# 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_xb0465_0m
_database_code_depnum_ccdc_archive 'CCDC 1552858'
_audit_update_record             
;
2017-07-30 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H14 Dy N7 O9, C2 H6 O'
_chemical_formula_sum            'C14 H20 Dy N7 O10'
_chemical_formula_weight         608.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1890 4.4100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   7.653(2)
_cell_length_b                   10.785(3)
_cell_length_c                   13.375(4)
_cell_angle_alpha                90.525(5)
_cell_angle_beta                 92.108(4)
_cell_angle_gamma                104.345(5)
_cell_volume                     1068.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2099
_cell_measurement_theta_min      24.38
_cell_measurement_theta_max      2.45

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_F_000             598
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2353
_exptl_crystal_size_mid          0.1911
_exptl_crystal_size_min          0.1316
_exptl_absorpt_coefficient_mu    3.563
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5250
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
'SADABS 2015/2 (Bruker,2015) was used for absorption correction. R(int) was 0.0921 before and 0.0353 after correction. The Ratio of minimum to maximum transmission is 0.7043. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5693
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.949
_diffrn_reflns_theta_max         26.125
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             4096
_reflns_number_gt                3559
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_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)+(0.0734P)²] 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         4096
_refine_ls_number_parameters     292
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.1098
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_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
Dy1 Dy 0.70952(4) 0.19788(3) 0.18478(2) 0.03004(14) Uani 1 1 d . . . . .
O8 O 0.5194(6) 0.3031(5) 0.2677(4) 0.0378(11) Uani 1 1 d . . . . .
H8A H 0.3960 0.2527 0.2741 0.057 Uiso 1 1 d DR U . . .
H8B H 0.5644 0.3297 0.3199 0.057 Uiso 1 1 d R U . . .
O1 O 0.7219(7) 0.0651(5) 0.0287(4) 0.0396(12) Uani 1 1 d . . . . .
O9 O 0.4102(7) 0.0747(6) 0.1488(4) 0.0489(14) Uani 1 1 d . . . . .
H9A H 0.3966 0.0556 0.0865 0.073 Uiso 1 1 d R U . . .
H9B H 0.3358 0.1183 0.1643 0.073 Uiso 1 1 d R U . . .
O4 O 0.7675(9) -0.0066(6) 0.2314(5) 0.0564(16) Uani 1 1 d . . . . .
O5 O 0.6158(8) 0.0719(6) 0.3379(4) 0.0503(14) Uani 1 1 d . . . . .
O6 O 0.6595(12) -0.1187(7) 0.3611(6) 0.086(2) Uani 1 1 d . . . . .
O7 O 0.9418(6) 0.2735(5) 0.3030(4) 0.0374(11) Uani 1 1 d . . . . .
O2 O 0.9709(7) 0.1936(5) 0.0817(4) 0.0441(13) Uani 1 1 d . . . . .
O3 O 0.9568(9) 0.0982(6) -0.0639(4) 0.0591(16) Uani 1 1 d . . . . .
N6 N 0.6286(8) 0.3154(6) 0.0267(4) 0.0355(13) Uani 1 1 d . . . . .
N4 N 0.8651(7) 0.4195(6) 0.1683(4) 0.0325(13) Uani 1 1 d . . . . .
N3 N 0.9876(8) 0.4800(6) 0.2471(5) 0.0410(15) Uani 1 1 d . . . . .
N1 N 0.8861(8) 0.1184(6) 0.0136(5) 0.0370(14) Uani 1 1 d . . . . .
N2 N 0.6793(9) -0.0215(7) 0.3129(5) 0.0458(16) Uani 1 1 d . . . . .
N7 N 1.3397(8) 0.5464(7) 0.5737(5) 0.0424(15) Uani 1 1 d . . . . .
N5 N 0.9205(9) 0.6204(6) 0.1010(5) 0.0493(17) Uani 1 1 d . . . . .
H5A H 0.9957 0.6533 0.1492 0.059 Uiso 1 1 calc R U . . .
H5B H 0.8981 0.6679 0.0534 0.059 Uiso 1 1 calc R U . . .
C8 C 1.1382(9) 0.4467(7) 0.3985(5) 0.0349(16) Uani 1 1 d . . . . .
C7 C 0.6954(10) 0.5043(8) -0.0726(6) 0.0423(18) Uani 1 1 d . . . . .
H7 H 0.7571 0.5894 -0.0795 0.051 Uiso 1 1 calc R U . . .
C2 C 0.8398(9) 0.4976(7) 0.1002(5) 0.0352(16) Uani 1 1 d . . . . .
C3 C 0.7165(9) 0.4397(7) 0.0163(6) 0.0344(16) Uani 1 1 d . . . . .
C4 C 0.5187(11) 0.2582(8) -0.0491(6) 0.0448(19) Uani 1 1 d . . . . .
H4 H 0.4557 0.1736 -0.0409 0.054 Uiso 1 1 calc R U . . .
C9 C 1.1541(11) 0.3687(8) 0.4778(6) 0.0448(19) Uani 1 1 d . . . . .
H9 H 1.0993 0.2815 0.4738 0.054 Uiso 1 1 calc R U . . .
C10 C 1.2537(11) 0.4226(8) 0.5640(6) 0.0464(19) Uani 1 1 d . . . . .
H10 H 1.2605 0.3695 0.6176 0.056 Uiso 1 1 calc R U . . .
C12 C 1.2310(11) 0.5750(8) 0.4065(6) 0.0451(19) Uani 1 1 d . . . . .
H12 H 1.2252 0.6306 0.3544 0.054 Uiso 1 1 calc R U . . .
C6 C 0.5821(11) 0.4400(9) -0.1495(6) 0.049(2) Uani 1 1 d . . . . .
H6 H 0.5676 0.4817 -0.2086 0.059 Uiso 1 1 calc R U . . .
C5 C 0.4913(12) 0.3144(9) -0.1384(6) 0.051(2) Uani 1 1 d . . . . .
H5 H 0.4144 0.2692 -0.1890 0.061 Uiso 1 1 calc R U . . .
C1 C 1.0138(9) 0.3945(7) 0.3117(5) 0.0345(16) Uani 1 1 d . . . . .
C11 C 1.3304(12) 0.6174(9) 0.4922(7) 0.053(2) Uani 1 1 d . . . . .
H11 H 1.3973 0.7022 0.4946 0.064 Uiso 1 1 calc R U . . .
O10 O 0.2018(7) 0.1253(6) 0.2998(4) 0.0467(13) Uani 1 1 d . . . . .
H10A H 0.1109 0.1514 0.2896 0.070 Uiso 1 1 calc DR U . . .
C14 C 0.157(2) -0.0952(12) 0.3481(12) 0.112(6) Uani 1 1 d . . . . .
H14A H 0.0899 -0.1102 0.2851 0.169 Uiso 1 1 calc R U . . .
H14B H 0.0939 -0.1528 0.3967 0.169 Uiso 1 1 calc R U . . .
H14C H 0.2744 -0.1094 0.3404 0.169 Uiso 1 1 calc R U . . .
C13 C 0.1743(15) 0.0377(12) 0.3820(9) 0.078(3) Uani 1 1 d . . . . .
H13A H 0.0660 0.0430 0.4154 0.093 Uiso 1 1 calc R U . . .
H13B H 0.2755 0.0625 0.4299 0.093 Uiso 1 1 calc R U . . .


_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 O7 2.319(5) . ?
Dy1 O8 2.355(5) . ?
Dy1 O9 2.376(5) . ?
Dy1 N4 2.408(6) . ?
Dy1 O4 2.437(6) . ?
Dy1 O2 2.481(5) . ?
Dy1 O5 2.496(5) . ?
Dy1 O1 2.538(5) . ?
Dy1 N6 2.607(6) . ?
Dy1 N2 2.902(7) . ?
Dy1 N1 2.927(6) . ?
O8 H8A 0.9729 . ?
O8 H8B 0.7863 . ?
O1 N1 1.270(8) . ?
O9 H9A 0.8526 . ?
O9 H9B 0.8525 . ?
O4 N2 1.294(9) . ?
O5 N2 1.270(9) . ?
O6 N2 1.216(9) . ?
O7 C1 1.287(8) . ?
O2 N1 1.261(8) . ?
O3 N1 1.229(8) . ?
N6 C4 1.336(9) . ?
N6 C3 1.353(9) . ?
N4 C2 1.288(9) . ?
N4 N3 1.424(8) . ?
N3 C1 1.315(10) . ?
N7 C10 1.337(10) . ?
N7 C11 1.348(11) . ?
N5 C2 1.316(10) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
C8 C9 1.380(11) . ?
C8 C12 1.391(11) . ?
C8 C1 1.487(10) . ?
C7 C6 1.384(12) . ?
C7 C3 1.408(10) . ?
C7 H7 0.9300 . ?
C2 C3 1.468(11) . ?
C4 C5 1.377(11) . ?
C4 H4 0.9300 . ?
C9 C10 1.398(11) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C12 C11 1.363(11) . ?
C12 H12 0.9300 . ?
C6 C5 1.372(12) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
C11 H11 0.9300 . ?
O10 C13 1.443(11) . ?
O10 H10A 0.8200 . ?
C14 C13 1.472(17) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?

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
O7 Dy1 O8 91.31(17) . . ?
O7 Dy1 O9 148.17(19) . . ?
O8 Dy1 O9 73.97(18) . . ?
O7 Dy1 N4 65.27(18) . . ?
O8 Dy1 N4 78.00(18) . . ?
O9 Dy1 N4 134.9(2) . . ?
O7 Dy1 O4 81.7(2) . . ?
O8 Dy1 O4 125.64(18) . . ?
O9 Dy1 O4 84.4(2) . . ?
N4 Dy1 O4 140.6(2) . . ?
O7 Dy1 O2 80.61(18) . . ?
O8 Dy1 O2 153.14(19) . . ?
O9 Dy1 O2 124.35(18) . . ?
N4 Dy1 O2 75.35(18) . . ?
O4 Dy1 O2 78.77(19) . . ?
O7 Dy1 O5 74.86(18) . . ?
O8 Dy1 O5 74.03(18) . . ?
O9 Dy1 O5 74.0(2) . . ?
N4 Dy1 O5 130.1(2) . . ?
O4 Dy1 O5 52.0(2) . . ?
O2 Dy1 O5 127.09(19) . . ?
O7 Dy1 O1 126.76(17) . . ?
O8 Dy1 O1 141.81(17) . . ?
O9 Dy1 O1 73.61(18) . . ?
N4 Dy1 O1 112.60(18) . . ?
O4 Dy1 O1 70.09(19) . . ?
O2 Dy1 O1 50.76(17) . . ?
O5 Dy1 O1 115.04(19) . . ?
O7 Dy1 N6 127.39(18) . . ?
O8 Dy1 N6 84.90(18) . . ?
O9 Dy1 N6 80.16(19) . . ?
N4 Dy1 N6 62.63(19) . . ?
O4 Dy1 N6 140.0(2) . . ?
O2 Dy1 N6 80.02(19) . . ?
O5 Dy1 N6 150.21(19) . . ?
O1 Dy1 N6 70.16(18) . . ?
O7 Dy1 N2 78.16(18) . . ?
O8 Dy1 N2 99.50(19) . . ?
O9 Dy1 N2 76.7(2) . . ?
N4 Dy1 N2 143.2(2) . . ?
O4 Dy1 N2 26.24(19) . . ?
O2 Dy1 N2 103.8(2) . . ?
O5 Dy1 N2 25.84(19) . . ?
O1 Dy1 N2 92.20(19) . . ?
N6 Dy1 N2 154.20(19) . . ?
O7 Dy1 N1 104.62(18) . . ?
O8 Dy1 N1 156.27(17) . . ?
O9 Dy1 N1 99.10(18) . . ?
N4 Dy1 N1 92.62(18) . . ?
O4 Dy1 N1 74.88(18) . . ?
O2 Dy1 N1 25.29(17) . . ?
O5 Dy1 N1 126.70(19) . . ?
O1 Dy1 N1 25.63(16) . . ?
N6 Dy1 N1 71.48(18) . . ?
N2 Dy1 N1 100.89(19) . . ?
Dy1 O8 H8A 115.1 . . ?
Dy1 O8 H8B 109.5 . . ?
H8A O8 H8B 111.6 . . ?
N1 O1 Dy1 94.5(4) . . ?
Dy1 O9 H9A 109.5 . . ?
Dy1 O9 H9B 109.4 . . ?
H9A O9 H9B 109.3 . . ?
N2 O4 Dy1 97.4(5) . . ?
N2 O5 Dy1 95.2(4) . . ?
C1 O7 Dy1 119.8(4) . . ?
N1 O2 Dy1 97.6(4) . . ?
C4 N6 C3 117.6(6) . . ?
C4 N6 Dy1 124.3(5) . . ?
C3 N6 Dy1 117.8(4) . . ?
C2 N4 N3 113.2(6) . . ?
C2 N4 Dy1 128.0(5) . . ?
N3 N4 Dy1 118.5(4) . . ?
C1 N3 N4 110.2(6) . . ?
O3 N1 O2 122.3(6) . . ?
O3 N1 O1 121.3(6) . . ?
O2 N1 O1 116.4(6) . . ?
O3 N1 Dy1 172.1(5) . . ?
O2 N1 Dy1 57.1(3) . . ?
O1 N1 Dy1 59.8(3) . . ?
O6 N2 O5 123.2(7) . . ?
O6 N2 O4 121.7(8) . . ?
O5 N2 O4 115.1(6) . . ?
O6 N2 Dy1 175.4(6) . . ?
O5 N2 Dy1 58.9(4) . . ?
O4 N2 Dy1 56.4(4) . . ?
C10 N7 C11 115.4(7) . . ?
C2 N5 H5A 120.0 . . ?
C2 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C9 C8 C12 117.9(7) . . ?
C9 C8 C1 119.7(7) . . ?
C12 C8 C1 122.3(7) . . ?
C6 C7 C3 119.4(8) . . ?
C6 C7 H7 120.3 . . ?
C3 C7 H7 120.3 . . ?
N4 C2 N5 124.2(7) . . ?
N4 C2 C3 115.3(7) . . ?
N5 C2 C3 120.4(7) . . ?
N6 C3 C7 120.7(7) . . ?
N6 C3 C2 115.7(6) . . ?
C7 C3 C2 123.5(7) . . ?
N6 C4 C5 125.3(8) . . ?
N6 C4 H4 117.4 . . ?
C5 C4 H4 117.4 . . ?
C8 C9 C10 119.1(8) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N7 C10 C9 123.6(8) . . ?
N7 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
C11 C12 C8 118.6(8) . . ?
C11 C12 H12 120.7 . . ?
C8 C12 H12 120.7 . . ?
C5 C6 C7 119.8(7) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C5 C4 117.2(8) . . ?
C6 C5 H5 121.4 . . ?
C4 C5 H5 121.4 . . ?
O7 C1 N3 124.5(7) . . ?
O7 C1 C8 120.3(7) . . ?
N3 C1 C8 115.2(6) . . ?
N7 C11 C12 125.2(8) . . ?
N7 C11 H11 117.4 . . ?
C12 C11 H11 117.4 . . ?
C13 O10 H10A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O10 C13 C14 111.9(10) . . ?
O10 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
O10 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N4 N3 C1 -177.2(6) . . . . ?
Dy1 N4 N3 C1 9.2(7) . . . . ?
Dy1 O2 N1 O3 170.7(6) . . . . ?
Dy1 O2 N1 O1 -8.6(6) . . . . ?
Dy1 O1 N1 O3 -171.0(6) . . . . ?
Dy1 O1 N1 O2 8.4(6) . . . . ?
Dy1 O5 N2 O6 -175.1(8) . . . . ?
Dy1 O5 N2 O4 4.7(7) . . . . ?
Dy1 O4 N2 O6 175.0(7) . . . . ?
Dy1 O4 N2 O5 -4.8(7) . . . . ?
N3 N4 C2 N5 1.4(10) . . . . ?
Dy1 N4 C2 N5 174.2(5) . . . . ?
N3 N4 C2 C3 179.1(5) . . . . ?
Dy1 N4 C2 C3 -8.1(9) . . . . ?
C4 N6 C3 C7 -1.7(10) . . . . ?
Dy1 N6 C3 C7 172.3(5) . . . . ?
C4 N6 C3 C2 -178.3(7) . . . . ?
Dy1 N6 C3 C2 -4.3(8) . . . . ?
C6 C7 C3 N6 0.7(11) . . . . ?
C6 C7 C3 C2 177.0(7) . . . . ?
N4 C2 C3 N6 7.6(9) . . . . ?
N5 C2 C3 N6 -174.6(7) . . . . ?
N4 C2 C3 C7 -168.9(7) . . . . ?
N5 C2 C3 C7 8.9(11) . . . . ?
C3 N6 C4 C5 1.9(12) . . . . ?
Dy1 N6 C4 C5 -171.6(6) . . . . ?
C12 C8 C9 C10 3.4(11) . . . . ?
C1 C8 C9 C10 -172.1(7) . . . . ?
C11 N7 C10 C9 -2.4(12) . . . . ?
C8 C9 C10 N7 -1.8(12) . . . . ?
C9 C8 C12 C11 -0.8(11) . . . . ?
C1 C8 C12 C11 174.5(7) . . . . ?
C3 C7 C6 C5 0.2(12) . . . . ?
C7 C6 C5 C4 0.0(12) . . . . ?
N6 C4 C5 C6 -1.1(13) . . . . ?
Dy1 O7 C1 N3 -12.1(9) . . . . ?
Dy1 O7 C1 C8 168.7(4) . . . . ?
N4 N3 C1 O7 1.5(10) . . . . ?
N4 N3 C1 C8 -179.3(5) . . . . ?
C9 C8 C1 O7 -10.3(10) . . . . ?
C12 C8 C1 O7 174.4(7) . . . . ?
C9 C8 C1 N3 170.4(7) . . . . ?
C12 C8 C1 N3 -4.9(10) . . . . ?
C10 N7 C11 C12 5.2(12) . . . . ?
C8 C12 C11 N7 -3.7(13) . . . . ?

_refine_diff_density_max         1.630
_refine_diff_density_min         -1.500
_refine_diff_density_rms         0.194

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_xb0043
_database_code_depnum_ccdc_archive 'CCDC 1552859'
_audit_update_record             
;
2017-07-30 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H22 Dy N7 O9, H2 O'
_chemical_formula_sum            'C16 H24 Dy N7 O10'
_chemical_formula_weight         636.92

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   10.892(4)
_cell_length_b                   24.650(9)
_cell_length_c                   9.988(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.966(7)
_cell_angle_gamma                90
_cell_volume                     2671.7(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1175
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      17.99

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             1260
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    2.854
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4775
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
'SADABS 2015/2 (Bruker, 2015) was used for absorption correction. R(int) was 0.1077 before and 0.0734 after correction. The Ratio of minimum to maximum transmission is 0.6405. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14073
_diffrn_reflns_av_unetI/netI     0.1912
_diffrn_reflns_av_R_equivalents  0.1345
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.207
_diffrn_reflns_theta_max         26.699
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             5461
_reflns_number_gt                2699
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0768P)²] 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         5461
_refine_ls_number_parameters     285
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1928
_refine_ls_R_factor_gt           0.0968
_refine_ls_wR_factor_ref         0.2276
_refine_ls_wR_factor_gt          0.1925
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.000
_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
Dy1 Dy 0.73190(7) 0.08863(3) 0.58616(7) 0.0375(3) Uani 1 1 d . . . . .
O1 O 0.8976(9) 0.0523(4) 0.7092(10) 0.040(3) Uani 1 1 d . . . . .
O2 O 0.8393(12) 0.1591(4) 0.4631(11) 0.055(3) Uani 1 1 d . . . . .
O3 O 0.8838(11) 0.0771(4) 0.4145(12) 0.060(3) Uani 1 1 d . . . . .
O4 O 0.9497(17) 0.1424(6) 0.3022(17) 0.117(6) Uani 1 1 d . . . . .
O5 O 0.5139(10) 0.0668(4) 0.4884(12) 0.053(3) Uani 1 1 d . . . . .
O6 O 0.6293(12) 0.1032(5) 0.3516(10) 0.060(3) Uani 1 1 d . . . . .
O7 O 0.4425(12) 0.0810(6) 0.2811(13) 0.079(4) Uani 1 1 d . . . . .
O8 O 0.6254(10) 0.0575(4) 0.7679(10) 0.048(3) Uani 1 1 d . . . . .
H8 H 0.6462 0.0192 0.7731 0.058 Uiso 1 1 d R U . . .
O9 O 0.7187(9) -0.0059(4) 0.5236(11) 0.046(3) Uani 1 1 d . . . . .
H9 H 0.6640 -0.0226 0.5833 0.055 Uiso 1 1 d R U . . .
N2 N 0.9244(13) 0.1275(5) 0.8411(13) 0.052(4) Uani 1 1 d . . . . .
N3 N 0.8239(12) 0.1462(5) 0.7609(13) 0.043(3) Uani 1 1 d . . . . .
N4 N 0.8496(16) 0.2247(5) 0.8920(15) 0.077(5) Uani 1 1 d D . . . .
H4A H 0.8560 0.2053 0.9674 0.116 Uiso 1 1 d R U . . .
H4B H 0.8068 0.2548 0.9046 0.116 Uiso 1 1 d R U . . .
N5 N 0.6244(9) 0.1817(3) 0.6179(10) 0.049(4) Uani 1 1 d G . . . .
C8 C 0.6861(8) 0.2171(4) 0.7087(10) 0.050(4) Uani 1 1 d DG . . . .
C9 C 0.6436(10) 0.2699(3) 0.7209(11) 0.059(5) Uani 1 1 d G . . . .
H9A H 0.6849 0.2936 0.7816 0.071 Uiso 1 1 calc R U . . .
C10 C 0.5395(11) 0.2872(3) 0.6423(12) 0.063(5) Uani 1 1 d G . . . .
H10 H 0.5110 0.3226 0.6505 0.076 Uiso 1 1 calc R U . . .
C11 C 0.4778(9) 0.2518(4) 0.5515(12) 0.071(6) Uani 1 1 d G . . . .
H11 H 0.4081 0.2634 0.4990 0.085 Uiso 1 1 calc R U . . .
C12 C 0.5203(9) 0.1990(4) 0.5393(10) 0.065(5) Uani 1 1 d G . . . .
H12 H 0.4790 0.1753 0.4786 0.077 Uiso 1 1 calc R U . . .
N6 N 0.8903(14) 0.1261(6) 0.3873(14) 0.052(4) Uani 1 1 d . . . . .
N7 N 0.5291(14) 0.0828(6) 0.3642(14) 0.050(4) Uani 1 1 d . . . . .
C5 C 1.2069(10) 0.0482(5) 1.0803(9) 0.066(6) Uani 1 1 d G . . . .
H5 H 1.2432 0.0643 1.1582 0.079 Uiso 1 1 calc R U . . .
N1 N 1.2445(9) -0.0030(5) 1.0424(10) 0.066(5) Uani 1 1 d G . . . .
C1 C 1.1903(10) -0.0270(4) 0.9260(11) 0.070(6) Uani 1 1 d G . . . .
H1 H 1.2154 -0.0612 0.9006 0.084 Uiso 1 1 calc R U . . .
C2 C 1.0984(10) 0.0003(4) 0.8474(9) 0.055(5) Uani 1 1 d G . . . .
H2 H 1.0622 -0.0157 0.7694 0.066 Uiso 1 1 calc R U . . .
C3 C 1.0608(9) 0.0515(4) 0.8853(10) 0.049(4) Uani 1 1 d DG . . . .
C4 C 1.1151(11) 0.0755(4) 1.0017(11) 0.060(5) Uani 1 1 d G . . . .
H4 H 1.0899 0.1098 1.0271 0.072 Uiso 1 1 calc R U . . .
C6 C 0.9560(11) 0.0789(6) 0.8044(14) 0.042(4) Uani 1 1 d D . . . .
C7 C 0.7931(12) 0.1936(6) 0.7928(14) 0.048(4) Uani 1 1 d D . . . .
C13 C 0.8265(15) -0.0425(6) 0.5231(17) 0.060(5) Uani 1 1 d D . . . .
H13A H 0.8924 -0.0240 0.4824 0.072 Uiso 1 1 calc R U . . .
H13B H 0.8558 -0.0514 0.6150 0.072 Uiso 1 1 calc R U . . .
C14 C 0.796(2) -0.0936(7) 0.448(3) 0.107(9) Uani 1 1 d D . . . .
H14A H 0.7204 -0.1083 0.4758 0.161 Uiso 1 1 calc R U . . .
H14B H 0.8611 -0.1194 0.4660 0.161 Uiso 1 1 calc R U . . .
H14C H 0.7858 -0.0860 0.3532 0.161 Uiso 1 1 calc R U . . .
C15 C 0.501(2) 0.0585(10) 0.797(2) 0.108(6) Uani 1 1 d D U . . .
H15A H 0.4771 0.0233 0.8298 0.130 Uiso 1 1 calc R U . . .
H15B H 0.4482 0.0667 0.7159 0.130 Uiso 1 1 calc R U . . .
C16 C 0.486(2) 0.1008(9) 0.901(2) 0.109(6) Uani 1 1 d D U . . .
H16A H 0.5083 0.1356 0.8665 0.163 Uiso 1 1 calc R U . . .
H16B H 0.5391 0.0925 0.9799 0.163 Uiso 1 1 calc R U . . .
H16C H 0.4021 0.1017 0.9223 0.163 Uiso 1 1 calc R U . . .
O11 O 1.065(5) 0.253(3) 0.640(5) 0.58(4) Uani 1 1 d D U . A 2
H11A H 1.0182 0.2257 0.5953 0.877 Uiso 1 1 d R U . A 2
H11B H 1.0463 0.2750 0.5720 0.877 Uiso 1 1 d R U . A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.278(9) . ?
Dy1 O8 2.366(10) . ?
Dy1 N3 2.400(12) . ?
Dy1 O9 2.414(10) . ?
Dy1 O2 2.479(11) . ?
Dy1 O3 2.500(11) . ?
Dy1 O6 2.533(10) . ?
Dy1 O5 2.546(11) . ?
Dy1 N5 2.607(7) . ?
Dy1 N6 2.893(15) . ?
O1 C6 1.279(15) . ?
O2 N6 1.270(17) . ?
O3 N6 1.243(16) . ?
O4 N6 1.182(17) . ?
O5 N7 1.326(16) . ?
O6 N7 1.218(16) . ?
O7 N7 1.202(16) . ?
O8 C15 1.41(2) . ?
O9 C13 1.482(17) . ?
N2 C6 1.306(18) . ?
N2 N3 1.378(16) . ?
N3 C7 1.265(17) . ?
N4 C7 1.358(18) . ?
N5 C8 1.3900 . ?
N5 C12 1.3900 . ?
C8 C9 1.3900 . ?
C8 C7 1.493(5) . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C5 N1 1.3900 . ?
C5 C4 1.3900 . ?
N1 C1 1.3900 . ?
C1 C2 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C3 C6 1.501(5) . ?
C13 C14 1.489(5) . ?
C15 C16 1.489(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O8 82.9(4) . . ?
O1 Dy1 N3 65.1(4) . . ?
O8 Dy1 N3 80.5(4) . . ?
O1 Dy1 O9 77.7(3) . . ?
O8 Dy1 O9 82.1(4) . . ?
N3 Dy1 O9 140.4(4) . . ?
O1 Dy1 O2 99.1(4) . . ?
O8 Dy1 O2 153.1(4) . . ?
N3 Dy1 O2 76.2(4) . . ?
O9 Dy1 O2 124.6(4) . . ?
O1 Dy1 O3 77.6(4) . . ?
O8 Dy1 O3 152.5(4) . . ?
N3 Dy1 O3 107.9(4) . . ?
O9 Dy1 O3 75.0(3) . . ?
O2 Dy1 O3 51.0(4) . . ?
O1 Dy1 O6 145.2(4) . . ?
O8 Dy1 O6 123.3(4) . . ?
N3 Dy1 O6 135.4(4) . . ?
O9 Dy1 O6 83.4(4) . . ?
O2 Dy1 O6 68.4(4) . . ?
O3 Dy1 O6 69.3(4) . . ?
O1 Dy1 O5 142.5(4) . . ?
O8 Dy1 O5 73.9(4) . . ?
N3 Dy1 O5 136.1(4) . . ?
O9 Dy1 O5 70.4(3) . . ?
O2 Dy1 O5 115.0(4) . . ?
O3 Dy1 O5 111.3(4) . . ?
O6 Dy1 O5 49.7(4) . . ?
O1 Dy1 N5 128.6(3) . . ?
O8 Dy1 N5 86.4(4) . . ?
N3 Dy1 N5 63.6(4) . . ?
O9 Dy1 N5 149.7(3) . . ?
O2 Dy1 N5 71.3(4) . . ?
O3 Dy1 N5 121.0(3) . . ?
O6 Dy1 N5 79.7(4) . . ?
O5 Dy1 N5 79.6(3) . . ?
O1 Dy1 N6 90.2(4) . . ?
O8 Dy1 N6 172.7(4) . . ?
N3 Dy1 N6 94.2(4) . . ?
O9 Dy1 N6 99.0(4) . . ?
O2 Dy1 N6 25.9(3) . . ?
O3 Dy1 N6 25.3(4) . . ?
O6 Dy1 N6 64.0(4) . . ?
O5 Dy1 N6 113.3(4) . . ?
N5 Dy1 N6 95.9(4) . . ?
C6 O1 Dy1 121.3(7) . . ?
N6 O2 Dy1 95.6(9) . . ?
N6 O3 Dy1 95.3(9) . . ?
N7 O5 Dy1 96.2(8) . . ?
N7 O6 Dy1 100.0(8) . . ?
C15 O8 Dy1 134.0(12) . . ?
C13 O9 Dy1 124.0(8) . . ?
C6 N2 N3 111.0(11) . . ?
C7 N3 N2 112.2(11) . . ?
C7 N3 Dy1 128.7(9) . . ?
N2 N3 Dy1 119.1(9) . . ?
C8 N5 C12 120.0 . . ?
C8 N5 Dy1 115.8(4) . . ?
C12 N5 Dy1 123.7(4) . . ?
N5 C8 C9 120.0 . . ?
N5 C8 C7 115.6(8) . . ?
C9 C8 C7 124.3(8) . . ?
C10 C9 C8 120.0 . . ?
C11 C10 C9 120.0 . . ?
C10 C11 C12 120.0 . . ?
C11 C12 N5 120.0 . . ?
O4 N6 O3 122.2(17) . . ?
O4 N6 O2 120.4(16) . . ?
O3 N6 O2 117.1(13) . . ?
O4 N6 Dy1 176.5(14) . . ?
O3 N6 Dy1 59.4(8) . . ?
O2 N6 Dy1 58.5(8) . . ?
O7 N7 O6 126.8(15) . . ?
O7 N7 O5 118.8(15) . . ?
O6 N7 O5 113.9(12) . . ?
N1 C5 C4 120.0 . . ?
C5 N1 C1 120.0 . . ?
N1 C1 C2 120.0 . . ?
C3 C2 C1 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 C6 120.5(9) . . ?
C2 C3 C6 119.4(9) . . ?
C3 C4 C5 120.0 . . ?
O1 C6 N2 123.6(9) . . ?
O1 C6 C3 118.4(11) . . ?
N2 C6 C3 117.9(12) . . ?
N3 C7 N4 126.3(11) . . ?
N3 C7 C8 115.4(11) . . ?
N4 C7 C8 118.3(12) . . ?
C14 C13 O9 111.9(14) . . ?
O8 C15 C16 108.4(19) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H11B N4 0.87 2.68 3.301(5) 129.8 4_565
C15 H15B O5 0.97 2.44 3.10(3) 125.2 .
C13 H13A O3 0.97 2.58 3.22(2) 123.6 .
C12 H12 N7 0.93 2.63 3.362(16) 136.2 .
C5 H5 O7 0.93 2.44 3.221(14) 142.1 1_656
C2 H2 O3 0.93 2.49 3.257(14) 139.9 3_756
N4 H4B O2 0.89 2.22 2.955(16) 139.3 4_566
O9 H9 N7 0.97 2.66 3.558(19) 153.5 3_656
O9 H9 O7 0.97 2.35 3.304(17) 166.9 3_656
O9 H9 O5 0.97 2.28 2.938(15) 124.0 3_656
O8 H8 N1 0.97 2.14 2.63(3) 109.7 3_757

_refine_diff_density_max         3.828
_refine_diff_density_min         -2.797
_refine_diff_density_rms         0.241

