#------------------------------------------------------------------------------
#$Date: 2021-09-01 02:02:28 +0300 (Wed, 01 Sep 2021) $
#$Revision: 268337 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/81/7708159.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7708159
loop_
_publ_author_name
'Ye, Hua-Jian'
'Zhang, Tian'
'Huang, Shu-Yuan'
'Liu, Xiao-Ling'
'Chen, Wen-Bin'
'Zhang, Yi-Quan'
'Tang, Jinkui'
'Dong, Wen'
_publ_section_title
;
 Syntheses, structural modulation and slow magnetic relaxation of
 three dysprosium(III) complexes with mononuclear, dinuclear and
 one-dimensional structures
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02532E
_journal_year                    2021
_chemical_formula_moiety         'C32 H28 Dy2 N10 O20, 5(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C36 H44 Dy2 N12 O25'
_chemical_formula_weight         1369.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-08-26 deposited with the CCDC.	2021-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                103.705(2)
_cell_angle_beta                 90.636(2)
_cell_angle_gamma                106.159(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6507(3)
_cell_length_b                   11.3380(2)
_cell_length_c                   11.8034(4)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    105.88(10)
_cell_measurement_theta_max      75.7670
_cell_measurement_theta_min      3.8760
_cell_volume                     1201.07(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105.88(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     24.00 117.00   0.50    0.05    --   45.87  77.00 -90.00  186
  2  ω     92.00 119.00   0.50    0.05    --   45.87  77.00-150.00   54
  3  ω     69.00  94.00   0.50    0.05    --   45.87 142.00-101.00   50
  4  ω     24.00  87.00   0.50    0.05    --   45.87  77.00-150.00  126
  5  ω     90.00 178.00   0.50    0.05    --  106.06  15.00 -30.00  176
  6  ω    117.00 164.00   0.50    0.05    --  106.06  45.00   0.00   94
  7  ω     95.00 120.00   0.50    0.05    --  106.06 142.00-101.00   50
  8  ω     85.00 128.00   0.50    0.05    --  106.06 127.00  88.00   86
  9  ω     37.00  73.00   0.50    0.05    --  106.06 -61.00-150.00   72
 10  ω     68.00 102.00   0.50    0.05    --  106.06 -94.00-150.00   68
 11  ω     92.00 123.00   0.50    0.05    --  106.06-142.00-157.00   62
 12  ω     55.00 111.00   0.50    0.05    --  106.06-125.00-120.00  112
 13  ω     58.00 112.00   0.50    0.05    --  106.06-125.00 -30.00  108
 14  ω     71.00  97.00   0.50    0.05    --  106.06 -94.00  30.00   52
 15  ω     46.00 112.00   0.50    0.05    --  106.06-127.00  12.00  132
 16  ω     53.00  93.00   0.50    0.05    --   45.87-127.00  12.00   80
 17  ω     36.00 111.00   0.50    0.05    --  106.06-125.00  30.00  150
 18  ω     34.00  66.00   0.50    0.05    --  106.06 -94.00  30.00   64
 19  ω     33.00  69.00   0.50    0.05    --  106.06 -61.00  30.00   72
 20  ω     34.00  73.00   0.50    0.05    --  106.06 -61.00 150.00   78
 21  ω     40.00  73.00   0.50    0.05    --  106.06 -61.00-120.00   66
 22  ω     33.00  67.00   0.50    0.05    --  106.06 -77.00-150.00   68
 23  ω     47.00  87.00   0.50    0.05    --  106.06-142.00-157.00   80
 24  ω     35.00 100.00   0.50    0.05    --   45.87-142.00-157.00  130
 25  ω    -55.00 -29.00   0.50    0.05    -- -102.00  61.00 120.00   52
 26  ω    -68.00 -30.00   0.50    0.05    -- -102.00  61.00  60.00   76
 27  ω    -88.00 -38.00   0.50    0.05    --  -45.87 127.00  88.00  100
 28  ω    -63.00 -31.00   0.50    0.05    -- -102.00  61.00-150.00   64
 29  ω    -86.00 -61.00   0.50    0.05    --  -45.87 142.00-101.00   50
 30  ω   -124.00 -98.00   0.50    0.05    -- -102.00 142.00-101.00   52
 31  ω   -111.00 -35.00   0.50    0.05    -- -102.00 127.00  88.00  152
 32  ω    -97.00 -29.00   0.50    0.05    -- -102.00  77.00 120.00  136
 33  ω   -141.00 -93.00   0.50    0.05    -- -102.00 -30.00  60.00   96
 34  ω   -104.00 -78.00   0.50    0.05    --  -45.87-127.00  12.00   52
 35  ω   -101.00 -76.00   0.50    0.05    --  -45.87-125.00  30.00   50
 36  ω   -111.00 -86.00   0.50    0.05    --  -45.87-125.00  90.00   50
 37  ω   -110.00 -85.00   0.50    0.05    -- -102.00-127.00  12.00   50
 38  ω   -145.00-112.00   0.50    0.05    -- -102.00 -77.00 -60.00   66
 39  ω   -117.00 -63.00   0.50    0.05    --  -45.87-142.00-157.00  108
 40  ω   -142.00-116.00   0.50    0.05    -- -102.00-142.00-157.00   52
 41  ω   -172.00 -29.00   0.50    0.05    -- -102.00   0.00-180.00  286
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1133099000
_diffrn_orient_matrix_UB_12      -0.0130545000
_diffrn_orient_matrix_UB_13      0.0855329000
_diffrn_orient_matrix_UB_21      -0.0819719000
_diffrn_orient_matrix_UB_22      0.0481737000
_diffrn_orient_matrix_UB_23      0.1039214000
_diffrn_orient_matrix_UB_31      -0.0908461000
_diffrn_orient_matrix_UB_32      -0.1373102000
_diffrn_orient_matrix_UB_33      -0.0075151000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.391
_diffrn_reflns_theta_min         3.868
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.346
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17858
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.092
_refine_diff_density_max         2.654
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.147
_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     350
_refine_ls_number_reflns         4814
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0419
_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)+(0.0827P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4539
_reflns_number_total             4814
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02532e2.cif
_cod_data_source_block           exp_646
_cod_database_code               7708159
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Dy'
_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.
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H9A,H9B} of O9, H13B of O13, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8, H5 of O5, {H10A,H10B} of O10, H1 of O1,
  {H11A,H11B} of O11, {H12A,H12B} of O12, H13A of O13
2. Restrained distances
 O9-H9B
 0.85 with sigma of 0.02
 H10B-H9B
 3 with sigma of 0.02
 H9B-H9A
 1.38 with sigma of 0.02
 O10-H9B
 3 with sigma of 0.02
3. Others
 Fixed Sof: O11(0.5) H11A(0.5) H11B(0.5)
4.a Riding coordinates:
 O9(H9A,H9B), O10(H10A,H10B), O12(H12A,H12B), O13(H13A,H13B)
4.b Free rotating group:
 O11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 N5(H5A), C4(H4), C5(H5B), C9(H9), C13(H13), C14(H14), C15(H15)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
4.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O5(H5), O8(H8)
;
_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 4.136
_oxdiff_exptl_absorpt_empirical_full_min 0.448
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.58058(2) 0.67669(2) 0.55479(2) 0.01613(11) Uani 1 1 d . . . . .
O1 O 1.1277(3) 0.5828(3) 0.6901(3) 0.0241(6) Uani 1 1 d . . . . .
H1 H 1.138079 0.641636 0.658741 0.036 Uiso 1 1 calc R U . . .
O2 O 1.0580(3) 0.7241(3) 0.5846(3) 0.0228(6) Uani 1 1 d . . . . .
O3 O 0.8282(3) 0.7182(3) 0.5600(3) 0.0210(6) Uani 1 1 d . . . . .
O4 O 0.6359(3) 0.4805(3) 0.5318(2) 0.0166(5) Uani 1 1 d . . . . .
O5 O 0.5347(4) 0.2952(3) 0.0808(3) 0.0322(8) Uani 1 1 d . . . . .
H5 H 0.488583 0.306309 0.138334 0.048 Uiso 1 1 calc R U . . .
O6 O 0.5132(3) 0.4145(3) 0.2883(2) 0.0212(6) Uani 1 1 d . . . . .
O7 O 0.6308(3) 0.6204(3) 0.3541(3) 0.0212(6) Uani 1 1 d . . . . .
O8 O 0.7508(5) 0.7474(3) 0.2148(3) 0.0355(8) Uani 1 1 d . . . . .
H8 H 0.719810 0.733819 0.276346 0.053 Uiso 1 1 calc R U . . .
O9 O 0.4028(3) 0.7742(3) 0.6521(3) 0.0220(6) Uani 1 1 d D . . . .
H9A H 0.405045 0.842451 0.633099 0.026 Uiso 1 1 d DR U . . .
H9B H 0.356075 0.753031 0.702059 0.026 Uiso 1 1 d DR U . . .
O10 O 0.6852(3) 0.8216(3) 0.7425(3) 0.0266(7) Uani 1 1 d D . . . .
H10A H 0.766534 0.818259 0.767930 0.040 Uiso 1 1 d R U . . .
H10B H 0.661944 0.881309 0.781440 0.040 Uiso 1 1 d DR U . . .
N1 N 0.5788(4) 0.2612(3) 0.5871(3) 0.0179(7) Uani 1 1 d . . . . .
N2 N 0.5411(4) 0.1578(3) 0.6226(3) 0.0190(7) Uani 1 1 d . . . . .
N3 N 0.3244(4) 0.1161(3) 0.4951(3) 0.0201(7) Uani 1 1 d . . . . .
N4 N 0.3346(4) -0.0184(3) 0.6063(3) 0.0195(7) Uani 1 1 d . . . . .
N5 N 0.2061(4) -0.0575(3) 0.5411(3) 0.0214(7) Uani 1 1 d . . . . .
H5A H 0.137424 -0.124678 0.541505 0.026 Uiso 1 1 calc R U . . .
C1 C 0.9226(5) 0.6696(4) 0.5832(4) 0.0191(8) Uani 1 1 d . . . . .
C2 C 0.8840(4) 0.5452(4) 0.6148(3) 0.0171(8) Uani 1 1 d . . . . .
C3 C 0.9909(5) 0.5105(4) 0.6701(4) 0.0205(8) Uani 1 1 d . . . . .
C4 C 0.9578(5) 0.3978(4) 0.7097(4) 0.0216(8) Uani 1 1 d . . . . .
H4 H 1.028209 0.380255 0.751992 0.026 Uiso 1 1 calc R U . . .
C5 C 0.8219(5) 0.3155(4) 0.6854(4) 0.0213(8) Uani 1 1 d . . . . .
H5B H 0.800197 0.241071 0.710385 0.026 Uiso 1 1 calc R U . . .
C6 C 0.7136(4) 0.3421(4) 0.6225(4) 0.0184(8) Uani 1 1 d . . . . .
C7 C 0.7410(4) 0.4589(4) 0.5873(3) 0.0163(7) Uani 1 1 d . . . . .
C8 C 0.4018(4) 0.0863(4) 0.5753(4) 0.0184(8) Uani 1 1 d . . . . .
C9 C 0.2013(5) 0.0233(4) 0.4763(4) 0.0219(8) Uani 1 1 d . . . . .
H9 H 0.123221 0.015489 0.425372 0.026 Uiso 1 1 calc R U . . .
C10 C 0.5929(4) 0.5182(4) 0.2731(4) 0.0198(8) Uani 1 1 d . . . . .
C11 C 0.6421(5) 0.5215(4) 0.1552(4) 0.0222(9) Uani 1 1 d . . . . .
C12 C 0.7196(5) 0.6357(5) 0.1308(4) 0.0279(10) Uani 1 1 d . . . . .
C13 C 0.7642(6) 0.6391(5) 0.0199(4) 0.0342(11) Uani 1 1 d . . . . .
H13 H 0.813745 0.715639 0.003921 0.041 Uiso 1 1 calc R U . . .
C14 C 0.7336(6) 0.5268(5) -0.0667(4) 0.0333(11) Uani 1 1 d . . . . .
H14 H 0.765009 0.528907 -0.140628 0.040 Uiso 1 1 calc R U . . .
C15 C 0.6584(6) 0.4124(5) -0.0470(4) 0.0326(11) Uani 1 1 d . . . . .
H15 H 0.638998 0.338145 -0.106382 0.039 Uiso 1 1 calc R U . . .
C16 C 0.6117(5) 0.4099(5) 0.0645(4) 0.0274(10) Uani 1 1 d . . . . .
O11 O 1.0230(8) 0.9147(8) 0.2345(7) 0.0390(17) Uani 0.5 1 d G . P . .
H11A H 0.944553 0.854712 0.216993 0.059 Uiso 0.5 1 d G U P . .
H11B H 1.009712 0.981631 0.221709 0.059 Uiso 0.5 1 d G U P . .
O12 O 0.6166(5) 0.0432(4) 0.8059(4) 0.0492(10) Uani 1 1 d . . . . .
H12A H 0.603706 0.091684 0.764885 0.074 Uiso 1 1 d R U . . .
H12B H 0.543966 0.032164 0.851665 0.074 Uiso 1 1 d R U . . .
O13 O 0.3659(6) 0.0818(4) 0.9044(4) 0.0547(11) Uani 1 1 d . . . . .
H13A H 0.315773 0.098194 0.853780 0.082 Uiso 1 1 d R U . . .
H13B H 0.415443 0.147004 0.952470 0.066 Uiso 1 1 d R U . . .
N6 N 1.0300(6) 0.1401(7) 0.1491(5) 0.0573(15) Uani 1 1 d . . . . .
C17 C 0.8378(10) 0.1974(11) 0.0386(7) 0.086(3) Uani 1 1 d . . . . .
H17A H 0.823969 0.149028 -0.041388 0.130 Uiso 1 1 calc R U . . .
H17B H 0.868720 0.286274 0.041312 0.130 Uiso 1 1 calc R U . . .
H17C H 0.748226 0.177970 0.074549 0.130 Uiso 1 1 calc R U . . .
C18 C 0.9471(7) 0.1658(8) 0.1011(5) 0.0562(18) Uani 1 1 d . . . . .
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -6 1 0.1294
-1 -3 7 0.0915
1 0 7 0.0496
0 0 -7 0.0325
0 0 7 0.0548
6 0 2 0.1026
1 -7 3 0.1193
-3 -3 6 0.1163
-5 -2 -1 0.1179
-4 6 -4 0.0805
3 5 -1 0.1453
2 6 -1 0.1447
3 5 -5 0.1302
-2 2 6 0.0556
2 -3 -6 0.0545
0 -6 -3 0.0998
-6 0 0 0.1071
5 -5 4 0.0818
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 Dy1 107.29(7) . 2_666 ?
O3 Dy1 O4 141.57(10) . 2_666 ?
O3 Dy1 O4 72.04(10) . . ?
O3 Dy1 O6 110.94(10) . 2_666 ?
O3 Dy1 O7 75.17(11) . . ?
O3 Dy1 O9 138.16(10) . . ?
O3 Dy1 O10 71.61(11) . . ?
O3 Dy1 N1 125.68(11) . 2_666 ?
O3 Dy1 N3 73.47(11) . 2_666 ?
O4 Dy1 Dy1 37.73(7) 2_666 2_666 ?
O4 Dy1 Dy1 37.42(7) . 2_666 ?
O4 Dy1 O4 75.15(11) 2_666 . ?
O4 Dy1 O6 76.15(10) 2_666 2_666 ?
O4 Dy1 O6 71.61(10) . 2_666 ?
O4 Dy1 O7 77.67(10) 2_666 . ?
O4 Dy1 O7 75.34(10) . . ?
O4 Dy1 O9 136.77(10) . . ?
O4 Dy1 O9 80.15(10) 2_666 . ?
O4 Dy1 O10 110.93(10) . . ?
O4 Dy1 O10 140.54(10) 2_666 . ?
O4 Dy1 N1 128.01(10) . 2_666 ?
O4 Dy1 N1 63.77(10) 2_666 2_666 ?
O4 Dy1 N3 139.56(11) . 2_666 ?
O4 Dy1 N3 124.91(11) 2_666 2_666 ?
O6 Dy1 Dy1 69.50(7) 2_666 2_666 ?
O6 Dy1 O9 68.32(10) 2_666 . ?
O6 Dy1 O10 69.79(11) 2_666 . ?
O6 Dy1 N1 123.12(11) 2_666 2_666 ?
O6 Dy1 N3 142.03(11) 2_666 2_666 ?
O7 Dy1 Dy1 72.88(7) . 2_666 ?
O7 Dy1 O6 141.97(10) . 2_666 ?
O7 Dy1 O9 132.68(10) . . ?
O7 Dy1 O10 141.71(11) . . ?
O7 Dy1 N1 66.21(11) . 2_666 ?
O7 Dy1 N3 75.98(11) . 2_666 ?
O9 Dy1 Dy1 110.72(7) . 2_666 ?
O9 Dy1 N1 66.52(10) . 2_666 ?
O9 Dy1 N3 83.60(11) . 2_666 ?
O10 Dy1 Dy1 135.36(8) . 2_666 ?
O10 Dy1 O9 69.30(10) . . ?
O10 Dy1 N1 120.99(11) . 2_666 ?
O10 Dy1 N3 76.78(11) . 2_666 ?
N1 Dy1 Dy1 96.43(7) 2_666 2_666 ?
N3 Dy1 Dy1 147.31(8) 2_666 2_666 ?
N3 Dy1 N1 61.44(11) 2_666 2_666 ?
C3 O1 H1 109.5 . . ?
C1 O3 Dy1 138.6(3) . . ?
Dy1 O4 Dy1 104.85(11) 2_666 . ?
C7 O4 Dy1 124.3(2) . 2_666 ?
C7 O4 Dy1 127.5(2) . . ?
C16 O5 H5 109.5 . . ?
C10 O6 Dy1 139.4(3) . 2_666 ?
C10 O7 Dy1 134.0(3) . . ?
C12 O8 H8 109.5 . . ?
Dy1 O9 H9A 111.6 . . ?
Dy1 O9 H9B 126.2 . . ?
H9A O9 H9B 121.6 . . ?
Dy1 O10 H10A 116.6 . . ?
Dy1 O10 H10B 130.4 . . ?
H10A O10 H10B 112.2 . . ?
N2 N1 Dy1 124.9(3) . 2_666 ?
N2 N1 C6 118.3(4) . . ?
C6 N1 Dy1 116.7(3) . 2_666 ?
N1 N2 C8 109.9(3) . . ?
C8 N3 Dy1 119.2(3) . 2_666 ?
C9 N3 Dy1 137.2(3) . 2_666 ?
C9 N3 C8 102.9(4) . . ?
C8 N4 N5 102.3(3) . . ?
N4 N5 H5A 124.9 . . ?
C9 N5 N4 110.2(3) . . ?
C9 N5 H5A 124.9 . . ?
O2 C1 C2 115.8(4) . . ?
O3 C1 O2 122.5(4) . . ?
O3 C1 C2 121.7(4) . . ?
C3 C2 C1 119.4(4) . . ?
C3 C2 C7 119.3(4) . . ?
C7 C2 C1 121.3(4) . . ?
O1 C3 C2 121.8(4) . . ?
O1 C3 C4 116.5(4) . . ?
C2 C3 C4 121.7(4) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.4(4) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5B 119.6 . . ?
C4 C5 C6 120.7(4) . . ?
C6 C5 H5B 119.6 . . ?
N1 C6 C5 124.5(4) . . ?
N1 C6 C7 114.2(4) . . ?
C5 C6 C7 121.3(4) . . ?
O4 C7 C2 123.7(4) . . ?
O4 C7 C6 119.0(4) . . ?
C2 C7 C6 117.3(4) . . ?
N3 C8 N2 124.1(4) . . ?
N4 C8 N2 121.3(4) . . ?
N4 C8 N3 114.6(4) . . ?
N3 C9 N5 110.0(4) . . ?
N3 C9 H9 125.0 . . ?
N5 C9 H9 125.0 . . ?
O6 C10 O7 123.0(4) . . ?
O6 C10 C11 118.6(4) . . ?
O7 C10 C11 118.4(4) . . ?
C12 C11 C10 121.0(4) . . ?
C12 C11 C16 118.2(4) . . ?
C16 C11 C10 120.9(4) . . ?
O8 C12 C11 120.9(4) . . ?
O8 C12 C13 118.0(4) . . ?
C13 C12 C11 121.0(5) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 119.0(5) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 118.9 . . ?
C15 C14 C13 122.1(4) . . ?
C15 C14 H14 118.9 . . ?
C14 C15 H15 120.7 . . ?
C14 C15 C16 118.6(5) . . ?
C16 C15 H15 120.7 . . ?
O5 C16 C11 121.7(4) . . ?
O5 C16 C15 117.2(4) . . ?
C15 C16 C11 121.1(5) . . ?
H11A O11 H11B 109.4 . . ?
H12A O12 H12B 107.7 . . ?
H13A O13 H13B 112.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
N6 C18 C17 179.2(10) . . ?
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 Dy1 3.7652(4) 2_666 ?
Dy1 O3 2.300(3) . ?
Dy1 O4 2.384(3) . ?
Dy1 O4 2.367(3) 2_666 ?
Dy1 O6 2.396(3) 2_666 ?
Dy1 O7 2.394(3) . ?
Dy1 O9 2.446(3) . ?
Dy1 O10 2.435(3) . ?
Dy1 N1 2.602(4) 2_666 ?
Dy1 N3 2.484(3) 2_666 ?
O1 H1 0.8200 . ?
O1 C3 1.330(5) . ?
O2 C1 1.279(5) . ?
O3 C1 1.247(5) . ?
O4 C7 1.311(5) . ?
O5 H5 0.8200 . ?
O5 C16 1.365(6) . ?
O6 C10 1.267(5) . ?
O7 C10 1.273(5) . ?
O8 H8 0.8200 . ?
O8 C12 1.365(6) . ?
O9 H9A 0.8502 . ?
O9 H9B 0.7880 . ?
O10 H10A 0.8510 . ?
O10 H10B 0.8121 . ?
N1 N2 1.297(5) . ?
N1 C6 1.360(5) . ?
N2 C8 1.392(5) . ?
N3 C8 1.359(5) . ?
N3 C9 1.325(6) . ?
N4 N5 1.356(5) . ?
N4 C8 1.322(5) . ?
N5 H5A 0.8600 . ?
N5 C9 1.335(6) . ?
C1 C2 1.492(6) . ?
C2 C3 1.406(6) . ?
C2 C7 1.434(6) . ?
C3 C4 1.419(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.362(6) . ?
C5 H5B 0.9300 . ?
C5 C6 1.414(6) . ?
C6 C7 1.436(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.481(6) . ?
C11 C12 1.401(7) . ?
C11 C16 1.406(7) . ?
C12 C13 1.389(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.387(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.373(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.399(7) . ?
O11 H11A 0.8499 . ?
O11 H11B 0.8505 . ?
O12 H12A 0.8449 . ?
O12 H12B 0.8891 . ?
O13 H13A 0.8500 . ?
O13 H13B 0.8342 . ?
N6 C18 1.115(9) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 C18 1.451(10) . ?
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 C1 O2 -175.1(3) . . . . ?
Dy1 O3 C1 C2 3.0(7) . . . . ?
Dy1 O4 C7 C2 -39.6(5) . . . . ?
Dy1 O4 C7 C2 164.5(3) 2_666 . . . ?
Dy1 O4 C7 C6 140.9(3) . . . . ?
Dy1 O4 C7 C6 -15.0(5) 2_666 . . . ?
Dy1 O6 C10 O7 -12.1(7) 2_666 . . . ?
Dy1 O6 C10 C11 169.1(3) 2_666 . . . ?
Dy1 O7 C10 O6 -1.5(6) . . . . ?
Dy1 O7 C10 C11 177.3(3) . . . . ?
Dy1 N1 N2 C8 -1.2(4) 2_666 . . . ?
Dy1 N1 C6 C5 -170.6(3) 2_666 . . . ?
Dy1 N1 C6 C7 7.6(4) 2_666 . . . ?
Dy1 N3 C8 N2 -8.0(5) 2_666 . . . ?
Dy1 N3 C8 N4 172.2(3) 2_666 . . . ?
Dy1 N3 C9 N5 -170.1(3) 2_666 . . . ?
O1 C3 C4 C5 -175.8(4) . . . . ?
O2 C1 C2 C3 15.3(6) . . . . ?
O2 C1 C2 C7 -163.2(4) . . . . ?
O3 C1 C2 C3 -162.9(4) . . . . ?
O3 C1 C2 C7 18.6(6) . . . . ?
O6 C10 C11 C12 174.4(4) . . . . ?
O6 C10 C11 C16 -5.4(6) . . . . ?
O7 C10 C11 C12 -4.5(6) . . . . ?
O7 C10 C11 C16 175.7(4) . . . . ?
O8 C12 C13 C14 180.0(5) . . . . ?
N1 N2 C8 N3 6.0(5) . . . . ?
N1 N2 C8 N4 -174.3(4) . . . . ?
N1 C6 C7 O4 3.5(5) . . . . ?
N1 C6 C7 C2 -176.0(3) . . . . ?
N2 N1 C6 C5 7.0(6) . . . . ?
N2 N1 C6 C7 -174.8(3) . . . . ?
N4 N5 C9 N3 0.5(5) . . . . ?
N5 N4 C8 N2 -179.7(4) . . . . ?
N5 N4 C8 N3 0.1(5) . . . . ?
C1 C2 C3 O1 -3.3(6) . . . . ?
C1 C2 C3 C4 175.3(4) . . . . ?
C1 C2 C7 O4 1.3(6) . . . . ?
C1 C2 C7 C6 -179.3(4) . . . . ?
C2 C3 C4 C5 5.5(7) . . . . ?
C3 C2 C7 O4 -177.1(4) . . . . ?
C3 C2 C7 C6 2.3(6) . . . . ?
C3 C4 C5 C6 -0.8(7) . . . . ?
C4 C5 C6 N1 175.0(4) . . . . ?
C4 C5 C6 C7 -3.1(6) . . . . ?
C5 C6 C7 O4 -178.3(4) . . . . ?
C5 C6 C7 C2 2.2(6) . . . . ?
C6 N1 N2 C8 -178.6(3) . . . . ?
C7 C2 C3 O1 175.1(4) . . . . ?
C7 C2 C3 C4 -6.2(6) . . . . ?
C8 N3 C9 N5 -0.4(5) . . . . ?
C8 N4 N5 C9 -0.3(4) . . . . ?
C9 N3 C8 N2 179.9(4) . . . . ?
C9 N3 C8 N4 0.2(5) . . . . ?
C10 C11 C12 O8 -0.6(7) . . . . ?
C10 C11 C12 C13 -179.1(5) . . . . ?
C10 C11 C16 O5 0.8(7) . . . . ?
C10 C11 C16 C15 -179.8(4) . . . . ?
C11 C12 C13 C14 -1.4(8) . . . . ?
C12 C11 C16 O5 -178.9(4) . . . . ?
C12 C11 C16 C15 0.5(7) . . . . ?
C12 C13 C14 C15 1.2(9) . . . . ?
C13 C14 C15 C16 -0.1(8) . . . . ?
C14 C15 C16 O5 178.7(5) . . . . ?
C14 C15 C16 C11 -0.8(8) . . . . ?
C16 C11 C12 O8 179.2(5) . . . . ?
C16 C11 C12 C13 0.6(7) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.5327 -6.2844 0.8443 -0.0194 -0.0894 0.9958
-0.5115 -3.2933 7.3843 0.6166 0.6507 0.4432
1.3483 0.4307 6.9320 0.7401 0.6306 -0.2337
-0.4429 0.2200 -7.4136 -0.6872 -0.7235 0.0657
-0.1950 0.1513 7.3930 0.6083 0.7916 -0.0586
5.5288 -0.1026 2.4569 0.8380 -0.2028 -0.5066
0.6499 -7.1757 2.8975 0.4151 -0.0978 0.9045
-3.2393 -2.9258 5.9010 0.1759 0.7378 0.6517
-4.9421 -2.0116 -1.4580 -0.6584 0.1567 0.7361
-4.4778 5.5485 -3.9679 -0.9192 0.2220 -0.3253
2.8994 5.2276 -0.5980 0.2091 -0.0480 -0.9767
1.6538 6.2417 -1.1279 0.0094 0.0479 -0.9988
2.9142 4.6061 -4.5599 -0.1199 -0.4909 -0.8629
-2.3554 2.4898 6.1990 0.2308 0.9572 -0.1745
2.3503 -2.5172 -6.1852 -0.2299 -0.9567 0.1786
0.1808 -5.8182 -2.7390 -0.1378 -0.5797 0.8031
-5.9355 -0.0672 -0.4652 -0.7115 0.4350 0.5519
4.9427 -4.7868 3.9062 0.9567 -0.2298 0.1789
