 
data_65
  
_audit_creation_method            'SHELXL-2018/3' 
_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety
 'C56 H52 Dy N8 Na O16, 0.75(C H4 O)'
_chemical_formula_sum 
 'C56.75 H55 Dy N8 Na O16.75' 
_chemical_formula_weight          1302.57 
  
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' 
 'Na'  'Na'   0.0362   0.0249 
 '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       tetragonal 
_space_group_IT_number            118 
_space_group_name_H-M_alt         'P -4 n 2' 
_space_group_name_Hall            'P -4 -2n' 
  
_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' 
 'y, -x, -z' 
 '-y, x, -z' 
 'x+1/2, -y+1/2, z+1/2' 
 '-x+1/2, y+1/2, z+1/2' 
 'y+1/2, x+1/2, -z+1/2' 
 '-y+1/2, -x+1/2, -z+1/2' 
  
_cell_length_a                    12.5821(4) 
_cell_length_b                    12.5821(4) 
_cell_length_c                    19.0063(10) 
_cell_angle_alpha                 90 
_cell_angle_beta                  90 
_cell_angle_gamma                 90 
_cell_volume                      3008.9(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     1374 
_cell_measurement_theta_min       3.2190 
_cell_measurement_theta_max       22.6100 
  
_exptl_crystal_description        blocks 
_exptl_crystal_colour             Colourless 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.438 
_exptl_crystal_F_000              1325 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.148 
_exptl_crystal_size_mid           0.127 
_exptl_crystal_size_min           0.062 
_exptl_absorpt_coefficient_mu     1.323 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.885 
_exptl_absorpt_correction_T_max   0.935 
_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             5118 
_diffrn_reflns_av_unetI/netI      0.0493 
_diffrn_reflns_av_R_equivalents   0.0289 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          2.528 
_diffrn_reflns_theta_max          28.324 
_diffrn_reflns_theta_full         25.242 
_diffrn_measured_fraction_theta_max   0.853 
_diffrn_measured_fraction_theta_full  0.991 
_diffrn_reflns_Laue_measured_fraction_max    0.853 
_diffrn_reflns_Laue_measured_fraction_full   0.991 
_diffrn_reflns_point_group_measured_fraction_max   0.703 
_diffrn_reflns_point_group_measured_fraction_full  0.848 
_reflns_number_total              2651 
_reflns_number_gt                 1893 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.511 
_reflns_Friedel_fraction_max      0.523 
_reflns_Friedel_fraction_full     0.672 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _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        '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           ? 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0729P)²+2.0965P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        . 
_refine_ls_abs_structure_details 
; 
 Flack x determined using 592 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
; 
_refine_ls_abs_structure_Flack    -0.019(14) 
_chemical_absolute_configuration  ? 
_refine_ls_number_reflns          2651 
_refine_ls_number_parameters      208 
_refine_ls_number_restraints      116 
_refine_ls_R_factor_all           0.0759 
_refine_ls_R_factor_gt            0.0473 
_refine_ls_wR_factor_ref          0.1321 
_refine_ls_wR_factor_gt           0.1169 
_refine_ls_goodness_of_fit_ref    1.048 
_refine_ls_restrained_S_all       1.077 
_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 
Dy1 Dy 0.000000 0.500000 0.250000 0.0413(2) Uani 1 4 d S T P . . 
Na1 Na 0.000000 0.000000 0.500000 0.0466(16) Uani 1 4 d S T P . . 
N1 N 0.0173(6) 0.1340(7) 0.4090(5) 0.051(2) Uani 1 1 d . . . . . 
N2 N -0.0242(6) 0.2358(7) 0.4092(4) 0.048(2) Uani 1 1 d . . . . . 
C3 C -0.0124(6) 0.2887(8) 0.3480(5) 0.042(2) Uani 1 1 d . . . . . 
O3 O -0.0448(6) 0.3834(5) 0.3376(4) 0.0502(16) Uani 1 1 d . . . . . 
C4 C 0.0402(8) 0.2144(7) 0.3030(5) 0.043(2) Uani 1 1 d . . . . . 
C5 C 0.0555(8) 0.1243(7) 0.3443(5) 0.047(2) Uani 1 1 d . . . . . 
H5 H 0.089951 0.061894 0.327693 0.056 Uiso 1 1 calc R U . . . 
C6 C -0.0612(10) 0.2826(9) 0.4740(5) 0.063(3) Uani 1 1 d D . . . . 
C7 C 0.0421(8) 0.3214(9) 0.5157(5) 0.093(5) Uani 0.83(3) 1 d DG U P A 1 
C8 C 0.0801(12) 0.2627(8) 0.5723(6) 0.116(7) Uani 0.83(3) 1 d DG U P A 1 
H8A H 0.044434 0.199729 0.586486 0.139 Uiso 0.83(3) 1 calc R U P A 1 
C9 C 0.1703(13) 0.2963(8) 0.6082(7) 0.080(6) Uani 0.83(3) 1 d DG U P A 1 
H9A H 0.196341 0.256174 0.646891 0.096 Uiso 0.83(3) 1 calc R U P A 1 
C10 C 0.2225(9) 0.3885(9) 0.5875(6) 0.112(7) Uani 0.83(3) 1 d DG U P A 1 
C11 C 0.1845(11) 0.4471(11) 0.5308(6) 0.148(9) Uani 0.83(3) 1 d DG U P A 1 
H11A H 0.220157 0.510126 0.516654 0.177 Uiso 0.83(3) 1 calc R U P A 1 
C12 C 0.0943(11) 0.4136(11) 0.4949(6) 0.116(7) Uani 0.83(3) 1 d DG U P A 1 
H12A H 0.068248 0.453684 0.456248 0.139 Uiso 0.83(3) 1 calc R U P A 1 
O13 O 0.3105(14) 0.4236(12) 0.6220(8) 0.162(7) Uani 0.83(3) 1 d D U P A 1 
C14 C 0.350(2) 0.369(2) 0.6789(11) 0.157(10) Uani 0.83(3) 1 d D U P A 1 
H14A H 0.413015 0.405004 0.697123 0.236 Uiso 0.83(3) 1 calc R U P A 1 
H14B H 0.295586 0.365128 0.715824 0.236 Uiso 0.83(3) 1 calc R U P A 1 
H14C H 0.369135 0.296342 0.664389 0.236 Uiso 0.83(3) 1 calc R U P A 1 
C7' C 0.0374(16) 0.312(2) 0.5221(13) 0.090(13) Uiso 0.17(3) 1 d DG U P A 2 
C8' C 0.041(4) 0.279(4) 0.5919(16) 0.127(15) Uiso 0.17(3) 1 d DG U P A 2 
H8'A H -0.016486 0.238785 0.610815 0.152 Uiso 0.17(3) 1 calc R U P A 2 
C9' C 0.127(4) 0.305(4) 0.634(2) 0.071(13) Uiso 0.17(3) 1 d DG U P A 2 
H9'A H 0.129406 0.282287 0.681531 0.085 Uiso 0.17(3) 1 calc R U P A 2 
C10' C 0.211(3) 0.364(4) 0.606(2) 0.089(14) Uiso 0.17(3) 1 d DG U P A 2 
C11' C 0.208(3) 0.397(7) 0.536(3) 0.153(17) Uiso 0.17(3) 1 d DG U P A 2 
H11B H 0.264549 0.437532 0.517495 0.184 Uiso 0.17(3) 1 calc R U P A 2 
C12' C 0.121(3) 0.371(6) 0.4944(19) 0.120(15) Uiso 0.17(3) 1 d DG U P A 2 
H12B H 0.118658 0.394030 0.446778 0.144 Uiso 0.17(3) 1 calc R U P A 2 
O13' O 0.295(4) 0.390(6) 0.648(3) 0.168(12) Uiso 0.17(3) 1 d D U P A 2 
C14' C 0.291(6) 0.353(5) 0.715(3) 0.09(3) Uiso 0.17(3) 1 d D . P A 2 
H14D H 0.354855 0.374994 0.740733 0.130 Uiso 0.17(3) 1 calc R U P A 2 
H14E H 0.227878 0.381726 0.738730 0.130 Uiso 0.17(3) 1 calc R U P A 2 
H14F H 0.286774 0.274891 0.714906 0.130 Uiso 0.17(3) 1 calc R U P A 2 
C15 C 0.0688(8) 0.2404(8) 0.2327(5) 0.055(3) Uani 1 1 d D . . . . 
O15 O 0.0527(6) 0.3261(5) 0.2030(4) 0.0519(16) Uani 1 1 d . . . . . 
O16 O 0.1283(16) 0.1642(11) 0.2024(9) 0.064(5) Uani 0.63(3) 1 d D U P B 1 
C17 C 0.157(3) 0.183(3) 0.1284(12) 0.121(10) Uani 0.63(3) 1 d D U P B 1 
H17A H 0.219415 0.138330 0.115986 0.145 Uiso 0.63(3) 1 calc R U P B 1 
H17B H 0.177241 0.258200 0.121941 0.145 Uiso 0.63(3) 1 calc R U P B 1 
C18 C 0.064(3) 0.155(4) 0.080(2) 0.201(15) Uani 0.63(3) 1 d D U P B 1 
H18A H 0.084317 0.168155 0.030726 0.301 Uiso 0.63(3) 1 calc R U P B 1 
H18B H 0.044653 0.080381 0.085716 0.301 Uiso 0.63(3) 1 calc R U P B 1 
H18C H 0.002545 0.200063 0.091661 0.301 Uiso 0.63(3) 1 calc R U P B 1 
O16' O 0.089(2) 0.153(2) 0.1929(17) 0.063(8) Uiso 0.37(3) 1 d D U P B 2 
C17' C 0.147(4) 0.162(9) 0.127(2) 0.139(14) Uiso 0.37(3) 1 d D U P B 2 
H17C H 0.119633 0.223879 0.099821 0.167 Uiso 0.37(3) 1 calc R U P B 2 
H17D H 0.134376 0.097642 0.098041 0.167 Uiso 0.37(3) 1 calc R U P B 2 
C18' C 0.267(4) 0.176(6) 0.137(4) 0.204(18) Uiso 0.37(3) 1 d D U P B 2 
H18D H 0.301799 0.181428 0.091061 0.306 Uiso 0.37(3) 1 calc R U P B 2 
H18E H 0.280424 0.240619 0.164233 0.306 Uiso 0.37(3) 1 calc R U P B 2 
H18F H 0.295175 0.114315 0.162451 0.306 Uiso 0.37(3) 1 calc R U P B 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 O3 2.289(7) . ? 
Dy1 O3 2.289(7) 7_455 ? 
Dy1 O3 2.289(7) 2_565 ? 
Dy1 O3 2.289(7) 8 ? 
Dy1 O15 2.455(6) 8 ? 
Dy1 O15 2.455(6) 7_455 ? 
Dy1 O15 2.455(6) 2_565 ? 
Dy1 O15 2.455(6) . ? 
Na1 N1 2.425(9) 2 ? 
Na1 N1 2.425(9) 3_556 ? 
Na1 N1 2.425(9) 4_556 ? 
Na1 N1 2.425(9) . ? 
N1 C5 1.328(13) . ? 
N1 N2 1.383(12) . ? 
N2 C3 1.348(13) . ? 
N2 C6 1.444(12) . ? 
C3 O3 1.275(11) . ? 
C3 C4 1.430(14) . ? 
C4 C5 1.392(13) . ? 
C4 C15 1.423(14) . ? 
C6 C7' 1.59(2) . ? 
C6 C7 1.598(15) . ? 
C7 C8 1.3900 . ? 
C7 C12 1.3900 . ? 
C8 C9 1.3900 . ? 
C9 C10 1.3900 . ? 
C10 O13 1.361(15) . ? 
C10 C11 1.3900 . ? 
C11 C12 1.3900 . ? 
O13 C14 1.38(2) . ? 
C7' C8' 1.3900 . ? 
C7' C12' 1.3900 . ? 
C8' C9' 1.3900 . ? 
C9' C10' 1.3900 . ? 
C10' O13' 1.36(2) . ? 
C10' C11' 1.3900 . ? 
C11' C12' 1.3900 . ? 
O13' C14' 1.37(3) . ? 
C15 O15 1.233(11) . ? 
C15 O16 1.346(12) . ? 
C15 O16' 1.36(2) . ? 
O16 C17 1.471(15) . ? 
C17 C18 1.54(2) . ? 
O16' C17' 1.464(18) . ? 
C17' C18' 1.53(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 
O3 Dy1 O3 102.3(4) . 7_455 ? 
O3 Dy1 O3 86.7(3) . 2_565 ? 
O3 Dy1 O3 147.6(3) 7_455 2_565 ? 
O3 Dy1 O3 147.6(3) . 8 ? 
O3 Dy1 O3 86.7(3) 7_455 8 ? 
O3 Dy1 O3 102.3(4) 2_565 8 ? 
O3 Dy1 O15 77.4(2) . 8 ? 
O3 Dy1 O15 140.3(2) 7_455 8 ? 
O3 Dy1 O15 71.9(3) 2_565 8 ? 
O3 Dy1 O15 76.1(2) 8 8 ? 
O3 Dy1 O15 71.9(3) . 7_455 ? 
O3 Dy1 O15 76.1(2) 7_455 7_455 ? 
O3 Dy1 O15 77.4(2) 2_565 7_455 ? 
O3 Dy1 O15 140.3(2) 8 7_455 ? 
O15 Dy1 O15 137.3(3) 8 7_455 ? 
O3 Dy1 O15 140.3(2) . 2_565 ? 
O3 Dy1 O15 77.4(2) 7_455 2_565 ? 
O3 Dy1 O15 76.1(2) 2_565 2_565 ? 
O3 Dy1 O15 71.9(3) 8 2_565 ? 
O15 Dy1 O15 127.9(4) 8 2_565 ? 
O15 Dy1 O15 69.6(4) 7_455 2_565 ? 
O3 Dy1 O15 76.1(2) . . ? 
O3 Dy1 O15 71.9(3) 7_455 . ? 
O3 Dy1 O15 140.3(2) 2_565 . ? 
O3 Dy1 O15 77.4(2) 8 . ? 
O15 Dy1 O15 69.6(4) 8 . ? 
O15 Dy1 O15 127.9(4) 7_455 . ? 
O15 Dy1 O15 137.3(3) 2_565 . ? 
N1 Na1 N1 120.5(2) 2 3_556 ? 
N1 Na1 N1 120.5(2) 2 4_556 ? 
N1 Na1 N1 89.1(4) 3_556 4_556 ? 
N1 Na1 N1 89.1(4) 2 . ? 
N1 Na1 N1 120.5(2) 3_556 . ? 
N1 Na1 N1 120.5(2) 4_556 . ? 
C5 N1 N2 103.0(8) . . ? 
C5 N1 Na1 129.0(7) . . ? 
N2 N1 Na1 127.5(6) . . ? 
C3 N2 N1 114.5(8) . . ? 
C3 N2 C6 124.8(9) . . ? 
N1 N2 C6 120.1(9) . . ? 
O3 C3 N2 124.1(9) . . ? 
O3 C3 C4 131.8(9) . . ? 
N2 C3 C4 104.1(8) . . ? 
C3 O3 Dy1 129.3(6) . . ? 
C5 C4 C15 133.0(9) . . ? 
C5 C4 C3 105.1(8) . . ? 
C15 C4 C3 121.9(9) . . ? 
N1 C5 C4 113.4(9) . . ? 
N2 C6 C7' 109.6(10) . . ? 
N2 C6 C7 106.5(7) . . ? 
C8 C7 C12 120.0 . . ? 
C8 C7 C6 120.1(7) . . ? 
C12 C7 C6 119.9(7) . . ? 
C9 C8 C7 120.0 . . ? 
C8 C9 C10 120.0 . . ? 
O13 C10 C11 118.8(7) . . ? 
O13 C10 C9 121.2(7) . . ? 
C11 C10 C9 120.0 . . ? 
C10 C11 C12 120.0 . . ? 
C11 C12 C7 120.0 . . ? 
C10 O13 C14 120.6(16) . . ? 
C8' C7' C12' 120.0 . . ? 
C8' C7' C6 120.1(10) . . ? 
C12' C7' C6 119.9(10) . . ? 
C7' C8' C9' 120.0 . . ? 
C8' C9' C10' 120.0 . . ? 
O13' C10' C11' 120.2(10) . . ? 
O13' C10' C9' 119.8(10) . . ? 
C11' C10' C9' 120.0 . . ? 
C10' C11' C12' 120.0 . . ? 
C11' C12' C7' 120.0 . . ? 
C10' O13' C14' 116(3) . . ? 
O15 C15 O16 121.3(11) . . ? 
O15 C15 O16' 118.8(18) . . ? 
O15 C15 C4 126.1(9) . . ? 
O16 C15 C4 112.2(11) . . ? 
O16' C15 C4 112.6(17) . . ? 
C15 O15 Dy1 131.1(6) . . ? 
C15 O16 C17 115.7(18) . . ? 
O16 C17 C18 111(3) . . ? 
C15 O16' C17' 121(5) . . ? 
O16' C17' C18' 113(4) . . ? 
  
_refine_diff_density_max    0.723 
_refine_diff_density_min   -0.429 
_refine_diff_density_rms    0.094 
  
  
  
  
#===END

