# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

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

data_20161009a
_database_code_depnum_ccdc_archive 'CCDC 1851900'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_audit_creation_date             2018-06-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H22 Dy N3 O7, C H4 O, 2(Cl)'
_chemical_formula_sum            'C16 H26 Cl2 Dy N3 O8'
_chemical_formula_weight         621.80
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 O1 Dy1 Cl1'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5612(3)
_cell_length_b                   15.4837(5)
_cell_length_c                   17.4652(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.758(3)
_cell_angle_gamma                90
_cell_volume                     2307.17(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3976
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      27.5650
_cell_measurement_theta_min      4.1290
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12761
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.729
_diffrn_reflns_theta_min         3.462
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     17.00  86.00   1.00    1.00    --   12.45  37.00-120.00   69
  2  ω     -4.00  22.00   1.00    1.00    --  -11.20 -99.00  30.00   26
  3  ω    -13.00  13.00   1.00    1.00    --   12.45 -99.00  60.00   26
  4  ω    -16.00  88.00   1.00    1.00    --   12.45  19.00-180.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0540284000
_diffrn_orient_matrix_UB_12      0.0051604000
_diffrn_orient_matrix_UB_13      -0.0283262000
_diffrn_orient_matrix_UB_21      0.0593630000
_diffrn_orient_matrix_UB_22      -0.0197407000
_diffrn_orient_matrix_UB_23      0.0248186000
_diffrn_orient_matrix_UB_31      -0.0218244000
_diffrn_orient_matrix_UB_32      -0.0410057000
_diffrn_orient_matrix_UB_33      -0.0155332000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3799
_reflns_number_total             4874
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_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         0.746
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4874
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.051
_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)+(0.0168P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0762
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 C14-H5
 1.898303 with sigma of 0.02
 C15-H7
 1.904916 with sigma of 0.02
 Dy1-H5
 2.856867 with sigma of 0.02
 Dy1-H7
 2.966144 with sigma of 0.02
3.a Rotating group:
 O6(H6A,H6B), O4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C12(H12), C11(H11), C10(H10), C13(H13), C7(H7A), C5(H5A), C4(H4),
 C3(H3), C2(H2A)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
3.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.63330(3) 0.37635(2) 0.78538(2) 0.01325(8) Uani 1 1 d D . . . .
O3 O 0.9602(4) 0.80928(19) 0.82946(17) 0.0167(8) Uani 1 1 d . . . . .
O2 O 0.7942(4) 0.50433(19) 0.80420(17) 0.0162(7) Uani 1 1 d . . . . .
O1 O 0.6453(4) 0.2455(2) 0.82731(18) 0.0210(8) Uani 1 1 d . . . . .
O7 O 0.3557(4) 0.3455(2) 0.80132(19) 0.0222(8) Uani 1 1 d D . . . .
H7 H 0.2885(18) 0.3786(19) 0.777(3) 0.033 Uiso 1 1 d DR . . . .
O5 O 0.4942(4) 0.4878(2) 0.7161(2) 0.0287(9) Uani 1 1 d D . . . .
H5 H 0.402(3) 0.4737(13) 0.698(3) 0.043 Uiso 1 1 d DR . . . .
O6 O 0.5579(4) 0.4416(2) 0.90057(19) 0.0309(9) Uani 1 1 d . . . . .
H6A H 0.4649 0.4262 0.9079 0.046 Uiso 1 1 d GR . . . .
H6B H 0.5614 0.4962 0.8959 0.046 Uiso 1 1 d GR . . . .
O4 O 0.8370(4) 0.3624(2) 0.70494(19) 0.0298(9) Uani 1 1 d . . . . .
H4A H 0.8696 0.4121 0.6931 0.045 Uiso 1 1 d GR . . . .
H4B H 0.8028 0.3357 0.6644 0.045 Uiso 1 1 d GR . . . .
N3 N 1.0338(5) 0.7344(2) 0.8409(2) 0.0133(9) Uani 1 1 d . . . . .
N2 N 0.9690(5) 0.4347(2) 0.8857(2) 0.0162(9) Uani 1 1 d . . . . .
H2 H 1.0556 0.4353 0.9145 0.019 Uiso 1 1 calc R . . . .
N1 N 0.8731(5) 0.3614(2) 0.8799(2) 0.0138(9) Uani 1 1 d . . . . .
C6 C 0.8413(6) 0.2167(3) 0.9299(3) 0.0166(11) Uani 1 1 d . . . . .
C12 C 1.1885(6) 0.7342(3) 0.8622(3) 0.0164(11) Uani 1 1 d . . . . .
H12 H 1.2438 0.7858 0.8665 0.020 Uiso 1 1 calc R . . . .
C11 C 1.2644(6) 0.6569(3) 0.8774(3) 0.0209(12) Uani 1 1 d . . . . .
H11 H 1.3714 0.6567 0.8920 0.025 Uiso 1 1 calc R . . . .
C10 C 1.1834(6) 0.5795(3) 0.8714(3) 0.0210(12) Uani 1 1 d . . . . .
H10 H 1.2347 0.5272 0.8809 0.025 Uiso 1 1 calc R . . . .
C9 C 1.0226(6) 0.5821(3) 0.8507(3) 0.0143(10) Uani 1 1 d . . . . .
C13 C 0.9498(6) 0.6604(3) 0.8346(3) 0.0140(10) Uani 1 1 d . . . . .
H13 H 0.8432 0.6623 0.8193 0.017 Uiso 1 1 calc R . . . .
C8 C 0.9204(6) 0.5032(3) 0.8449(3) 0.0155(11) Uani 1 1 d . . . . .
C7 C 0.9171(6) 0.2993(3) 0.9264(2) 0.0148(11) Uani 1 1 d . . . . .
H7A H 1.0049 0.3089 0.9604 0.018 Uiso 1 1 calc R . . . .
C5 C 0.9055(6) 0.1575(3) 0.9856(3) 0.0213(12) Uani 1 1 d . . . . .
H5A H 0.9932 0.1732 1.0176 0.026 Uiso 1 1 calc R . . . .
C4 C 0.8405(6) 0.0770(3) 0.9934(3) 0.0257(13) Uani 1 1 d . . . . .
H4 H 0.8804 0.0392 1.0315 0.031 Uiso 1 1 calc R . . . .
C3 C 0.7145(7) 0.0535(3) 0.9431(3) 0.0318(14) Uani 1 1 d . . . . .
H3 H 0.6722 -0.0015 0.9471 0.038 Uiso 1 1 calc R . . . .
C2 C 0.6493(7) 0.1084(3) 0.8874(3) 0.0263(13) Uani 1 1 d . . . . .
H2A H 0.5647 0.0898 0.8547 0.032 Uiso 1 1 calc R . . . .
C1 C 0.7089(6) 0.1922(3) 0.8794(3) 0.0190(11) Uani 1 1 d . . . . .
C14 C 0.5000(7) 0.5796(3) 0.7158(3) 0.0366(15) Uani 1 1 d D . . . .
H14A H 0.5106 0.5997 0.6645 0.055 Uiso 1 1 calc GR . . . .
H14B H 0.5882 0.5988 0.7490 0.055 Uiso 1 1 calc GR . . . .
H14C H 0.4052 0.6023 0.7337 0.055 Uiso 1 1 calc GR . . . .
C15 C 0.2762(6) 0.2704(3) 0.8268(3) 0.0246(12) Uani 1 1 d D . . . .
H15A H 0.1792 0.2629 0.7959 0.037 Uiso 1 1 calc GR . . . .
H15B H 0.2553 0.2777 0.8796 0.037 Uiso 1 1 calc GR . . . .
H15C H 0.3411 0.2204 0.8220 0.037 Uiso 1 1 calc GR . . . .
O8 O 0.8735(6) 0.2606(3) 0.5843(2) 0.0569(14) Uani 1 1 d . . . . .
H8 H 0.8376 0.2149 0.5669 0.085 Uiso 1 1 calc GR . . . .
C16 C 0.9404(8) 0.3077(4) 0.5248(3) 0.0433(17) Uani 1 1 d . . . . .
H16A H 0.8582 0.3323 0.4909 0.065 Uiso 1 1 calc GR . . . .
H16B H 1.0024 0.2695 0.4964 0.065 Uiso 1 1 calc GR . . . .
H16C H 1.0057 0.3531 0.5471 0.065 Uiso 1 1 calc GR . . . .
Cl2 Cl 0.77410(15) 0.08822(8) 0.50517(7) 0.0210(3) Uani 1 1 d . . . . .
Cl1 Cl 0.14784(15) 0.45258(8) 0.68999(8) 0.0276(3) 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
Dy1 O3 2.340(3) 2_646 ?
Dy1 O2 2.420(3) . ?
Dy1 O1 2.154(3) . ?
Dy1 O7 2.462(3) . ?
Dy1 O5 2.370(3) . ?
Dy1 O6 2.387(3) . ?
Dy1 O4 2.338(4) . ?
Dy1 N1 2.536(4) . ?
O3 Dy1 2.340(3) 2_656 ?
O3 N3 1.326(4) . ?
O2 C8 1.243(5) . ?
O1 C1 1.313(5) . ?
O7 H7 0.854(9) . ?
O7 C15 1.437(6) . ?
O5 H5 0.856(9) . ?
O5 C14 1.422(6) . ?
O6 H6A 0.8503 . ?
O6 H6B 0.8501 . ?
O4 H4A 0.8499 . ?
O4 H4B 0.8505 . ?
N3 C12 1.345(6) . ?
N3 C13 1.352(6) . ?
N2 H2 0.8600 . ?
N2 N1 1.400(5) . ?
N2 C8 1.326(6) . ?
N1 C7 1.295(5) . ?
C6 C7 1.439(6) . ?
C6 C5 1.415(6) . ?
C6 C1 1.428(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.377(6) . ?
C11 H11 0.9300 . ?
C11 C10 1.384(7) . ?
C10 H10 0.9300 . ?
C10 C9 1.394(6) . ?
C9 C13 1.381(6) . ?
C9 C8 1.501(6) . ?
C13 H13 0.9300 . ?
C7 H7A 0.9300 . ?
C5 H5A 0.9300 . ?
C5 C4 1.376(7) . ?
C4 H4 0.9300 . ?
C4 C3 1.381(7) . ?
C3 H3 0.9300 . ?
C3 C2 1.374(7) . ?
C2 H2A 0.9300 . ?
C2 C1 1.406(7) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
O8 H8 0.8200 . ?
O8 C16 1.428(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 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
O3 Dy1 O2 129.07(11) 2_646 . ?
O3 Dy1 O7 75.29(12) 2_646 . ?
O3 Dy1 O5 76.36(11) 2_646 . ?
O3 Dy1 O6 144.37(12) 2_646 . ?
O3 Dy1 N1 135.93(12) 2_646 . ?
O2 Dy1 O7 133.41(11) . . ?
O2 Dy1 N1 64.23(11) . . ?
O1 Dy1 O3 82.95(11) . 2_646 ?
O1 Dy1 O2 135.51(11) . . ?
O1 Dy1 O7 78.38(12) . . ?
O1 Dy1 O5 150.01(12) . . ?
O1 Dy1 O6 96.89(13) . . ?
O1 Dy1 O4 95.77(13) . . ?
O1 Dy1 N1 71.31(11) . . ?
O7 Dy1 N1 130.20(12) . . ?
O5 Dy1 O2 74.30(11) . . ?
O5 Dy1 O7 75.53(12) . . ?
O5 Dy1 O6 87.85(13) . . ?
O5 Dy1 N1 138.05(11) . . ?
O6 Dy1 O2 74.33(11) . . ?
O6 Dy1 O7 69.85(12) . . ?
O6 Dy1 N1 75.58(12) . . ?
O4 Dy1 O3 70.32(12) . 2_646 ?
O4 Dy1 O2 73.30(12) . . ?
O4 Dy1 O7 145.58(12) . . ?
O4 Dy1 O5 97.39(13) . . ?
O4 Dy1 O6 144.36(12) . . ?
O4 Dy1 N1 77.23(12) . . ?
N3 O3 Dy1 129.9(2) . 2_656 ?
C8 O2 Dy1 121.6(3) . . ?
C1 O1 Dy1 146.4(3) . . ?
Dy1 O7 H7 116.5(14) . . ?
C15 O7 Dy1 132.7(3) . . ?
C15 O7 H7 108.7(14) . . ?
Dy1 O5 H5 114.3(14) . . ?
C14 O5 Dy1 135.5(3) . . ?
C14 O5 H5 106.5(14) . . ?
Dy1 O6 H6A 109.3 . . ?
Dy1 O6 H6B 109.0 . . ?
H6A O6 H6B 109.5 . . ?
Dy1 O4 H4A 109.9 . . ?
Dy1 O4 H4B 108.8 . . ?
H4A O4 H4B 109.6 . . ?
O3 N3 C12 119.3(4) . . ?
O3 N3 C13 119.0(4) . . ?
C12 N3 C13 121.6(4) . . ?
N1 N2 H2 121.5 . . ?
C8 N2 H2 121.5 . . ?
C8 N2 N1 116.9(4) . . ?
N2 N1 Dy1 114.3(3) . . ?
C7 N1 Dy1 130.8(3) . . ?
C7 N1 N2 114.7(4) . . ?
C5 C6 C7 117.0(4) . . ?
C5 C6 C1 119.7(4) . . ?
C1 C6 C7 123.2(4) . . ?
N3 C12 H12 120.2 . . ?
N3 C12 C11 119.6(4) . . ?
C11 C12 H12 120.2 . . ?
C12 C11 H11 119.6 . . ?
C12 C11 C10 120.8(5) . . ?
C10 C11 H11 119.6 . . ?
C11 C10 H10 120.9 . . ?
C11 C10 C9 118.2(5) . . ?
C9 C10 H10 120.9 . . ?
C10 C9 C8 123.4(4) . . ?
C13 C9 C10 119.8(4) . . ?
C13 C9 C8 116.7(4) . . ?
N3 C13 C9 119.9(4) . . ?
N3 C13 H13 120.0 . . ?
C9 C13 H13 120.0 . . ?
O2 C8 N2 122.5(4) . . ?
O2 C8 C9 120.1(4) . . ?
N2 C8 C9 117.3(4) . . ?
N1 C7 C6 125.3(4) . . ?
N1 C7 H7A 117.3 . . ?
C6 C7 H7A 117.3 . . ?
C6 C5 H5A 119.4 . . ?
C4 C5 C6 121.1(5) . . ?
C4 C5 H5A 119.4 . . ?
C5 C4 H4 120.8 . . ?
C5 C4 C3 118.5(5) . . ?
C3 C4 H4 120.8 . . ?
C4 C3 H3 118.8 . . ?
C2 C3 C4 122.5(5) . . ?
C2 C3 H3 118.8 . . ?
C3 C2 H2A 119.6 . . ?
C3 C2 C1 120.7(5) . . ?
C1 C2 H2A 119.6 . . ?
O1 C1 C6 121.5(4) . . ?
O1 C1 C2 121.1(4) . . ?
C2 C1 C6 117.4(4) . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 O8 H8 109.5 . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 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 O3 N3 C12 105.9(4) 2_656 . . . ?
Dy1 O3 N3 C13 -77.3(5) 2_656 . . . ?
Dy1 O2 C8 N2 -5.9(6) . . . . ?
Dy1 O2 C8 C9 175.6(3) . . . . ?
Dy1 O1 C1 C6 -11.8(9) . . . . ?
Dy1 O1 C1 C2 168.4(4) . . . . ?
Dy1 N1 C7 C6 6.2(7) . . . . ?
O3 N3 C12 C11 177.2(4) . . . . ?
O3 N3 C13 C9 -176.2(4) . . . . ?
N3 C12 C11 C10 -0.2(7) . . . . ?
N2 N1 C7 C6 -178.0(4) . . . . ?
N1 N2 C8 O2 1.6(7) . . . . ?
N1 N2 C8 C9 -179.9(4) . . . . ?
C6 C5 C4 C3 2.8(8) . . . . ?
C12 N3 C13 C9 0.6(7) . . . . ?
C12 C11 C10 C9 -1.0(7) . . . . ?
C11 C10 C9 C13 2.0(7) . . . . ?
C11 C10 C9 C8 -177.8(5) . . . . ?
C10 C9 C13 N3 -1.8(7) . . . . ?
C10 C9 C8 O2 -157.1(5) . . . . ?
C10 C9 C8 N2 24.4(7) . . . . ?
C13 N3 C12 C11 0.4(7) . . . . ?
C13 C9 C8 O2 23.2(7) . . . . ?
C13 C9 C8 N2 -155.4(4) . . . . ?
C8 N2 N1 Dy1 3.1(5) . . . . ?
C8 N2 N1 C7 -173.5(4) . . . . ?
C8 C9 C13 N3 178.0(4) . . . . ?
C7 C6 C5 C4 179.8(5) . . . . ?
C7 C6 C1 O1 -1.8(8) . . . . ?
C7 C6 C1 C2 178.0(5) . . . . ?
C5 C6 C7 N1 -179.0(5) . . . . ?
C5 C6 C1 O1 179.5(5) . . . . ?
C5 C6 C1 C2 -0.6(7) . . . . ?
C5 C4 C3 C2 -1.9(9) . . . . ?
C4 C3 C2 C1 -0.3(9) . . . . ?
C3 C2 C1 O1 -178.7(5) . . . . ?
C3 C2 C1 C6 1.5(8) . . . . ?
C1 C6 C7 N1 2.3(8) . . . . ?
C1 C6 C5 C4 -1.5(8) . . . . ?

_olex2_date_sample_data_collection 2016-10-09
_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 1.245
_oxdiff_exptl_absorpt_empirical_full_min 0.856
####################################################################### 
# 
# 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_20170714a
_database_code_depnum_ccdc_archive 'CCDC 1851901'
_audit_update_record             
;
2018-09-05 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H22 Dy N5 O6, Cl O4'
_chemical_formula_sum            'C24 H22 Cl Dy N5 O10'
_chemical_formula_weight         738.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 H10 O10 N10 Dy2 Cl2'
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'
Cl Cl 0.3639 0.7018 '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                   11.0697(15)
_cell_length_b                   11.7807(16)
_cell_length_c                   12.2202(17)
_cell_angle_alpha                62.152(14)
_cell_angle_beta                 71.245(12)
_cell_angle_gamma                81.049(11)
_cell_volume                     1334.2(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2983
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7750
_cell_measurement_theta_min      4.2330
_shelx_estimated_absorpt_T_max   0.937
_shelx_estimated_absorpt_T_min   0.908
_exptl_absorpt_coefficient_mu    16.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_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    1.838
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.006
_exptl_crystal_size_mid          0.006
_exptl_crystal_size_min          0.004
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7893
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.073
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         4.218
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -109.00 -18.00   1.00   17.50    --  -39.24 -57.00 -60.00   91
  2  ω    -66.00  34.00   1.00   17.50    --  -39.24  57.00  90.00  100
  3  ω     47.00  74.00   1.00   17.50    --   39.24 -99.00 -90.00   27
  4  ω     70.00 126.00   1.00   17.50    --   39.24 178.00-150.00   56
  5  ω      3.00  46.00   1.00   17.50    --   39.24 -99.00 -90.00   43
  6  ω    -35.00  64.00   1.00   17.50    --   39.24 -37.00 150.00   99
  7  ω     37.00 126.00   1.00   50.00    --  108.77 -61.00 -60.00   89
  8  ω     29.00 109.00   1.00   50.00    --  108.77 -94.00 150.00   80
  9  ω    120.00 177.00   1.00   50.00    --  108.77  30.00  30.00   57
 10  ω     82.00 120.00   1.00   50.00    --  108.77-125.00   0.00   38
 11  ω     85.00 161.00   1.00   50.00    --  108.77  45.00   0.00   76
 12  ω     88.00 169.00   1.00   50.00    --  108.77  45.00 -90.00   81
 13  ω     36.00  63.00   1.00   50.00    --  108.77-125.00 120.00   27
 14  ω     85.00 121.00   1.00   50.00    --  108.77-125.00 120.00   36
 15  ω    122.00 147.00   1.00   50.00    --  108.77 103.00 166.00   25
 16  ω     77.00 134.00   1.00   50.00    --  108.77 -77.00-180.00   57
 17  ω     42.00  96.00   1.00   50.00    --  108.77 -45.00 150.00   54
 18  ω    100.00 170.00   1.00   50.00    --  108.77 125.00-150.00   70
 19  ω     79.00 176.00   1.00   50.00    --  108.77  77.00 -60.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0981320000
_diffrn_orient_matrix_UB_12      -0.0608055000
_diffrn_orient_matrix_UB_13      -0.0797968000
_diffrn_orient_matrix_UB_21      0.0711831000
_diffrn_orient_matrix_UB_22      0.1287115000
_diffrn_orient_matrix_UB_23      -0.0851550000
_diffrn_orient_matrix_UB_31      0.0830971000
_diffrn_orient_matrix_UB_32      -0.0401380000
_diffrn_orient_matrix_UB_33      0.0922271000
_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              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3861
_reflns_number_total             4734
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.069
_refine_diff_density_min         -2.021
_refine_diff_density_rms         0.284
_refine_ls_extinction_coef       0.0082(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.1014
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2851
_refine_ls_wR_factor_ref         0.3087
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6-H6
 0.86 with sigma of 0.02
 Cl1-O7
 1.42 with sigma of 0.02
 Cl1-O8
 1.42 with sigma of 0.02
 Cl1-O9
 1.42 with sigma of 0.02
 Cl1-O10
 1.42 with sigma of 0.02
 O7-O8 \\sim O7-O9 \\sim O7-O10 \\sim O8-O9 \\sim O8-O10 \\sim O9-O10
 with sigma of 0.02
3. Rigid bond restraints
 C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim
Ueq, Uanis(O10) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Riding coordinates:
 O6(H6)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C19(H19), C11(H11), C20(H20), C18(H18), C17(H17), C15(H15), C14(H14),
 C13(H13), C23(H23), C22(H22), C7(H7), C9(H9), C10(H10), C2(H2A), C3(H3),
 C4(H4), C5(H5)
5.c Fitted hexagon refined as free rotating group:
 N4(C18,C17,C16,C15,C14)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.47631(6) 0.69882(7) 0.41109(5) 0.0572(4) Uani 1 1 d . . . A 6
O2 O 0.5858(8) 0.7585(8) 0.1947(7) 0.059(2) Uani 1 1 d . . . A 6
O4 O 0.4911(9) 0.4965(9) 0.4009(7) 0.065(2) Uani 1 1 d . . . A 6
N5 N 0.4938(11) 0.4924(10) 0.2908(9) 0.061(3) Uani 1 1 d . . . A 6
N1 N 0.3386(11) 0.7573(13) 0.2662(11) 0.071(3) Uani 1 1 d . . . A 6
O3 O 0.4503(12) 0.9217(11) 0.3328(8) 0.080(3) Uani 1 1 d . . . A 6
N2 N 0.4020(12) 0.7995(12) 0.1331(10) 0.069(3) Uani 1 1 d . . . A 6
H2 H 0.3639 0.8228 0.0745 0.083 Uiso 1 1 calc R . . A 6
C19 C 0.6057(15) 0.5040(13) 0.2015(12) 0.069(4) Uani 1 1 d . . . A 6
H19 H 0.6802 0.5126 0.2164 0.083 Uiso 1 1 calc R . . A 6
C8 C 0.5251(13) 0.7987(11) 0.1105(11) 0.058(3) Uani 1 1 d . . . A 6
O5 O 0.6886(11) 0.7112(13) 0.3916(11) 0.095(3) Uani 1 1 d . U . A 6
C11 C 0.2734(16) 1.1665(16) 0.0683(13) 0.074(4) Uani 1 1 d . . . A 6
H11 H 0.2319 1.2209 0.0069 0.089 Uiso 1 1 calc R . . A 6
C20 C 0.6112(16) 0.5034(14) 0.0905(14) 0.070(3) Uani 1 1 d . . . A 6
H20 H 0.6896 0.5070 0.0306 0.084 Uiso 1 1 calc R . . A 6
N4 N 0.7783(12) 0.7907(13) 0.2808(11) 0.094(4) Uani 1 1 d . U . A 6
C18 C 0.8765(16) 0.7383(12) 0.2133(16) 0.156(9) Uani 1 1 d G U . A 6
H18 H 0.8829 0.6498 0.2427 0.187 Uiso 1 1 calc R . . A 6
C17 C 0.9651(15) 0.8182(16) 0.1020(16) 0.133(7) Uani 1 1 d G U . A 6
H17 H 1.0308 0.7832 0.0568 0.160 Uiso 1 1 calc R . . A 6
C16 C 0.9555(14) 0.9505(15) 0.0581(13) 0.122(6) Uani 1 1 d G U . A 6
C15 C 0.8573(15) 1.0029(11) 0.1256(16) 0.117(6) Uani 1 1 d G U . A 6
H15 H 0.8509 1.0914 0.0962 0.141 Uiso 1 1 calc R . . A 6
C14 C 0.7687(12) 0.9230(14) 0.2369(15) 0.124(7) Uani 1 1 d G U . A 6
H14 H 0.7031 0.9580 0.2821 0.149 Uiso 1 1 calc R . . A 6
C24 C 0.4945(15) 0.8552(13) 0.5897(13) 0.065(3) Uani 1 1 d . . . A 6
H24A H 0.5646 0.9100 0.5261 0.097 Uiso 1 1 calc GR . . A 6
H24B H 0.5068 0.8216 0.6737 0.097 Uiso 1 1 calc GR . . A 6
H24C H 0.4164 0.9038 0.5881 0.097 Uiso 1 1 calc GR . . A 6
C21 C 0.4959(15) 0.4970(13) 0.0648(12) 0.068(4) Uani 1 1 d . . . A 6
C13 C 0.4605(15) 1.0636(11) 0.1190(11) 0.059(3) Uani 1 1 d . . . A 6
H13 H 0.5479 1.0492 0.0935 0.071 Uiso 1 1 calc R . . A 6
C23 C 0.3887(16) 0.4759(18) 0.2720(13) 0.081(5) Uani 1 1 d . . . A 6
H23 H 0.3132 0.4600 0.3386 0.097 Uiso 1 1 calc R . . A 6
N3 N 0.3903(13) 1.0049(12) 0.2446(9) 0.069(3) Uani 1 1 d . . . A 6
C12 C 0.3958(15) 1.1461(12) 0.0303(11) 0.062(3) Uani 1 1 d . . . A 6
C22 C 0.3855(15) 0.4809(17) 0.1603(12) 0.078(4) Uani 1 1 d . . . A 6
H22 H 0.3084 0.4735 0.1489 0.094 Uiso 1 1 calc R . . A 6
O6 O 0.4892(17) 0.7688(16) 0.5664(13) 0.115(4) Uani 1 1 d D U . A 6
H6 H 0.5291 0.7000 0.6023 0.138 Uiso 1 1 d DR . . A 6
O1 O 0.2820(15) 0.6657(19) 0.5307(15) 0.132(5) Uani 1 1 d . U . A 6
C7 C 0.2144(16) 0.768(2) 0.2919(18) 0.096(6) Uani 1 1 d . . . A 6
H7 H 0.1805 0.8004 0.2224 0.115 Uiso 1 1 calc R . . A 6
C9 C 0.2672(19) 1.033(2) 0.2838(14) 0.100(6) Uani 1 1 d . . . A 6
H9 H 0.2251 0.9998 0.3717 0.120 Uiso 1 1 calc R . . A 6
C6 C 0.1272(16) 0.7350(18) 0.4150(18) 0.087(4) Uani 1 1 d . U . A 6
C10 C 0.203(2) 1.109(2) 0.1979(15) 0.107(7) Uani 1 1 d . . . A 6
H10 H 0.1158 1.1229 0.2238 0.128 Uiso 1 1 calc R . . A 6
C1 C 0.161(2) 0.678(2) 0.528(2) 0.106(6) Uani 1 1 d . U . A 6
C2 C 0.0642(19) 0.654(2) 0.638(2) 0.102(5) Uani 1 1 d . U . A 6
H2A H 0.0829 0.6112 0.7166 0.123 Uiso 1 1 calc R . . A 6
C3 C -0.058(3) 0.688(3) 0.638(3) 0.121(7) Uani 1 1 d . U . A 6
H3 H -0.1196 0.6777 0.7149 0.146 Uiso 1 1 calc R . . A 6
C4 C -0.090(3) 0.740(3) 0.524(3) 0.135(8) Uani 1 1 d . U . A 6
H4 H -0.1749 0.7543 0.5240 0.162 Uiso 1 1 calc R . . A 6
C5 C 0.001(3) 0.768(3) 0.417(3) 0.129(8) Uani 1 1 d . U . A 6
H5 H -0.0192 0.8116 0.3390 0.155 Uiso 1 1 calc R . . A 6
Cl1 Cl 0.9553(11) 0.4206(11) 0.0106(11) 0.194(4) Uani 1 1 d D U . B -1
O7 O 1.0889(18) 0.422(3) -0.055(3) 0.226(15) Uani 1 1 d D U . B -1
O8 O 0.929(2) 0.2979(19) 0.127(2) 0.198(10) Uani 1 1 d D U . B -1
O9 O 0.913(2) 0.524(2) 0.042(3) 0.197(12) Uani 1 1 d D U . B -1
O10 O 0.884(2) 0.420(2) -0.071(2) 0.189(10) Uani 1 1 d D U . B -1


_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 O2 2.328(8) . ?
Dy1 O4 2.458(8) 2_666 ?
Dy1 O4 2.422(10) . ?
Dy1 N1 2.492(10) . ?
Dy1 O3 2.343(12) . ?
Dy1 O5 2.305(11) . ?
Dy1 O6 2.445(14) . ?
Dy1 O1 2.150(16) . ?
O2 C8 1.276(15) . ?
O4 Dy1 2.458(8) 2_666 ?
O4 N5 1.359(13) . ?
N5 C19 1.337(19) . ?
N5 C23 1.315(17) . ?
N1 N2 1.416(16) . ?
N1 C7 1.31(2) . ?
O3 N3 1.354(15) . ?
N2 H2 0.8600 . ?
N2 C8 1.300(18) . ?
C19 H19 0.9300 . ?
C19 C20 1.34(2) . ?
C8 C12 1.521(16) 2_675 ?
O5 N4 1.391(15) . ?
C11 H11 0.9300 . ?
C11 C12 1.31(2) . ?
C11 C10 1.39(2) . ?
C20 H20 0.9300 . ?
C20 C21 1.428(18) . ?
N4 C18 1.3900 . ?
N4 C14 1.3900 . ?
C18 H18 0.9300 . ?
C18 C17 1.3900 . ?
C17 H17 0.9300 . ?
C17 C16 1.3900 . ?
C16 C16 1.50(2) 2_775 ?
C16 C15 1.3900 . ?
C15 H15 0.9300 . ?
C15 C14 1.3900 . ?
C14 H14 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 O6 1.19(2) . ?
C21 C21 1.53(2) 2_665 ?
C21 C22 1.36(2) . ?
C13 H13 0.9300 . ?
C13 N3 1.359(16) . ?
C13 C12 1.390(18) . ?
C23 H23 0.9300 . ?
C23 C22 1.350(19) . ?
N3 C9 1.34(2) . ?
C12 C8 1.521(16) 2_675 ?
C22 H22 0.9300 . ?
O6 H6 0.8512 . ?
O1 C1 1.33(3) . ?
C7 H7 0.9300 . ?
C7 C6 1.41(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.34(3) . ?
C6 C1 1.38(3) . ?
C6 C5 1.39(3) . ?
C10 H10 0.9300 . ?
C1 C2 1.35(3) . ?
C2 H2A 0.9300 . ?
C2 C3 1.35(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.38(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.30(4) . ?
C5 H5 0.9300 . ?
Cl1 O7 1.437(18) . ?
Cl1 O8 1.462(16) . ?
Cl1 O9 1.409(16) . ?
Cl1 O10 1.462(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O4 78.4(3) . . ?
O2 Dy1 O4 127.3(3) . 2_666 ?
O2 Dy1 N1 65.0(4) . . ?
O2 Dy1 O3 81.5(3) . . ?
O2 Dy1 O6 132.9(5) . . ?
O4 Dy1 O4 62.5(3) . 2_666 ?
O4 Dy1 N1 82.2(4) . . ?
O4 Dy1 N1 134.7(4) 2_666 . ?
O4 Dy1 O6 136.3(4) . . ?
O3 Dy1 O4 154.9(3) . . ?
O3 Dy1 O4 142.5(3) . 2_666 ?
O3 Dy1 N1 75.7(4) . . ?
O3 Dy1 O6 68.8(4) . . ?
O5 Dy1 O2 73.6(4) . . ?
O5 Dy1 O4 96.7(4) . . ?
O5 Dy1 O4 77.2(4) . 2_666 ?
O5 Dy1 N1 137.9(4) . . ?
O5 Dy1 O3 91.8(5) . . ?
O5 Dy1 O6 71.7(6) . . ?
O6 Dy1 O4 73.7(4) . 2_666 ?
O6 Dy1 N1 134.6(5) . . ?
O1 Dy1 O2 137.5(5) . . ?
O1 Dy1 O4 81.1(5) . 2_666 ?
O1 Dy1 O4 92.8(6) . . ?
O1 Dy1 N1 72.8(5) . . ?
O1 Dy1 O3 92.0(6) . . ?
O1 Dy1 O5 148.8(6) . . ?
O1 Dy1 O6 80.9(7) . . ?
C8 O2 Dy1 120.4(8) . . ?
Dy1 O4 Dy1 117.5(3) . 2_666 ?
N5 O4 Dy1 121.0(7) . 2_666 ?
N5 O4 Dy1 121.2(7) . . ?
C19 N5 O4 119.1(10) . . ?
C23 N5 O4 121.0(12) . . ?
C23 N5 C19 119.9(12) . . ?
N2 N1 Dy1 116.5(8) . . ?
C7 N1 Dy1 129.6(11) . . ?
C7 N1 N2 113.6(12) . . ?
N3 O3 Dy1 129.6(9) . . ?
N1 N2 H2 124.3 . . ?
C8 N2 N1 111.5(10) . . ?
C8 N2 H2 124.3 . . ?
N5 C19 H19 119.8 . . ?
N5 C19 C20 120.5(12) . . ?
C20 C19 H19 119.8 . . ?
O2 C8 N2 126.3(11) . . ?
O2 C8 C12 116.8(12) . 2_675 ?
N2 C8 C12 116.8(11) . 2_675 ?
N4 O5 Dy1 125.5(9) . . ?
C12 C11 H11 119.0 . . ?
C12 C11 C10 122.0(15) . . ?
C10 C11 H11 119.0 . . ?
C19 C20 H20 120.2 . . ?
C19 C20 C21 119.7(15) . . ?
C21 C20 H20 120.2 . . ?
C18 N4 O5 120.3(12) . . ?
C18 N4 C14 120.0 . . ?
C14 N4 O5 119.7(12) . . ?
N4 C18 H18 120.0 . . ?
C17 C18 N4 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C17 H17 120.0 . . ?
C18 C17 C16 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C16 C16 127(2) . 2_775 ?
C15 C16 C17 120.0 . . ?
C15 C16 C16 113(2) . 2_775 ?
C16 C15 H15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C14 C15 H15 120.0 . . ?
N4 C14 H14 120.0 . . ?
C15 C14 N4 120.0 . . ?
C15 C14 H14 120.0 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O6 C24 H24A 109.5 . . ?
O6 C24 H24B 109.5 . . ?
O6 C24 H24C 109.5 . . ?
C20 C21 C21 118.7(18) . 2_665 ?
C22 C21 C20 117.4(12) . . ?
C22 C21 C21 123.8(15) . 2_665 ?
N3 C13 H13 121.5 . . ?
N3 C13 C12 116.9(13) . . ?
C12 C13 H13 121.5 . . ?
N5 C23 H23 118.5 . . ?
N5 C23 C22 122.9(15) . . ?
C22 C23 H23 118.5 . . ?
O3 N3 C13 118.2(12) . . ?
C9 N3 O3 119.6(11) . . ?
C9 N3 C13 122.0(12) . . ?
C11 C12 C8 123.8(12) . 2_675 ?
C11 C12 C13 120.6(12) . . ?
C13 C12 C8 115.5(13) . 2_675 ?
C21 C22 H22 120.4 . . ?
C23 C22 C21 119.2(13) . . ?
C23 C22 H22 120.4 . . ?
Dy1 O6 H6 90.2 . . ?
C24 O6 Dy1 148.3(12) . . ?
C24 O6 H6 117.1 . . ?
C1 O1 Dy1 143.8(15) . . ?
N1 C7 H7 117.0 . . ?
N1 C7 C6 126.0(15) . . ?
C6 C7 H7 117.0 . . ?
N3 C9 H9 119.6 . . ?
N3 C9 C10 120.9(14) . . ?
C10 C9 H9 119.6 . . ?
C1 C6 C7 124.3(17) . . ?
C1 C6 C5 120(2) . . ?
C5 C6 C7 116(2) . . ?
C11 C10 H10 121.4 . . ?
C9 C10 C11 117.2(18) . . ?
C9 C10 H10 121.4 . . ?
O1 C1 C6 122(2) . . ?
O1 C1 C2 121(2) . . ?
C2 C1 C6 116.2(19) . . ?
C1 C2 H2A 118.4 . . ?
C3 C2 C1 123(2) . . ?
C3 C2 H2A 118.4 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119(3) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 119(3) . . ?
C5 C4 H4 120.7 . . ?
C6 C5 H5 119.0 . . ?
C4 C5 C6 122(3) . . ?
C4 C5 H5 119.0 . . ?
O7 Cl1 O8 107.2(12) . . ?
O7 Cl1 O10 107.9(12) . . ?
O8 Cl1 O10 106.1(11) . . ?
O9 Cl1 O7 115.2(13) . . ?
O9 Cl1 O8 110.6(12) . . ?
O9 Cl1 O10 109.4(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O2 C8 N2 -7.3(18) . . . . ?
Dy1 O2 C8 C12 171.3(8) . . . 2_675 ?
Dy1 O4 N5 C19 -87.2(12) 2_666 . . . ?
Dy1 O4 N5 C19 86.3(13) . . . . ?
Dy1 O4 N5 C23 -94.5(14) . . . . ?
Dy1 O4 N5 C23 92.0(15) 2_666 . . . ?
Dy1 N1 N2 C8 0.7(15) . . . . ?
Dy1 N1 C7 C6 -7(3) . . . . ?
Dy1 O3 N3 C13 -92.6(15) . . . . ?
Dy1 O3 N3 C9 91.7(17) . . . . ?
Dy1 O5 N4 C18 -111.6(12) . . . . ?
Dy1 O5 N4 C14 67.8(15) . . . . ?
Dy1 O1 C1 C6 -3(5) . . . . ?
Dy1 O1 C1 C2 -172(2) . . . . ?
O4 N5 C19 C20 -178.5(12) . . . . ?
O4 N5 C23 C22 174.8(16) . . . . ?
N5 C19 C20 C21 3(2) . . . . ?
N5 C23 C22 C21 4(3) . . . . ?
N1 N2 C8 O2 4(2) . . . . ?
N1 N2 C8 C12 -174.4(11) . . . 2_675 ?
N1 C7 C6 C1 -4(4) . . . . ?
N1 C7 C6 C5 173(2) . . . . ?
O3 N3 C9 C10 -176(2) . . . . ?
N2 N1 C7 C6 -179.2(19) . . . . ?
C19 N5 C23 C22 -6(3) . . . . ?
C19 C20 C21 C21 177.1(15) . . . 2_665 ?
C19 C20 C21 C22 -5(2) . . . . ?
O5 N4 C18 C17 179.3(12) . . . . ?
O5 N4 C14 C15 -179.3(12) . . . . ?
C20 C21 C22 C23 2(2) . . . . ?
N4 C18 C17 C16 0.0 . . . . ?
C18 N4 C14 C15 0.0 . . . . ?
C18 C17 C16 C16 179(3) . . . 2_775 ?
C18 C17 C16 C15 0.0 . . . . ?
C17 C16 C15 C14 0.0 . . . . ?
C16 C16 C15 C14 -179(2) 2_775 . . . ?
C16 C15 C14 N4 0.0 . . . . ?
C14 N4 C18 C17 0.0 . . . . ?
C21 C21 C22 C23 179.4(18) 2_665 . . . ?
C13 N3 C9 C10 9(3) . . . . ?
C23 N5 C19 C20 2(2) . . . . ?
N3 C13 C12 C8 -175.0(11) . . . 2_675 ?
N3 C13 C12 C11 1(2) . . . . ?
N3 C9 C10 C11 -6(4) . . . . ?
C12 C11 C10 C9 1(3) . . . . ?
C12 C13 N3 O3 178.5(12) . . . . ?
C12 C13 N3 C9 -6(2) . . . . ?
O1 C1 C2 C3 166(2) . . . . ?
C7 N1 N2 C8 173.9(15) . . . . ?
C7 C6 C1 O1 10(4) . . . . ?
C7 C6 C1 C2 180(2) . . . . ?
C7 C6 C5 C4 178(3) . . . . ?
C6 C1 C2 C3 -4(4) . . . . ?
C10 C11 C12 C8 176.9(18) . . . 2_675 ?
C10 C11 C12 C13 1(3) . . . . ?
C1 C6 C5 C4 -4(4) . . . . ?
C1 C2 C3 C4 7(4) . . . . ?
C2 C3 C4 C5 -8(4) . . . . ?
C3 C4 C5 C6 7(5) . . . . ?
C5 C6 C1 O1 -168(3) . . . . ?
C5 C6 C1 C2 2(3) . . . . ?

_olex2_date_sample_data_collection 2017-07-14
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.680
####################################################################### 
# 
# 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_20170503c
_database_code_depnum_ccdc_archive 'CCDC 1851922'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_audit_creation_date             2018-06-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        dpbo
_chemical_formula_moiety         'C24 H22 Dy N5 O6, 3(C H4 O), Cl O4'
_chemical_formula_sum            'C27 H34 Cl Dy N5 O13'
_chemical_formula_weight         834.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 H10 O10 N10 Dy2 Cl2'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.8598(6)
_cell_length_b                   12.0997(7)
_cell_length_c                   13.4297(7)
_cell_angle_alpha                102.794(5)
_cell_angle_beta                 98.239(4)
_cell_angle_gamma                117.449(5)
_cell_volume                     1599.30(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3312
_cell_measurement_temperature    100.03(11)
_cell_measurement_theta_max      26.2650
_cell_measurement_theta_min      3.6120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_preparation       'Solvent thermal method'
_exptl_crystal_recrystallization_method 'Solvent thermal method'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.1134
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11065
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         3.244
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00 103.00   1.00    6.00    --   23.13  57.00 -30.00  107
  2  ω    100.00 126.00   1.00    6.00    --   23.13 178.00  90.00   26
  3  ω    -14.00 103.00   1.00    6.00    --   23.13  57.00  90.00  117
  4  ω    -20.00   6.00   1.00    6.00    --  -21.88 -99.00-150.00   26
  5  ω    -19.00 107.00   1.00    6.00    --   23.13  57.00-150.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0310165000
_diffrn_orient_matrix_UB_12      0.0106723000
_diffrn_orient_matrix_UB_13      -0.0411286000
_diffrn_orient_matrix_UB_21      -0.0069470000
_diffrn_orient_matrix_UB_22      -0.0632857000
_diffrn_orient_matrix_UB_23      -0.0111196000
_diffrn_orient_matrix_UB_31      -0.0626798000
_diffrn_orient_matrix_UB_32      -0.0277208000
_diffrn_orient_matrix_UB_33      -0.0370757000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5531
_reflns_number_total             6717
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6717
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0543
_refine_ls_restrained_S_all      1.035
_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)+(0.0225P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1089
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 H7A-O7
 0.82 with sigma of 0.02
 H2-H7A
 2.5 with sigma of 0.1
 C24-H6
 1.91236 with sigma of 0.02
 Dy1-H6
 2.987004 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C27) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C14(H14), C18(H18), C15(H15), C13(H13), C23(H23), C7(H7), C12(H12),
 C17(H17), C22(H22), C2(H2A), C10(H10), C11(H11), C3(H3), C19(H19), C20(H20),
 C4(H4), C5(H5)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
4.c Idealised tetrahedral OH refined as rotating group:
 O8(H8), O9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 0.80027(3) 0.41289(3) 0.49933(2) 0.01428(10) Uani 1 1 d D . . . .
O1 O 0.8630(4) 0.5642(4) 0.6530(4) 0.0230(10) Uani 1 1 d . . . . .
O4 O 0.9997(4) 0.4028(4) 0.5150(3) 0.0152(9) Uani 1 1 d . . . . .
O2 O 0.7159(4) 0.1873(4) 0.4358(3) 0.0160(9) Uani 1 1 d . . . . .
O6 O 0.7191(4) 0.5498(4) 0.4509(3) 0.0190(10) Uani 1 1 d D . . . .
H6 H 0.683(5) 0.535(4) 0.3855(9) 0.028 Uiso 1 1 d DR . . . .
O5 O 0.7734(4) 0.3773(4) 0.3186(3) 0.0227(10) Uani 1 1 d . . . . .
O3 O 0.4285(4) -0.3179(4) 0.5127(3) 0.0184(10) Uani 1 1 d . . . . .
N4 N 1.0009(4) 0.2915(4) 0.5114(4) 0.0130(11) Uani 1 1 d . . . . .
O7 O 0.7386(5) 0.0458(5) 0.7620(4) 0.0335(12) Uani 1 1 d D U . . .
H7A H 0.770(7) 0.110(4) 0.814(3) 0.050 Uiso 1 1 d DR . . . .
N3 N 0.4916(5) -0.2402(5) 0.4594(4) 0.0165(12) Uani 1 1 d . . . . .
N5 N 0.6976(5) 0.2731(5) 0.2316(4) 0.0182(12) Uani 1 1 d . . . . .
N1 N 0.7904(5) 0.3054(5) 0.6391(4) 0.0166(11) Uani 1 1 d . . . . .
N2 N 0.7361(5) 0.1682(5) 0.6040(4) 0.0170(11) Uani 1 1 d . . . . .
H2 H 0.7278 0.1216 0.6454 0.020 Uiso 1 1 calc DR . . . .
C14 C 0.9564(5) 0.1978(5) 0.4154(5) 0.0141(13) Uani 1 1 d . . . . .
H14 H 0.9269 0.2112 0.3537 0.017 Uiso 1 1 calc R . . . .
O8 O 0.5445(5) 0.4727(5) 0.2665(4) 0.0449(15) Uani 1 1 d . . . . .
H8 H 0.5799 0.5098 0.2261 0.067 Uiso 1 1 calc GR . . . .
C18 C 1.0473(5) 0.2764(6) 0.6010(5) 0.0162(13) Uani 1 1 d . . . . .
H18 H 1.0785 0.3434 0.6655 0.019 Uiso 1 1 calc R . . . .
C8 C 0.6997(5) 0.1207(6) 0.4993(5) 0.0125(13) Uani 1 1 d . . . . .
C15 C 0.9555(5) 0.0821(5) 0.4104(5) 0.0143(13) Uani 1 1 d . . . . .
H15 H 0.9240 0.0169 0.3448 0.017 Uiso 1 1 calc R . . . .
C1 C 0.8892(6) 0.5893(6) 0.7545(5) 0.0195(14) Uani 1 1 d . . . . .
C13 C 0.5667(5) -0.1077(5) 0.5080(5) 0.0151(13) Uani 1 1 d . . . . .
H13 H 0.5779 -0.0716 0.5799 0.018 Uiso 1 1 calc R . . . .
C24 C 0.6920(6) 0.6390(6) 0.5184(5) 0.0261(16) Uani 1 1 d D . . . .
H24A H 0.7212 0.7174 0.4990 0.039 Uiso 1 1 calc GR . . . .
H24B H 0.7382 0.6616 0.5913 0.039 Uiso 1 1 calc GR . . . .
H24C H 0.5984 0.5976 0.5102 0.039 Uiso 1 1 calc GR . . . .
C23 C 0.5721(6) 0.1849(6) 0.2260(5) 0.0236(15) Uani 1 1 d . . . . .
H23 H 0.5387 0.1968 0.2835 0.028 Uiso 1 1 calc R . . . .
C7 C 0.8226(6) 0.3554(6) 0.7418(5) 0.0227(15) Uani 1 1 d . . . . .
H7 H 0.8129 0.2983 0.7805 0.027 Uiso 1 1 calc R . . . .
C12 C 0.4791(6) -0.2949(6) 0.3557(5) 0.0214(15) Uani 1 1 d . . . . .
H12 H 0.4305 -0.3861 0.3245 0.026 Uiso 1 1 calc R . . . .
C21 C 0.5408(6) 0.0575(6) 0.0490(5) 0.0181(14) Uani 1 1 d . . . . .
C17 C 1.0496(5) 0.1645(5) 0.5994(5) 0.0148(13) Uani 1 1 d . . . . .
H17 H 1.0832 0.1558 0.6623 0.018 Uiso 1 1 calc R . . . .
C16 C 1.0007(6) 0.0617(6) 0.5017(5) 0.0180(14) Uani 1 1 d . . . . .
C9 C 0.6266(5) -0.0263(6) 0.4505(5) 0.0138(13) Uani 1 1 d . U . . .
C22 C 0.4938(6) 0.0777(7) 0.1357(5) 0.0253(16) Uani 1 1 d . . . . .
H22 H 0.4077 0.0176 0.1327 0.030 Uiso 1 1 calc R . . . .
C2 C 0.9364(6) 0.7192(6) 0.8230(5) 0.0242(16) Uani 1 1 d . . . . .
H2A H 0.9472 0.7846 0.7932 0.029 Uiso 1 1 calc R . . . .
C6 C 0.8727(6) 0.4927(7) 0.8025(5) 0.0248(15) Uani 1 1 d . . . . .
C10 C 0.6100(6) -0.0826(6) 0.3428(5) 0.0207(15) Uani 1 1 d . . . . .
H10 H 0.6478 -0.0292 0.3027 0.025 Uiso 1 1 calc R . . . .
C11 C 0.5374(6) -0.2174(6) 0.2963(5) 0.0247(15) Uani 1 1 d . . . . .
H11 H 0.5279 -0.2558 0.2252 0.030 Uiso 1 1 calc R . . . .
C3 C 0.9662(7) 0.7500(7) 0.9306(6) 0.0335(18) Uani 1 1 d . U . . .
H3 H 0.9956 0.8353 0.9732 0.040 Uiso 1 1 calc R . . . .
C19 C 0.7472(7) 0.2571(7) 0.1497(6) 0.0350(19) Uani 1 1 d . . . . .
H19 H 0.8341 0.3178 0.1549 0.042 Uiso 1 1 calc R . . . .
C25 C 0.8267(7) -0.0032(8) 0.7675(6) 0.040(2) Uani 1 1 d . . . . .
H25A H 0.8072 -0.0642 0.6992 0.059 Uiso 1 1 calc GR . . . .
H25B H 0.8160 -0.0472 0.8198 0.059 Uiso 1 1 calc GR . . . .
H25C H 0.9162 0.0688 0.7871 0.059 Uiso 1 1 calc GR . . . .
C20 C 0.6709(6) 0.1520(7) 0.0584(6) 0.0347(19) Uani 1 1 d . . . . .
H20 H 0.7061 0.1432 0.0015 0.042 Uiso 1 1 calc R . . . .
C4 C 0.9530(8) 0.6555(8) 0.9770(6) 0.048(2) Uani 1 1 d . U . . .
H4 H 0.9781 0.6781 1.0507 0.058 Uiso 1 1 calc R . . . .
C5 C 0.9025(8) 0.5272(8) 0.9137(6) 0.049(2) Uani 1 1 d . . . . .
H5 H 0.8881 0.4625 0.9453 0.059 Uiso 1 1 calc R . . . .
C26 C 0.4156(7) 0.3661(8) 0.2090(7) 0.051(2) Uani 1 1 d . . . . .
H26A H 0.4209 0.3058 0.1526 0.077 Uiso 1 1 calc GR . . . .
H26B H 0.3634 0.3987 0.1794 0.077 Uiso 1 1 calc GR . . . .
H26C H 0.3749 0.3214 0.2560 0.077 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.75707(17) 0.89467(17) 0.10349(14) 0.0291(4) Uani 1 1 d . . . . .
O11 O 0.8195(5) 0.8356(5) 0.1550(4) 0.0441(14) Uani 1 1 d . . . . .
O13 O 0.7912(5) 1.0186(5) 0.1790(4) 0.0450(14) Uani 1 1 d . . . . .
O10 O 0.8012(5) 0.9158(5) 0.0129(4) 0.0478(15) Uani 1 1 d . . . . .
O12 O 0.6163(5) 0.8079(5) 0.0717(4) 0.0464(15) Uani 1 1 d . . . . .
O9 O 0.6899(9) 0.5722(7) 0.1402(6) 0.094(3) Uani 1 1 d . . . . .
H9 H 0.7101 0.6442 0.1336 0.141 Uiso 1 1 calc GR . . . .
C27 C 0.6517(14) 0.4833(12) 0.0444(12) 0.157(7) Uani 1 1 d . U . . .
H27A H 0.5866 0.4874 -0.0035 0.235 Uiso 1 1 calc GR . . . .
H27B H 0.6142 0.3967 0.0506 0.235 Uiso 1 1 calc GR . . . .
H27C H 0.7270 0.5019 0.0175 0.235 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 2.189(4) . ?
Dy1 O4 2.406(4) . ?
Dy1 O4 2.466(4) 2_766 ?
Dy1 O2 2.321(4) . ?
Dy1 O6 2.421(4) . ?
Dy1 O5 2.316(4) . ?
Dy1 O3 2.372(4) 2_656 ?
Dy1 N1 2.496(5) . ?
O1 C1 1.286(7) . ?
O4 Dy1 2.466(4) 2_766 ?
O4 N4 1.343(5) . ?
O2 C8 1.273(7) . ?
O6 H6 0.859(9) . ?
O6 C24 1.436(7) . ?
O5 N5 1.328(6) . ?
O3 Dy1 2.372(4) 2_656 ?
O3 N3 1.327(6) . ?
N4 C14 1.353(7) . ?
N4 C18 1.335(7) . ?
O7 H7A 0.80(2) . ?
O7 C25 1.420(8) . ?
N3 C13 1.357(7) . ?
N3 C12 1.358(8) . ?
N5 C23 1.352(7) . ?
N5 C19 1.337(8) . ?
N1 N2 1.405(6) . ?
N1 C7 1.296(8) . ?
N2 H2 0.8600 . ?
N2 C8 1.317(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.382(8) . ?
O8 H8 0.8200 . ?
O8 C26 1.414(8) . ?
C18 H18 0.9300 . ?
C18 C17 1.363(8) . ?
C8 C9 1.498(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.384(8) . ?
C1 C2 1.425(8) . ?
C1 C6 1.407(9) . ?
C13 H13 0.9300 . ?
C13 C9 1.387(8) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C23 H23 0.9300 . ?
C23 C22 1.373(8) . ?
C7 H7 0.9300 . ?
C7 C6 1.458(9) . ?
C12 H12 0.9300 . ?
C12 C11 1.373(9) . ?
C21 C21 1.479(12) 2_655 ?
C21 C22 1.382(9) . ?
C21 C20 1.400(8) . ?
C17 H17 0.9300 . ?
C17 C16 1.414(8) . ?
C16 C16 1.476(11) 2_756 ?
C9 C10 1.397(8) . ?
C22 H22 0.9300 . ?
C2 H2A 0.9300 . ?
C2 C3 1.359(9) . ?
C6 C5 1.402(10) . ?
C10 H10 0.9300 . ?
C10 C11 1.376(8) . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.378(10) . ?
C19 H19 0.9300 . ?
C19 C20 1.368(9) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C20 H20 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.380(10) . ?
C5 H5 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
Cl1 O11 1.449(5) . ?
Cl1 O13 1.445(5) . ?
Cl1 O10 1.420(5) . ?
Cl1 O12 1.433(5) . ?
O9 H9 0.8200 . ?
O9 C27 1.338(13) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 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 O4 78.65(15) . 2_766 ?
O1 Dy1 O4 98.02(15) . . ?
O1 Dy1 O2 137.41(16) . . ?
O1 Dy1 O6 78.26(15) . . ?
O1 Dy1 O5 143.61(15) . . ?
O1 Dy1 O3 94.01(15) . 2_656 ?
O1 Dy1 N1 72.78(16) . . ?
O4 Dy1 O4 60.92(15) . 2_766 ?
O4 Dy1 O6 137.90(14) . . ?
O4 Dy1 N1 78.80(14) . . ?
O4 Dy1 N1 126.02(14) 2_766 . ?
O2 Dy1 O4 130.48(13) . 2_766 ?
O2 Dy1 O4 78.30(13) . . ?
O2 Dy1 O6 131.77(14) . . ?
O2 Dy1 O3 75.53(13) . 2_656 ?
O2 Dy1 N1 64.84(15) . . ?
O6 Dy1 O4 77.42(13) . 2_766 ?
O6 Dy1 N1 136.41(15) . . ?
O5 Dy1 O4 89.74(14) . . ?
O5 Dy1 O4 74.31(14) . 2_766 ?
O5 Dy1 O2 78.96(14) . . ?
O5 Dy1 O6 72.47(15) . . ?
O5 Dy1 O3 95.62(15) . 2_656 ?
O5 Dy1 N1 143.48(15) . . ?
O3 Dy1 O4 151.70(13) 2_656 . ?
O3 Dy1 O4 147.10(13) 2_656 2_766 ?
O3 Dy1 O6 69.68(14) 2_656 . ?
O3 Dy1 N1 80.48(15) 2_656 . ?
C1 O1 Dy1 144.9(4) . . ?
Dy1 O4 Dy1 119.08(15) . 2_766 ?
N4 O4 Dy1 117.3(3) . 2_766 ?
N4 O4 Dy1 122.5(3) . . ?
C8 O2 Dy1 120.8(4) . . ?
Dy1 O6 H6 120.9(15) . . ?
C24 O6 Dy1 128.2(4) . . ?
C24 O6 H6 109.1(15) . . ?
N5 O5 Dy1 134.3(4) . . ?
N3 O3 Dy1 125.6(3) . 2_656 ?
O4 N4 C14 118.3(5) . . ?
C18 N4 O4 120.0(5) . . ?
C18 N4 C14 121.7(5) . . ?
C25 O7 H7A 106(5) . . ?
O3 N3 C13 120.3(5) . . ?
O3 N3 C12 119.1(5) . . ?
C13 N3 C12 120.7(6) . . ?
O5 N5 C23 120.3(5) . . ?
O5 N5 C19 119.0(5) . . ?
C19 N5 C23 120.6(6) . . ?
N2 N1 Dy1 117.1(4) . . ?
C7 N1 Dy1 130.1(4) . . ?
C7 N1 N2 112.8(5) . . ?
N1 N2 H2 124.6 . . ?
C8 N2 N1 110.8(5) . . ?
C8 N2 H2 124.6 . . ?
N4 C14 H14 120.5 . . ?
N4 C14 C15 119.1(6) . . ?
C15 C14 H14 120.5 . . ?
C26 O8 H8 109.5 . . ?
N4 C18 H18 119.5 . . ?
N4 C18 C17 121.1(6) . . ?
C17 C18 H18 119.5 . . ?
O2 C8 N2 126.3(5) . . ?
O2 C8 C9 117.0(5) . . ?
N2 C8 C9 116.6(5) . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 121.0(6) . . ?
C16 C15 H15 119.5 . . ?
O1 C1 C2 120.0(6) . . ?
O1 C1 C6 122.7(6) . . ?
C6 C1 C2 117.4(6) . . ?
N3 C13 H13 120.0 . . ?
N3 C13 C9 120.1(6) . . ?
C9 C13 H13 120.0 . . ?
O6 C24 H24A 109.5 . . ?
O6 C24 H24B 109.5 . . ?
O6 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C23 H23 119.9 . . ?
N5 C23 C22 120.2(6) . . ?
C22 C23 H23 119.9 . . ?
N1 C7 H7 116.8 . . ?
N1 C7 C6 126.3(6) . . ?
C6 C7 H7 116.8 . . ?
N3 C12 H12 119.6 . . ?
N3 C12 C11 120.8(6) . . ?
C11 C12 H12 119.6 . . ?
C22 C21 C21 122.4(7) . 2_655 ?
C22 C21 C20 116.5(6) . . ?
C20 C21 C21 121.1(7) . 2_655 ?
C18 C17 H17 120.2 . . ?
C18 C17 C16 119.7(6) . . ?
C16 C17 H17 120.2 . . ?
C15 C16 C17 117.4(5) . . ?
C15 C16 C16 121.9(7) . 2_756 ?
C17 C16 C16 120.6(7) . 2_756 ?
C13 C9 C8 121.2(5) . . ?
C13 C9 C10 119.1(5) . . ?
C10 C9 C8 119.5(6) . . ?
C23 C22 C21 121.2(6) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C1 C2 H2A 119.1 . . ?
C3 C2 C1 121.8(7) . . ?
C3 C2 H2A 119.1 . . ?
C1 C6 C7 123.1(6) . . ?
C5 C6 C1 119.5(6) . . ?
C5 C6 C7 117.4(6) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.7(6) . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 119.5(6) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(7) . . ?
C4 C3 H3 119.8 . . ?
N5 C19 H19 119.8 . . ?
N5 C19 C20 120.4(6) . . ?
C20 C19 H19 119.8 . . ?
O7 C25 H25A 109.5 . . ?
O7 C25 H25B 109.5 . . ?
O7 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C21 C20 H20 119.4 . . ?
C19 C20 C21 121.1(6) . . ?
C19 C20 H20 119.4 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.8(7) . . ?
C5 C4 H4 120.1 . . ?
C6 C5 H5 119.5 . . ?
C4 C5 C6 121.0(7) . . ?
C4 C5 H5 119.5 . . ?
O8 C26 H26A 109.5 . . ?
O8 C26 H26B 109.5 . . ?
O8 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O13 Cl1 O11 108.5(3) . . ?
O10 Cl1 O11 110.1(3) . . ?
O10 Cl1 O13 110.2(3) . . ?
O10 Cl1 O12 109.8(3) . . ?
O12 Cl1 O11 108.8(3) . . ?
O12 Cl1 O13 109.4(3) . . ?
C27 O9 H9 109.5 . . ?
O9 C27 H27A 109.5 . . ?
O9 C27 H27B 109.5 . . ?
O9 C27 H27C 109.5 . . ?
H27A C27 H27B 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 O1 C1 C2 176.6(4) . . . . ?
Dy1 O1 C1 C6 -3.7(11) . . . . ?
Dy1 O4 N4 C14 77.3(5) . . . . ?
Dy1 O4 N4 C14 -90.2(5) 2_766 . . . ?
Dy1 O4 N4 C18 88.6(5) 2_766 . . . ?
Dy1 O4 N4 C18 -103.9(5) . . . . ?
Dy1 O2 C8 N2 -5.7(7) . . . . ?
Dy1 O2 C8 C9 171.2(3) . . . . ?
Dy1 O5 N5 C23 37.2(8) . . . . ?
Dy1 O5 N5 C19 -143.0(5) . . . . ?
Dy1 O3 N3 C13 101.3(5) 2_656 . . . ?
Dy1 O3 N3 C12 -78.2(6) 2_656 . . . ?
Dy1 N1 N2 C8 0.2(5) . . . . ?
Dy1 N1 C7 C6 1.1(9) . . . . ?
O1 C1 C2 C3 -179.5(6) . . . . ?
O1 C1 C6 C7 -1.0(10) . . . . ?
O1 C1 C6 C5 -179.6(7) . . . . ?
O4 N4 C14 C15 -179.2(5) . . . . ?
O4 N4 C18 C17 -180.0(5) . . . . ?
O2 C8 C9 C13 -158.9(5) . . . . ?
O2 C8 C9 C10 16.4(7) . . . . ?
O5 N5 C23 C22 179.6(6) . . . . ?
O5 N5 C19 C20 -178.9(6) . . . . ?
O3 N3 C13 C9 -176.5(5) . . . . ?
O3 N3 C12 C11 176.7(5) . . . . ?
N4 C14 C15 C16 -0.8(8) . . . . ?
N4 C18 C17 C16 -0.8(9) . . . . ?
N3 C13 C9 C8 174.4(5) . . . . ?
N3 C13 C9 C10 -0.9(8) . . . . ?
N3 C12 C11 C10 0.4(9) . . . . ?
N5 C23 C22 C21 0.0(10) . . . . ?
N5 C19 C20 C21 -1.4(12) . . . . ?
N1 N2 C8 O2 3.4(8) . . . . ?
N1 N2 C8 C9 -173.5(4) . . . . ?
N1 C7 C6 C1 1.7(10) . . . . ?
N1 C7 C6 C5 -179.7(7) . . . . ?
N2 N1 C7 C6 -175.5(6) . . . . ?
N2 C8 C9 C13 18.4(8) . . . . ?
N2 C8 C9 C10 -166.4(5) . . . . ?
C14 N4 C18 C17 -1.1(8) . . . . ?
C14 C15 C16 C17 -1.0(8) . . . . ?
C14 C15 C16 C16 179.4(7) . . . 2_756 ?
C18 N4 C14 C15 1.9(8) . . . . ?
C18 C17 C16 C15 1.8(8) . . . . ?
C18 C17 C16 C16 -178.6(7) . . . 2_756 ?
C8 C9 C10 C11 -176.9(5) . . . . ?
C1 C2 C3 C4 0.9(11) . . . . ?
C1 C6 C5 C4 -2.7(12) . . . . ?
C13 N3 C12 C11 -2.8(9) . . . . ?
C13 C9 C10 C11 -1.5(9) . . . . ?
C23 N5 C19 C20 0.9(11) . . . . ?
C7 N1 N2 C8 177.4(5) . . . . ?
C7 C6 C5 C4 178.6(7) . . . . ?
C12 N3 C13 C9 3.0(8) . . . . ?
C21 C21 C22 C23 179.6(7) 2_655 . . . ?
C21 C21 C20 C19 -178.9(8) 2_655 . . . ?
C9 C10 C11 C12 1.7(9) . . . . ?
C22 C21 C20 C19 1.1(11) . . . . ?
C2 C1 C6 C7 178.7(6) . . . . ?
C2 C1 C6 C5 0.1(10) . . . . ?
C2 C3 C4 C5 -3.5(13) . . . . ?
C6 C1 C2 C3 0.8(9) . . . . ?
C3 C4 C5 C6 4.5(13) . . . . ?
C19 N5 C23 C22 -0.2(10) . . . . ?
C20 C21 C22 C23 -0.5(10) . . . . ?

_olex2_date_sample_data_collection 2017-05-03
_olex2_exptl_crystal_mounting_method loop
_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.794
