 
data_66
  
_audit_creation_method            'SHELXL-2018/3' 
_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety
 'C36 H37 Dy N6 O11' 
_chemical_formula_sum 
 'C36 H37 Dy N6 O11' 
_chemical_formula_weight          892.21 
  
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       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                    9.6822(3) 
_cell_length_b                    15.0267(5) 
_cell_length_c                    15.0409(5) 
_cell_angle_alpha                 110.887(3) 
_cell_angle_beta                  98.160(3) 
_cell_angle_gamma                 105.058(3) 
_cell_volume                      1906.44(12) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     5603 
_cell_measurement_theta_min       2.7400 
_cell_measurement_theta_max       27.5160 
  
_exptl_crystal_description        blocks 
_exptl_crystal_colour             Colourless 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.554 
_exptl_crystal_F_000              898 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.162 
_exptl_crystal_size_mid           0.119 
_exptl_crystal_size_min           0.071 
_exptl_absorpt_coefficient_mu     2.026 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.795 
_exptl_absorpt_correction_T_max   0.876 
_exptl_absorpt_process_details     
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
; 
_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_source                    'Enhance (Mo) X-ray Source' 
_diffrn_measurement_device_type   'Agilent Xcalibur 3 E' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  16.0382 
_diffrn_reflns_number             13501 
_diffrn_reflns_av_unetI/netI      0.1155 
_diffrn_reflns_av_R_equivalents   0.0346
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.691 
_diffrn_reflns_theta_max          28.203 
_diffrn_reflns_theta_full         25.242 
_diffrn_measured_fraction_theta_max   0.804 
_diffrn_measured_fraction_theta_full  0.983 
_diffrn_reflns_Laue_measured_fraction_max    0.804 
_diffrn_reflns_Laue_measured_fraction_full   0.983 
_diffrn_reflns_point_group_measured_fraction_max   0.804 
_diffrn_reflns_point_group_measured_fraction_full  0.983 
_reflns_number_total              13501 
_reflns_number_gt                 6989 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.000 
_reflns_Friedel_fraction_max      . 
_reflns_Friedel_fraction_full     . 
  
_reflns_special_details 
; 
 _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. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
; 
  
_computing_data_collection        'CrysAlisPro, Rigaku OD' 
_computing_cell_refinement        'CrysAlisPro, Rigaku OD' 
_computing_data_reduction         'CrysAlisPro, Rigaku OD' 
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2017)' 
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'CIFTAB-2014 (Sheldrick, 2017)' 
_refine_special_details 
; 
 Refined as a 2-component twin. 
; 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0344P)²] 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          13501 
_refine_ls_number_parameters      507 
_refine_ls_number_restraints      48 
_refine_ls_R_factor_all           0.0870 
_refine_ls_R_factor_gt            0.0385 
_refine_ls_wR_factor_ref          0.0777 
_refine_ls_wR_factor_gt           0.0730 
_refine_ls_goodness_of_fit_ref    0.777 
_refine_ls_restrained_S_all       0.781 
_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 
Dy1 Dy 0.17481(3) 0.67749(2) 0.32721(2) 0.02676(8) Uani 1 1 d D . . . . 
N1 N 0.1691(4) 0.5554(3) 0.6305(3) 0.0346(10) Uani 1 1 d . . . . . 
N2 N 0.2104(4) 0.5321(3) 0.5426(3) 0.0298(9) Uani 1 1 d . . . . . 
C3 C 0.1760(5) 0.5908(3) 0.4965(3) 0.0256(11) Uani 1 1 d . . . . . 
O3 O 0.2019(3) 0.5845(2) 0.4132(2) 0.0296(7) Uani 1 1 d . . . . . 
C4 C 0.1122(5) 0.6534(3) 0.5579(3) 0.0277(11) Uani 1 1 d . . . . . 
C5 C 0.1127(5) 0.6263(3) 0.6387(3) 0.0337(12) Uani 1 1 d . . . . . 
H5A H 0.075833 0.656712 0.692952 0.040 Uiso 1 1 calc R U . . . 
C6 C 0.2791(5) 0.4576(3) 0.5120(4) 0.0290(11) Uani 1 1 d . . . . . 
C7 C 0.3321(6) 0.4235(3) 0.5804(4) 0.0432(14) Uani 1 1 d . . . . . 
H7A H 0.318892 0.448159 0.645064 0.052 Uiso 1 1 calc R U . . . 
C8 C 0.4034(6) 0.3541(4) 0.5536(5) 0.0514(15) Uani 1 1 d . . . . . 
H8A H 0.440685 0.331501 0.600414 0.062 Uiso 1 1 calc R U . . . 
C9 C 0.4218(6) 0.3168(4) 0.4601(5) 0.0475(15) Uani 1 1 d . . . . . 
H9A H 0.473627 0.270088 0.442469 0.057 Uiso 1 1 calc R U . . . 
C10 C 0.3642(6) 0.3479(4) 0.3928(4) 0.0505(15) Uani 1 1 d . . . . . 
H10A H 0.373512 0.320771 0.327341 0.061 Uiso 1 1 calc R U . . . 
C11 C 0.2932(6) 0.4177(3) 0.4183(4) 0.0422(13) Uani 1 1 d . . . . . 
H11A H 0.253665 0.438318 0.370404 0.051 Uiso 1 1 calc R U . . . 
C12 C 0.0585(5) 0.7236(3) 0.5348(4) 0.0294(11) Uani 1 1 d . . . . . 
O12 O 0.0493(3) 0.7316(2) 0.4555(2) 0.0316(8) Uani 1 1 d . . . . . 
O13 O 0.0179(4) 0.7836(2) 0.6093(2) 0.0391(9) Uani 1 1 d . . . . . 
C14 C -0.0360(6) 0.8604(3) 0.5943(4) 0.0445(14) Uani 1 1 d . . . . . 
H14A H -0.145496 0.834677 0.572085 0.053 Uiso 1 1 calc R U . . . 
H14B H 0.003275 0.877983 0.543194 0.053 Uiso 1 1 calc R U . . . 
C15 C 0.0140(11) 0.9494(5) 0.6875(6) 0.132(4) Uani 1 1 d . . . . . 
H15A H -0.040844 0.935153 0.733658 0.198 Uiso 1 1 calc R U . . . 
H15B H -0.003722 1.006348 0.676383 0.198 Uiso 1 1 calc R U . . . 
H15C H 0.120104 0.966507 0.715249 0.198 Uiso 1 1 calc R U . . . 
N21 N 0.1794(4) 0.5779(3) -0.0637(3) 0.0366(10) Uani 1 1 d . . . . . 
N22 N 0.1207(4) 0.6361(3) 0.0053(3) 0.0317(9) Uani 1 1 d . . . . . 
C23 C 0.1385(5) 0.6190(3) 0.0901(3) 0.0293(11) Uani 1 1 d . . . . . 
O23 O 0.0949(3) 0.6615(2) 0.1639(2) 0.0316(8) Uani 1 1 d . . . . . 
C24 C 0.2143(5) 0.5479(3) 0.0726(3) 0.0311(12) Uani 1 1 d . . . . . 
C25 C 0.2333(5) 0.5272(3) -0.0222(4) 0.0355(12) Uani 1 1 d . . . . . 
H25A H 0.280509 0.480970 -0.053177 0.043 Uiso 1 1 calc R U . . . 
C26 C 0.0655(5) 0.7068(3) -0.0147(4) 0.0345(12) Uani 1 1 d . . . . . 
C27 C 0.1006(7) 0.7346(4) -0.0887(4) 0.0512(15) Uani 1 1 d . . . . . 
H27A H 0.161682 0.705862 -0.125790 0.061 Uiso 1 1 calc R U . . . 
C28 C 0.0477(7) 0.8039(4) -0.1094(5) 0.0635(18) Uani 1 1 d . . . . . 
H28A H 0.070442 0.821113 -0.161893 0.076 Uiso 1 1 calc R U . . . 
C29 C -0.0379(7) 0.8484(4) -0.0544(5) 0.0586(17) Uani 1 1 d . . . . . 
H29A H -0.073061 0.896855 -0.067882 0.070 Uiso 1 1 calc R U . . . 
C30 C -0.0711(6) 0.8214(4) 0.0195(5) 0.0560(16) Uani 1 1 d . . . . . 
H30A H -0.129151 0.852097 0.058136 0.067 Uiso 1 1 calc R U . . . 
C31 C -0.0218(6) 0.7503(4) 0.0394(4) 0.0443(14) Uani 1 1 d . . . . . 
H31A H -0.047961 0.731326 0.090227 0.053 Uiso 1 1 calc R U . . . 
C32 C 0.2584(5) 0.5114(3) 0.1429(4) 0.0314(12) Uani 1 1 d . . . . . 
O32 O 0.2362(4) 0.5373(2) 0.2263(2) 0.0354(8) Uani 1 1 d . . . . . 
O33 O 0.3300(4) 0.4460(2) 0.1131(2) 0.0380(8) Uani 1 1 d . . . . . 
C34 C 0.3712(6) 0.4023(4) 0.1809(4) 0.0434(13) Uani 1 1 d . . . . . 
H34A H 0.281706 0.355777 0.185414 0.052 Uiso 1 1 calc R U . . . 
H34B H 0.422816 0.456352 0.247523 0.052 Uiso 1 1 calc R U . . . 
C35 C 0.4707(7) 0.3463(5) 0.1421(5) 0.0653(18) Uani 1 1 d . . . . . 
H35A H 0.418639 0.293254 0.076129 0.098 Uiso 1 1 calc R U . . . 
H35B H 0.499665 0.315635 0.186069 0.098 Uiso 1 1 calc R U . . . 
H35C H 0.559281 0.393206 0.138638 0.098 Uiso 1 1 calc R U . . . 
N41 N 0.7002(4) 0.9893(3) 0.5685(3) 0.0359(10) Uani 1 1 d . . . . . 
N42 N 0.5676(4) 0.9322(2) 0.5763(3) 0.0297(9) Uani 1 1 d D . . . . 
C43 C 0.4788(5) 0.8625(3) 0.4842(4) 0.0277(11) Uani 1 1 d . . . . . 
O43 O 0.3521(3) 0.8005(2) 0.4695(2) 0.0318(8) Uani 1 1 d . . . . . 
C44 C 0.5607(5) 0.8771(3) 0.4175(4) 0.0279(11) Uani 1 1 d . . . . . 
C45 C 0.6929(6) 0.9553(3) 0.4747(4) 0.0365(12) Uani 1 1 d . . . . . 
H45A H 0.769260 0.981029 0.448028 0.044 Uiso 1 1 calc R U . . . 
C46 C 0.5500(7) 0.9451(4) 0.6694(3) 0.037(4) Uani 0.734(14) 1 d DG U P A 1 
C47 C 0.6700(6) 0.9967(7) 0.7521(5) 0.059(3) Uani 0.734(14) 1 d G U P A 1 
H47A H 0.766402 1.022861 0.745227 0.071 Uiso 0.734(14) 1 calc R U P A 1 
C48 C 0.6489(7) 1.0101(7) 0.8449(4) 0.090(4) Uani 0.734(14) 1 d G U P A 1 
H48A H 0.730926 1.045325 0.901429 0.109 Uiso 0.734(14) 1 calc R U P A 1 
C49 C 0.5079(8) 0.9718(6) 0.8550(3) 0.101(5) Uani 0.734(14) 1 d G U P A 1 
H49A H 0.493453 0.980909 0.918418 0.121 Uiso 0.734(14) 1 calc R U P A 1 
C50 C 0.3879(6) 0.9202(7) 0.7723(4) 0.064(3) Uani 0.734(14) 1 d G U P A 1 
H50A H 0.291454 0.894030 0.779204 0.077 Uiso 0.734(14) 1 calc R U P A 1 
C51 C 0.4089(6) 0.9068(6) 0.6795(4) 0.043(2) Uani 0.734(14) 1 d G U P A 1 
H51A H 0.326927 0.871565 0.623000 0.051 Uiso 0.734(14) 1 calc R U P A 1 
C46' C 0.5350(19) 0.9448(12) 0.6704(10) 0.033(9) Uiso 0.266(14) 1 d DG U P A 2 
C47' C 0.621(2) 1.0326(10) 0.7523(13) 0.033(5) Uiso 0.266(14) 1 d G U P A 2 
H47B H 0.693283 1.084047 0.744585 0.039 Uiso 0.266(14) 1 calc R U P A 2 
C48' C 0.603(2) 1.0450(12) 0.8454(10) 0.061(7) Uiso 0.266(14) 1 d G U P A 2 
H48B H 0.661691 1.105024 0.901323 0.073 Uiso 0.266(14) 1 calc R U P A 2 
C49' C 0.498(2) 0.9697(15) 0.8566(11) 0.110(11) Uiso 0.266(14) 1 d G U P A 2 
H49B H 0.484681 0.978236 0.920219 0.131 Uiso 0.266(14) 1 calc R U P A 2 
C50' C 0.411(2) 0.8819(14) 0.7747(14) 0.052(7) Uiso 0.266(14) 1 d G U P A 2 
H50B H 0.339262 0.830471 0.782377 0.063 Uiso 0.266(14) 1 calc R U P A 2 
C51' C 0.4299(18) 0.8695(11) 0.6816(12) 0.037(6) Uiso 0.266(14) 1 d G U P A 2 
H51B H 0.370851 0.809493 0.625638 0.044 Uiso 0.266(14) 1 calc R U P A 2 
C52 C 0.5102(6) 0.8156(3) 0.3147(4) 0.0327(12) Uani 1 1 d . . . . . 
O52 O 0.3909(4) 0.7449(2) 0.2755(2) 0.0365(8) Uani 1 1 d . . . . . 
O53 O 0.6028(4) 0.8399(2) 0.2633(3) 0.0481(10) Uani 1 1 d . . . . . 
C54 C 0.5647(7) 0.7760(4) 0.1584(4) 0.0601(18) Uani 1 1 d . . . . . 
H54A H 0.607172 0.816164 0.122978 0.072 Uiso 1 1 calc R U . . . 
H54B H 0.455764 0.748435 0.131653 0.072 Uiso 1 1 calc R U . . . 
C55 C 0.6253(8) 0.6912(5) 0.1437(5) 0.081(2) Uani 1 1 d . . . . . 
H55A H 0.730647 0.718700 0.178405 0.122 Uiso 1 1 calc R U . . . 
H55B H 0.613320 0.653780 0.073145 0.122 Uiso 1 1 calc R U . . . 
H55C H 0.571501 0.645539 0.169777 0.122 Uiso 1 1 calc R U . . . 
O60 O 0.1129(4) 0.81952(19) 0.32106(19) 0.0455(9) Uani 1 1 d D . . . . 
H60A H 0.1798(11) 0.8818(4) 0.356(2) 0.055(16) Uiso 1 1 d D . . . . 
H60B H 0.099(3) 0.8129(8) 0.2582(3) 0.082 Uiso 1 1 d D U . . . 
O70 O -0.0669(3) 0.55851(19) 0.26546(18) 0.0304(7) Uani 1 1 d D . . . . 
H70A H -0.090(4) 0.5130(8) 0.2027(4) 0.068(19) Uiso 1 1 d D . . . . 
H70B H -0.1107(10) 0.5287(5) 0.3014(3) 0.061(17) Uiso 1 1 d D . . . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Dy1 O3 2.253(3) . ? 
Dy1 O43 2.331(3) . ? 
Dy1 O70 2.358(3) . ? 
Dy1 O23 2.374(3) . ? 
Dy1 O60 2.390(3) . ? 
Dy1 O32 2.392(3) . ? 
Dy1 O12 2.433(3) . ? 
Dy1 O52 2.436(3) . ? 
N1 C5 1.296(6) . ? 
N1 N2 1.386(5) . ? 
N2 C3 1.376(5) . ? 
N2 C6 1.419(6) . ? 
C3 O3 1.288(5) . ? 
C3 C4 1.401(6) . ? 
C4 C5 1.412(6) . ? 
C4 C12 1.414(6) . ? 
C6 C11 1.364(6) . ? 
C6 C7 1.396(6) . ? 
C7 C8 1.371(7) . ? 
C8 C9 1.373(8) . ? 
C9 C10 1.366(7) . ? 
C10 C11 1.372(7) . ? 
C12 O12 1.233(5) . ? 
C12 O13 1.347(5) . ? 
O13 C14 1.456(5) . ? 
C14 C15 1.457(8) . ? 
N21 C25 1.302(6) . ? 
N21 N22 1.393(5) . ? 
N22 C23 1.385(6) . ? 
N22 C26 1.408(6) . ? 
C23 O23 1.259(5) . ? 
C23 C24 1.418(7) . ? 
C24 C25 1.397(6) . ? 
C24 C32 1.418(7) . ? 
C26 C27 1.376(7) . ? 
C26 C31 1.380(7) . ? 
C27 C28 1.381(8) . ? 
C28 C29 1.381(8) . ? 
C29 C30 1.364(8) . ? 
C30 C31 1.383(7) . ? 
C32 O32 1.242(5) . ? 
C32 O33 1.332(5) . ? 
O33 C34 1.459(6) . ? 
C34 C35 1.484(7) . ? 
N41 C45 1.303(6) . ? 
N41 N42 1.393(5) . ? 
N42 C43 1.384(6) . ? 
N42 C46 1.385(6) . ? 
N42 C46' 1.450(13) . ? 
C43 O43 1.267(5) . ? 
C43 C44 1.404(6) . ? 
C44 C45 1.395(6) . ? 
C44 C52 1.420(6) . ? 
C46 C47 1.3900 . ? 
C46 C51 1.3900 . ? 
C47 C48 1.3900 . ? 
C48 C49 1.3900 . ? 
C49 C50 1.3900 . ? 
C50 C51 1.3900 . ? 
C46' C47' 1.3900 . ? 
C46' C51' 1.3900 . ? 
C47' C48' 1.3900 . ? 
C48' C49' 1.3900 . ? 
C49' C50' 1.3900 . ? 
C50' C51' 1.3900 . ? 
C52 O52 1.238(5) . ? 
C52 O53 1.328(5) . ? 
O53 C54 1.455(6) . ? 
C54 C55 1.496(8) . ? 
  
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 
O3 Dy1 O43 79.57(10) . . ? 
O3 Dy1 O70 81.54(10) . . ? 
O43 Dy1 O70 144.52(10) . . ? 
O3 Dy1 O23 141.58(10) . . ? 
O43 Dy1 O23 135.03(10) . . ? 
O70 Dy1 O23 74.96(9) . . ? 
O3 Dy1 O60 147.42(10) . . ? 
O43 Dy1 O60 82.86(10) . . ? 
O70 Dy1 O60 97.85(10) . . ? 
O23 Dy1 O60 67.03(9) . . ? 
O3 Dy1 O32 72.10(10) . . ? 
O43 Dy1 O32 118.64(11) . . ? 
O70 Dy1 O32 82.98(10) . . ? 
O23 Dy1 O32 75.17(10) . . ? 
O60 Dy1 O32 140.40(10) . . ? 
O3 Dy1 O12 76.47(10) . . ? 
O43 Dy1 O12 71.76(11) . . ? 
O70 Dy1 O12 74.78(9) . . ? 
O23 Dy1 O12 124.14(11) . . ? 
O60 Dy1 O12 72.05(10) . . ? 
O32 Dy1 O12 143.69(10) . . ? 
O3 Dy1 O52 115.86(11) . . ? 
O43 Dy1 O52 73.24(11) . . ? 
O70 Dy1 O52 142.24(10) . . ? 
O23 Dy1 O52 71.36(11) . . ? 
O60 Dy1 O52 84.44(11) . . ? 
O32 Dy1 O52 72.42(10) . . ? 
O12 Dy1 O52 139.70(10) . . ? 
C5 N1 N2 106.4(4) . . ? 
C3 N2 N1 110.2(4) . . ? 
C3 N2 C6 128.9(4) . . ? 
N1 N2 C6 120.9(4) . . ? 
O3 C3 N2 123.3(4) . . ? 
O3 C3 C4 130.4(4) . . ? 
N2 C3 C4 106.4(4) . . ? 
C3 O3 Dy1 131.0(3) . . ? 
C3 C4 C5 104.7(4) . . ? 
C3 C4 C12 123.5(4) . . ? 
C5 C4 C12 131.7(4) . . ? 
N1 C5 C4 112.3(4) . . ? 
C11 C6 C7 119.3(5) . . ? 
C11 C6 N2 122.3(4) . . ? 
C7 C6 N2 118.4(4) . . ? 
C8 C7 C6 119.5(5) . . ? 
C7 C8 C9 120.9(5) . . ? 
C10 C9 C8 118.9(5) . . ? 
C9 C10 C11 121.1(6) . . ? 
C6 C11 C10 120.2(5) . . ? 
O12 C12 O13 121.9(4) . . ? 
O12 C12 C4 125.0(4) . . ? 
O13 C12 C4 113.1(4) . . ? 
C12 O12 Dy1 130.7(3) . . ? 
C12 O13 C14 117.8(4) . . ? 
O13 C14 C15 108.1(5) . . ? 
C25 N21 N22 105.5(4) . . ? 
C23 N22 N21 111.3(4) . . ? 
C23 N22 C26 129.4(4) . . ? 
N21 N22 C26 119.1(4) . . ? 
O23 C23 N22 124.3(4) . . ? 
O23 C23 C24 131.0(4) . . ? 
N22 C23 C24 104.6(4) . . ? 
C23 O23 Dy1 127.5(3) . . ? 
C25 C24 C23 105.7(4) . . ? 
C25 C24 C32 131.0(5) . . ? 
C23 C24 C32 123.2(4) . . ? 
N21 C25 C24 112.8(4) . . ? 
C27 C26 C31 119.0(5) . . ? 
C27 C26 N22 119.5(5) . . ? 
C31 C26 N22 121.4(4) . . ? 
C26 C27 C28 120.5(5) . . ? 
C29 C28 C27 120.4(6) . . ? 
C30 C29 C28 118.8(6) . . ? 
C29 C30 C31 121.2(6) . . ? 
C26 C31 C30 119.9(5) . . ? 
O32 C32 O33 121.1(4) . . ? 
O32 C32 C24 124.7(4) . . ? 
O33 C32 C24 114.2(4) . . ? 
C32 O32 Dy1 133.1(3) . . ? 
C32 O33 C34 116.3(4) . . ? 
O33 C34 C35 107.6(4) . . ? 
C45 N41 N42 105.6(4) . . ? 
C43 N42 C46 130.5(4) . . ? 
C43 N42 N41 110.7(4) . . ? 
C46 N42 N41 118.5(4) . . ? 
C43 N42 C46' 126.7(8) . . ? 
N41 N42 C46' 122.6(8) . . ? 
O43 C43 N42 124.2(4) . . ? 
O43 C43 C44 130.6(4) . . ? 
N42 C43 C44 105.2(4) . . ? 
C43 O43 Dy1 133.0(3) . . ? 
C45 C44 C43 105.8(4) . . ? 
C45 C44 C52 131.5(5) . . ? 
C43 C44 C52 122.6(4) . . ? 
N41 C45 C44 112.6(4) . . ? 
N42 C46 C47 121.1(4) . . ? 
N42 C46 C51 118.8(4) . . ? 
C47 C46 C51 120.0 . . ? 
C46 C47 C48 120.0 . . ? 
C49 C48 C47 120.0 . . ? 
C48 C49 C50 120.0 . . ? 
C51 C50 C49 120.0 . . ? 
C50 C51 C46 120.0 . . ? 
C47' C46' C51' 120.0 . . ? 
C47' C46' N42 117.6(11) . . ? 
C51' C46' N42 122.2(11) . . ? 
C48' C47' C46' 120.0 . . ? 
C47' C48' C49' 120.0 . . ? 
C48' C49' C50' 120.0 . . ? 
C51' C50' C49' 120.0 . . ? 
C50' C51' C46' 120.0 . . ? 
O52 C52 O53 122.3(5) . . ? 
O52 C52 C44 123.5(5) . . ? 
O53 C52 C44 114.2(4) . . ? 
C52 O52 Dy1 136.5(3) . . ? 
C52 O53 C54 117.7(4) . . ? 
O53 C54 C55 109.0(5) . . ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
 _geom_hbond_publ_flag 
O60 H60A N41  0.9000(2) 1.810(5) 2.708(4) 174.3(19) 2_676 yes 
O60 H60B O23  0.9000(2) 2.196(12) 2.631(4) 109.0(9) . yes 
O70 H70A N21  0.9000(1) 1.955(8) 2.840(4) 167(3) 2_565 yes 
O70 H70B N1  0.9000(1) 1.920(5) 2.798(4) 164.6(11) 2_566 yes 
  
_refine_diff_density_max    3.898 
_refine_diff_density_min   -2.664 
_refine_diff_density_rms    0.303 
  
  
  
#===END

