#------------------------------------------------------------------------------
#$Date: 2021-02-05 00:38:45 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261551 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/75/7127571.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_7127571
loop_
_publ_author_name
'Thomas-Hargreaves, Lewis R'
'Hunger, David'
'Kern, Michal'
'Wooles, Ashley J.'
'van Slageren, Joris'
'Chilton, Nicholas F.'
'Liddle, Stephen T.'
_publ_section_title
;
 Insights into D₄ₕ@metal-symmetry single-molecule
 magnetism: the case of a dysprosium-bis(boryloxide) complex.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              733
_journal_page_last               736
_journal_paper_doi               10.1039/d0cc07446b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C60 H92 B3 Dy N4 O4, C6 H6'
_chemical_formula_sum            'C66 H98 B3 Dy N4 O4'
_chemical_formula_weight         1206.41
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-11 deposited with the CCDC.	2020-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                107.413(6)
_cell_angle_beta                 92.621(5)
_cell_angle_gamma                98.825(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7769(7)
_cell_length_b                   13.6689(7)
_cell_length_c                   19.8264(15)
_cell_measurement_reflns_used    8170
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3800
_cell_measurement_theta_min      2.9890
_cell_volume                     3249.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  50.00   1.00   15.00    --  -18.77  57.00 -30.00   83
  2  ω    -20.00  24.00   1.00   15.00    --  -18.77 -99.00 -30.00   44
  3  ω    -88.00 -22.00   1.00   15.00    --  -18.77 -57.00-180.00   66
  4  ω    -20.00   7.00   1.00   15.00    --  -18.77 -99.00-150.00   27
  5  ω     36.00  67.00   1.00   15.00    --   20.02 178.00 120.00   31
  6  ω     39.00  94.00   1.00   15.00    --   20.02 178.00-120.00   55
  7  ω    -52.00  45.00   1.00   15.00    --   20.02 -38.00-150.00   97
  8  ω     40.00  65.00   1.00   15.00    --   20.02 178.00  30.00   25
  9  ω    -24.00  49.00   1.00   15.00    --   20.02 -77.00  90.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0558365000
_diffrn_orient_matrix_UB_12      -0.0038842000
_diffrn_orient_matrix_UB_13      0.0012246000
_diffrn_orient_matrix_UB_21      0.0076644000
_diffrn_orient_matrix_UB_22      0.0225338000
_diffrn_orient_matrix_UB_23      0.0374551000
_diffrn_orient_matrix_UB_31      0.0031226000
_diffrn_orient_matrix_UB_32      0.0502844000
_diffrn_orient_matrix_UB_33      -0.0038495000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.1498
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11803
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.322
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1270
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.175
_refine_diff_density_max         4.601
_refine_diff_density_min         -4.057
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         11803
_refine_ls_number_restraints     1088
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.1325
_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)+(0.0933P)²+94.6784P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3221
_refine_ls_wR_factor_ref         0.3354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9412
_reflns_number_total             11803
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc07446b2.cif
_cod_data_source_block           1Dy
_cod_depositor_comments
'Adding full bibliography for 7127568--7127571.cif.'
_cod_database_code               7127571
_manchester_internal_diff_code   ASTL483
_manchester_internal_coll_client LTH
_manchester_internal_coll_date   15/08/2019
_manchester_internal_process_date 10/03/2020
_manchester_internal_process_user AW
_manchester_internal_solution_date 10/03/2020
_manchester_internal_solution_user AW
_manchester_internal_refinement_date 16/03/2020
_manchester_internal_refinement_user AW
_manchester_internal_validation_date 16/03/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 16/03/2020
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Dy C70 H90 B3 O4 N4'
_chemical_oxdiff_usercomment     LTH/STL
_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   0.818
_shelx_estimated_absorpt_t_min   0.686
_reflns_odcompleteness_completeness 88.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.773(4)
 0.227(4)
2. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H,H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 B3-H3D = B3-H3B = B3-H3C = B3-H3A
 1.05 with sigma of 0.01
 H3B-H3C \\sim H3C-H3A \\sim H3B-H3A \\sim H3D-H3A \\sim H3B-H3D \\sim H3C-H3D
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C4 \\sim C10 \\sim C9 \\sim C3 \\sim C5: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24), C35(H35), C38(H38), C47(H47), C50(H50)
6.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,
 H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19),
 C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C43(H43), C44(H44), C45(H45),
  C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   4414
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.944
_oxdiff_exptl_absorpt_empirical_full_min 0.614
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 0.79616(6) 0.98974(6) 0.65725(4) 0.0245(2) Uani 1 1 d . U . . .
O1 O 0.8407(8) 1.1424(8) 0.7283(6) 0.031(2) Uani 1 1 d . U . . .
O2 O 0.7609(9) 0.8726(8) 0.7046(6) 0.033(2) Uani 1 1 d . U . . .
O3 O 0.9770(8) 0.9665(8) 0.6545(6) 0.031(2) Uani 1 1 d . U . . .
O4 O 0.6174(8) 1.0171(9) 0.6536(7) 0.035(2) Uani 1 1 d . U . . .
N1 N 0.9635(11) 1.2911(11) 0.8165(7) 0.032(2) Uani 1 1 d . U . . .
N2 N 0.8062(10) 1.3271(10) 0.7754(7) 0.029(2) Uani 1 1 d . U . . .
N3 N 0.6476(11) 0.7610(11) 0.7645(7) 0.034(2) Uani 1 1 d . U . . .
N4 N 0.7893(11) 0.6981(10) 0.7114(7) 0.033(2) Uani 1 1 d . U . . .
C1 C 0.9604(14) 1.3979(13) 0.8464(9) 0.034(3) Uani 1 1 d . U . . .
H1 H 1.015072 1.447726 0.877950 0.041 Uiso 1 1 calc R . . . .
C2 C 0.8672(13) 1.4185(13) 0.8229(9) 0.032(3) Uani 1 1 d . U . . .
H2 H 0.846209 1.484831 0.836504 0.039 Uiso 1 1 calc R . . . .
C3 C 0.7100(12) 1.3309(12) 0.7401(8) 0.026(2) Uani 1 1 d . U . . .
C4 C 0.6977(11) 1.3133(11) 0.6632(7) 0.0200(17) Uiso 1 1 d . U . . .
C5 C 0.6015(13) 1.3230(12) 0.6330(8) 0.028(2) Uani 1 1 d . U . . .
H5 H 0.591911 1.310613 0.583174 0.034 Uiso 1 1 calc R . . . .
C6 C 0.5215(14) 1.3494(13) 0.6723(9) 0.035(3) Uani 1 1 d . U . . .
H6 H 0.457158 1.355824 0.649321 0.042 Uiso 1 1 calc R . . . .
C7 C 0.5293(14) 1.3677(14) 0.7453(9) 0.039(3) Uani 1 1 d . U . . .
H7 H 0.470377 1.385164 0.771083 0.047 Uiso 1 1 calc R . . . .
C8 C 0.6240(14) 1.3604(14) 0.7812(9) 0.038(3) Uani 1 1 d . U . . .
C9 C 0.7955(13) 1.2975(12) 0.6257(8) 0.027(2) Uani 1 1 d . U . . .
H9 H 0.830592 1.248530 0.643809 0.033 Uiso 1 1 calc R . . . .
C10 C 0.7696(15) 1.2472(14) 0.5445(9) 0.039(3) Uani 1 1 d . U . . .
H10A H 0.726319 1.177857 0.534585 0.059 Uiso 1 1 calc GR . . . .
H10B H 0.835931 1.241096 0.521973 0.059 Uiso 1 1 calc GR . . . .
H10C H 0.730002 1.290833 0.525629 0.059 Uiso 1 1 calc GR . . . .
C11 C 0.8753(15) 1.3972(14) 0.6399(10) 0.042(4) Uani 1 1 d . U . . .
H11A H 0.842485 1.447714 0.623894 0.064 Uiso 1 1 calc GR . . . .
H11B H 0.937527 1.382355 0.614034 0.064 Uiso 1 1 calc GR . . . .
H11C H 0.897534 1.426079 0.690909 0.064 Uiso 1 1 calc GR . . . .
C12 C 0.6310(15) 1.3789(15) 0.8596(9) 0.041(3) Uani 1 1 d . U . . .
H12 H 0.700465 1.362600 0.874444 0.049 Uiso 1 1 calc R . . . .
C13 C 0.5415(15) 1.3103(17) 0.8823(11) 0.049(4) Uani 1 1 d . U . . .
H13A H 0.472362 1.321142 0.865128 0.073 Uiso 1 1 calc GR . . . .
H13B H 0.547122 1.329058 0.934231 0.073 Uiso 1 1 calc GR . . . .
H13C H 0.547800 1.236934 0.862017 0.073 Uiso 1 1 calc GR . . . .
C14 C 0.6281(17) 1.4932(16) 0.8997(11) 0.051(4) Uani 1 1 d . U . . .
H14A H 0.693003 1.537125 0.893701 0.076 Uiso 1 1 calc GR . . . .
H14B H 0.623733 1.501710 0.950294 0.076 Uiso 1 1 calc GR . . . .
H14C H 0.565852 1.513896 0.880691 0.076 Uiso 1 1 calc GR . . . .
C15 C 1.0650(13) 1.2570(13) 0.8200(9) 0.035(2) Uani 1 1 d . U . . .
C16 C 1.1326(14) 1.2626(14) 0.7674(10) 0.037(2) Uani 1 1 d . U . . .
C17 C 1.2316(14) 1.2301(15) 0.7707(10) 0.043(3) Uani 1 1 d . U . . .
H17 H 1.277938 1.232322 0.734901 0.052 Uiso 1 1 calc R . . . .
C18 C 1.2606(15) 1.1959(15) 0.8246(11) 0.045(3) Uani 1 1 d . U . . .
H18 H 1.329114 1.177553 0.827424 0.054 Uiso 1 1 calc R . . . .
C19 C 1.1909(15) 1.1864(15) 0.8776(10) 0.045(3) Uani 1 1 d . U . . .
H19 H 1.211546 1.158998 0.913908 0.054 Uiso 1 1 calc R . . . .
C20 C 1.0913(14) 1.2182(15) 0.8756(10) 0.041(3) Uani 1 1 d . U . . .
C21 C 1.0971(15) 1.3044(14) 0.7056(10) 0.041(3) Uani 1 1 d . U . . .
H21 H 1.032533 1.336719 0.717859 0.049 Uiso 1 1 calc R . . . .
C22 C 1.1882(18) 1.3885(16) 0.6982(11) 0.055(5) Uani 1 1 d . U . . .
H22A H 1.216796 1.435499 0.745443 0.083 Uiso 1 1 calc GR . . . .
H22B H 1.160469 1.428325 0.669928 0.083 Uiso 1 1 calc GR . . . .
H22C H 1.244787 1.354691 0.674561 0.083 Uiso 1 1 calc GR . . . .
C23 C 1.0711(16) 1.2182(14) 0.6373(10) 0.043(4) Uani 1 1 d . U . . .
H23A H 1.134094 1.186324 0.624812 0.065 Uiso 1 1 calc GR . . . .
H23B H 1.048905 1.245945 0.599742 0.065 Uiso 1 1 calc GR . . . .
H23C H 1.013162 1.165634 0.642293 0.065 Uiso 1 1 calc GR . . . .
C24 C 1.0208(16) 1.2170(16) 0.9338(10) 0.046(3) Uani 1 1 d . U . . .
H24 H 0.947138 1.218866 0.915469 0.056 Uiso 1 1 calc R . . . .
C25 C 1.0536(18) 1.3105(17) 0.9980(11) 0.057(5) Uani 1 1 d . U . . .
H25A H 1.129884 1.318457 1.011761 0.085 Uiso 1 1 calc GR . . . .
H25B H 1.013315 1.301429 1.037265 0.085 Uiso 1 1 calc GR . . . .
H25C H 1.039223 1.372753 0.987093 0.085 Uiso 1 1 calc GR . . . .
C26 C 1.0166(17) 1.1152(17) 0.9535(11) 0.053(4) Uani 1 1 d . U . . .
H26A H 1.007135 1.055716 0.909957 0.080 Uiso 1 1 calc GR . . . .
H26B H 0.956758 1.107377 0.981758 0.080 Uiso 1 1 calc GR . . . .
H26C H 1.083174 1.118059 0.981105 0.080 Uiso 1 1 calc GR . . . .
C27 C 0.7320(14) 0.6257(13) 0.7414(9) 0.034(3) Uani 1 1 d . U . . .
H27 H 0.749039 0.559523 0.738990 0.041 Uiso 1 1 calc R . . . .
C28 C 0.6534(14) 0.6633(13) 0.7725(9) 0.034(3) Uani 1 1 d . U . . .
H28 H 0.605965 0.629378 0.797297 0.041 Uiso 1 1 calc R . . . .
C29 C 0.5613(14) 0.8141(14) 0.7843(9) 0.036(2) Uani 1 1 d . U . . .
C30 C 0.4658(14) 0.7784(15) 0.7383(10) 0.040(3) Uani 1 1 d . U . . .
C31 C 0.3803(15) 0.8291(15) 0.7572(11) 0.043(3) Uani 1 1 d . U . . .
H31 H 0.316222 0.807886 0.726367 0.052 Uiso 1 1 calc R . . . .
C32 C 0.3862(16) 0.9076(16) 0.8180(11) 0.049(3) Uani 1 1 d . U . . .
H32 H 0.325801 0.939874 0.829800 0.059 Uiso 1 1 calc R . . . .
C33 C 0.4794(16) 0.9428(17) 0.8644(11) 0.049(3) Uani 1 1 d . U . . .
H33 H 0.483372 0.999042 0.906976 0.059 Uiso 1 1 calc R . . . .
C34 C 0.5683(15) 0.8919(15) 0.8461(10) 0.043(3) Uani 1 1 d . U . . .
C35 C 0.4595(15) 0.6903(15) 0.6655(10) 0.043(3) Uani 1 1 d . U . . .
H35 H 0.528300 0.663801 0.664473 0.051 Uiso 1 1 calc R . . . .
C36 C 0.448(2) 0.723(2) 0.6035(12) 0.068(5) Uani 1 1 d . U . . .
H36A H 0.377654 0.741029 0.598766 0.101 Uiso 1 1 calc GR . . . .
H36B H 0.457458 0.666647 0.561272 0.101 Uiso 1 1 calc GR . . . .
H36C H 0.502856 0.784432 0.608158 0.101 Uiso 1 1 calc GR . . . .
C37 C 0.372(2) 0.5993(19) 0.6641(15) 0.078(6) Uani 1 1 d . U . . .
H37A H 0.392127 0.567869 0.700084 0.116 Uiso 1 1 calc GR . . . .
H37B H 0.362724 0.547033 0.617072 0.116 Uiso 1 1 calc GR . . . .
H37C H 0.304985 0.624923 0.674341 0.116 Uiso 1 1 calc GR . . . .
C38 C 0.6765(17) 0.9334(18) 0.8961(11) 0.056(4) Uani 1 1 d . U . . .
H38 H 0.725951 0.882543 0.880803 0.067 Uiso 1 1 calc R . . . .
C39 C 0.728(2) 1.038(2) 0.8912(14) 0.076(6) Uani 1 1 d . U . . .
H39A H 0.741779 1.031132 0.841931 0.114 Uiso 1 1 calc GR . . . .
H39B H 0.795634 1.061895 0.921627 0.114 Uiso 1 1 calc GR . . . .
H39C H 0.680693 1.088472 0.906969 0.114 Uiso 1 1 calc GR . . . .
C40 C 0.656(2) 0.945(2) 0.9737(12) 0.078(6) Uani 1 1 d . U . . .
H40A H 0.580524 0.946623 0.979186 0.116 Uiso 1 1 calc GR . . . .
H40B H 0.698786 1.010354 1.004791 0.116 Uiso 1 1 calc GR . . . .
H40C H 0.676223 0.886351 0.986636 0.116 Uiso 1 1 calc GR . . . .
C41 C 0.8733(14) 0.6759(13) 0.6725(9) 0.035(2) Uani 1 1 d . U . . .
C42 C 0.9726(15) 0.6693(13) 0.7056(10) 0.038(3) Uani 1 1 d . U . . .
C43 C 1.0569(15) 0.6421(13) 0.6645(10) 0.041(3) Uani 1 1 d . U . . .
H43 H 1.122171 0.635530 0.686203 0.049 Uiso 1 1 calc R . . . .
C44 C 1.0430(17) 0.6248(14) 0.5908(11) 0.046(3) Uani 1 1 d . U . . .
H44 H 1.100670 0.609498 0.563158 0.055 Uiso 1 1 calc R . . . .
C45 C 0.9493(16) 0.6294(14) 0.5583(11) 0.043(3) Uani 1 1 d . U . . .
H45 H 0.942453 0.615821 0.508321 0.052 Uiso 1 1 calc R . . . .
C46 C 0.8608(15) 0.6538(13) 0.5968(10) 0.039(3) Uani 1 1 d . U . . .
C47 C 0.7550(16) 0.6496(13) 0.5604(9) 0.040(3) Uani 1 1 d . U . . .
H47 H 0.723710 0.708882 0.590234 0.048 Uiso 1 1 calc R . . . .
C48 C 0.7578(19) 0.6609(16) 0.4858(10) 0.054(5) Uani 1 1 d . U . . .
H48A H 0.797572 0.729653 0.488953 0.081 Uiso 1 1 calc GR . . . .
H48B H 0.684907 0.653634 0.464884 0.081 Uiso 1 1 calc GR . . . .
H48C H 0.792604 0.606724 0.455943 0.081 Uiso 1 1 calc GR . . . .
C49 C 0.6819(17) 0.5500(14) 0.5579(11) 0.049(4) Uani 1 1 d . U . . .
H49A H 0.705283 0.490592 0.524326 0.073 Uiso 1 1 calc GR . . . .
H49B H 0.608958 0.553416 0.542411 0.073 Uiso 1 1 calc GR . . . .
H49C H 0.684104 0.541487 0.605255 0.073 Uiso 1 1 calc GR . . . .
C50 C 0.9883(16) 0.6905(15) 0.7851(10) 0.045(3) Uani 1 1 d . U . . .
H50 H 0.923336 0.651333 0.797639 0.054 Uiso 1 1 calc R . . . .
C51 C 1.0818(17) 0.6459(19) 0.8071(12) 0.058(5) Uani 1 1 d . U . . .
H51A H 1.084211 0.578428 0.772126 0.086 Uiso 1 1 calc GR . . . .
H51B H 1.073088 0.636617 0.853822 0.086 Uiso 1 1 calc GR . . . .
H51C H 1.148304 0.693927 0.809644 0.086 Uiso 1 1 calc GR . . . .
C52 C 0.9931(19) 0.8004(16) 0.8268(10) 0.052(4) Uani 1 1 d . U . . .
H52A H 1.057342 0.842434 0.818178 0.078 Uiso 1 1 calc GR . . . .
H52B H 0.994966 0.806845 0.877439 0.078 Uiso 1 1 calc GR . . . .
H52C H 0.930102 0.825106 0.812576 0.078 Uiso 1 1 calc GR . . . .
C53 C 1.0429(14) 0.9251(15) 0.5973(10) 0.041(3) Uani 1 1 d . U . . .
H53A H 1.042811 0.962603 0.561652 0.049 Uiso 1 1 calc R . . . .
H53B H 1.017552 0.849832 0.573336 0.049 Uiso 1 1 calc R . . . .
C54 C 1.1509(14) 0.9442(15) 0.6359(10) 0.041(3) Uani 1 1 d . U . . .
H54A H 1.188219 1.015832 0.642163 0.050 Uiso 1 1 calc R . . . .
H54B H 1.194473 0.894144 0.609572 0.050 Uiso 1 1 calc R . . . .
C55 C 1.1310(13) 0.9290(14) 0.7072(10) 0.038(3) Uani 1 1 d . U . . .
H55A H 1.114688 0.854366 0.703705 0.046 Uiso 1 1 calc R . . . .
H55B H 1.191849 0.964334 0.743461 0.046 Uiso 1 1 calc R . . . .
C56 C 1.0353(13) 0.9810(14) 0.7221(9) 0.036(3) Uani 1 1 d . U . . .
H56A H 0.989784 0.949413 0.751932 0.043 Uiso 1 1 calc R . . . .
H56B H 1.057829 1.056163 0.747727 0.043 Uiso 1 1 calc R . . . .
C57 C 0.5465(14) 1.0257(17) 0.5972(11) 0.047(3) Uani 1 1 d . U . . .
H57A H 0.544758 0.966554 0.553431 0.057 Uiso 1 1 calc R . . . .
H57B H 0.570064 1.091450 0.586463 0.057 Uiso 1 1 calc R . . . .
C58 C 0.4376(14) 1.0244(17) 0.6248(11) 0.050(3) Uani 1 1 d . U . . .
H58A H 0.392976 1.061503 0.602440 0.061 Uiso 1 1 calc R . . . .
H58B H 0.400003 0.952263 0.616593 0.061 Uiso 1 1 calc R . . . .
C59 C 0.4656(14) 1.0812(16) 0.7034(11) 0.046(3) Uani 1 1 d . U . . .
H59A H 0.410088 1.058982 0.731563 0.055 Uiso 1 1 calc R . . . .
H59B H 0.473689 1.157478 0.713024 0.055 Uiso 1 1 calc R . . . .
C60 C 0.5706(13) 1.0506(15) 0.7208(11) 0.042(3) Uani 1 1 d . U . . .
H60A H 0.618351 1.110718 0.754877 0.050 Uiso 1 1 calc R . . . .
H60B H 0.558510 0.993234 0.741914 0.050 Uiso 1 1 calc R . . . .
B1 B 0.8677(15) 1.2414(14) 0.7699(10) 0.030(3) Uani 1 1 d . U . . .
B2 B 0.7366(16) 0.7884(15) 0.7255(10) 0.032(2) Uani 1 1 d . U . . .
B3 B 0.7764(19) 0.942(2) 0.5215(12) 0.052(6) Uani 1 1 d D U . . .
H3A H 0.703(5) 0.926(9) 0.541(6) 0.062 Uiso 1 1 d DR . . . .
H3B H 0.831(7) 0.903(8) 0.539(6) 0.062 Uiso 1 1 d DR . . . .
H3C H 0.805(9) 1.023(3) 0.540(6) 0.062 Uiso 1 1 d DR . . . .
H3D H 0.766(9) 0.917(9) 0.4658(13) 0.062 Uiso 1 1 d DR . . . .
C61 C 0.7829(19) 1.4210(19) 1.0303(13) 0.064(4) Uani 1 1 d . U . . .
H61 H 0.831889 1.449129 1.003399 0.077 Uiso 1 1 calc R . . . .
C62 C 0.737(2) 1.483(2) 1.0839(13) 0.068(4) Uani 1 1 d . U . . .
H62 H 0.753452 1.556398 1.094623 0.082 Uiso 1 1 calc R . . . .
C63 C 0.667(2) 1.440(2) 1.1227(14) 0.072(4) Uani 1 1 d . U . . .
H63 H 0.637411 1.485202 1.160652 0.087 Uiso 1 1 calc R . . . .
C64 C 0.638(2) 1.333(2) 1.1076(13) 0.070(4) Uani 1 1 d . U . . .
H64 H 0.586858 1.303521 1.132550 0.084 Uiso 1 1 calc R . . . .
C65 C 0.687(2) 1.272(2) 1.0548(12) 0.065(4) Uani 1 1 d . U . . .
H65 H 0.672526 1.198753 1.045058 0.078 Uiso 1 1 calc R . . . .
C66 C 0.7532(19) 1.3120(19) 1.0171(12) 0.062(4) Uani 1 1 d . U . . .
H66 H 0.782373 1.266102 0.979665 0.074 Uiso 1 1 calc R . . . .
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'
B B 0.0013 0.0007 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
18 -3 -2 0.1091
-10 3 21 0.0925
12 -7 19 0.1109
-13 -6 -12 0.1201
-11 10 -19 0.1341
7 15 2 0.1439
-13 -7 20 0.1057
-3 -1 -25 0.0876
14 0 -18 0.1174
14 -2 17 0.0884
2 -19 9 0.2069
-14 1 17 0.1026
-2 19 -9 0.1312
0 19 -11 0.1322
3 1 25 0.0876
10 -3 -21 0.0991
18 -7 1 0.1117
14 -8 -12 0.1252
-17 -3 5 0.1009
4 -4 26 0.0929
-18 3 2 0.1091
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O3 91.3(4) . . ?
O1 Dy1 O4 88.7(4) . . ?
O1 Dy1 B3 125.1(7) . . ?
O1 Dy1 H3A 132(3) . . ?
O1 Dy1 H3B 135(3) . . ?
O1 Dy1 H3C 101.3(8) . . ?
O2 Dy1 O1 115.5(4) . . ?
O2 Dy1 O3 90.9(4) . . ?
O2 Dy1 O4 92.5(4) . . ?
O2 Dy1 B3 119.4(7) . . ?
O2 Dy1 H3A 107(2) . . ?
O2 Dy1 H3B 105(2) . . ?
O2 Dy1 H3C 143.2(8) . . ?
O3 Dy1 B3 89.9(6) . . ?
O3 Dy1 H3A 111.5(14) . . ?
O3 Dy1 H3B 69.5(16) . . ?
O3 Dy1 H3C 89(3) . . ?
O4 Dy1 O3 176.2(4) . . ?
O4 Dy1 B3 87.0(6) . . ?
O4 Dy1 H3A 65.9(16) . . ?
O4 Dy1 H3B 108.0(15) . . ?
O4 Dy1 H3C 87(3) . . ?
B3 Dy1 H3A 24.2(3) . . ?
B3 Dy1 H3B 24.2(3) . . ?
B3 Dy1 H3C 23.9(5) . . ?
H3A Dy1 H3B 42.1(11) . . ?
H3A Dy1 H3C 41.0(11) . . ?
H3B Dy1 H3C 41.0(11) . . ?
B1 O1 Dy1 176.4(11) . . ?
B2 O2 Dy1 171.9(12) . . ?
C53 O3 Dy1 134.0(10) . . ?
C56 O3 Dy1 116.5(9) . . ?
C56 O3 C53 108.8(12) . . ?
C57 O4 Dy1 131.9(10) . . ?
C57 O4 C60 109.0(12) . . ?
C60 O4 Dy1 118.1(9) . . ?
C1 N1 C15 118.3(14) . . ?
C1 N1 B1 109.0(14) . . ?
B1 N1 C15 130.0(14) . . ?
C2 N2 B1 107.3(13) . . ?
C3 N2 C2 120.3(13) . . ?
C3 N2 B1 132.2(14) . . ?
C28 N3 C29 123.4(14) . . ?
C28 N3 B2 108.2(14) . . ?
C29 N3 B2 128.0(14) . . ?
C27 N4 B2 107.8(14) . . ?
C41 N4 C27 122.3(14) . . ?
C41 N4 B2 129.8(14) . . ?
N1 C1 H1 125.3 . . ?
C2 C1 N1 109.4(15) . . ?
C2 C1 H1 125.3 . . ?
N2 C2 H2 125.0 . . ?
C1 C2 N2 110.1(15) . . ?
C1 C2 H2 125.0 . . ?
N2 C3 C4 121.9(14) . . ?
N2 C3 C8 118.9(14) . . ?
C8 C3 C4 119.1(14) . . ?
C3 C4 C9 116.0(13) . . ?
C5 C4 C3 118.2(13) . . ?
C5 C4 C9 125.4(13) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.7(15) . . ?
C6 C5 H5 119.1 . . ?
C5 C6 H6 118.8 . . ?
C5 C6 C7 122.4(17) . . ?
C7 C6 H6 118.8 . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.3(17) . . ?
C8 C7 H7 119.8 . . ?
C3 C8 C12 121.9(15) . . ?
C7 C8 C3 118.2(16) . . ?
C7 C8 C12 119.9(16) . . ?
C4 C9 H9 107.5 . . ?
C4 C9 C10 112.3(14) . . ?
C4 C9 C11 112.9(13) . . ?
C10 C9 H9 107.5 . . ?
C11 C9 H9 107.5 . . ?
C11 C9 C10 108.9(13) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12 108.1 . . ?
C8 C12 C13 113.1(16) . . ?
C8 C12 C14 110.9(16) . . ?
C13 C12 H12 108.1 . . ?
C14 C12 H12 108.1 . . ?
C14 C12 C13 108.4(16) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N1 118.6(15) . . ?
C16 C15 C20 122.5(16) . . ?
C20 C15 N1 118.9(15) . . ?
C15 C16 C17 118.8(17) . . ?
C15 C16 C21 119.9(15) . . ?
C17 C16 C21 121.3(16) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.2(18) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 119.2 . . ?
C17 C18 C19 121.6(18) . . ?
C19 C18 H18 119.2 . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.5(18) . . ?
C20 C19 H19 120.3 . . ?
C15 C20 C19 117.4(17) . . ?
C15 C20 C24 122.2(16) . . ?
C19 C20 C24 120.3(17) . . ?
C16 C21 H21 109.0 . . ?
C22 C21 C16 109.0(16) . . ?
C22 C21 H21 109.0 . . ?
C23 C21 C16 110.9(15) . . ?
C23 C21 H21 109.0 . . ?
C23 C21 C22 110.0(16) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 H24 107.5 . . ?
C20 C24 C26 111.0(17) . . ?
C25 C24 C20 112.1(17) . . ?
C25 C24 H24 107.5 . . ?
C25 C24 C26 110.9(17) . . ?
C26 C24 H24 107.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N4 C27 H27 125.0 . . ?
C28 C27 N4 110.1(15) . . ?
C28 C27 H27 125.0 . . ?
N3 C28 H28 124.5 . . ?
C27 C28 N3 110.9(15) . . ?
C27 C28 H28 124.5 . . ?
C30 C29 N3 117.2(16) . . ?
C34 C29 N3 121.2(16) . . ?
C34 C29 C30 121.5(17) . . ?
C29 C30 C35 121.1(16) . . ?
C31 C30 C29 117.9(18) . . ?
C31 C30 C35 120.8(17) . . ?
C30 C31 H31 119.3 . . ?
C32 C31 C30 121.5(19) . . ?
C32 C31 H31 119.3 . . ?
C31 C32 H32 119.4 . . ?
C31 C32 C33 121.3(19) . . ?
C33 C32 H32 119.4 . . ?
C32 C33 H33 120.9 . . ?
C32 C33 C34 118.3(19) . . ?
C34 C33 H33 120.9 . . ?
C29 C34 C33 119.6(18) . . ?
C29 C34 C38 121.1(17) . . ?
C33 C34 C38 119.2(18) . . ?
C30 C35 H35 106.6 . . ?
C36 C35 C30 115.2(17) . . ?
C36 C35 H35 106.6 . . ?
C36 C35 C37 112(2) . . ?
C37 C35 C30 109.1(16) . . ?
C37 C35 H35 106.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38 109.0 . . ?
C39 C38 C34 110.4(18) . . ?
C39 C38 H38 109.0 . . ?
C39 C38 C40 109(2) . . ?
C40 C38 C34 110.5(18) . . ?
C40 C38 H38 109.0 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N4 C41 C42 121.0(16) . . ?
N4 C41 C46 120.0(16) . . ?
C42 C41 C46 118.9(16) . . ?
C41 C42 C50 120.4(15) . . ?
C43 C42 C41 120.4(17) . . ?
C43 C42 C50 119.1(17) . . ?
C42 C43 H43 120.5 . . ?
C44 C43 C42 119.0(19) . . ?
C44 C43 H43 120.5 . . ?
C43 C44 H44 119.3 . . ?
C45 C44 C43 121.5(18) . . ?
C45 C44 H44 119.3 . . ?
C44 C45 H45 119.0 . . ?
C44 C45 C46 122.0(19) . . ?
C46 C45 H45 119.0 . . ?
C41 C46 C47 119.8(16) . . ?
C45 C46 C41 118.2(18) . . ?
C45 C46 C47 121.9(17) . . ?
C46 C47 H47 107.2 . . ?
C46 C47 C48 114.9(17) . . ?
C46 C47 C49 109.7(15) . . ?
C48 C47 H47 107.2 . . ?
C49 C47 H47 107.2 . . ?
C49 C47 C48 110.2(16) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C42 C50 H50 105.8 . . ?
C42 C50 C51 112.3(16) . . ?
C51 C50 H50 105.8 . . ?
C52 C50 C42 114.2(16) . . ?
C52 C50 H50 105.8 . . ?
C52 C50 C51 112.0(18) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O3 C53 H53A 111.2 . . ?
O3 C53 H53B 111.2 . . ?
O3 C53 C54 103.0(14) . . ?
H53A C53 H53B 109.1 . . ?
C54 C53 H53A 111.2 . . ?
C54 C53 H53B 111.2 . . ?
C53 C54 H54A 110.7 . . ?
C53 C54 H54B 110.7 . . ?
C53 C54 C55 105.0(15) . . ?
H54A C54 H54B 108.8 . . ?
C55 C54 H54A 110.7 . . ?
C55 C54 H54B 110.7 . . ?
C54 C55 H55A 111.9 . . ?
C54 C55 H55B 111.9 . . ?
H55A C55 H55B 109.6 . . ?
C56 C55 C54 99.4(14) . . ?
C56 C55 H55A 111.9 . . ?
C56 C55 H55B 111.9 . . ?
O3 C56 C55 107.5(14) . . ?
O3 C56 H56A 110.2 . . ?
O3 C56 H56B 110.2 . . ?
C55 C56 H56A 110.2 . . ?
C55 C56 H56B 110.2 . . ?
H56A C56 H56B 108.5 . . ?
O4 C57 H57A 110.6 . . ?
O4 C57 H57B 110.6 . . ?
O4 C57 C58 105.7(16) . . ?
H57A C57 H57B 108.7 . . ?
C58 C57 H57A 110.6 . . ?
C58 C57 H57B 110.6 . . ?
C57 C58 H58A 111.4 . . ?
C57 C58 H58B 111.4 . . ?
H58A C58 H58B 109.2 . . ?
C59 C58 C57 102.0(15) . . ?
C59 C58 H58A 111.4 . . ?
C59 C58 H58B 111.4 . . ?
C58 C59 H59A 110.9 . . ?
C58 C59 H59B 110.9 . . ?
C58 C59 C60 104.3(15) . . ?
H59A C59 H59B 108.9 . . ?
C60 C59 H59A 110.9 . . ?
C60 C59 H59B 110.9 . . ?
O4 C60 C59 106.2(15) . . ?
O4 C60 H60A 110.5 . . ?
O4 C60 H60B 110.5 . . ?
C59 C60 H60A 110.5 . . ?
C59 C60 H60B 110.5 . . ?
H60A C60 H60B 108.7 . . ?
O1 B1 N1 128.8(15) . . ?
O1 B1 N2 127.0(15) . . ?
N1 B1 N2 104.1(14) . . ?
O2 B2 N3 129.0(16) . . ?
O2 B2 N4 127.9(16) . . ?
N4 B2 N3 103.0(13) . . ?
Dy1 B3 H3A 68(6) . . ?
Dy1 B3 H3B 68(6) . . ?
Dy1 B3 H3C 75(6) . . ?
Dy1 B3 H3D 176(6) . . ?
H3A B3 H3B 109.4(10) . . ?
H3A B3 H3C 109.5(10) . . ?
H3A B3 H3D 109.5(10) . . ?
H3B B3 H3C 109.4(10) . . ?
H3B B3 H3D 109.4(10) . . ?
H3C B3 H3D 109.6(10) . . ?
C62 C61 H61 122.0 . . ?
C62 C61 C66 116(3) . . ?
C66 C61 H61 122.0 . . ?
C61 C62 H62 119.5 . . ?
C61 C62 C63 121(3) . . ?
C63 C62 H62 119.5 . . ?
C62 C63 H63 119.3 . . ?
C62 C63 C64 121(3) . . ?
C64 C63 H63 119.3 . . ?
C63 C64 H64 121.7 . . ?
C65 C64 C63 117(3) . . ?
C65 C64 H64 121.7 . . ?
C64 C65 H65 118.9 . . ?
C66 C65 C64 122(3) . . ?
C66 C65 H65 118.9 . . ?
C61 C66 H66 118.7 . . ?
C65 C66 C61 123(3) . . ?
C65 C66 H66 118.7 . . ?
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 2.113(11) . ?
Dy1 O2 2.089(10) . ?
Dy1 O3 2.381(10) . ?
Dy1 O4 2.372(10) . ?
Dy1 B3 2.56(2) . ?
Dy1 H3A 2.39(11) . ?
Dy1 H3B 2.39(11) . ?
Dy1 H3C 2.50(11) . ?
O1 B1 1.34(2) . ?
O2 B2 1.33(2) . ?
O3 C53 1.47(2) . ?
O3 C56 1.45(2) . ?
O4 C57 1.45(2) . ?
O4 C60 1.46(2) . ?
N1 C1 1.41(2) . ?
N1 C15 1.45(2) . ?
N1 B1 1.44(2) . ?
N2 C2 1.41(2) . ?
N2 C3 1.402(19) . ?
N2 B1 1.49(2) . ?
N3 C28 1.40(2) . ?
N3 C29 1.42(2) . ?
N3 B2 1.47(2) . ?
N4 C27 1.43(2) . ?
N4 C41 1.37(2) . ?
N4 B2 1.46(2) . ?
C1 H1 0.9500 . ?
C1 C2 1.36(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.47(2) . ?
C3 C8 1.43(2) . ?
C4 C5 1.38(2) . ?
C4 C9 1.49(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.34(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.39(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.41(2) . ?
C8 C12 1.50(2) . ?
C9 H9 1.0000 . ?
C9 C10 1.55(2) . ?
C9 C11 1.52(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12 1.0000 . ?
C12 C13 1.54(3) . ?
C12 C14 1.53(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.40(2) . ?
C15 C20 1.41(2) . ?
C16 C17 1.41(2) . ?
C16 C21 1.57(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.35(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.43(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.41(3) . ?
C20 C24 1.50(3) . ?
C21 H21 1.0000 . ?
C21 C22 1.55(2) . ?
C21 C23 1.49(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24 1.0000 . ?
C24 C25 1.50(3) . ?
C24 C26 1.55(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 0.9500 . ?
C27 C28 1.30(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.42(2) . ?
C29 C34 1.35(3) . ?
C30 C31 1.39(3) . ?
C30 C35 1.57(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.34(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.40(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.43(3) . ?
C34 C38 1.59(3) . ?
C35 H35 1.0000 . ?
C35 C36 1.44(3) . ?
C35 C37 1.53(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38 1.0000 . ?
C38 C39 1.51(3) . ?
C38 C40 1.54(3) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.43(3) . ?
C41 C46 1.44(2) . ?
C42 C43 1.41(2) . ?
C42 C50 1.51(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.41(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.35(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.42(3) . ?
C46 C47 1.49(3) . ?
C47 H47 1.0000 . ?
C47 C48 1.53(2) . ?
C47 C49 1.51(2) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50 1.0000 . ?
C50 C51 1.53(3) . ?
C50 C52 1.47(3) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.49(2) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C55 1.52(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.50(2) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.52(2) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.52(3) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.52(2) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
B3 H3A 1.050(10) . ?
B3 H3B 1.051(10) . ?
B3 H3C 1.049(10) . ?
B3 H3D 1.050(10) . ?
C61 H61 0.9500 . ?
C61 C62 1.36(3) . ?
C61 C66 1.42(3) . ?
C62 H62 0.9500 . ?
C62 C63 1.38(4) . ?
C63 H63 0.9500 . ?
C63 C64 1.39(4) . ?
C64 H64 0.9500 . ?
C64 C65 1.37(3) . ?
C65 H65 0.9500 . ?
C65 C66 1.32(3) . ?
C66 H66 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
Dy1 O3 C53 C54 175.2(10) . . . . ?
Dy1 O3 C56 C55 161.2(10) . . . . ?
Dy1 O4 C57 C58 170.6(11) . . . . ?
Dy1 O4 C60 C59 169.5(11) . . . . ?
O3 C53 C54 C55 34.8(18) . . . . ?
O4 C57 C58 C59 34(2) . . . . ?
N1 C1 C2 N2 -1.5(19) . . . . ?
N1 C15 C16 C17 179.7(16) . . . . ?
N1 C15 C16 C21 -1(2) . . . . ?
N1 C15 C20 C19 -179.6(16) . . . . ?
N1 C15 C20 C24 -4(3) . . . . ?
N2 C3 C4 C5 -177.2(14) . . . . ?
N2 C3 C4 C9 -4(2) . . . . ?
N2 C3 C8 C7 177.7(15) . . . . ?
N2 C3 C8 C12 -5(2) . . . . ?
N3 C29 C30 C31 179.5(15) . . . . ?
N3 C29 C30 C35 -5(2) . . . . ?
N3 C29 C34 C33 -179.4(16) . . . . ?
N3 C29 C34 C38 5(3) . . . . ?
N4 C27 C28 N3 2(2) . . . . ?
N4 C41 C42 C43 177.3(15) . . . . ?
N4 C41 C42 C50 -2(3) . . . . ?
N4 C41 C46 C45 -178.9(15) . . . . ?
N4 C41 C46 C47 -3(2) . . . . ?
C1 N1 C15 C16 -85(2) . . . . ?
C1 N1 C15 C20 96(2) . . . . ?
C1 N1 B1 O1 176.2(17) . . . . ?
C1 N1 B1 N2 -1.0(18) . . . . ?
C2 N2 C3 C4 111.3(17) . . . . ?
C2 N2 C3 C8 -64(2) . . . . ?
C2 N2 B1 O1 -177.2(17) . . . . ?
C2 N2 B1 N1 0.1(17) . . . . ?
C3 N2 C2 C1 -175.2(14) . . . . ?
C3 N2 B1 O1 -2(3) . . . . ?
C3 N2 B1 N1 175.5(15) . . . . ?
C3 C4 C5 C6 1(2) . . . . ?
C3 C4 C9 C10 162.6(13) . . . . ?
C3 C4 C9 C11 -73.8(17) . . . . ?
C3 C8 C12 C13 -123.2(19) . . . . ?
C3 C8 C12 C14 114.8(19) . . . . ?
C4 C3 C8 C7 2(2) . . . . ?
C4 C3 C8 C12 179.6(15) . . . . ?
C4 C5 C6 C7 -1(3) . . . . ?
C5 C4 C9 C10 -24(2) . . . . ?
C5 C4 C9 C11 99.3(18) . . . . ?
C5 C6 C7 C8 1(3) . . . . ?
C6 C7 C8 C3 -2(3) . . . . ?
C6 C7 C8 C12 -179.2(17) . . . . ?
C7 C8 C12 C13 54(2) . . . . ?
C7 C8 C12 C14 -68(2) . . . . ?
C8 C3 C4 C5 -2(2) . . . . ?
C8 C3 C4 C9 171.8(14) . . . . ?
C9 C4 C5 C6 -171.9(15) . . . . ?
C15 N1 C1 C2 164.9(15) . . . . ?
C15 N1 B1 O1 16(3) . . . . ?
C15 N1 B1 N2 -161.7(15) . . . . ?
C15 C16 C17 C18 -1(3) . . . . ?
C15 C16 C21 C22 130.5(18) . . . . ?
C15 C16 C21 C23 -108.3(19) . . . . ?
C15 C20 C24 C25 -95(2) . . . . ?
C15 C20 C24 C26 140.0(19) . . . . ?
C16 C15 C20 C19 1(3) . . . . ?
C16 C15 C20 C24 177.1(18) . . . . ?
C16 C17 C18 C19 3(3) . . . . ?
C17 C16 C21 C22 -50(2) . . . . ?
C17 C16 C21 C23 71(2) . . . . ?
C17 C18 C19 C20 -3(3) . . . . ?
C18 C19 C20 C15 1(3) . . . . ?
C18 C19 C20 C24 -175.1(18) . . . . ?
C19 C20 C24 C25 80(2) . . . . ?
C19 C20 C24 C26 -44(3) . . . . ?
C20 C15 C16 C17 -1(3) . . . . ?
C20 C15 C16 C21 178.6(17) . . . . ?
C21 C16 C17 C18 179.2(17) . . . . ?
C27 N4 C41 C42 -71(2) . . . . ?
C27 N4 C41 C46 106.5(19) . . . . ?
C27 N4 B2 O2 -177.1(18) . . . . ?
C27 N4 B2 N3 -0.2(18) . . . . ?
C28 N3 C29 C30 -77(2) . . . . ?
C28 N3 C29 C34 100(2) . . . . ?
C28 N3 B2 O2 178.2(18) . . . . ?
C28 N3 B2 N4 1.4(18) . . . . ?
C29 N3 C28 C27 171.0(16) . . . . ?
C29 N3 B2 O2 5(3) . . . . ?
C29 N3 B2 N4 -171.3(16) . . . . ?
C29 C30 C31 C32 -2(3) . . . . ?
C29 C30 C35 C36 -111(2) . . . . ?
C29 C30 C35 C37 122(2) . . . . ?
C29 C34 C38 C39 105(2) . . . . ?
C29 C34 C38 C40 -134(2) . . . . ?
C30 C29 C34 C33 -3(3) . . . . ?
C30 C29 C34 C38 -178.3(17) . . . . ?
C30 C31 C32 C33 1(3) . . . . ?
C31 C30 C35 C36 64(2) . . . . ?
C31 C30 C35 C37 -63(2) . . . . ?
C31 C32 C33 C34 -1(3) . . . . ?
C32 C33 C34 C29 2(3) . . . . ?
C32 C33 C34 C38 177.4(18) . . . . ?
C33 C34 C38 C39 -70(3) . . . . ?
C33 C34 C38 C40 50(3) . . . . ?
C34 C29 C30 C31 3(3) . . . . ?
C34 C29 C30 C35 178.1(17) . . . . ?
C35 C30 C31 C32 -177.2(17) . . . . ?
C41 N4 C27 C28 -176.8(16) . . . . ?
C41 N4 B2 O2 -2(3) . . . . ?
C41 N4 B2 N3 175.0(17) . . . . ?
C41 C42 C43 C44 2(3) . . . . ?
C41 C42 C50 C51 161.0(17) . . . . ?
C41 C42 C50 C52 -70(2) . . . . ?
C41 C46 C47 C48 161.1(16) . . . . ?
C41 C46 C47 C49 -74(2) . . . . ?
C42 C41 C46 C45 -2(2) . . . . ?
C42 C41 C46 C47 173.8(15) . . . . ?
C42 C43 C44 C45 -3(3) . . . . ?
C43 C42 C50 C51 -18(2) . . . . ?
C43 C42 C50 C52 110(2) . . . . ?
C43 C44 C45 C46 1(3) . . . . ?
C44 C45 C46 C41 1(3) . . . . ?
C44 C45 C46 C47 -174.4(17) . . . . ?
C45 C46 C47 C48 -23(2) . . . . ?
C45 C46 C47 C49 101(2) . . . . ?
C46 C41 C42 C43 0(2) . . . . ?
C46 C41 C42 C50 -179.2(16) . . . . ?
C50 C42 C43 C44 -178.5(16) . . . . ?
C53 O3 C56 C55 -10.7(18) . . . . ?
C53 C54 C55 C56 -40.3(17) . . . . ?
C54 C55 C56 O3 31.0(17) . . . . ?
C56 O3 C53 C54 -14.9(18) . . . . ?
C57 O4 C60 C59 0(2) . . . . ?
C57 C58 C59 C60 -34(2) . . . . ?
C58 C59 C60 O4 22(2) . . . . ?
C60 O4 C57 C58 -22(2) . . . . ?
B1 N1 C1 C2 1.6(19) . . . . ?
B1 N1 C15 C16 74(2) . . . . ?
B1 N1 C15 C20 -105(2) . . . . ?
B1 N2 C2 C1 0.8(19) . . . . ?
B1 N2 C3 C4 -64(2) . . . . ?
B1 N2 C3 C8 121.1(19) . . . . ?
B2 N3 C28 C27 -2(2) . . . . ?
B2 N3 C29 C30 95(2) . . . . ?
B2 N3 C29 C34 -88(2) . . . . ?
B2 N4 C27 C28 -1(2) . . . . ?
B2 N4 C41 C42 115(2) . . . . ?
B2 N4 C41 C46 -68(2) . . . . ?
C61 C62 C63 C64 -2(4) . . . . ?
C62 C61 C66 C65 -1(3) . . . . ?
C62 C63 C64 C65 3(4) . . . . ?
C63 C64 C65 C66 -4(4) . . . . ?
C64 C65 C66 C61 3(4) . . . . ?
C66 C61 C62 C63 1(3) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.773(4)
2 0.227(4)
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
18.0192 -2.5079 -1.7484 -0.9985 0.0161 -0.0631
-10.4020 3.3220 21.2606 0.5939 0.7914 0.0527
12.3905 -7.3095 19.0740 -0.6401 0.6447 -0.4023
-12.7471 -5.6058 -12.1612 0.7186 -0.6795 -0.2749
-11.3524 10.2637 -18.9661 0.5708 -0.5661 0.5537
7.1538 14.7139 1.7084 -0.4545 0.4504 0.7556
-12.5914 -6.5900 20.1340 0.7533 0.5091 -0.4482
-3.4032 -0.9186 -25.3150 0.1626 -0.9950 0.0406
14.4407 -0.4282 -18.0348 -0.8267 -0.5745 0.0930
13.5646 -2.3650 16.9906 -0.7274 0.6871 -0.1420
1.5091 -18.9461 9.0318 0.0004 -0.0771 -0.9828
-14.4023 1.4216 17.0400 0.8195 0.5599 -0.0391
-1.5091 18.9461 -9.0318 -0.0004 0.0771 0.9828
-0.4621 18.9146 -10.9635 -0.0611 0.0120 0.9919
3.4032 0.9186 25.3150 -0.1626 0.9950 -0.0406
10.4020 -3.3220 -21.2606 -0.5939 -0.7914 -0.0527
17.8755 -7.4778 1.2236 -0.9676 0.0143 -0.3249
14.1817 -8.3782 -12.0784 -0.7741 -0.5325 -0.3305
-17.1786 -3.4853 4.7845 0.9786 -0.0310 -0.2473
4.3065 -4.0829 26.3552 -0.1923 0.9281 -0.2933
-18.0192 2.5079 1.7484 0.9985 -0.0161 0.0631
