# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_180607a
_database_code_depnum_ccdc_archive 'CCDC 2278244'
loop_
_audit_author_name
_audit_author_address
'Luis Cunha Silva'
;Univ of Porto
Portugal
;
_audit_update_record             
;
2023-06-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;

_audit_creation_date             2018-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C30 H26 Dy2 N8 O20'
_chemical_formula_sum            'C30 H26 Dy2 N8 O20'
_chemical_formula_weight         1143.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         DyNOC
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7495(3)
_cell_length_b                   10.3059(3)
_cell_length_c                   10.8266(2)
_cell_angle_alpha                91.834(2)
_cell_angle_beta                 112.263(2)
_cell_angle_gamma                112.030(3)
_cell_volume                     913.81(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6878
_cell_measurement_temperature    293.0(1)
_cell_measurement_theta_max      76.6690
_cell_measurement_theta_min      4.5000
_shelx_estimated_absorpt_T_max   0.806
_shelx_estimated_absorpt_T_min   0.399
_exptl_absorpt_coefficient_mu    22.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8071
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.063
_diffrn_reflns_theta_min         4.507
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -61.00 -24.00   0.50    0.05    --  -48.45  11.00 -93.00   74
  2  ω   -116.00 -50.00   0.50    0.05    --  -48.45 -11.00  93.00  132
  3  ω     65.00 119.00   0.50    0.05    --   48.45  11.00 -93.00  108
  4  ω   -102.00 -74.00   0.50    0.20    --  -86.25  11.00 -93.00   56
  5  ω   -158.00 -99.00   0.50    0.20    --  -86.25 -11.00  93.00  118
  6  ω    -67.00 -41.00   0.50    0.20    --  -86.25  11.00 -93.00   52
  7  ω    151.00 177.00   0.50    0.20    --  107.75  11.00 -93.00   52
  8  ω    114.00 146.00   0.50    0.20    --  107.75  11.00 -93.00   64
  9  ω     -8.00  20.00   0.50    0.05    --  -48.45  11.00 -93.00   56
 10  ω    -63.00  19.00   0.50    0.05    --  -48.45  57.00 -90.00  164
 11  ω     -5.00  20.00   0.50    0.05    --   48.45 -11.00  93.00   50
 12  ω   -105.00 -17.00   0.50    0.20    --  -86.25  77.00 120.00  176
 13  ω    -99.00 -16.00   0.50    0.20    --  -86.25  37.00 -90.00  166
 14  ω     36.00 120.00   0.50    0.20    --  107.75 -37.00 -90.00  168
 15  ω     95.00 176.00   0.50    0.20    --  107.75  19.00 120.00  162
 16  ω     95.00 124.00   0.50    0.20    --  107.75 -11.00  93.00   58
 17  ω     92.00 117.00   0.50    0.20    --  107.75-125.00 120.00   50
 18  ω     44.00  85.00   0.50    0.20    --  107.75-125.00 120.00   82
 19  ω     50.00  87.00   0.50    0.20    --  107.75 -99.00-150.00   74
 20  ω     37.00 108.00   0.50    0.20    --  107.75 -77.00 -90.00  142
 21  ω     51.00 108.00   0.50    0.20    --  107.75 -99.00 150.00  114
 22  ω     41.00 119.00   0.50    0.20    --  107.75 -57.00 -60.00  156
 23  ω     37.00 108.00   0.50    0.20    --  107.75 -99.00 -90.00  142
 24  ω     49.00  92.00   0.50    0.20    --  107.75 -11.00  93.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1676846000
_diffrn_orient_matrix_UB_12      -0.1157469000
_diffrn_orient_matrix_UB_13      -0.0223152000
_diffrn_orient_matrix_UB_21      -0.0639685000
_diffrn_orient_matrix_UB_22      0.1158742000
_diffrn_orient_matrix_UB_23      -0.0000976000
_diffrn_orient_matrix_UB_31      -0.0560124000
_diffrn_orient_matrix_UB_32      -0.0172191000
_diffrn_orient_matrix_UB_33      -0.1554298000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3037
_reflns_number_total             3221
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0241
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0309P)²+0.4383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0596
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7091(4) 0.3097(3) 0.1890(3) 0.0290(6) Uani 1 1 d . . . . .
C2 C 0.5600(4) 0.2642(3) 0.0643(3) 0.0311(6) Uani 1 1 d . . . . .
C3 C 0.5278(4) 0.1655(4) -0.0433(4) 0.0387(7) Uani 1 1 d . . . . .
H3 H 0.6025 0.1274 -0.0365 0.046 Uiso 1 1 calc R . . . .
C4 C 0.3841(5) 0.1222(4) -0.1625(4) 0.0448(8) Uani 1 1 d . . . . .
H4 H 0.3638 0.0557 -0.2346 0.054 Uiso 1 1 calc R . . . .
C5 C 0.2727(4) 0.1772(4) -0.1735(4) 0.0418(8) Uani 1 1 d . . . . .
H5 H 0.1765 0.1462 -0.2527 0.050 Uiso 1 1 calc R . . . .
C6 C 0.3018(4) 0.2796(4) -0.0672(3) 0.0337(7) Uani 1 1 d . . . . .
C7 C 0.4485(4) 0.3253(3) 0.0539(3) 0.0292(6) Uani 1 1 d . . . . .
C8 C 0.1922(4) 0.3421(4) -0.0767(3) 0.0353(7) Uani 1 1 d . . . . .
H8 H 0.0955 0.3132 -0.1551 0.042 Uiso 1 1 calc R . . . .
C9 C 0.2265(4) 0.4454(4) 0.0284(4) 0.0367(7) Uani 1 1 d . . . . .
H9 H 0.1526 0.4846 0.0205 0.044 Uiso 1 1 calc R . . . .
C10 C 0.3723(4) 0.4914(4) 0.1468(3) 0.0340(7) Uani 1 1 d . . . . .
H10 H 0.3954 0.5618 0.2168 0.041 Uiso 1 1 calc R . . . .
C11 C 0.4819(4) 0.4320(3) 0.1598(3) 0.0297(6) Uani 1 1 d . . . . .
C12 C 0.6345(4) 0.4813(3) 0.2821(3) 0.0292(6) Uani 1 1 d . . . . .
C13 C 0.6909(4) 0.7605(4) 0.6374(3) 0.0344(7) Uani 1 1 d . . . . .
H13 H 0.6037 0.7129 0.5533 0.041 Uiso 1 1 calc R . . . .
C14 C 0.5530(5) 0.9072(4) 0.6551(4) 0.0440(8) Uani 1 1 d . . . . .
H14A H 0.5937 1.0029 0.6401 0.066 Uiso 1 1 calc GR . . . .
H14B H 0.5069 0.9041 0.7197 0.066 Uiso 1 1 calc GR . . . .
H14C H 0.4705 0.8437 0.5705 0.066 Uiso 1 1 calc GR . . . .
C15 C 0.8240(5) 0.9505(5) 0.8350(4) 0.0516(9) Uani 1 1 d . . . . .
H15A H 0.8710 1.0468 0.8233 0.077 Uiso 1 1 calc GR . . . .
H15B H 0.9047 0.9125 0.8598 0.077 Uiso 1 1 calc GR . . . .
H15C H 0.7872 0.9499 0.9057 0.077 Uiso 1 1 calc GR . . . .
Dy1 Dy 0.92896(2) 0.62597(2) 0.58267(2) 0.02827(8) Uani 1 1 d . . . . .
N1 N 0.6863(3) 0.8630(3) 0.7080(3) 0.0343(6) Uani 1 1 d . . . . .
N2 N 0.7951(4) 0.3849(3) 0.6976(3) 0.0369(6) Uani 1 1 d . . . . .
N3 N 1.1035(4) 0.8763(3) 0.5023(3) 0.0385(6) Uani 1 1 d . . . . .
N4 N 0.7339(3) 0.4134(3) 0.2881(3) 0.0289(5) Uani 1 1 d . . . . .
O1 O 0.8064(3) 0.7229(3) 0.6770(2) 0.0370(5) Uani 1 1 d . . . . .
O2 O 1.0474(3) 0.8828(3) 0.5894(3) 0.0469(6) Uani 1 1 d . . . . .
O3 O 1.2024(4) 0.9816(3) 0.4874(3) 0.0619(8) Uani 1 1 d . . . . .
O4 O 1.0515(4) 0.7534(3) 0.4345(3) 0.0519(7) Uani 1 1 d . . . . .
O5 O 0.7088(3) 0.4044(3) 0.5845(2) 0.0418(5) Uani 1 1 d . . . . .
O6 O 0.9375(3) 0.4839(3) 0.7611(2) 0.0390(5) Uani 1 1 d . . . . .
O7 O 0.7447(4) 0.2800(3) 0.7436(3) 0.0517(7) Uani 1 1 d . . . . .
O8 O 0.8730(3) 0.4549(2) 0.4033(2) 0.0332(5) Uani 1 1 d . . . . .
O9 O 0.6802(3) 0.5769(3) 0.3808(2) 0.0354(5) Uani 1 1 d . . . . .
O10 O 0.8121(3) 0.2603(3) 0.2127(2) 0.0358(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.455(4) . ?
C1 N4 1.374(4) . ?
C1 O10 1.238(4) . ?
C2 C3 1.377(5) . ?
C2 C7 1.421(5) . ?
C3 C4 1.397(5) . ?
C4 C5 1.372(6) . ?
C5 C6 1.404(5) . ?
C6 C7 1.421(4) . ?
C6 C8 1.416(5) . ?
C7 C11 1.413(5) . ?
C8 C9 1.381(5) . ?
C9 C10 1.401(5) . ?
C10 C11 1.386(5) . ?
C11 C12 1.457(4) . ?
C12 N4 1.377(4) . ?
C12 O9 1.247(4) . ?
C13 N1 1.308(4) . ?
C13 O1 1.254(4) . ?
C14 N1 1.457(5) . ?
C15 N1 1.456(5) . ?
Dy1 N2 2.901(3) . ?
Dy1 N3 2.878(3) . ?
Dy1 O1 2.286(2) . ?
Dy1 O2 2.445(3) . ?
Dy1 O4 2.476(3) . ?
Dy1 O5 2.486(3) . ?
Dy1 O6 2.456(2) . ?
Dy1 O8 2.332(2) 2_766 ?
Dy1 O8 2.331(2) . ?
Dy1 O9 2.430(2) . ?
Dy1 O10 2.456(2) 2_766 ?
N2 O5 1.269(4) . ?
N2 O6 1.269(4) . ?
N2 O7 1.216(4) . ?
N3 O2 1.267(4) . ?
N3 O3 1.216(4) . ?
N3 O4 1.256(4) . ?
N4 O8 1.352(3) . ?
O8 Dy1 2.332(2) 2_766 ?
O10 Dy1 2.456(2) 2_766 ?

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
N4 C1 C2 116.8(3) . . ?
O10 C1 C2 124.9(3) . . ?
O10 C1 N4 118.3(3) . . ?
C3 C2 C1 121.1(3) . . ?
C3 C2 C7 120.2(3) . . ?
C7 C2 C1 118.8(3) . . ?
C2 C3 C4 120.6(3) . . ?
C5 C4 C3 120.3(3) . . ?
C4 C5 C6 121.0(3) . . ?
C5 C6 C7 119.1(3) . . ?
C5 C6 C8 122.5(3) . . ?
C7 C6 C8 118.3(3) . . ?
C6 C7 C2 118.8(3) . . ?
C11 C7 C2 121.5(3) . . ?
C11 C7 C6 119.6(3) . . ?
C9 C8 C6 121.1(3) . . ?
C8 C9 C10 120.3(3) . . ?
C11 C10 C9 120.1(3) . . ?
C7 C11 C12 119.4(3) . . ?
C10 C11 C7 120.5(3) . . ?
C10 C11 C12 120.1(3) . . ?
N4 C12 C11 116.1(3) . . ?
O9 C12 C11 125.7(3) . . ?
O9 C12 N4 118.2(3) . . ?
O1 C13 N1 123.6(3) . . ?
N3 Dy1 N2 171.99(8) . . ?
O1 Dy1 N2 82.78(8) . . ?
O1 Dy1 N3 98.16(9) . . ?
O1 Dy1 O2 73.47(9) . . ?
O1 Dy1 O4 119.55(9) . . ?
O1 Dy1 O5 79.89(9) . . ?
O1 Dy1 O6 84.38(8) . . ?
O1 Dy1 O8 142.49(8) . . ?
O1 Dy1 O8 152.74(8) . 2_766 ?
O1 Dy1 O9 80.90(8) . . ?
O1 Dy1 O10 90.88(8) . 2_766 ?
O2 Dy1 N2 151.42(8) . . ?
O2 Dy1 N3 25.95(9) . . ?
O2 Dy1 O4 51.30(9) . . ?
O2 Dy1 O5 151.62(9) . . ?
O2 Dy1 O6 133.01(8) . . ?
O2 Dy1 O10 71.19(9) . 2_766 ?
O4 Dy1 N2 156.64(8) . . ?
O4 Dy1 N3 25.77(9) . . ?
O4 Dy1 O5 143.44(9) . . ?
O5 Dy1 N2 25.79(8) . . ?
O5 Dy1 N3 162.22(8) . . ?
O6 Dy1 N2 25.72(8) . . ?
O6 Dy1 N3 146.30(8) . . ?
O6 Dy1 O4 150.34(9) . . ?
O6 Dy1 O5 51.42(8) . . ?
O6 Dy1 O10 68.23(8) . 2_766 ?
O8 Dy1 N2 85.63(8) . . ?
O8 Dy1 N2 87.12(8) 2_766 . ?
O8 Dy1 N3 98.15(9) . . ?
O8 Dy1 N3 88.55(9) 2_766 . ?
O8 Dy1 O2 106.85(9) 2_766 . ?
O8 Dy1 O2 122.94(8) . . ?
O8 Dy1 O4 75.50(9) 2_766 . ?
O8 Dy1 O4 72.40(9) . . ?
O8 Dy1 O5 101.29(8) 2_766 . ?
O8 Dy1 O5 74.43(8) . . ?
O8 Dy1 O6 99.87(8) . . ?
O8 Dy1 O6 75.83(8) 2_766 . ?
O8 Dy1 O8 60.99(8) . 2_766 ?
O8 Dy1 O9 65.36(7) . . ?
O8 Dy1 O9 125.63(7) 2_766 . ?
O8 Dy1 O10 125.51(7) . 2_766 ?
O8 Dy1 O10 64.56(7) 2_766 2_766 ?
O9 Dy1 N2 97.30(8) . . ?
O9 Dy1 N3 90.70(8) . . ?
O9 Dy1 O2 94.46(9) . . ?
O9 Dy1 O4 80.95(9) . . ?
O9 Dy1 O5 71.52(8) . . ?
O9 Dy1 O6 122.71(8) . . ?
O9 Dy1 O10 165.10(8) . 2_766 ?
O10 Dy1 N2 93.94(8) 2_766 . ?
O10 Dy1 N3 78.11(8) 2_766 . ?
O10 Dy1 O4 92.54(10) 2_766 . ?
O10 Dy1 O5 119.45(8) 2_766 . ?
C13 N1 C14 121.6(3) . . ?
C13 N1 C15 121.4(3) . . ?
C14 N1 C15 116.5(3) . . ?
O5 N2 Dy1 58.50(16) . . ?
O5 N2 O6 115.4(3) . . ?
O6 N2 Dy1 57.13(16) . . ?
O7 N2 Dy1 175.8(2) . . ?
O7 N2 O5 122.6(3) . . ?
O7 N2 O6 122.0(3) . . ?
O2 N3 Dy1 57.59(16) . . ?
O3 N3 Dy1 168.0(2) . . ?
O3 N3 O2 122.1(3) . . ?
O3 N3 O4 122.7(3) . . ?
O4 N3 Dy1 58.98(17) . . ?
O4 N3 O2 115.2(3) . . ?
C1 N4 C12 127.3(3) . . ?
O8 N4 C1 116.2(2) . . ?
O8 N4 C12 116.5(2) . . ?
C13 O1 Dy1 138.1(2) . . ?
N3 O2 Dy1 96.5(2) . . ?
N3 O4 Dy1 95.26(19) . . ?
N2 O5 Dy1 95.71(18) . . ?
N2 O6 Dy1 97.15(18) . . ?
Dy1 O8 Dy1 119.01(8) . 2_766 ?
N4 O8 Dy1 120.61(17) . 2_766 ?
N4 O8 Dy1 120.11(17) . . ?
C12 O9 Dy1 119.6(2) . . ?
C1 O10 Dy1 119.3(2) . 2_766 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.798
_oxdiff_exptl_absorpt_empirical_full_min 0.719
####################################################################### 
# 
# 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_aw823c
_database_code_depnum_ccdc_archive 'CCDC 2278245'
loop_
_audit_author_name
_audit_author_address
'Luis Cunha Silva'
;Univ of Porto
Portugal
;
_audit_update_record             
;
2023-06-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H12 Dy2 N8 O24, 2(C2 H3 N), 2(C4 H12 N)'
_chemical_formula_sum            'C36 H42 Dy2 N12 O24'
_chemical_formula_weight         1351.81
_chemical_melting_point          ?
_chemical_oxdiff_formula         DyCNO
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9643(3)
_cell_length_b                   11.4838(3)
_cell_length_c                   11.7527(5)
_cell_angle_alpha                115.252(3)
_cell_angle_beta                 109.857(3)
_cell_angle_gamma                96.441(2)
_cell_volume                     1199.95(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7372
_cell_measurement_temperature    293.0(1)
_cell_measurement_theta_max      76.4880
_cell_measurement_theta_min      4.4380
_shelx_estimated_absorpt_T_max   0.478
_shelx_estimated_absorpt_T_min   0.338
_exptl_absorpt_coefficient_mu    17.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10900
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         4.466
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -90.00 -45.00   1.00    0.10    --  -48.45 -49.00 147.00   45
  2  ω     47.00 121.00   1.00    0.10    --   48.45  49.00 -64.00   74
  3  ω     -7.00  58.00   1.00    0.10    --   48.45 -49.00 147.00   65
  4  ω   -159.00 -73.00   1.00    0.20    --  -86.25 -49.00 147.00   86
  5  ω    -48.00 -14.00   1.00    0.20    --  -86.25  49.00 -64.00   34
  6  ω     86.00 118.00   1.00    0.20    --  107.75 -49.00 147.00   32
  7  ω     37.00  63.00   1.00    0.20    --  107.75 -49.00 147.00   26
  8  ω     95.00 177.00   1.00    0.20    --  107.75  49.00 -64.00   82
  9  ω   -120.00 -71.00   1.00    0.10    --  -48.45-125.00  90.00   49
 10  ω    -61.00 -32.00   1.00    0.10    --  -48.45  49.00 -64.00   29
 11  ω   -119.00 -75.00   1.00    0.10    --  -48.45-125.00-150.00   44
 12  ω    -24.00  15.00   1.00    0.10    --  -48.45  49.00 -64.00   39
 13  ω     39.00  96.00   1.00    0.10    --   48.45-125.00-180.00   57
 14  ω    -58.00 -13.00   1.00    0.20    --  -86.25 125.00  30.00   45
 15  ω    -90.00 -63.00   1.00    0.20    --  -86.25 125.00  30.00   27
 16  ω     40.00  95.00   1.00    0.20    --  107.75 -99.00  60.00   55
 17  ω     35.00 125.00   1.00    0.20    --  107.75 -77.00 120.00   90
 18  ω     35.00 116.00   1.00    0.20    --  107.75-125.00  30.00   81
 19  ω     95.00 172.00   1.00    0.20    --  107.75  57.00-150.00   77
 20  ω     93.00 177.00   1.00    0.20    --  107.75  57.00-180.00   84
 21  ω    110.00 178.00   1.00    0.20    --  107.75 125.00  90.00   68
 22  ω     44.00 115.00   1.00    0.20    --  107.75-125.00 -60.00   71
 23  ω     35.00 109.00   1.00    0.20    --  107.75 -99.00 120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0978183000
_diffrn_orient_matrix_UB_12      0.0708067000
_diffrn_orient_matrix_UB_13      0.0500285000
_diffrn_orient_matrix_UB_21      0.1053846000
_diffrn_orient_matrix_UB_22      0.0625108000
_diffrn_orient_matrix_UB_23      0.1525524000
_diffrn_orient_matrix_UB_31      0.0623373000
_diffrn_orient_matrix_UB_32      0.1236551000
_diffrn_orient_matrix_UB_33      -0.0052616000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3823
_reflns_number_total             4225
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0282
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0268P)²+0.8884P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0696
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.69373(2) 0.57724(2) 0.65936(2) 0.01546(8) Uani 1 1 d . . . . .
O1 O 0.7634(2) 0.7416(3) 0.5961(3) 0.0202(6) Uani 1 1 d . . . . .
O2 O 0.5173(2) 0.5971(2) 0.4912(3) 0.0185(6) Uani 1 1 d . . . . .
O3 O 0.3199(3) 0.6310(2) 0.3248(3) 0.0202(6) Uani 1 1 d . . . . .
O4 O 0.6384(3) 0.7705(3) 0.8017(3) 0.0290(6) Uani 1 1 d . . . . .
O5 O 0.5537(3) 0.5863(3) 0.7924(3) 0.0280(6) Uani 1 1 d . . . . .
O6 O 0.5100(3) 0.7697(4) 0.9077(4) 0.0496(9) Uani 1 1 d . . . . .
O7 O 0.8462(3) 0.6198(3) 0.8906(3) 0.0254(6) Uani 1 1 d . . . . .
O8 O 0.9132(3) 0.7716(3) 0.8474(3) 0.0314(7) Uani 1 1 d . . . . .
O9 O 1.0338(3) 0.7826(3) 1.0441(3) 0.0356(7) Uani 1 1 d . . . . .
O10 O 0.8901(3) 0.5140(3) 0.6320(3) 0.0268(6) Uani 1 1 d . . . . .
O11 O 0.8928(3) 0.3647(3) 0.4411(3) 0.0306(7) Uani 1 1 d . . . . .
O12 O 0.7094(3) 0.4240(3) 0.4387(3) 0.0274(6) Uani 1 1 d . . . . .
N1 N 0.5432(3) 0.6977(3) 0.4634(3) 0.0161(6) Uani 1 1 d . . . . .
N2 N 0.8328(3) 0.4320(3) 0.5006(3) 0.0214(7) Uani 1 1 d . . . . .
N3 N 0.9342(3) 0.7275(3) 0.9314(3) 0.0211(7) Uani 1 1 d . . . . .
N4 N 0.5649(3) 0.7095(4) 0.8357(4) 0.0270(8) Uani 1 1 d . . . . .
C1 C 0.4324(4) 0.7113(4) 0.3747(4) 0.0162(7) Uani 1 1 d . . . . .
C2 C 0.4608(4) 0.8223(4) 0.3474(4) 0.0170(7) Uani 1 1 d . . . . .
C3 C 0.3554(4) 0.8475(4) 0.2646(4) 0.0225(8) Uani 1 1 d . . . . .
H3 H 0.2663 0.7937 0.2256 0.027 Uiso 1 1 calc R . . . .
C4 C 0.3833(4) 0.9540(4) 0.2398(4) 0.0264(9) Uani 1 1 d . . . . .
H4 H 0.3122 0.9698 0.1832 0.032 Uiso 1 1 calc R . . . .
C5 C 0.5136(5) 1.0356(4) 0.2976(4) 0.0262(9) Uani 1 1 d . . . . .
H5 H 0.5300 1.1055 0.2792 0.031 Uiso 1 1 calc R . . . .
C6 C 0.6243(4) 1.0143(4) 0.3855(4) 0.0238(8) Uani 1 1 d . . . . .
C7 C 0.5964(4) 0.9037(4) 0.4076(4) 0.0189(8) Uani 1 1 d . . . . .
C8 C 0.7059(4) 0.8825(4) 0.4958(4) 0.0176(7) Uani 1 1 d . . . . .
C9 C 0.8358(4) 0.9667(4) 0.5591(4) 0.0236(8) Uani 1 1 d . . . . .
H9 H 0.9063 0.9521 0.6177 0.028 Uiso 1 1 calc R . . . .
C10 C 0.8629(4) 1.0748(4) 0.5359(5) 0.0306(10) Uani 1 1 d . . . . .
H10 H 0.9513 1.1317 0.5788 0.037 Uiso 1 1 calc R . . . .
C11 C 0.7592(5) 1.0969(4) 0.4500(5) 0.0301(10) Uani 1 1 d . . . . .
H11 H 0.7786 1.1680 0.4341 0.036 Uiso 1 1 calc R . . . .
C12 C 0.6767(4) 0.7721(4) 0.5234(4) 0.0171(7) Uani 1 1 d . . . . .
N5 N 0.8041(5) 0.8456(5) 1.1888(5) 0.0515(11) Uani 1 1 d . . . . .
C13 C 0.8083(5) 0.9277(5) 1.1602(5) 0.0393(11) Uani 1 1 d . . . . .
C14 C 0.8148(7) 1.0346(6) 1.1250(6) 0.0620(17) Uani 1 1 d . . . . .
H14A H 0.7243 1.0325 1.0742 0.093 Uiso 1 1 calc GR . . . .
H14B H 0.8635 1.0213 1.0685 0.093 Uiso 1 1 calc GR . . . .
H14C H 0.8610 1.1205 1.2089 0.093 Uiso 1 1 calc GR . . . .
N6 N 0.2047(3) 0.4995(3) 0.8500(3) 0.0232(7) Uani 1 1 d . . . . .
C15 C 0.3285(5) 0.5133(5) 0.9658(5) 0.0416(12) Uani 1 1 d . . . . .
H15A H 0.4084 0.5539 0.9635 0.062 Uiso 1 1 calc GR . . . .
H15B H 0.3293 0.4256 0.9548 0.062 Uiso 1 1 calc GR . . . .
H15C H 0.3273 0.5692 1.0535 0.062 Uiso 1 1 calc GR . . . .
C16 C 0.2053(5) 0.4096(5) 0.7134(5) 0.0347(10) Uani 1 1 d . . . . .
H16A H 0.1235 0.3966 0.6387 0.052 Uiso 1 1 calc GR . . . .
H16B H 0.2100 0.3238 0.7060 0.052 Uiso 1 1 calc GR . . . .
H16C H 0.2828 0.4506 0.7079 0.052 Uiso 1 1 calc GR . . . .
C17 C 0.2055(4) 0.6352(4) 0.8641(5) 0.0300(9) Uani 1 1 d . . . . .
H17A H 0.1271 0.6258 0.7882 0.045 Uiso 1 1 calc GR . . . .
H17B H 0.2865 0.6743 0.8624 0.045 Uiso 1 1 calc GR . . . .
H17C H 0.2032 0.6929 0.9508 0.045 Uiso 1 1 calc GR . . . .
C18 C 0.0812(4) 0.4388(5) 0.8555(5) 0.0337(10) Uani 1 1 d . . . . .
H18A H 0.0803 0.4966 0.9428 0.051 Uiso 1 1 calc GR . . . .
H18B H 0.0821 0.3519 0.8468 0.051 Uiso 1 1 calc GR . . . .
H18C H 0.0015 0.4285 0.7804 0.051 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.441(2) . ?
Dy1 O2 2.377(2) 2_666 ?
Dy1 O2 2.364(2) . ?
Dy1 O3 2.469(2) 2_666 ?
Dy1 O4 2.433(3) . ?
Dy1 O5 2.518(3) . ?
Dy1 O7 2.452(3) . ?
Dy1 O8 2.575(3) . ?
Dy1 O10 2.426(3) . ?
Dy1 O12 2.516(3) . ?
Dy1 N2 2.904(3) . ?
Dy1 N4 2.895(3) . ?
O1 C12 1.239(4) . ?
O2 Dy1 2.377(2) 2_666 ?
O2 N1 1.355(3) . ?
O3 Dy1 2.469(2) 2_666 ?
O3 C1 1.228(4) . ?
O4 N4 1.277(4) . ?
O5 N4 1.257(4) . ?
O6 N4 1.223(5) . ?
O7 N3 1.266(4) . ?
O8 N3 1.258(4) . ?
O9 N3 1.222(4) . ?
O10 N2 1.278(4) . ?
O11 N2 1.218(4) . ?
O12 N2 1.271(4) . ?
N1 C1 1.382(5) . ?
N1 C12 1.368(5) . ?
C1 C2 1.467(5) . ?
C2 C3 1.384(5) . ?
C2 C7 1.412(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.398(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.371(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.424(6) . ?
C6 C7 1.423(5) . ?
C6 C11 1.405(6) . ?
C7 C8 1.418(5) . ?
C8 C9 1.369(5) . ?
C8 C12 1.465(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.403(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.371(6) . ?
C11 H11 0.9300 . ?
N5 C13 1.129(7) . ?
C13 C14 1.455(7) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
N6 C15 1.494(5) . ?
N6 C16 1.496(5) . ?
N6 C17 1.494(5) . ?
N6 C18 1.487(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O3 156.44(9) . 2_666 ?
O1 Dy1 O5 128.69(9) . . ?
O1 Dy1 O7 115.03(8) . . ?
O1 Dy1 O8 64.87(8) . . ?
O1 Dy1 O12 79.69(9) . . ?
O1 Dy1 N2 81.36(8) . . ?
O1 Dy1 N4 103.64(10) . . ?
O2 Dy1 O1 64.32(8) . . ?
O2 Dy1 O1 120.04(8) 2_666 . ?
O2 Dy1 O2 58.82(9) . 2_666 ?
O2 Dy1 O3 122.71(8) . 2_666 ?
O2 Dy1 O3 64.13(8) 2_666 2_666 ?
O2 Dy1 O4 77.21(10) . . ?
O2 Dy1 O4 105.12(9) 2_666 . ?
O2 Dy1 O5 70.70(9) 2_666 . ?
O2 Dy1 O5 90.97(9) . . ?
O2 Dy1 O7 124.75(8) 2_666 . ?
O2 Dy1 O7 157.96(10) . . ?
O2 Dy1 O8 123.47(8) . . ?
O2 Dy1 O8 172.77(9) 2_666 . ?
O2 Dy1 O10 115.06(9) 2_666 . ?
O2 Dy1 O10 124.58(9) . . ?
O2 Dy1 O12 78.51(9) . . ?
O2 Dy1 O12 72.27(9) 2_666 . ?
O2 Dy1 N2 93.13(9) 2_666 . ?
O2 Dy1 N2 102.39(9) . . ?
O2 Dy1 N4 82.92(9) . . ?
O2 Dy1 N4 87.24(9) 2_666 . ?
O3 Dy1 O5 74.85(9) 2_666 . ?
O3 Dy1 O8 113.79(9) 2_666 . ?
O3 Dy1 O12 80.09(9) 2_666 . ?
O3 Dy1 N2 75.17(8) 2_666 . ?
O3 Dy1 N4 99.67(9) 2_666 . ?
O4 Dy1 O1 78.44(9) . . ?
O4 Dy1 O3 124.24(9) . 2_666 ?
O4 Dy1 O5 51.57(9) . . ?
O4 Dy1 O7 81.11(10) . . ?
O4 Dy1 O8 69.95(10) . . ?
O4 Dy1 O12 152.58(9) . . ?
O4 Dy1 N2 157.68(9) . . ?
O4 Dy1 N4 25.93(9) . . ?
O5 Dy1 O8 102.13(9) . . ?
O5 Dy1 N2 149.84(9) . . ?
O5 Dy1 N4 25.66(9) . . ?
O7 Dy1 O3 67.57(9) . 2_666 ?
O7 Dy1 O5 72.27(9) . . ?
O7 Dy1 O8 50.17(8) . . ?
O7 Dy1 O12 123.50(9) . . ?
O7 Dy1 N2 99.15(9) . . ?
O7 Dy1 N4 75.82(10) . . ?
O8 Dy1 N2 92.92(10) . . ?
O8 Dy1 N4 86.33(10) . . ?
O10 Dy1 O1 82.47(9) . . ?
O10 Dy1 O3 75.52(9) . 2_666 ?
O10 Dy1 O4 139.80(10) . . ?
O10 Dy1 O5 142.50(9) . . ?
O10 Dy1 O7 75.49(9) . . ?
O10 Dy1 O8 69.94(10) . . ?
O10 Dy1 O12 51.60(9) . . ?
O10 Dy1 N2 25.79(9) . . ?
O10 Dy1 N4 150.47(9) . . ?
O12 Dy1 O5 141.55(9) . . ?
O12 Dy1 O8 114.60(9) . . ?
O12 Dy1 N2 25.87(9) . . ?
O12 Dy1 N4 157.46(9) . . ?
N4 Dy1 N2 174.00(9) . . ?
C12 O1 Dy1 120.2(2) . . ?
Dy1 O2 Dy1 121.18(9) . 2_666 ?
N1 O2 Dy1 119.68(19) . . ?
N1 O2 Dy1 118.21(19) . 2_666 ?
C1 O3 Dy1 118.7(2) . 2_666 ?
N4 O4 Dy1 97.7(2) . . ?
N4 O5 Dy1 94.2(2) . . ?
N3 O7 Dy1 100.0(2) . . ?
N3 O8 Dy1 94.3(2) . . ?
N2 O10 Dy1 98.5(2) . . ?
N2 O12 Dy1 94.4(2) . . ?
O2 N1 C1 116.3(3) . . ?
O2 N1 C12 116.3(3) . . ?
C12 N1 C1 127.4(3) . . ?
O10 N2 Dy1 55.71(18) . . ?
O11 N2 Dy1 173.9(2) . . ?
O11 N2 O10 121.6(3) . . ?
O11 N2 O12 123.1(3) . . ?
O12 N2 Dy1 59.73(18) . . ?
O12 N2 O10 115.3(3) . . ?
O7 N3 Dy1 54.97(17) . . ?
O8 N3 Dy1 60.52(18) . . ?
O8 N3 O7 115.5(3) . . ?
O9 N3 Dy1 176.1(3) . . ?
O9 N3 O7 121.6(3) . . ?
O9 N3 O8 122.9(3) . . ?
O4 N4 Dy1 56.38(19) . . ?
O5 N4 Dy1 60.15(18) . . ?
O5 N4 O4 116.5(3) . . ?
O6 N4 Dy1 176.8(3) . . ?
O6 N4 O4 120.9(4) . . ?
O6 N4 O5 122.6(4) . . ?
O3 C1 N1 118.6(3) . . ?
O3 C1 C2 125.4(3) . . ?
N1 C1 C2 116.0(3) . . ?
C3 C2 C1 120.2(3) . . ?
C3 C2 C7 120.6(3) . . ?
C7 C2 C1 119.2(3) . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 121.1(4) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.7(3) . . ?
C6 C5 H5 119.7 . . ?
C7 C6 C5 118.2(4) . . ?
C11 C6 C5 122.9(3) . . ?
C11 C6 C7 118.8(4) . . ?
C2 C7 C6 119.6(3) . . ?
C2 C7 C8 121.8(3) . . ?
C8 C7 C6 118.6(4) . . ?
C7 C8 C12 118.7(3) . . ?
C9 C8 C7 121.0(3) . . ?
C9 C8 C12 120.2(3) . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.2(4) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 120.0 . . ?
C6 C11 H11 119.3 . . ?
C10 C11 C6 121.4(3) . . ?
C10 C11 H11 119.3 . . ?
O1 C12 N1 118.3(3) . . ?
O1 C12 C8 124.9(3) . . ?
N1 C12 C8 116.8(3) . . ?
N5 C13 C14 179.4(6) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 N6 C16 109.3(4) . . ?
C15 N6 C17 109.6(3) . . ?
C17 N6 C16 109.1(3) . . ?
C18 N6 C15 109.3(3) . . ?
C18 N6 C16 109.3(3) . . ?
C18 N6 C17 110.2(3) . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 H17A 109.5 . . ?
N6 C17 H17B 109.5 . . ?
N6 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N6 C18 H18A 109.5 . . ?
N6 C18 H18B 109.5 . . ?
N6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.727
####################################################################### 
# 
# 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_AW684Dsq
_database_code_depnum_ccdc_archive 'CCDC 2278246'
loop_
_audit_author_name
_audit_author_address
'Luis Cunha Silva'
;Univ of Porto
Portugal
;
_audit_update_record             
;
2023-06-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;

# ========================================================================= #

_audit_creation_method           'SHELXL-2019/2 and enCIFer'
_shelx_SHELXL_version_number     2019/2
_audit_creation_date             '05 January 2023'

# ========================================================================= #

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H28 Dy2 N6 O20, 2(C3 H7 N O)'
_chemical_formula_sum            'C54 H42 Dy2 N8 O22'
_chemical_formula_weight         1479.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   10.8846(5)
_cell_length_b                   12.5023(6)
_cell_length_c                   14.2375(6)
_cell_angle_alpha                64.886(4)
_cell_angle_beta                 84.877(3)
_cell_angle_gamma                76.325(4)
_cell_volume                     1704.45(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8299
_cell_measurement_theta_min      3.9600
_cell_measurement_theta_max      75.6410

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_F_000             730
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    12.224
_shelx_estimated_absorpt_T_min   0.374
_shelx_estimated_absorpt_T_max   0.441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_T_max  0.356
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15758
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.003
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_full        66.594
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_standards_number         3
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        0


_reflns_number_total             5965
_reflns_number_gt                5288
_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.
 
 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_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2019)'


_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)+(0.1701P)²+11.8409P] 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         5965
_refine_ls_number_parameters     427
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1606
_refine_ls_wR_factor_gt          0.1325
_refine_ls_goodness_of_fit_ref   0.700
_refine_ls_restrained_S_all      0.700
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.46776(3) 0.65321(3) 0.86418(2) 0.02222(15) Uani 1 1 d . . . . .
O4 O 0.5001(5) 0.7163(4) 0.6814(3) 0.0312(10) Uani 1 1 d . . . . .
O1 O 0.2767(4) 0.6060(4) 0.8172(4) 0.0335(10) Uani 1 1 d . . . . .
O2 O 0.3897(4) 0.4931(4) 0.9958(3) 0.0253(9) Uani 1 1 d . . . . .
O3 O 0.3243(4) 0.3041(4) 1.1368(3) 0.0316(10) Uani 1 1 d . . . . .
O5 O 0.5687(4) 0.4974(4) 0.8166(3) 0.0299(10) Uani 1 1 d . . . . .
O1W O 0.4266(5) 0.7165(5) 1.0093(3) 0.0374(11) Uani 1 1 d D . . . .
O7 O 0.4580(5) 0.8784(4) 0.7937(4) 0.0374(11) Uani 1 1 d . . . . .
O6 O 0.6796(6) 0.3249(5) 0.7584(4) 0.0465(13) Uani 1 1 d . . . . .
N1 N 0.2862(5) 0.4589(5) 0.9803(4) 0.0246(10) Uani 1 1 d . . . . .
N2 N 0.5879(5) 0.5238(5) 0.7137(4) 0.0300(12) Uani 1 1 d . . . . .
O8 O 0.2823(5) 0.8265(5) 0.8041(5) 0.0478(13) Uani 1 1 d . . . . .
N4 N 0.7114(6) 0.9603(5) 0.9723(4) 0.0348(12) Uani 1 1 d . . . . .
N3 N 0.3410(7) 0.9086(6) 0.7879(6) 0.0554(19) Uani 1 1 d . . . . .
C1 C 0.2272(5) 0.5253(6) 0.8844(5) 0.0257(13) Uani 1 1 d . . . . .
C17 C 0.6473(6) 0.4238(7) 0.6899(5) 0.0348(15) Uani 1 1 d . . . . .
C5 C 0.2551(6) 0.3586(5) 1.0591(5) 0.0247(12) Uani 1 1 d . . . . .
O10 O 0.6124(8) 0.8053(7) 1.0530(5) 0.073(2) Uani 1 1 d . . . . .
C13 C 0.5495(6) 0.6402(6) 0.6453(5) 0.0296(14) Uani 1 1 d . . . . .
C4 C 0.1403(6) 0.3255(6) 1.0457(5) 0.0300(13) Uani 1 1 d . . . . .
C12 C 0.0992(7) 0.2319(6) 1.1217(6) 0.0366(15) Uani 1 1 d . . . . .
H12 H 0.147410 0.185409 1.184042 0.044 Uiso 1 1 calc R U . . .
O9 O 0.2823(7) 1.0134(6) 0.7681(10) 0.114(4) Uani 1 1 d . U . . .
C2 C 0.1125(6) 0.4936(6) 0.8684(5) 0.0302(14) Uani 1 1 d . . . . .
C6 C 0.0417(7) 0.5611(8) 0.7784(6) 0.0385(16) Uani 1 1 d . . . . .
H6 H 0.069399 0.627323 0.724398 0.046 Uiso 1 1 calc R U . . .
C8 C -0.1145(7) 0.4382(8) 0.8454(6) 0.0420(17) Uani 1 1 d . . . . .
H8 H -0.192947 0.422065 0.837238 0.050 Uiso 1 1 calc R U . . .
C3 C 0.0702(6) 0.3960(7) 0.9501(5) 0.0314(14) Uani 1 1 d . . . . .
C10 C -0.0841(7) 0.2691(7) 1.0207(7) 0.0439(18) Uani 1 1 d . . . . .
H10 H -0.161575 0.250334 1.014125 0.053 Uiso 1 1 calc R U . . .
C15 C 0.6197(7) 0.5776(7) 0.5035(5) 0.0366(16) Uani 1 1 d . . . . .
C9 C -0.0430(7) 0.3658(7) 0.9383(6) 0.0395(16) Uani 1 1 d . . . . .
C11 C -0.0131(7) 0.2020(8) 1.1102(7) 0.0438(18) Uani 1 1 d . . . . .
H11 H -0.040075 0.135444 1.164183 0.053 Uiso 1 1 calc R U . . .
C16 C 0.6605(6) 0.4575(7) 0.5762(5) 0.0319(14) Uani 1 1 d . . . . .
C7 C -0.0711(7) 0.5323(9) 0.7664(7) 0.049(2) Uani 1 1 d . . . . .
H7 H -0.118228 0.577783 0.703387 0.058 Uiso 1 1 calc R U . . .
C21 C 0.6312(8) 0.6035(9) 0.3962(6) 0.048(2) Uani 1 1 d . . . . .
C14 C 0.5659(6) 0.6689(7) 0.5364(5) 0.0337(15) Uani 1 1 d . . . . .
C24 C 0.5240(8) 0.7851(8) 0.4656(6) 0.0452(18) Uani 1 1 d . . . . .
H24 H 0.486283 0.846493 0.488419 0.054 Uiso 1 1 calc R U . . .
C19 C 0.7223(8) 0.3936(9) 0.4382(6) 0.0476(19) Uani 1 1 d . . . . .
H19 H 0.757155 0.331220 0.415848 0.057 Uiso 1 1 calc R U . . .
C22 C 0.5872(10) 0.7246(10) 0.3247(7) 0.059(2) Uani 1 1 d . . . . .
H22 H 0.592933 0.744041 0.252493 0.071 Uiso 1 1 calc R U . . .
C20 C 0.6831(8) 0.5092(9) 0.3668(6) 0.047(2) Uani 1 1 d . . . . .
H20 H 0.691312 0.526247 0.295170 0.057 Uiso 1 1 calc R U . . .
C18 C 0.7117(8) 0.3653(9) 0.5453(7) 0.0476(19) Uani 1 1 d . . . . .
H18 H 0.739269 0.284473 0.595293 0.057 Uiso 1 1 calc R U . . .
C23 C 0.5366(10) 0.8149(9) 0.3564(6) 0.055(2) Uani 1 1 d . . . . .
H23 H 0.510254 0.896197 0.306884 0.066 Uiso 1 1 calc R U . . .
C26 C 0.7018(15) 0.8637(13) 1.0508(10) 0.036(3) Uani 0.5 1 d . . P A 2
H26 H 0.758292 0.832816 1.108070 0.043 Uiso 0.5 1 calc R U P A 2
C30 C 0.6345(17) 1.0076(13) 0.8783(10) 0.044(4) Uani 0.5 1 d . . P A 2
H30A H 0.585848 0.948697 0.883356 0.065 Uiso 0.5 1 calc R U P A 2
H30B H 0.689696 1.021921 0.817913 0.065 Uiso 0.5 1 calc R U P A 2
H30C H 0.576376 1.083888 0.870620 0.065 Uiso 0.5 1 calc R U P A 2
C28 C 0.8062(16) 1.0298(14) 0.9689(14) 0.046(4) Uani 0.5 1 d . . P A 2
H28A H 0.763151 1.112985 0.956423 0.070 Uiso 0.5 1 calc R U P A 2
H28B H 0.865684 1.030966 0.912706 0.070 Uiso 0.5 1 calc R U P A 2
H28C H 0.852452 0.991414 1.035141 0.070 Uiso 0.5 1 calc R U P A 2
C25 C 0.6178(15) 0.9008(14) 0.9700(13) 0.044(4) Uani 0.5 1 d . . P A 1
H25 H 0.563202 0.928871 0.911923 0.053 Uiso 0.5 1 calc R U P A 1
C29 C 0.732(3) 1.0652(18) 0.8841(19) 0.080(7) Uani 0.5 1 d . . P A 1
H29A H 0.657362 1.100912 0.838472 0.120 Uiso 0.5 1 calc R U P A 1
H29B H 0.805705 1.042177 0.846144 0.120 Uiso 0.5 1 calc R U P A 1
H29C H 0.747776 1.124522 0.907007 0.120 Uiso 0.5 1 calc R U P A 1
C27 C 0.781(3) 0.913(3) 1.065(2) 0.104(10) Uani 0.5 1 d . . P A 1
H27A H 0.741897 0.852691 1.119530 0.156 Uiso 0.5 1 calc R U P A 1
H27B H 0.782169 0.979161 1.084635 0.156 Uiso 0.5 1 calc R U P A 1
H27C H 0.867858 0.875837 1.054145 0.156 Uiso 0.5 1 calc R U P A 1
H2W H 0.481(12) 0.755(11) 1.019(10) 0.13(6) Uiso 1 1 d D . . . .
H1W H 0.423(15) 0.652(9) 1.070(6) 0.14(6) 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 O5 2.332(4) . ?
Dy1 O2 2.362(4) . ?
Dy1 O4 2.396(4) . ?
Dy1 O2 2.417(4) 2_667 ?
Dy1 O3 2.442(5) 2_667 ?
Dy1 O1W 2.480(5) . ?
Dy1 O8 2.483(5) . ?
Dy1 O1 2.507(5) . ?
Dy1 O7 2.535(5) . ?
O4 C13 1.259(8) . ?
O1 C1 1.253(8) . ?
O2 N1 1.360(6) . ?
O3 C5 1.234(8) . ?
O5 N2 1.366(7) . ?
O1W H2W 0.90(2) . ?
O1W H1W 0.90(2) . ?
O7 N3 1.240(9) . ?
O6 C17 1.199(9) . ?
N1 C5 1.374(8) . ?
N1 C1 1.381(8) . ?
N2 C13 1.350(9) . ?
N2 C17 1.426(9) . ?
O8 N3 1.264(9) . ?
N4 C26 1.269(16) . ?
N4 C27 1.40(3) . ?
N4 C25 1.406(18) . ?
N4 C29 1.43(2) . ?
N4 C30 1.461(15) . ?
N4 C28 1.484(16) . ?
N3 O9 1.236(10) . ?
C1 C2 1.460(9) . ?
C17 C16 1.493(9) . ?
C5 C4 1.457(9) . ?
O10 C25 1.285(18) . ?
O10 C26 1.339(17) . ?
C13 C14 1.440(9) . ?
C4 C12 1.351(10) . ?
C4 C3 1.436(10) . ?
C12 C11 1.401(10) . ?
C12 H12 0.9500 . ?
C2 C6 1.378(10) . ?
C2 C3 1.421(10) . ?
C6 C7 1.402(11) . ?
C6 H6 0.9500 . ?
C8 C7 1.384(13) . ?
C8 C9 1.418(11) . ?
C8 H8 0.9500 . ?
C3 C9 1.414(9) . ?
C10 C11 1.373(12) . ?
C10 C9 1.412(12) . ?
C10 H10 0.9500 . ?
C15 C14 1.398(11) . ?
C15 C16 1.403(11) . ?
C15 C21 1.422(10) . ?
C11 H11 0.9500 . ?
C16 C18 1.383(11) . ?
C7 H7 0.9500 . ?
C21 C20 1.394(13) . ?
C21 C22 1.412(14) . ?
C14 C24 1.364(11) . ?
C24 C23 1.438(11) . ?
C24 H24 0.9500 . ?
C19 C20 1.357(13) . ?
C19 C18 1.413(11) . ?
C19 H19 0.9500 . ?
C22 C23 1.369(15) . ?
C22 H22 0.9500 . ?
C20 H20 0.9500 . ?
C18 H18 0.9500 . ?
C23 H23 0.9500 . ?
C26 H26 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C25 H25 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?

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
O5 Dy1 O2 81.34(15) . . ?
O5 Dy1 O4 65.65(14) . . ?
O2 Dy1 O4 134.75(15) . . ?
O5 Dy1 O2 72.38(14) . 2_667 ?
O2 Dy1 O2 62.11(16) . 2_667 ?
O4 Dy1 O2 127.90(15) . 2_667 ?
O5 Dy1 O3 87.25(16) . 2_667 ?
O2 Dy1 O3 125.89(14) . 2_667 ?
O4 Dy1 O3 84.11(16) . 2_667 ?
O2 Dy1 O3 64.00(14) 2_667 2_667 ?
O5 Dy1 O1W 144.85(15) . . ?
O2 Dy1 O1W 76.55(17) . . ?
O4 Dy1 O1W 146.23(16) . . ?
O2 Dy1 O1W 73.19(15) 2_667 . ?
O3 Dy1 O1W 84.05(17) 2_667 . ?
O5 Dy1 O8 137.14(18) . . ?
O2 Dy1 O8 105.10(16) . . ?
O4 Dy1 O8 82.36(18) . . ?
O2 Dy1 O8 148.39(18) 2_667 . ?
O3 Dy1 O8 118.25(16) 2_667 . ?
O1W Dy1 O8 75.72(19) . . ?
O5 Dy1 O1 81.10(16) . . ?
O2 Dy1 O1 63.95(14) . . ?
O4 Dy1 O1 80.44(16) . . ?
O2 Dy1 O1 122.36(15) 2_667 . ?
O3 Dy1 O1 163.48(16) 2_667 . ?
O1W Dy1 O1 112.14(17) . . ?
O8 Dy1 O1 65.45(17) . . ?
O5 Dy1 O7 135.45(16) . . ?
O2 Dy1 O7 143.19(16) . . ?
O4 Dy1 O7 75.14(16) . . ?
O2 Dy1 O7 121.83(15) 2_667 . ?
O3 Dy1 O7 67.95(15) 2_667 . ?
O1W Dy1 O7 71.10(17) . . ?
O8 Dy1 O7 50.33(16) . . ?
O1 Dy1 O7 113.11(15) . . ?
C13 O4 Dy1 120.6(4) . . ?
C1 O1 Dy1 119.5(4) . . ?
N1 O2 Dy1 121.8(3) . . ?
N1 O2 Dy1 117.1(3) . 2_667 ?
Dy1 O2 Dy1 117.89(16) . 2_667 ?
C5 O3 Dy1 120.6(4) . 2_667 ?
N2 O5 Dy1 118.7(3) . . ?
Dy1 O1W H2W 118(10) . . ?
Dy1 O1W H1W 110(10) . . ?
H2W O1W H1W 107(3) . . ?
N3 O7 Dy1 95.1(4) . . ?
O2 N1 C5 116.9(5) . . ?
O2 N1 C1 116.4(5) . . ?
C5 N1 C1 126.7(5) . . ?
C13 N2 O5 117.6(5) . . ?
C13 N2 C17 126.7(6) . . ?
O5 N2 C17 115.8(5) . . ?
N3 O8 Dy1 96.9(4) . . ?
C27 N4 C25 117.3(14) . . ?
C27 N4 C29 121.9(17) . . ?
C25 N4 C29 120.8(13) . . ?
C26 N4 C30 122.7(10) . . ?
C26 N4 C28 121.6(10) . . ?
C30 N4 C28 115.6(10) . . ?
O9 N3 O7 122.6(7) . . ?
O9 N3 O8 120.4(7) . . ?
O7 N3 O8 117.0(6) . . ?
O1 C1 N1 118.2(5) . . ?
O1 C1 C2 124.8(6) . . ?
N1 C1 C2 117.0(6) . . ?
O6 C17 N2 120.0(6) . . ?
O6 C17 C16 126.8(6) . . ?
N2 C17 C16 113.2(6) . . ?
O3 C5 N1 118.2(5) . . ?
O3 C5 C4 124.5(6) . . ?
N1 C5 C4 117.2(5) . . ?
O4 C13 N2 117.4(6) . . ?
O4 C13 C14 124.4(6) . . ?
N2 C13 C14 118.2(6) . . ?
C12 C4 C3 120.4(6) . . ?
C12 C4 C5 121.1(6) . . ?
C3 C4 C5 118.4(6) . . ?
C4 C12 C11 121.3(7) . . ?
C4 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C6 C2 C3 120.2(6) . . ?
C6 C2 C1 120.9(7) . . ?
C3 C2 C1 118.8(6) . . ?
C2 C6 C7 120.0(8) . . ?
C2 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C7 C8 C9 120.6(7) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C9 C3 C2 120.1(7) . . ?
C9 C3 C4 118.3(6) . . ?
C2 C3 C4 121.5(6) . . ?
C11 C10 C9 120.7(7) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C14 C15 C16 120.5(6) . . ?
C14 C15 C21 120.9(7) . . ?
C16 C15 C21 118.6(7) . . ?
C10 C9 C3 119.3(7) . . ?
C10 C9 C8 122.4(7) . . ?
C3 C9 C8 118.3(7) . . ?
C10 C11 C12 119.9(7) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C18 C16 C15 121.4(7) . . ?
C18 C16 C17 117.4(7) . . ?
C15 C16 C17 121.2(6) . . ?
C8 C7 C6 120.7(7) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C20 C21 C22 123.5(7) . . ?
C20 C21 C15 119.0(8) . . ?
C22 C21 C15 117.5(8) . . ?
C24 C14 C15 120.4(7) . . ?
C24 C14 C13 119.4(7) . . ?
C15 C14 C13 120.2(6) . . ?
C14 C24 C23 120.2(8) . . ?
C14 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C20 C19 C18 120.6(8) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C23 C22 C21 121.9(8) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C19 C20 C21 121.6(7) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C16 C18 C19 118.8(8) . . ?
C16 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C22 C23 C24 119.2(9) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
N4 C26 O10 120.2(11) . . ?
N4 C26 H26 119.9 . . ?
O10 C26 H26 119.9 . . ?
N4 C30 H30A 109.5 . . ?
N4 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N4 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N4 C28 H28A 109.5 . . ?
N4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O10 C25 N4 114.3(13) . . ?
O10 C25 H25 122.9 . . ?
N4 C25 H25 122.9 . . ?
N4 C29 H29A 109.5 . . ?
N4 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N4 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N4 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N4 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

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
Dy1 O2 N1 C5 174.9(4) . . . . ?
Dy1 O2 N1 C5 15.6(6) 2_667 . . . ?
Dy1 O2 N1 C1 -1.8(6) . . . . ?
Dy1 O2 N1 C1 -161.1(4) 2_667 . . . ?
Dy1 O5 N2 C13 1.5(7) . . . . ?
Dy1 O5 N2 C17 -178.5(4) . . . . ?
Dy1 O7 N3 O9 171.2(10) . . . . ?
Dy1 O7 N3 O8 -8.3(8) . . . . ?
Dy1 O8 N3 O9 -171.0(10) . . . . ?
Dy1 O8 N3 O7 8.5(8) . . . . ?
Dy1 O1 C1 N1 -4.8(7) . . . . ?
Dy1 O1 C1 C2 176.8(4) . . . . ?
O2 N1 C1 O1 4.3(8) . . . . ?
C5 N1 C1 O1 -172.0(5) . . . . ?
O2 N1 C1 C2 -177.1(5) . . . . ?
C5 N1 C1 C2 6.6(9) . . . . ?
C13 N2 C17 O6 178.2(7) . . . . ?
O5 N2 C17 O6 -1.8(9) . . . . ?
C13 N2 C17 C16 -2.5(9) . . . . ?
O5 N2 C17 C16 177.5(5) . . . . ?
Dy1 O3 C5 N1 -12.5(7) 2_667 . . . ?
Dy1 O3 C5 C4 168.8(4) 2_667 . . . ?
O2 N1 C5 O3 -2.3(8) . . . . ?
C1 N1 C5 O3 174.1(5) . . . . ?
O2 N1 C5 C4 176.5(5) . . . . ?
C1 N1 C5 C4 -7.1(9) . . . . ?
Dy1 O4 C13 N2 -2.8(8) . . . . ?
Dy1 O4 C13 C14 176.3(5) . . . . ?
O5 N2 C13 O4 0.9(9) . . . . ?
C17 N2 C13 O4 -179.2(6) . . . . ?
O5 N2 C13 C14 -178.3(5) . . . . ?
C17 N2 C13 C14 1.6(10) . . . . ?
O3 C5 C4 C12 2.1(10) . . . . ?
N1 C5 C4 C12 -176.6(6) . . . . ?
O3 C5 C4 C3 -178.8(6) . . . . ?
N1 C5 C4 C3 2.5(8) . . . . ?
C3 C4 C12 C11 -0.9(10) . . . . ?
C5 C4 C12 C11 178.1(6) . . . . ?
O1 C1 C2 C6 -6.9(10) . . . . ?
N1 C1 C2 C6 174.6(6) . . . . ?
O1 C1 C2 C3 177.1(6) . . . . ?
N1 C1 C2 C3 -1.4(8) . . . . ?
C3 C2 C6 C7 -1.3(10) . . . . ?
C1 C2 C6 C7 -177.2(6) . . . . ?
C6 C2 C3 C9 1.8(9) . . . . ?
C1 C2 C3 C9 177.8(6) . . . . ?
C6 C2 C3 C4 -178.7(6) . . . . ?
C1 C2 C3 C4 -2.6(9) . . . . ?
C12 C4 C3 C9 0.7(9) . . . . ?
C5 C4 C3 C9 -178.3(6) . . . . ?
C12 C4 C3 C2 -178.9(6) . . . . ?
C5 C4 C3 C2 2.1(9) . . . . ?
C11 C10 C9 C3 -2.3(11) . . . . ?
C11 C10 C9 C8 -179.1(7) . . . . ?
C2 C3 C9 C10 -179.6(6) . . . . ?
C4 C3 C9 C10 0.8(9) . . . . ?
C2 C3 C9 C8 -2.6(9) . . . . ?
C4 C3 C9 C8 177.8(6) . . . . ?
C7 C8 C9 C10 180.0(7) . . . . ?
C7 C8 C9 C3 3.1(11) . . . . ?
C9 C10 C11 C12 2.1(11) . . . . ?
C4 C12 C11 C10 -0.5(11) . . . . ?
C14 C15 C16 C18 178.7(7) . . . . ?
C21 C15 C16 C18 0.4(10) . . . . ?
C14 C15 C16 C17 0.3(10) . . . . ?
C21 C15 C16 C17 -178.1(6) . . . . ?
O6 C17 C16 C18 2.1(11) . . . . ?
N2 C17 C16 C18 -177.1(6) . . . . ?
O6 C17 C16 C15 -179.3(7) . . . . ?
N2 C17 C16 C15 1.4(9) . . . . ?
C9 C8 C7 C6 -2.7(12) . . . . ?
C2 C6 C7 C8 1.8(11) . . . . ?
C14 C15 C21 C20 -178.7(7) . . . . ?
C16 C15 C21 C20 -0.4(10) . . . . ?
C14 C15 C21 C22 0.5(11) . . . . ?
C16 C15 C21 C22 178.8(7) . . . . ?
C16 C15 C14 C24 -178.7(7) . . . . ?
C21 C15 C14 C24 -0.4(11) . . . . ?
C16 C15 C14 C13 -1.2(10) . . . . ?
C21 C15 C14 C13 177.1(6) . . . . ?
O4 C13 C14 C24 -1.3(11) . . . . ?
N2 C13 C14 C24 177.8(7) . . . . ?
O4 C13 C14 C15 -178.7(6) . . . . ?
N2 C13 C14 C15 0.4(9) . . . . ?
C15 C14 C24 C23 -1.0(12) . . . . ?
C13 C14 C24 C23 -178.4(7) . . . . ?
C20 C21 C22 C23 180.0(8) . . . . ?
C15 C21 C22 C23 0.8(12) . . . . ?
C18 C19 C20 C21 -0.2(13) . . . . ?
C22 C21 C20 C19 -178.9(8) . . . . ?
C15 C21 C20 C19 0.3(12) . . . . ?
C15 C16 C18 C19 -0.2(11) . . . . ?
C17 C16 C18 C19 178.3(7) . . . . ?
C20 C19 C18 C16 0.1(12) . . . . ?
C21 C22 C23 C24 -2.1(13) . . . . ?
C14 C24 C23 C22 2.2(13) . . . . ?
C30 N4 C26 O10 -5.0(18) . . . . ?
C28 N4 C26 O10 177.7(11) . . . . ?
C27 N4 C25 O10 -3(2) . . . . ?
C29 N4 C25 O10 177.5(14) . . . . ?

_refine_diff_density_max         0.867
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.127





#=============================================================================#
#                           05/01/2023  *   END    #
#=============================================================================#
####################################################################### 
# 
# 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_aw1062a_0m_a_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2278247'
loop_
_audit_author_name
_audit_author_address
'Luis Cunha Silva'
;Univ of Porto
Portugal
;
_audit_update_record             
;
2023-06-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT602_aw1062a_0m_a_a_sq   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! 
RESPONSE: Disordered solvent was removed from the electron density 
Map using PLATON/SQUEEZE.
;
# end Validation Reply Form

_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            'C78 H54 Dy2 N8 O22'
_chemical_formula_weight         1780.29

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                   12.1938(8)
_cell_length_b                   12.3905(8)
_cell_length_c                   14.0035(9)
_cell_angle_alpha                94.080(3)
_cell_angle_beta                 93.689(3)
_cell_angle_gamma                94.619(3)
_cell_volume                     2098.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9105
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      28.46

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_F_000             886
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.840
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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            62031
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.680
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7395
_reflns_number_gt                6965
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;         
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.011  0.005  0.000       513       256 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details    The unit cell contains 28.5
methanol molecules which have been treated  as a diffuse contribution to the overal scattering without specific atom positions by SQUEEZE/PLATON
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0909P)²+35.5448P] 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         7395
_refine_ls_number_parameters     453
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0714
_refine_ls_wR_factor_ref         0.2032
_refine_ls_wR_factor_gt          0.2009
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_restrained_S_all      1.253
_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
Dy01 Dy 0.55115(3) 0.59439(3) 0.62495(3) 0.01151(17) Uani 1 1 d . . . . .
N1 N 0.4106(7) 0.4460(7) 0.7606(5) 0.0169(10) Uani 1 1 d . . . . .
N2 N 0.3160(6) 0.5831(6) 0.4935(5) 0.0127(15) Uani 1 1 d . . . . .
N3 N 0.6944(7) 0.8135(7) 0.7060(6) 0.0188(17) Uani 1 1 d . . . . .
N4 N 0.8553(13) 0.9858(9) 0.4234(9) 0.062(4) Uani 1 1 d . . . . .
O1 O 0.4228(5) 0.5595(5) 0.4883(4) 0.0133(13) Uani 1 1 d . . . . .
O2 O 0.2844(5) 0.5095(5) 0.3407(5) 0.0175(14) Uani 1 1 d . . . . .
O3 O 0.3565(5) 0.6403(6) 0.6487(5) 0.0196(14) Uani 1 1 d . . . . .
O4 O 0.5291(6) 0.7879(6) 0.6221(5) 0.0240(16) Uani 1 1 d . . . . .
O5 O 0.6973(6) 0.7048(5) 0.7007(5) 0.0198(14) Uani 1 1 d . . . . .
O6 O 0.8579(6) 0.8340(6) 0.7952(5) 0.0252(16) Uani 1 1 d . . . . .
O7 O 0.4567(5) 0.4387(5) 0.6743(4) 0.0169(10) Uani 1 1 d . . . . .
O8 O 0.5105(6) 0.6067(6) 0.7938(5) 0.0241(8) Uani 1 1 d . . . . .
O9 O 0.3086(7) 0.2858(7) 0.7178(5) 0.0310(18) Uani 1 1 d . . . . .
O10 O 0.7550(8) 0.8639(7) 0.5006(6) 0.038(2) Uani 1 1 d . . . . .
O11 O 0.6524(5) 0.6544(5) 0.4919(5) 0.0180(14) Uani 1 1 d D . . . .
H11 H 0.6203 0.6269 0.4399 0.027 Uiso 1 1 calc DR U . . .
C1 C 0.4438(9) 0.5358(9) 0.8201(7) 0.0241(8) Uani 1 1 d . . . . .
C2 C 0.3999(9) 0.5433(9) 0.9140(7) 0.0241(8) Uani 1 1 d . . . . .
C3 C 0.4303(9) 0.6315(9) 0.9797(7) 0.0241(8) Uani 1 1 d . . . . .
H3 H 0.4759 0.6911 0.9611 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3946(9) 0.6343(9) 1.0734(7) 0.0241(8) Uani 1 1 d . . . . .
H4 H 0.4155 0.6956 1.1174 0.029 Uiso 1 1 calc R U . . .
C5 C 0.3293(9) 0.5479(9) 1.1010(7) 0.0241(8) Uani 1 1 d . . . . .
H5 H 0.3048 0.5517 1.1640 0.029 Uiso 1 1 calc R U . . .
C6 C 0.2973(9) 0.4542(10) 1.0398(7) 0.031(3) Uani 1 1 d . . . . .
C7 C 0.2380(10) 0.3615(11) 1.0683(8) 0.037(3) Uani 1 1 d . . . . .
H7 H 0.2186 0.3599 1.1328 0.044 Uiso 1 1 calc R U . . .
C8 C 0.2083(10) 0.2756(13) 1.0065(10) 0.043(3) Uani 1 1 d . . . . .
H8 H 0.1665 0.2146 1.0271 0.052 Uiso 1 1 calc R U . . .
C9 C 0.2391(10) 0.2743(11) 0.9083(9) 0.037(3) Uani 1 1 d . . . . .
H9 H 0.2181 0.2127 0.8648 0.044 Uiso 1 1 calc R U . . .
C10 C 0.2984(9) 0.3621(9) 0.8789(7) 0.026(2) Uani 1 1 d . . . . .
C11 C 0.3316(8) 0.4540(10) 0.9438(7) 0.024(2) Uani 1 1 d . . . . .
H11A H 0.703(8) 0.718(6) 0.490(3) 0.036 Uiso 1 1 d D U . . .
C12 C 0.3371(8) 0.3582(8) 0.7797(7) 0.020(2) Uani 1 1 d . . . . .
C13 C 0.2858(8) 0.6251(7) 0.5809(6) 0.0143(18) Uani 1 1 d . . . . .
C14 C 0.1698(8) 0.6496(7) 0.5860(7) 0.0175(19) Uani 1 1 d . . . . .
C15 C 0.1334(9) 0.6882(9) 0.6722(8) 0.026(2) Uani 1 1 d . . . . .
H15 H 0.1835 0.7013 0.7274 0.031 Uiso 1 1 calc R U . . .
C16 C 0.0234(9) 0.7079(9) 0.6779(9) 0.028(2) Uani 1 1 d . . . . .
H16 H -0.0014 0.7337 0.7376 0.033 Uiso 1 1 calc R U . . .
C17 C -0.0502(9) 0.6907(9) 0.5990(9) 0.029(3) Uani 1 1 d . . . . .
H17 H -0.1250 0.7047 0.6045 0.035 Uiso 1 1 calc R U . . .
C18 C -0.0148(8) 0.6519(8) 0.5086(8) 0.024(2) Uani 1 1 d . . . . .
C19 C 0.0979(8) 0.6296(7) 0.5029(8) 0.019(2) Uani 1 1 d . . . . .
C20 C -0.0878(9) 0.6313(9) 0.4235(9) 0.031(3) Uani 1 1 d . . . . .
H20 H -0.1629 0.6459 0.4258 0.037 Uiso 1 1 calc R U . . .
C21 C -0.0508(9) 0.5912(10) 0.3396(9) 0.032(3) Uani 1 1 d . . . . .
H21 H -0.0996 0.5798 0.2835 0.038 Uiso 1 1 calc R U . . .
C22 C 0.0602(8) 0.5664(8) 0.3360(8) 0.023(2) Uani 1 1 d . . . . .
H22 H 0.0849 0.5364 0.2777 0.028 Uiso 1 1 calc R U . . .
C23 C 0.1326(8) 0.5854(8) 0.4157(7) 0.0177(19) Uani 1 1 d . . . . .
C24 C 0.2475(7) 0.5565(7) 0.4124(6) 0.0125(18) Uani 1 1 d . . . . .
C25 C 0.6041(9) 0.8531(9) 0.6612(7) 0.026(2) Uani 1 1 d . . . . .
C26 C 0.6002(10) 0.9726(9) 0.6629(8) 0.032(3) Uani 1 1 d . . . . .
C27 C 0.5101(13) 1.0156(11) 0.6188(11) 0.047(3) Uani 1 1 d . . . . .
H27 H 0.4498 0.9690 0.5895 0.056 Uiso 1 1 calc R U . . .
C28 C 0.5090(14) 1.1293(11) 0.6179(12) 0.055(4) Uani 1 1 d . . . . .
H28 H 0.4486 1.1586 0.5857 0.066 Uiso 1 1 calc R U . . .
C29 C 0.5938(13) 1.1989(10) 0.6629(10) 0.047(3) Uani 1 1 d . . . . .
H29 H 0.5906 1.2752 0.6631 0.056 Uiso 1 1 calc R U . . .
C30 C 0.6864(12) 1.1553(9) 0.7091(9) 0.037(3) Uani 1 1 d . . . . .
C31 C 0.6890(10) 1.0397(9) 0.7092(9) 0.031(3) Uani 1 1 d . . . . .
C32 C 0.7800(9) 0.9964(9) 0.7551(8) 0.026(2) Uani 1 1 d . . . . .
C33 C 0.8695(11) 1.0645(9) 0.7974(9) 0.035(3) Uani 1 1 d . . . . .
H33 H 0.9311 1.0348 0.8275 0.042 Uiso 1 1 calc R U . . .
C34 C 0.8674(14) 1.1767(11) 0.7948(11) 0.051(4) Uani 1 1 d . . . . .
H34 H 0.9281 1.2233 0.8234 0.061 Uiso 1 1 calc R U . . .
C35 C 0.7777(12) 1.2212(10) 0.7510(10) 0.043(3) Uani 1 1 d . . . . .
H35 H 0.7785 1.2978 0.7495 0.052 Uiso 1 1 calc R U . . .
C36 C 0.7836(8) 0.8781(8) 0.7558(7) 0.021(2) Uani 1 1 d . . . . .
C37 C 0.8101(18) 0.8874(12) 0.4350(13) 0.074(3) Uani 1 1 d . . . . .
H37 H 0.8217 0.8308 0.3883 0.089 Uiso 1 1 calc R U . . .
C38 C 0.9158(18) 1.0074(12) 0.3387(13) 0.074(3) Uani 1 1 d . . . . .
H38A H 0.9881 1.0452 0.3591 0.111 Uiso 1 1 calc R U . . .
H38B H 0.8740 1.0528 0.2978 0.111 Uiso 1 1 calc R U . . .
H38C H 0.9257 0.9385 0.3027 0.111 Uiso 1 1 calc R U . . .
C39 C 0.8353(19) 1.0774(12) 0.4891(13) 0.074(3) Uani 1 1 d . . . . .
H39A H 0.7863 1.1242 0.4565 0.111 Uiso 1 1 calc R U . . .
H39B H 0.9055 1.1191 0.5101 0.111 Uiso 1 1 calc R U . . .
H39C H 0.8006 1.0506 0.5451 0.111 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy01 O5 2.309(7) . ?
Dy01 O7 2.337(6) . ?
Dy01 O1 2.384(6) . ?
Dy01 O11 2.429(7) . ?
Dy01 O4 2.436(7) . ?
Dy01 O8 2.443(7) . ?
Dy01 O1 2.447(6) 2_666 ?
Dy01 O2 2.509(6) 2_666 ?
Dy01 O3 2.522(7) . ?
N1 C1 1.360(14) . ?
N1 O7 1.365(10) . ?
N1 C12 1.404(13) . ?
N2 O1 1.362(9) . ?
N2 C24 1.371(12) . ?
N2 C13 1.379(12) . ?
N3 O5 1.347(10) . ?
N3 C25 1.374(14) . ?
N3 C36 1.411(13) . ?
N4 C37 1.323(18) . ?
N4 C39 1.456(18) . ?
N4 C38 1.465(18) . ?
O1 Dy01 2.447(6) 2_666 ?
O2 C24 1.251(11) . ?
O2 Dy01 2.509(6) 2_666 ?
O3 C13 1.234(12) . ?
O4 C25 1.242(13) . ?
O6 C36 1.218(13) . ?
O8 C1 1.240(13) . ?
O9 C12 1.215(13) . ?
O10 C37 1.210(18) . ?
O11 H11 0.8400 . ?
O11 H11A 0.960(10) . ?
C1 C2 1.451(14) . ?
C2 C3 1.388(15) . ?
C2 C11 1.433(16) . ?
C3 C4 1.408(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(16) . ?
C4 H4 0.9500 . ?
C5 C6 1.406(17) . ?
C5 H5 0.9500 . ?
C6 C7 1.404(18) . ?
C6 C11 1.434(14) . ?
C7 C8 1.33(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.447(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.360(16) . ?
C9 H9 0.9500 . ?
C10 C11 1.420(16) . ?
C10 C12 1.495(13) . ?
C13 C14 1.475(13) . ?
C14 C15 1.379(15) . ?
C14 C19 1.407(15) . ?
C15 C16 1.390(15) . ?
C15 H15 0.9500 . ?
C16 C17 1.370(17) . ?
C16 H16 0.9500 . ?
C17 C18 1.427(16) . ?
C17 H17 0.9500 . ?
C18 C19 1.430(14) . ?
C18 C20 1.435(16) . ?
C19 C23 1.406(14) . ?
C20 C21 1.360(18) . ?
C20 H20 0.9500 . ?
C21 C22 1.416(15) . ?
C21 H21 0.9500 . ?
C22 C23 1.372(14) . ?
C22 H22 0.9500 . ?
C23 C24 1.476(13) . ?
C25 C26 1.483(15) . ?
C26 C27 1.389(18) . ?
C26 C31 1.403(17) . ?
C27 C28 1.410(19) . ?
C27 H27 0.9500 . ?
C28 C29 1.38(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.43(2) . ?
C29 H29 0.9500 . ?
C30 C35 1.40(2) . ?
C30 C31 1.435(15) . ?
C31 C32 1.410(17) . ?
C32 C33 1.397(16) . ?
C32 C36 1.470(15) . ?
C33 C34 1.395(18) . ?
C33 H33 0.9500 . ?
C34 C35 1.39(2) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?

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
O5 Dy01 O7 130.2(2) . . ?
O5 Dy01 O1 147.3(2) . . ?
O7 Dy01 O1 82.6(2) . . ?
O5 Dy01 O11 77.1(2) . . ?
O7 Dy01 O11 140.4(2) . . ?
O1 Dy01 O11 75.4(2) . . ?
O5 Dy01 O4 66.0(2) . . ?
O7 Dy01 O4 138.7(2) . . ?
O1 Dy01 O4 89.6(2) . . ?
O11 Dy01 O4 74.4(2) . . ?
O5 Dy01 O8 75.8(2) . . ?
O7 Dy01 O8 65.6(2) . . ?
O1 Dy01 O8 127.4(2) . . ?
O11 Dy01 O8 152.1(2) . . ?
O4 Dy01 O8 88.7(2) . . ?
O5 Dy01 O1 122.4(2) . 2_666 ?
O7 Dy01 O1 71.3(2) . 2_666 ?
O1 Dy01 O1 62.4(2) . 2_666 ?
O11 Dy01 O1 69.3(2) . 2_666 ?
O4 Dy01 O1 138.4(2) . 2_666 ?
O8 Dy01 O1 132.5(2) . 2_666 ?
O5 Dy01 O2 68.3(2) . 2_666 ?
O7 Dy01 O2 82.4(2) . 2_666 ?
O1 Dy01 O2 125.4(2) . 2_666 ?
O11 Dy01 O2 84.0(2) . 2_666 ?
O4 Dy01 O2 132.5(2) . 2_666 ?
O8 Dy01 O2 91.9(2) . 2_666 ?
O1 Dy01 O2 63.0(2) 2_666 2_666 ?
O5 Dy01 O3 119.5(2) . . ?
O7 Dy01 O3 73.2(2) . . ?
O1 Dy01 O3 63.8(2) . . ?
O11 Dy01 O3 122.6(2) . . ?
O4 Dy01 O3 67.0(2) . . ?
O8 Dy01 O3 67.3(2) . . ?
O1 Dy01 O3 117.9(2) 2_666 . ?
O2 Dy01 O3 152.8(2) 2_666 . ?
C1 N1 O7 116.4(8) . . ?
C1 N1 C12 127.0(8) . . ?
O7 N1 C12 116.6(7) . . ?
O1 N2 C24 116.3(7) . . ?
O1 N2 C13 117.3(7) . . ?
C24 N2 C13 126.3(8) . . ?
O5 N3 C25 116.8(8) . . ?
O5 N3 C36 118.3(8) . . ?
C25 N3 C36 124.9(9) . . ?
C37 N4 C39 120.3(12) . . ?
C37 N4 C38 121.0(12) . . ?
C39 N4 C38 118.4(11) . . ?
N2 O1 Dy01 120.6(5) . . ?
N2 O1 Dy01 114.6(5) . 2_666 ?
Dy01 O1 Dy01 117.6(2) . 2_666 ?
C24 O2 Dy01 115.5(6) . 2_666 ?
C13 O3 Dy01 119.7(6) . . ?
C25 O4 Dy01 118.3(7) . . ?
N3 O5 Dy01 120.0(5) . . ?
N1 O7 Dy01 118.2(5) . . ?
C1 O8 Dy01 117.4(6) . . ?
Dy01 O11 H11 109.5 . . ?
Dy01 O11 H11A 129(4) . . ?
H11 O11 H11A 118.3 . . ?
O8 C1 N1 119.9(9) . . ?
O8 C1 C2 122.5(10) . . ?
N1 C1 C2 117.6(10) . . ?
C3 C2 C11 118.5(9) . . ?
C3 C2 C1 121.4(10) . . ?
C11 C2 C1 119.8(10) . . ?
C2 C3 C4 121.2(10) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.6(10) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 122.8(10) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C7 C6 C5 124.1(10) . . ?
C7 C6 C11 119.1(11) . . ?
C5 C6 C11 116.8(11) . . ?
C8 C7 C6 121.3(11) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C9 120.7(12) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C10 C9 C8 119.5(12) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 120.7(10) . . ?
C9 C10 C12 119.7(11) . . ?
C11 C10 C12 119.4(9) . . ?
C10 C11 C2 120.4(9) . . ?
C10 C11 C6 118.6(10) . . ?
C2 C11 C6 121.0(11) . . ?
O9 C12 N1 120.5(8) . . ?
O9 C12 C10 124.1(9) . . ?
N1 C12 C10 115.4(9) . . ?
O3 C13 N2 118.6(8) . . ?
O3 C13 C14 124.5(8) . . ?
N2 C13 C14 116.9(8) . . ?
C15 C14 C19 121.5(9) . . ?
C15 C14 C13 119.7(9) . . ?
C19 C14 C13 118.8(9) . . ?
C14 C15 C16 119.8(11) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 121.2(10) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 120.3(10) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C19 118.6(10) . . ?
C17 C18 C20 123.1(10) . . ?
C19 C18 C20 118.3(10) . . ?
C23 C19 C14 122.1(9) . . ?
C23 C19 C18 119.3(10) . . ?
C14 C19 C18 118.6(9) . . ?
C21 C20 C18 120.9(10) . . ?
C21 C20 H20 119.5 . . ?
C18 C20 H20 119.5 . . ?
C20 C21 C22 120.0(11) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 120.7(11) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C19 120.6(9) . . ?
C22 C23 C24 120.6(9) . . ?
C19 C23 C24 118.8(9) . . ?
O2 C24 N2 119.2(8) . . ?
O2 C24 C23 123.8(8) . . ?
N2 C24 C23 116.9(8) . . ?
O4 C25 N3 118.9(10) . . ?
O4 C25 C26 123.0(10) . . ?
N3 C25 C26 118.1(10) . . ?
C27 C26 C31 121.5(11) . . ?
C27 C26 C25 119.8(11) . . ?
C31 C26 C25 118.7(10) . . ?
C26 C27 C28 119.4(14) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C29 C28 C27 121.4(13) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C30 119.6(12) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C35 C30 C29 122.3(12) . . ?
C35 C30 C31 118.3(12) . . ?
C29 C30 C31 119.4(12) . . ?
C26 C31 C32 121.7(10) . . ?
C26 C31 C30 118.8(11) . . ?
C32 C31 C30 119.5(11) . . ?
C33 C32 C31 120.8(10) . . ?
C33 C32 C36 119.1(11) . . ?
C31 C32 C36 120.1(10) . . ?
C34 C33 C32 119.2(13) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C35 C34 C33 121.0(13) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C30 121.2(12) . . ?
C34 C35 H35 119.4 . . ?
C30 C35 H35 119.4 . . ?
O6 C36 N3 119.2(9) . . ?
O6 C36 C32 124.4(10) . . ?
N3 C36 C32 116.4(9) . . ?
O10 C37 N4 125.0(14) . . ?
O10 C37 H37 117.5 . . ?
N4 C37 H37 117.5 . . ?
N4 C38 H38A 109.5 . . ?
N4 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N4 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N4 C39 H39A 109.5 . . ?
N4 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N4 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

_refine_diff_density_max         3.393
_refine_diff_density_min         -2.629
_refine_diff_density_rms         0.271

