# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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 1515256'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H16 N3 O13 Tb'
_chemical_formula_weight         521.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.9542(13)
_cell_length_b                   8.4901(9)
_cell_length_c                   15.1312(16)
_cell_angle_alpha                90
_cell_angle_beta                 91.8560(10)
_cell_angle_gamma                90
_cell_volume                     1534.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    5403
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      27.43

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    4.687
_shelx_estimated_absorpt_T_min   0.581
_shelx_estimated_absorpt_T_max   0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5810
_exptl_absorpt_correction_T_max  0.6778
_exptl_absorpt_process_details   'SADABS (Bruker, 2011)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8841
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.704
_diffrn_reflns_theta_max         27.446
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3459
_reflns_number_gt                3225
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0226P)²+1.0857P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3459
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0476
_refine_ls_wR_factor_gt          0.0466
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C1 C 0.2150(2) 0.0709(4) 0.83230(18) 0.0217(6) Uani 1 1 d . . . . .
H1A H 0.239975 0.165418 0.800061 0.026 Uiso 1 1 calc R U . . .
H1B H 0.169674 0.004311 0.791121 0.026 Uiso 1 1 calc R U . . .
C2 C 0.3136(2) -0.0191(3) 0.86891(18) 0.0210(6) Uani 1 1 d . . . . .
H2A H 0.288383 -0.121206 0.892775 0.025 Uiso 1 1 calc R U . . .
H2B H 0.366247 -0.040795 0.821185 0.025 Uiso 1 1 calc R U . . .
C3 C 0.4642(2) 0.1656(3) 0.9133(2) 0.0211(6) Uani 1 1 d . . . . .
H3A H 0.499375 0.117464 0.861472 0.025 Uiso 1 1 calc R U . . .
H3B H 0.520710 0.168387 0.962589 0.025 Uiso 1 1 calc R U . . .
C4 C 0.4276(3) 0.3311(3) 0.8908(2) 0.0235(6) Uani 1 1 d . . . . .
H4A H 0.493493 0.401644 0.889237 0.028 Uiso 1 1 calc R U . . .
H4B H 0.388840 0.333308 0.832032 0.028 Uiso 1 1 calc R U . . .
C5 C 0.3049(2) 0.5360(3) 0.9400(2) 0.0227(6) Uani 1 1 d . . . . .
H5A H 0.290435 0.549415 0.875642 0.027 Uiso 1 1 calc R U . . .
H5B H 0.357078 0.619720 0.960693 0.027 Uiso 1 1 calc R U . . .
C6 C 0.1965(2) 0.5470(3) 0.98832(19) 0.0227(6) Uani 1 1 d . . . . .
H6A H 0.213049 0.564736 1.052082 0.027 Uiso 1 1 calc R U . . .
H6B H 0.152355 0.637627 0.965385 0.027 Uiso 1 1 calc R U . . .
C7 C 0.0839(2) 0.3805(3) 0.88888(19) 0.0225(6) Uani 1 1 d . . . . .
H7A H 0.138645 0.407270 0.843559 0.027 Uiso 1 1 calc R U . . .
H7B H 0.016602 0.447174 0.879403 0.027 Uiso 1 1 calc R U . . .
C8 C 0.0532(2) 0.2092(3) 0.88350(19) 0.0203(6) Uani 1 1 d . . . . .
H8A H -0.007815 0.186268 0.924274 0.024 Uiso 1 1 calc R U . . .
H8B H 0.026634 0.182792 0.822655 0.024 Uiso 1 1 calc R U . . .
N1 N 0.0353(2) 0.2245(3) 1.13455(15) 0.0203(5) Uani 1 1 d . . . . .
N2 N 0.2471(2) -0.0980(3) 1.15216(17) 0.0245(5) Uani 1 1 d . . . . .
N3 N 0.4330(2) 0.2904(3) 1.15561(15) 0.0203(5) Uani 1 1 d . . . . .
O1 O 0.05170(17) 0.1186(2) 1.07644(13) 0.0228(4) Uani 1 1 d . . . . .
O2 O 0.11728(17) 0.3149(2) 1.15234(13) 0.0216(4) Uani 1 1 d . . . . .
O3 O -0.05396(18) 0.2375(3) 1.17084(14) 0.0300(5) Uani 1 1 d . . . . .
O4 O 0.24401(18) 0.0366(2) 1.18921(13) 0.0255(5) Uani 1 1 d . . . . .
O5 O 0.25017(17) -0.0965(2) 1.06744(13) 0.0233(4) Uani 1 1 d . . . . .
O6 O 0.2469(2) -0.2200(3) 1.19353(16) 0.0374(6) Uani 1 1 d . . . . .
O7 O 0.34140(16) 0.3675(2) 1.15191(13) 0.0216(4) Uani 1 1 d . . . . .
O8 O 0.43675(17) 0.1683(2) 1.10707(13) 0.0230(4) Uani 1 1 d . . . . .
O9 O 0.51232(18) 0.3311(3) 1.20314(14) 0.0278(5) Uani 1 1 d . . . . .
O10 O 0.15060(16) 0.1158(2) 0.90740(12) 0.0182(4) Uani 1 1 d . . . . .
O11 O 0.37004(15) 0.0708(2) 0.93847(12) 0.0177(4) Uani 1 1 d . . . . .
O12 O 0.35291(17) 0.3827(2) 0.95799(13) 0.0207(4) Uani 1 1 d . . . . .
O13 O 0.13223(16) 0.4045(2) 0.97685(12) 0.0196(4) Uani 1 1 d . . . . .
Tb1 Tb 0.24430(2) 0.18563(2) 1.04763(2) 0.01543(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O10 1.445(3) . ?
C1 C2 1.496(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O11 1.449(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O11 1.445(3) . ?
C3 C4 1.507(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O12 1.443(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O12 1.445(3) . ?
C5 C6 1.510(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O13 1.441(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O13 1.448(3) . ?
C7 C8 1.501(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O10 1.445(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
N1 O3 1.221(3) . ?
N1 O2 1.266(3) . ?
N1 O1 1.277(3) . ?
N1 Tb1 2.879(2) . ?
N2 O6 1.211(3) . ?
N2 O4 1.273(3) . ?
N2 O5 1.284(3) . ?
N2 Tb1 2.880(2) . ?
N3 O9 1.222(3) . ?
N3 O8 1.273(3) . ?
N3 O7 1.275(3) . ?
N3 Tb1 2.883(2) . ?
O1 Tb1 2.425(2) . ?
O2 Tb1 2.485(2) . ?
O4 Tb1 2.488(2) . ?
O5 Tb1 2.414(2) . ?
O7 Tb1 2.471(2) . ?
O8 Tb1 2.447(2) . ?
O10 Tb1 2.4402(19) . ?
O11 Tb1 2.4697(18) . ?
O12 Tb1 2.5374(19) . ?
O13 Tb1 2.5100(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 C1 C2 106.1(2) . . ?
O10 C1 H1A 110.5 . . ?
C2 C1 H1A 110.5 . . ?
O10 C1 H1B 110.5 . . ?
C2 C1 H1B 110.5 . . ?
H1A C1 H1B 108.7 . . ?
O11 C2 C1 110.0(2) . . ?
O11 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
O11 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
O11 C3 C4 110.9(2) . . ?
O11 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
O11 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
O12 C4 C3 107.8(2) . . ?
O12 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
O12 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.5 . . ?
O12 C5 C6 107.8(2) . . ?
O12 C5 H5A 110.1 . . ?
C6 C5 H5A 110.1 . . ?
O12 C5 H5B 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.5 . . ?
O13 C6 C5 110.6(2) . . ?
O13 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
O13 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
O13 C7 C8 106.0(2) . . ?
O13 C7 H7A 110.5 . . ?
C8 C7 H7A 110.5 . . ?
O13 C7 H7B 110.5 . . ?
C8 C7 H7B 110.5 . . ?
H7A C7 H7B 108.7 . . ?
O10 C8 C7 109.0(2) . . ?
O10 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
O10 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O3 N1 O2 122.1(2) . . ?
O3 N1 O1 121.9(2) . . ?
O2 N1 O1 116.0(2) . . ?
O3 N1 Tb1 178.5(2) . . ?
O2 N1 Tb1 59.34(13) . . ?
O1 N1 Tb1 56.66(13) . . ?
O6 N2 O4 122.6(2) . . ?
O6 N2 O5 121.7(2) . . ?
O4 N2 O5 115.7(2) . . ?
O6 N2 Tb1 177.7(2) . . ?
O4 N2 Tb1 59.48(13) . . ?
O5 N2 Tb1 56.19(13) . . ?
O9 N3 O8 121.9(2) . . ?
O9 N3 O7 122.0(2) . . ?
O8 N3 O7 116.1(2) . . ?
O9 N3 Tb1 178.03(19) . . ?
O8 N3 Tb1 57.53(13) . . ?
O7 N3 Tb1 58.59(13) . . ?
N1 O1 Tb1 97.23(15) . . ?
N1 O2 Tb1 94.67(15) . . ?
N2 O4 Tb1 94.37(15) . . ?
N2 O5 Tb1 97.60(15) . . ?
N3 O7 Tb1 95.28(15) . . ?
N3 O8 Tb1 96.45(15) . . ?
C1 O10 C8 113.2(2) . . ?
C1 O10 Tb1 120.44(16) . . ?
C8 O10 Tb1 115.32(15) . . ?
C3 O11 C2 116.8(2) . . ?
C3 O11 Tb1 116.90(15) . . ?
C2 O11 Tb1 114.52(15) . . ?
C4 O12 C5 113.1(2) . . ?
C4 O12 Tb1 121.04(15) . . ?
C5 O12 Tb1 119.18(16) . . ?
C6 O13 C7 115.1(2) . . ?
C6 O13 Tb1 107.15(16) . . ?
C7 O13 Tb1 118.67(15) . . ?
O5 Tb1 O1 76.63(7) . . ?
O5 Tb1 O10 82.97(7) . . ?
O1 Tb1 O10 71.79(6) . . ?
O5 Tb1 O8 82.61(7) . . ?
O1 Tb1 O8 143.76(7) . . ?
O10 Tb1 O8 134.79(6) . . ?
O5 Tb1 O11 71.06(6) . . ?
O1 Tb1 O11 129.02(6) . . ?
O10 Tb1 O11 66.09(6) . . ?
O8 Tb1 O11 68.70(6) . . ?
O5 Tb1 O7 121.98(7) . . ?
O1 Tb1 O7 117.46(6) . . ?
O10 Tb1 O7 154.18(7) . . ?
O8 Tb1 O7 52.14(6) . . ?
O11 Tb1 O7 112.98(6) . . ?
O5 Tb1 O2 112.01(6) . . ?
O1 Tb1 O2 52.10(6) . . ?
O10 Tb1 O2 112.89(6) . . ?
O8 Tb1 O2 112.26(7) . . ?
O11 Tb1 O2 176.78(6) . . ?
O7 Tb1 O2 66.48(6) . . ?
O5 Tb1 O4 52.37(7) . . ?
O1 Tb1 O4 72.43(7) . . ?
O10 Tb1 O4 127.71(7) . . ?
O8 Tb1 O4 71.36(7) . . ?
O11 Tb1 O4 113.12(6) . . ?
O7 Tb1 O4 77.40(7) . . ?
O2 Tb1 O4 69.99(7) . . ?
O5 Tb1 O13 143.15(7) . . ?
O1 Tb1 O13 75.74(7) . . ?
O10 Tb1 O13 65.50(6) . . ?
O8 Tb1 O13 133.14(6) . . ?
O11 Tb1 O13 109.57(6) . . ?
O7 Tb1 O13 92.46(7) . . ?
O2 Tb1 O13 67.45(6) . . ?
O4 Tb1 O13 136.74(6) . . ?
O5 Tb1 O12 135.00(6) . . ?
O1 Tb1 O12 139.12(7) . . ?
O10 Tb1 O12 85.63(6) . . ?
O8 Tb1 O12 75.22(7) . . ?
O11 Tb1 O12 64.53(6) . . ?
O7 Tb1 O12 72.01(6) . . ?
O2 Tb1 O12 112.54(6) . . ?
O4 Tb1 O12 144.15(7) . . ?
O13 Tb1 O12 63.84(6) . . ?
O5 Tb1 N1 94.55(7) . . ?
O1 Tb1 N1 26.11(6) . . ?
O10 Tb1 N1 92.55(6) . . ?
O8 Tb1 N1 131.16(7) . . ?
O11 Tb1 N1 155.03(7) . . ?
O7 Tb1 N1 91.90(7) . . ?
O2 Tb1 N1 25.99(6) . . ?
O4 Tb1 N1 68.88(7) . . ?
O13 Tb1 N1 69.58(6) . . ?
O12 Tb1 N1 129.42(6) . . ?
O5 Tb1 N2 26.22(7) . . ?
O1 Tb1 N2 72.51(7) . . ?
O10 Tb1 N2 105.74(7) . . ?
O8 Tb1 N2 75.74(7) . . ?
O11 Tb1 N2 92.33(7) . . ?
O7 Tb1 N2 100.07(7) . . ?
O2 Tb1 N2 90.89(7) . . ?
O4 Tb1 N2 26.15(7) . . ?
O13 Tb1 N2 148.17(7) . . ?
O12 Tb1 N2 147.95(7) . . ?
N1 Tb1 N2 80.79(7) . . ?

_refine_diff_density_max         0.453
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.100

####################################################################### 
# 
# 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 1515258'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H16 Er N3 O13'
_chemical_formula_weight         529.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.0930(19)
_cell_length_b                   8.5348(14)
_cell_length_c                   15.134(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.562(2)
_cell_angle_gamma                90
_cell_volume                     1561.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3661
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      27.00

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_F_000             1028
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    5.452
_shelx_estimated_absorpt_T_min   0.476
_shelx_estimated_absorpt_T_max   0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4758
_exptl_absorpt_correction_T_max  0.5607
_exptl_absorpt_process_details   'SADABS (Bruker, 2011)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9043
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.685
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3524
_reflns_number_gt                3060
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0201P)²+0.6557P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3524
_refine_ls_number_parameters     226
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0513
_refine_ls_wR_factor_gt          0.0491
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
C1 C 0.2147(3) 0.0656(5) 0.8345(2) 0.0432(9) Uani 1 1 d . . . . .
H1A H 0.238012 0.156252 0.801143 0.052 Uiso 1 1 calc R U . . .
H1B H 0.170446 -0.001572 0.795804 0.052 Uiso 1 1 calc R U . . .
C2 C 0.3129(3) -0.0214(4) 0.8712(3) 0.0448(10) Uani 1 1 d . . . . .
H2A H 0.289238 -0.120360 0.895947 0.054 Uiso 1 1 calc R U . . .
H2B H 0.363637 -0.043528 0.824296 0.054 Uiso 1 1 calc R U . . .
C3 C 0.4609(3) 0.1647(4) 0.9129(3) 0.0422(9) Uani 1 1 d . . . . .
H3A H 0.494637 0.117226 0.862049 0.051 Uiso 1 1 calc R U . . .
H3B H 0.515888 0.168197 0.960742 0.051 Uiso 1 1 calc R U . . .
C4 C 0.4245(4) 0.3280(4) 0.8902(3) 0.0474(10) Uani 1 1 d . . . . .
H4A H 0.488175 0.396933 0.887835 0.057 Uiso 1 1 calc R U . . .
H4B H 0.386578 0.329318 0.832915 0.057 Uiso 1 1 calc R U . . .
C5 C 0.3042(3) 0.5323(4) 0.9402(3) 0.0470(10) Uani 1 1 d . . . . .
H5A H 0.290992 0.545892 0.877174 0.056 Uiso 1 1 calc R U . . .
H5B H 0.354823 0.613436 0.960804 0.056 Uiso 1 1 calc R U . . .
C6 C 0.1972(3) 0.5437(4) 0.9879(3) 0.0467(10) Uani 1 1 d . . . . .
H6A H 0.212528 0.563163 1.050170 0.056 Uiso 1 1 calc R U . . .
H6B H 0.154215 0.630877 0.964414 0.056 Uiso 1 1 calc R U . . .
C7 C 0.0859(3) 0.3760(5) 0.8907(3) 0.0447(9) Uani 1 1 d . . . . .
H7A H 0.138492 0.402043 0.845705 0.054 Uiso 1 1 calc R U . . .
H7B H 0.020637 0.440907 0.881926 0.054 Uiso 1 1 calc R U . . .
C8 C 0.0557(3) 0.2058(4) 0.8858(3) 0.0429(9) Uani 1 1 d . . . . .
H8A H -0.003791 0.183748 0.925628 0.051 Uiso 1 1 calc R U . . .
H8B H 0.030582 0.179422 0.826182 0.051 Uiso 1 1 calc R U . . .
N1 N 0.0410(3) 0.2258(4) 1.1350(2) 0.0415(8) Uani 1 1 d . . . . .
N2 N 0.2485(3) -0.0911(4) 1.1517(2) 0.0461(8) Uani 1 1 d . . . . .
N3 N 0.4291(3) 0.2902(4) 1.1531(2) 0.0393(7) Uani 1 1 d . U . . .
O1 O 0.0575(2) 0.1201(3) 1.07791(17) 0.0454(7) Uani 1 1 d . . . . .
O2 O 0.1210(2) 0.3167(3) 1.15192(18) 0.0438(6) Uani 1 1 d . . . . .
O3 O -0.0474(2) 0.2401(4) 1.1720(2) 0.0612(8) Uani 1 1 d . . . . .
O4 O 0.2451(2) 0.0418(3) 1.18849(17) 0.0496(7) Uani 1 1 d . . . . .
O5 O 0.2501(2) -0.0900(3) 1.06752(17) 0.0470(7) Uani 1 1 d . . . . .
O6 O 0.2481(3) -0.2121(3) 1.1934(2) 0.0771(11) Uani 1 1 d . . . . .
O7 O 0.3395(2) 0.3673(3) 1.14889(17) 0.0425(6) Uani 1 1 d . . . . .
O8 O 0.4328(2) 0.1679(3) 1.10541(17) 0.0432(6) Uani 1 1 d . U . . .
O9 O 0.5077(2) 0.3306(3) 1.20019(19) 0.0547(8) Uani 1 1 d . . . . .
O10 O 0.1517(2) 0.1137(3) 0.91012(15) 0.0370(6) Uani 1 1 d . . . . .
O11 O 0.3683(2) 0.0710(3) 0.93915(15) 0.0352(6) Uani 1 1 d . . . . .
O12 O 0.3510(2) 0.3799(3) 0.95786(17) 0.0403(6) Uani 1 1 d . . . . .
O13 O 0.1343(2) 0.4006(3) 0.97776(16) 0.0400(6) Uani 1 1 d . . . . .
Er1 Er 0.24474(2) 0.18587(2) 1.04742(2) 0.03131(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O10 1.451(4) . ?
C1 C2 1.494(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O11 1.446(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O11 1.441(4) . ?
C3 C4 1.498(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O12 1.444(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O12 1.440(4) . ?
C5 C6 1.502(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 O13 1.445(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O13 1.443(4) . ?
C7 C8 1.499(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O10 1.442(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
N1 O3 1.226(4) . ?
N1 O2 1.261(4) . ?
N1 O1 1.269(4) . ?
N1 Er1 2.851(3) . ?
N2 O6 1.210(4) . ?
N2 O4 1.264(4) . ?
N2 O5 1.275(4) . ?
N2 Er1 2.843(3) . ?
N3 O9 1.223(4) . ?
N3 O7 1.268(4) . ?
N3 O8 1.270(4) . ?
N3 Er1 2.851(3) . ?
O1 Er1 2.390(3) . ?
O2 Er1 2.473(2) . ?
O4 Er1 2.464(3) . ?
O5 Er1 2.375(3) . ?
O7 Er1 2.444(3) . ?
O8 Er1 2.420(3) . ?
O10 Er1 2.415(2) . ?
O11 Er1 2.452(2) . ?
O12 Er1 2.515(2) . ?
O13 Er1 2.485(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 C1 C2 106.0(3) . . ?
O10 C1 H1A 110.5 . . ?
C2 C1 H1A 110.5 . . ?
O10 C1 H1B 110.5 . . ?
C2 C1 H1B 110.5 . . ?
H1A C1 H1B 108.7 . . ?
O11 C2 C1 110.0(3) . . ?
O11 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
O11 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
O11 C3 C4 110.8(3) . . ?
O11 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
O11 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
O12 C4 C3 107.8(3) . . ?
O12 C4 H4A 110.2 . . ?
C3 C4 H4A 110.2 . . ?
O12 C4 H4B 110.2 . . ?
C3 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
O12 C5 C6 108.0(3) . . ?
O12 C5 H5A 110.1 . . ?
C6 C5 H5A 110.1 . . ?
O12 C5 H5B 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
O13 C6 C5 110.7(3) . . ?
O13 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
O13 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
O13 C7 C8 106.2(3) . . ?
O13 C7 H7A 110.5 . . ?
C8 C7 H7A 110.5 . . ?
O13 C7 H7B 110.5 . . ?
C8 C7 H7B 110.5 . . ?
H7A C7 H7B 108.7 . . ?
O10 C8 C7 108.8(3) . . ?
O10 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
O10 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O3 N1 O2 121.3(3) . . ?
O3 N1 O1 122.5(3) . . ?
O2 N1 O1 116.2(3) . . ?
O3 N1 Er1 178.7(3) . . ?
O2 N1 Er1 59.96(17) . . ?
O1 N1 Er1 56.22(17) . . ?
O6 N2 O4 122.4(3) . . ?
O6 N2 O5 121.9(4) . . ?
O4 N2 O5 115.8(3) . . ?
O6 N2 Er1 177.4(3) . . ?
O4 N2 Er1 59.87(17) . . ?
O5 N2 Er1 55.89(17) . . ?
O9 N3 O7 122.2(3) . . ?
O9 N3 O8 121.6(3) . . ?
O7 N3 O8 116.2(3) . . ?
O9 N3 Er1 177.8(2) . . ?
O7 N3 Er1 58.64(18) . . ?
O8 N3 Er1 57.59(18) . . ?
N1 O1 Er1 97.6(2) . . ?
N1 O2 Er1 93.8(2) . . ?
N2 O4 Er1 93.8(2) . . ?
N2 O5 Er1 97.7(2) . . ?
N3 O7 Er1 95.1(2) . . ?
N3 O8 Er1 96.1(2) . . ?
C8 O10 C1 112.9(3) . . ?
C8 O10 Er1 115.7(2) . . ?
C1 O10 Er1 120.6(2) . . ?
C3 O11 C2 117.1(3) . . ?
C3 O11 Er1 117.0(2) . . ?
C2 O11 Er1 114.5(2) . . ?
C5 O12 C4 113.1(3) . . ?
C5 O12 Er1 119.4(2) . . ?
C4 O12 Er1 120.9(2) . . ?
C7 O13 C6 114.8(3) . . ?
C7 O13 Er1 118.7(2) . . ?
C6 O13 Er1 107.6(2) . . ?
O5 Er1 O1 76.42(9) . . ?
O5 Er1 O10 82.41(9) . . ?
O1 Er1 O10 71.63(9) . . ?
O5 Er1 O8 82.46(9) . . ?
O1 Er1 O8 143.23(9) . . ?
O10 Er1 O8 134.97(8) . . ?
O5 Er1 O7 122.48(9) . . ?
O1 Er1 O7 117.25(8) . . ?
O10 Er1 O7 154.34(9) . . ?
O8 Er1 O7 52.58(9) . . ?
O5 Er1 O11 70.99(8) . . ?
O1 Er1 O11 129.27(9) . . ?
O10 Er1 O11 66.50(8) . . ?
O8 Er1 O11 68.49(8) . . ?
O7 Er1 O11 112.92(8) . . ?
O5 Er1 O4 52.75(9) . . ?
O1 Er1 O4 72.24(9) . . ?
O10 Er1 O4 127.45(9) . . ?
O8 Er1 O4 71.01(9) . . ?
O7 Er1 O4 77.40(9) . . ?
O11 Er1 O4 113.13(9) . . ?
O5 Er1 O2 112.36(9) . . ?
O1 Er1 O2 52.37(9) . . ?
O10 Er1 O2 112.92(9) . . ?
O8 Er1 O2 112.07(9) . . ?
O7 Er1 O2 66.03(9) . . ?
O11 Er1 O2 176.60(8) . . ?
O4 Er1 O2 70.00(9) . . ?
O5 Er1 O13 142.92(9) . . ?
O1 Er1 O13 75.75(9) . . ?
O10 Er1 O13 65.84(8) . . ?
O8 Er1 O13 133.58(8) . . ?
O7 Er1 O13 92.11(9) . . ?
O11 Er1 O13 109.97(8) . . ?
O4 Er1 O13 136.38(9) . . ?
O2 Er1 O13 67.10(9) . . ?
O5 Er1 O12 135.19(8) . . ?
O1 Er1 O12 139.39(9) . . ?
O10 Er1 O12 86.39(8) . . ?
O8 Er1 O12 75.42(9) . . ?
O7 Er1 O12 71.57(9) . . ?
O11 Er1 O12 64.76(8) . . ?
O4 Er1 O12 143.78(9) . . ?
O2 Er1 O12 111.98(8) . . ?
O13 Er1 O12 64.05(8) . . ?
O5 Er1 N2 26.40(9) . . ?
O1 Er1 N2 72.46(9) . . ?
O10 Er1 N2 105.43(10) . . ?
O8 Er1 N2 75.23(9) . . ?
O7 Er1 N2 100.23(10) . . ?
O11 Er1 N2 92.16(9) . . ?
O4 Er1 N2 26.35(9) . . ?
O2 Er1 N2 91.21(9) . . ?
O13 Er1 N2 148.13(9) . . ?
O12 Er1 N2 147.80(9) . . ?
O5 Er1 N1 94.58(9) . . ?
O1 Er1 N1 26.18(9) . . ?
O10 Er1 N1 92.43(9) . . ?
O8 Er1 N1 130.90(9) . . ?
O7 Er1 N1 91.63(9) . . ?
O11 Er1 N1 155.36(9) . . ?
O4 Er1 N1 68.77(9) . . ?
O2 Er1 N1 26.19(9) . . ?
O13 Er1 N1 69.37(9) . . ?
O12 Er1 N1 129.25(8) . . ?
N2 Er1 N1 80.92(9) . . ?

_refine_diff_density_max         0.374
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.104

####################################################################### 
# 
# 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 1515255'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H16 Dy N3 O13'
_chemical_formula_weight         524.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.0939(13)
_cell_length_b                   8.5411(9)
_cell_length_c                   15.1800(17)
_cell_angle_alpha                90
_cell_angle_beta                 91.6790(10)
_cell_angle_gamma                90
_cell_volume                     1567.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4258
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      27.40

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.224
_exptl_crystal_F_000             1020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    4.845
_shelx_estimated_absorpt_T_min   0.476
_shelx_estimated_absorpt_T_max   0.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4759
_exptl_absorpt_correction_T_max  0.5302
_exptl_absorpt_process_details   'SADABS (Bruker, 2011)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8770
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.737
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3391
_reflns_number_gt                3030
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0401P)²+0.8342P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3391
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0607
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_restrained_S_all      0.938
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
C1 C 0.2148(3) 0.0674(5) 0.8343(2) 0.0418(9) Uani 1 1 d . . . . .
H1A H 0.238189 0.158630 0.801606 0.050 Uiso 1 1 calc R U . . .
H1B H 0.170902 0.000809 0.795115 0.050 Uiso 1 1 calc R U . . .
C2 C 0.3131(3) -0.0199(5) 0.8709(2) 0.0418(9) Uani 1 1 d . . . . .
H2A H 0.289400 -0.118916 0.895276 0.050 Uiso 1 1 calc R U . . .
H2B H 0.363800 -0.041696 0.824117 0.050 Uiso 1 1 calc R U . . .
C3 C 0.4605(3) 0.1647(4) 0.9128(3) 0.0392(9) Uani 1 1 d . . . . .
H3A H 0.493995 0.117272 0.862051 0.047 Uiso 1 1 calc R U . . .
H3B H 0.515683 0.167637 0.960490 0.047 Uiso 1 1 calc R U . . .
C4 C 0.4250(4) 0.3285(5) 0.8903(3) 0.0473(10) Uani 1 1 d . . . . .
H4A H 0.488974 0.396802 0.888336 0.057 Uiso 1 1 calc R U . . .
H4B H 0.387186 0.330511 0.833110 0.057 Uiso 1 1 calc R U . . .
C5 C 0.3037(3) 0.5324(5) 0.9395(3) 0.0462(10) Uani 1 1 d . . . . .
H5A H 0.290044 0.544855 0.876585 0.055 Uiso 1 1 calc R U . . .
H5B H 0.354038 0.614344 0.959479 0.055 Uiso 1 1 calc R U . . .
C6 C 0.1971(3) 0.5433(4) 0.9872(3) 0.0445(9) Uani 1 1 d . . . . .
H6A H 0.212780 0.562387 1.049342 0.053 Uiso 1 1 calc R U . . .
H6B H 0.153968 0.630654 0.964140 0.053 Uiso 1 1 calc R U . . .
C7 C 0.0855(3) 0.3754(5) 0.8899(3) 0.0446(9) Uani 1 1 d . . . . .
H7A H 0.138161 0.400712 0.845075 0.053 Uiso 1 1 calc R U . . .
H7B H 0.020324 0.440181 0.880745 0.053 Uiso 1 1 calc R U . . .
C8 C 0.0553(3) 0.2061(5) 0.8854(3) 0.0421(9) Uani 1 1 d . . . . .
H8A H -0.003768 0.184358 0.925536 0.050 Uiso 1 1 calc R U . . .
H8B H 0.029423 0.179586 0.826170 0.050 Uiso 1 1 calc R U . . .
N1 N 0.0397(3) 0.2259(4) 1.1355(2) 0.0424(8) Uani 1 1 d . . . . .
N2 N 0.2480(3) -0.0946(4) 1.1525(2) 0.0483(8) Uani 1 1 d . . . . .
N3 N 0.4309(3) 0.2901(4) 1.1537(2) 0.0385(7) Uani 1 1 d . . . . .
O1 O 0.0556(2) 0.1202(3) 1.07839(18) 0.0450(6) Uani 1 1 d . . . . .
O2 O 0.1204(2) 0.3151(3) 1.15263(19) 0.0437(7) Uani 1 1 d . . . . .
O3 O -0.0484(2) 0.2408(5) 1.1719(2) 0.0637(9) Uani 1 1 d . . . . .
O4 O 0.2453(2) 0.0380(4) 1.18912(18) 0.0503(7) Uani 1 1 d . . . . .
O5 O 0.2501(2) -0.0926(3) 1.06813(18) 0.0459(7) Uani 1 1 d . . . . .
O6 O 0.2478(3) -0.2154(4) 1.1935(2) 0.0754(11) Uani 1 1 d . . . . .
O7 O 0.3411(2) 0.3665(3) 1.15097(18) 0.0425(6) Uani 1 1 d . . . . .
O8 O 0.4347(2) 0.1683(3) 1.10628(18) 0.0434(6) Uani 1 1 d . . . . .
O9 O 0.5089(2) 0.3309(4) 1.2013(2) 0.0554(8) Uani 1 1 d . . . . .
O10 O 0.1514(2) 0.1141(3) 0.90924(15) 0.0366(6) Uani 1 1 d . . . . .
O11 O 0.36849(19) 0.0717(3) 0.93876(15) 0.0352(5) Uani 1 1 d . . . . .
O12 O 0.3514(2) 0.3805(3) 0.95789(18) 0.0418(6) Uani 1 1 d . . . . .
O13 O 0.1342(2) 0.4016(3) 0.97722(17) 0.0397(6) Uani 1 1 d . . . . .
Dy1 Dy 0.24483(2) 0.18539(2) 1.04807(2) 0.03038(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O10 1.447(4) . ?
C1 C2 1.496(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O11 1.443(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O11 1.432(4) . ?
C3 C4 1.499(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O12 1.448(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O12 1.444(5) . ?
C5 C6 1.501(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 O13 1.435(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O13 1.452(4) . ?
C7 C8 1.492(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O10 1.441(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
N1 O3 1.222(4) . ?
N1 O2 1.260(4) . ?
N1 O1 1.270(4) . ?
N1 Dy1 2.869(3) . ?
N2 O6 1.205(4) . ?
N2 O4 1.263(4) . ?
N2 O5 1.282(4) . ?
N2 Dy1 2.869(3) . ?
N3 O9 1.222(4) . ?
N3 O8 1.267(4) . ?
N3 O7 1.267(4) . ?
N3 Dy1 2.868(3) . ?
O1 Dy1 2.412(3) . ?
O2 Dy1 2.480(3) . ?
O4 Dy1 2.484(3) . ?
O5 Dy1 2.395(3) . ?
O7 Dy1 2.466(3) . ?
O8 Dy1 2.441(3) . ?
O10 Dy1 2.439(2) . ?
O11 Dy1 2.465(2) . ?
O12 Dy1 2.533(3) . ?
O13 Dy1 2.505(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 C1 C2 106.2(3) . . ?
O10 C1 H1A 110.5 . . ?
C2 C1 H1A 110.5 . . ?
O10 C1 H1B 110.5 . . ?
C2 C1 H1B 110.5 . . ?
H1A C1 H1B 108.7 . . ?
O11 C2 C1 110.0(3) . . ?
O11 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
O11 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
O11 C3 C4 111.1(3) . . ?
O11 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
O11 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O12 C4 C3 107.6(3) . . ?
O12 C4 H4A 110.2 . . ?
C3 C4 H4A 110.2 . . ?
O12 C4 H4B 110.2 . . ?
C3 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
O12 C5 C6 107.8(3) . . ?
O12 C5 H5A 110.1 . . ?
C6 C5 H5A 110.1 . . ?
O12 C5 H5B 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.5 . . ?
O13 C6 C5 110.9(3) . . ?
O13 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
O13 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.0 . . ?
O13 C7 C8 106.5(3) . . ?
O13 C7 H7A 110.4 . . ?
C8 C7 H7A 110.4 . . ?
O13 C7 H7B 110.4 . . ?
C8 C7 H7B 110.4 . . ?
H7A C7 H7B 108.6 . . ?
O10 C8 C7 108.8(3) . . ?
O10 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
O10 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O3 N1 O2 121.6(4) . . ?
O3 N1 O1 122.4(4) . . ?
O2 N1 O1 116.0(3) . . ?
O3 N1 Dy1 178.8(3) . . ?
O2 N1 Dy1 59.53(18) . . ?
O1 N1 Dy1 56.48(17) . . ?
O6 N2 O4 122.7(4) . . ?
O6 N2 O5 121.9(4) . . ?
O4 N2 O5 115.5(3) . . ?
O6 N2 Dy1 177.4(3) . . ?
O4 N2 Dy1 59.70(18) . . ?
O5 N2 Dy1 55.76(18) . . ?
O9 N3 O8 122.0(3) . . ?
O9 N3 O7 121.3(3) . . ?
O8 N3 O7 116.7(3) . . ?
O9 N3 Dy1 177.4(3) . . ?
O8 N3 Dy1 57.78(17) . . ?
O7 N3 Dy1 58.93(17) . . ?
N1 O1 Dy1 97.5(2) . . ?
N1 O2 Dy1 94.5(2) . . ?
N2 O4 Dy1 94.3(2) . . ?
N2 O5 Dy1 98.0(2) . . ?
N3 O7 Dy1 95.0(2) . . ?
N3 O8 Dy1 96.2(2) . . ?
C8 O10 C1 113.3(3) . . ?
C8 O10 Dy1 115.5(2) . . ?
C1 O10 Dy1 120.4(2) . . ?
C3 O11 C2 116.9(3) . . ?
C3 O11 Dy1 117.3(2) . . ?
C2 O11 Dy1 114.6(2) . . ?
C5 O12 C4 112.9(3) . . ?
C5 O12 Dy1 119.3(2) . . ?
C4 O12 Dy1 121.0(2) . . ?
C6 O13 C7 115.2(3) . . ?
C6 O13 Dy1 107.6(2) . . ?
C7 O13 Dy1 118.4(2) . . ?
O5 Dy1 O1 76.62(10) . . ?
O5 Dy1 O10 82.65(9) . . ?
O1 Dy1 O10 71.89(9) . . ?
O5 Dy1 O8 82.74(9) . . ?
O1 Dy1 O8 143.60(10) . . ?
O10 Dy1 O8 134.84(9) . . ?
O5 Dy1 O11 71.38(9) . . ?
O1 Dy1 O11 129.42(9) . . ?
O10 Dy1 O11 66.11(8) . . ?
O8 Dy1 O11 68.73(9) . . ?
O5 Dy1 O7 122.09(10) . . ?
O1 Dy1 O7 117.18(9) . . ?
O10 Dy1 O7 154.43(9) . . ?
O8 Dy1 O7 52.14(9) . . ?
O11 Dy1 O7 112.89(8) . . ?
O5 Dy1 O2 112.08(9) . . ?
O1 Dy1 O2 51.99(9) . . ?
O10 Dy1 O2 112.96(9) . . ?
O8 Dy1 O2 112.15(9) . . ?
O11 Dy1 O2 176.43(9) . . ?
O7 Dy1 O2 66.33(9) . . ?
O5 Dy1 O4 52.29(10) . . ?
O1 Dy1 O4 72.34(10) . . ?
O10 Dy1 O4 127.41(9) . . ?
O8 Dy1 O4 71.30(10) . . ?
O11 Dy1 O4 113.23(9) . . ?
O7 Dy1 O4 77.46(10) . . ?
O2 Dy1 O4 70.17(10) . . ?
O5 Dy1 O13 142.90(9) . . ?
O1 Dy1 O13 75.78(9) . . ?
O10 Dy1 O13 65.48(9) . . ?
O8 Dy1 O13 133.20(9) . . ?
O11 Dy1 O13 109.17(8) . . ?
O7 Dy1 O13 92.63(9) . . ?
O2 Dy1 O13 67.60(9) . . ?
O4 Dy1 O13 137.02(9) . . ?
O5 Dy1 O12 135.16(9) . . ?
O1 Dy1 O12 139.07(9) . . ?
O10 Dy1 O12 85.84(9) . . ?
O8 Dy1 O12 75.32(9) . . ?
O11 Dy1 O12 64.35(8) . . ?
O7 Dy1 O12 72.03(9) . . ?
O2 Dy1 O12 112.33(9) . . ?
O4 Dy1 O12 144.21(9) . . ?
O13 Dy1 O12 63.69(9) . . ?
O5 Dy1 N3 102.76(10) . . ?
O1 Dy1 N3 134.31(9) . . ?
O10 Dy1 N3 153.77(8) . . ?
O8 Dy1 N3 26.05(9) . . ?
O11 Dy1 N3 91.01(9) . . ?
O7 Dy1 N3 26.10(9) . . ?
O2 Dy1 N3 89.07(9) . . ?
O4 Dy1 N3 72.21(9) . . ?
O13 Dy1 N3 114.25(9) . . ?
O12 Dy1 N3 72.15(9) . . ?
O5 Dy1 N2 26.26(10) . . ?
O1 Dy1 N2 72.52(10) . . ?
O10 Dy1 N2 105.52(10) . . ?
O8 Dy1 N2 75.70(9) . . ?
O11 Dy1 N2 92.58(9) . . ?
O7 Dy1 N2 100.05(10) . . ?
O2 Dy1 N2 90.99(10) . . ?
O4 Dy1 N2 26.03(10) . . ?
O13 Dy1 N2 148.24(9) . . ?
O12 Dy1 N2 148.03(9) . . ?
N3 Dy1 N2 87.35(10) . . ?

_refine_diff_density_max         0.324
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.108

####################################################################### 
# 
# 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 1515257'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H16 Ho N3 O13'
_chemical_formula_weight         527.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.9303(8)
_cell_length_b                   8.4868(5)
_cell_length_c                   15.0895(9)
_cell_angle_alpha                90
_cell_angle_beta                 91.7000(10)
_cell_angle_gamma                90
_cell_volume                     1527.14(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    5502
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      27.41

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_F_000             1024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    5.260
_shelx_estimated_absorpt_T_min   0.571
_shelx_estimated_absorpt_T_max   0.649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5709
_exptl_absorpt_correction_T_max  0.6489
_exptl_absorpt_process_details   'SADABS (Bruker, 2011)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8732
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.754
_diffrn_reflns_theta_max         27.410
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3417
_reflns_number_gt                3204
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0158P)²+1.2257P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3417
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0205
_refine_ls_wR_factor_ref         0.0437
_refine_ls_wR_factor_gt          0.0429
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C1 C 0.0362(2) 0.1652(3) 0.0868(2) 0.0209(6) Uani 1 1 d . . . . .
H1A H 0.001244 0.116711 0.138912 0.025 Uiso 1 1 calc R U . . .
H1B H -0.020653 0.168261 0.037720 0.025 Uiso 1 1 calc R U . . .
C2 C 0.0728(3) 0.3306(3) 0.1095(2) 0.0244(6) Uani 1 1 d . . . . .
H2A H 0.006877 0.401214 0.111342 0.029 Uiso 1 1 calc R U . . .
H2B H 0.111829 0.332612 0.168317 0.029 Uiso 1 1 calc R U . . .
C3 C 0.1949(2) 0.5358(3) 0.0594(2) 0.0234(6) Uani 1 1 d . . . . .
H3A H 0.208798 0.549898 0.123865 0.028 Uiso 1 1 calc R U . . .
H3B H 0.142340 0.618877 0.038189 0.028 Uiso 1 1 calc R U . . .
C4 C 0.3038(2) 0.5467(3) 0.0110(2) 0.0227(6) Uani 1 1 d . . . . .
H4A H 0.287658 0.565091 -0.052891 0.027 Uiso 1 1 calc R U . . .
H4B H 0.348200 0.636948 0.034340 0.027 Uiso 1 1 calc R U . . .
C5 C 0.4158(2) 0.3796(4) 0.1107(2) 0.0231(6) Uani 1 1 d . . . . .
H5A H 0.360687 0.405669 0.156199 0.028 Uiso 1 1 calc R U . . .
H5B H 0.482879 0.446855 0.120247 0.028 Uiso 1 1 calc R U . . .
C6 C 0.4472(2) 0.2087(3) 0.1158(2) 0.0214(6) Uani 1 1 d . . . . .
H6A H 0.508327 0.186202 0.074696 0.026 Uiso 1 1 calc R U . . .
H6B H 0.473987 0.182130 0.176746 0.026 Uiso 1 1 calc R U . . .
C7 C 0.2850(2) 0.0694(4) 0.16757(18) 0.0220(6) Uani 1 1 d . . . . .
H7A H 0.260127 0.163534 0.200377 0.026 Uiso 1 1 calc R U . . .
H7B H 0.330695 0.002337 0.208375 0.026 Uiso 1 1 calc R U . . .
C8 C 0.1861(2) -0.0204(3) 0.13077(19) 0.0218(6) Uani 1 1 d . . . . .
H8A H 0.211319 -0.122420 0.106607 0.026 Uiso 1 1 calc R U . . .
H8B H 0.133204 -0.042099 0.178571 0.026 Uiso 1 1 calc R U . . .
Ho1 Ho 0.25577(2) 0.18624(2) -0.04718(2) 0.01561(5) Uani 1 1 d . . . . .
N1 N 0.2524(2) -0.0946(3) -0.15186(17) 0.0239(5) Uani 1 1 d . . . . .
N2 N 0.4634(2) 0.2246(3) -0.13418(16) 0.0206(5) Uani 1 1 d . . . . .
N3 N 0.06847(19) 0.2905(3) -0.15433(16) 0.0196(5) Uani 1 1 d . . . . .
O1 O 0.25030(16) -0.0929(2) -0.06655(13) 0.0231(4) Uani 1 1 d . . . . .
O2 O 0.25575(17) 0.0399(2) -0.18858(14) 0.0259(5) Uani 1 1 d . . . . .
O3 O 0.2525(2) -0.2168(3) -0.19358(16) 0.0377(6) Uani 1 1 d . . . . .
O4 O 0.44668(16) 0.1183(2) -0.07606(13) 0.0226(4) Uani 1 1 d . . . . .
O5 O 0.38141(16) 0.3155(2) -0.15184(14) 0.0224(4) Uani 1 1 d . . . . .
O6 O 0.55302(17) 0.2382(3) -0.17065(15) 0.0302(5) Uani 1 1 d . . . . .
O7 O 0.06490(16) 0.1674(2) -0.10601(13) 0.0221(4) Uani 1 1 d . . . . .
O8 O 0.15990(16) 0.3685(2) -0.15027(13) 0.0215(4) Uani 1 1 d . . . . .
O9 O -0.01078(17) 0.3313(3) -0.20205(14) 0.0281(5) Uani 1 1 d . . . . .
O10 O 0.13011(15) 0.0709(2) 0.06101(12) 0.0180(4) Uani 1 1 d . . . . .
O11 O 0.14776(16) 0.3819(2) 0.04158(13) 0.0206(4) Uani 1 1 d . . . . .
O12 O 0.36738(16) 0.4036(2) 0.02239(13) 0.0201(4) Uani 1 1 d . . . . .
O13 O 0.34926(15) 0.1153(2) 0.09194(12) 0.0186(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O10 1.440(3) . ?
C1 C2 1.506(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O11 1.447(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O11 1.443(3) . ?
C3 C4 1.511(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O12 1.440(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O12 1.451(3) . ?
C5 C6 1.499(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O13 1.449(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O13 1.447(3) . ?
C7 C8 1.497(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O10 1.454(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
Ho1 O1 2.387(2) . ?
Ho1 O4 2.4018(19) . ?
Ho1 O13 2.4237(18) . ?
Ho1 O7 2.4246(19) . ?
Ho1 O8 2.452(2) . ?
Ho1 O10 2.4528(18) . ?
Ho1 O5 2.467(2) . ?
Ho1 O2 2.469(2) . ?
Ho1 O12 2.4890(19) . ?
Ho1 O11 2.5130(19) . ?
Ho1 N2 2.856(2) . ?
Ho1 N1 2.859(2) . ?
N1 O3 1.213(3) . ?
N1 O2 1.271(3) . ?
N1 O1 1.288(3) . ?
N2 O6 1.222(3) . ?
N2 O5 1.267(3) . ?
N2 O4 1.278(3) . ?
N3 O9 1.221(3) . ?
N3 O7 1.276(3) . ?
N3 O8 1.276(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 C1 C2 110.9(2) . . ?
O10 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O10 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.0 . . ?
O11 C2 C1 107.5(2) . . ?
O11 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
O11 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O11 C3 C4 107.5(2) . . ?
O11 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
O11 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
O12 C4 C3 110.4(2) . . ?
O12 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
O12 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
O12 C5 C6 106.0(2) . . ?
O12 C5 H5A 110.5 . . ?
C6 C5 H5A 110.5 . . ?
O12 C5 H5B 110.5 . . ?
C6 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
O13 C6 C5 108.5(2) . . ?
O13 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
O13 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O13 C7 C8 105.9(2) . . ?
O13 C7 H7A 110.5 . . ?
C8 C7 H7A 110.5 . . ?
O13 C7 H7B 110.5 . . ?
C8 C7 H7B 110.5 . . ?
H7A C7 H7B 108.7 . . ?
O10 C8 C7 109.7(2) . . ?
O10 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
O10 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
O1 Ho1 O4 76.25(7) . . ?
O1 Ho1 O13 82.52(7) . . ?
O4 Ho1 O13 71.52(7) . . ?
O1 Ho1 O7 82.39(7) . . ?
O4 Ho1 O7 143.43(7) . . ?
O13 Ho1 O7 134.73(6) . . ?
O1 Ho1 O8 122.52(7) . . ?
O4 Ho1 O8 117.59(7) . . ?
O13 Ho1 O8 154.15(7) . . ?
O7 Ho1 O8 52.72(6) . . ?
O1 Ho1 O10 70.76(6) . . ?
O4 Ho1 O10 128.80(7) . . ?
O13 Ho1 O10 66.36(6) . . ?
O7 Ho1 O10 68.37(6) . . ?
O8 Ho1 O10 113.03(6) . . ?
O1 Ho1 O5 112.19(7) . . ?
O4 Ho1 O5 52.62(7) . . ?
O13 Ho1 O5 113.09(6) . . ?
O7 Ho1 O5 112.15(7) . . ?
O8 Ho1 O5 66.07(6) . . ?
O10 Ho1 O5 177.01(6) . . ?
O1 Ho1 O2 52.83(7) . . ?
O4 Ho1 O2 72.44(7) . . ?
O13 Ho1 O2 127.73(7) . . ?
O7 Ho1 O2 71.00(7) . . ?
O8 Ho1 O2 77.35(7) . . ?
O10 Ho1 O2 112.96(7) . . ?
O5 Ho1 O2 69.80(7) . . ?
O1 Ho1 O12 143.07(6) . . ?
O4 Ho1 O12 75.88(7) . . ?
O13 Ho1 O12 65.92(6) . . ?
O7 Ho1 O12 133.49(6) . . ?
O8 Ho1 O12 91.93(7) . . ?
O10 Ho1 O12 110.18(6) . . ?
O5 Ho1 O12 67.23(7) . . ?
O2 Ho1 O12 136.36(7) . . ?
O1 Ho1 O11 135.10(6) . . ?
O4 Ho1 O11 139.40(7) . . ?
O13 Ho1 O11 86.13(6) . . ?
O7 Ho1 O11 75.40(7) . . ?
O8 Ho1 O11 71.60(7) . . ?
O10 Ho1 O11 64.90(6) . . ?
O5 Ho1 O11 112.24(7) . . ?
O2 Ho1 O11 143.73(7) . . ?
O12 Ho1 O11 64.01(6) . . ?
O1 Ho1 N2 94.47(7) . . ?
O4 Ho1 N2 26.36(7) . . ?
O13 Ho1 N2 92.48(7) . . ?
O7 Ho1 N2 131.09(7) . . ?
O8 Ho1 N2 91.78(7) . . ?
O10 Ho1 N2 155.08(7) . . ?
O5 Ho1 N2 26.26(7) . . ?
O2 Ho1 N2 68.78(7) . . ?
O12 Ho1 N2 69.44(7) . . ?
O11 Ho1 N2 129.42(7) . . ?
O1 Ho1 N1 26.53(7) . . ?
O4 Ho1 N1 72.40(7) . . ?
O13 Ho1 N1 105.67(7) . . ?
O7 Ho1 N1 75.23(7) . . ?
O8 Ho1 N1 100.19(7) . . ?
O10 Ho1 N1 92.07(7) . . ?
O5 Ho1 N1 90.90(7) . . ?
O2 Ho1 N1 26.30(7) . . ?
O12 Ho1 N1 148.15(7) . . ?
O11 Ho1 N1 147.83(6) . . ?
N2 Ho1 N1 80.76(7) . . ?
O3 N1 O2 122.8(3) . . ?
O3 N1 O1 121.9(3) . . ?
O2 N1 O1 115.3(2) . . ?
O3 N1 Ho1 177.6(2) . . ?
O2 N1 Ho1 59.43(13) . . ?
O1 N1 Ho1 55.85(13) . . ?
O6 N2 O5 121.9(2) . . ?
O6 N2 O4 122.1(2) . . ?
O5 N2 O4 116.0(2) . . ?
O6 N2 Ho1 178.7(2) . . ?
O5 N2 Ho1 59.44(13) . . ?
O4 N2 Ho1 56.56(12) . . ?
O9 N3 O7 122.1(2) . . ?
O9 N3 O8 121.8(2) . . ?
O7 N3 O8 116.1(2) . . ?
O9 N3 Ho1 177.91(19) . . ?
O7 N3 Ho1 57.46(12) . . ?
O8 N3 Ho1 58.72(13) . . ?
N1 O1 Ho1 97.63(16) . . ?
N1 O2 Ho1 94.27(15) . . ?
N2 O4 Ho1 97.08(15) . . ?
N2 O5 Ho1 94.30(15) . . ?
N3 O7 Ho1 96.21(15) . . ?
N3 O8 Ho1 94.88(15) . . ?
C1 O10 C8 116.4(2) . . ?
C1 O10 Ho1 117.01(16) . . ?
C8 O10 Ho1 114.69(15) . . ?
C3 O11 C2 112.7(2) . . ?
C3 O11 Ho1 119.59(16) . . ?
C2 O11 Ho1 121.05(16) . . ?
C4 O12 C5 115.0(2) . . ?
C4 O12 Ho1 107.54(15) . . ?
C5 O12 Ho1 118.47(16) . . ?
C7 O13 C6 113.2(2) . . ?
C7 O13 Ho1 120.61(15) . . ?
C6 O13 Ho1 115.27(16) . . ?

_refine_diff_density_max         0.648
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.095

