1 C1 C2 116.21(17) . . ?
C3 C2 C7 120.23(17) . . ?
C3 C2 C1 120.04(17) . . ?
C7 C2 C1 119.69(17) . . ?
C4 C3 C2 118.46(19) . . ?
C4 C3 H3A 120.8 . . ?
C2 C3 H3A 120.8 . . ?
C5 C4 C3 123.2(2) . . ?
C5 C4 N1 117.7(2) . . ?
C3 C4 N1 119.0(2) . . ?
C6 C5 C4 116.40(19) . . ?
C6 C5 H5A 121.8 . . ?
C4 C5 H5A 121.8 . . ?
C5 C6 C7 123.4(2) . . ?
C5 C6 N2 117.64(19) . . ?
C7 C6 N2 118.9(2) . . ?
C6 C7 C2 118.23(18) . . ?
C6 C7 H7A 120.9 . . ?
C2 C7 H7A 120.9 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O7 C9 C10 125.0(2) . . ?
O7 C9 C8 115.68(19) . . ?
C10 C9 C8 119.30(19) . . ?
C9 C10 C11 123.88(19) . . ?
C9 C10 H10A 118.1 . . ?
C11 C10 H10A 118.1 . . ?
O8 C11 C10 123.74(19) . . ?
O8 C11 C12 117.4(2) . . ?
C10 C11 C12 118.88(19) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O9 C14 C15 125.0(2) . . ?
O9 C14 C13 115.7(2) . . ?
C15 C14 C13 119.3(2) . . ?
C14 C15 C16 124.1(2) . . ?
C14 C15 H15A 118 . . ?
C16 C15 H15A 118 . . ?
O10 C16 C15 124.3(2) . . ?
O10 C16 C17 116.6(2) . . ?
C15 C16 C17 119.1(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Tm1 O11 H1 120.3 . . ?
Tm1 O11 H2 116 . . ?
H1 O11 H2 99.2 . . ?
C183 O12 Tm1 134.9(6) . . ?
C18 O12 Tm1 132.46(19) . . ?
C182 O12 Tm1 124.5(5) . . ?
C183 O12 H3 113.4 . . ?
C18 O12 H3 112.4 . . ?
C182 O12 H3 127.1 . . ?
Tm1 O12 H3 107.9 . . ?
O12 C18 C19 112.2(4) . . ?
O12 C18 H18A 109.2 . . ?
C19 C18 H18A 109.2 . . ?
O12 C18 H18B 109.2 . . ?
C19 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O12 C182 C192 107.6(9) . . ?
O12 C182 H18C 110.2 . . ?
C192 C182 H18C 110.2 . . ?
O12 C182 H18D 110.2 . . ?
C192 C182 H18D 110.2 . . ?
H18C C182 H18D 108.5 . . ?
C182 C192 H19D 109.5 . . ?
C182 C192 H19E 109.5 . . ?
H19D C192 H19E 109.5 . . ?
C182 C192 H19F 109.5 . . ?
H19D C192 H19F 109.5 . . ?
H19E C192 H19F 109.5 . . ?
O12 C183 C193 112.7(13) . . ?
O12 C183 H18E 109 . . ?
C193 C183 H18E 109 . . ?
O12 C183 H18F 109 . . ?
C193 C183 H18F 109 . . ?
H18E C183 H18F 107.8 . . ?
C183 C193 H19G 109.5 . . ?
C183 C193 H19H 109.5 . . ?
H19G C193 H19H 109.5 . . ?
C183 C193 H19I 109.5 . . ?
H19G C193 H19I 109.5 . . ?
H19H C193 H19I 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C12 H12C O10 0.98 2.59 3.548(3) 166.1 2_646
O11 H1 O9 0.85 1.94 2.724(2) 153.2 2_656
O11 H2 O7 0.83 1.94 2.7025(19) 153.5 2_656
O12 H3 O11 0.96 1.88 2.793(2) 157.3 2_556


# END of CIF
_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_8
_database_code_depnum_ccdc_archive 'CCDC 1554931'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;

_audit_creation_date             2017-05-20T08:38:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C38 H50 N4 O24 Yb2'
_chemical_formula_sum            'C38 H50 N4 O24 Yb2'
_chemical_formula_weight         1292.9

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1618(4)
_cell_length_b                   12.1248(7)
_cell_length_c                   13.1973(7)
_cell_angle_alpha                69.077(2)
_cell_angle_beta                 89.278(2)
_cell_angle_gamma                74.064(2)
_cell_volume                     1167.69(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5559
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      27.55

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             638

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.07
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_T_min  0.5283
_exptl_absorpt_correction_T_max  0.7458

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_number            15398
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.607
_diffrn_reflns_theta_max         29.215
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_reflns_Friedel_coverage         0
_reflns_number_total             6300
_reflns_number_gt                5466
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6300
_refine_ls_number_parameters     327
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0627
_refine_ls_wR_factor_gt          0.0593
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.981
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.623
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.123

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.385 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Yb1 Yb 0.27457(2) -0.12893(2) 0.45504(2) 0.02132(5) Uani 1 1 d . . . . .
O1 O 0.0848(3) 0.0520(2) 0.34440(18) 0.0313(5) Uani 1 1 d . . . . .
O2 O -0.1673(3) 0.1550(2) 0.37981(18) 0.0307(5) Uani 1 1 d . . . . .
O3 O 0.1920(5) 0.1637(4) -0.0446(3) 0.0780(12) Uani 1 1 d . . . . .
O4 O 0.1208(5) 0.3599(4) -0.1402(2) 0.0693(10) Uani 1 1 d . . . . .
O5 O -0.4717(4) 0.5551(3) 0.0991(3) 0.0566(8) Uani 1 1 d . . . . .
O6 O -0.3473(4) 0.6290(3) -0.0441(3) 0.0643(10) Uani 1 1 d . . . . .
O7 O 0.5337(3) -0.2074(2) 0.56118(18) 0.0271(5) Uani 1 1 d . . . . .
O8 O 0.3282(3) -0.3353(2) 0.52378(19) 0.0313(5) Uani 1 1 d . . . . .
O9 O 0.4575(3) -0.0317(2) 0.34399(17) 0.0285(5) Uani 1 1 d . . . . .
O10 O 0.2785(3) -0.1760(2) 0.30516(19) 0.0322(5) Uani 1 1 d . . . . .
N1 N 0.1142(5) 0.2708(4) -0.0598(3) 0.0526(10) Uani 1 1 d . . . . .
N2 N -0.3589(5) 0.5459(3) 0.0405(3) 0.0441(8) Uani 1 1 d . . . . .
C1 C -0.0529(4) 0.1373(3) 0.3199(2) 0.0222(6) Uani 1 1 d . . . . .
C2 C -0.0806(4) 0.2293(3) 0.2031(2) 0.0204(6) Uani 1 1 d . . . . .
C3 C 0.0250(4) 0.2055(3) 0.1260(3) 0.0263(7) Uani 1 1 d . . . . .
H3A H 0.111764 0.129119 0.144028 0.032 Uiso 1 1 calc R U . . .
C4 C 0.0026(4) 0.2946(3) 0.0223(3) 0.0311(7) Uani 1 1 d . . . . .
C5 C -0.1205(5) 0.4074(3) -0.0073(3) 0.0346(8) Uani 1 1 d . . . . .
H5A H -0.132024 0.468736 -0.078127 0.041 Uiso 1 1 calc R U . . .
C6 C -0.2249(4) 0.4264(3) 0.0703(3) 0.0305(7) Uani 1 1 d . . . . .
C7 C -0.2099(4) 0.3397(3) 0.1751(2) 0.0247(6) Uani 1 1 d . . . . .
H7A H -0.286422 0.35564 0.226389 0.03 Uiso 1 1 calc R U . . .
C8 C 0.7788(5) -0.3196(4) 0.6868(3) 0.0410(9) Uani 1 1 d . . . . .
H8A H 0.749659 -0.268914 0.731599 0.061 Uiso 1 1 calc R U . . .
H8B H 0.855491 -0.288401 0.633367 0.061 Uiso 1 1 calc R U . . .
H8C H 0.835956 -0.405263 0.733511 0.061 Uiso 1 1 calc R U . . .
C9 C 0.6189(4) -0.3139(3) 0.6285(3) 0.0270(7) Uani 1 1 d . . . . .
C10 C 0.5695(4) -0.4198(3) 0.6504(3) 0.0318(8) Uani 1 1 d . . . . .
H10A H 0.63759 -0.493575 0.704815 0.038 Uiso 1 1 calc R U . . .
C11 C 0.4270(4) -0.4259(3) 0.5982(3) 0.0285(7) Uani 1 1 d . . . . .
C12 C 0.3835(5) -0.5463(3) 0.6314(3) 0.0396(9) Uani 1 1 d . . . . .
H12A H 0.313089 -0.545809 0.571517 0.059 Uiso 1 1 calc R U . . .
H12B H 0.319873 -0.556739 0.69597 0.059 Uiso 1 1 calc R U . . .
H12C H 0.489202 -0.614569 0.648186 0.059 Uiso 1 1 calc R U . . .
C13 C 0.5963(6) 0.0770(4) 0.1985(3) 0.0506(11) Uani 1 1 d . . . . .
H13A H 0.583962 0.106716 0.118741 0.076 Uiso 1 1 calc R U . . .
H13B H 0.716136 0.031499 0.225506 0.076 Uiso 1 1 calc R U . . .
H13C H 0.560789 0.147357 0.222086 0.076 Uiso 1 1 calc R U . . .
C14 C 0.4841(4) -0.0081(4) 0.2440(3) 0.0346(8) Uani 1 1 d . . . . .
C15 C 0.4204(5) -0.0546(4) 0.1765(3) 0.0380(9) Uani 1 1 d . . . . .
H15A H 0.445459 -0.029046 0.102602 0.046 Uiso 1 1 calc R U . . .
C16 C 0.3221(5) -0.1363(3) 0.2095(3) 0.0348(8) Uani 1 1 d . . . . .
C17 C 0.2625(6) -0.1820(4) 0.1291(3) 0.0527(11) Uani 1 1 d . . . . .
H17A H 0.231028 -0.257575 0.168329 0.079 Uiso 1 1 calc R U . . .
H17B H 0.354869 -0.199508 0.083895 0.079 Uiso 1 1 calc R U . . .
H17C H 0.16281 -0.118854 0.082635 0.079 Uiso 1 1 calc R U . . .
O11 O 0.3035(3) 0.03111(19) 0.51435(17) 0.0231(5) Uani 1 1 d . . . . .
H1 H 0.365329 0.013 0.572679 0.028 Uiso 1 1 d R U . . .
H2 H 0.345309 0.08255 0.4723 0.028 Uiso 1 1 d R U . . .
O12 O 0.0028(3) -0.1706(2) 0.4409(2) 0.0326(5) Uani 1 1 d D . . . .
H3 H -0.083269 -0.112246 0.461564 0.039 Uiso 1 1 d R U . A .
C18 C -0.0695(8) -0.2136(6) 0.3684(6) 0.0337(15) Uani 0.55 1 d D . P A 1
H18A H -0.050798 -0.168028 0.292445 0.04 Uiso 0.55 1 calc R U P A 1
H18B H -0.194435 -0.19669 0.373494 0.04 Uiso 0.55 1 calc R U P A 1
C19 C 0.0099(10) -0.3493(7) 0.3960(8) 0.0453(19) Uani 0.55 1 d D . P A 1
H19A H -0.041639 -0.375947 0.345535 0.068 Uiso 0.55 1 calc R U P A 1
H19B H 0.133338 -0.366039 0.389827 0.068 Uiso 0.55 1 calc R U P A 1
H19C H -0.010164 -0.394674 0.4708 0.068 Uiso 0.55 1 calc R U P A 1
C182 C -0.014(3) -0.2736(16) 0.4163(16) 0.041(5) Uiso 0.26 1 d D . P A 2
H18C H -0.05243 -0.331324 0.479693 0.049 Uiso 0.26 1 calc R U P A 2
H18D H 0.097213 -0.31858 0.399929 0.049 Uiso 0.26 1 calc R U P A 2
C192 C -0.143(2) -0.2256(18) 0.3203(14) 0.059(5) Uiso 0.26 1 d D . P A 2
H19D H -0.156342 -0.294545 0.302304 0.088 Uiso 0.26 1 calc R U P A 2
H19E H -0.252961 -0.181641 0.337393 0.088 Uiso 0.26 1 calc R U P A 2
H19F H -0.103832 -0.168941 0.257903 0.088 Uiso 0.26 1 calc R U P A 2
C183 C -0.044(3) -0.2779(16) 0.4438(16) 0.027(5) Uiso 0.19 1 d D . P A 3
H18E H -0.167933 -0.264642 0.45205 0.032 Uiso 0.19 1 calc R U P A 3
H18F H 0.019589 -0.350325 0.507465 0.032 Uiso 0.19 1 calc R U P A 3
C193 C -0.004(5) -0.303(3) 0.341(2) 0.083(12) Uiso 0.19 1 d D . P A 3
H19G H -0.036646 -0.375887 0.343882 0.125 Uiso 0.19 1 calc R U P A 3
H19H H -0.068364 -0.231458 0.277665 0.125 Uiso 0.19 1 calc R U P A 3
H19I H 0.118867 -0.317007 0.332994 0.125 Uiso 0.19 1 calc R U P A 3



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Yb1 O10 2.243(2) . ?
Yb1 O8 2.250(2) . ?
Yb1 O2 2.287(2) 2_556 ?
Yb1 O1 2.290(2) . ?
Yb1 O7 2.315(2) . ?
Yb1 O9 2.333(2) . ?
Yb1 O11 2.403(2) . ?
Yb1 O12 2.429(2) . ?
Yb1 Yb1 5.1081(3) 2_556 ?
O1 C1 1.253(4) . ?
O2 C1 1.240(4) . ?
O3 N1 1.223(5) . ?
O4 N1 1.228(5) . ?
O5 N2 1.202(4) . ?
O6 N2 1.233(4) . ?
O7 C9 1.282(4) . ?
O8 C11 1.259(4) . ?
O9 C14 1.275(4) . ?
O10 C16 1.265(4) . ?
N1 C4 1.463(5) . ?
N2 C6 1.477(4) . ?
C1 C2 1.521(4) . ?
C2 C3 1.383(4) . ?
C2 C7 1.386(4) . ?
C3 C4 1.385(4) . ?
C3 H3A 0.95 . ?
C4 C5 1.380(5) . ?
C5 C6 1.366(5) . ?
C5 H5A 0.95 . ?
C6 C7 1.389(4) . ?
C7 H7A 0.95 . ?
C8 C9 1.496(5) . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 C10 1.383(5) . ?
C10 C11 1.391(5) . ?
C10 H10A 0.95 . ?
C11 C12 1.508(5) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C14 1.525(5) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C15 1.384(5) . ?
C15 C16 1.391(5) . ?
C15 H15A 0.95 . ?
C16 C17 1.500(5) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
O11 H1 0.8508 . ?
O11 H2 0.8237 . ?
O12 C182 1.439(14) . ?
O12 C18 1.440(7) . ?
O12 C183 1.441(14) . ?
O12 H3 0.9638 . ?
C18 C19 1.501(9) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C182 C192 1.489(16) . ?
C182 H18C 0.99 . ?
C182 H18D 0.99 . ?
C192 H19D 0.98 . ?
C192 H19E 0.98 . ?
C192 H19F 0.98 . ?
C183 C193 1.512(18) . ?
C183 H18E 0.99 . ?
C183 H18F 0.99 . ?
C193 H19G 0.98 . ?
C193 H19H 0.98 . ?
C193 H19I 0.98 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Yb1 O8 77.09(9) . . ?
O10 Yb1 O2 145.39(9) . 2_556 ?
O8 Yb1 O2 79.91(9) . 2_556 ?
O10 Yb1 O1 82.89(9) . . ?
O8 Yb1 O1 144.08(9) . . ?
O2 Yb1 O1 101.76(8) 2_556 . ?
O10 Yb1 O7 114.64(8) . . ?
O8 Yb1 O7 73.47(8) . . ?
O2 Yb1 O7 82.49(8) 2_556 . ?
O1 Yb1 O7 142.44(8) . . ?
O10 Yb1 O9 73.58(8) . . ?
O8 Yb1 O9 122.34(8) . . ?
O2 Yb1 O9 141.03(8) 2_556 . ?
O1 Yb1 O9 78.68(8) . . ?
O7 Yb1 O9 75.50(8) . . ?
O10 Yb1 O11 141.23(8) . . ?
O8 Yb1 O11 138.26(8) . . ?
O2 Yb1 O11 70.67(8) 2_556 . ?
O1 Yb1 O11 72.60(8) . . ?
O7 Yb1 O11 73.89(7) . . ?
O9 Yb1 O11 72.48(8) . . ?
O10 Yb1 O12 75.34(8) . . ?
O8 Yb1 O12 73.38(8) . . ?
O2 Yb1 O12 73.50(8) 2_556 . ?
O1 Yb1 O12 72.84(8) . . ?
O7 Yb1 O12 141.80(8) . . ?
O9 Yb1 O12 139.87(8) . . ?
O11 Yb1 O12 122.74(7) . . ?
O10 Yb1 Yb1 120.89(6) . 2_556 ?
O8 Yb1 Yb1 117.71(6) . 2_556 ?
O2 Yb1 Yb1 51.17(6) 2_556 2_556 ?
O1 Yb1 Yb1 50.79(6) . 2_556 ?
O7 Yb1 Yb1 124.46(6) . 2_556 ?
O9 Yb1 Yb1 119.94(6) . 2_556 ?
O11 Yb1 Yb1 63.85(5) . 2_556 ?
O12 Yb1 Yb1 58.89(5) . 2_556 ?
C1 O1 Yb1 155.0(2) . . ?
C1 O2 Yb1 154.0(2) . 2_556 ?
C9 O7 Yb1 135.1(2) . . ?
C11 O8 Yb1 137.5(2) . . ?
C14 O9 Yb1 133.5(2) . . ?
C16 O10 Yb1 137.5(2) . . ?
O3 N1 O4 124.6(4) . . ?
O3 N1 C4 117.9(4) . . ?
O4 N1 C4 117.5(4) . . ?
O5 N2 O6 124.6(3) . . ?
O5 N2 C6 118.4(3) . . ?
O6 N2 C6 117.0(4) . . ?
O2 C1 O1 127.5(3) . . ?
O2 C1 C2 116.9(3) . . ?
O1 C1 C2 115.6(3) . . ?
C3 C2 C7 120.0(3) . . ?
C3 C2 C1 120.6(3) . . ?
C7 C2 C1 119.4(3) . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3A 120.5 . . ?
C4 C3 H3A 120.5 . . ?
C5 C4 C3 122.5(3) . . ?
C5 C4 N1 117.9(3) . . ?
C3 C4 N1 119.6(3) . . ?
C6 C5 C4 116.7(3) . . ?
C6 C5 H5A 121.7 . . ?
C4 C5 H5A 121.7 . . ?
C5 C6 C7 123.2(3) . . ?
C5 C6 N2 117.9(3) . . ?
C7 C6 N2 118.9(3) . . ?
C2 C7 C6 118.5(3) . . ?
C2 C7 H7A 120.8 . . ?
C6 C7 H7A 120.8 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O7 C9 C10 123.9(3) . . ?
O7 C9 C8 116.3(3) . . ?
C10 C9 C8 119.8(3) . . ?
C9 C10 C11 124.5(3) . . ?
C9 C10 H10A 117.7 . . ?
C11 C10 H10A 117.7 . . ?
O8 C11 C10 123.9(3) . . ?
O8 C11 C12 116.5(3) . . ?
C10 C11 C12 119.6(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O9 C14 C15 124.8(3) . . ?
O9 C14 C13 116.1(3) . . ?
C15 C14 C13 119.1(3) . . ?
C14 C15 C16 124.4(3) . . ?
C14 C15 H15A 117.8 . . ?
C16 C15 H15A 117.8 . . ?
O10 C16 C15 123.8(3) . . ?
O10 C16 C17 116.7(4) . . ?
C15 C16 C17 119.5(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Yb1 O11 H1 120.2 . . ?
Yb1 O11 H2 116.1 . . ?
H1 O11 H2 99.1 . . ?
C182 O12 Yb1 123.6(8) . . ?
C18 O12 Yb1 133.0(3) . . ?
C183 O12 Yb1 133.8(9) . . ?
C182 O12 H3 128.4 . . ?
C18 O12 H3 111.8 . . ?
C183 O12 H3 114.8 . . ?
Yb1 O12 H3 107.8 . . ?
O12 C18 C19 111.3(6) . . ?
O12 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
O12 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O12 C182 C192 108.3(14) . . ?
O12 C182 H18C 110 . . ?
C192 C182 H18C 110 . . ?
O12 C182 H18D 110 . . ?
C192 C182 H18D 110 . . ?
H18C C182 H18D 108.4 . . ?
C182 C192 H19D 109.5 . . ?
C182 C192 H19E 109.5 . . ?
H19D C192 H19E 109.5 . . ?
C182 C192 H19F 109.5 . . ?
H19D C192 H19F 109.5 . . ?
H19E C192 H19F 109.5 . . ?
O12 C183 C193 110.5(18) . . ?
O12 C183 H18E 109.5 . . ?
C193 C183 H18E 109.5 . . ?
O12 C183 H18F 109.5 . . ?
C193 C183 H18F 109.5 . . ?
H18E C183 H18F 108.1 . . ?
C183 C193 H19G 109.5 . . ?
C183 C193 H19H 109.5 . . ?
H19G C193 H19H 109.5 . . ?
C183 C193 H19I 109.5 . . ?
H19G C193 H19I 109.5 . . ?
H19H C193 H19I 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C12 H12C O10 0.98 2.59 3.549(4) 167.1 2_646
O11 H1 O9 0.85 1.94 2.723(3) 153 2_656
O11 H2 O7 0.82 1.95 2.708(3) 153.1 2_656
O12 H3 O11 0.96 1.88 2.795(3) 157.4 2_556


# END of CIF
_exptl_crystal_preparation       ', Magnetic properties'
