#------------------------------------------------------------------------------
#$Date: 2022-03-12 01:53:35 +0200 (Sat, 12 Mar 2022) $
#$Revision: 273670 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/97/7709741.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_7709741
loop_
_publ_author_name
'Jin, Da'
'Sun, Xiaofei'
'Hinz, Alexander'
'Roesky, Peter W.'
_publ_section_title
;
 Rare-earth metal complexes with redox-active formazanate ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00456A
_journal_year                    2022
_chemical_formula_moiety         'C33 H33 Dy N4'
_chemical_formula_sum            'C33 H33 Dy N4'
_chemical_formula_weight         648.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-16 deposited with the CCDC.	2022-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.62(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.179(2)
_cell_length_b                   11.509(2)
_cell_length_c                   12.716(3)
_cell_measurement_reflns_used    42320
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      1.67
_cell_volume                     1411.7(6)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
 394 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23042
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.848
_diffrn_reflns_theta_min         1.690
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.675
_exptl_absorpt_correction_T_max  0.5329
_exptl_absorpt_correction_T_min  0.2423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.194
_refine_diff_density_max         2.531
_refine_diff_density_min         -3.059
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details
;
 Flack x determined using 2983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7733
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0546
_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)+(0.1046P)²+1.7769P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1421
_reflns_d_resolution_high        0.721
_reflns_d_resolution_low         12.192
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.923
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              17
_reflns_limit_l_min              -17
_reflns_number_gt                7090
_reflns_number_total             7733
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00456a4.cif
_cod_data_source_block           jd064
_cod_original_cell_volume        1411.6(5)
_cod_database_code               7709741
_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.
;
_shelx_estimated_absorpt_t_max   0.625
_shelx_estimated_absorpt_t_min   0.339
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5-C8A \\sim C5-C8B
 with sigma of 0.02
 C9A-C10A \\sim C10B-C11B
 with sigma of 0.04
 C9A-C11A \\sim C10B-C9B
 with sigma of 0.04
 C10A-C11A \\sim C11B-C9B
 with sigma of 0.04
 C5-C9A \\sim C5-C10B
 with sigma of 0.04
 C5-C10A \\sim C5-C11B
 with sigma of 0.04
 C5-C11A \\sim C5-C9B
 with sigma of 0.04
 C8A-C9A \\sim C8B-C10B
 with sigma of 0.04
 C8A-C10A \\sim C8B-C11B
 with sigma of 0.04
 C8A-C11A \\sim C8B-C9B
 with sigma of 0.04
3. Rigid bond restraints
 C8A, C8B, C9A, C9B, C10A, C10B, C11A, C11B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C8A \\sim C8B \\sim C9A \\sim C9B \\sim C10A \\sim C10B \\sim C11A \\sim C11B:
within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
5. Others
 Sof(C8B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(C8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
6.b Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C10A(H10A,H10B,H10C), C10B(H10D,
 H10E,H10F), C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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
Dy Dy -0.06831(3) -0.98917(6) -0.32576(2) 0.02628(12) Uani 1 1 d . . . . .
N1 N -0.0987(9) -1.1376(7) -0.2064(7) 0.0268(15) Uani 1 1 d . . . . .
N2 N -0.1889(8) -1.1496(6) -0.1557(6) 0.0265(14) Uani 1 1 d . . . . .
N3 N -0.3630(8) -1.0119(5) -0.2607(6) 0.0245(17) Uani 1 1 d . . . . .
N4 N -0.3029(7) -0.9781(9) -0.3324(5) 0.0241(14) Uani 1 1 d . . . . .
C1 C -0.3016(9) -1.0814(7) -0.1757(7) 0.0240(15) Uani 1 1 d . . . . .
C2 C -0.3778(9) -1.0960(7) -0.0950(7) 0.0242(15) Uani 1 1 d . . . . .
C3 C -0.3416(10) -1.1812(8) -0.0127(8) 0.0294(17) Uani 1 1 d . . . . .
H3 H -0.270992 -1.235736 -0.011376 0.035 Uiso 1 1 calc R U . . .
C4 C -0.4067(11) -1.1873(8) 0.0665(8) 0.0312(18) Uani 1 1 d . . . . .
H4 H -0.382205 -1.248311 0.119478 0.037 Uiso 1 1 calc R U . . .
C5 C -0.5066(9) -1.1083(7) 0.0724(7) 0.0250(15) Uani 1 1 d D . . . .
C6 C -0.5437(12) -1.0245(9) -0.0096(8) 0.036(2) Uani 1 1 d . . . . .
H6 H -0.613438 -0.969637 -0.009725 0.043 Uiso 1 1 calc R U . . .
C7 C -0.4810(11) -1.0187(8) -0.0922(9) 0.034(2) Uani 1 1 d . . . . .
H7 H -0.509603 -0.960451 -0.147774 0.040 Uiso 1 1 calc R U . . .
C8A C -0.564(4) -1.111(4) 0.168(3) 0.036(4) Uani 0.49(3) 1 d D U P A 1
C8B C -0.564(4) -1.102(3) 0.168(2) 0.035(4) Uani 0.51(3) 1 d D U P A 2
C9A C -0.689(3) -1.036(3) 0.149(3) 0.049(5) Uani 0.49(3) 1 d D U P A 1
H9AA H -0.672026 -0.980099 0.210579 0.074 Uiso 0.49(3) 1 calc R U P A 1
H9AB H -0.769031 -1.084060 0.146152 0.074 Uiso 0.49(3) 1 calc R U P A 1
H9AC H -0.706424 -0.993533 0.079269 0.074 Uiso 0.49(3) 1 calc R U P A 1
C9B C -0.715(2) -1.080(3) 0.132(2) 0.044(4) Uani 0.51(3) 1 d D U P A 2
H9BA H -0.735235 -1.005331 0.093487 0.066 Uiso 0.51(3) 1 calc R U P A 2
H9BB H -0.746805 -1.078268 0.197319 0.066 Uiso 0.51(3) 1 calc R U P A 2
H9BC H -0.764016 -1.142194 0.081920 0.066 Uiso 0.51(3) 1 calc R U P A 2
C10A C -0.452(3) -1.066(3) 0.273(2) 0.055(5) Uani 0.49(3) 1 d D U P A 1
H10A H -0.367895 -1.113289 0.287603 0.083 Uiso 0.49(3) 1 calc R U P A 1
H10B H -0.486033 -1.070060 0.336633 0.083 Uiso 0.49(3) 1 calc R U P A 1
H10C H -0.429465 -0.984676 0.261508 0.083 Uiso 0.49(3) 1 calc R U P A 1
C10B C -0.482(3) -1.008(3) 0.245(2) 0.052(5) Uani 0.51(3) 1 d D U P A 2
H10D H -0.394602 -0.993871 0.229642 0.078 Uiso 0.51(3) 1 calc R U P A 2
H10E H -0.461467 -1.032508 0.322292 0.078 Uiso 0.51(3) 1 calc R U P A 2
H10F H -0.536193 -0.935815 0.232715 0.078 Uiso 0.51(3) 1 calc R U P A 2
C11A C -0.587(3) -1.234(2) 0.199(3) 0.047(4) Uani 0.49(3) 1 d D U P A 1
H11A H -0.683765 -1.256623 0.162082 0.070 Uiso 0.49(3) 1 calc R U P A 1
H11B H -0.567081 -1.239183 0.279974 0.070 Uiso 0.49(3) 1 calc R U P A 1
H11C H -0.525455 -1.286852 0.176683 0.070 Uiso 0.49(3) 1 calc R U P A 1
C11B C -0.528(3) -1.209(2) 0.244(2) 0.047(4) Uani 0.51(3) 1 d D U P A 2
H11D H -0.587592 -1.273761 0.208706 0.070 Uiso 0.51(3) 1 calc R U P A 2
H11E H -0.541835 -1.190178 0.314803 0.070 Uiso 0.51(3) 1 calc R U P A 2
H11F H -0.430587 -1.229735 0.257010 0.070 Uiso 0.51(3) 1 calc R U P A 2
C12 C -0.0010(10) -1.2330(8) -0.1803(8) 0.0286(17) Uani 1 1 d . . . . .
C13 C -0.0438(12) -1.3476(9) -0.1724(10) 0.039(2) Uani 1 1 d . . . . .
H13 H -0.138477 -1.363007 -0.181381 0.047 Uiso 1 1 calc R U . . .
C14 C 0.0483(13) -1.4372(11) -0.1522(12) 0.049(3) Uani 1 1 d . . . . .
H14 H 0.017579 -1.514469 -0.147815 0.059 Uiso 1 1 calc R U . . .
C15 C 0.1882(13) -1.4156(11) -0.1378(10) 0.046(3) Uani 1 1 d . . . . .
H15 H 0.252576 -1.478045 -0.123682 0.055 Uiso 1 1 calc R U . . .
C16 C 0.2335(11) -1.2999(11) -0.1445(10) 0.042(2) Uani 1 1 d . . . . .
H16 H 0.328500 -1.284256 -0.133754 0.050 Uiso 1 1 calc R U . . .
C17 C 0.1376(12) -1.2095(10) -0.1668(10) 0.040(2) Uani 1 1 d . . . . .
H17 H 0.166697 -1.132040 -0.172816 0.048 Uiso 1 1 calc R U . . .
C18 C -0.3986(9) -0.9200(7) -0.4228(7) 0.0260(16) Uani 1 1 d . . . . .
C19 C -0.5405(11) -0.9382(10) -0.4547(9) 0.038(2) Uani 1 1 d . . . . .
H19 H -0.578223 -0.993319 -0.416682 0.045 Uiso 1 1 calc R U . . .
C20 C -0.6263(13) -0.8754(13) -0.5420(11) 0.052(3) Uani 1 1 d . . . . .
H20 H -0.723391 -0.889034 -0.565269 0.063 Uiso 1 1 calc R U . . .
C21 C -0.5734(14) -0.7932(13) -0.5961(11) 0.055(3) Uani 1 1 d . . . . .
H21 H -0.634139 -0.748975 -0.654653 0.066 Uiso 1 1 calc R U . . .
C22 C -0.4347(12) -0.7754(10) -0.5659(9) 0.040(2) Uani 1 1 d . . . . .
H22 H -0.398432 -0.719851 -0.604592 0.048 Uiso 1 1 calc R U . . .
C23 C -0.3459(10) -0.8374(9) -0.4795(8) 0.0312(18) Uani 1 1 d . . . . .
H23 H -0.248863 -0.824070 -0.458410 0.037 Uiso 1 1 calc R U . . .
C24 C 0.041(2) -1.0087(19) -0.4877(14) 0.076(6) Uani 1 1 d . . . . .
H24 H 0.105545 -0.951056 -0.493214 0.091 Uiso 1 1 calc R U . . .
C25 C 0.0736(17) -1.1104(18) -0.4271(13) 0.067(4) Uani 1 1 d . . . . .
H25 H 0.163933 -1.132715 -0.382045 0.081 Uiso 1 1 calc R U . . .
C26 C -0.044(2) -1.1740(13) -0.4419(11) 0.065(5) Uani 1 1 d . . . . .
H26 H -0.050964 -1.248932 -0.412616 0.078 Uiso 1 1 calc R U . . .
C27 C -0.1549(19) -1.1057(15) -0.5095(11) 0.060(4) Uani 1 1 d . . . . .
H27 H -0.250523 -1.125303 -0.531342 0.072 Uiso 1 1 calc R U . . .
C28 C -0.0993(17) -1.0053(18) -0.5384(10) 0.060(5) Uani 1 1 d . . . . .
H28 H -0.149673 -0.944942 -0.585070 0.072 Uiso 1 1 calc R U . . .
C29 C 0.0852(14) -0.9032(11) -0.1355(10) 0.050(3) Uani 1 1 d . . . . .
H29 H 0.114392 -0.954753 -0.074011 0.060 Uiso 1 1 calc R U . . .
C30 C 0.1523(14) -0.8838(13) -0.2114(13) 0.058(4) Uani 1 1 d . . . . .
H30 H 0.234890 -0.920506 -0.213859 0.070 Uiso 1 1 calc R U . . .
C31 C 0.072(2) -0.7959(16) -0.2876(12) 0.087(7) Uani 1 1 d . . . . .
H31 H 0.093264 -0.762014 -0.348604 0.104 Uiso 1 1 calc R U . . .
C32 C -0.0411(19) -0.7718(12) -0.2521(17) 0.077(6) Uani 1 1 d . . . . .
H32 H -0.113110 -0.718389 -0.286480 0.093 Uiso 1 1 calc R U . . .
C33 C -0.033(2) -0.8345(13) -0.1637(15) 0.065(4) Uani 1 1 d . . . . .
H33 H -0.098846 -0.832991 -0.124876 0.078 Uiso 1 1 calc R U . . .
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 -1 0.2400
-5 -1 6 0.2770
3 -7 -2 0.2620
-1 5 0 0.2380
4 -3 6 0.0840
-4 1 -6 0.1100
-3 -6 4 0.2400
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 Dy C24 127.7(5) . . ?
N1 Dy C25 97.8(5) . . ?
N1 Dy C26 80.3(4) . . ?
N1 Dy C27 97.4(4) . . ?
N1 Dy C28 127.7(5) . . ?
N1 Dy C29 80.9(4) . . ?
N1 Dy C30 104.4(4) . . ?
N1 Dy C31 132.3(4) . . ?
N1 Dy C32 118.3(5) . . ?
N1 Dy C33 89.9(5) . . ?
N4 Dy N1 74.0(3) . . ?
N4 Dy C24 130.4(5) . . ?
N4 Dy C25 136.0(5) . . ?
N4 Dy C26 107.2(5) . . ?
N4 Dy C27 87.0(4) . . ?
N4 Dy C28 100.3(4) . . ?
N4 Dy C29 108.1(4) . . ?
N4 Dy C30 133.4(5) . . ?
N4 Dy C31 116.7(7) . . ?
N4 Dy C32 87.3(5) . . ?
N4 Dy C33 82.9(5) . . ?
C24 Dy C32 109.4(7) . . ?
C24 Dy C33 132.4(7) . . ?
C25 Dy C24 30.4(6) . . ?
C25 Dy C26 30.1(6) . . ?
C25 Dy C28 50.3(5) . . ?
C25 Dy C32 131.5(7) . . ?
C25 Dy C33 141.0(6) . . ?
C26 Dy C24 50.2(6) . . ?
C26 Dy C32 159.6(7) . . ?
C26 Dy C33 163.2(5) . . ?
C27 Dy C24 50.3(6) . . ?
C27 Dy C25 50.5(5) . . ?
C27 Dy C26 31.3(5) . . ?
C27 Dy C28 30.8(6) . . ?
C27 Dy C29 163.5(5) . . ?
C27 Dy C31 128.2(5) . . ?
C27 Dy C32 140.6(6) . . ?
C27 Dy C33 165.4(6) . . ?
C28 Dy C24 30.1(5) . . ?
C28 Dy C26 51.0(5) . . ?
C28 Dy C32 113.2(6) . . ?
C28 Dy C33 141.9(6) . . ?
C29 Dy C24 118.4(6) . . ?
C29 Dy C25 113.3(5) . . ?
C29 Dy C26 133.3(5) . . ?
C29 Dy C28 144.9(5) . . ?
C29 Dy C32 49.7(5) . . ?
C29 Dy C33 30.5(5) . . ?
C30 Dy C24 88.3(6) . . ?
C30 Dy C25 90.6(6) . . ?
C30 Dy C26 118.6(6) . . ?
C30 Dy C27 137.9(6) . . ?
C30 Dy C28 114.4(6) . . ?
C30 Dy C29 30.6(5) . . ?
C30 Dy C31 32.7(6) . . ?
C30 Dy C32 51.6(5) . . ?
C30 Dy C33 50.6(6) . . ?
C31 Dy C24 82.8(7) . . ?
C31 Dy C25 100.9(8) . . ?
C31 Dy C26 130.3(7) . . ?
C31 Dy C28 97.5(6) . . ?
C31 Dy C29 51.4(4) . . ?
C31 Dy C32 30.8(6) . . ?
C31 Dy C33 49.8(6) . . ?
C32 Dy C33 28.7(6) . . ?
N2 N1 Dy 131.1(6) . . ?
N2 N1 C12 110.6(8) . . ?
C12 N1 Dy 118.2(6) . . ?
N1 N2 C1 123.0(8) . . ?
N4 N3 C1 122.8(7) . . ?
N3 N4 Dy 130.5(5) . . ?
N3 N4 C18 110.7(7) . . ?
C18 N4 Dy 118.7(5) . . ?
N2 C1 C2 114.0(7) . . ?
N3 C1 N2 131.0(8) . . ?
N3 C1 C2 114.7(7) . . ?
C3 C2 C1 121.9(7) . . ?
C7 C2 C1 121.0(7) . . ?
C7 C2 C3 116.9(8) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(8) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 118.6 . . ?
C3 C4 C5 122.8(8) . . ?
C5 C4 H4 118.6 . . ?
C4 C5 C8A 120.8(18) . . ?
C4 C5 C8B 123.7(17) . . ?
C6 C5 C4 116.5(8) . . ?
C6 C5 C8A 122.7(18) . . ?
C6 C5 C8B 119.6(17) . . ?
C5 C6 H6 119.3 . . ?
C5 C6 C7 121.5(9) . . ?
C7 C6 H6 119.3 . . ?
C2 C7 C6 121.5(8) . . ?
C2 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C5 C8A C10A 108(3) . . ?
C5 C8A C11A 111(3) . . ?
C9A C8A C5 113(3) . . ?
C9A C8A C10A 107(3) . . ?
C9A C8A C11A 113(3) . . ?
C11A C8A C10A 103(3) . . ?
C5 C8B C10B 106(2) . . ?
C5 C8B C11B 113(2) . . ?
C9B C8B C5 113(2) . . ?
C9B C8B C10B 112(3) . . ?
C9B C8B C11B 110(2) . . ?
C10B C8B C11B 101(2) . . ?
C8A C9A H9AA 109.5 . . ?
C8A C9A H9AB 109.5 . . ?
C8A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C8B C9B H9BA 109.5 . . ?
C8B C9B H9BB 109.5 . . ?
C8B C9B H9BC 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
C8A C10A H10A 109.5 . . ?
C8A C10A H10B 109.5 . . ?
C8A C10A H10C 109.5 . . ?
H10A C10A H10B 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C8B C10B H10D 109.5 . . ?
C8B C10B H10E 109.5 . . ?
C8B C10B H10F 109.5 . . ?
H10D C10B H10E 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C8A C11A H11A 109.5 . . ?
C8A C11A H11B 109.5 . . ?
C8A C11A H11C 109.5 . . ?
H11A C11A H11B 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
C8B C11B H11D 109.5 . . ?
C8B C11B H11E 109.5 . . ?
C8B C11B H11F 109.5 . . ?
H11D C11B H11E 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
C13 C12 N1 121.5(9) . . ?
C17 C12 N1 118.5(8) . . ?
C17 C12 C13 120.0(9) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.0(11) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C15 120.1(11) . . ?
C15 C14 H14 120.0 . . ?
C14 C15 H15 120.2 . . ?
C14 C15 C16 119.7(10) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.6(10) . . ?
C17 C16 H16 120.2 . . ?
C12 C17 H17 120.1 . . ?
C16 C17 C12 119.8(10) . . ?
C16 C17 H17 120.1 . . ?
C19 C18 N4 123.3(8) . . ?
C19 C18 C23 119.1(8) . . ?
C23 C18 N4 117.5(8) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.3(10) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 121.0(12) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.1(11) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.8 . . ?
C21 C22 C23 120.4(10) . . ?
C23 C22 H22 119.8 . . ?
C18 C23 H23 120.0 . . ?
C22 C23 C18 120.1(9) . . ?
C22 C23 H23 120.0 . . ?
Dy C24 H24 118.0 . . ?
C25 C24 Dy 73.9(8) . . ?
C25 C24 H24 125.8 . . ?
C28 C24 Dy 74.2(7) . . ?
C28 C24 H24 125.8 . . ?
C28 C24 C25 108.3(17) . . ?
Dy C25 H25 115.2 . . ?
C24 C25 Dy 75.7(9) . . ?
C24 C25 H25 125.2 . . ?
C26 C25 Dy 75.8(8) . . ?
C26 C25 C24 109.5(15) . . ?
C26 C25 H25 125.2 . . ?
Dy C26 H26 118.8 . . ?
C25 C26 Dy 74.1(9) . . ?
C25 C26 H26 126.9 . . ?
C25 C26 C27 106.2(15) . . ?
C27 C26 Dy 72.3(7) . . ?
C27 C26 H26 126.9 . . ?
Dy C27 H27 114.1 . . ?
C26 C27 Dy 76.3(8) . . ?
C26 C27 H27 125.9 . . ?
C28 C27 Dy 76.0(8) . . ?
C28 C27 C26 108.1(16) . . ?
C28 C27 H27 125.9 . . ?
Dy C28 H28 117.0 . . ?
C24 C28 Dy 75.7(8) . . ?
C24 C28 C27 107.7(16) . . ?
C24 C28 H28 126.1 . . ?
C27 C28 Dy 73.2(7) . . ?
C27 C28 H28 126.1 . . ?
Dy C29 H29 117.5 . . ?
C30 C29 Dy 72.2(7) . . ?
C30 C29 H29 125.9 . . ?
C30 C29 C33 108.2(14) . . ?
C33 C29 Dy 76.3(8) . . ?
C33 C29 H29 125.9 . . ?
Dy C30 H30 113.3 . . ?
C29 C30 Dy 77.2(7) . . ?
C29 C30 H30 126.7 . . ?
C29 C30 C31 106.5(15) . . ?
C31 C30 Dy 75.5(7) . . ?
C31 C30 H30 126.7 . . ?
Dy C31 H31 116.8 . . ?
C30 C31 Dy 71.8(7) . . ?
C30 C31 H31 127.3 . . ?
C32 C31 Dy 76.5(8) . . ?
C32 C31 C30 105.4(13) . . ?
C32 C31 H31 127.3 . . ?
Dy C32 H32 118.0 . . ?
C31 C32 Dy 72.7(9) . . ?
C31 C32 H32 125.2 . . ?
C33 C32 Dy 75.9(8) . . ?
C33 C32 C31 109.7(16) . . ?
C33 C32 H32 125.2 . . ?
Dy C33 H33 118.2 . . ?
C29 C33 Dy 73.2(8) . . ?
C29 C33 H33 124.9 . . ?
C32 C33 Dy 75.5(10) . . ?
C32 C33 C29 110.2(18) . . ?
C32 C33 H33 124.9 . . ?
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
Dy N1 2.370(8) . ?
Dy N4 2.366(7) . ?
Dy C24 2.646(12) . ?
Dy C25 2.623(14) . ?
Dy C26 2.644(13) . ?
Dy C27 2.593(13) . ?
Dy C28 2.627(11) . ?
Dy C29 2.619(11) . ?
Dy C30 2.558(12) . ?
Dy C31 2.607(12) . ?
Dy C32 2.654(14) . ?
Dy C33 2.659(14) . ?
N1 N2 1.286(11) . ?
N1 C12 1.447(12) . ?
N2 C1 1.346(10) . ?
N3 N4 1.309(10) . ?
N3 C1 1.329(10) . ?
N4 C18 1.415(11) . ?
C1 C2 1.480(11) . ?
C2 C3 1.396(11) . ?
C2 C7 1.385(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.372(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(12) . ?
C5 C6 1.381(12) . ?
C5 C8A 1.507(19) . ?
C5 C8B 1.507(18) . ?
C6 H6 0.9500 . ?
C6 C7 1.394(13) . ?
C7 H7 0.9500 . ?
C8A C9A 1.49(4) . ?
C8A C10A 1.55(4) . ?
C8A C11A 1.51(4) . ?
C8B C9B 1.48(4) . ?
C8B C10B 1.53(4) . ?
C8B C11B 1.53(4) . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C9B H9BA 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11C 0.9800 . ?
C11B H11D 0.9800 . ?
C11B H11E 0.9800 . ?
C11B H11F 0.9800 . ?
C12 C13 1.403(14) . ?
C12 C17 1.392(16) . ?
C13 H13 0.9500 . ?
C13 C14 1.362(15) . ?
C14 H14 0.9500 . ?
C14 C15 1.398(18) . ?
C15 H15 0.9500 . ?
C15 C16 1.421(18) . ?
C16 H16 0.9500 . ?
C16 C17 1.392(15) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(13) . ?
C18 C23 1.399(13) . ?
C19 H19 0.9500 . ?
C19 C20 1.378(14) . ?
C20 H20 0.9500 . ?
C20 C21 1.376(18) . ?
C21 H21 0.9500 . ?
C21 C22 1.355(18) . ?
C22 H22 0.9500 . ?
C22 C23 1.378(14) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C24 C25 1.38(3) . ?
C24 C28 1.37(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.37(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.42(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.39(3) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C29 C30 1.37(2) . ?
C29 C33 1.39(2) . ?
C30 H30 0.9500 . ?
C30 C31 1.46(2) . ?
C31 H31 0.9500 . ?
C31 C32 1.40(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.32(3) . ?
C33 H33 0.9500 . ?
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
Dy N1 N2 C1 10.0(13) . . . . ?
Dy N1 C12 C13 -140.9(9) . . . . ?
Dy N1 C12 C17 36.7(12) . . . . ?
Dy N4 C18 C19 159.0(8) . . . . ?
Dy N4 C18 C23 -23.2(11) . . . . ?
Dy C24 C25 C26 69.0(11) . . . . ?
Dy C24 C28 C27 -66.8(9) . . . . ?
Dy C25 C26 C27 65.7(9) . . . . ?
Dy C26 C27 C28 70.0(9) . . . . ?
Dy C27 C28 C24 68.5(11) . . . . ?
Dy C29 C30 C31 70.4(9) . . . . ?
Dy C29 C33 C32 -67.0(10) . . . . ?
Dy C30 C31 C32 69.8(9) . . . . ?
Dy C31 C32 C33 67.5(10) . . . . ?
Dy C32 C33 C29 65.5(9) . . . . ?
N1 N2 C1 N3 17.6(15) . . . . ?
N1 N2 C1 C2 -169.6(8) . . . . ?
N1 C12 C13 C14 177.3(11) . . . . ?
N1 C12 C17 C16 -178.3(10) . . . . ?
N2 N1 C12 C13 40.3(13) . . . . ?
N2 N1 C12 C17 -142.0(10) . . . . ?
N2 C1 C2 C3 -5.8(12) . . . . ?
N2 C1 C2 C7 168.6(9) . . . . ?
N3 N4 C18 C19 -24.7(14) . . . . ?
N3 N4 C18 C23 153.0(9) . . . . ?
N3 C1 C2 C3 168.2(8) . . . . ?
N3 C1 C2 C7 -17.4(13) . . . . ?
N4 N3 C1 N2 -15.8(15) . . . . ?
N4 N3 C1 C2 171.5(8) . . . . ?
N4 C18 C19 C20 178.3(11) . . . . ?
N4 C18 C23 C22 -177.9(9) . . . . ?
C1 N3 N4 Dy -13.3(14) . . . . ?
C1 N3 N4 C18 171.0(8) . . . . ?
C1 C2 C3 C4 174.9(9) . . . . ?
C1 C2 C7 C6 -173.4(10) . . . . ?
C2 C3 C4 C5 -2.5(16) . . . . ?
C3 C2 C7 C6 1.2(15) . . . . ?
C3 C4 C5 C6 3.1(15) . . . . ?
C3 C4 C5 C8A -174(2) . . . . ?
C3 C4 C5 C8B -171(2) . . . . ?
C4 C5 C6 C7 -1.5(16) . . . . ?
C4 C5 C8A C9A -169(2) . . . . ?
C4 C5 C8A C10A 72(3) . . . . ?
C4 C5 C8A C11A -40(4) . . . . ?
C4 C5 C8B C9B -140(2) . . . . ?
C4 C5 C8B C10B 96(3) . . . . ?
C4 C5 C8B C11B -13(4) . . . . ?
C5 C6 C7 C2 -0.6(17) . . . . ?
C6 C5 C8A C9A 15(4) . . . . ?
C6 C5 C8A C10A -104(3) . . . . ?
C6 C5 C8A C11A 143(2) . . . . ?
C6 C5 C8B C9B 46(3) . . . . ?
C6 C5 C8B C10B -77(3) . . . . ?
C6 C5 C8B C11B 173(2) . . . . ?
C7 C2 C3 C4 0.3(14) . . . . ?
C8A C5 C6 C7 175(2) . . . . ?
C8B C5 C6 C7 172(2) . . . . ?
C12 N1 N2 C1 -171.4(8) . . . . ?
C12 C13 C14 C15 1(2) . . . . ?
C13 C12 C17 C16 -0.7(18) . . . . ?
C13 C14 C15 C16 0(2) . . . . ?
C14 C15 C16 C17 -0.9(19) . . . . ?
C15 C16 C17 C12 1.2(19) . . . . ?
C17 C12 C13 C14 -0.3(18) . . . . ?
C18 C19 C20 C21 -2(2) . . . . ?
C19 C18 C23 C22 -0.1(15) . . . . ?
C19 C20 C21 C22 2(2) . . . . ?
C20 C21 C22 C23 -1(2) . . . . ?
C21 C22 C23 C18 0.5(18) . . . . ?
C23 C18 C19 C20 0.6(17) . . . . ?
C24 C25 C26 Dy -68.9(11) . . . . ?
C24 C25 C26 C27 -3.2(16) . . . . ?
C25 C24 C28 Dy 66.6(11) . . . . ?
C25 C24 C28 C27 -0.2(17) . . . . ?
C25 C26 C27 Dy -66.9(10) . . . . ?
C25 C26 C27 C28 3.1(15) . . . . ?
C26 C27 C28 Dy -70.3(8) . . . . ?
C26 C27 C28 C24 -1.8(15) . . . . ?
C28 C24 C25 Dy -66.8(11) . . . . ?
C28 C24 C25 C26 2.2(18) . . . . ?
C29 C30 C31 Dy -71.6(9) . . . . ?
C29 C30 C31 C32 -1.8(15) . . . . ?
C30 C29 C33 Dy 65.8(9) . . . . ?
C30 C29 C33 C32 -1.2(16) . . . . ?
C30 C31 C32 Dy -66.5(9) . . . . ?
C30 C31 C32 C33 1.1(16) . . . . ?
C31 C32 C33 Dy -65.5(11) . . . . ?
C31 C32 C33 C29 0.1(17) . . . . ?
C33 C29 C30 Dy -68.5(9) . . . . ?
C33 C29 C30 C31 1.8(14) . . . . ?
