# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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 1554984'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;

_audit_creation_date             2017-03-24T17:36:23-00:00
_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         'C15 H21 Ho N2 O8'
_chemical_formula_sum            'C15 H21 Ho N2 O8'
_chemical_formula_weight         522.27

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.7665(4)
_cell_length_b                   29.8018(15)
_cell_length_c                   8.2632(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.8680(10)
_cell_angle_gamma                90
_cell_volume                     1839.68(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9501
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      31.04

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

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1024

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

_exptl_absorpt_coefficient_mu    4.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_T_min  0.5243
_exptl_absorpt_correction_T_max  0.7462

#----------------------------------------------------------------------------#
#                   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  0.0329
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_number            22854
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.652
_diffrn_reflns_theta_max         31.064
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.991
_reflns_Friedel_coverage         0
_reflns_number_total             5845
_reflns_number_gt                5491
_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)+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5845
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.039
_refine_ls_wR_factor_ref         0.0728
_refine_ls_wR_factor_gt          0.0721
_refine_ls_goodness_of_fit_ref   1.562
_refine_ls_restrained_S_all      1.562
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.76
_refine_diff_density_min         -1.881
_refine_diff_density_rms         0.141

#----------------------------------------------------------------------------#
#                   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 0.27361(2) 0.09469(2) 0.18497(2) 0.01338(5) Uani 1 1 d . . . . .
O1 O 0.4540(3) 0.09605(9) 0.4572(3) 0.0187(5) Uani 1 1 d . . . . .
O2 O 0.5391(4) 0.12294(10) 0.1668(3) 0.0207(6) Uani 1 1 d . . . . .
O3 O 0.2202(4) 0.16327(9) 0.2818(3) 0.0207(6) Uani 1 1 d . . . . .
O4 O 0.1736(4) 0.13938(9) -0.0506(4) 0.0222(6) Uani 1 1 d . . . . .
O5 O -0.0048(4) 0.06340(10) 0.0376(3) 0.0185(5) Uani 1 1 d . . . . .
O6 O -0.2712(3) 0.03245(9) 0.0237(3) 0.0173(5) Uani 1 1 d . . . . .
O7 O 0.3283(4) 0.01650(9) 0.2613(3) 0.0181(5) Uani 1 1 d . . . . .
H1 H 0.305284 0.000131 0.181462 0.022 Uiso 1 1 d R U . . .
H2 H 0.271384 0.005431 0.321262 0.022 Uiso 1 1 d R U . . .
O8 O 0.3602(4) 0.05625(9) -0.0397(3) 0.0182(5) Uani 1 1 d . . . . .
H3 H 0.351525 0.028838 -0.042898 0.022 Uiso 1 1 d R U . . .
H4 H 0.465025 0.057638 -0.034998 0.022 Uiso 1 1 d R U . . .
N1 N 0.0640(4) 0.07586(10) 0.3693(4) 0.0139(6) Uani 1 1 d . . . . .
N2 N -0.1628(4) 0.03902(11) 0.5446(4) 0.0170(6) Uani 1 1 d . . . . .
C1 C 0.6299(6) 0.12403(16) 0.7177(5) 0.0286(9) Uani 1 1 d . . . . .
H1A H 0.655442 0.093558 0.762383 0.043 Uiso 1 1 calc R U . . .
H1B H 0.530387 0.136628 0.754682 0.043 Uiso 1 1 calc R U . . .
H1C H 0.736332 0.142837 0.759233 0.043 Uiso 1 1 calc R U . . .
C2 C 0.5796(5) 0.12259(13) 0.5274(5) 0.0190(7) Uani 1 1 d . . . . .
C3 C 0.6755(6) 0.14890(14) 0.4417(5) 0.0237(8) Uani 1 1 d . . . . .
H3A H 0.761412 0.169342 0.505628 0.028 Uiso 1 1 calc R U . . .
C4 C 0.6530(5) 0.14704(13) 0.2679(5) 0.0193(7) Uani 1 1 d . . . . .
C5 C 0.7736(6) 0.17463(16) 0.1914(6) 0.0301(9) Uani 1 1 d . . . . .
H5A H 0.701307 0.196021 0.110784 0.045 Uiso 1 1 calc R U . . .
H5B H 0.837791 0.15478 0.133233 0.045 Uiso 1 1 calc R U . . .
H5C H 0.860005 0.19103 0.280405 0.045 Uiso 1 1 calc R U . . .
C6 C 0.2338(8) 0.24019(16) 0.3495(6) 0.0355(11) Uani 1 1 d . . . . .
H6A H 0.130781 0.238834 0.396316 0.053 Uiso 1 1 calc R U . . .
H6B H 0.233753 0.269026 0.292455 0.053 Uiso 1 1 calc R U . . .
H6C H 0.344575 0.237217 0.440554 0.053 Uiso 1 1 calc R U . . .
C7 C 0.2218(6) 0.20255(14) 0.2253(5) 0.0235(8) Uani 1 1 d . . . . .
C8 C 0.2101(7) 0.21301(15) 0.0586(6) 0.0299(10) Uani 1 1 d . . . . .
H8A H 0.222167 0.243562 0.030706 0.036 Uiso 1 1 calc R U . . .
C9 C 0.1816(6) 0.18103(15) -0.0708(5) 0.0244(8) Uani 1 1 d . . . . .
C10 C 0.1569(8) 0.19740(17) -0.2489(6) 0.0361(11) Uani 1 1 d . . . . .
H10A H 0.074503 0.177332 -0.327401 0.054 Uiso 1 1 calc R U . . .
H10B H 0.272806 0.197638 -0.274607 0.054 Uiso 1 1 calc R U . . .
H10C H 0.107246 0.227837 -0.26022 0.054 Uiso 1 1 calc R U . . .
C11 C -0.0877(5) 0.05481(12) 0.2897(4) 0.0121(6) Uani 1 1 d . . . . .
C12 C -0.2014(5) 0.03682(12) 0.3774(4) 0.0145(7) Uani 1 1 d . . . . .
H12A H -0.309233 0.022643 0.316423 0.017 Uiso 1 1 calc R U . . .
C13 C -0.0148(5) 0.06123(14) 0.6232(5) 0.0184(7) Uani 1 1 d . . . . .
H13A H 0.014193 0.064595 0.741926 0.022 Uiso 1 1 calc R U . . .
C14 C 0.0983(5) 0.07964(13) 0.5366(5) 0.0172(7) Uani 1 1 d . . . . .
H14A H 0.202518 0.095288 0.597458 0.021 Uiso 1 1 calc R U . . .
C15 C -0.1239(5) 0.04978(12) 0.1021(4) 0.0139(6) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   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 O2 2.270(3) . ?
Ho1 O3 2.274(3) . ?
Ho1 O1 2.302(3) . ?
Ho1 O4 2.311(3) . ?
Ho1 O5 2.364(3) . ?
Ho1 O7 2.421(3) . ?
Ho1 O8 2.427(3) . ?
Ho1 N1 2.577(3) . ?
O1 C2 1.266(5) . ?
O2 C4 1.262(5) . ?
O3 C7 1.262(5) . ?
O4 C9 1.256(5) . ?
O5 C15 1.255(4) . ?
O6 C15 1.261(4) . ?
O7 H1 0.8005 . ?
O7 H2 0.8181 . ?
O8 H3 0.8195 . ?
O8 H4 0.8058 . ?
N1 C11 1.338(5) . ?
N1 C14 1.339(5) . ?
N2 C13 1.331(5) . ?
N2 C12 1.333(5) . ?
C1 C2 1.514(6) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.400(6) . ?
C3 C4 1.400(6) . ?
C3 H3A 0.95 . ?
C4 C5 1.509(6) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.506(6) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.391(6) . ?
C8 C9 1.404(6) . ?
C8 H8A 0.95 . ?
C9 C10 1.512(6) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.394(5) . ?
C11 C15 1.505(5) . ?
C12 H12A 0.95 . ?
C13 C14 1.389(5) . ?
C13 H13A 0.95 . ?
C14 H14A 0.95 . ?

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
O2 Ho1 O3 86.93(10) . . ?
O2 Ho1 O1 74.76(10) . . ?
O3 Ho1 O1 76.17(10) . . ?
O2 Ho1 O4 80.35(10) . . ?
O3 Ho1 O4 74.15(10) . . ?
O1 Ho1 O4 141.94(10) . . ?
O2 Ho1 O5 146.27(9) . . ?
O3 Ho1 O5 107.86(10) . . ?
O1 Ho1 O5 137.46(9) . . ?
O4 Ho1 O5 75.17(10) . . ?
O2 Ho1 O7 106.05(10) . . ?
O3 Ho1 O7 144.01(9) . . ?
O1 Ho1 O7 75.28(9) . . ?
O4 Ho1 O7 140.25(10) . . ?
O5 Ho1 O7 79.93(10) . . ?
O2 Ho1 O8 71.21(10) . . ?
O3 Ho1 O8 143.96(10) . . ?
O1 Ho1 O8 122.26(9) . . ?
O4 Ho1 O8 74.18(10) . . ?
O5 Ho1 O8 79.95(9) . . ?
O7 Ho1 O8 71.31(9) . . ?
O2 Ho1 N1 148.42(10) . . ?
O3 Ho1 N1 77.42(10) . . ?
O1 Ho1 N1 74.94(9) . . ?
O4 Ho1 N1 120.16(10) . . ?
O5 Ho1 N1 65.30(9) . . ?
O7 Ho1 N1 74.37(9) . . ?
O8 Ho1 N1 134.51(9) . . ?
C2 O1 Ho1 130.2(3) . . ?
C4 O2 Ho1 130.7(3) . . ?
C7 O3 Ho1 133.0(3) . . ?
C9 O4 Ho1 131.6(3) . . ?
C15 O5 Ho1 125.8(2) . . ?
Ho1 O7 H1 112.8 . . ?
Ho1 O7 H2 117.4 . . ?
H1 O7 H2 102.6 . . ?
Ho1 O8 H3 117.3 . . ?
Ho1 O8 H4 115.3 . . ?
H3 O8 H4 97.2 . . ?
C11 N1 C14 116.5(3) . . ?
C11 N1 Ho1 115.1(2) . . ?
C14 N1 Ho1 127.8(2) . . ?
C13 N2 C12 116.7(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.6(4) . . ?
O1 C2 C1 116.2(4) . . ?
C3 C2 C1 119.2(4) . . ?
C4 C3 C2 124.2(4) . . ?
C4 C3 H3A 117.9 . . ?
C2 C3 H3A 117.9 . . ?
O2 C4 C3 124.7(4) . . ?
O2 C4 C5 115.9(4) . . ?
C3 C4 C5 119.4(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 124.8(4) . . ?
O3 C7 C6 116.3(4) . . ?
C8 C7 C6 118.9(4) . . ?
C7 C8 C9 123.8(4) . . ?
C7 C8 H8A 118.1 . . ?
C9 C8 H8A 118.1 . . ?
O4 C9 C8 124.9(4) . . ?
O4 C9 C10 116.8(4) . . ?
C8 C9 C10 118.3(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 121.5(3) . . ?
N1 C11 C15 116.4(3) . . ?
C12 C11 C15 122.0(3) . . ?
N2 C12 C11 121.6(3) . . ?
N2 C12 H12A 119.2 . . ?
C11 C12 H12A 119.2 . . ?
N2 C13 C14 121.9(3) . . ?
N2 C13 H13A 119 . . ?
C14 C13 H13A 119 . . ?
N1 C14 C13 121.6(3) . . ?
N1 C14 H14A 119.2 . . ?
C13 C14 H14A 119.2 . . ?
O5 C15 O6 125.8(3) . . ?
O5 C15 C11 117.0(3) . . ?
O6 C15 C11 117.2(3) . . ?

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
O7 H1 O6 0.8 1.91 2.702(4) 171.1 3
O7 H2 N2 0.82 2.05 2.844(4) 163.3 3_556
O8 H3 O6 0.82 1.95 2.744(4) 162.9 3
O8 H4 O6 0.81 2.11 2.855(4) 153.9 1_655
C13 H13A O5 0.95 2.49 3.404(4) 162.1 1_556
C14 H14A O1 0.95 2.53 3.048(5) 114.5 .


# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1554983'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;

_audit_creation_date             2017-03-24T17:32:17-00:00
_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         'C15 H21 Dy N2 O8'
_chemical_formula_sum            'C15 H21 Dy N2 O8'
_chemical_formula_weight         519.84

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.7900(5)
_cell_length_b                   29.8733(18)
_cell_length_c                   8.2641(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.941(2)
_cell_angle_gamma                90
_cell_volume                     1849.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9916
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      32.48

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

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1020

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

_exptl_absorpt_coefficient_mu    4.085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_correction_T_min  0.4472
_exptl_absorpt_correction_T_max  0.7465

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

_diffrn_ambient_temperature      173(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  0.0872
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_number            22347
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.652
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_Friedel_coverage         0
_reflns_number_total             4583
_reflns_number_gt                4361
_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+9.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4583
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.1114
_refine_ls_wR_factor_gt          0.11
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_restrained_S_all      1.222
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.496
_refine_diff_density_min         -2.223
_refine_diff_density_rms         0.156

#----------------------------------------------------------------------------#
#                   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 0.27293(3) 0.09478(2) 0.18456(3) 0.01446(9) Uani 1 1 d . . . . .
O1 O 0.4536(5) 0.09633(13) 0.4567(5) 0.0202(8) Uani 1 1 d . . . . .
O2 O 0.5386(5) 0.12300(14) 0.1674(5) 0.0219(8) Uani 1 1 d . . . . .
O3 O 0.2190(5) 0.16382(14) 0.2808(5) 0.0223(8) Uani 1 1 d . . . . .
O4 O 0.1731(6) 0.13945(13) -0.0519(5) 0.0237(8) Uani 1 1 d . . . . .
O5 O -0.0069(5) 0.06353(14) 0.0373(5) 0.0195(8) Uani 1 1 d . . . . .
O6 O -0.2710(5) 0.03242(13) 0.0249(5) 0.0178(7) Uani 1 1 d . . . . .
O7 O 0.3282(5) 0.01631(12) 0.2611(5) 0.0201(8) Uani 1 1 d . . . . .
H1 H 0.303324 0.002007 0.184134 0.024 Uiso 1 1 d R U . . .
H2 H 0.276125 0.003407 0.327334 0.024 Uiso 1 1 d R U . . .
O8 O 0.3605(5) 0.05601(13) -0.0409(5) 0.0193(8) Uani 1 1 d . . . . .
H3 H 0.34569 0.030964 -0.065571 0.023 Uiso 1 1 d R U . . .
H4 H 0.475291 0.057064 -0.038671 0.023 Uiso 1 1 d R U . . .
N1 N 0.0633(6) 0.07574(14) 0.3699(5) 0.0144(8) Uani 1 1 d . . . . .
N2 N -0.1629(6) 0.03894(15) 0.5445(6) 0.0183(9) Uani 1 1 d . . . . .
C1 C 0.6293(9) 0.1242(2) 0.7181(8) 0.0310(13) Uani 1 1 d . . . . .
H1A H 0.656152 0.093843 0.763009 0.047 Uiso 1 1 calc R U . . .
H1B H 0.529282 0.136413 0.754591 0.047 Uiso 1 1 calc R U . . .
H1C H 0.734486 0.143259 0.759823 0.047 Uiso 1 1 calc R U . . .
C2 C 0.5797(7) 0.12268(18) 0.5278(7) 0.0185(10) Uani 1 1 d . . . . .
C3 C 0.6754(8) 0.14864(19) 0.4421(8) 0.0249(12) Uani 1 1 d . . . . .
H3A H 0.761214 0.168976 0.506263 0.03 Uiso 1 1 calc R U . . .
C4 C 0.6541(7) 0.14686(17) 0.2682(7) 0.0186(10) Uani 1 1 d . . . . .
C5 C 0.7731(8) 0.1745(2) 0.1930(9) 0.0317(14) Uani 1 1 d . . . . .
H5A H 0.701493 0.197053 0.117718 0.048 Uiso 1 1 calc R U . . .
H5B H 0.832176 0.155131 0.129092 0.048 Uiso 1 1 calc R U . . .
H5C H 0.863322 0.189481 0.283049 0.048 Uiso 1 1 calc R U . . .
C6 C 0.2330(12) 0.2401(2) 0.3483(10) 0.0412(18) Uani 1 1 d . . . . .
H6A H 0.340482 0.236231 0.442305 0.062 Uiso 1 1 calc R U . . .
H6B H 0.12728 0.239543 0.390851 0.062 Uiso 1 1 calc R U . . .
H6C H 0.238844 0.268789 0.292857 0.062 Uiso 1 1 calc R U . . .
C7 C 0.2211(8) 0.20266(19) 0.2241(8) 0.0239(11) Uani 1 1 d . . . . .
C8 C 0.2086(10) 0.2133(2) 0.0558(9) 0.0333(14) Uani 1 1 d . . . . .
H8A H 0.21963 0.243765 0.027415 0.04 Uiso 1 1 calc R U . . .
C9 C 0.1808(8) 0.1813(2) -0.0721(8) 0.0262(12) Uani 1 1 d . . . . .
C10 C 0.1583(11) 0.1973(2) -0.2507(9) 0.0383(16) Uani 1 1 d . . . . .
H10A H 0.083224 0.176079 -0.329743 0.057 Uiso 1 1 calc R U . . .
H10B H 0.275527 0.199327 -0.272404 0.057 Uiso 1 1 calc R U . . .
H10C H 0.101444 0.226843 -0.265412 0.057 Uiso 1 1 calc R U . . .
C11 C -0.0885(7) 0.05487(16) 0.2899(6) 0.0130(9) Uani 1 1 d . . . . .
C12 C -0.2019(6) 0.03707(17) 0.3781(6) 0.0149(9) Uani 1 1 d . . . . .
H12A H -0.310185 0.023221 0.317197 0.018 Uiso 1 1 calc R U . . .
C13 C -0.0160(7) 0.06135(19) 0.6236(7) 0.0198(10) Uani 1 1 d . . . . .
H13A H 0.012249 0.06505 0.742144 0.024 Uiso 1 1 calc R U . . .
C14 C 0.0968(7) 0.07946(18) 0.5363(7) 0.0181(10) Uani 1 1 d . . . . .
H14A H 0.200997 0.094962 0.597241 0.022 Uiso 1 1 calc R U . . .
C15 C -0.1250(6) 0.04968(17) 0.1025(6) 0.0132(9) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   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 O2 2.275(4) . ?
Dy1 O3 2.290(4) . ?
Dy1 O1 2.303(4) . ?
Dy1 O4 2.317(4) . ?
Dy1 O5 2.376(4) . ?
Dy1 O7 2.435(4) . ?
Dy1 O8 2.445(4) . ?
Dy1 N1 2.590(4) . ?
O1 C2 1.269(6) . ?
O2 C4 1.264(7) . ?
O3 C7 1.253(7) . ?
O4 C9 1.264(7) . ?
O5 C15 1.257(6) . ?
O6 C15 1.253(6) . ?
O7 H1 0.7465 . ?
O7 H2 0.8568 . ?
O8 H3 0.7758 . ?
O8 H4 0.8899 . ?
N1 C14 1.332(7) . ?
N1 C11 1.340(6) . ?
N2 C12 1.325(7) . ?
N2 C13 1.332(7) . ?
C1 C2 1.513(8) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.396(8) . ?
C3 C4 1.402(9) . ?
C3 H3A 0.95 . ?
C4 C5 1.498(8) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.503(9) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.403(9) . ?
C8 C9 1.398(9) . ?
C8 H8A 0.95 . ?
C9 C10 1.515(9) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.396(7) . ?
C11 C15 1.504(7) . ?
C12 H12A 0.95 . ?
C13 C14 1.390(8) . ?
C13 H13A 0.95 . ?
C14 H14A 0.95 . ?

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
O2 Dy1 O3 86.83(14) . . ?
O2 Dy1 O1 74.38(14) . . ?
O3 Dy1 O1 76.35(14) . . ?
O2 Dy1 O4 80.48(15) . . ?
O3 Dy1 O4 73.92(15) . . ?
O1 Dy1 O4 141.77(14) . . ?
O2 Dy1 O5 146.73(14) . . ?
O3 Dy1 O5 107.55(14) . . ?
O1 Dy1 O5 137.45(13) . . ?
O4 Dy1 O5 75.30(14) . . ?
O2 Dy1 O7 105.90(14) . . ?
O3 Dy1 O7 144.36(14) . . ?
O1 Dy1 O7 75.44(13) . . ?
O4 Dy1 O7 140.17(14) . . ?
O5 Dy1 O7 80.03(14) . . ?
O2 Dy1 O8 71.28(14) . . ?
O3 Dy1 O8 143.84(14) . . ?
O1 Dy1 O8 122.03(14) . . ?
O4 Dy1 O8 74.30(14) . . ?
O5 Dy1 O8 80.36(13) . . ?
O7 Dy1 O8 71.08(13) . . ?
O2 Dy1 N1 148.23(14) . . ?
O3 Dy1 N1 77.70(14) . . ?
O1 Dy1 N1 75.07(14) . . ?
O4 Dy1 N1 120.33(14) . . ?
O5 Dy1 N1 65.03(13) . . ?
O7 Dy1 N1 74.34(13) . . ?
O8 Dy1 N1 134.42(13) . . ?
C2 O1 Dy1 130.7(4) . . ?
C4 O2 Dy1 131.5(4) . . ?
C7 O3 Dy1 132.9(4) . . ?
C9 O4 Dy1 131.6(4) . . ?
C15 O5 Dy1 125.9(3) . . ?
Dy1 O7 H1 110.1 . . ?
Dy1 O7 H2 121.2 . . ?
H1 O7 H2 103.3 . . ?
Dy1 O8 H3 127.2 . . ?
Dy1 O8 H4 117.2 . . ?
H3 O8 H4 96.6 . . ?
C14 N1 C11 116.4(4) . . ?
C14 N1 Dy1 128.0(3) . . ?
C11 N1 Dy1 115.1(3) . . ?
C12 N2 C13 116.9(5) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.2(5) . . ?
O1 C2 C1 116.3(5) . . ?
C3 C2 C1 119.4(5) . . ?
C2 C3 C4 124.7(5) . . ?
C2 C3 H3A 117.6 . . ?
C4 C3 H3A 117.6 . . ?
O2 C4 C3 124.0(5) . . ?
O2 C4 C5 116.6(5) . . ?
C3 C4 C5 119.4(5) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 125.1(6) . . ?
O3 C7 C6 115.9(6) . . ?
C8 C7 C6 118.9(6) . . ?
C9 C8 C7 123.3(6) . . ?
C9 C8 H8A 118.4 . . ?
C7 C8 H8A 118.4 . . ?
O4 C9 C8 125.4(6) . . ?
O4 C9 C10 116.4(6) . . ?
C8 C9 C10 118.2(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 121.3(4) . . ?
N1 C11 C15 116.6(4) . . ?
C12 C11 C15 122.1(4) . . ?
N2 C12 C11 121.9(5) . . ?
N2 C12 H12A 119.1 . . ?
C11 C12 H12A 119.1 . . ?
N2 C13 C14 121.4(5) . . ?
N2 C13 H13A 119.3 . . ?
C14 C13 H13A 119.3 . . ?
N1 C14 C13 122.0(5) . . ?
N1 C14 H14A 119 . . ?
C13 C14 H14A 119 . . ?
O6 C15 O5 125.8(5) . . ?
O6 C15 C11 117.2(4) . . ?
O5 C15 C11 117.0(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H1 O6 0.75 1.97 2.707(5) 171.5 3
O7 H2 N2 0.86 2 2.846(6) 167.4 3_556
O8 H4 O6 0.89 2.04 2.859(5) 152.9 1_655
O8 H3 O6 0.78 2.04 2.745(5) 151.9 3
C13 H13A O5 0.95 2.49 3.401(7) 162 1_556
C14 H14A O1 0.95 2.55 3.069(7) 114.9 .


# 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 1554987'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;

_audit_creation_date             2017-03-09T13:16:01-00:00
_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         'C15 H21 N2 O8 Yb'
_chemical_formula_sum            'C15 H21 N2 O8 Yb'
_chemical_formula_weight         530.38

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.7360(7)
_cell_length_b                   29.710(2)
_cell_length_c                   8.2611(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.765(2)
_cell_angle_gamma                90
_cell_volume                     1827.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4092
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      30.36

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

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1036

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

_exptl_absorpt_coefficient_mu    5.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_T_min  0.5435
_exptl_absorpt_correction_T_max  0.7462

#----------------------------------------------------------------------------#
#                   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  0.0487
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_number            18741
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.652
_diffrn_reflns_theta_max         31.101
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_reflns_Friedel_coverage         0
_reflns_number_total             5726
_reflns_number_gt                4739
_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, 2015)'
_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+1.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5726
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0836
_refine_ls_wR_factor_gt          0.0785
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.207
_refine_diff_density_min         -1.29
_refine_diff_density_rms         0.168

#----------------------------------------------------------------------------#
#                   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 0.27252(2) 0.09439(2) 0.18519(2) 0.01303(6) Uani 1 1 d . . . . .
O1 O 0.4523(4) 0.09530(10) 0.4528(4) 0.0193(6) Uani 1 1 d . . . . .
O2 O 0.5334(4) 0.12295(11) 0.1644(4) 0.0207(6) Uani 1 1 d . . . . .
O3 O 0.2184(4) 0.16214(10) 0.2843(3) 0.0198(6) Uani 1 1 d . . . . .
O4 O 0.1729(4) 0.13850(10) -0.0473(4) 0.0211(6) Uani 1 1 d . . . . .
O5 O -0.0007(4) 0.06298(10) 0.0380(3) 0.0177(6) Uani 1 1 d . . . . .
O6 O -0.2700(4) 0.03285(10) 0.0215(3) 0.0166(6) Uani 1 1 d . . . . .
O7 O 0.3282(4) 0.01719(9) 0.2606(3) 0.0180(6) Uani 1 1 d . . . . .
H1 H 0.261882 0.001928 0.315903 0.022 Uiso 1 1 d R U . . .
H2 H 0.330732 -0.002562 0.185663 0.022 Uiso 1 1 d R U . . .
O8 O 0.3579(4) 0.05652(10) -0.0377(3) 0.0183(6) Uani 1 1 d . . . . .
H3 H 0.481098 0.053124 -0.000418 0.022 Uiso 1 1 d R U . . .
H4 H 0.337008 0.027934 -0.064918 0.022 Uiso 1 1 d R U . . .
N1 N 0.0651(5) 0.07586(11) 0.3688(4) 0.0133(6) Uani 1 1 d . . . . .
N2 N -0.1642(5) 0.03894(12) 0.5432(4) 0.0174(7) Uani 1 1 d . . . . .
C1 C 0.6263(7) 0.12348(17) 0.7135(5) 0.0277(10) Uani 1 1 d . . . . .
H1A H 0.648557 0.092845 0.758357 0.042 Uiso 1 1 calc R U . . .
H1B H 0.527416 0.1369 0.750003 0.042 Uiso 1 1 calc R U . . .
H1C H 0.734945 0.141676 0.755341 0.042 Uiso 1 1 calc R U . . .
C2 C 0.5771(6) 0.12195(15) 0.5243(5) 0.0192(8) Uani 1 1 d . . . . .
C3 C 0.6714(6) 0.14893(15) 0.4380(5) 0.0221(9) Uani 1 1 d . . . . .
H3A H 0.755728 0.169806 0.501977 0.026 Uiso 1 1 calc R U . . .
C4 C 0.6501(6) 0.14731(14) 0.2646(5) 0.0193(8) Uani 1 1 d . . . . .
C5 C 0.7702(6) 0.17493(18) 0.1878(6) 0.0299(10) Uani 1 1 d . . . . .
H5A H 0.696992 0.19559 0.104364 0.045 Uiso 1 1 calc R U . . .
H5B H 0.837866 0.154955 0.132961 0.045 Uiso 1 1 calc R U . . .
H5C H 0.854076 0.19227 0.276024 0.045 Uiso 1 1 calc R U . . .
C6 C 0.2344(8) 0.23924(17) 0.3547(6) 0.0353(13) Uani 1 1 d . . . . .
H6A H 0.125546 0.239617 0.393768 0.053 Uiso 1 1 calc R U . . .
H6B H 0.246527 0.268108 0.301501 0.053 Uiso 1 1 calc R U . . .
H6C H 0.33945 0.234347 0.450728 0.053 Uiso 1 1 calc R U . . .
C7 C 0.2215(6) 0.20181(15) 0.2291(6) 0.0216(9) Uani 1 1 d . . . . .
C8 C 0.2106(7) 0.21249(16) 0.0615(6) 0.0277(10) Uani 1 1 d . . . . .
H8A H 0.22424 0.243083 0.033876 0.033 Uiso 1 1 calc R U . . .
C9 C 0.1804(6) 0.18019(16) -0.0685(6) 0.0235(9) Uani 1 1 d . . . . .
C10 C 0.1545(7) 0.19691(18) -0.2470(6) 0.0321(11) Uani 1 1 d . . . . .
H10A H 0.087514 0.174416 -0.326396 0.048 Uiso 1 1 calc R U . . .
H10B H 0.272023 0.20185 -0.26752 0.048 Uiso 1 1 calc R U . . .
H10C H 0.087243 0.225257 -0.262476 0.048 Uiso 1 1 calc R U . . .
C11 C -0.0881(5) 0.05483(13) 0.2881(4) 0.0120(7) Uani 1 1 d . . . . .
C12 C -0.2027(5) 0.03687(14) 0.3757(5) 0.0148(8) Uani 1 1 d . . . . .
H12A H -0.311101 0.022792 0.31458 0.018 Uiso 1 1 calc R U . . .
C13 C -0.0161(6) 0.06147(15) 0.6219(5) 0.0177(8) Uani 1 1 d . . . . .
H13A H 0.011921 0.065096 0.740409 0.021 Uiso 1 1 calc R U . . .
C14 C 0.0989(6) 0.07987(14) 0.5356(5) 0.0168(8) Uani 1 1 d . . . . .
H14A H 0.203343 0.095558 0.596576 0.02 Uiso 1 1 calc R U . . .
C15 C -0.1223(5) 0.04992(13) 0.1009(4) 0.0126(7) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   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 O2 2.239(3) . ?
Yb1 O3 2.255(3) . ?
Yb1 O1 2.270(3) . ?
Yb1 O4 2.279(3) . ?
Yb1 O5 2.328(3) . ?
Yb1 O7 2.385(3) . ?
Yb1 O8 2.399(3) . ?
Yb1 N1 2.550(3) . ?
O1 C2 1.264(5) . ?
O2 C4 1.272(5) . ?
O3 C7 1.266(5) . ?
O4 C9 1.254(5) . ?
O5 C15 1.253(4) . ?
O6 C15 1.259(5) . ?
O7 H1 0.8969 . ?
O7 H2 0.8572 . ?
O8 H3 0.9241 . ?
O8 H4 0.8822 . ?
N1 C14 1.336(5) . ?
N1 C11 1.346(5) . ?
N2 C13 1.334(5) . ?
N2 C12 1.336(5) . ?
C1 C2 1.505(6) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.402(6) . ?
C3 C4 1.398(6) . ?
C3 H3A 0.95 . ?
C4 C5 1.503(6) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.506(6) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.400(6) . ?
C8 C9 1.412(6) . ?
C8 H8A 0.95 . ?
C9 C10 1.517(6) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.394(5) . ?
C11 C15 1.504(5) . ?
C12 H12A 0.95 . ?
C13 C14 1.394(6) . ?
C13 H13A 0.95 . ?
C14 H14A 0.95 . ?

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
O2 Yb1 O3 87.12(11) . . ?
O2 Yb1 O1 75.15(11) . . ?
O3 Yb1 O1 76.15(11) . . ?
O2 Yb1 O4 79.81(11) . . ?
O3 Yb1 O4 74.87(10) . . ?
O1 Yb1 O4 142.30(11) . . ?
O2 Yb1 O5 145.22(10) . . ?
O3 Yb1 O5 108.40(11) . . ?
O1 Yb1 O5 137.95(10) . . ?
O4 Yb1 O5 74.88(10) . . ?
O2 Yb1 O7 106.38(11) . . ?
O3 Yb1 O7 143.29(10) . . ?
O1 Yb1 O7 74.79(10) . . ?
O4 Yb1 O7 140.25(10) . . ?
O5 Yb1 O7 79.91(11) . . ?
O2 Yb1 O8 71.14(10) . . ?
O3 Yb1 O8 144.54(10) . . ?
O1 Yb1 O8 121.99(11) . . ?
O4 Yb1 O8 73.95(10) . . ?
O5 Yb1 O8 79.13(10) . . ?
O7 Yb1 O8 71.45(9) . . ?
O2 Yb1 N1 148.61(10) . . ?
O3 Yb1 N1 76.56(11) . . ?
O1 Yb1 N1 74.99(11) . . ?
O4 Yb1 N1 120.13(11) . . ?
O5 Yb1 N1 66.14(10) . . ?
O7 Yb1 N1 74.64(10) . . ?
O8 Yb1 N1 134.80(10) . . ?
C2 O1 Yb1 130.6(3) . . ?
C4 O2 Yb1 131.4(3) . . ?
C7 O3 Yb1 132.6(3) . . ?
C9 O4 Yb1 131.9(3) . . ?
C15 O5 Yb1 125.8(2) . . ?
Yb1 O7 H1 122.1 . . ?
Yb1 O7 H2 120.5 . . ?
H1 O7 H2 98.6 . . ?
Yb1 O8 H3 105.6 . . ?
Yb1 O8 H4 125.3 . . ?
H3 O8 H4 94.6 . . ?
C14 N1 C11 116.9(3) . . ?
C14 N1 Yb1 128.0(3) . . ?
C11 N1 Yb1 114.7(2) . . ?
C13 N2 C12 116.6(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.9(4) . . ?
O1 C2 C1 116.7(4) . . ?
C3 C2 C1 119.4(4) . . ?
C4 C3 C2 124.7(4) . . ?
C4 C3 H3A 117.7 . . ?
C2 C3 H3A 117.7 . . ?
O2 C4 C3 123.5(4) . . ?
O2 C4 C5 116.5(4) . . ?
C3 C4 C5 120.0(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 124.4(4) . . ?
O3 C7 C6 116.3(4) . . ?
C8 C7 C6 119.3(4) . . ?
C7 C8 C9 123.5(4) . . ?
C7 C8 H8A 118.3 . . ?
C9 C8 H8A 118.3 . . ?
O4 C9 C8 124.7(4) . . ?
O4 C9 C10 117.4(4) . . ?
C8 C9 C10 117.9(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 121.3(3) . . ?
N1 C11 C15 116.1(3) . . ?
C12 C11 C15 122.5(3) . . ?
N2 C12 C11 121.7(4) . . ?
N2 C12 H12A 119.1 . . ?
C11 C12 H12A 119.1 . . ?
N2 C13 C14 122.1(4) . . ?
N2 C13 H13A 119 . . ?
C14 C13 H13A 119 . . ?
N1 C14 C13 121.3(4) . . ?
N1 C14 H14A 119.4 . . ?
C13 C14 H14A 119.4 . . ?
O5 C15 O6 125.9(3) . . ?
O5 C15 C11 117.0(3) . . ?
O6 C15 C11 117.1(3) . . ?

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
O7 H1 N2 0.9 1.97 2.852(4) 167.7 3_556
O7 H2 O6 0.86 1.88 2.697(4) 159.7 3
O8 H3 O6 0.92 1.98 2.873(4) 162.5 1_655
O8 H4 O6 0.88 1.94 2.753(4) 152.8 3
C13 H13A O5 0.95 2.49 3.408(4) 163.1 1_556
C14 H14A O1 0.95 2.52 3.028(5) 113.4 .


# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1554980'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;

_audit_creation_date             2017-03-24T17:20:19-00:00
_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         'C15 H21 Eu N2 O8'
_chemical_formula_sum            'C15 H21 Eu N2 O8'
_chemical_formula_weight         509.3

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.8334(9)
_cell_length_b                   30.012(4)
_cell_length_c                   8.2681(10)
_cell_angle_alpha                90
_cell_angle_beta                 106.095(2)
_cell_angle_gamma                90
_cell_volume                     1867.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7197
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      30.45

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

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1008

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

_exptl_absorpt_coefficient_mu    3.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_correction_T_min  0.5651
_exptl_absorpt_correction_T_max  0.7462

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

_diffrn_ambient_temperature      173(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  0.0404
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_number            23238
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.652
_diffrn_reflns_theta_max         31.556
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.976
_reflns_Friedel_coverage         0
_reflns_number_total             6097
_reflns_number_gt                5428
_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+3.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6097
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.083
_refine_ls_wR_factor_gt          0.0803
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_restrained_S_all      1.168
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.26
_refine_diff_density_min         -2.056
_refine_diff_density_rms         0.132

#----------------------------------------------------------------------------#
#                   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'
Eu Eu -0.1578 3.6682 '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
Eu1 Eu 0.27389(2) 0.09519(2) 0.18388(2) 0.01487(5) Uani 1 1 d . . . . .
O1 O 0.4557(3) 0.09737(8) 0.4610(3) 0.0213(5) Uani 1 1 d . . . . .
O2 O 0.5449(3) 0.12321(9) 0.1704(3) 0.0233(5) Uani 1 1 d . . . . .
O3 O 0.2210(3) 0.16530(9) 0.2777(3) 0.0238(5) Uani 1 1 d . . . . .
O4 O 0.1760(4) 0.14051(8) -0.0558(3) 0.0248(5) Uani 1 1 d . . . . .
O5 O -0.0115(3) 0.06398(9) 0.0377(3) 0.0209(5) Uani 1 1 d . . . . .
O6 O -0.2721(3) 0.03215(8) 0.0269(3) 0.0188(5) Uani 1 1 d . . . . .
O7 O 0.3281(3) 0.01556(8) 0.2608(3) 0.0204(5) Uani 1 1 d . . . . .
H1 H 0.286633 0.001174 0.172868 0.024 Uiso 1 1 d R U . . .
H2 H 0.264833 0.003274 0.320968 0.024 Uiso 1 1 d R U . . .
O8 O 0.3628(3) 0.05579(8) -0.0444(3) 0.0204(5) Uani 1 1 d . . . . .
H3 H 0.337664 0.027186 -0.057113 0.024 Uiso 1 1 d R U . . .
H4 H 0.452564 0.058286 -0.054413 0.024 Uiso 1 1 d R U . . .
N1 N 0.0616(4) 0.07560(9) 0.3721(3) 0.0152(5) Uani 1 1 d . . . . .
N2 N -0.1626(4) 0.03905(10) 0.5467(4) 0.0199(6) Uani 1 1 d . . . . .
C1 C 0.6326(6) 0.12457(15) 0.7220(5) 0.0321(9) Uani 1 1 d . . . . .
H1A H 0.657029 0.094306 0.766961 0.048 Uiso 1 1 calc R U . . .
H1B H 0.534286 0.13735 0.758549 0.048 Uiso 1 1 calc R U . . .
H1C H 0.738865 0.143049 0.763747 0.048 Uiso 1 1 calc R U . . .
C2 C 0.5827(4) 0.12304(12) 0.5324(4) 0.0202(7) Uani 1 1 d . . . . .
C3 C 0.6791(5) 0.14874(12) 0.4464(5) 0.0258(7) Uani 1 1 d . . . . .
H3A H 0.765268 0.168782 0.510865 0.031 Uiso 1 1 calc R U . . .
C4 C 0.6578(5) 0.14710(12) 0.2726(5) 0.0210(7) Uani 1 1 d . . . . .
C5 C 0.7787(5) 0.17437(15) 0.1976(6) 0.0341(9) Uani 1 1 d . . . . .
H5A H 0.707224 0.194756 0.112929 0.051 Uiso 1 1 calc R U . . .
H5B H 0.846465 0.15448 0.144532 0.051 Uiso 1 1 calc R U . . .
H5C H 0.860765 0.191591 0.286663 0.051 Uiso 1 1 calc R U . . .
C6 C 0.2321(7) 0.24165(15) 0.3413(6) 0.0436(12) Uani 1 1 d . . . . .
H6A H 0.338469 0.238071 0.436361 0.065 Uiso 1 1 calc R U . . .
H6B H 0.126239 0.241302 0.382433 0.065 Uiso 1 1 calc R U . . .
H6C H 0.238412 0.270089 0.284936 0.065 Uiso 1 1 calc R U . . .
C7 C 0.2218(5) 0.20400(13) 0.2185(5) 0.0265(8) Uani 1 1 d . . . . .
C8 C 0.2102(6) 0.21389(14) 0.0512(5) 0.0341(9) Uani 1 1 d . . . . .
H8A H 0.220856 0.244183 0.022109 0.041 Uiso 1 1 calc R U . . .
C9 C 0.1839(5) 0.18199(13) -0.0765(5) 0.0261(8) Uani 1 1 d . . . . .
C10 C 0.1615(7) 0.19788(15) -0.2549(5) 0.0398(11) Uani 1 1 d . . . . .
H10A H 0.091184 0.176095 -0.334141 0.06 Uiso 1 1 calc R U . . .
H10B H 0.278581 0.201134 -0.274708 0.06 Uiso 1 1 calc R U . . .
H10C H 0.100326 0.226703 -0.271325 0.06 Uiso 1 1 calc R U . . .
C11 C -0.0903(4) 0.05488(10) 0.2917(4) 0.0138(6) Uani 1 1 d . . . . .
C12 C -0.2013(4) 0.03688(11) 0.3795(4) 0.0164(6) Uani 1 1 d . . . . .
H12A H -0.30799 0.022599 0.318599 0.02 Uiso 1 1 calc R U . . .
C13 C -0.0150(5) 0.06101(12) 0.6253(4) 0.0205(7) Uani 1 1 d . . . . .
H13A H 0.014451 0.064339 0.744155 0.025 Uiso 1 1 calc R U . . .
C14 C 0.0973(5) 0.07921(12) 0.5385(4) 0.0184(6) Uani 1 1 d . . . . .
H14A H 0.201458 0.094527 0.599296 0.022 Uiso 1 1 calc R U . . .
C15 C -0.1266(4) 0.04990(11) 0.1040(4) 0.0154(6) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   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
Eu1 O2 2.314(2) . ?
Eu1 O3 2.319(3) . ?
Eu1 O1 2.340(2) . ?
Eu1 O4 2.350(3) . ?
Eu1 O5 2.416(2) . ?
Eu1 O7 2.479(2) . ?
Eu1 O8 2.485(2) . ?
Eu1 N1 2.640(3) . ?
O1 C2 1.267(4) . ?
O2 C4 1.263(4) . ?
O3 C7 1.261(5) . ?
O4 C9 1.261(4) . ?
O5 C15 1.251(4) . ?
O6 C15 1.260(4) . ?
O7 H1 0.8302 . ?
O7 H2 0.8751 . ?
O8 H3 0.8803 . ?
O8 H4 0.7346 . ?
N1 C14 1.331(4) . ?
N1 C11 1.343(4) . ?
N2 C12 1.333(4) . ?
N2 C13 1.333(5) . ?
C1 C2 1.508(5) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.403(5) . ?
C3 C4 1.401(5) . ?
C3 H3A 0.95 . ?
C4 C5 1.509(5) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.506(6) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.393(6) . ?
C8 C9 1.397(6) . ?
C8 H8A 0.95 . ?
C9 C10 1.514(5) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.387(4) . ?
C11 C15 1.506(4) . ?
C12 H12A 0.95 . ?
C13 C14 1.392(5) . ?
C13 H13A 0.95 . ?
C14 H14A 0.95 . ?

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
O2 Eu1 O3 86.43(9) . . ?
O2 Eu1 O1 73.71(9) . . ?
O3 Eu1 O1 76.33(9) . . ?
O2 Eu1 O4 80.69(9) . . ?
O3 Eu1 O4 73.16(9) . . ?
O1 Eu1 O4 141.02(9) . . ?
O2 Eu1 O5 148.27(8) . . ?
O3 Eu1 O5 107.02(9) . . ?
O1 Eu1 O5 136.76(8) . . ?
O4 Eu1 O5 76.24(9) . . ?
O2 Eu1 O7 105.58(9) . . ?
O3 Eu1 O7 145.34(8) . . ?
O1 Eu1 O7 76.20(8) . . ?
O4 Eu1 O7 140.07(8) . . ?
O5 Eu1 O7 79.83(9) . . ?
O2 Eu1 O8 71.49(9) . . ?
O3 Eu1 O8 143.08(9) . . ?
O1 Eu1 O8 122.32(9) . . ?
O4 Eu1 O8 74.31(9) . . ?
O5 Eu1 O8 81.41(8) . . ?
O7 Eu1 O8 70.85(8) . . ?
O2 Eu1 N1 147.72(9) . . ?
O3 Eu1 N1 78.74(9) . . ?
O1 Eu1 N1 74.98(9) . . ?
O4 Eu1 N1 120.96(9) . . ?
O5 Eu1 N1 64.01(8) . . ?
O7 Eu1 N1 74.05(8) . . ?
O8 Eu1 N1 134.17(8) . . ?
C2 O1 Eu1 131.2(2) . . ?
C4 O2 Eu1 131.0(2) . . ?
C7 O3 Eu1 133.2(3) . . ?
C9 O4 Eu1 132.0(2) . . ?
C15 O5 Eu1 126.2(2) . . ?
Eu1 O7 H1 106.2 . . ?
Eu1 O7 H2 117.9 . . ?
H1 O7 H2 97.6 . . ?
Eu1 O8 H3 117 . . ?
Eu1 O8 H4 121.1 . . ?
H3 O8 H4 106 . . ?
C14 N1 C11 116.9(3) . . ?
C14 N1 Eu1 127.3(2) . . ?
C11 N1 Eu1 115.3(2) . . ?
C12 N2 C13 116.6(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.2(3) . . ?
O1 C2 C1 116.5(3) . . ?
C3 C2 C1 119.3(3) . . ?
C4 C3 C2 125.0(3) . . ?
C4 C3 H3A 117.5 . . ?
C2 C3 H3A 117.5 . . ?
O2 C4 C3 124.6(3) . . ?
O2 C4 C5 115.8(3) . . ?
C3 C4 C5 119.5(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 125.2(4) . . ?
O3 C7 C6 115.7(4) . . ?
C8 C7 C6 119.1(4) . . ?
C7 C8 C9 124.0(4) . . ?
C7 C8 H8A 118 . . ?
C9 C8 H8A 118 . . ?
O4 C9 C8 125.2(4) . . ?
O4 C9 C10 116.5(4) . . ?
C8 C9 C10 118.3(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 121.3(3) . . ?
N1 C11 C15 116.4(3) . . ?
C12 C11 C15 122.3(3) . . ?
N2 C12 C11 121.9(3) . . ?
N2 C12 H12A 119.1 . . ?
C11 C12 H12A 119.1 . . ?
N2 C13 C14 121.9(3) . . ?
N2 C13 H13A 119 . . ?
C14 C13 H13A 119 . . ?
N1 C14 C13 121.3(3) . . ?
N1 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
O5 C15 O6 125.6(3) . . ?
O5 C15 C11 117.7(3) . . ?
O6 C15 C11 116.7(3) . . ?

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
O7 H1 O6 0.83 1.91 2.705(3) 161.1 3
O7 H2 N2 0.88 1.98 2.836(4) 164.2 3_556
O8 H4 O6 0.73 2.22 2.846(3) 144.2 1_655
O8 H3 O6 0.88 1.89 2.747(3) 164.4 3
C13 H13A O5 0.95 2.49 3.403(4) 160.9 1_556
C14 H14A O1 0.95 2.56 3.097(4) 116.2 .


# 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 1554985'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;

_audit_creation_date             2017-03-24T17:54:05-00:00
_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         'C15 H21 Er N2 O8'
_chemical_formula_sum            'C15 H21 Er N2 O8'
_chemical_formula_weight         524.6

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.7499(8)
_cell_length_b                   29.727(3)
_cell_length_c                   8.2564(9)
_cell_angle_alpha                90
_cell_angle_beta                 105.8480(10)
_cell_angle_gamma                90
_cell_volume                     1829.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9161
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      31.66

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

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1028

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

_exptl_absorpt_coefficient_mu    4.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_T_min  0.4999
_exptl_absorpt_correction_T_max  0.7462

#----------------------------------------------------------------------------#
#                   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  0.0928
_diffrn_reflns_av_unetI/netI     0.059
_diffrn_reflns_number            13406
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.654
_diffrn_reflns_theta_max         25.848
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             3527
_reflns_number_gt                3357
_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)+2.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3527
_refine_ls_number_parameters     239
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.045
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0864
_refine_ls_goodness_of_fit_ref   1.607
_refine_ls_restrained_S_all      1.609
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.465
_refine_diff_density_min         -2.6
_refine_diff_density_rms         0.17

#----------------------------------------------------------------------------#
#                   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 0.27355(3) 0.09461(2) 0.18507(3) 0.01345(11) Uani 1 1 d . . . . .
O1 O 0.4532(5) 0.09588(15) 0.4559(5) 0.0210(10) Uani 1 1 d . . . . .
O2 O 0.5375(5) 0.12306(15) 0.1652(5) 0.0188(10) Uani 1 1 d . . . . .
O3 O 0.2197(5) 0.16272(16) 0.2831(5) 0.0181(10) Uani 1 1 d . . . . .
O4 O 0.1732(5) 0.13885(15) -0.0498(5) 0.0202(10) Uani 1 1 d . . . . .
O5 O -0.0039(5) 0.06343(16) 0.0375(5) 0.0180(10) Uani 1 1 d . . . . .
O6 O -0.2710(5) 0.03246(15) 0.0234(5) 0.0157(9) Uani 1 1 d . . . . .
O7 O 0.3290(5) 0.01670(14) 0.2614(5) 0.0168(9) Uani 1 1 d . . . . .
H1 H 0.281929 -0.00094 0.170991 0.02 Uiso 1 1 d R U . . .
H2 H 0.267829 0.00586 0.31339 0.02 Uiso 1 1 d R U . . .
O8 O 0.3602(5) 0.05630(15) -0.0379(5) 0.0161(9) Uani 1 1 d . . . . .
H3 H 0.476233 0.054797 -0.038724 0.019 Uiso 1 1 d R U . . .
H4 H 0.347332 0.030397 -0.049224 0.019 Uiso 1 1 d R U . . .
N1 N 0.0666(6) 0.07567(18) 0.3694(6) 0.0134(11) Uani 1 1 d . . . . .
N2 N -0.1634(6) 0.03889(19) 0.5443(6) 0.0173(12) Uani 1 1 d . . . . .
C1 C 0.6282(8) 0.1241(3) 0.7162(8) 0.0272(16) Uani 1 1 d . . . . .
H1A H 0.657637 0.093725 0.761716 0.041 Uiso 1 1 calc R U . . .
H1B H 0.525981 0.135731 0.751678 0.041 Uiso 1 1 calc R U . . .
H1C H 0.731944 0.143845 0.758345 0.041 Uiso 1 1 calc R U . . .
C2 C 0.5804(7) 0.1224(2) 0.5262(7) 0.0190(14) Uani 1 1 d . . . . .
C3 C 0.6746(8) 0.1488(2) 0.4396(8) 0.0212(14) Uani 1 1 d . . . . .
H3A H 0.759789 0.169628 0.502844 0.025 Uiso 1 1 calc R U . . .
C4 C 0.6519(7) 0.1468(2) 0.2672(8) 0.0176(14) Uani 1 1 d . . . . .
C5 C 0.7722(8) 0.1748(3) 0.1899(8) 0.0282(17) Uani 1 1 d . . . . .
H5A H 0.698754 0.195672 0.107451 0.042 Uiso 1 1 calc R U . . .
H5B H 0.838923 0.154987 0.13378 0.042 Uiso 1 1 calc R U . . .
H5C H 0.856687 0.191902 0.278503 0.042 Uiso 1 1 calc R U . . .
C6 C 0.2347(10) 0.2397(3) 0.3514(9) 0.0337(18) Uani 1 1 d . U . . .
H6A H 0.130674 0.238815 0.397227 0.05 Uiso 1 1 calc R U . . .
H6B H 0.237154 0.268627 0.294892 0.05 Uiso 1 1 calc R U . . .
H6C H 0.344873 0.23632 0.443246 0.05 Uiso 1 1 calc R U . . .
C7 C 0.2215(8) 0.2020(2) 0.2267(8) 0.0214(15) Uani 1 1 d . . . . .
C8 C 0.2112(9) 0.2129(2) 0.0589(8) 0.0283(16) Uani 1 1 d . . . . .
H8A H 0.224853 0.243435 0.031342 0.034 Uiso 1 1 calc R U . . .
C9 C 0.1817(8) 0.1808(3) -0.0698(8) 0.0233(15) Uani 1 1 d . . . . .
C10 C 0.1582(10) 0.1972(3) -0.2493(8) 0.0346(18) Uani 1 1 d . . . . .
H10A H 0.093649 0.174478 -0.328818 0.052 Uiso 1 1 calc R U . . .
H10B H 0.276298 0.202477 -0.267657 0.052 Uiso 1 1 calc R U . . .
H10C H 0.089675 0.225367 -0.266705 0.052 Uiso 1 1 calc R U . . .
C11 C -0.0882(7) 0.0552(2) 0.2895(6) 0.0111(12) Uani 1 1 d . . . . .
C12 C -0.2013(7) 0.0371(2) 0.3765(7) 0.0147(13) Uani 1 1 d . . . . .
H12A H -0.30907 0.022867 0.314955 0.018 Uiso 1 1 calc R U . . .
C13 C -0.0146(7) 0.0615(2) 0.6225(7) 0.0151(13) Uani 1 1 d . . . . .
H13A H 0.014043 0.065123 0.741237 0.018 Uiso 1 1 calc R U . . .
C14 C 0.0989(7) 0.0798(2) 0.5364(7) 0.0156(13) Uani 1 1 d . . . . .
H14A H 0.202448 0.095767 0.59758 0.019 Uiso 1 1 calc R U . . .
C15 C -0.1231(7) 0.0496(2) 0.1012(7) 0.0112(12) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   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 O2 2.261(4) . ?
Er1 O3 2.261(5) . ?
Er1 O1 2.289(4) . ?
Er1 O4 2.296(4) . ?
Er1 O5 2.352(4) . ?
Er1 O7 2.408(4) . ?
Er1 O8 2.411(4) . ?
Er1 N1 2.557(4) . ?
O1 C2 1.272(7) . ?
O2 C4 1.259(7) . ?
O3 C7 1.258(8) . ?
O4 C9 1.261(8) . ?
O5 C15 1.251(6) . ?
O6 C15 1.258(6) . ?
O7 H1 0.9038 . ?
O7 H2 0.79 . ?
O8 H3 0.9022 . ?
O8 H4 0.7787 . ?
N1 C14 1.338(7) . ?
N1 C11 1.346(7) . ?
N2 C12 1.337(7) . ?
N2 C13 1.338(7) . ?
C1 C2 1.510(8) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.395(8) . ?
C3 C4 1.387(8) . ?
C3 H3A 0.95 . ?
C4 C5 1.515(9) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.507(9) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.404(9) . ?
C8 C9 1.400(9) . ?
C8 H8A 0.95 . ?
C9 C10 1.523(9) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.385(7) . ?
C11 C15 1.513(7) . ?
C12 H12A 0.95 . ?
C13 C14 1.385(8) . ?
C13 H13A 0.95 . ?
C14 H14A 0.95 . ?

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
O2 Er1 O3 87.13(15) . . ?
O2 Er1 O1 75.14(14) . . ?
O3 Er1 O1 76.00(15) . . ?
O2 Er1 O4 80.16(15) . . ?
O3 Er1 O4 74.71(15) . . ?
O1 Er1 O4 142.28(15) . . ?
O2 Er1 O5 145.79(13) . . ?
O3 Er1 O5 107.83(14) . . ?
O1 Er1 O5 137.60(14) . . ?
O4 Er1 O5 74.77(14) . . ?
O2 Er1 O7 106.17(15) . . ?
O3 Er1 O7 143.59(14) . . ?
O1 Er1 O7 75.08(14) . . ?
O4 Er1 O7 140.10(14) . . ?
O5 Er1 O7 80.17(14) . . ?
O2 Er1 O8 71.04(14) . . ?
O3 Er1 O8 144.42(14) . . ?
O1 Er1 O8 122.12(14) . . ?
O4 Er1 O8 74.12(14) . . ?
O5 Er1 O8 79.88(13) . . ?
O7 Er1 O8 71.25(13) . . ?
O2 Er1 N1 148.50(14) . . ?
O3 Er1 N1 77.13(16) . . ?
O1 Er1 N1 74.65(14) . . ?
O4 Er1 N1 120.39(15) . . ?
O5 Er1 N1 65.70(14) . . ?
O7 Er1 N1 74.25(15) . . ?
O8 Er1 N1 134.53(15) . . ?
C2 O1 Er1 130.2(4) . . ?
C4 O2 Er1 130.3(4) . . ?
C7 O3 Er1 132.6(4) . . ?
C9 O4 Er1 131.2(4) . . ?
C15 O5 Er1 126.0(3) . . ?
Er1 O7 H1 109.8 . . ?
Er1 O7 H2 116.3 . . ?
H1 O7 H2 92.6 . . ?
Er1 O8 H3 121 . . ?
Er1 O8 H4 120.3 . . ?
H3 O8 H4 92.6 . . ?
C14 N1 C11 115.9(5) . . ?
C14 N1 Er1 128.5(4) . . ?
C11 N1 Er1 115.3(3) . . ?
C12 N2 C13 115.9(5) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.3(5) . . ?
O1 C2 C1 115.7(6) . . ?
C3 C2 C1 120.0(6) . . ?
C4 C3 C2 124.3(6) . . ?
C4 C3 H3A 117.8 . . ?
C2 C3 H3A 117.8 . . ?
O2 C4 C3 125.4(6) . . ?
O2 C4 C5 115.4(5) . . ?
C3 C4 C5 119.2(6) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 125.1(6) . . ?
O3 C7 C6 116.3(6) . . ?
C8 C7 C6 118.6(7) . . ?
C9 C8 C7 123.1(7) . . ?
C9 C8 H8A 118.4 . . ?
C7 C8 H8A 118.4 . . ?
O4 C9 C8 125.3(6) . . ?
O4 C9 C10 116.7(6) . . ?
C8 C9 C10 118.1(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 121.8(5) . . ?
N1 C11 C15 116.0(5) . . ?
C12 C11 C15 121.9(5) . . ?
N2 C12 C11 122.0(5) . . ?
N2 C12 H12A 119 . . ?
C11 C12 H12A 119 . . ?
N2 C13 C14 122.3(5) . . ?
N2 C13 H13A 118.9 . . ?
C14 C13 H13A 118.9 . . ?
N1 C14 C13 121.8(5) . . ?
N1 C14 H14A 119.1 . . ?
C13 C14 H14A 119.1 . . ?
O5 C15 O6 126.4(5) . . ?
O5 C15 C11 116.7(5) . . ?
O6 C15 C11 116.8(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
O7 H1 O6 0.9 1.84 2.700(5) 158.1 3
O7 H2 N2 0.79 2.08 2.842(6) 162.1 3_556
O8 H3 O6 0.9 2 2.852(5) 157.5 1_655
O8 H4 O6 0.78 1.99 2.738(6) 161.5 3
C13 H13A O5 0.95 2.49 3.405(6) 162.1 1_556
C14 H14A O1 0.95 2.53 3.035(7) 113.6 .


# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1554988'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;

_audit_creation_date             2017-04-02T22:33:42-00:00
_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         'C15 H21 N2 O8 Y'
_chemical_formula_sum            'C15 H21 N2 O8 Y'
_chemical_formula_weight         446.25

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.7630(5)
_cell_length_b                   29.772(2)
_cell_length_c                   8.2595(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.8460(10)
_cell_angle_gamma                90
_cell_volume                     1836.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5107
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      30.37

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

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             912

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

_exptl_absorpt_coefficient_mu    3.22
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_T_min  0.3597
_exptl_absorpt_correction_T_max  0.648

#----------------------------------------------------------------------------#
#                   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  0.0528
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_number            22694
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.653
_diffrn_reflns_theta_max         31.005
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.99
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.99
_reflns_Friedel_coverage         0
_reflns_number_total             5789
_reflns_number_gt                4542
_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+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5789
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.087
_refine_ls_wR_factor_gt          0.0815
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.091

#----------------------------------------------------------------------------#
#                   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'
Y Y -2.7962 3.5667 '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
Y1 Y 0.27388(3) 0.09484(2) 0.18463(2) 0.01171(6) Uani 1 1 d . . . . .
O1 O 0.4544(2) 0.09618(5) 0.45671(19) 0.0171(3) Uani 1 1 d . . . . .
O2 O 0.5394(2) 0.12302(5) 0.16625(19) 0.0179(3) Uani 1 1 d . . . . .
O3 O 0.2199(2) 0.16344(5) 0.28190(19) 0.0183(3) Uani 1 1 d . . . . .
O4 O 0.1738(2) 0.13949(5) -0.05123(19) 0.0199(3) Uani 1 1 d . . . . .
O5 O -0.0053(2) 0.06365(5) 0.03753(18) 0.0169(3) Uani 1 1 d . . . . .
O6 O -0.27108(19) 0.03247(5) 0.02351(18) 0.0149(3) Uani 1 1 d . . . . .
O7 O 0.3274(2) 0.01663(5) 0.26038(19) 0.0166(3) Uani 1 1 d . . . . .
H1 H 0.298014 -0.00145 0.1827 0.02 Uiso 1 1 d R U . . .
H2 H 0.283114 0.00135 0.3363 0.02 Uiso 1 1 d R U . . .
O8 O 0.3605(2) 0.05632(5) -0.03952(19) 0.0161(3) Uani 1 1 d . . . . .
H3 H 0.471698 0.056473 -0.033646 0.019 Uiso 1 1 d R U . . .
H4 H 0.341198 0.030973 -0.062746 0.019 Uiso 1 1 d R U . . .
N1 N 0.0642(2) 0.07594(6) 0.3707(2) 0.0121(3) Uani 1 1 d . . . . .
N2 N -0.1635(2) 0.03879(6) 0.5448(2) 0.0154(4) Uani 1 1 d . . . . .
C1 C 0.6302(3) 0.12397(9) 0.7173(3) 0.0253(5) Uani 1 1 d . . . . .
H1A H 0.65158 0.093394 0.76226 0.038 Uiso 1 1 calc R U . . .
H1B H 0.532287 0.137612 0.754049 0.038 Uiso 1 1 calc R U . . .
H1C H 0.739134 0.141931 0.758957 0.038 Uiso 1 1 calc R U . . .
C2 C 0.5804(3) 0.12241(7) 0.5278(3) 0.0169(4) Uani 1 1 d . . . . .
C3 C 0.6766(3) 0.14903(8) 0.4413(3) 0.0207(5) Uani 1 1 d . . . . .
H3A H 0.762469 0.169512 0.505274 0.025 Uiso 1 1 calc R U . . .
C4 C 0.6541(3) 0.14727(7) 0.2678(3) 0.0178(4) Uani 1 1 d . . . . .
C5 C 0.7740(3) 0.17498(9) 0.1907(3) 0.0267(5) Uani 1 1 d . . . . .
H5A H 0.700875 0.195634 0.107452 0.04 Uiso 1 1 calc R U . . .
H5B H 0.841217 0.155072 0.135619 0.04 Uiso 1 1 calc R U . . .
H5C H 0.857834 0.192231 0.279075 0.04 Uiso 1 1 calc R U . . .
C6 C 0.2336(4) 0.24041(9) 0.3493(3) 0.0308(6) Uani 1 1 d . . . . .
H6A H 0.130855 0.238756 0.396424 0.046 Uiso 1 1 calc R U . . .
H6B H 0.232717 0.269376 0.292654 0.046 Uiso 1 1 calc R U . . .
H6C H 0.344727 0.237496 0.440058 0.046 Uiso 1 1 calc R U . . .
C7 C 0.2223(3) 0.20290(8) 0.2242(3) 0.0202(5) Uani 1 1 d . . . . .
C8 C 0.2109(3) 0.21338(8) 0.0575(3) 0.0250(5) Uani 1 1 d . . . . .
H8A H 0.223456 0.243938 0.029625 0.03 Uiso 1 1 calc R U . . .
C9 C 0.1818(3) 0.18136(8) -0.0720(3) 0.0218(5) Uani 1 1 d . . . . .
C10 C 0.1572(4) 0.19748(9) -0.2496(3) 0.0313(6) Uani 1 1 d . . . . .
H10A H 0.089361 0.175059 -0.328531 0.047 Uiso 1 1 calc R U . . .
H10B H 0.274645 0.20189 -0.26992 0.047 Uiso 1 1 calc R U . . .
H10C H 0.091556 0.225982 -0.265961 0.047 Uiso 1 1 calc R U . . .
C11 C -0.0885(3) 0.05487(7) 0.2901(2) 0.0106(4) Uani 1 1 d . . . . .
C12 C -0.2017(3) 0.03675(7) 0.3774(3) 0.0129(4) Uani 1 1 d . . . . .
H12A H -0.309326 0.022516 0.316147 0.016 Uiso 1 1 calc R U . . .
C13 C -0.0144(3) 0.06141(7) 0.6241(3) 0.0159(4) Uani 1 1 d . . . . .
H13A H 0.014236 0.064931 0.742842 0.019 Uiso 1 1 calc R U . . .
C14 C 0.0986(3) 0.07976(7) 0.5375(3) 0.0152(4) Uani 1 1 d . . . . .
H14A H 0.202859 0.095409 0.598273 0.018 Uiso 1 1 calc R U . . .
C15 C -0.1239(3) 0.05007(7) 0.1021(3) 0.0122(4) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   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
Y1 O2 2.2683(15) . ?
Y1 O3 2.2752(16) . ?
Y1 O1 2.3012(15) . ?
Y1 O4 2.3107(15) . ?
Y1 O5 2.3657(15) . ?
Y1 O7 2.4175(15) . ?
Y1 O8 2.4236(15) . ?
Y1 N1 2.5874(17) . ?
O1 C2 1.264(3) . ?
O2 C4 1.269(3) . ?
O3 C7 1.270(3) . ?
O4 C9 1.262(3) . ?
O5 C15 1.251(2) . ?
O6 C15 1.263(2) . ?
O7 H1 0.8207 . ?
O7 H2 0.9143 . ?
O8 H3 0.8516 . ?
O8 H4 0.783 . ?
N1 C14 1.334(3) . ?
N1 C11 1.346(2) . ?
N2 C12 1.334(3) . ?
N2 C13 1.344(3) . ?
C1 C2 1.508(3) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.410(3) . ?
C3 C4 1.397(3) . ?
C3 H3A 0.95 . ?
C4 C5 1.509(3) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.508(3) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.391(3) . ?
C8 C9 1.404(3) . ?
C8 H8A 0.95 . ?
C9 C10 1.505(3) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.389(3) . ?
C11 C15 1.508(3) . ?
C12 H12A 0.95 . ?
C13 C14 1.387(3) . ?
C13 H13A 0.95 . ?
C14 H14A 0.95 . ?

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
O2 Y1 O3 87.13(6) . . ?
O2 Y1 O1 74.74(5) . . ?
O3 Y1 O1 76.19(5) . . ?
O2 Y1 O4 80.41(6) . . ?
O3 Y1 O4 74.29(6) . . ?
O1 Y1 O4 142.03(6) . . ?
O2 Y1 O5 146.35(5) . . ?
O3 Y1 O5 107.61(6) . . ?
O1 Y1 O5 137.43(5) . . ?
O4 Y1 O5 75.10(5) . . ?
O2 Y1 O7 106.17(5) . . ?
O3 Y1 O7 143.95(5) . . ?
O1 Y1 O7 75.41(5) . . ?
O4 Y1 O7 140.07(5) . . ?
O5 Y1 O7 79.83(5) . . ?
O2 Y1 O8 71.18(5) . . ?
O3 Y1 O8 144.17(5) . . ?
O1 Y1 O8 122.16(5) . . ?
O4 Y1 O8 74.20(5) . . ?
O5 Y1 O8 80.10(5) . . ?
O7 Y1 O8 71.22(5) . . ?
O2 Y1 N1 148.27(5) . . ?
O3 Y1 N1 77.23(6) . . ?
O1 Y1 N1 74.79(5) . . ?
O4 Y1 N1 120.31(6) . . ?
O5 Y1 N1 65.37(5) . . ?
O7 Y1 N1 74.23(5) . . ?
O8 Y1 N1 134.55(5) . . ?
C2 O1 Y1 130.68(14) . . ?
C4 O2 Y1 130.76(14) . . ?
C7 O3 Y1 132.46(15) . . ?
C9 O4 Y1 131.70(15) . . ?
C15 O5 Y1 125.87(13) . . ?
Y1 O7 H1 116 . . ?
Y1 O7 H2 125.9 . . ?
H1 O7 H2 97.7 . . ?
Y1 O8 H3 116.3 . . ?
Y1 O8 H4 124.7 . . ?
H3 O8 H4 98.2 . . ?
C14 N1 C11 116.82(18) . . ?
C14 N1 Y1 127.88(14) . . ?
C11 N1 Y1 114.79(13) . . ?
C12 N2 C13 116.50(18) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.2(2) . . ?
O1 C2 C1 116.6(2) . . ?
C3 C2 C1 119.2(2) . . ?
C4 C3 C2 124.3(2) . . ?
C4 C3 H3A 117.9 . . ?
C2 C3 H3A 117.9 . . ?
O2 C4 C3 124.6(2) . . ?
O2 C4 C5 115.8(2) . . ?
C3 C4 C5 119.6(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 125.1(2) . . ?
O3 C7 C6 115.6(2) . . ?
C8 C7 C6 119.2(2) . . ?
C7 C8 C9 123.7(2) . . ?
C7 C8 H8A 118.1 . . ?
C9 C8 H8A 118.1 . . ?
O4 C9 C8 124.8(2) . . ?
O4 C9 C10 116.7(2) . . ?
C8 C9 C10 118.5(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 121.40(18) . . ?
N1 C11 C15 116.24(17) . . ?
C12 C11 C15 122.28(18) . . ?
N2 C12 C11 121.80(19) . . ?
N2 C12 H12A 119.1 . . ?
C11 C12 H12A 119.1 . . ?
N2 C13 C14 121.83(19) . . ?
N2 C13 H13A 119.1 . . ?
C14 C13 H13A 119.1 . . ?
N1 C14 C13 121.5(2) . . ?
N1 C14 H14A 119.2 . . ?
C13 C14 H14A 119.2 . . ?
O5 C15 O6 125.68(19) . . ?
O5 C15 C11 117.37(18) . . ?
O6 C15 C11 116.95(18) . . ?

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
O7 H2 N2 0.91 1.94 2.837(2) 167.6 3_556
O7 H1 O6 0.82 1.9 2.696(2) 163.7 3
O8 H4 O6 0.78 2.02 2.745(2) 154.9 3
O8 H3 O6 0.85 2.05 2.854(2) 156.9 1_655
C13 H13A O5 0.95 2.48 3.396(3) 162 1_556
C14 H14A O1 0.95 2.54 3.053(3) 114.4 .

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1554981'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;

_audit_creation_date             2017-03-24T17:26:24-00:00
_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         'C15 H21 Gd N2 O8'
_chemical_formula_sum            'C15 H21 Gd N2 O8'
_chemical_formula_weight         514.59

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.8191(9)
_cell_length_b                   29.984(3)
_cell_length_c                   8.2673(9)
_cell_angle_alpha                90
_cell_angle_beta                 105.950(2)
_cell_angle_gamma                90
_cell_volume                     1863.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5258
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      30.12

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

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1012

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

_exptl_absorpt_coefficient_mu    3.603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.7461

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

_diffrn_ambient_temperature      173(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  0.0375
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_number            16029
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.651
_diffrn_reflns_theta_max         30.606
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_reflns_Friedel_coverage         0
_reflns_number_total             5575
_reflns_number_gt                4610
_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+3.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5575
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.0804
_refine_ls_wR_factor_gt          0.0761
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.257
_refine_diff_density_min         -2.339
_refine_diff_density_rms         0.142

#----------------------------------------------------------------------------#
#                   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'
Gd Gd -0.1653 3.9035 '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
Gd1 Gd 0.27378(3) 0.09497(2) 0.18403(2) 0.01502(6) Uani 1 1 d . . . . .
O1 O 0.4550(4) 0.09714(9) 0.4600(4) 0.0220(6) Uani 1 1 d . . . . .
O2 O 0.5433(4) 0.12289(10) 0.1690(4) 0.0227(6) Uani 1 1 d . . . . .
O3 O 0.2209(4) 0.16469(9) 0.2790(4) 0.0232(6) Uani 1 1 d . . . . .
O4 O 0.1747(4) 0.14017(9) -0.0546(4) 0.0250(6) Uani 1 1 d . . . . .
O5 O -0.0105(4) 0.06367(10) 0.0374(3) 0.0208(6) Uani 1 1 d . . . . .
O6 O -0.2719(4) 0.03208(9) 0.0264(3) 0.0187(6) Uani 1 1 d . . . . .
O7 O 0.3281(4) 0.01577(9) 0.2611(3) 0.0202(6) Uani 1 1 d . . . . .
H1 H 0.3031 -0.001574 0.165468 0.024 Uiso 1 1 d R U . . .
H2 H 0.27472 -0.003374 0.318388 0.024 Uiso 1 1 d R U . . .
O8 O 0.3624(4) 0.05587(9) -0.0435(4) 0.0206(6) Uani 1 1 d . . . . .
H3 H 0.481297 0.05498 -0.046901 0.025 Uiso 1 1 d R U . . .
H4 H 0.333497 0.03158 -0.036101 0.025 Uiso 1 1 d R U . . .
N1 N 0.0623(4) 0.07567(10) 0.3711(4) 0.0151(6) Uani 1 1 d . . . . .
N2 N -0.1621(5) 0.03902(11) 0.5458(4) 0.0193(7) Uani 1 1 d . . . . .
C1 C 0.6322(7) 0.12434(17) 0.7204(6) 0.0326(10) Uani 1 1 d . . . . .
H1A H 0.657961 0.094061 0.765032 0.049 Uiso 1 1 calc R U . . .
H1B H 0.533307 0.136782 0.757421 0.049 Uiso 1 1 calc R U . . .
H1C H 0.737778 0.143098 0.761859 0.049 Uiso 1 1 calc R U . . .
C2 C 0.5821(6) 0.12293(13) 0.5312(5) 0.0207(8) Uani 1 1 d . . . . .
C3 C 0.6778(6) 0.14855(13) 0.4446(6) 0.0244(9) Uani 1 1 d . . . . .
H3A H 0.764131 0.168611 0.508765 0.029 Uiso 1 1 calc R U . . .
C4 C 0.6565(5) 0.14700(12) 0.2713(6) 0.0205(8) Uani 1 1 d . . . . .
C5 C 0.7778(7) 0.17420(16) 0.1959(7) 0.0335(10) Uani 1 1 d . . . . .
H5A H 0.843297 0.154281 0.140201 0.05 Uiso 1 1 calc R U . . .
H5B H 0.862169 0.19083 0.285122 0.05 Uiso 1 1 calc R U . . .
H5C H 0.706748 0.195155 0.113393 0.05 Uiso 1 1 calc R U . . .
C6 C 0.2325(8) 0.24128(15) 0.3437(7) 0.0416(13) Uani 1 1 d . . . . .
H6A H 0.129127 0.240344 0.388963 0.062 Uiso 1 1 calc R U . . .
H6B H 0.235019 0.269907 0.287247 0.062 Uiso 1 1 calc R U . . .
H6C H 0.341577 0.237924 0.43588 0.062 Uiso 1 1 calc R U . . .
C7 C 0.2200(6) 0.20378(13) 0.2192(6) 0.0257(9) Uani 1 1 d . . . . .
C8 C 0.2118(7) 0.21385(15) 0.0535(6) 0.0336(11) Uani 1 1 d . . . . .
H8A H 0.226031 0.244094 0.025584 0.04 Uiso 1 1 calc R U . . .
C9 C 0.1833(6) 0.18171(14) -0.0760(6) 0.0274(9) Uani 1 1 d . . . . .
C10 C 0.1602(8) 0.19763(17) -0.2536(6) 0.0397(13) Uani 1 1 d . . . . .
H10A H 0.102118 0.174286 -0.332686 0.06 Uiso 1 1 calc R U . . .
H10B H 0.276957 0.204359 -0.270031 0.06 Uiso 1 1 calc R U . . .
H10C H 0.086555 0.224593 -0.273627 0.06 Uiso 1 1 calc R U . . .
C11 C -0.0892(5) 0.05478(11) 0.2916(5) 0.0136(7) Uani 1 1 d . . . . .
C12 C -0.2013(5) 0.03703(12) 0.3791(5) 0.0168(7) Uani 1 1 d . . . . .
H12A H -0.308925 0.023105 0.318278 0.02 Uiso 1 1 calc R U . . .
C13 C -0.0151(6) 0.06104(13) 0.6253(5) 0.0205(8) Uani 1 1 d . . . . .
H13A H 0.0135 0.064403 0.744032 0.025 Uiso 1 1 calc R U . . .
C14 C 0.0970(6) 0.07914(13) 0.5389(5) 0.0196(8) Uani 1 1 d . . . . .
H14A H 0.201148 0.094428 0.599962 0.024 Uiso 1 1 calc R U . . .
C15 C -0.1263(5) 0.04997(12) 0.1028(5) 0.0146(7) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   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
Gd1 O2 2.302(3) . ?
Gd1 O3 2.310(3) . ?
Gd1 O1 2.333(3) . ?
Gd1 O4 2.343(3) . ?
Gd1 O5 2.411(3) . ?
Gd1 O7 2.465(3) . ?
Gd1 O8 2.472(3) . ?
Gd1 N1 2.620(3) . ?
O1 C2 1.269(5) . ?
O2 C4 1.269(5) . ?
O3 C7 1.271(5) . ?
O4 C9 1.262(5) . ?
O5 C15 1.245(4) . ?
O6 C15 1.260(5) . ?
O7 H1 0.9211 . ?
O7 H2 0.9147 . ?
O8 H3 0.9384 . ?
O8 H4 0.7699 . ?
N1 C11 1.341(5) . ?
N1 C14 1.343(5) . ?
N2 C12 1.328(5) . ?
N2 C13 1.332(5) . ?
C1 C2 1.505(6) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.399(6) . ?
C3 C4 1.397(6) . ?
C3 H3A 0.95 . ?
C4 C5 1.510(6) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.510(6) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.386(7) . ?
C8 C9 1.412(6) . ?
C8 H8A 0.95 . ?
C9 C10 1.507(6) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.387(5) . ?
C11 C15 1.514(5) . ?
C12 H12A 0.95 . ?
C13 C14 1.385(6) . ?
C13 H13A 0.95 . ?
C14 H14A 0.95 . ?

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
O2 Gd1 O3 86.63(10) . . ?
O2 Gd1 O1 73.97(10) . . ?
O3 Gd1 O1 76.09(10) . . ?
O2 Gd1 O4 80.78(11) . . ?
O3 Gd1 O4 73.39(10) . . ?
O1 Gd1 O4 141.17(10) . . ?
O2 Gd1 O5 147.72(10) . . ?
O3 Gd1 O5 107.28(10) . . ?
O1 Gd1 O5 136.98(10) . . ?
O4 Gd1 O5 75.87(10) . . ?
O2 Gd1 O7 105.61(10) . . ?
O3 Gd1 O7 144.90(10) . . ?
O1 Gd1 O7 76.05(10) . . ?
O4 Gd1 O7 140.21(10) . . ?
O5 Gd1 O7 79.89(10) . . ?
O2 Gd1 O8 71.29(10) . . ?
O3 Gd1 O8 143.30(9) . . ?
O1 Gd1 O8 122.39(10) . . ?
O4 Gd1 O8 74.36(10) . . ?
O5 Gd1 O8 81.08(10) . . ?
O7 Gd1 O8 71.05(9) . . ?
O2 Gd1 N1 147.96(10) . . ?
O3 Gd1 N1 78.37(10) . . ?
O1 Gd1 N1 74.99(10) . . ?
O4 Gd1 N1 120.57(11) . . ?
O5 Gd1 N1 64.32(9) . . ?
O7 Gd1 N1 74.13(9) . . ?
O8 Gd1 N1 134.32(9) . . ?
C2 O1 Gd1 131.1(3) . . ?
C4 O2 Gd1 130.7(3) . . ?
C7 O3 Gd1 133.2(3) . . ?
C9 O4 Gd1 132.1(3) . . ?
C15 O5 Gd1 126.1(2) . . ?
Gd1 O7 H1 109.9 . . ?
Gd1 O7 H2 131.9 . . ?
H1 O7 H2 94.1 . . ?
Gd1 O8 H3 121.6 . . ?
Gd1 O8 H4 103.8 . . ?
H3 O8 H4 106.9 . . ?
C11 N1 C14 116.3(3) . . ?
C11 N1 Gd1 115.4(2) . . ?
C14 N1 Gd1 127.7(3) . . ?
C12 N2 C13 117.1(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.0(4) . . ?
O1 C2 C1 116.5(4) . . ?
C3 C2 C1 119.6(4) . . ?
C4 C3 C2 125.2(4) . . ?
C4 C3 H3A 117.4 . . ?
C2 C3 H3A 117.4 . . ?
O2 C4 C3 124.6(4) . . ?
O2 C4 C5 115.8(4) . . ?
C3 C4 C5 119.6(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 125.4(4) . . ?
O3 C7 C6 115.4(4) . . ?
C8 C7 C6 119.2(4) . . ?
C7 C8 C9 123.7(4) . . ?
C7 C8 H8A 118.1 . . ?
C9 C8 H8A 118.1 . . ?
O4 C9 C8 124.8(4) . . ?
O4 C9 C10 116.9(4) . . ?
C8 C9 C10 118.3(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 121.6(3) . . ?
N1 C11 C15 116.3(3) . . ?
C12 C11 C15 122.1(3) . . ?
N2 C12 C11 121.7(4) . . ?
N2 C12 H12A 119.2 . . ?
C11 C12 H12A 119.2 . . ?
N2 C13 C14 121.5(4) . . ?
N2 C13 H13A 119.3 . . ?
C14 C13 H13A 119.3 . . ?
N1 C14 C13 121.8(4) . . ?
N1 C14 H14A 119.1 . . ?
C13 C14 H14A 119.1 . . ?
O5 C15 O6 125.9(4) . . ?
O5 C15 C11 117.4(3) . . ?
O6 C15 C11 116.7(3) . . ?

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
O7 H1 O6 0.92 1.79 2.706(4) 174.1 3
O7 H2 N2 0.91 1.93 2.841(4) 174.4 3_556
O8 H3 O6 0.94 1.98 2.848(4) 153 1_655
O8 H4 O6 0.77 1.98 2.744(4) 175.8 3
C13 H13A O5 0.95 2.48 3.398(5) 161.5 1_556
C14 H14A O1 0.95 2.56 3.091(5) 115.7 .


# 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 1554986'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;

_audit_creation_date             2017-03-09T13:34:41-00:00
_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         'C15 H21 N2 O8 Tm'
_chemical_formula_sum            'C15 H21 N2 O8 Tm'
_chemical_formula_weight         526.27

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.7410(7)
_cell_length_b                   29.734(3)
_cell_length_c                   8.2614(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.8110(10)
_cell_angle_gamma                90
_cell_volume                     1829.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4701
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      30.36

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

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1032

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

_exptl_absorpt_coefficient_mu    4.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_T_min  0.4999
_exptl_absorpt_correction_T_max  0.7462

#----------------------------------------------------------------------------#
#                   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  0.0484
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_number            20052
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.652
_diffrn_reflns_theta_max         31.53
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.972
_reflns_Friedel_coverage         0
_reflns_number_total             5941
_reflns_number_gt                4966
_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, 2015)'
_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+2.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5941
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0807
_refine_ls_wR_factor_gt          0.0765
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.53
_refine_diff_density_rms         0.166

#----------------------------------------------------------------------------#
#                   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 0.27305(2) 0.09452(2) 0.18525(2) 0.01305(5) Uani 1 1 d . . . . .
O1 O 0.4527(4) 0.09570(10) 0.4545(3) 0.0179(6) Uani 1 1 d . . . . .
O2 O 0.5349(4) 0.12319(10) 0.1652(4) 0.0203(6) Uani 1 1 d . . . . .
O3 O 0.2201(4) 0.16253(10) 0.2826(4) 0.0197(6) Uani 1 1 d . . . . .
O4 O 0.1730(4) 0.13870(10) -0.0484(4) 0.0212(6) Uani 1 1 d . . . . .
O5 O -0.0022(4) 0.06285(10) 0.0380(3) 0.0190(6) Uani 1 1 d . . . . .
O6 O -0.2705(3) 0.03263(10) 0.0223(3) 0.0169(6) Uani 1 1 d . . . . .
O7 O 0.3277(4) 0.01693(9) 0.2606(3) 0.0176(6) Uani 1 1 d . . . . .
H1 H 0.312845 0.00482 0.345499 0.021 Uiso 1 1 d R U . . .
H2 H 0.296645 -0.00198 0.186899 0.021 Uiso 1 1 d R U . . .
O8 O 0.3594(4) 0.05644(10) -0.0376(3) 0.0179(6) Uani 1 1 d . . . . .
H3 H 0.335884 0.030396 -0.056878 0.021 Uiso 1 1 d R U . . .
H4 H 0.466684 0.058196 -0.046978 0.021 Uiso 1 1 d R U . . .
N1 N 0.0649(4) 0.07586(11) 0.3696(4) 0.0125(6) Uani 1 1 d . . . . .
N2 N -0.1646(4) 0.03878(12) 0.5432(4) 0.0166(6) Uani 1 1 d . . . . .
C1 C 0.6277(6) 0.12386(17) 0.7152(6) 0.0283(10) Uani 1 1 d . . . . .
H1A H 0.656598 0.093433 0.759943 0.042 Uiso 1 1 calc R U . . .
H1B H 0.526595 0.135699 0.752177 0.042 Uiso 1 1 calc R U . . .
H1C H 0.73245 0.143394 0.756629 0.042 Uiso 1 1 calc R U . . .
C2 C 0.5778(5) 0.12243(14) 0.5257(5) 0.0186(8) Uani 1 1 d . . . . .
C3 C 0.6737(6) 0.14905(14) 0.4389(6) 0.0232(9) Uani 1 1 d . . . . .
H3A H 0.759305 0.16968 0.502586 0.028 Uiso 1 1 calc R U . . .
C4 C 0.6517(5) 0.14721(14) 0.2672(5) 0.0186(8) Uani 1 1 d . . . . .
C5 C 0.7710(6) 0.17479(17) 0.1890(6) 0.0313(10) Uani 1 1 d . . . . .
H5A H 0.697173 0.195166 0.104854 0.047 Uiso 1 1 calc R U . . .
H5B H 0.838912 0.154755 0.134679 0.047 Uiso 1 1 calc R U . . .
H5C H 0.854647 0.192384 0.276466 0.047 Uiso 1 1 calc R U . . .
C6 C 0.2343(7) 0.23965(16) 0.3522(6) 0.0345(11) Uani 1 1 d . . . . .
H6A H 0.125988 0.239568 0.391925 0.052 Uiso 1 1 calc R U . . .
H6B H 0.244037 0.268533 0.29825 0.052 Uiso 1 1 calc R U . . .
H6C H 0.340152 0.235245 0.447937 0.052 Uiso 1 1 calc R U . . .
C7 C 0.2231(5) 0.20193(15) 0.2264(6) 0.0223(9) Uani 1 1 d . . . . .
C8 C 0.2122(6) 0.21264(15) 0.0602(6) 0.0281(10) Uani 1 1 d . . . . .
H8A H 0.226134 0.243211 0.032792 0.034 Uiso 1 1 calc R U . . .
C9 C 0.1817(6) 0.18066(15) -0.0693(6) 0.0243(9) Uani 1 1 d . . . . .
C10 C 0.1558(7) 0.19685(18) -0.2481(6) 0.0345(11) Uani 1 1 d . . . . .
H10A H 0.070444 0.177117 -0.325601 0.052 Uiso 1 1 calc R U . . .
H10B H 0.271238 0.196271 -0.275563 0.052 Uiso 1 1 calc R U . . .
H10C H 0.109004 0.227653 -0.258894 0.052 Uiso 1 1 calc R U . . .
C11 C -0.0881(4) 0.05493(13) 0.2891(4) 0.0117(7) Uani 1 1 d . . . . .
C12 C -0.2023(5) 0.03681(14) 0.3755(5) 0.0157(7) Uani 1 1 d . . . . .
H12A H -0.310099 0.022627 0.31386 0.019 Uiso 1 1 calc R U . . .
C13 C -0.0156(5) 0.06143(14) 0.6223(5) 0.0179(8) Uani 1 1 d . . . . .
H13A H 0.012483 0.065164 0.740871 0.021 Uiso 1 1 calc R U . . .
C14 C 0.0986(5) 0.07954(14) 0.5359(5) 0.0166(8) Uani 1 1 d . . . . .
H14A H 0.203659 0.094973 0.596965 0.02 Uiso 1 1 calc R U . . .
C15 C -0.1229(5) 0.04993(13) 0.1014(5) 0.0127(7) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   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 O2 2.246(3) . ?
Tm1 O3 2.255(3) . ?
Tm1 O1 2.280(3) . ?
Tm1 O4 2.289(3) . ?
Tm1 O5 2.344(3) . ?
Tm1 O7 2.397(3) . ?
Tm1 O8 2.406(3) . ?
Tm1 N1 2.561(3) . ?
O1 C2 1.267(5) . ?
O2 C4 1.274(5) . ?
O3 C7 1.263(5) . ?
O4 C9 1.264(5) . ?
O5 C15 1.250(4) . ?
O6 C15 1.261(4) . ?
O7 H1 0.8239 . ?
O7 H2 0.8154 . ?
O8 H3 0.8013 . ?
O8 H4 0.8564 . ?
N1 C14 1.331(5) . ?
N1 C11 1.343(4) . ?
N2 C12 1.337(5) . ?
N2 C13 1.342(5) . ?
C1 C2 1.507(6) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.408(6) . ?
C3 C4 1.383(6) . ?
C3 H3A 0.95 . ?
C4 C5 1.506(6) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.516(6) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.390(6) . ?
C8 C9 1.402(6) . ?
C8 H8A 0.95 . ?
C9 C10 1.514(6) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.387(5) . ?
C11 C15 1.507(5) . ?
C12 H12A 0.95 . ?
C13 C14 1.388(6) . ?
C13 H13A 0.95 . ?
C14 H14A 0.95 . ?

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
O2 Tm1 O3 86.62(10) . . ?
O2 Tm1 O1 75.13(10) . . ?
O3 Tm1 O1 76.10(10) . . ?
O2 Tm1 O4 79.90(10) . . ?
O3 Tm1 O4 74.54(10) . . ?
O1 Tm1 O4 142.23(10) . . ?
O2 Tm1 O5 145.61(10) . . ?
O3 Tm1 O5 108.52(10) . . ?
O1 Tm1 O5 137.65(10) . . ?
O4 Tm1 O5 75.05(10) . . ?
O2 Tm1 O7 106.59(10) . . ?
O3 Tm1 O7 143.80(10) . . ?
O1 Tm1 O7 75.16(10) . . ?
O4 Tm1 O7 140.06(10) . . ?
O5 Tm1 O7 79.59(10) . . ?
O2 Tm1 O8 71.21(10) . . ?
O3 Tm1 O8 144.13(10) . . ?
O1 Tm1 O8 122.09(10) . . ?
O4 Tm1 O8 74.05(10) . . ?
O5 Tm1 O8 79.43(9) . . ?
O7 Tm1 O8 71.32(9) . . ?
O2 Tm1 N1 148.49(10) . . ?
O3 Tm1 N1 77.13(10) . . ?
O1 Tm1 N1 74.84(10) . . ?
O4 Tm1 N1 120.18(10) . . ?
O5 Tm1 N1 65.87(9) . . ?
O7 Tm1 N1 74.47(10) . . ?
O8 Tm1 N1 134.74(10) . . ?
C2 O1 Tm1 130.4(3) . . ?
C4 O2 Tm1 131.0(3) . . ?
C7 O3 Tm1 132.7(3) . . ?
C9 O4 Tm1 131.6(3) . . ?
C15 O5 Tm1 125.7(2) . . ?
Tm1 O7 H1 125.9 . . ?
Tm1 O7 H2 118.3 . . ?
H1 O7 H2 104.7 . . ?
Tm1 O8 H3 120.7 . . ?
Tm1 O8 H4 121.2 . . ?
H3 O8 H4 102.4 . . ?
C14 N1 C11 116.6(3) . . ?
C14 N1 Tm1 128.1(2) . . ?
C11 N1 Tm1 114.8(2) . . ?
C12 N2 C13 116.3(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.9(4) . . ?
O1 C2 C1 116.6(4) . . ?
C3 C2 C1 119.4(4) . . ?
C4 C3 C2 124.5(4) . . ?
C4 C3 H3A 117.8 . . ?
C2 C3 H3A 117.8 . . ?
O2 C4 C3 124.6(4) . . ?
O2 C4 C5 115.4(4) . . ?
C3 C4 C5 120.0(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 125.0(4) . . ?
O3 C7 C6 116.0(4) . . ?
C8 C7 C6 119.0(4) . . ?
C7 C8 C9 123.4(4) . . ?
C7 C8 H8A 118.3 . . ?
C9 C8 H8A 118.3 . . ?
O4 C9 C8 124.7(4) . . ?
O4 C9 C10 116.7(4) . . ?
C8 C9 C10 118.6(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 121.6(3) . . ?
N1 C11 C15 116.2(3) . . ?
C12 C11 C15 122.1(3) . . ?
N2 C12 C11 121.8(3) . . ?
N2 C12 H12A 119.1 . . ?
C11 C12 H12A 119.1 . . ?
N2 C13 C14 121.8(3) . . ?
N2 C13 H13A 119.1 . . ?
C14 C13 H13A 119.1 . . ?
N1 C14 C13 121.7(3) . . ?
N1 C14 H14A 119.1 . . ?
C13 C14 H14A 119.1 . . ?
O5 C15 O6 125.7(3) . . ?
O5 C15 C11 117.2(3) . . ?
O6 C15 C11 117.2(3) . . ?

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
O7 H1 N2 0.82 2.1 2.843(4) 149.5 3_556
O7 H2 O6 0.82 1.92 2.695(4) 159.9 3
O8 H3 O6 0.8 1.98 2.748(4) 159.7 3
O8 H4 O6 0.86 2.1 2.860(4) 147.6 1_655
C13 H13A O5 0.95 2.49 3.408(5) 162.6 1_556
C14 H14A O1 0.95 2.52 3.033(5) 114.2 .


# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1554982'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;

_audit_creation_date             2017-03-09T13:25:46-00:00
_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         'C15 H21 N2 O8 Tb'
_chemical_formula_sum            'C15 H21 N2 O8 Tb'
_chemical_formula_weight         516.26

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.7951(5)
_cell_length_b                   29.903(2)
_cell_length_c                   8.2627(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.8510(10)
_cell_angle_gamma                90
_cell_volume                     1852.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7054
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      31.43

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

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.2
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1016

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

_exptl_absorpt_coefficient_mu    3.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_T_min  0.5086
_exptl_absorpt_correction_T_max  0.7462

#----------------------------------------------------------------------------#
#                   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  0.0359
_diffrn_reflns_av_unetI/netI     0.036
_diffrn_reflns_number            21133
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.651
_diffrn_reflns_theta_max         31.564
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.972
_reflns_Friedel_coverage         0
_reflns_number_total             6036
_reflns_number_gt                5396
_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, 2015)'
_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)+(0.0200P)²+3.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6036
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0671
_refine_ls_wR_factor_gt          0.0652
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.136
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.028
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.13

#----------------------------------------------------------------------------#
#                   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'
Tb Tb -0.1723 4.1537 '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
Tb1 Tb 0.27386(2) 0.09502(2) 0.18426(2) 0.01299(4) Uani 1 1 d . . . . .
O1 O 0.4548(3) 0.09683(7) 0.4588(3) 0.0184(4) Uani 1 1 d . . . . .
O2 O 0.5420(3) 0.12309(8) 0.1678(3) 0.0203(5) Uani 1 1 d . . . . .
O3 O 0.2221(3) 0.16440(8) 0.2800(3) 0.0207(5) Uani 1 1 d . . . . .
O4 O 0.1748(3) 0.14001(8) -0.0535(3) 0.0222(5) Uani 1 1 d . . . . .
O5 O -0.0080(3) 0.06372(8) 0.0377(3) 0.0189(4) Uani 1 1 d . . . . .
O6 O -0.2713(3) 0.03232(7) 0.0251(3) 0.0172(4) Uani 1 1 d . . . . .
O7 O 0.3284(3) 0.01621(7) 0.2604(3) 0.0177(4) Uani 1 1 d . . . . .
H1 H 0.302787 -0.001988 0.182799 0.021 Uiso 1 1 d R U . . .
H2 H 0.284287 0.002612 0.317399 0.021 Uiso 1 1 d R U . . .
O8 O 0.3613(3) 0.05601(7) -0.0431(3) 0.0178(4) Uani 1 1 d . . . . .
H3 H 0.466531 0.059679 -0.04227 0.021 Uiso 1 1 d R U . . .
H4 H 0.330731 0.028979 -0.05157 0.021 Uiso 1 1 d R U . . .
N1 N 0.0626(3) 0.07574(8) 0.3708(3) 0.0136(5) Uani 1 1 d . . . . .
N2 N -0.1626(3) 0.03893(9) 0.5461(3) 0.0173(5) Uani 1 1 d . . . . .
C1 C 0.6316(5) 0.12414(13) 0.7194(4) 0.0290(8) Uani 1 1 d . . . . .
H1A H 0.650235 0.093611 0.763882 0.043 Uiso 1 1 calc R U . . .
H1B H 0.535495 0.138322 0.756371 0.043 Uiso 1 1 calc R U . . .
H1C H 0.741752 0.141404 0.761046 0.043 Uiso 1 1 calc R U . . .
C2 C 0.5816(4) 0.12271(10) 0.5299(4) 0.0181(6) Uani 1 1 d . . . . .
C3 C 0.6781(4) 0.14880(11) 0.4431(4) 0.0228(6) Uani 1 1 d . . . . .
H3A H 0.764322 0.169001 0.507141 0.027 Uiso 1 1 calc R U . . .
C4 C 0.6562(4) 0.14714(10) 0.2699(4) 0.0198(6) Uani 1 1 d . . . . .
C5 C 0.7769(5) 0.17463(13) 0.1938(5) 0.0296(8) Uani 1 1 d . . . . .
H5A H 0.704883 0.195197 0.110086 0.044 Uiso 1 1 calc R U . . .
H5B H 0.844383 0.154735 0.13953 0.044 Uiso 1 1 calc R U . . .
H5C H 0.859947 0.191797 0.282548 0.044 Uiso 1 1 calc R U . . .
C6 C 0.2345(6) 0.24128(13) 0.3450(5) 0.0362(9) Uani 1 1 d . . . . .
H6A H 0.130334 0.240432 0.389787 0.054 Uiso 1 1 calc R U . . .
H6B H 0.237266 0.2699 0.288028 0.054 Uiso 1 1 calc R U . . .
H6C H 0.343393 0.238042 0.437617 0.054 Uiso 1 1 calc R U . . .
C7 C 0.2229(4) 0.20342(11) 0.2211(5) 0.0229(7) Uani 1 1 d . . . . .
C8 C 0.2115(5) 0.21355(12) 0.0543(5) 0.0290(8) Uani 1 1 d . . . . .
H8A H 0.223864 0.243942 0.025854 0.035 Uiso 1 1 calc R U . . .
C9 C 0.1829(4) 0.18161(12) -0.0746(4) 0.0234(7) Uani 1 1 d . . . . .
C10 C 0.1612(6) 0.19766(14) -0.2524(5) 0.0361(9) Uani 1 1 d . . . . .
H10A H 0.088685 0.176171 -0.331762 0.054 Uiso 1 1 calc R U . . .
H10B H 0.278822 0.200324 -0.272946 0.054 Uiso 1 1 calc R U . . .
H10C H 0.102195 0.226895 -0.267758 0.054 Uiso 1 1 calc R U . . .
C11 C -0.0889(4) 0.05483(9) 0.2905(4) 0.0122(5) Uani 1 1 d . . . . .
C12 C -0.2015(4) 0.03692(10) 0.3788(4) 0.0158(6) Uani 1 1 d . . . . .
H12A H -0.309135 0.022863 0.318109 0.019 Uiso 1 1 calc R U . . .
C13 C -0.0154(4) 0.06101(11) 0.6253(4) 0.0182(6) Uani 1 1 d . . . . .
H13A H 0.013426 0.064371 0.744051 0.022 Uiso 1 1 calc R U . . .
C14 C 0.0975(4) 0.07935(11) 0.5377(4) 0.0171(6) Uani 1 1 d . . . . .
H14A H 0.201842 0.094788 0.598294 0.02 Uiso 1 1 calc R U . . .
C15 C -0.1256(4) 0.04995(10) 0.1030(4) 0.0131(5) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   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
Tb1 O2 2.290(2) . ?
Tb1 O3 2.295(2) . ?
Tb1 O1 2.322(2) . ?
Tb1 O4 2.332(2) . ?
Tb1 O5 2.391(2) . ?
Tb1 O7 2.446(2) . ?
Tb1 O8 2.460(2) . ?
Tb1 N1 2.609(2) . ?
O1 C2 1.266(4) . ?
O2 C4 1.269(4) . ?
O3 C7 1.265(4) . ?
O4 C9 1.260(4) . ?
O5 C15 1.254(3) . ?
O6 C15 1.258(3) . ?
O7 H1 0.8228 . ?
O7 H2 0.7707 . ?
O8 H3 0.8259 . ?
O8 H4 0.8402 . ?
N1 C14 1.335(4) . ?
N1 C11 1.341(4) . ?
N2 C13 1.331(4) . ?
N2 C12 1.333(4) . ?
C1 C2 1.507(5) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C3 1.408(5) . ?
C3 C4 1.395(5) . ?
C3 H3A 0.95 . ?
C4 C5 1.510(5) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.512(5) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 C8 1.391(5) . ?
C8 C9 1.402(5) . ?
C8 H8A 0.95 . ?
C9 C10 1.510(5) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.392(4) . ?
C11 C15 1.504(4) . ?
C12 H12A 0.95 . ?
C13 C14 1.396(4) . ?
C13 H13A 0.95 . ?
C14 H14A 0.95 . ?

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
O2 Tb1 O3 86.46(8) . . ?
O2 Tb1 O1 74.26(8) . . ?
O3 Tb1 O1 76.07(8) . . ?
O2 Tb1 O4 80.57(8) . . ?
O3 Tb1 O4 73.75(8) . . ?
O1 Tb1 O4 141.52(8) . . ?
O2 Tb1 O5 147.20(8) . . ?
O3 Tb1 O5 107.75(8) . . ?
O1 Tb1 O5 137.14(7) . . ?
O4 Tb1 O5 75.65(8) . . ?
O2 Tb1 O7 105.73(8) . . ?
O3 Tb1 O7 144.76(8) . . ?
O1 Tb1 O7 75.80(7) . . ?
O4 Tb1 O7 140.05(8) . . ?
O5 Tb1 O7 79.87(8) . . ?
O2 Tb1 O8 71.40(8) . . ?
O3 Tb1 O8 143.45(8) . . ?
O1 Tb1 O8 122.41(7) . . ?
O4 Tb1 O8 74.17(8) . . ?
O5 Tb1 O8 80.53(7) . . ?
O7 Tb1 O8 71.01(7) . . ?
O2 Tb1 N1 148.15(8) . . ?
O3 Tb1 N1 78.31(8) . . ?
O1 Tb1 N1 74.99(8) . . ?
O4 Tb1 N1 120.54(8) . . ?
O5 Tb1 N1 64.64(7) . . ?
O7 Tb1 N1 74.25(7) . . ?
O8 Tb1 N1 134.22(7) . . ?
C2 O1 Tb1 131.0(2) . . ?
C4 O2 Tb1 130.9(2) . . ?
C7 O3 Tb1 133.0(2) . . ?
C9 O4 Tb1 131.9(2) . . ?
C15 O5 Tb1 126.14(19) . . ?
Tb1 O7 H1 116.7 . . ?
Tb1 O7 H2 126.2 . . ?
H1 O7 H2 94.2 . . ?
Tb1 O8 H3 114.4 . . ?
Tb1 O8 H4 112.9 . . ?
H3 O8 H4 112.8 . . ?
C14 N1 C11 116.9(3) . . ?
C14 N1 Tb1 127.49(19) . . ?
C11 N1 Tb1 115.06(18) . . ?
C13 N2 C12 117.0(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.1(3) . . ?
O1 C2 C1 116.5(3) . . ?
C3 C2 C1 119.4(3) . . ?
C4 C3 C2 124.8(3) . . ?
C4 C3 H3A 117.6 . . ?
C2 C3 H3A 117.6 . . ?
O2 C4 C3 124.7(3) . . ?
O2 C4 C5 115.9(3) . . ?
C3 C4 C5 119.5(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 125.2(3) . . ?
O3 C7 C6 115.8(3) . . ?
C8 C7 C6 118.9(3) . . ?
C7 C8 C9 123.9(3) . . ?
C7 C8 H8A 118 . . ?
C9 C8 H8A 118 . . ?
O4 C9 C8 124.9(3) . . ?
O4 C9 C10 116.8(3) . . ?
C8 C9 C10 118.3(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 121.1(3) . . ?
N1 C11 C15 116.7(2) . . ?
C12 C11 C15 122.2(3) . . ?
N2 C12 C11 121.9(3) . . ?
N2 C12 H12A 119 . . ?
C11 C12 H12A 119 . . ?
N2 C13 C14 121.4(3) . . ?
N2 C13 H13A 119.3 . . ?
C14 C13 H13A 119.3 . . ?
N1 C14 C13 121.6(3) . . ?
N1 C14 H14A 119.2 . . ?
C13 C14 H14A 119.2 . . ?
O5 C15 O6 125.6(3) . . ?
O5 C15 C11 117.1(2) . . ?
O6 C15 C11 117.3(2) . . ?

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
O7 H1 O6 0.82 1.9 2.701(3) 164.8 3
O7 H2 N2 0.77 2.07 2.841(3) 174.4 3_556
O8 H3 O6 0.83 2.13 2.853(3) 146.2 1_655
O8 H4 O6 0.84 1.92 2.747(3) 169.1 3
C13 H13A O5 0.95 2.48 3.393(4) 161.9 1_556
C14 H14A O1 0.95 2.54 3.073(4) 115.5 .


# END of CIF
_exptl_crystal_preparation       ', Magnetic properties'
