#------------------------------------------------------------------------------
#$Date: 2024-04-05 01:45:28 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290838 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/08/1570823.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_1570823
loop_
_publ_author_name
'Rieser, Theresa E.'
'Schädle, Dorothea'
'Maichle-Mössmer, Cäcilia'
'Anwander, Reiner'
_publ_section_title
;
 Terminal dysprosium and holmium organoimides.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              3562
_journal_page_last               3570
_journal_paper_doi               10.1039/d3sc06584g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C46.5 H71 B Dy N9'
_chemical_formula_weight         929.43
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-12-05 deposited with the CCDC.	2024-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.940(3)
_cell_length_b                   11.5627(7)
_cell_length_c                   19.9969(12)
_cell_measurement_reflns_used    8224
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.46
_cell_measurement_theta_min      2.31
_cell_volume                     9452.8(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5,SHELXS-13 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II DUO'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75914
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.720
_diffrn_reflns_theta_min         1.830
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       needle
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.056
_exptl_transmission_factor_max   0.7443
_exptl_transmission_factor_min   0.6574
_refine_diff_density_max         1.744
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         12234
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0275P)²+15.5748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9093
_reflns_number_total             12234
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc06584g2.cif
_cod_data_source_block           4-Dy_mo_TR123_0m
_cod_depositor_comments
'Adding full bibliography for 1570817--1570831.cif.'
_cod_original_cell_volume        9452.7(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C46.50 H71 B Dy N9'
_cod_database_code               1570823
_shelx_shelxl_version_number     2014/7
_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_min   0.799
_shelx_estimated_absorpt_t_max   0.915
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.38803(10) 0.2772(3) 0.56245(17) 0.0285(8) Uani 1 1 d . . . . .
C2 C 0.35620(10) 0.2939(3) 0.56652(18) 0.0308(9) Uani 1 1 d . . . . .
H2 H 0.3445 0.2500 0.5933 0.037 Uiso 1 1 calc R U . . .
C3 C 0.34413(8) 0.3872(3) 0.52422(17) 0.0245(8) Uani 1 1 d . . . . .
C4 C 0.31050(9) 0.4399(3) 0.51384(19) 0.0305(9) Uani 1 1 d . . . . .
C5 C 0.30071(9) 0.5089(4) 0.44777(19) 0.0372(10) Uani 1 1 d . . . . .
H5A H 0.3021 0.4593 0.4087 0.056 Uiso 1 1 calc R U . . .
H5B H 0.3155 0.5749 0.4494 0.056 Uiso 1 1 calc R U . . .
H5C H 0.2782 0.5369 0.4425 0.056 Uiso 1 1 calc R U . . .
C6 C 0.30995(10) 0.5198(4) 0.5749(2) 0.0405(10) Uani 1 1 d . . . . .
H6A H 0.3256 0.5830 0.5757 0.061 Uiso 1 1 calc R U . . .
H6B H 0.3160 0.4756 0.6177 0.061 Uiso 1 1 calc R U . . .
H6C H 0.2879 0.5518 0.5703 0.061 Uiso 1 1 calc R U . . .
C7 C 0.28540(10) 0.3420(4) 0.5126(2) 0.0515(12) Uani 1 1 d . . . . .
H7A H 0.2634 0.3751 0.5051 0.077 Uiso 1 1 calc R U . . .
H7B H 0.2904 0.3008 0.5565 0.077 Uiso 1 1 calc R U . . .
H7C H 0.2865 0.2881 0.4754 0.077 Uiso 1 1 calc R U . . .
C8 C 0.41144(11) 0.1862(3) 0.5956(2) 0.0395(10) Uani 1 1 d . . . . .
H8A H 0.4005 0.1340 0.6219 0.059 Uiso 1 1 calc R U . . .
H8B H 0.4302 0.2226 0.6263 0.059 Uiso 1 1 calc R U . . .
H8C H 0.4190 0.1421 0.5602 0.059 Uiso 1 1 calc R U . . .
C9 C 0.41903(7) 0.4166(3) 0.31070(15) 0.0175(6) Uani 1 1 d . . . . .
C10 C 0.42319(8) 0.2967(3) 0.31300(17) 0.0226(7) Uani 1 1 d . . . . .
H10 H 0.4244 0.2471 0.2758 0.027 Uiso 1 1 calc R U . . .
C11 C 0.42523(8) 0.2651(3) 0.38043(17) 0.0202(7) Uani 1 1 d . . . . .
C12 C 0.41647(8) 0.4947(3) 0.24888(17) 0.0211(7) Uani 1 1 d . . . . .
C13 C 0.44930(9) 0.4950(3) 0.2272(2) 0.0331(9) Uani 1 1 d . . . . .
H13A H 0.4549 0.4158 0.2166 0.050 Uiso 1 1 calc R U . . .
H13B H 0.4664 0.5256 0.2647 0.050 Uiso 1 1 calc R U . . .
H13C H 0.4476 0.5437 0.1865 0.050 Uiso 1 1 calc R U . . .
C14 C 0.38991(10) 0.4489(3) 0.18890(19) 0.0339(9) Uani 1 1 d . . . . .
H14A H 0.3882 0.5000 0.1492 0.051 Uiso 1 1 calc R U . . .
H14B H 0.3689 0.4468 0.2025 0.051 Uiso 1 1 calc R U . . .
H14C H 0.3957 0.3707 0.1769 0.051 Uiso 1 1 calc R U . . .
C15 C 0.40800(9) 0.6181(3) 0.26544(18) 0.0265(8) Uani 1 1 d . . . . .
H15A H 0.4077 0.6678 0.2256 0.040 Uiso 1 1 calc R U . . .
H15B H 0.4244 0.6466 0.3048 0.040 Uiso 1 1 calc R U . . .
H15C H 0.3864 0.6192 0.2766 0.040 Uiso 1 1 calc R U . . .
C16 C 0.42867(9) 0.1473(3) 0.41172(18) 0.0261(8) Uani 1 1 d . . . . .
H16A H 0.4331 0.0911 0.3782 0.039 Uiso 1 1 calc R U . . .
H16B H 0.4084 0.1263 0.4253 0.039 Uiso 1 1 calc R U . . .
H16C H 0.4468 0.1470 0.4522 0.039 Uiso 1 1 calc R U . . .
C17 C 0.45458(8) 0.6716(3) 0.53224(16) 0.0191(7) Uani 1 1 d . . . . .
C18 C 0.48243(8) 0.6147(3) 0.56950(17) 0.0218(7) Uani 1 1 d . . . . .
H18 H 0.5019 0.6497 0.5950 0.026 Uiso 1 1 calc R U . . .
C19 C 0.47602(8) 0.4981(3) 0.56178(16) 0.0208(7) Uani 1 1 d . . . . .
C20 C 0.44883(8) 0.7997(3) 0.52106(19) 0.0270(8) Uani 1 1 d . . . . .
C21 C 0.42253(9) 0.8389(3) 0.5578(2) 0.0335(9) Uani 1 1 d . . . . .
H21A H 0.4185 0.9219 0.5502 0.050 Uiso 1 1 calc R U . . .
H21B H 0.4299 0.8240 0.6071 0.050 Uiso 1 1 calc R U . . .
H21C H 0.4023 0.7961 0.5398 0.050 Uiso 1 1 calc R U . . .
C22 C 0.43746(9) 0.8265(3) 0.44390(19) 0.0295(8) Uani 1 1 d . . . . .
H22A H 0.4537 0.7976 0.4196 0.044 Uiso 1 1 calc R U . . .
H22B H 0.4350 0.9103 0.4373 0.044 Uiso 1 1 calc R U . . .
H22C H 0.4164 0.7887 0.4257 0.044 Uiso 1 1 calc R U . . .
C23 C 0.48056(9) 0.8661(3) 0.5489(2) 0.0393(10) Uani 1 1 d . . . . .
H23A H 0.4973 0.8416 0.5246 0.059 Uiso 1 1 calc R U . . .
H23B H 0.4882 0.8502 0.5980 0.059 Uiso 1 1 calc R U . . .
H23C H 0.4766 0.9492 0.5420 0.059 Uiso 1 1 calc R U . . .
C24 C 0.49777(8) 0.3996(3) 0.59125(17) 0.0257(8) Uani 1 1 d . . . . .
H24A H 0.4978 0.3417 0.5555 0.039 Uiso 1 1 calc R U . . .
H24B H 0.4897 0.3643 0.6288 0.039 Uiso 1 1 calc R U . . .
H24C H 0.5201 0.4282 0.6087 0.039 Uiso 1 1 calc R U . . .
C25 C 0.34992(8) 0.8534(3) 0.41806(17) 0.0208(7) Uani 1 1 d . . . . .
C26 C 0.34001(8) 0.9085(3) 0.47496(17) 0.0240(7) Uani 1 1 d . . . . .
C27 C 0.33483(9) 1.0264(3) 0.47435(19) 0.0289(8) Uani 1 1 d . . . . .
H27 H 0.3288 1.0607 0.5129 0.035 Uiso 1 1 calc R U . . .
C28 C 0.33801(9) 1.0971(3) 0.42054(19) 0.0309(8) Uani 1 1 d . . . . .
H28 H 0.3347 1.1782 0.4221 0.037 Uiso 1 1 calc R U . . .
C29 C 0.34625(9) 1.0449(3) 0.36406(19) 0.0289(8) Uani 1 1 d . . . . .
H29 H 0.3481 1.0915 0.3260 0.035 Uiso 1 1 calc R U . . .
C30 C 0.35191(8) 0.9271(3) 0.36151(16) 0.0222(7) Uani 1 1 d . . . . .
C31 C 0.33291(9) 0.8363(3) 0.53272(18) 0.0291(8) Uani 1 1 d . . . . .
H31 H 0.3437 0.7594 0.5313 0.035 Uiso 1 1 calc R U . . .
C32 C 0.34567(11) 0.8872(4) 0.6045(2) 0.0456(11) Uani 1 1 d . . . . .
H32A H 0.3688 0.9081 0.6102 0.068 Uiso 1 1 calc R U . . .
H32B H 0.3434 0.8297 0.6391 0.068 Uiso 1 1 calc R U . . .
H32C H 0.3330 0.9563 0.6100 0.068 Uiso 1 1 calc R U . . .
C33 C 0.29595(10) 0.8153(4) 0.5218(2) 0.0447(11) Uani 1 1 d . . . . .
H33A H 0.2847 0.8893 0.5231 0.067 Uiso 1 1 calc R U . . .
H33B H 0.2917 0.7648 0.5582 0.067 Uiso 1 1 calc R U . . .
H33C H 0.2878 0.7783 0.4771 0.067 Uiso 1 1 calc R U . . .
C34 C 0.35848(9) 0.8753(3) 0.29607(18) 0.0286(8) Uani 1 1 d . . . . .
H34 H 0.3645 0.7924 0.3058 0.034 Uiso 1 1 calc R U . . .
C35 C 0.32729(10) 0.8775(4) 0.23842(19) 0.0400(10) Uani 1 1 d . . . . .
H35A H 0.3312 0.8354 0.1985 0.060 Uiso 1 1 calc R U . . .
H35B H 0.3214 0.9577 0.2255 0.060 Uiso 1 1 calc R U . . .
H35C H 0.3094 0.8406 0.2545 0.060 Uiso 1 1 calc R U . . .
C36 C 0.38668(10) 0.9326(3) 0.2723(2) 0.0376(10) Uani 1 1 d . . . . .
H36A H 0.3901 0.8938 0.2309 0.056 Uiso 1 1 calc R U . . .
H36B H 0.4066 0.9267 0.3086 0.056 Uiso 1 1 calc R U . . .
H36C H 0.3815 1.0143 0.2622 0.056 Uiso 1 1 calc R U . . .
C37 C 0.33672(9) 0.3809(3) 0.31175(18) 0.0266(8) Uani 1 1 d . . . . .
H37 H 0.3530 0.3299 0.3361 0.032 Uiso 1 1 calc R U . . .
C38 C 0.31013(9) 0.3332(3) 0.26746(19) 0.0309(8) Uani 1 1 d . . . . .
H38 H 0.3082 0.2517 0.2623 0.037 Uiso 1 1 calc R U . . .
C39 C 0.28570(8) 0.4063(4) 0.22985(18) 0.0329(9) Uani 1 1 d . . . . .
C40 C 0.29093(9) 0.5254(4) 0.23997(18) 0.0316(9) Uani 1 1 d . . . . .
H40 H 0.2757 0.5792 0.2150 0.038 Uiso 1 1 calc R U . . .
C41 C 0.31782(9) 0.5638(3) 0.28549(18) 0.0273(8) Uani 1 1 d . . . . .
H41 H 0.3204 0.6450 0.2915 0.033 Uiso 1 1 calc R U . . .
C42 C 0.23350(10) 0.4471(5) 0.1518(2) 0.0652(16) Uani 1 1 d . . . . .
H42A H 0.2426 0.4955 0.1203 0.098 Uiso 1 1 calc R U . . .
H42B H 0.2266 0.4964 0.1859 0.098 Uiso 1 1 calc R U . . .
H42C H 0.2146 0.4040 0.1259 0.098 Uiso 1 1 calc R U . . .
C43 C 0.25248(13) 0.2439(5) 0.1804(2) 0.0710(17) Uani 1 1 d . . . . .
H43A H 0.2307 0.2303 0.1511 0.106 Uiso 1 1 calc R U . . .
H43B H 0.2535 0.2107 0.2259 0.106 Uiso 1 1 calc R U . . .
H43C H 0.2691 0.2073 0.1598 0.106 Uiso 1 1 calc R U . . .
C44 C 0.5000 1.0688(6) 0.2500 0.0667(18) Uani 1 2 d DS TU P . .
C45 C 0.52337(17) 0.9978(5) 0.2360(3) 0.0879(17) Uani 1 1 d D U . . .
H45A H 0.5427 1.0339 0.2288 0.105 Uiso 1 1 calc R U . . .
C46 C 0.5222(2) 0.8744(5) 0.2309(4) 0.110(2) Uani 1 1 d D U . . .
H46 H 0.5385 0.8362 0.2127 0.132 Uiso 1 1 calc R U . . .
C47 C 0.5000 0.8120(8) 0.2500 0.090(2) Uani 1 2 d DS TU P . .
H47 H 0.5000 0.7298 0.2500 0.108 Uiso 1 2 calc R U P . .
C48 C 0.5000 1.1955(6) 0.2500 0.0559(17) Uani 1 2 d S TU P . .
H48A H 0.4785 1.2238 0.2257 0.084 Uiso 0.5 1 calc R U P . .
H48B H 0.5168 1.2238 0.2269 0.084 Uiso 0.5 1 calc R U P . .
H48C H 0.5047 1.2238 0.2974 0.084 Uiso 0.5 1 calc R U P . .
N1 N 0.39516(7) 0.3594(2) 0.51921(14) 0.0219(6) Uani 1 1 d . . . . .
N2 N 0.36808(7) 0.4285(2) 0.49523(14) 0.0220(6) Uani 1 1 d . . . . .
N3 N 0.42263(6) 0.3625(2) 0.41664(14) 0.0189(6) Uani 1 1 d . . . . .
N4 N 0.41841(7) 0.4573(2) 0.37290(13) 0.0184(6) Uani 1 1 d . . . . .
N5 N 0.44575(7) 0.4854(2) 0.52235(13) 0.0194(6) Uani 1 1 d . . . . .
N6 N 0.43206(6) 0.5927(2) 0.50334(13) 0.0190(6) Uani 1 1 d . . . . .
N7 N 0.35748(6) 0.7381(2) 0.41912(13) 0.0207(6) Uani 1 1 d . . . . .
N8 N 0.34111(7) 0.4952(2) 0.32283(14) 0.0214(6) Uani 1 1 d . . . . .
N9 N 0.25853(8) 0.3657(4) 0.18674(17) 0.0468(10) Uani 1 1 d . . . . .
B1 B 0.42791(9) 0.3722(3) 0.4961(2) 0.0206(8) Uani 1 1 d . . . . .
H1 H 0.4432(7) 0.300(3) 0.5200(15) 0.011(8) Uiso 1 1 d . . . . .
Dy1 Dy 0.37955(2) 0.58296(2) 0.41997(2) 0.01759(5) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
N N 0.0061 0.0033 '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'
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 C2 107.1(3) . . ?
N1 C1 C8 123.9(3) . . ?
C2 C1 C8 128.9(3) . . ?
C1 C2 C3 107.5(3) . . ?
C1 C2 H2 126.3 . . ?
C3 C2 H2 126.3 . . ?
N2 C3 C2 109.2(3) . . ?
N2 C3 C4 124.0(3) . . ?
C2 C3 C4 126.7(3) . . ?
C3 C4 C5 113.2(3) . . ?
C3 C4 C6 108.2(3) . . ?
C5 C4 C6 109.1(3) . . ?
C3 C4 C7 108.7(3) . . ?
C5 C4 C7 108.7(3) . . ?
C6 C4 C7 108.9(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C1 C8 H8A 109.5 . . ?
C1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 110.3(3) . . ?
N4 C9 C12 122.5(3) . . ?
C10 C9 C12 127.2(3) . . ?
C11 C10 C9 106.0(3) . . ?
C11 C10 H10 127.0 . . ?
C9 C10 H10 127.0 . . ?
N3 C11 C10 107.8(3) . . ?
N3 C11 C16 123.1(3) . . ?
C10 C11 C16 129.1(3) . . ?
C9 C12 C15 111.0(3) . . ?
C9 C12 C13 109.1(3) . . ?
C15 C12 C13 109.1(3) . . ?
C9 C12 C14 109.8(3) . . ?
C15 C12 C14 109.2(3) . . ?
C13 C12 C14 108.7(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 C18 109.4(3) . . ?
N6 C17 C20 121.8(3) . . ?
C18 C17 C20 128.8(3) . . ?
C19 C18 C17 106.3(3) . . ?
C19 C18 H18 126.8 . . ?
C17 C18 H18 126.8 . . ?
N5 C19 C18 108.0(3) . . ?
N5 C19 C24 124.1(3) . . ?
C18 C19 C24 127.9(3) . . ?
C17 C20 C21 109.2(3) . . ?
C17 C20 C23 110.0(3) . . ?
C21 C20 C23 109.8(3) . . ?
C17 C20 C22 110.5(3) . . ?
C21 C20 C22 109.1(3) . . ?
C23 C20 C22 108.2(3) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N7 C25 C30 122.5(3) . . ?
N7 C25 C26 121.6(3) . . ?
C30 C25 C26 116.0(3) . . ?
C27 C26 C25 120.1(3) . . ?
C27 C26 C31 119.7(3) . . ?
C25 C26 C31 120.0(3) . . ?
C26 C27 C28 123.3(3) . . ?
C26 C27 H27 118.3 . . ?
C28 C27 H27 118.3 . . ?
C27 C28 C29 117.4(3) . . ?
C27 C28 H28 121.3 . . ?
C29 C28 H28 121.3 . . ?
C30 C29 C28 122.1(3) . . ?
C30 C29 H29 118.9 . . ?
C28 C29 H29 118.9 . . ?
C29 C30 C25 121.0(3) . . ?
C29 C30 C34 119.0(3) . . ?
C25 C30 C34 120.0(3) . . ?
C26 C31 C32 114.7(3) . . ?
C26 C31 C33 110.1(3) . . ?
C32 C31 C33 108.9(3) . . ?
C26 C31 H31 107.6 . . ?
C32 C31 H31 107.6 . . ?
C33 C31 H31 107.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 C36 113.6(3) . . ?
C30 C34 C35 110.6(3) . . ?
C36 C34 C35 110.4(3) . . ?
C30 C34 H34 107.3 . . ?
C36 C34 H34 107.3 . . ?
C35 C34 H34 107.3 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N8 C37 C38 124.1(3) . . ?
N8 C37 H37 117.9 . . ?
C38 C37 H37 117.9 . . ?
C37 C38 C39 119.5(4) . . ?
C37 C38 H38 120.3 . . ?
C39 C38 H38 120.3 . . ?
N9 C39 C40 121.1(4) . . ?
N9 C39 C38 122.8(4) . . ?
C40 C39 C38 116.1(3) . . ?
C41 C40 C39 119.8(4) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
N8 C41 C40 124.8(4) . . ?
N8 C41 H41 117.6 . . ?
C40 C41 H41 117.6 . . ?
N9 C42 H42A 109.5 . . ?
N9 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N9 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C43 H43A 109.5 . . ?
N9 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N9 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C45 105.4(8) . 2_655 ?
C45 C44 C48 127.3(4) . . ?
C45 C44 C48 127.3(4) 2_655 . ?
C44 C45 C46 127.2(7) . . ?
C44 C45 H45A 116.4 . . ?
C46 C45 H45A 116.4 . . ?
C47 C46 C45 123.2(8) . . ?
C47 C46 H46 118.4 . . ?
C45 C46 H46 118.4 . . ?
C46 C47 C46 112.6(10) . 2_655 ?
C46 C47 H47 123.7 . . ?
C46 C47 H47 123.7 2_655 . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C1 N1 N2 110.1(3) . . ?
C1 N1 B1 126.2(3) . . ?
N2 N1 B1 123.7(3) . . ?
C3 N2 N1 106.2(3) . . ?
C3 N2 Dy1 141.8(2) . . ?
N1 N2 Dy1 112.01(19) . . ?
C11 N3 N4 109.5(3) . . ?
C11 N3 B1 126.5(3) . . ?
N4 N3 B1 123.6(3) . . ?
C9 N4 N3 106.4(3) . . ?
C9 N4 Dy1 134.5(2) . . ?
N3 N4 Dy1 102.85(18) . . ?
C19 N5 N6 110.0(3) . . ?
C19 N5 B1 128.0(3) . . ?
N6 N5 B1 121.9(3) . . ?
C17 N6 N5 106.3(2) . . ?
C17 N6 Dy1 139.5(2) . . ?
N5 N6 Dy1 113.58(18) . . ?
C25 N7 Dy1 166.0(2) . . ?
C37 N8 C41 115.5(3) . . ?
C37 N8 Dy1 125.4(2) . . ?
C41 N8 Dy1 117.6(2) . . ?
C39 N9 C43 120.4(4) . . ?
C39 N9 C42 119.6(4) . . ?
C43 N9 C42 119.7(4) . . ?
N5 B1 N1 112.0(3) . . ?
N5 B1 N3 110.9(3) . . ?
N1 B1 N3 111.3(3) . . ?
N5 B1 H1 107.9(16) . . ?
N1 B1 H1 105.6(16) . . ?
N3 B1 H1 108.9(16) . . ?
N7 Dy1 N6 107.81(10) . . ?
N7 Dy1 N8 98.18(10) . . ?
N6 Dy1 N8 152.99(9) . . ?
N7 Dy1 N2 120.04(10) . . ?
N6 Dy1 N2 83.43(9) . . ?
N8 Dy1 N2 90.02(9) . . ?
N7 Dy1 N4 147.59(10) . . ?
N6 Dy1 N4 73.88(9) . . ?
N8 Dy1 N4 80.27(9) . . ?
N2 Dy1 N4 92.37(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
C1 N1 1.363(4) . ?
C1 C2 1.369(5) . ?
C1 C8 1.490(5) . ?
C2 C3 1.395(5) . ?
C2 H2 0.9500 . ?
C3 N2 1.353(4) . ?
C3 C4 1.507(5) . ?
C4 C5 1.519(5) . ?
C4 C6 1.535(5) . ?
C4 C7 1.541(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.335(4) . ?
C9 C10 1.397(4) . ?
C9 C12 1.515(4) . ?
C10 C11 1.381(4) . ?
C10 H10 0.9500 . ?
C11 N3 1.356(4) . ?
C11 C16 1.492(4) . ?
C12 C15 1.524(5) . ?
C12 C13 1.533(5) . ?
C12 C14 1.537(5) . ?
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 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N6 1.347(4) . ?
C17 C18 1.401(4) . ?
C17 C20 1.509(5) . ?
C18 C19 1.377(5) . ?
C18 H18 0.9500 . ?
C19 N5 1.345(4) . ?
C19 C24 1.496(4) . ?
C20 C21 1.524(5) . ?
C20 C23 1.530(5) . ?
C20 C22 1.541(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
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 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N7 1.369(4) . ?
C25 C30 1.433(5) . ?
C25 C26 1.443(5) . ?
C26 C27 1.380(5) . ?
C26 C31 1.507(5) . ?
C27 C28 1.381(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.386(5) . ?
C29 H29 0.9500 . ?
C30 C34 1.519(5) . ?
C31 C32 1.532(5) . ?
C31 C33 1.536(5) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.521(5) . ?
C34 C35 1.539(5) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 N8 1.346(4) . ?
C37 C38 1.375(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.409(5) . ?
C38 H38 0.9500 . ?
C39 N9 1.350(4) . ?
C39 C40 1.403(5) . ?
C40 C41 1.356(5) . ?
C40 H40 0.9500 . ?
C41 N8 1.347(4) . ?
C41 H41 0.9500 . ?
C42 N9 1.466(6) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N9 1.432(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.355(6) . ?
C44 C45 1.355(6) 2_655 ?
C44 C48 1.466(9) . ?
C45 C46 1.430(7) . ?
C45 H45A 0.9500 . ?
C46 C47 1.301(7) . ?
C46 H46 0.9500 . ?
C47 C46 1.301(7) 2_655 ?
C47 H47 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N1 N2 1.384(4) . ?
N1 B1 1.551(5) . ?
N2 Dy1 2.452(3) . ?
N3 N4 1.389(4) . ?
N3 B1 1.559(5) . ?
N4 Dy1 2.517(3) . ?
N5 N6 1.385(3) . ?
N5 B1 1.540(5) . ?
N6 Dy1 2.450(3) . ?
N7 Dy1 2.017(3) . ?
N8 Dy1 2.450(3) . ?
B1 H1 1.10(3) . ?
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
N1 C1 C2 C3 0.6(4) . . . . ?
C8 C1 C2 C3 -177.5(4) . . . . ?
C1 C2 C3 N2 -0.8(4) . . . . ?
C1 C2 C3 C4 -178.0(3) . . . . ?
N2 C3 C4 C5 23.9(5) . . . . ?
C2 C3 C4 C5 -159.2(3) . . . . ?
N2 C3 C4 C6 -97.1(4) . . . . ?
C2 C3 C4 C6 79.7(4) . . . . ?
N2 C3 C4 C7 144.8(3) . . . . ?
C2 C3 C4 C7 -38.4(5) . . . . ?
N4 C9 C10 C11 -0.2(4) . . . . ?
C12 C9 C10 C11 178.1(3) . . . . ?
C9 C10 C11 N3 -0.4(4) . . . . ?
C9 C10 C11 C16 177.9(3) . . . . ?
N4 C9 C12 C15 -8.7(4) . . . . ?
C10 C9 C12 C15 173.2(3) . . . . ?
N4 C9 C12 C13 111.5(3) . . . . ?
C10 C9 C12 C13 -66.6(4) . . . . ?
N4 C9 C12 C14 -129.5(3) . . . . ?
C10 C9 C12 C14 52.4(4) . . . . ?
N6 C17 C18 C19 0.3(4) . . . . ?
C20 C17 C18 C19 -177.6(3) . . . . ?
C17 C18 C19 N5 -0.5(4) . . . . ?
C17 C18 C19 C24 -180.0(3) . . . . ?
N6 C17 C20 C21 69.7(4) . . . . ?
C18 C17 C20 C21 -112.7(4) . . . . ?
N6 C17 C20 C23 -169.8(3) . . . . ?
C18 C17 C20 C23 7.9(5) . . . . ?
N6 C17 C20 C22 -50.3(4) . . . . ?
C18 C17 C20 C22 127.3(4) . . . . ?
N7 C25 C26 C27 175.3(3) . . . . ?
C30 C25 C26 C27 -3.5(5) . . . . ?
N7 C25 C26 C31 -9.1(5) . . . . ?
C30 C25 C26 C31 172.0(3) . . . . ?
C25 C26 C27 C28 1.3(5) . . . . ?
C31 C26 C27 C28 -174.2(3) . . . . ?
C26 C27 C28 C29 1.3(6) . . . . ?
C27 C28 C29 C30 -1.5(6) . . . . ?
C28 C29 C30 C25 -0.9(5) . . . . ?
C28 C29 C30 C34 175.8(3) . . . . ?
N7 C25 C30 C29 -175.5(3) . . . . ?
C26 C25 C30 C29 3.3(5) . . . . ?
N7 C25 C30 C34 7.8(5) . . . . ?
C26 C25 C30 C34 -173.3(3) . . . . ?
C27 C26 C31 C32 -45.1(5) . . . . ?
C25 C26 C31 C32 139.3(3) . . . . ?
C27 C26 C31 C33 78.2(4) . . . . ?
C25 C26 C31 C33 -97.4(4) . . . . ?
C29 C30 C34 C36 55.0(4) . . . . ?
C25 C30 C34 C36 -128.2(3) . . . . ?
C29 C30 C34 C35 -69.8(4) . . . . ?
C25 C30 C34 C35 106.9(4) . . . . ?
N8 C37 C38 C39 0.9(6) . . . . ?
C37 C38 C39 N9 -178.3(3) . . . . ?
C37 C38 C39 C40 1.2(5) . . . . ?
N9 C39 C40 C41 177.5(3) . . . . ?
C38 C39 C40 C41 -2.0(5) . . . . ?
C39 C40 C41 N8 0.9(6) . . . . ?
C45 C44 C45 C46 5.2(5) 2_655 . . . ?
C48 C44 C45 C46 -174.8(5) . . . . ?
C44 C45 C46 C47 -11.3(12) . . . . ?
C45 C46 C47 C46 4.9(5) . . . 2_655 ?
C2 C1 N1 N2 -0.3(4) . . . . ?
C8 C1 N1 N2 177.9(3) . . . . ?
C2 C1 N1 B1 -177.3(3) . . . . ?
C8 C1 N1 B1 1.0(5) . . . . ?
C2 C3 N2 N1 0.6(4) . . . . ?
C4 C3 N2 N1 177.9(3) . . . . ?
C2 C3 N2 Dy1 -176.8(3) . . . . ?
C4 C3 N2 Dy1 0.5(6) . . . . ?
C1 N1 N2 C3 -0.2(3) . . . . ?
B1 N1 N2 C3 176.9(3) . . . . ?
C1 N1 N2 Dy1 178.1(2) . . . . ?
B1 N1 N2 Dy1 -4.8(4) . . . . ?
C10 C11 N3 N4 0.9(4) . . . . ?
C16 C11 N3 N4 -177.5(3) . . . . ?
C10 C11 N3 B1 -171.8(3) . . . . ?
C16 C11 N3 B1 9.8(5) . . . . ?
C10 C9 N4 N3 0.7(3) . . . . ?
C12 C9 N4 N3 -177.6(3) . . . . ?
C10 C9 N4 Dy1 -127.1(3) . . . . ?
C12 C9 N4 Dy1 54.5(4) . . . . ?
C11 N3 N4 C9 -1.0(3) . . . . ?
B1 N3 N4 C9 171.9(3) . . . . ?
C11 N3 N4 Dy1 143.7(2) . . . . ?
B1 N3 N4 Dy1 -43.4(3) . . . . ?
C18 C19 N5 N6 0.4(4) . . . . ?
C24 C19 N5 N6 180.0(3) . . . . ?
C18 C19 N5 B1 176.9(3) . . . . ?
C24 C19 N5 B1 -3.6(5) . . . . ?
C18 C17 N6 N5 -0.1(3) . . . . ?
C20 C17 N6 N5 178.0(3) . . . . ?
C18 C17 N6 Dy1 -170.5(2) . . . . ?
C20 C17 N6 Dy1 7.6(5) . . . . ?
C19 N5 N6 C17 -0.2(3) . . . . ?
B1 N5 N6 C17 -176.9(3) . . . . ?
C19 N5 N6 Dy1 173.0(2) . . . . ?
B1 N5 N6 Dy1 -3.7(3) . . . . ?
C30 C25 N7 Dy1 63.0(10) . . . . ?
C26 C25 N7 Dy1 -115.8(9) . . . . ?
C38 C37 N8 C41 -2.0(5) . . . . ?
C38 C37 N8 Dy1 163.5(3) . . . . ?
C40 C41 N8 C37 1.1(5) . . . . ?
C40 C41 N8 Dy1 -165.6(3) . . . . ?
C40 C39 N9 C43 -175.8(4) . . . . ?
C38 C39 N9 C43 3.6(6) . . . . ?
C40 C39 N9 C42 -2.3(6) . . . . ?
C38 C39 N9 C42 177.2(4) . . . . ?
C19 N5 B1 N1 122.1(3) . . . . ?
N6 N5 B1 N1 -61.9(4) . . . . ?
C19 N5 B1 N3 -112.9(3) . . . . ?
N6 N5 B1 N3 63.1(4) . . . . ?
C1 N1 B1 N5 -114.8(3) . . . . ?
N2 N1 B1 N5 68.6(4) . . . . ?
C1 N1 B1 N3 120.4(3) . . . . ?
N2 N1 B1 N3 -56.2(4) . . . . ?
C11 N3 B1 N5 141.1(3) . . . . ?
N4 N3 B1 N5 -30.6(4) . . . . ?
C11 N3 B1 N1 -93.5(4) . . . . ?
N4 N3 B1 N1 94.8(3) . . . . ?
