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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mm464
_database_code_depnum_ccdc_archive 'CCDC 1812511'
_audit_update_record             
;
2017-12-19 deposited with the CCDC.
2018-02-08 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         ?
_chemical_formula_sum            'C8.75 H14 Gd2 N18 O8.75'
_chemical_formula_weight         825.88

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'
Gd Gd -0.1653 3.9035 '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                   6.5239(2)
_cell_length_b                   7.8414(2)
_cell_length_c                   10.6792(3)
_cell_angle_alpha                104.2714(12)
_cell_angle_beta                 97.0307(14)
_cell_angle_gamma                97.8719(13)
_cell_volume                     517.48(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    5574
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      28.33

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      n/a
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.650
_exptl_crystal_F_000             390
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    6.444
_shelx_estimated_absorpt_T_min   0.407
_shelx_estimated_absorpt_T_max   0.565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4985
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(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            6019
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.912
_diffrn_reflns_theta_max         28.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             2524
_reflns_number_gt                2482
_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       'APEX II, Bruker (2009)'
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_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)+(0.0312P)²+2.0905P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2524
_refine_ls_number_parameters     191
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0591
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.034
_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
Gd1 Gd 0.60089(3) 0.62336(2) 0.68572(2) 0.01975(7) Uani 1 1 d . U . . .
O1 O 0.8278(5) 0.8783(4) 0.6754(3) 0.0280(6) Uani 1 1 d . . . . .
H1A H 0.8949 0.9822 0.7432 0.042 Uiso 1 1 d R U . . .
H1B H 0.8230 0.9035 0.5875 0.042 Uiso 1 1 d R U . . .
O2 O 0.3630(5) 0.4962(4) 0.8080(3) 0.0275(6) Uani 1 1 d . . . . .
H2A H 0.2606 0.5597 0.8455 0.041 Uiso 1 1 d R U . . .
H2B H 0.3088 0.3641 0.7812 0.041 Uiso 1 1 d R U . . .
O3 O 0.7090(6) 0.3547(4) 0.7040(3) 0.0405(8) Uani 1 1 d . . . . .
H3A H 0.7264 0.3145 0.7815 0.061 Uiso 1 1 d R U . . .
H3B H 0.7045 0.2534 0.6244 0.061 Uiso 1 1 d R U . . .
O4 O 0.6587(17) 0.5655(18) 0.4763(11) 0.043(3) Uani 0.625 1 d . . P A 1
H4A H 0.7859 0.6171 0.4551 0.4(3) Uiso 0.625 1 calc R . P A 1
N1 N 0.5554(4) 0.8912(4) 0.8925(3) 0.0142(5) Uani 1 1 d . . . . .
N2 N 0.8632(5) 0.6965(4) 0.9017(3) 0.0177(5) Uani 1 1 d . . . . .
N3 N 1.0517(5) 0.6545(4) 0.9322(3) 0.0207(6) Uani 1 1 d . . . . .
N4 N 1.1304(5) 0.7390(4) 1.0547(3) 0.0203(6) Uani 1 1 d . . . . .
N5 N 0.9949(5) 0.8383(4) 1.1076(3) 0.0183(5) Uani 1 1 d . . . . .
N6 N 0.6460(5) 1.1622(4) 1.3535(3) 0.0207(6) Uani 1 1 d . . . . .
N7 N 0.7106(5) 1.1230(4) 1.4653(3) 0.0224(6) Uani 1 1 d . . . . .
N8 N 0.7604(5) 0.9636(4) 1.4387(3) 0.0205(6) Uani 1 1 d . . . . .
N9 N 0.7323(5) 0.8932(4) 1.3088(3) 0.0188(5) Uani 1 1 d . . . . .
C1 C 0.6525(5) 0.9004(4) 1.0126(3) 0.0135(5) Uani 1 1 d . . . . .
C2 C 0.8328(5) 0.8079(4) 1.0110(3) 0.0156(6) Uani 1 1 d . . . . .
C3 C 0.5919(5) 1.0090(4) 1.1228(3) 0.0133(5) Uani 1 1 d . . . . .
C4 C 0.6642(5) 1.0189(4) 1.2599(3) 0.0149(6) Uani 1 1 d . . . . .
O4' O 0.700(4) 0.542(3) 0.472(2) 0.048(4) Uani 0.375 1 d . U P A -2
C5 C 0.874(3) 0.544(2) 0.4800(17) 0.058(3) Uani 0.375 1 d . U P A -2
H5A H 0.9501 0.5396 0.4092 0.070 Uiso 0.375 1 calc R U P A -2
O5 O 0.9652(18) 0.5531(14) 0.6086(12) 0.053(2) Uani 0.375 1 d . U P 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
Gd1 O4 2.259(12) . ?
Gd1 O4 2.321(12) 2_666 ?
Gd1 O1 2.353(3) . ?
Gd1 O3 2.355(3) . ?
Gd1 O4' 2.41(2) . ?
Gd1 O2 2.413(3) . ?
Gd1 N6 2.554(3) 2_677 ?
Gd1 N2 2.587(3) . ?
Gd1 O5 2.692(10) . ?
Gd1 N1 2.724(3) . ?
Gd1 C5 2.997(19) . ?
Gd1 Gd1 3.9308(3) 2_666 ?
O4 Gd1 2.321(11) 2_666 ?
N1 C3 1.339(4) 2_677 ?
N1 C1 1.339(4) . ?
N2 C2 1.329(4) . ?
N2 N3 1.339(4) . ?
N3 N4 1.315(4) . ?
N4 N5 1.342(4) . ?
N5 C2 1.335(4) . ?
N6 C4 1.338(4) . ?
N6 N7 1.338(4) . ?
N6 Gd1 2.554(3) 2_677 ?
N7 N8 1.307(5) . ?
N8 N9 1.340(4) . ?
N9 C4 1.326(4) . ?
C1 C3 1.407(4) . ?
C1 C2 1.464(4) . ?
C3 N1 1.339(4) 2_677 ?
C3 C4 1.462(4) . ?
O4' C5 1.13(3) . ?
C5 O5 1.41(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
O4 Gd1 O4 61.8(6) . 2_666 ?
O4 Gd1 O1 74.9(4) . . ?
O4 Gd1 O1 128.6(4) 2_666 . ?
O4 Gd1 O3 90.2(3) . . ?
O4 Gd1 O3 83.6(3) 2_666 . ?
O1 Gd1 O3 124.42(13) . . ?
O1 Gd1 O4' 75.4(5) . . ?
O3 Gd1 O4' 83.7(5) . . ?
O4 Gd1 O2 137.0(3) . . ?
O4 Gd1 O2 76.6(3) 2_666 . ?
O1 Gd1 O2 146.51(10) . . ?
O3 Gd1 O2 74.08(12) . . ?
O4' Gd1 O2 137.7(5) . . ?
O4 Gd1 N6 91.6(3) . 2_677 ?
O4 Gd1 N6 78.7(3) 2_666 2_677 ?
O1 Gd1 N6 76.25(11) . 2_677 ?
O3 Gd1 N6 158.86(12) . 2_677 ?
O4' Gd1 N6 99.1(6) . 2_677 ?
O2 Gd1 N6 90.48(10) . 2_677 ?
O4 Gd1 N2 130.1(3) . . ?
O4 Gd1 N2 152.6(4) 2_666 . ?
O1 Gd1 N2 77.42(9) . . ?
O3 Gd1 N2 72.64(10) . . ?
O4' Gd1 N2 123.6(6) . . ?
O2 Gd1 N2 83.69(10) . . ?
N6 Gd1 N2 120.79(9) 2_677 . ?
O1 Gd1 O5 66.4(2) . . ?
O3 Gd1 O5 61.5(3) . . ?
O4' Gd1 O5 48.3(7) . . ?
O2 Gd1 O5 134.7(3) . . ?
N6 Gd1 O5 134.7(3) 2_677 . ?
N2 Gd1 O5 75.7(3) . . ?
O4 Gd1 N1 142.9(4) . . ?
O4 Gd1 N1 128.1(3) 2_666 . ?
O1 Gd1 N1 74.28(9) . . ?
O3 Gd1 N1 124.44(9) . . ?
O4' Gd1 N1 147.1(5) . . ?
O2 Gd1 N1 72.38(9) . . ?
N6 Gd1 N1 61.33(9) 2_677 . ?
N2 Gd1 N1 60.82(8) . . ?
O5 Gd1 N1 126.2(3) . . ?
O1 Gd1 C5 66.9(3) . . ?
O3 Gd1 C5 75.6(4) . . ?
O4' Gd1 C5 20.6(7) . . ?
O2 Gd1 C5 145.3(3) . . ?
N6 Gd1 C5 113.4(4) 2_677 . ?
N2 Gd1 C5 103.0(4) . . ?
O5 Gd1 C5 28.0(5) . . ?
N1 Gd1 C5 140.6(3) . . ?
O4 Gd1 Gd1 31.4(3) . 2_666 ?
O4 Gd1 Gd1 30.4(3) 2_666 2_666 ?
O1 Gd1 Gd1 102.65(6) . 2_666 ?
O3 Gd1 Gd1 86.36(7) . 2_666 ?
O4' Gd1 Gd1 35.3(6) . 2_666 ?
O2 Gd1 Gd1 106.50(7) . 2_666 ?
N6 Gd1 Gd1 84.28(7) 2_677 2_666 ?
N2 Gd1 Gd1 153.40(6) . 2_666 ?
O5 Gd1 Gd1 80.1(3) . 2_666 ?
N1 Gd1 Gd1 145.40(6) . 2_666 ?
C5 Gd1 Gd1 54.8(3) . 2_666 ?
Gd1 O4 Gd1 118.2(6) . 2_666 ?
C3 N1 C1 120.2(3) 2_677 . ?
C3 N1 Gd1 119.4(2) 2_677 . ?
C1 N1 Gd1 119.4(2) . . ?
C2 N2 N3 104.7(3) . . ?
C2 N2 Gd1 121.8(2) . . ?
N3 N2 Gd1 133.3(2) . . ?
N4 N3 N2 109.5(3) . . ?
N3 N4 N5 109.5(3) . . ?
C2 N5 N4 104.3(3) . . ?
C4 N6 N7 104.2(3) . . ?
C4 N6 Gd1 122.4(2) . 2_677 ?
N7 N6 Gd1 128.6(2) . 2_677 ?
N8 N7 N6 109.4(3) . . ?
N7 N8 N9 110.1(3) . . ?
C4 N9 N8 104.1(3) . . ?
N1 C1 C3 119.6(3) . . ?
N1 C1 C2 113.1(3) . . ?
C3 C1 C2 126.9(3) . . ?
N2 C2 N5 112.0(3) . . ?
N2 C2 C1 121.1(3) . . ?
N5 C2 C1 126.4(3) . . ?
N1 C3 C1 120.2(3) 2_677 . ?
N1 C3 C4 113.2(3) 2_677 . ?
C1 C3 C4 126.5(3) . . ?
N9 C4 N6 112.2(3) . . ?
N9 C4 C3 128.0(3) . . ?
N6 C4 C3 119.5(3) . . ?
C5 O4' Gd1 110.6(17) . . ?
O4' C5 O5 111.6(18) . . ?
O4' C5 Gd1 48.9(13) . . ?
O5 C5 Gd1 63.9(8) . . ?
C5 O5 Gd1 88.1(11) . . ?

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 N2 N3 N4 -0.4(4) . . . . ?
Gd1 N2 N3 N4 174.2(2) . . . . ?
N2 N3 N4 N5 0.1(4) . . . . ?
N3 N4 N5 C2 0.3(4) . . . . ?
C4 N6 N7 N8 -1.1(4) . . . . ?
Gd1 N6 N7 N8 154.2(2) 2_677 . . . ?
N6 N7 N8 N9 0.6(4) . . . . ?
N7 N8 N9 C4 0.2(4) . . . . ?
C3 N1 C1 C3 3.0(5) 2_677 . . . ?
Gd1 N1 C1 C3 -164.8(2) . . . . ?
C3 N1 C1 C2 -170.0(3) 2_677 . . . ?
Gd1 N1 C1 C2 22.2(3) . . . . ?
N3 N2 C2 N5 0.6(4) . . . . ?
Gd1 N2 C2 N5 -174.7(2) . . . . ?
N3 N2 C2 C1 172.8(3) . . . . ?
Gd1 N2 C2 C1 -2.6(4) . . . . ?
N4 N5 C2 N2 -0.5(4) . . . . ?
N4 N5 C2 C1 -172.2(3) . . . . ?
N1 C1 C2 N2 -13.5(4) . . . . ?
C3 C1 C2 N2 174.1(3) . . . . ?
N1 C1 C2 N5 157.5(3) . . . . ?
C3 C1 C2 N5 -14.9(6) . . . . ?
N1 C1 C3 N1 -3.0(5) . . . 2_677 ?
C2 C1 C3 N1 168.9(3) . . . 2_677 ?
N1 C1 C3 C4 172.6(3) . . . . ?
C2 C1 C3 C4 -15.4(5) . . . . ?
N8 N9 C4 N6 -1.0(4) . . . . ?
N8 N9 C4 C3 -174.6(3) . . . . ?
N7 N6 C4 N9 1.3(4) . . . . ?
Gd1 N6 C4 N9 -156.0(2) 2_677 . . . ?
N7 N6 C4 C3 175.5(3) . . . . ?
Gd1 N6 C4 C3 18.3(4) 2_677 . . . ?
N1 C3 C4 N9 148.8(3) 2_677 . . . ?
C1 C3 C4 N9 -27.1(5) . . . . ?
N1 C3 C4 N6 -24.4(4) 2_677 . . . ?
C1 C3 C4 N6 159.7(3) . . . . ?
Gd1 O4' C5 O5 13(2) . . . . ?
O4' C5 O5 Gd1 -10.9(17) . . . . ?

_refine_diff_density_max         1.860
_refine_diff_density_min         -2.952
_refine_diff_density_rms         0.149

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1812514'
_audit_update_record             
;
2017-12-19 deposited with the CCDC.
2018-02-08 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         ?
_chemical_formula_sum            'C12 H27 Dy N27 O12'
_chemical_formula_weight         904.10

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      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                   9.7883(6)
_cell_length_b                   11.1740(6)
_cell_length_c                   14.3567(8)
_cell_angle_alpha                101.599(3)
_cell_angle_beta                 97.500(3)
_cell_angle_gamma                93.781(3)
_cell_volume                     1518.14(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9890
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      28.41
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_F_000             900
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.566
_shelx_estimated_absorpt_T_min   0.602
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5547
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(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            17057
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.464
_diffrn_reflns_theta_max         28.411
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             7372
_reflns_number_gt                6864
_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       'APEX II (Bruker, 2009)'
_computing_cell_refinement       'APEX II (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker)'
_computing_structure_solution    'XT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.0248P)²+3.0347P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7372
_refine_ls_number_parameters     676
_refine_ls_number_restraints     592
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0640
_refine_ls_wR_factor_gt          0.0621
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.056
_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
Dy1 Dy 0.42949(2) 0.17255(2) 0.84268(2) 0.01634(4) Uani 1 1 d . . . . .
C1 C 0.3388(3) 0.1197(2) 0.58191(18) 0.0140(5) Uani 1 1 d D U . . .
C2 C 0.3360(3) 0.2504(2) 0.62379(19) 0.0153(5) Uani 1 1 d D U . . .
C3 C 0.3738(3) -0.0683(2) 0.62252(18) 0.0140(5) Uani 1 1 d D U . . .
C4 C 0.4121(3) -0.1244(2) 0.70448(19) 0.0156(5) Uani 1 1 d D U . . .
C5 C 0.3167(3) 0.0610(2) 0.48345(19) 0.0148(5) Uani 1 1 d D U . . .
C6 C 0.2862(3) 0.1185(2) 0.40027(19) 0.0175(5) Uani 1 1 d D U . . .
C7 C 0.3495(3) -0.1259(2) 0.52452(18) 0.0135(5) Uani 1 1 d D U . . .
C8 C 0.3507(3) -0.2578(2) 0.48091(19) 0.0146(5) Uani 1 1 d D U . . .
N1 N 0.3683(2) 0.05313(19) 0.64862(16) 0.0144(4) Uani 1 1 d D U . . .
N2 N 0.3234(2) -0.05944(19) 0.45765(16) 0.0149(4) Uani 1 1 d D U . . .
N3 N 0.3601(3) 0.2934(2) 0.71879(17) 0.0201(5) Uani 1 1 d D U . . .
N4 N 0.3502(3) 0.4148(2) 0.73072(18) 0.0240(5) Uani 1 1 d D U . . .
N5 N 0.3229(3) 0.4436(2) 0.64657(18) 0.0222(5) Uani 1 1 d D U . . .
N6 N 0.3138(3) 0.3411(2) 0.57787(17) 0.0188(5) Uani 1 1 d D U . . .
N7 N 0.4456(3) -0.0554(2) 0.79348(16) 0.0180(4) Uani 1 1 d D U . . .
N8 N 0.4771(3) -0.1350(2) 0.84894(17) 0.0243(5) Uani 1 1 d D U . . .
N9 N 0.4633(3) -0.2470(2) 0.79627(18) 0.0263(5) Uani 1 1 d D U . . .
N10 N 0.4217(3) -0.2427(2) 0.70427(17) 0.0211(5) Uani 1 1 d D U . . .
N11 N 0.2655(3) 0.0556(2) 0.30972(17) 0.0232(5) Uani 1 1 d D U . . .
N12 N 0.2398(3) 0.1385(2) 0.25493(18) 0.0272(5) Uani 1 1 d D U . . .
N13 N 0.2454(3) 0.2485(2) 0.30835(18) 0.0269(5) Uani 1 1 d D U . . .
N14 N 0.2745(3) 0.2366(2) 0.39935(17) 0.0213(5) Uani 1 1 d D U . . .
H14A H 0.2845 0.2969 0.4504 0.026 Uiso 1 1 calc R U . . .
N15 N 0.3395(3) -0.2996(2) 0.38662(17) 0.0190(5) Uani 1 1 d D U . . .
N16 N 0.3412(3) -0.4225(2) 0.37372(17) 0.0210(5) Uani 1 1 d D U . . .
N17 N 0.3526(3) -0.4561(2) 0.45563(18) 0.0224(5) Uani 1 1 d D U . . .
N18 N 0.3590(3) -0.3540(2) 0.52312(17) 0.0188(4) Uani 1 1 d D U . . .
H18A H 0.3673 -0.3504 0.5854 0.023 Uiso 1 1 calc R U . . .
C9 C 1.0219(8) 0.5679(6) 0.5679(5) 0.0172(13) Uani 0.5 1 d D U P A -1
C10 C 1.0541(7) 0.6651(6) 0.6546(5) 0.0169(13) Uani 0.5 1 d D U P A -1
C11 C 0.9984(10) 0.5307(7) 0.4018(5) 0.0176(15) Uani 0.5 1 d D U P A -1
C12 C 1.0099(8) 0.5909(6) 0.3207(6) 0.0185(15) Uani 0.5 1 d D U P A -1
C13 C 0.9934(8) 0.4406(7) 0.5631(6) 0.0153(15) Uani 0.5 1 d D U P A -1
C14 C 0.9943(9) 0.3793(7) 0.6447(6) 0.0210(15) Uani 0.5 1 d D U P A -1
C15 C 0.9638(8) 0.4049(7) 0.3965(5) 0.0171(13) Uani 0.5 1 d D U P A -1
C16 C 0.9233(8) 0.3111(6) 0.3085(6) 0.0204(14) Uani 0.5 1 d D U P A -1
N19 N 1.0254(7) 0.6085(7) 0.4868(5) 0.0155(13) Uani 0.5 1 d D U P A -1
N20 N 0.9647(9) 0.3637(7) 0.4775(5) 0.0193(14) Uani 0.5 1 d D U P A -1
N21 N 1.0831(8) 0.7824(6) 0.6516(5) 0.0226(14) Uani 0.5 1 d D U P A -1
N22 N 1.1058(9) 0.8425(7) 0.7444(6) 0.0253(16) Uani 0.5 1 d D U P A -1
N23 N 1.0912(7) 0.7673(6) 0.8020(5) 0.0306(13) Uani 0.5 1 d D U P A -1
N24 N 1.0582(7) 0.6565(5) 0.7464(4) 0.0248(11) Uani 0.5 1 d D U P A -1
N25 N 0.9954(8) 0.7100(6) 0.3297(5) 0.0241(15) Uani 0.5 1 d D U P A -1
H25 H 0.9745 0.7599 0.3805 0.029 Uiso 0.5 1 calc R U P A -1
N26 N 1.0183(10) 0.7397(9) 0.2473(6) 0.0298(18) Uani 0.5 1 d D U P A -1
N27 N 1.0486(9) 0.6413(7) 0.1910(6) 0.0304(16) Uani 0.5 1 d D U P A -1
N28 N 1.0459(8) 0.5464(6) 0.2355(5) 0.0261(14) Uani 0.5 1 d D U P A -1
N29 N 1.0004(9) 0.2582(6) 0.6337(5) 0.0279(15) Uani 0.5 1 d D U P A -1
N30 N 0.9991(10) 0.2357(8) 0.7211(6) 0.0306(18) Uani 0.5 1 d D U P A -1
N31 N 0.9916(9) 0.3365(9) 0.7835(6) 0.0337(16) Uani 0.5 1 d D U P A -1
N32 N 0.9890(8) 0.4292(6) 0.7356(6) 0.0270(15) Uani 0.5 1 d D U P A -1
H32 H 0.9846 0.5074 0.7602 0.032 Uiso 0.5 1 calc R U P A -1
N33 N 0.9257(8) 0.1922(6) 0.3101(6) 0.0226(14) Uani 0.5 1 d D U P A -1
N34 N 0.8796(10) 0.1334(7) 0.2189(6) 0.0278(17) Uani 0.5 1 d D U P A -1
N35 N 0.8456(8) 0.2125(5) 0.1668(5) 0.0331(14) Uani 0.5 1 d D U P A -1
N36 N 0.8713(8) 0.3258(5) 0.2215(4) 0.0306(12) Uani 0.5 1 d D U P A -1
O1 O 0.6272(2) 0.16809(19) 0.76116(15) 0.0229(4) Uani 1 1 d D . . . .
H1A H 0.661(4) 0.105(2) 0.744(3) 0.034 Uiso 1 1 d D U . . .
H1B H 0.642(4) 0.211(3) 0.724(2) 0.034 Uiso 1 1 d D U . . .
O2 O 0.5523(3) 0.36916(19) 0.89991(17) 0.0316(5) Uani 1 1 d D . . . .
H2A H 0.577(4) 0.416(3) 0.868(2) 0.047 Uiso 1 1 d D U . . .
H2B H 0.593(4) 0.391(4) 0.9533(16) 0.047 Uiso 1 1 d D U . . .
O3 O 0.6273(2) 0.1504(2) 0.95194(16) 0.0270(5) Uani 1 1 d D . . . .
H3A H 0.701(3) 0.189(3) 0.952(3) 0.041 Uiso 1 1 d D U . . .
H3B H 0.634(4) 0.123(4) 0.999(2) 0.041 Uiso 1 1 d D U . . .
O4 O 0.2873(3) 0.3115(2) 0.9237(2) 0.0432(7) Uani 1 1 d D . . . .
H4A H 0.291(5) 0.384(2) 0.924(4) 0.065 Uiso 1 1 d D U . . .
H4B H 0.237(5) 0.299(4) 0.961(3) 0.065 Uiso 1 1 d D U . . .
O5 O 0.3614(2) 0.0861(2) 0.97039(15) 0.0253(4) Uani 1 1 d D . . . .
H5A H 0.2793(19) 0.079(4) 0.976(3) 0.038 Uiso 1 1 d D U . . .
H5B H 0.409(3) 0.100(4) 1.0233(18) 0.038 Uiso 1 1 d D U . . .
O6 O 0.1938(2) 0.0958(2) 0.79734(17) 0.0262(4) Uani 1 1 d D . . . .
H6A H 0.170(4) 0.0236(17) 0.789(3) 0.039 Uiso 1 1 d D U . . .
H6B H 0.132(3) 0.137(3) 0.785(3) 0.039 Uiso 1 1 d D U . . .
O7 O 0.6445(3) 0.5575(2) 0.82119(18) 0.0352(6) Uani 1 1 d D . . . .
H7A H 0.653(5) 0.526(4) 0.7650(18) 0.053 Uiso 1 1 d D U . . .
H7B H 0.586(4) 0.606(3) 0.821(3) 0.053 Uiso 1 1 d D U . . .
O8 O 0.3075(3) 0.5540(2) 0.91756(19) 0.0394(6) Uani 1 1 d D . . . .
H8A H 0.238(3) 0.588(4) 0.924(3) 0.059 Uiso 1 1 d D U . . .
H8B H 0.325(5) 0.539(4) 0.8634(19) 0.059 Uiso 1 1 d D U . . .
O9 O 0.1258(8) 0.1035(6) 1.0532(6) 0.0411(12) Uani 0.5 1 d D . P B 1
H9A H 0.143(11) 0.090(8) 1.107(3) 0.062 Uiso 0.5 1 d D U P C 1
H9B H 0.109(11) 0.175(3) 1.061(6) 0.062 Uiso 0.5 1 d D U P D 1
O10 O 0.8604(6) 0.3088(7) 0.9799(5) 0.0531(13) Uani 0.5 1 d D . P E 1
H10A H 0.860(7) 0.342(9) 0.935(5) 0.080 Uiso 0.5 1 d D U P F 1
H10B H 0.931(3) 0.288(3) 0.9934(13) 0.080 Uiso 1 1 d D U . . .
O11 O 0.0969(6) 0.3461(5) 1.0849(5) 0.0463(10) Uani 0.5 1 d D . P G 1
H11A H 0.0553 0.3442 1.1305 0.069 Uiso 0.5 1 d DR U P G 1
H11B H 0.1744 0.3743 1.1127 0.069 Uiso 1 1 d DR U . . .
O12 O 0.9889(7) 0.9096(5) 0.5329(5) 0.0364(10) Uani 0.5 1 d D . P H 1
H12A H 1.021(10) 0.884(8) 0.580(4) 0.055 Uiso 0.5 1 d D U P I 1
H12B H 0.991(17) 0.854(8) 0.487(4) 0.055 Uiso 0.5 1 d D U P J 1
O9' O 0.1164(8) 0.0421(6) 1.0375(6) 0.0411(12) Uani 0.5 1 d D . P K 2
H9C H 0.121(10) -0.006(7) 1.074(5) 0.062 Uiso 0.5 1 d D U P L 2
H9D H 0.058(7) 0.015(8) 0.990(4) 0.062 Uiso 0.5 1 d D U P M 2
O10' O 0.8834(6) 0.2417(7) 0.9375(5) 0.0531(13) Uani 0.5 1 d D . P N 2
H10D H 0.9121 0.2782 0.8981 0.080 Uiso 0.5 1 d DR U P N 2
O11' O 0.1325(6) 0.2914(6) 1.0596(5) 0.0463(10) Uani 0.5 1 d D . P O 2
H11C H 0.1415 0.2517 1.1006 0.069 Uiso 0.5 1 d DR U P O 2
O12' O 0.9680(8) 0.8671(6) 0.4815(5) 0.0364(10) Uani 0.5 1 d D . P P 2
H12C H 1.019(10) 0.857(8) 0.529(5) 0.055 Uiso 0.5 1 d D U P Q 2
H12D H 0.983(9) 0.938(4) 0.475(6) 0.055 Uiso 0.5 1 d D U P R 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 O6 2.367(2) . ?
Dy1 O2 2.370(2) . ?
Dy1 O4 2.384(2) . ?
Dy1 O5 2.384(2) . ?
Dy1 O1 2.387(2) . ?
Dy1 O3 2.387(2) . ?
Dy1 N3 2.494(2) . ?
Dy1 N7 2.524(2) . ?
Dy1 N1 2.805(2) . ?
C1 N1 1.341(3) . ?
C1 C5 1.416(3) . ?
C1 C2 1.466(3) . ?
C2 N6 1.331(3) . ?
C2 N3 1.336(3) . ?
C3 N1 1.340(3) . ?
C3 C7 1.407(3) . ?
C3 C4 1.460(3) . ?
C4 N10 1.331(3) . ?
C4 N7 1.340(3) . ?
C5 N2 1.330(3) . ?
C5 C6 1.472(3) . ?
C6 N11 1.330(4) . ?
C6 N14 1.335(3) . ?
C7 N2 1.336(3) . ?
C7 C8 1.483(3) . ?
C8 N15 1.328(3) . ?
C8 N18 1.338(3) . ?
N3 N4 1.345(3) . ?
N4 N5 1.310(3) . ?
N5 N6 1.342(3) . ?
N7 N8 1.333(3) . ?
N8 N9 1.314(3) . ?
N9 N10 1.342(3) . ?
N11 N12 1.346(3) . ?
N12 N13 1.305(4) . ?
N13 N14 1.335(3) . ?
N14 H14A 0.8800 . ?
N15 N16 1.350(3) . ?
N16 N17 1.298(3) . ?
N17 N18 1.332(3) . ?
N18 H18A 0.8800 . ?
C9 N19 1.334(8) . ?
C9 C13 1.418(9) . ?
C9 C10 1.462(8) . ?
C10 N21 1.334(8) . ?
C10 N24 1.337(8) . ?
C11 N19 1.332(8) . ?
C11 C15 1.409(9) . ?
C11 C12 1.471(9) . ?
C12 N28 1.326(9) . ?
C12 N25 1.330(8) . ?
C13 N20 1.335(8) . ?
C13 C14 1.470(9) . ?
C14 N32 1.321(9) . ?
C14 N29 1.337(9) . ?
C15 N20 1.332(9) . ?
C15 C16 1.461(9) . ?
C16 N36 1.332(9) . ?
C16 N33 1.334(8) . ?
N21 N22 1.349(8) . ?
N22 N23 1.306(9) . ?
N23 N24 1.325(8) . ?
N25 N26 1.332(9) . ?
N25 H25 0.8800 . ?
N26 N27 1.304(9) . ?
N27 N28 1.345(8) . ?
N29 N30 1.329(9) . ?
N30 N31 1.304(10) . ?
N31 N32 1.353(9) . ?
N32 H32 0.8800 . ?
N33 N34 1.345(8) . ?
N34 N35 1.300(9) . ?
N35 N36 1.337(8) . ?
O1 H1A 0.812(18) . ?
O1 H1B 0.801(18) . ?
O2 H2A 0.804(18) . ?
O2 H2B 0.799(18) . ?
O3 H3A 0.817(18) . ?
O3 H3B 0.796(18) . ?
O4 H4A 0.808(19) . ?
O4 H4B 0.802(19) . ?
O5 H5A 0.820(18) . ?
O5 H5B 0.818(18) . ?
O6 H6A 0.806(18) . ?
O6 H6B 0.800(18) . ?
O7 H7A 0.831(19) . ?
O7 H7B 0.816(19) . ?
O8 H8A 0.802(19) . ?
O8 H8B 0.806(19) . ?
O9 H9A 0.81(2) . ?
O9 H9B 0.81(2) . ?
O10 H10A 0.81(2) . ?
O10 H10B 0.756(19) . ?
O11 H11A 0.8184 . ?
O11 H11B 0.8207 . ?
O12 H12A 0.82(2) . ?
O12 H12B 0.82(2) . ?
O9' H9C 0.82(2) . ?
O9' H9D 0.82(2) . ?
O10' H10B 0.913(19) . ?
O10' H10D 0.8266 . ?
O11' H11B 1.0914 . ?
O11' H11C 0.8049 . ?
O12' H12C 0.83(2) . ?
O12' H12D 0.82(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
O6 Dy1 O2 135.67(8) . . ?
O6 Dy1 O4 70.16(9) . . ?
O2 Dy1 O4 69.61(10) . . ?
O6 Dy1 O5 72.76(8) . . ?
O2 Dy1 O5 111.93(8) . . ?
O4 Dy1 O5 73.36(9) . . ?
O6 Dy1 O1 134.40(8) . . ?
O2 Dy1 O1 74.83(8) . . ?
O4 Dy1 O1 141.69(8) . . ?
O5 Dy1 O1 135.22(7) . . ?
O6 Dy1 O3 140.00(8) . . ?
O2 Dy1 O3 72.44(8) . . ?
O4 Dy1 O3 109.69(10) . . ?
O5 Dy1 O3 69.36(8) . . ?
O1 Dy1 O3 71.39(8) . . ?
O6 Dy1 N3 80.15(8) . . ?
O2 Dy1 N3 74.35(8) . . ?
O4 Dy1 N3 78.50(9) . . ?
O5 Dy1 N3 146.05(8) . . ?
O1 Dy1 N3 78.65(8) . . ?
O3 Dy1 N3 139.83(8) . . ?
O6 Dy1 N7 77.93(8) . . ?
O2 Dy1 N7 146.40(9) . . ?
O4 Dy1 N7 139.59(9) . . ?
O5 Dy1 N7 73.97(7) . . ?
O1 Dy1 N7 78.71(7) . . ?
O3 Dy1 N7 79.78(8) . . ?
N3 Dy1 N7 120.16(7) . . ?
O6 Dy1 N1 67.34(7) . . ?
O2 Dy1 N1 124.83(7) . . ?
O4 Dy1 N1 124.37(9) . . ?
O5 Dy1 N1 123.25(7) . . ?
O1 Dy1 N1 67.07(7) . . ?
O3 Dy1 N1 125.95(7) . . ?
N3 Dy1 N1 60.47(7) . . ?
N7 Dy1 N1 59.70(7) . . ?
N1 C1 C5 119.4(2) . . ?
N1 C1 C2 112.7(2) . . ?
C5 C1 C2 127.9(2) . . ?
N6 C2 N3 110.7(2) . . ?
N6 C2 C1 127.9(2) . . ?
N3 C2 C1 121.4(2) . . ?
N1 C3 C7 119.7(2) . . ?
N1 C3 C4 112.5(2) . . ?
C7 C3 C4 127.7(2) . . ?
N10 C4 N7 111.2(2) . . ?
N10 C4 C3 128.0(2) . . ?
N7 C4 C3 120.9(2) . . ?
N2 C5 C1 120.2(2) . . ?
N2 C5 C6 112.5(2) . . ?
C1 C5 C6 127.3(2) . . ?
N11 C6 N14 108.1(2) . . ?
N11 C6 C5 123.2(2) . . ?
N14 C6 C5 128.7(2) . . ?
N2 C7 C3 120.1(2) . . ?
N2 C7 C8 111.7(2) . . ?
C3 C7 C8 128.2(2) . . ?
N15 C8 N18 107.9(2) . . ?
N15 C8 C7 122.5(2) . . ?
N18 C8 C7 129.6(2) . . ?
C3 N1 C1 120.3(2) . . ?
C3 N1 Dy1 120.43(16) . . ?
C1 N1 Dy1 119.17(16) . . ?
C5 N2 C7 120.2(2) . . ?
C2 N3 N4 105.1(2) . . ?
C2 N3 Dy1 126.04(16) . . ?
N4 N3 Dy1 128.65(18) . . ?
N5 N4 N3 109.6(2) . . ?
N4 N5 N6 108.8(2) . . ?
C2 N6 N5 105.9(2) . . ?
N8 N7 C4 104.8(2) . . ?
N8 N7 Dy1 128.75(17) . . ?
C4 N7 Dy1 126.24(17) . . ?
N9 N8 N7 109.9(2) . . ?
N8 N9 N10 108.9(2) . . ?
C4 N10 N9 105.2(2) . . ?
C6 N11 N12 105.9(2) . . ?
N13 N12 N11 110.7(2) . . ?
N12 N13 N14 106.4(2) . . ?
N13 N14 C6 108.9(2) . . ?
N13 N14 H14A 125.5 . . ?
C6 N14 H14A 125.5 . . ?
C8 N15 N16 105.9(2) . . ?
N17 N16 N15 110.7(2) . . ?
N16 N17 N18 106.5(2) . . ?
N17 N18 C8 109.0(2) . . ?
N17 N18 H18A 125.5 . . ?
C8 N18 H18A 125.5 . . ?
N19 C9 C13 119.5(6) . . ?
N19 C9 C10 113.4(6) . . ?
C13 C9 C10 127.1(6) . . ?
N21 C10 N24 108.6(6) . . ?
N21 C10 C9 122.6(6) . . ?
N24 C10 C9 128.8(6) . . ?
N19 C11 C15 120.2(6) . . ?
N19 C11 C12 113.0(6) . . ?
C15 C11 C12 126.8(7) . . ?
N28 C12 N25 109.7(6) . . ?
N28 C12 C11 129.4(6) . . ?
N25 C12 C11 120.6(7) . . ?
N20 C13 C9 119.5(6) . . ?
N20 C13 C14 113.7(6) . . ?
C9 C13 C14 126.8(7) . . ?
N32 C14 N29 110.1(6) . . ?
N32 C14 C13 128.1(7) . . ?
N29 C14 C13 121.8(7) . . ?
N20 C15 C11 119.3(7) . . ?
N20 C15 C16 114.7(6) . . ?
C11 C15 C16 126.0(6) . . ?
N36 C16 N33 110.8(6) . . ?
N36 C16 C15 128.4(6) . . ?
N33 C16 C15 120.6(7) . . ?
C9 N19 C11 120.4(6) . . ?
C15 N20 C13 120.9(6) . . ?
C10 N21 N22 104.8(6) . . ?
N23 N22 N21 111.3(7) . . ?
N22 N23 N24 106.4(6) . . ?
N23 N24 C10 108.8(6) . . ?
N26 N25 C12 107.1(6) . . ?
N26 N25 H25 126.4 . . ?
C12 N25 H25 126.4 . . ?
N27 N26 N25 107.8(7) . . ?
N26 N27 N28 110.0(7) . . ?
C12 N28 N27 105.3(6) . . ?
N30 N29 C14 105.2(7) . . ?
N31 N30 N29 110.8(7) . . ?
N30 N31 N32 107.3(7) . . ?
C14 N32 N31 106.6(7) . . ?
C14 N32 H32 126.7 . . ?
N31 N32 H32 126.7 . . ?
C16 N33 N34 104.6(7) . . ?
N35 N34 N33 109.8(6) . . ?
N34 N35 N36 109.2(6) . . ?
C16 N36 N35 105.5(6) . . ?
Dy1 O1 H1A 121(3) . . ?
Dy1 O1 H1B 124(3) . . ?
H1A O1 H1B 107(3) . . ?
Dy1 O2 H2A 127(3) . . ?
Dy1 O2 H2B 123(3) . . ?
H2A O2 H2B 108(3) . . ?
Dy1 O3 H3A 120(3) . . ?
Dy1 O3 H3B 131(3) . . ?
H3A O3 H3B 107(3) . . ?
Dy1 O4 H4A 125(3) . . ?
Dy1 O4 H4B 127(3) . . ?
H4A O4 H4B 107(3) . . ?
Dy1 O5 H5A 119(3) . . ?
Dy1 O5 H5B 121(3) . . ?
H5A O5 H5B 110(3) . . ?
Dy1 O6 H6A 122(3) . . ?
Dy1 O6 H6B 124(3) . . ?
H6A O6 H6B 114(3) . . ?
H7A O7 H7B 109(3) . . ?
H8A O8 H8B 115(3) . . ?
H9A O9 H9B 106(3) . . ?
H10A O10 H10B 111(4) . . ?
H11A O11 H11B 100.9 . . ?
H12A O12 H12B 105(3) . . ?
H9C O9' H9D 111(4) . . ?
H10B O10' H10D 100.4 . . ?
H11B O11' H11C 90.1 . . ?
H12C O12' H12D 109(4) . . ?

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
N1 C1 C2 N6 178.1(3) . . . . ?
C5 C1 C2 N6 -0.9(5) . . . . ?
N1 C1 C2 N3 -0.5(4) . . . . ?
C5 C1 C2 N3 -179.4(3) . . . . ?
N1 C3 C4 N10 177.3(3) . . . . ?
C7 C3 C4 N10 -5.5(5) . . . . ?
N1 C3 C4 N7 -4.1(4) . . . . ?
C7 C3 C4 N7 173.2(3) . . . . ?
N1 C1 C5 N2 0.9(4) . . . . ?
C2 C1 C5 N2 179.8(2) . . . . ?
N1 C1 C5 C6 -178.6(2) . . . . ?
C2 C1 C5 C6 0.2(4) . . . . ?
N2 C5 C6 N11 1.1(4) . . . . ?
C1 C5 C6 N11 -179.3(3) . . . . ?
N2 C5 C6 N14 -178.7(3) . . . . ?
C1 C5 C6 N14 0.9(5) . . . . ?
N1 C3 C7 N2 1.2(4) . . . . ?
C4 C3 C7 N2 -175.9(2) . . . . ?
N1 C3 C7 C8 180.0(2) . . . . ?
C4 C3 C7 C8 2.9(4) . . . . ?
N2 C7 C8 N15 5.7(4) . . . . ?
C3 C7 C8 N15 -173.2(3) . . . . ?
N2 C7 C8 N18 -172.5(3) . . . . ?
C3 C7 C8 N18 8.6(4) . . . . ?
C7 C3 N1 C1 0.5(4) . . . . ?
C4 C3 N1 C1 178.0(2) . . . . ?
C7 C3 N1 Dy1 -176.91(17) . . . . ?
C4 C3 N1 Dy1 0.6(3) . . . . ?
C5 C1 N1 C3 -1.5(4) . . . . ?
C2 C1 N1 C3 179.4(2) . . . . ?
C5 C1 N1 Dy1 175.93(17) . . . . ?
C2 C1 N1 Dy1 -3.1(3) . . . . ?
C1 C5 N2 C7 0.7(4) . . . . ?
C6 C5 N2 C7 -179.6(2) . . . . ?
C3 C7 N2 C5 -1.8(4) . . . . ?
C8 C7 N2 C5 179.3(2) . . . . ?
N6 C2 N3 N4 0.9(3) . . . . ?
C1 C2 N3 N4 179.6(2) . . . . ?
N6 C2 N3 Dy1 -174.16(18) . . . . ?
C1 C2 N3 Dy1 4.6(4) . . . . ?
C2 N3 N4 N5 -0.7(3) . . . . ?
Dy1 N3 N4 N5 174.15(19) . . . . ?
N3 N4 N5 N6 0.3(3) . . . . ?
N3 C2 N6 N5 -0.7(3) . . . . ?
C1 C2 N6 N5 -179.4(3) . . . . ?
N4 N5 N6 C2 0.2(3) . . . . ?
N10 C4 N7 N8 0.2(3) . . . . ?
C3 C4 N7 N8 -178.7(2) . . . . ?
N10 C4 N7 Dy1 -174.89(18) . . . . ?
C3 C4 N7 Dy1 6.2(4) . . . . ?
C4 N7 N8 N9 -0.1(3) . . . . ?
Dy1 N7 N8 N9 174.8(2) . . . . ?
N7 N8 N9 N10 -0.1(4) . . . . ?
N7 C4 N10 N9 -0.3(3) . . . . ?
C3 C4 N10 N9 178.5(3) . . . . ?
N8 N9 N10 C4 0.2(3) . . . . ?
N14 C6 N11 N12 -0.7(3) . . . . ?
C5 C6 N11 N12 179.5(3) . . . . ?
C6 N11 N12 N13 0.6(3) . . . . ?
N11 N12 N13 N14 -0.3(3) . . . . ?
N12 N13 N14 C6 -0.1(3) . . . . ?
N11 C6 N14 N13 0.5(3) . . . . ?
C5 C6 N14 N13 -179.7(3) . . . . ?
N18 C8 N15 N16 0.0(3) . . . . ?
C7 C8 N15 N16 -178.5(2) . . . . ?
C8 N15 N16 N17 0.1(3) . . . . ?
N15 N16 N17 N18 -0.2(3) . . . . ?
N16 N17 N18 C8 0.3(3) . . . . ?
N15 C8 N18 N17 -0.2(3) . . . . ?
C7 C8 N18 N17 178.3(3) . . . . ?
N19 C9 C10 N21 0.4(10) . . . . ?
C13 C9 C10 N21 178.2(8) . . . . ?
N19 C9 C10 N24 179.2(7) . . . . ?
C13 C9 C10 N24 -3.0(12) . . . . ?
N19 C11 C12 N28 149.6(8) . . . . ?
C15 C11 C12 N28 -30.0(14) . . . . ?
N19 C11 C12 N25 -23.9(11) . . . . ?
C15 C11 C12 N25 156.4(8) . . . . ?
N19 C9 C13 N20 -2.8(11) . . . . ?
C10 C9 C13 N20 179.5(7) . . . . ?
N19 C9 C13 C14 175.8(8) . . . . ?
C10 C9 C13 C14 -1.9(12) . . . . ?
N20 C13 C14 N32 -163.9(9) . . . . ?
C9 C13 C14 N32 17.4(14) . . . . ?
N20 C13 C14 N29 15.7(11) . . . . ?
C9 C13 C14 N29 -163.0(8) . . . . ?
N19 C11 C15 N20 -3.1(12) . . . . ?
C12 C11 C15 N20 176.6(7) . . . . ?
N19 C11 C15 C16 175.8(7) . . . . ?
C12 C11 C15 C16 -4.5(13) . . . . ?
N20 C15 C16 N36 156.9(8) . . . . ?
C11 C15 C16 N36 -22.0(13) . . . . ?
N20 C15 C16 N33 -17.6(11) . . . . ?
C11 C15 C16 N33 163.5(8) . . . . ?
C13 C9 N19 C11 2.0(10) . . . . ?
C10 C9 N19 C11 180.0(7) . . . . ?
C15 C11 N19 C9 0.9(11) . . . . ?
C12 C11 N19 C9 -178.8(7) . . . . ?
C11 C15 N20 C13 2.2(12) . . . . ?
C16 C15 N20 C13 -176.8(7) . . . . ?
C9 C13 N20 C15 0.7(11) . . . . ?
C14 C13 N20 C15 -178.1(7) . . . . ?
N24 C10 N21 N22 0.6(8) . . . . ?
C9 C10 N21 N22 179.7(7) . . . . ?
C10 N21 N22 N23 -0.3(9) . . . . ?
N21 N22 N23 N24 -0.1(9) . . . . ?
N22 N23 N24 C10 0.5(9) . . . . ?
N21 C10 N24 N23 -0.7(9) . . . . ?
C9 C10 N24 N23 -179.7(7) . . . . ?
N28 C12 N25 N26 2.0(10) . . . . ?
C11 C12 N25 N26 176.7(8) . . . . ?
C12 N25 N26 N27 -1.2(10) . . . . ?
N25 N26 N27 N28 0.0(11) . . . . ?
N25 C12 N28 N27 -2.0(9) . . . . ?
C11 C12 N28 N27 -176.0(8) . . . . ?
N26 N27 N28 C12 1.2(10) . . . . ?
N32 C14 N29 N30 -0.2(10) . . . . ?
C13 C14 N29 N30 -179.9(8) . . . . ?
C14 N29 N30 N31 0.4(11) . . . . ?
N29 N30 N31 N32 -0.5(11) . . . . ?
N29 C14 N32 N31 -0.1(10) . . . . ?
C13 C14 N32 N31 179.6(8) . . . . ?
N30 N31 N32 C14 0.3(10) . . . . ?
N36 C16 N33 N34 3.1(10) . . . . ?
C15 C16 N33 N34 178.5(7) . . . . ?
C16 N33 N34 N35 -2.8(10) . . . . ?
N33 N34 N35 N36 1.5(10) . . . . ?
N33 C16 N36 N35 -2.2(9) . . . . ?
C15 C16 N36 N35 -177.2(7) . . . . ?
N34 N35 N36 C16 0.4(9) . . . . ?

_refine_diff_density_max         1.663
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_mm467
_database_code_depnum_ccdc_archive 'CCDC 1812513'
_audit_update_record             
;
2017-12-19 deposited with the CCDC.
2018-02-08 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         ?
_chemical_formula_sum            'C8.70 H14 Dy2 N18 O8.70'
_chemical_formula_weight         834.98

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      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                   6.5214(2)
_cell_length_b                   7.8070(2)
_cell_length_c                   10.6509(3)
_cell_angle_alpha                104.2559(12)
_cell_angle_beta                 97.5429(14)
_cell_angle_gamma                98.3219(15)
_cell_volume                     512.09(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    4956
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      28.31

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      n/a
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.708
_exptl_crystal_F_000             394
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    7.332
_shelx_estimated_absorpt_T_min   0.252
_shelx_estimated_absorpt_T_max   0.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5233
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(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            5663
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.003
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             2479
_reflns_number_gt                2408
_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       'APEX II, Bruker (2009)'
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_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)+(0.0154P)²+3.1905P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2479
_refine_ls_number_parameters     191
_refine_ls_number_restraints     339
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0565
_refine_ls_wR_factor_gt          0.0559
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.052
_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
Dy1 Dy 0.59348(3) 0.62407(2) 0.68425(2) 0.01827(7) Uani 1 1 d . U . . .
O1 O 0.8244(5) 0.8765(4) 0.6774(3) 0.0268(7) Uani 1 1 d . U . . .
H1A H 0.8915 0.9804 0.7451 0.040 Uiso 1 1 d R U . . .
H1B H 0.8196 0.9017 0.5895 0.040 Uiso 1 1 d R U . . .
O2 O 0.3578(5) 0.4968(4) 0.8038(3) 0.0269(7) Uani 1 1 d . U . . .
H2A H 0.2555 0.5603 0.8414 0.040 Uiso 1 1 d R U . . .
H2B H 0.3036 0.3647 0.7770 0.040 Uiso 1 1 d R U . . .
O3 O 0.7089(6) 0.3606(5) 0.7023(3) 0.0375(9) Uani 1 1 d . U . . .
H3A H 0.7264 0.3203 0.7798 0.056 Uiso 1 1 d R U . . .
H3B H 0.7044 0.2592 0.6228 0.056 Uiso 1 1 d R U . . .
O4 O 0.664(2) 0.562(2) 0.4836(12) 0.029(2) Uani 0.65 1 d . U P A 1
H4A H 0.7967 0.6096 0.4662 0.23(15) Uiso 0.65 1 calc R . P A 1
N1 N 0.5520(5) 0.8907(4) 0.8918(3) 0.0144(6) Uani 1 1 d . U . . .
N2 N 0.8587(5) 0.6962(4) 0.8994(3) 0.0169(6) Uani 1 1 d . U . . .
N3 N 1.0474(6) 0.6534(5) 0.9288(3) 0.0206(7) Uani 1 1 d . U . . .
N4 N 1.1280(5) 0.7364(5) 1.0525(3) 0.0199(7) Uani 1 1 d . U . . .
N5 N 0.9952(5) 0.8354(5) 1.1068(3) 0.0173(6) Uani 1 1 d . U . . .
N6 N 0.6487(6) 1.1633(5) 1.3543(3) 0.0211(7) Uani 1 1 d . U . . .
N7 N 0.7129(6) 1.1242(5) 1.4672(3) 0.0230(7) Uani 1 1 d . U . . .
N8 N 0.7634(6) 0.9649(5) 1.4414(3) 0.0207(7) Uani 1 1 d . U . . .
N9 N 0.7348(6) 0.8933(5) 1.3106(3) 0.0182(6) Uani 1 1 d . U . . .
C1 C 0.6501(6) 0.9000(5) 1.0119(3) 0.0130(6) Uani 1 1 d . U . . .
C2 C 0.8320(6) 0.8063(5) 1.0106(3) 0.0147(7) Uani 1 1 d . U . . .
C3 C 0.5925(6) 1.0093(5) 1.1231(3) 0.0127(6) Uani 1 1 d . U . . .
C4 C 0.6671(6) 1.0192(5) 1.2606(3) 0.0150(7) Uani 1 1 d . U . . .
O4' O 0.697(6) 0.550(5) 0.467(3) 0.040(4) Uani 0.35 1 d . U P A -2
C5 C 0.872(3) 0.546(3) 0.4870(18) 0.050(3) Uani 0.35 1 d . U P A -2
H5A H 0.9513 0.5360 0.4177 0.060 Uiso 0.35 1 calc R U P A -2
O5 O 0.965(2) 0.5564(19) 0.6089(13) 0.055(3) Uani 0.35 1 d . U P 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 O4 2.198(10) . ?
Dy1 O4 2.313(16) 2_666 ?
Dy1 O1 2.323(3) . ?
Dy1 O3 2.333(3) . ?
Dy1 O2 2.380(3) . ?
Dy1 O4' 2.45(2) . ?
Dy1 N6 2.519(3) 2_677 ?
Dy1 N2 2.569(3) . ?
Dy1 N1 2.711(3) . ?
Dy1 O5 2.731(14) . ?
Dy1 C5 2.96(2) . ?
Dy1 Dy1 3.8678(4) 2_666 ?
O4 Dy1 2.313(16) 2_666 ?
N1 C3 1.326(5) 2_677 ?
N1 C1 1.333(5) . ?
N2 C2 1.330(5) . ?
N2 N3 1.339(5) . ?
N3 N4 1.316(5) . ?
N4 N5 1.337(5) . ?
N5 C2 1.328(5) . ?
N6 C4 1.338(5) . ?
N6 N7 1.342(5) . ?
N6 Dy1 2.519(3) 2_677 ?
N7 N8 1.306(5) . ?
N8 N9 1.344(4) . ?
N9 C4 1.329(5) . ?
C1 C3 1.408(5) . ?
C1 C2 1.481(5) . ?
C3 N1 1.326(5) 2_677 ?
C3 C4 1.461(5) . ?
O4' C5 1.14(4) . ?
C5 O5 1.34(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
O4 Dy1 O4 62.0(6) . 2_666 ?
O4 Dy1 O1 75.0(5) . . ?
O4 Dy1 O1 127.7(4) 2_666 . ?
O4 Dy1 O3 87.0(4) . . ?
O4 Dy1 O3 85.6(4) 2_666 . ?
O1 Dy1 O3 121.87(14) . . ?
O4 Dy1 O2 137.7(5) . . ?
O4 Dy1 O2 78.2(3) 2_666 . ?
O1 Dy1 O2 146.53(11) . . ?
O3 Dy1 O2 75.52(13) . . ?
O1 Dy1 O4' 74.2(8) . . ?
O3 Dy1 O4' 84.1(8) . . ?
O2 Dy1 O4' 139.0(8) . . ?
O4 Dy1 N6 94.9(4) . 2_677 ?
O4 Dy1 N6 78.4(4) 2_666 2_677 ?
O1 Dy1 N6 77.10(13) . 2_677 ?
O3 Dy1 N6 160.58(14) . 2_677 ?
O2 Dy1 N6 90.41(12) . 2_677 ?
O4' Dy1 N6 98.7(9) . 2_677 ?
O4 Dy1 N2 126.7(4) . . ?
O4 Dy1 N2 154.0(4) 2_666 . ?
O1 Dy1 N2 76.50(11) . . ?
O3 Dy1 N2 71.49(11) . . ?
O2 Dy1 N2 84.08(11) . . ?
O4' Dy1 N2 122.7(9) . . ?
N6 Dy1 N2 121.03(10) 2_677 . ?
O4 Dy1 N1 144.9(4) . . ?
O4 Dy1 N1 128.9(3) 2_666 . ?
O1 Dy1 N1 74.50(10) . . ?
O3 Dy1 N1 124.25(11) . . ?
O2 Dy1 N1 72.27(10) . . ?
O4' Dy1 N1 146.0(8) . . ?
N6 Dy1 N1 61.41(10) 2_677 . ?
N2 Dy1 N1 61.07(10) . . ?
O1 Dy1 O5 65.3(3) . . ?
O3 Dy1 O5 60.2(3) . . ?
O2 Dy1 O5 134.9(3) . . ?
O4' Dy1 O5 48.4(9) . . ?
N6 Dy1 O5 134.7(3) 2_677 . ?
N2 Dy1 O5 74.7(3) . . ?
N1 Dy1 O5 125.6(3) . . ?
O1 Dy1 C5 66.5(4) . . ?
O3 Dy1 C5 73.6(4) . . ?
O2 Dy1 C5 145.2(4) . . ?
O4' Dy1 C5 21.8(9) . . ?
N6 Dy1 C5 114.8(5) 2_677 . ?
N2 Dy1 C5 100.9(4) . . ?
N1 Dy1 C5 140.2(4) . . ?
O5 Dy1 C5 26.8(5) . . ?
O4 Dy1 Dy1 31.9(4) . 2_666 ?
O4 Dy1 Dy1 30.1(3) 2_666 2_666 ?
O1 Dy1 Dy1 102.63(7) . 2_666 ?
O3 Dy1 Dy1 85.66(8) . 2_666 ?
O2 Dy1 Dy1 107.35(8) . 2_666 ?
O4' Dy1 Dy1 34.9(9) . 2_666 ?
N6 Dy1 Dy1 85.88(7) 2_677 2_666 ?
N2 Dy1 Dy1 151.26(7) . 2_666 ?
N1 Dy1 Dy1 147.14(7) . 2_666 ?
O5 Dy1 Dy1 78.9(3) . 2_666 ?
C5 Dy1 Dy1 54.7(4) . 2_666 ?
Dy1 O4 Dy1 118.0(6) . 2_666 ?
C3 N1 C1 120.0(3) 2_677 . ?
C3 N1 Dy1 119.5(2) 2_677 . ?
C1 N1 Dy1 119.5(2) . . ?
C2 N2 N3 104.5(3) . . ?
C2 N2 Dy1 122.4(3) . . ?
N3 N2 Dy1 133.0(2) . . ?
N4 N3 N2 109.1(3) . . ?
N3 N4 N5 109.8(3) . . ?
C2 N5 N4 104.2(3) . . ?
C4 N6 N7 104.2(3) . . ?
C4 N6 Dy1 123.1(3) . 2_677 ?
N7 N6 Dy1 128.0(3) . 2_677 ?
N8 N7 N6 109.6(3) . . ?
N7 N8 N9 109.9(3) . . ?
C4 N9 N8 104.1(3) . . ?
N1 C1 C3 119.9(3) . . ?
N1 C1 C2 113.2(3) . . ?
C3 C1 C2 126.5(3) . . ?
N5 C2 N2 112.4(3) . . ?
N5 C2 C1 127.0(3) . . ?
N2 C2 C1 120.0(3) . . ?
N1 C3 C1 120.1(3) 2_677 . ?
N1 C3 C4 113.1(3) 2_677 . ?
C1 C3 C4 126.7(3) . . ?
N9 C4 N6 112.2(3) . . ?
N9 C4 C3 128.5(3) . . ?
N6 C4 C3 119.0(3) . . ?
C5 O4' Dy1 105(2) . . ?
O4' C5 O5 119(2) . . ?
O4' C5 Dy1 52.9(16) . . ?
O5 C5 Dy1 67.0(10) . . ?
C5 O5 Dy1 86.3(12) . . ?

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 N2 N3 N4 -0.3(4) . . . . ?
Dy1 N2 N3 N4 174.9(3) . . . . ?
N2 N3 N4 N5 -0.1(4) . . . . ?
N3 N4 N5 C2 0.5(4) . . . . ?
C4 N6 N7 N8 -0.9(5) . . . . ?
Dy1 N6 N7 N8 154.9(3) 2_677 . . . ?
N6 N7 N8 N9 0.1(5) . . . . ?
N7 N8 N9 C4 0.7(5) . . . . ?
C3 N1 C1 C3 3.2(6) 2_677 . . . ?
Dy1 N1 C1 C3 -165.2(3) . . . . ?
C3 N1 C1 C2 -169.6(3) 2_677 . . . ?
Dy1 N1 C1 C2 22.0(4) . . . . ?
N4 N5 C2 N2 -0.8(4) . . . . ?
N4 N5 C2 C1 -171.9(4) . . . . ?
N3 N2 C2 N5 0.7(4) . . . . ?
Dy1 N2 C2 N5 -175.1(3) . . . . ?
N3 N2 C2 C1 172.6(3) . . . . ?
Dy1 N2 C2 C1 -3.3(5) . . . . ?
N1 C1 C2 N5 157.7(4) . . . . ?
C3 C1 C2 N5 -14.5(6) . . . . ?
N1 C1 C2 N2 -12.9(5) . . . . ?
C3 C1 C2 N2 174.9(4) . . . . ?
N1 C1 C3 N1 -3.2(6) . . . 2_677 ?
C2 C1 C3 N1 168.5(4) . . . 2_677 ?
N1 C1 C3 C4 172.8(4) . . . . ?
C2 C1 C3 C4 -15.5(6) . . . . ?
N8 N9 C4 N6 -1.3(5) . . . . ?
N8 N9 C4 C3 -174.0(4) . . . . ?
N7 N6 C4 N9 1.3(5) . . . . ?
Dy1 N6 C4 N9 -155.9(3) 2_677 . . . ?
N7 N6 C4 C3 174.8(4) . . . . ?
Dy1 N6 C4 C3 17.6(5) 2_677 . . . ?
N1 C3 C4 N9 148.9(4) 2_677 . . . ?
C1 C3 C4 N9 -27.2(7) . . . . ?
N1 C3 C4 N6 -23.3(5) 2_677 . . . ?
C1 C3 C4 N6 160.5(4) . . . . ?
Dy1 O4' C5 O5 9(3) . . . . ?
O4' C5 O5 Dy1 -7(3) . . . . ?

_refine_diff_density_max         3.948
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.149

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1812512'
_audit_update_record             
;
2017-12-19 deposited with the CCDC.
2018-02-08 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         ?
_chemical_formula_sum            'C12 H27 Gd N27 O12'
_chemical_formula_weight         898.85

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'
Gd Gd -0.1653 3.9035 '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                   9.8069(5)
_cell_length_b                   11.2059(6)
_cell_length_c                   14.4149(7)
_cell_angle_alpha                101.7440(10)
_cell_angle_beta                 97.8160(10)
_cell_angle_gamma                93.9320(10)
_cell_volume                     1528.97(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9848
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      28.33
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.273
_shelx_estimated_absorpt_T_min   0.539
_shelx_estimated_absorpt_T_max   0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5945
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(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            14787
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0121
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.865
_diffrn_reflns_theta_max         28.331
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7516
_reflns_number_gt                7166
_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       'APEX II (Bruker, 2009)'
_computing_cell_refinement       'APEX II (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker)'
_computing_structure_solution    'XT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.0217P)²+0.7587P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7516
_refine_ls_number_parameters     695
_refine_ls_number_restraints     592
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0173
_refine_ls_wR_factor_ref         0.0429
_refine_ls_wR_factor_gt          0.0424
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.003
_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
Gd1 Gd 0.43010(2) 0.17350(2) 0.84314(2) 0.01688(3) Uani 1 1 d . . . . .
C1 C 0.33901(15) 0.11909(13) 0.58154(11) 0.0152(3) Uani 1 1 d D U . . .
C2 C 0.33647(16) 0.25019(14) 0.62288(12) 0.0165(3) Uani 1 1 d D U . . .
C3 C 0.37387(16) -0.06853(14) 0.62206(11) 0.0152(3) Uani 1 1 d D U . . .
C4 C 0.41239(16) -0.12460(14) 0.70391(11) 0.0168(3) Uani 1 1 d D U . . .
C5 C 0.31639(16) 0.06011(14) 0.48307(11) 0.0156(3) Uani 1 1 d D U . . .
C6 C 0.28554(16) 0.11666(15) 0.39987(12) 0.0181(3) Uani 1 1 d D U . . .
C7 C 0.34911(15) -0.12657(13) 0.52398(11) 0.0149(3) Uani 1 1 d D U . . .
C8 C 0.35050(16) -0.25826(14) 0.48055(11) 0.0158(3) Uani 1 1 d D U . . .
N1 N 0.36832(14) 0.05291(12) 0.64777(10) 0.0161(3) Uani 1 1 d D U . . .
N2 N 0.32280(14) -0.06040(12) 0.45759(10) 0.0164(3) Uani 1 1 d D U . . .
N3 N 0.35986(16) 0.29364(12) 0.71729(11) 0.0218(3) Uani 1 1 d D U . . .
N4 N 0.35074(18) 0.41512(13) 0.72861(11) 0.0261(3) Uani 1 1 d D U . . .
N5 N 0.32392(16) 0.44273(13) 0.64451(11) 0.0237(3) Uani 1 1 d D U . . .
N6 N 0.31479(15) 0.33967(12) 0.57631(10) 0.0198(3) Uani 1 1 d D U . . .
N7 N 0.44633(15) -0.05608(12) 0.79264(10) 0.0192(3) Uani 1 1 d D U . . .
N8 N 0.47806(18) -0.13569(13) 0.84789(11) 0.0257(3) Uani 1 1 d D U . . .
N9 N 0.46405(19) -0.24707(14) 0.79483(11) 0.0283(3) Uani 1 1 d D U . . .
N10 N 0.42202(17) -0.24292(13) 0.70320(11) 0.0230(3) Uani 1 1 d D U . . .
N11 N 0.26407(16) 0.05286(14) 0.30949(11) 0.0244(3) Uani 1 1 d D U . . .
N12 N 0.23866(18) 0.13537(15) 0.25452(11) 0.0290(3) Uani 1 1 d D U . . .
N13 N 0.24449(18) 0.24540(15) 0.30722(11) 0.0284(3) Uani 1 1 d D U . . .
N14 N 0.27432(16) 0.23455(13) 0.39820(11) 0.0225(3) Uani 1 1 d D U . . .
H14A H 0.2849 0.2952 0.4489 0.027 Uiso 1 1 calc R U . . .
N15 N 0.33885(15) -0.30007(12) 0.38641(10) 0.0200(3) Uani 1 1 d D U . . .
N16 N 0.34031(16) -0.42287(13) 0.37334(11) 0.0227(3) Uani 1 1 d D U . . .
N17 N 0.35201(16) -0.45683(13) 0.45450(11) 0.0234(3) Uani 1 1 d D U . . .
N18 N 0.35885(15) -0.35422(12) 0.52232(10) 0.0198(3) Uani 1 1 d D U . . .
H18A H 0.3674 -0.3506 0.5844 0.024 Uiso 1 1 calc R U . . .
C9 C 1.0218(5) 0.5654(4) 0.5665(3) 0.0198(9) Uani 0.5 1 d D U P A -1
C10 C 1.0539(4) 0.6632(4) 0.6530(4) 0.0190(8) Uani 0.5 1 d D U P A -1
C11 C 0.9982(6) 0.5283(4) 0.4002(4) 0.0205(9) Uani 0.5 1 d D U P A -1
C12 C 1.0100(5) 0.5895(4) 0.3206(5) 0.0206(10) Uani 0.5 1 d D U P A -1
C13 C 0.9943(4) 0.4389(5) 0.5613(4) 0.0172(9) Uani 0.5 1 d D U P A -1
C14 C 0.9949(5) 0.3773(4) 0.6420(4) 0.0228(10) Uani 0.5 1 d D U P A -1
C15 C 0.9631(5) 0.4027(4) 0.3951(4) 0.0182(8) Uani 0.5 1 d D U P A -1
C16 C 0.9225(5) 0.3092(4) 0.3066(4) 0.0217(9) Uani 0.5 1 d D U P A -1
N19 N 1.0245(4) 0.6060(4) 0.4856(4) 0.0187(9) Uani 0.5 1 d D U P A -1
N20 N 0.9641(5) 0.3615(4) 0.4761(3) 0.0205(8) Uani 0.5 1 d D U P A -1
N21 N 1.0814(4) 0.7808(4) 0.6499(3) 0.0256(9) Uani 0.5 1 d D U P A -1
N22 N 1.1048(5) 0.8406(4) 0.7428(4) 0.0270(10) Uani 0.5 1 d D U P A -1
N23 N 1.0920(4) 0.7657(3) 0.8005(3) 0.0309(8) Uani 0.5 1 d D U P A -1
N24 N 1.0584(4) 0.6544(3) 0.7441(3) 0.0272(7) Uani 0.5 1 d D U P A -1
N25 N 0.9955(5) 0.7076(4) 0.3286(3) 0.0273(9) Uani 0.5 1 d D U P A -1
H25 H 0.9738 0.7574 0.3788 0.033 Uiso 0.5 1 calc R U P A -1
N26 N 1.0195(6) 0.7379(6) 0.2467(4) 0.0320(11) Uani 0.5 1 d D U P A -1
N27 N 1.0497(5) 0.6393(4) 0.1912(3) 0.0316(9) Uani 0.5 1 d D U P A -1
N28 N 1.0449(5) 0.5445(4) 0.2349(3) 0.0282(9) Uani 0.5 1 d D U P A -1
N29 N 1.0002(5) 0.2566(4) 0.6315(3) 0.0286(9) Uani 0.5 1 d D U P A -1
N30 N 0.9983(6) 0.2347(5) 0.7195(4) 0.0315(11) Uani 0.5 1 d D U P A -1
N31 N 0.9925(5) 0.3362(5) 0.7813(4) 0.0326(9) Uani 0.5 1 d D U P A -1
N32 N 0.9899(5) 0.4282(4) 0.7334(4) 0.0288(9) Uani 0.5 1 d D U P A -1
H32 H 0.9858 0.5063 0.7578 0.035 Uiso 0.5 1 calc R U P A -1
N33 N 0.9263(5) 0.1906(4) 0.3080(4) 0.0252(9) Uani 0.5 1 d D U P A -1
N34 N 0.8781(6) 0.1323(4) 0.2176(3) 0.0282(10) Uani 0.5 1 d D U P A -1
N35 N 0.8424(5) 0.2108(3) 0.1654(3) 0.0300(7) Uani 0.5 1 d D U P A -1
N36 N 0.8694(4) 0.3244(3) 0.2207(3) 0.0297(7) Uani 0.5 1 d D U P A -1
O1 O 0.63032(14) 0.17027(12) 0.76152(9) 0.0239(3) Uani 1 1 d D . . . .
H1A H 0.667(2) 0.1089(16) 0.7466(17) 0.036 Uiso 1 1 d D U . . .
H1B H 0.642(3) 0.2115(18) 0.7231(16) 0.036 Uiso 1 1 d D U . . .
O2 O 0.55316(17) 0.37315(12) 0.90185(11) 0.0340(3) Uani 1 1 d D . . . .
H2A H 0.575(3) 0.425(2) 0.8752(17) 0.051 Uiso 1 1 d D U . . .
H2B H 0.591(3) 0.388(2) 0.9548(13) 0.051 Uiso 1 1 d D U . . .
O3 O 0.63092(14) 0.15224(13) 0.95395(10) 0.0278(3) Uani 1 1 d D . . . .
H3A H 0.707(2) 0.189(2) 0.9548(18) 0.042 Uiso 1 1 d D U . . .
H3B H 0.638(3) 0.124(2) 0.9999(15) 0.042 Uiso 1 1 d D U . . .
O4 O 0.2852(2) 0.31327(14) 0.92416(13) 0.0445(4) Uani 1 1 d D . . . .
H4A H 0.283(3) 0.3862(17) 0.924(2) 0.067 Uiso 1 1 d D U . . .
H4B H 0.229(3) 0.296(3) 0.954(2) 0.067 Uiso 1 1 d D U . . .
O5 O 0.36187(14) 0.08585(13) 0.97149(9) 0.0256(3) Uani 1 1 d D . . . .
H5A H 0.2815(16) 0.081(2) 0.9816(17) 0.038 Uiso 1 1 d D U . . .
H5B H 0.412(2) 0.098(2) 1.0242(14) 0.038 Uiso 1 1 d D U . . .
O6 O 0.19089(14) 0.09519(13) 0.79616(11) 0.0295(3) Uani 1 1 d D . . . .
H6A H 0.165(3) 0.0240(15) 0.790(2) 0.044 Uiso 1 1 d D U . . .
H6B H 0.130(2) 0.1352(19) 0.784(2) 0.044 Uiso 1 1 d D U . . .
O7 O 0.64551(18) 0.55855(13) 0.82127(11) 0.0371(3) Uani 1 1 d D . . . .
H7A H 0.659(3) 0.526(2) 0.7669(15) 0.056 Uiso 1 1 d D U . . .
H7B H 0.589(3) 0.608(2) 0.816(2) 0.056 Uiso 1 1 d D U . . .
O8 O 0.30695(18) 0.55398(15) 0.91490(12) 0.0402(4) Uani 1 1 d D . . . .
H8A H 0.239(2) 0.588(3) 0.923(2) 0.060 Uiso 1 1 d D U . . .
H8B H 0.322(3) 0.539(3) 0.8616(15) 0.060 Uiso 1 1 d D U . . .
O9 O 0.1249(4) 0.1003(5) 1.0528(3) 0.0390(7) Uani 0.536(5) 1 d D . P B 1
H9A H 0.148(6) 0.089(5) 1.107(2) 0.059 Uiso 0.536(5) 1 d D U P B 1
H9B H 0.128(7) 0.174(2) 1.060(4) 0.059 Uiso 0.536(5) 1 d D U P B 1
O10 O 0.8625(3) 0.3067(3) 0.9775(2) 0.0479(6) Uani 0.633(3) 1 d D . P C 1
H10A H 0.870(5) 0.333(5) 0.928(2) 0.072 Uiso 0.633(3) 1 d D U P C 1
H10B H 0.938(2) 0.281(2) 0.9874(17) 0.072 Uiso 1 1 d D U . . .
O11 O 0.0989(4) 0.3470(4) 1.0872(3) 0.0429(6) Uani 0.498(3) 1 d D . P D 1
H11A H 0.059(5) 0.395(4) 1.124(4) 0.064 Uiso 0.498(3) 1 d D U P D 1
H11B H 0.174(3) 0.387(5) 1.091(4) 0.064 Uiso 0.498(3) 1 d D U P D 1
O12 O 0.9881(4) 0.9119(3) 0.5349(3) 0.0359(5) Uani 0.477(3) 1 d D . P E 1
H12A H 1.034(5) 0.896(6) 0.583(2) 0.054 Uiso 0.477(3) 1 d D U P E 1
H12B H 1.030(6) 0.875(6) 0.492(3) 0.054 Uiso 0.477(3) 1 d D U P E 1
O9' O 0.1169(5) 0.0413(5) 1.0376(4) 0.0390(7) Uani 0.464(5) 1 d D . P B 2
H9C H 0.131(6) 0.010(5) 1.084(3) 0.059 Uiso 0.464(5) 1 d D U P B 2
H9D H 0.057(4) -0.003(5) 0.998(3) 0.059 Uiso 0.464(5) 1 d D U P B 2
O10' O 0.8889(5) 0.2350(5) 0.9333(4) 0.0479(6) Uani 0.367(3) 1 d D . P C 2
H10D H 0.868(9) 0.289(4) 0.904(4) 0.072 Uiso 0.367(3) 1 d D U P C 2
O11' O 0.1285(4) 0.2897(4) 1.0572(3) 0.0429(6) Uani 0.502(3) 1 d D . P D 2
H11C H 0.107(7) 0.221(3) 1.067(4) 0.064 Uiso 0.502(3) 1 d D U P D 2
H11D H 0.184(6) 0.328(5) 1.103(3) 0.064 Uiso 0.502(3) 1 d D U P D 2
O12' O 0.9674(4) 0.8645(3) 0.4803(3) 0.0359(5) Uani 0.523(3) 1 d D . P E 2
H12C H 1.006(6) 0.849(5) 0.531(3) 0.054 Uiso 0.523(3) 1 d D U P E 2
H12D H 0.989(6) 0.936(2) 0.480(4) 0.054 Uiso 0.523(3) 1 d D U P E 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
Gd1 O2 2.3998(14) . ?
Gd1 O6 2.4033(14) . ?
Gd1 O5 2.4129(13) . ?
Gd1 O4 2.4180(14) . ?
Gd1 O3 2.4188(13) . ?
Gd1 O1 2.4211(13) . ?
Gd1 N3 2.5217(14) . ?
Gd1 N7 2.5494(13) . ?
Gd1 N1 2.8282(14) . ?
C1 N1 1.337(2) . ?
C1 C5 1.419(2) . ?
C1 C2 1.472(2) . ?
C2 N6 1.329(2) . ?
C2 N3 1.331(2) . ?
C3 N1 1.3425(19) . ?
C3 C7 1.411(2) . ?
C3 C4 1.464(2) . ?
C4 N10 1.334(2) . ?
C4 N7 1.336(2) . ?
C5 N2 1.334(2) . ?
C5 C6 1.473(2) . ?
C6 N11 1.334(2) . ?
C6 N14 1.338(2) . ?
C7 N2 1.334(2) . ?
C7 C8 1.483(2) . ?
C8 N15 1.329(2) . ?
C8 N18 1.337(2) . ?
N3 N4 1.3483(19) . ?
N4 N5 1.308(2) . ?
N5 N6 1.3447(19) . ?
N7 N8 1.3368(19) . ?
N8 N9 1.312(2) . ?
N9 N10 1.340(2) . ?
N11 N12 1.349(2) . ?
N12 N13 1.303(2) . ?
N13 N14 1.336(2) . ?
N14 H14A 0.8800 . ?
N15 N16 1.3517(19) . ?
N16 N17 1.295(2) . ?
N17 N18 1.3404(19) . ?
N18 H18A 0.8800 . ?
C9 N19 1.337(6) . ?
C9 C13 1.409(6) . ?
C9 C10 1.464(6) . ?
C10 N24 1.332(6) . ?
C10 N21 1.337(6) . ?
C11 N19 1.336(5) . ?
C11 C15 1.410(6) . ?
C11 C12 1.465(7) . ?
C12 N25 1.324(6) . ?
C12 N28 1.335(6) . ?
C13 N20 1.334(6) . ?
C13 C14 1.469(6) . ?
C14 N32 1.335(6) . ?
C14 N29 1.335(6) . ?
C15 N20 1.341(6) . ?
C15 C16 1.463(6) . ?
C16 N36 1.326(6) . ?
C16 N33 1.337(6) . ?
N21 N22 1.350(6) . ?
N22 N23 1.309(6) . ?
N23 N24 1.336(5) . ?
N25 N26 1.338(6) . ?
N25 H25 0.8800 . ?
N26 N27 1.303(6) . ?
N27 N28 1.342(6) . ?
N29 N30 1.342(6) . ?
N30 N31 1.304(6) . ?
N31 N32 1.352(6) . ?
N32 H32 0.8800 . ?
N33 N34 1.339(5) . ?
N34 N35 1.305(6) . ?
N35 N36 1.345(5) . ?
O1 H1A 0.804(15) . ?
O1 H1B 0.805(16) . ?
O2 H2A 0.789(16) . ?
O2 H2B 0.783(16) . ?
O3 H3A 0.822(16) . ?
O3 H3B 0.786(16) . ?
O4 H4A 0.820(17) . ?
O4 H4B 0.777(17) . ?
O5 H5A 0.821(16) . ?
O5 H5B 0.826(16) . ?
O6 H6A 0.805(16) . ?
O6 H6B 0.794(16) . ?
O7 H7A 0.826(17) . ?
O7 H7B 0.813(16) . ?
O8 H8A 0.800(17) . ?
O8 H8B 0.790(17) . ?
O9 H9A 0.821(19) . ?
O9 H9B 0.808(19) . ?
O10 H10A 0.842(19) . ?
O10 H10B 0.813(18) . ?
O11 H11A 0.832(19) . ?
O11 H11B 0.83(2) . ?
O12 H12A 0.83(2) . ?
O12 H12B 0.84(2) . ?
O9' H9C 0.82(2) . ?
O9' H9D 0.82(2) . ?
O10' H10B 0.898(18) . ?
O10' H10D 0.83(2) . ?
O11' H11C 0.83(2) . ?
O11' H11D 0.82(2) . ?
O12' H12C 0.83(2) . ?
O12' H12D 0.814(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
O2 Gd1 O6 135.23(5) . . ?
O2 Gd1 O5 111.85(5) . . ?
O6 Gd1 O5 72.91(5) . . ?
O2 Gd1 O4 69.46(6) . . ?
O6 Gd1 O4 69.87(6) . . ?
O5 Gd1 O4 73.51(5) . . ?
O2 Gd1 O3 72.58(5) . . ?
O6 Gd1 O3 140.25(5) . . ?
O5 Gd1 O3 69.41(5) . . ?
O4 Gd1 O3 109.96(6) . . ?
O2 Gd1 O1 75.00(5) . . ?
O6 Gd1 O1 134.46(5) . . ?
O5 Gd1 O1 135.22(5) . . ?
O4 Gd1 O1 141.63(5) . . ?
O3 Gd1 O1 71.31(5) . . ?
O2 Gd1 N3 74.56(5) . . ?
O6 Gd1 N3 79.95(5) . . ?
O5 Gd1 N3 146.33(5) . . ?
O4 Gd1 N3 78.74(6) . . ?
O3 Gd1 N3 139.79(5) . . ?
O1 Gd1 N3 78.35(5) . . ?
O2 Gd1 N7 146.73(5) . . ?
O6 Gd1 N7 78.03(5) . . ?
O5 Gd1 N7 74.12(5) . . ?
O4 Gd1 N7 139.62(5) . . ?
O3 Gd1 N7 79.96(5) . . ?
O1 Gd1 N7 78.72(4) . . ?
N3 Gd1 N7 119.53(4) . . ?
O2 Gd1 N1 124.93(5) . . ?
O6 Gd1 N1 67.36(4) . . ?
O5 Gd1 N1 123.22(4) . . ?
O4 Gd1 N1 124.17(6) . . ?
O3 Gd1 N1 125.87(4) . . ?
O1 Gd1 N1 67.11(4) . . ?
N3 Gd1 N1 60.07(4) . . ?
N7 Gd1 N1 59.46(4) . . ?
N1 C1 C5 119.31(14) . . ?
N1 C1 C2 113.16(13) . . ?
C5 C1 C2 127.52(14) . . ?
N6 C2 N3 111.00(14) . . ?
N6 C2 C1 127.68(15) . . ?
N3 C2 C1 121.31(14) . . ?
N1 C3 C7 119.51(14) . . ?
N1 C3 C4 112.93(13) . . ?
C7 C3 C4 127.51(14) . . ?
N10 C4 N7 111.16(14) . . ?
N10 C4 C3 127.84(15) . . ?
N7 C4 C3 120.98(14) . . ?
N2 C5 C1 119.92(14) . . ?
N2 C5 C6 112.52(14) . . ?
C1 C5 C6 127.56(14) . . ?
N11 C6 N14 107.94(15) . . ?
N11 C6 C5 123.12(14) . . ?
N14 C6 C5 128.94(15) . . ?
N2 C7 C3 119.94(14) . . ?
N2 C7 C8 111.92(13) . . ?
C3 C7 C8 128.13(14) . . ?
N15 C8 N18 107.81(14) . . ?
N15 C8 C7 122.33(14) . . ?
N18 C8 C7 129.84(15) . . ?
C1 N1 C3 120.72(14) . . ?
C1 N1 Gd1 119.09(10) . . ?
C3 N1 Gd1 120.14(10) . . ?
C5 N2 C7 120.59(14) . . ?
C2 N3 N4 104.99(13) . . ?
C2 N3 Gd1 126.12(10) . . ?
N4 N3 Gd1 128.61(11) . . ?
N5 N4 N3 109.54(14) . . ?
N4 N5 N6 108.78(13) . . ?
C2 N6 N5 105.69(14) . . ?
N8 N7 C4 104.89(13) . . ?
N8 N7 Gd1 128.64(10) . . ?
C4 N7 Gd1 126.25(10) . . ?
N9 N8 N7 109.68(14) . . ?
N8 N9 N10 109.20(14) . . ?
C4 N10 N9 105.08(14) . . ?
C6 N11 N12 105.73(14) . . ?
N13 N12 N11 110.96(15) . . ?
N12 N13 N14 106.28(14) . . ?
N13 N14 C6 109.08(15) . . ?
N13 N14 H14A 125.5 . . ?
C6 N14 H14A 125.5 . . ?
C8 N15 N16 105.84(13) . . ?
N17 N16 N15 111.08(14) . . ?
N16 N17 N18 106.14(13) . . ?
C8 N18 N17 109.12(14) . . ?
C8 N18 H18A 125.4 . . ?
N17 N18 H18A 125.4 . . ?
N19 C9 C13 119.4(4) . . ?
N19 C9 C10 113.1(4) . . ?
C13 C9 C10 127.5(4) . . ?
N24 C10 N21 108.9(5) . . ?
N24 C10 C9 128.3(4) . . ?
N21 C10 C9 122.7(4) . . ?
N19 C11 C15 119.7(5) . . ?
N19 C11 C12 112.6(4) . . ?
C15 C11 C12 127.7(5) . . ?
N25 C12 N28 109.1(4) . . ?
N25 C12 C11 121.9(5) . . ?
N28 C12 C11 128.9(4) . . ?
N20 C13 C9 120.1(4) . . ?
N20 C13 C14 112.9(4) . . ?
C9 C13 C14 127.0(5) . . ?
N32 C14 N29 110.0(4) . . ?
N32 C14 C13 127.5(5) . . ?
N29 C14 C13 122.5(5) . . ?
N20 C15 C11 119.5(5) . . ?
N20 C15 C16 115.0(4) . . ?
C11 C15 C16 125.5(4) . . ?
N36 C16 N33 111.4(4) . . ?
N36 C16 C15 128.1(4) . . ?
N33 C16 C15 120.3(5) . . ?
C11 N19 C9 120.7(4) . . ?
C13 N20 C15 120.4(4) . . ?
C10 N21 N22 104.6(4) . . ?
N23 N22 N21 111.7(4) . . ?
N22 N23 N24 105.8(4) . . ?
C10 N24 N23 109.0(4) . . ?
C12 N25 N26 107.9(4) . . ?
C12 N25 H25 126.1 . . ?
N26 N25 H25 126.1 . . ?
N27 N26 N25 107.2(5) . . ?
N26 N27 N28 110.4(4) . . ?
C12 N28 N27 105.4(4) . . ?
C14 N29 N30 105.2(4) . . ?
N31 N30 N29 110.6(4) . . ?
N30 N31 N32 107.7(5) . . ?
C14 N32 N31 106.5(5) . . ?
C14 N32 H32 126.8 . . ?
N31 N32 H32 126.8 . . ?
C16 N33 N34 104.2(4) . . ?
N35 N34 N33 110.4(4) . . ?
N34 N35 N36 108.6(4) . . ?
C16 N36 N35 105.4(3) . . ?
Gd1 O1 H1A 122.0(17) . . ?
Gd1 O1 H1B 123.6(17) . . ?
H1A O1 H1B 107(2) . . ?
Gd1 O2 H2A 132(2) . . ?
Gd1 O2 H2B 117.2(19) . . ?
H2A O2 H2B 110(2) . . ?
Gd1 O3 H3A 121.7(17) . . ?
Gd1 O3 H3B 131.4(18) . . ?
H3A O3 H3B 106(2) . . ?
Gd1 O4 H4A 127(2) . . ?
Gd1 O4 H4B 125(2) . . ?
H4A O4 H4B 107(2) . . ?
Gd1 O5 H5A 122.3(17) . . ?
Gd1 O5 H5B 120.9(17) . . ?
H5A O5 H5B 107(2) . . ?
Gd1 O6 H6A 122.7(18) . . ?
Gd1 O6 H6B 124.6(18) . . ?
H6A O6 H6B 113(2) . . ?
H7A O7 H7B 108(2) . . ?
H8A O8 H8B 116(3) . . ?
H9A O9 H9B 105(3) . . ?
H10A O10 H10B 101(3) . . ?
H11A O11 H11B 102(3) . . ?
H12A O12 H12B 100(3) . . ?
H9C O9' H9D 108(3) . . ?
H10B O10' H10D 100(3) . . ?
H11C O11' H11D 108(3) . . ?
H12C O12' H12D 108(3) . . ?

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
N1 C1 C2 N6 177.84(15) . . . . ?
C5 C1 C2 N6 -1.2(3) . . . . ?
N1 C1 C2 N3 -0.9(2) . . . . ?
C5 C1 C2 N3 -179.89(16) . . . . ?
N1 C3 C4 N10 177.32(16) . . . . ?
C7 C3 C4 N10 -5.4(3) . . . . ?
N1 C3 C4 N7 -4.1(2) . . . . ?
C7 C3 C4 N7 173.15(15) . . . . ?
N1 C1 C5 N2 0.8(2) . . . . ?
C2 C1 C5 N2 179.83(15) . . . . ?
N1 C1 C5 C6 -178.85(14) . . . . ?
C2 C1 C5 C6 0.1(3) . . . . ?
N2 C5 C6 N11 1.2(2) . . . . ?
C1 C5 C6 N11 -179.12(16) . . . . ?
N2 C5 C6 N14 -178.49(16) . . . . ?
C1 C5 C6 N14 1.2(3) . . . . ?
N1 C3 C7 N2 1.1(2) . . . . ?
C4 C3 C7 N2 -175.98(15) . . . . ?
N1 C3 C7 C8 179.84(14) . . . . ?
C4 C3 C7 C8 2.7(3) . . . . ?
N2 C7 C8 N15 5.6(2) . . . . ?
C3 C7 C8 N15 -173.22(15) . . . . ?
N2 C7 C8 N18 -172.43(16) . . . . ?
C3 C7 C8 N18 8.8(3) . . . . ?
C5 C1 N1 C3 -1.3(2) . . . . ?
C2 C1 N1 C3 179.59(13) . . . . ?
C5 C1 N1 Gd1 176.12(10) . . . . ?
C2 C1 N1 Gd1 -3.01(16) . . . . ?
C7 C3 N1 C1 0.3(2) . . . . ?
C4 C3 N1 C1 177.84(14) . . . . ?
C7 C3 N1 Gd1 -177.05(10) . . . . ?
C4 C3 N1 Gd1 0.47(17) . . . . ?
C1 C5 N2 C7 0.6(2) . . . . ?
C6 C5 N2 C7 -179.65(13) . . . . ?
C3 C7 N2 C5 -1.6(2) . . . . ?
C8 C7 N2 C5 179.52(13) . . . . ?
N6 C2 N3 N4 0.55(19) . . . . ?
C1 C2 N3 N4 179.44(15) . . . . ?
N6 C2 N3 Gd1 -173.78(11) . . . . ?
C1 C2 N3 Gd1 5.1(2) . . . . ?
C2 N3 N4 N5 -0.4(2) . . . . ?
Gd1 N3 N4 N5 173.77(12) . . . . ?
N3 N4 N5 N6 0.1(2) . . . . ?
N3 C2 N6 N5 -0.52(19) . . . . ?
C1 C2 N6 N5 -179.32(15) . . . . ?
N4 N5 N6 C2 0.27(19) . . . . ?
N10 C4 N7 N8 0.14(19) . . . . ?
C3 C4 N7 N8 -178.64(15) . . . . ?
N10 C4 N7 Gd1 -174.76(11) . . . . ?
C3 C4 N7 Gd1 6.5(2) . . . . ?
C4 N7 N8 N9 0.1(2) . . . . ?
Gd1 N7 N8 N9 174.81(12) . . . . ?
N7 N8 N9 N10 -0.3(2) . . . . ?
N7 C4 N10 N9 -0.3(2) . . . . ?
C3 C4 N10 N9 178.37(16) . . . . ?
N8 N9 N10 C4 0.3(2) . . . . ?
N14 C6 N11 N12 -0.57(19) . . . . ?
C5 C6 N11 N12 179.71(15) . . . . ?
C6 N11 N12 N13 0.3(2) . . . . ?
N11 N12 N13 N14 0.0(2) . . . . ?
N12 N13 N14 C6 -0.4(2) . . . . ?
N11 C6 N14 N13 0.6(2) . . . . ?
C5 C6 N14 N13 -179.68(16) . . . . ?
N18 C8 N15 N16 0.07(18) . . . . ?
C7 C8 N15 N16 -178.30(14) . . . . ?
C8 N15 N16 N17 0.08(19) . . . . ?
N15 N16 N17 N18 -0.20(19) . . . . ?
N15 C8 N18 N17 -0.20(18) . . . . ?
C7 C8 N18 N17 178.02(15) . . . . ?
N16 N17 N18 C8 0.25(18) . . . . ?
N19 C9 C10 N24 179.1(4) . . . . ?
C13 C9 C10 N24 -3.0(8) . . . . ?
N19 C9 C10 N21 0.7(6) . . . . ?
C13 C9 C10 N21 178.6(5) . . . . ?
N19 C11 C12 N25 -23.8(7) . . . . ?
C15 C11 C12 N25 155.8(5) . . . . ?
N19 C11 C12 N28 150.9(5) . . . . ?
C15 C11 C12 N28 -29.4(9) . . . . ?
N19 C9 C13 N20 -3.5(7) . . . . ?
C10 C9 C13 N20 178.8(4) . . . . ?
N19 C9 C13 C14 176.3(4) . . . . ?
C10 C9 C13 C14 -1.5(8) . . . . ?
N20 C13 C14 N32 -163.6(5) . . . . ?
C9 C13 C14 N32 16.7(8) . . . . ?
N20 C13 C14 N29 16.1(7) . . . . ?
C9 C13 C14 N29 -163.7(5) . . . . ?
N19 C11 C15 N20 -3.7(8) . . . . ?
C12 C11 C15 N20 176.6(4) . . . . ?
N19 C11 C15 C16 175.5(4) . . . . ?
C12 C11 C15 C16 -4.2(8) . . . . ?
N20 C15 C16 N36 156.0(5) . . . . ?
C11 C15 C16 N36 -23.2(8) . . . . ?
N20 C15 C16 N33 -18.2(6) . . . . ?
C11 C15 C16 N33 162.5(5) . . . . ?
C15 C11 N19 C9 1.9(7) . . . . ?
C12 C11 N19 C9 -178.4(4) . . . . ?
C13 C9 N19 C11 1.6(6) . . . . ?
C10 C9 N19 C11 179.6(4) . . . . ?
C9 C13 N20 C15 1.7(7) . . . . ?
C14 C13 N20 C15 -178.1(4) . . . . ?
C11 C15 N20 C13 1.8(7) . . . . ?
C16 C15 N20 C13 -177.5(4) . . . . ?
N24 C10 N21 N22 1.1(5) . . . . ?
C9 C10 N21 N22 179.8(4) . . . . ?
C10 N21 N22 N23 -0.4(5) . . . . ?
N21 N22 N23 N24 -0.4(5) . . . . ?
N21 C10 N24 N23 -1.5(5) . . . . ?
C9 C10 N24 N23 179.9(4) . . . . ?
N22 N23 N24 C10 1.1(5) . . . . ?
N28 C12 N25 N26 0.8(6) . . . . ?
C11 C12 N25 N26 176.5(5) . . . . ?
C12 N25 N26 N27 -0.8(6) . . . . ?
N25 N26 N27 N28 0.5(6) . . . . ?
N25 C12 N28 N27 -0.5(6) . . . . ?
C11 C12 N28 N27 -175.8(5) . . . . ?
N26 N27 N28 C12 0.0(6) . . . . ?
N32 C14 N29 N30 0.0(6) . . . . ?
C13 C14 N29 N30 -179.7(5) . . . . ?
C14 N29 N30 N31 -0.2(6) . . . . ?
N29 N30 N31 N32 0.3(6) . . . . ?
N29 C14 N32 N31 0.1(6) . . . . ?
C13 C14 N32 N31 179.8(5) . . . . ?
N30 N31 N32 C14 -0.2(6) . . . . ?
N36 C16 N33 N34 2.4(6) . . . . ?
C15 C16 N33 N34 177.5(4) . . . . ?
C16 N33 N34 N35 -2.2(6) . . . . ?
N33 N34 N35 N36 1.2(6) . . . . ?
N33 C16 N36 N35 -1.7(6) . . . . ?
C15 C16 N36 N35 -176.4(4) . . . . ?
N34 N35 N36 C16 0.3(5) . . . . ?

_refine_diff_density_max         0.718
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.064

