#------------------------------------------------------------------------------
#$Date: 2024-01-06 09:55:03 +0200 (Sat, 06 Jan 2024) $
#$Revision: 288779 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/74/7247421.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_7247421
loop_
_publ_author_name
'Mao, Pan-Dong'
'Sun, Hui-Ying'
'Yan, Fei-Fei'
'Zhang, Shi-Hui'
'Li, Xin-Feng'
'Zhou, Ren-He'
'Zhang, Yi-Quan'
'Meng, Yin-Shan'
'Liu, Tao'
_publ_section_title
;
 Dinuclear and trinuclear cyano-bridged {DyIIIMIV} (M = W, Mo) single-ion
 magnets supported by pentadentate Schiff-base ligands
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6030
_journal_page_last               6038
_journal_paper_doi               10.1039/D3CE00720K
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C29 H26 Dy N15 O5 W, 11(H2 O), 0.5(O)'
_chemical_formula_sum            'C29 H48 Dy N15 O16.5 W'
_chemical_formula_weight         1217.17
_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
_audit_creation_date             2023-05-11
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-05-11 deposited with the CCDC.	2023-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                93.031(3)
_cell_angle_beta                 95.698(3)
_cell_angle_gamma                108.135(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4246(11)
_cell_length_b                   11.7295(11)
_cell_length_c                   18.7320(19)
_cell_measurement_reflns_used    9263
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.50
_cell_volume                     2157.4(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            75085
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         2.219
_exptl_absorpt_coefficient_mu    4.468
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1042 before and 0.0561 after correction. The Ratio of minimum to maximum transmission is 0.7386. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       prism
_exptl_crystal_F_000             1198
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.914
_refine_diff_density_min         -1.808
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9909
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0230P)²+17.1708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8395
_reflns_number_total             9909
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce00720k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7247418--7247421.cif.'
_cod_original_formula_sum        'C29 H48 Dy N15 O16.50 W'
_cod_database_code               7247421
_shelx_shelxl_version_number     2018/3
_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.
;
_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,H) groups
2. Restrained distances
 H15B-H16E_$1
 2 with sigma of 0.01
 H16E_$1-H15A
 2 with sigma of 0.02
 H15A-H17A
 2 with sigma of 0.01
 H15B-H17A
 2 with sigma of 0.01
 H6A-H7A
 2.1 with sigma of 0.01
 H6A-H7B
 2.1 with sigma of 0.01
 H13A-H16D
 2.1 with sigma of 0.01
 H8A-H15
 2.2 with sigma of 0.02
 O30-N1_$2
 3 with sigma of 0.02
3. Rigid bond restraints
 O17
 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(O30) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O30(0.5)
7.a Everything fixed:
 H16E, H16D, H17A, H17B
7.b Riding coordinates:
 O12(H12A,H12B), O13(H13A,H13B), O15(H15A,H15B)
7.c Free rotating group:
 O6(H6A,H6B), O7(H7A,H7B), O8(H8A,H8B), O9(H9B,H9C), O10(H10B,H10C), O11(H11A,
 H11B)
7.d Rotating group:
 O2(H2A,H2B), O4(H4A,H4B), O5(H5A,H5B)
7.e Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C18(H18), C19(H19), C20(H20), C26(H26),
 C27(H27), C28(H28), C29(H29), N10(H10A), N15(H15)
7.f Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
C1 C 0.8542(6) 0.6737(6) 0.8550(3) 0.0307(13) Uani 1 1 d . . . . .
C2 C 0.7304(5) 0.7926(6) 0.7794(3) 0.0271(12) Uani 1 1 d . . . . .
C3 C 0.8317(5) 0.5411(5) 0.7362(3) 0.0225(11) Uani 1 1 d . . . . .
C4 C 0.6734(5) 0.6418(5) 0.6675(3) 0.0200(10) Uani 1 1 d . . . . .
C5 C 0.4748(5) 0.6130(5) 0.7501(3) 0.0244(12) Uani 1 1 d . . . . .
C6 C 0.5987(6) 0.6449(6) 0.8765(3) 0.0331(14) Uani 1 1 d . . . . .
C7 C 0.6635(6) 0.4500(5) 0.8439(3) 0.0269(12) Uani 1 1 d . . . . .
C8 C 0.5585(5) 0.4340(5) 0.7138(3) 0.0196(10) Uani 1 1 d . . . . .
C9 C 0.1304(8) 0.4377(6) 0.8273(4) 0.0394(16) Uani 1 1 d . . . . .
H9 H 0.080774 0.428659 0.780802 0.047 Uiso 1 1 calc R U . . .
C10 C 0.1096(11) 0.5094(8) 0.8821(4) 0.060(2) Uani 1 1 d . . . . .
H10 H 0.044284 0.549950 0.873623 0.072 Uiso 1 1 calc R U . . .
C11 C 0.2724(9) 0.4711(8) 0.9605(4) 0.055(2) Uani 1 1 d . . . . .
H11 H 0.322360 0.484674 1.007172 0.066 Uiso 1 1 calc R U . . .
C12 C 0.2982(8) 0.3975(8) 0.9085(4) 0.049(2) Uani 1 1 d . . . . .
H12 H 0.365696 0.359819 0.918647 0.059 Uiso 1 1 calc R U . . .
C13 C 0.2245(5) 0.3789(5) 0.8408(3) 0.0234(11) Uani 1 1 d . . . . .
C14 C 0.2471(5) 0.3032(5) 0.7797(3) 0.0204(10) Uani 1 1 d . . . . .
C15 C 0.4050(6) 0.0889(5) 0.7491(3) 0.0268(12) Uani 1 1 d . . . . .
C16 C 0.4761(7) 0.0757(7) 0.8201(3) 0.0373(15) Uani 1 1 d . . . . .
H16A H 0.423791 0.001329 0.839142 0.056 Uiso 1 1 calc R U . . .
H16B H 0.484066 0.144774 0.854046 0.056 Uiso 1 1 calc R U . . .
H16C H 0.567103 0.072355 0.813724 0.056 Uiso 1 1 calc R U . . .
C17 C 0.4165(5) 0.0194(5) 0.6831(3) 0.0228(11) Uani 1 1 d . . . . .
C18 C 0.4808(6) -0.0689(6) 0.6868(3) 0.0307(13) Uani 1 1 d . . . . .
H18 H 0.524328 -0.081492 0.731272 0.037 Uiso 1 1 calc R U . . .
C19 C 0.4796(6) -0.1373(6) 0.6244(4) 0.0340(14) Uani 1 1 d . . . . .
H19 H 0.524689 -0.196357 0.625213 0.041 Uiso 1 1 calc R U . . .
C20 C 0.4128(6) -0.1196(5) 0.5611(3) 0.0269(12) Uani 1 1 d . . . . .
H20 H 0.409319 -0.167218 0.517892 0.032 Uiso 1 1 calc R U . . .
C21 C 0.3497(5) -0.0301(5) 0.5613(3) 0.0209(11) Uani 1 1 d . . . . .
C22 C 0.2681(5) -0.0126(5) 0.4961(3) 0.0208(11) Uani 1 1 d . . . . .
C23 C 0.2528(6) -0.0879(5) 0.4264(3) 0.0284(12) Uani 1 1 d . . . . .
H23A H 0.335711 -0.109377 0.422669 0.043 Uiso 1 1 calc R U . . .
H23B H 0.237663 -0.042060 0.385969 0.043 Uiso 1 1 calc R U . . .
H23C H 0.175074 -0.161500 0.425124 0.043 Uiso 1 1 calc R U . . .
C24 C 0.0935(5) 0.1821(5) 0.4582(3) 0.0172(10) Uani 1 1 d . . . . .
C25 C 0.0062(5) 0.2085(5) 0.3968(3) 0.0191(10) Uani 1 1 d . . . . .
C26 C -0.0716(6) 0.2826(6) 0.4103(4) 0.0300(13) Uani 1 1 d . . . . .
H26 H -0.068476 0.317185 0.457699 0.036 Uiso 1 1 calc R U . . .
C27 C -0.1531(6) 0.3053(6) 0.3541(4) 0.0389(16) Uani 1 1 d . . . . .
H27 H -0.206679 0.355858 0.362728 0.047 Uiso 1 1 calc R U . . .
C28 C -0.0799(6) 0.1893(6) 0.2719(3) 0.0335(14) Uani 1 1 d . . . . .
H28 H -0.082536 0.158962 0.223602 0.040 Uiso 1 1 calc R U . . .
C29 C 0.0039(5) 0.1641(5) 0.3263(3) 0.0264(12) Uani 1 1 d . . . . .
H29 H 0.059681 0.116558 0.315529 0.032 Uiso 1 1 calc R U . . .
Dy1 Dy 0.27323(2) 0.22820(2) 0.61225(2) 0.01492(6) Uani 1 1 d . . . . .
N1 N 0.9486(5) 0.7148(5) 0.8966(3) 0.0423(15) Uani 1 1 d . . . . .
N2 N 0.7609(5) 0.8960(5) 0.7817(3) 0.0345(12) Uani 1 1 d . . . . .
N3 N 0.9097(5) 0.5050(4) 0.7124(3) 0.0281(11) Uani 1 1 d . . . . .
N4 N 0.6653(5) 0.6600(4) 0.6080(3) 0.0254(10) Uani 1 1 d . . . . .
N5 N 0.3689(5) 0.6200(5) 0.7323(3) 0.0324(12) Uani 1 1 d . . . . .
N6 N 0.5603(6) 0.6726(6) 0.9275(3) 0.0457(15) Uani 1 1 d . . . . .
N7 N 0.6586(6) 0.3712(5) 0.8786(3) 0.0386(13) Uani 1 1 d . . . . .
N8 N 0.4948(4) 0.3498(4) 0.6773(2) 0.0225(9) Uani 1 1 d . . . . .
N9 N 0.1790(8) 0.5230(6) 0.9463(3) 0.0512(18) Uani 1 1 d . . . . .
N10 N 0.3076(5) 0.2211(5) 0.7971(3) 0.0254(10) Uani 1 1 d . . . . .
H10A H 0.331619 0.209743 0.841894 0.030 Uiso 1 1 calc R U . . .
N11 N 0.3286(4) 0.1559(4) 0.7382(3) 0.0227(9) Uani 1 1 d . . . . .
N12 N 0.3564(4) 0.0415(4) 0.6211(3) 0.0203(9) Uani 1 1 d . . . . .
N13 N 0.2091(4) 0.0685(4) 0.5054(2) 0.0193(9) Uani 1 1 d . . . . .
N14 N 0.1261(4) 0.0830(4) 0.4458(2) 0.0194(9) Uani 1 1 d . . . . .
N15 N -0.1572(5) 0.2568(5) 0.2878(3) 0.0351(13) Uani 1 1 d . . . . .
H15 H -0.212989 0.269589 0.253027 0.042 Uiso 1 1 calc DR U . . .
O1 O 0.2156(3) 0.3206(3) 0.71716(19) 0.0197(7) Uani 1 1 d . . . . .
O2 O 0.2767(4) 0.4371(3) 0.6031(2) 0.0230(8) Uani 1 1 d . . . . .
H2A H 0.316064 0.466624 0.564778 0.034 Uiso 1 1 d R U . . .
H2B H 0.323153 0.483513 0.642408 0.034 Uiso 1 1 d R U . . .
O3 O 0.1278(4) 0.2541(3) 0.5146(2) 0.0216(8) Uani 1 1 d . . . . .
O4 O 0.4308(4) 0.2880(3) 0.5260(2) 0.0219(8) Uani 1 1 d . . . . .
H4A H 0.501769 0.352857 0.543730 0.033 Uiso 1 1 d R U . . .
H4B H 0.390417 0.306795 0.485660 0.033 Uiso 1 1 d R U . . .
O5 O 0.0637(4) 0.1069(3) 0.6371(2) 0.0247(8) Uani 1 1 d . . . . .
H5A H 0.066224 0.069928 0.680859 0.037 Uiso 1 1 d R U . . .
H5B H 0.026233 0.038758 0.603868 0.037 Uiso 1 1 d R U . . .
W1 W 0.67402(2) 0.59861(2) 0.77839(2) 0.01903(6) Uani 1 1 d . . . . .
O6 O -0.0540(5) 0.1217(4) 0.7563(3) 0.0426(12) Uani 1 1 d G . . . .
H6A H -0.107418 0.165691 0.755781 0.064 Uiso 1 1 d DG U . . .
H6B H -0.098697 0.055902 0.773891 0.064 Uiso 1 1 d G U . . .
O7 O -0.2092(17) 0.2374(10) 0.7556(6) 0.207(8) Uani 1 1 d G . . . .
H7A H -0.215661 0.273310 0.796319 0.310 Uiso 1 1 d DG U . . .
H7B H -0.210507 0.284552 0.721430 0.310 Uiso 1 1 d DG U . . .
O8 O -0.3135(9) 0.2235(7) 0.1511(5) 0.098(3) Uani 1 1 d G . . A -1
H8A H -0.235283 0.232272 0.135649 0.148 Uiso 1 1 d DG U . A -1
H8B H -0.355212 0.257057 0.120327 0.148 Uiso 1 1 d G U . A -1
O9 O 0.2945(4) 0.5512(4) 0.4732(2) 0.0275(9) Uani 1 1 d G . . . .
H9B H 0.220221 0.567223 0.459671 0.041 Uiso 1 1 d G U . . .
H9C H 0.290169 0.488410 0.445014 0.041 Uiso 1 1 d G U . . .
O10 O 0.9475(4) 0.3963(4) 0.5810(3) 0.0370(10) Uani 1 1 d G . . . .
H10B H 0.951428 0.428434 0.624568 0.056 Uiso 1 1 d G U . . .
H10C H 1.026863 0.391316 0.574088 0.056 Uiso 1 1 d G U . . .
O11 O 0.0983(7) 0.6648(7) 1.0372(4) 0.083(2) Uani 1 1 d G . . . .
H11A H 0.172246 0.726063 1.039841 0.124 Uiso 1 1 d G U . . .
H11B H 0.048397 0.672962 0.998989 0.124 Uiso 1 1 d G U . . .
O12 O 0.4099(9) 0.7822(8) 1.0006(5) 0.107(3) Uani 1 1 d . . . . .
H12A H 0.372224 0.745713 1.036134 0.160 Uiso 1 1 d R U . . .
H12B H 0.461924 0.744223 0.983874 0.160 Uiso 1 1 d R U . . .
O13 O 0.3712(8) 0.9720(11) 0.9847(5) 0.138(4) Uani 1 1 d . U . B -1
H13A H 0.398992 1.043346 0.969495 0.207 Uiso 1 1 d DR U . B -1
H13B H 0.400632 0.983326 1.030485 0.207 Uiso 1 1 d R U . B -1
O15 O -0.0283(5) 0.8502(9) 1.0310(5) 0.186(6) Uani 1 1 d . . . . .
H15A H -0.041159 0.918379 1.022353 0.278 Uiso 1 1 d DR U . . .
H15B H -0.038399 0.837229 1.075713 0.278 Uiso 1 1 d DR U . . .
O16 O 0.2698(14) 1.1265(14) 0.9287(7) 0.219(8) Uani 1 1 d . . . . .
H16E H 0.213880 1.142360 0.956260 0.329 Uiso 1 1 d . U . . .
H16D H 0.230030 1.055530 0.908910 0.329 Uiso 1 1 d D U . . .
O17 O 0.2149(15) 0.9468(17) 1.0856(7) 0.221(7) Uani 1 1 d . U . . .
H17A H 0.136050 0.954970 1.082200 0.331 Uiso 1 1 d D U . . .
H17B H 0.270570 1.024860 1.095140 0.331 Uiso 1 1 d . U . . .
O30 O 0.2289(18) 0.873(2) 0.9278(15) 0.166(9) Uani 0.5 1 d D U P C -1
H9A H 0.171(9) 0.574(8) 0.974(5) 0.06(3) Uiso 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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1 C1 W1 178.6(6) . . ?
N2 C2 W1 178.4(5) . . ?
N3 C3 W1 176.3(5) . . ?
N4 C4 W1 175.9(5) . . ?
N5 C5 W1 177.5(5) . . ?
N6 C6 W1 178.0(6) . . ?
N7 C7 W1 179.7(6) . . ?
N8 C8 W1 176.8(5) . . ?
C10 C9 H9 120.7 . . ?
C10 C9 C13 118.7(7) . . ?
C13 C9 H9 120.7 . . ?
C9 C10 H10 119.6 . . ?
N9 C10 C9 120.9(7) . . ?
N9 C10 H10 119.6 . . ?
C12 C11 H11 119.8 . . ?
N9 C11 H11 119.8 . . ?
N9 C11 C12 120.3(7) . . ?
C11 C12 H12 120.5 . . ?
C11 C12 C13 119.0(7) . . ?
C13 C12 H12 120.5 . . ?
C9 C13 C12 119.0(6) . . ?
C9 C13 C14 117.5(5) . . ?
C12 C13 C14 123.4(6) . . ?
N10 C14 C13 116.6(5) . . ?
O1 C14 C13 120.2(5) . . ?
O1 C14 N10 123.2(5) . . ?
C17 C15 C16 120.2(5) . . ?
N11 C15 C16 126.1(6) . . ?
N11 C15 C17 113.7(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C15 121.0(5) . . ?
N12 C17 C15 116.4(5) . . ?
N12 C17 C18 122.5(5) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 C17 118.6(6) . . ?
C19 C18 H18 120.7 . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.5(5) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 120.5 . . ?
C19 C20 C21 119.0(6) . . ?
C21 C20 H20 120.5 . . ?
C20 C21 C22 121.4(5) . . ?
N12 C21 C20 121.9(5) . . ?
N12 C21 C22 116.6(5) . . ?
C21 C22 C23 121.2(5) . . ?
N13 C22 C21 114.6(5) . . ?
N13 C22 C23 124.1(5) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N14 C24 C25 114.2(4) . . ?
O3 C24 C25 118.4(4) . . ?
O3 C24 N14 127.4(5) . . ?
C26 C25 C24 119.3(5) . . ?
C29 C25 C24 121.9(5) . . ?
C29 C25 C26 118.8(5) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 C25 119.2(6) . . ?
C27 C26 H26 120.4 . . ?
C26 C27 H27 119.9 . . ?
N15 C27 C26 120.2(6) . . ?
N15 C27 H27 119.9 . . ?
C29 C28 H28 120.2 . . ?
N15 C28 H28 120.2 . . ?
N15 C28 C29 119.5(6) . . ?
C25 C29 H29 120.2 . . ?
C28 C29 C25 119.6(6) . . ?
C28 C29 H29 120.2 . . ?
N8 Dy1 N11 66.03(15) . . ?
N8 Dy1 N12 87.71(15) . . ?
N8 Dy1 N13 131.93(14) . . ?
N12 Dy1 N11 59.68(14) . . ?
N13 Dy1 N11 116.11(14) . . ?
N13 Dy1 N12 61.12(14) . . ?
O1 Dy1 N8 75.90(14) . . ?
O1 Dy1 N11 61.69(13) . . ?
O1 Dy1 N12 120.82(13) . . ?
O1 Dy1 N13 150.67(13) . . ?
O1 Dy1 O2 65.20(13) . . ?
O2 Dy1 N8 75.82(14) . . ?
O2 Dy1 N11 119.90(14) . . ?
O2 Dy1 N12 160.73(13) . . ?
O2 Dy1 N13 123.95(13) . . ?
O3 Dy1 N8 135.39(14) . . ?
O3 Dy1 N11 154.55(13) . . ?
O3 Dy1 N12 124.10(14) . . ?
O3 Dy1 N13 63.13(13) . . ?
O3 Dy1 O1 105.62(12) . . ?
O3 Dy1 O2 65.68(12) . . ?
O3 Dy1 O4 79.73(13) . . ?
O4 Dy1 N8 71.81(14) . . ?
O4 Dy1 N11 125.05(13) . . ?
O4 Dy1 N12 85.69(13) . . ?
O4 Dy1 N13 70.32(13) . . ?
O4 Dy1 O1 137.00(13) . . ?
O4 Dy1 O2 79.76(13) . . ?
O5 Dy1 N8 139.05(14) . . ?
O5 Dy1 N11 76.60(14) . . ?
O5 Dy1 N12 87.54(14) . . ?
O5 Dy1 N13 79.09(13) . . ?
O5 Dy1 O1 71.94(12) . . ?
O5 Dy1 O2 111.44(13) . . ?
O5 Dy1 O3 78.43(14) . . ?
O5 Dy1 O4 148.06(13) . . ?
C8 N8 Dy1 149.0(4) . . ?
C10 N9 H9A 116(7) . . ?
C11 N9 C10 122.1(7) . . ?
C11 N9 H9A 121(7) . . ?
C14 N10 H10A 123.1 . . ?
C14 N10 N11 113.8(4) . . ?
N11 N10 H10A 123.1 . . ?
C15 N11 Dy1 123.5(4) . . ?
C15 N11 N10 118.0(5) . . ?
N10 N11 Dy1 115.8(3) . . ?
C17 N12 C21 118.3(5) . . ?
C17 N12 Dy1 121.6(4) . . ?
C21 N12 Dy1 119.9(4) . . ?
C22 N13 Dy1 124.4(4) . . ?
C22 N13 N14 115.9(4) . . ?
N14 N13 Dy1 118.3(3) . . ?
C24 N14 N13 109.4(4) . . ?
C27 N15 C28 122.5(5) . . ?
C27 N15 H15 118.7 . . ?
C28 N15 H15 118.7 . . ?
C14 O1 Dy1 124.8(3) . . ?
Dy1 O2 H2A 110.7 . . ?
Dy1 O2 H2B 110.4 . . ?
H2A O2 H2B 108.3 . . ?
C24 O3 Dy1 121.7(3) . . ?
Dy1 O4 H4A 111.2 . . ?
Dy1 O4 H4B 110.8 . . ?
H4A O4 H4B 108.0 . . ?
Dy1 O5 H5A 114.4 . . ?
Dy1 O5 H5B 112.8 . . ?
H5A O5 H5B 100.7 . . ?
C1 W1 C2 72.8(2) . . ?
C1 W1 C3 73.8(2) . . ?
C1 W1 C4 120.8(2) . . ?
C1 W1 C6 75.4(2) . . ?
C1 W1 C7 78.5(2) . . ?
C2 W1 C4 72.7(2) . . ?
C2 W1 C6 78.5(2) . . ?
C2 W1 C7 144.8(2) . . ?
C3 W1 C2 108.5(2) . . ?
C3 W1 C4 73.7(2) . . ?
C3 W1 C6 144.4(2) . . ?
C3 W1 C7 81.9(2) . . ?
C4 W1 C6 139.2(2) . . ?
C4 W1 C7 141.4(2) . . ?
C5 W1 C1 141.5(2) . . ?
C5 W1 C2 81.5(2) . . ?
C5 W1 C3 143.0(2) . . ?
C5 W1 C4 75.9(2) . . ?
C5 W1 C6 71.6(2) . . ?
C5 W1 C7 110.8(2) . . ?
C5 W1 C8 74.0(2) . . ?
C7 W1 C6 74.8(2) . . ?
C8 W1 C1 141.3(2) . . ?
C8 W1 C2 142.3(2) . . ?
C8 W1 C3 77.70(19) . . ?
C8 W1 C4 73.8(2) . . ?
C8 W1 C6 118.6(2) . . ?
C8 W1 C7 72.0(2) . . ?
H6A O6 H6B 104.8 . . ?
H7A O7 H7B 109.5 . . ?
H8A O8 H8B 104.5 . . ?
H9B O9 H9C 104.7 . . ?
H10B O10 H10C 109.4 . . ?
H11A O11 H11B 104.5 . . ?
H12A O12 H12B 109.5 . . ?
H13A O13 H13B 104.4 . . ?
H15A O15 H15B 109.4 . . ?
H16E O16 H16D 106.1 . . ?
H17A O17 H17B 102.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.149(8) . ?
C1 W1 2.160(6) . ?
C2 N2 1.152(8) . ?
C2 W1 2.164(6) . ?
C3 N3 1.143(7) . ?
C3 W1 2.162(5) . ?
C4 N4 1.144(7) . ?
C4 W1 2.165(5) . ?
C5 N5 1.151(7) . ?
C5 W1 2.152(5) . ?
C6 N6 1.142(8) . ?
C6 W1 2.176(6) . ?
C7 N7 1.150(8) . ?
C7 W1 2.165(6) . ?
C8 N8 1.147(7) . ?
C8 W1 2.158(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.370(9) . ?
C9 C13 1.376(8) . ?
C10 H10 0.9500 . ?
C10 N9 1.316(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.370(10) . ?
C11 N9 1.313(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(9) . ?
C13 C14 1.493(7) . ?
C14 N10 1.342(7) . ?
C14 O1 1.231(6) . ?
C15 C16 1.498(8) . ?
C15 C17 1.479(8) . ?
C15 N11 1.291(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.399(8) . ?
C17 N12 1.341(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.378(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.374(9) . ?
C20 H20 0.9500 . ?
C20 C21 1.401(7) . ?
C21 C22 1.478(8) . ?
C21 N12 1.347(7) . ?
C22 C23 1.504(8) . ?
C22 N13 1.297(7) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.501(7) . ?
C24 N14 1.324(6) . ?
C24 O3 1.265(6) . ?
C25 C26 1.391(8) . ?
C25 C29 1.389(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(9) . ?
C27 H27 0.9500 . ?
C27 N15 1.330(9) . ?
C28 H28 0.9500 . ?
C28 C29 1.379(8) . ?
C28 N15 1.336(9) . ?
C29 H29 0.9500 . ?
Dy1 N8 2.462(4) . ?
Dy1 N11 2.619(5) . ?
Dy1 N12 2.602(4) . ?
Dy1 N13 2.553(4) . ?
Dy1 O1 2.411(4) . ?
Dy1 O2 2.454(4) . ?
Dy1 O3 2.353(4) . ?
Dy1 O4 2.394(4) . ?
Dy1 O5 2.313(4) . ?
N9 H9A 0.80(9) . ?
N10 H10A 0.8800 . ?
N10 N11 1.385(6) . ?
N13 N14 1.393(6) . ?
N15 H15 0.8800 . ?
O2 H2A 0.8946 . ?
O2 H2B 0.8923 . ?
O4 H4A 0.8999 . ?
O4 H4B 0.8994 . ?
O5 H5A 0.9498 . ?
O5 H5B 0.9396 . ?
O6 H6A 0.8686 . ?
O6 H6B 0.8689 . ?
O7 H7A 0.8702 . ?
O7 H7B 0.8697 . ?
O8 H8A 0.8702 . ?
O8 H8B 0.8701 . ?
O9 H9B 0.8699 . ?
O9 H9C 0.8689 . ?
O10 H10B 0.8716 . ?
O10 H10C 0.8691 . ?
O11 H11A 0.8701 . ?
O11 H11B 0.8701 . ?
O12 H12A 0.8703 . ?
O12 H12B 0.8717 . ?
O13 H13A 0.8697 . ?
O13 H13B 0.8698 . ?
O15 H15A 0.8717 . ?
O15 H15B 0.8690 . ?
O16 H16E 0.8706 . ?
O16 H16D 0.8510 . ?
O17 H17A 0.8539 . ?
O17 H17B 0.9160 . ?
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
C9 C10 N9 C11 1.4(14) . . . . ?
C9 C13 C14 N10 -161.7(6) . . . . ?
C9 C13 C14 O1 21.1(8) . . . . ?
C10 C9 C13 C12 -2.2(11) . . . . ?
C10 C9 C13 C14 -178.8(7) . . . . ?
C11 C12 C13 C9 1.9(11) . . . . ?
C11 C12 C13 C14 178.3(7) . . . . ?
C12 C11 N9 C10 -1.8(14) . . . . ?
C12 C13 C14 N10 21.9(8) . . . . ?
C12 C13 C14 O1 -155.3(6) . . . . ?
C13 C9 C10 N9 0.6(13) . . . . ?
C13 C14 N10 N11 -178.5(4) . . . . ?
C13 C14 O1 Dy1 170.7(3) . . . . ?
C14 N10 N11 C15 169.2(5) . . . . ?
C14 N10 N11 Dy1 7.2(6) . . . . ?
C15 C17 C18 C19 175.1(5) . . . . ?
C15 C17 N12 C21 -171.9(5) . . . . ?
C15 C17 N12 Dy1 13.7(6) . . . . ?
C16 C15 C17 C18 7.1(8) . . . . ?
C16 C15 C17 N12 -176.3(5) . . . . ?
C16 C15 N11 Dy1 159.5(5) . . . . ?
C16 C15 N11 N10 -1.0(9) . . . . ?
C17 C15 N11 Dy1 -21.8(7) . . . . ?
C17 C15 N11 N10 177.7(4) . . . . ?
C17 C18 C19 C20 -1.8(9) . . . . ?
C18 C17 N12 C21 4.7(7) . . . . ?
C18 C17 N12 Dy1 -169.8(4) . . . . ?
C18 C19 C20 C21 1.4(9) . . . . ?
C19 C20 C21 C22 -175.6(5) . . . . ?
C19 C20 C21 N12 2.1(8) . . . . ?
C20 C21 C22 C23 -1.8(8) . . . . ?
C20 C21 C22 N13 176.0(5) . . . . ?
C20 C21 N12 C17 -5.1(7) . . . . ?
C20 C21 N12 Dy1 169.5(4) . . . . ?
C21 C22 N13 Dy1 16.6(6) . . . . ?
C21 C22 N13 N14 -177.0(4) . . . . ?
C22 C21 N12 C17 172.7(4) . . . . ?
C22 C21 N12 Dy1 -12.7(6) . . . . ?
C22 N13 N14 C24 -168.3(4) . . . . ?
C23 C22 N13 Dy1 -165.7(4) . . . . ?
C23 C22 N13 N14 0.7(7) . . . . ?
C24 C25 C26 C27 -179.0(5) . . . . ?
C24 C25 C29 C28 178.9(5) . . . . ?
C25 C24 N14 N13 178.7(4) . . . . ?
C25 C24 O3 Dy1 -176.9(3) . . . . ?
C25 C26 C27 N15 0.0(9) . . . . ?
C26 C25 C29 C28 -3.1(8) . . . . ?
C26 C27 N15 C28 -2.9(10) . . . . ?
C29 C25 C26 C27 2.9(8) . . . . ?
C29 C28 N15 C27 2.7(9) . . . . ?
Dy1 N13 N14 C24 -1.1(5) . . . . ?
N9 C11 C12 C13 0.1(13) . . . . ?
N10 C14 O1 Dy1 -6.3(7) . . . . ?
N11 C15 C17 C18 -171.7(5) . . . . ?
N11 C15 C17 N12 4.9(7) . . . . ?
N12 C17 C18 C19 -1.4(8) . . . . ?
N12 C21 C22 C23 -179.6(5) . . . . ?
N12 C21 C22 N13 -1.8(7) . . . . ?
N14 C24 C25 C26 158.4(5) . . . . ?
N14 C24 C25 C29 -23.7(7) . . . . ?
N14 C24 O3 Dy1 3.0(7) . . . . ?
N15 C28 C29 C25 0.4(8) . . . . ?
O1 C14 N10 N11 -1.4(7) . . . . ?
O3 C24 C25 C26 -21.8(7) . . . . ?
O3 C24 C25 C29 156.2(5) . . . . ?
O3 C24 N14 N13 -1.1(7) . . . . ?
