#------------------------------------------------------------------------------
#$Date: 2017-03-04 15:13:39 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193431 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/50/4345065.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_4345065
loop_
_publ_author_name
'Botezat, Olga'
'van Leusen, Jan'
'Kravtsov, Victor Ch'
'Kögerler, Paul'
'Baca, Svetlana G.'
_publ_section_title
;
 Ultralarge 3d/4f Coordination Wheels: From Carboxylate/Amino
 Alcohol-Supported {Fe4Ln2} to {Fe18Ln6} Rings.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1814
_journal_page_last               1822
_journal_paper_doi               10.1021/acs.inorgchem.6b02100
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C198 H474 Dy6 Fe18 N42 O132'
_chemical_formula_weight         7536.46
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   37.390(6)
_cell_length_b                   37.390(6)
_cell_length_c                   25.583(4)
_cell_measurement_reflns_used    7976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.08
_cell_measurement_theta_min      2.18
_cell_volume                     30974(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1296
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            107347
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.029
_exptl_absorpt_coefficient_mu    1.752
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             11628
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.115
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         12106
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0997P)²+421.1902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8915
_reflns_number_total             12106
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02100_si_011.cif
_cod_data_source_block           O361asb
_cod_depositor_comments
'Adding full bibliography for 4345065--4345072.cif.'
_cod_original_cell_volume        30974(11)
_cod_database_code               4345065
_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   0.817
_shelx_estimated_absorpt_t_max   0.873
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.80945(2) 0.11766(2) 0.33837(2) 0.01959(13) Uani 1 1 d . . . . .
Fe1 Fe 0.88188(3) 0.20970(3) 0.38709(4) 0.0163(2) Uani 1 1 d . . . . .
Fe2 Fe 0.91962(3) 0.30093(3) 0.34473(4) 0.0165(2) Uani 1 1 d . . . . .
Fe3 Fe 0.93836(3) 0.39009(3) 0.38322(4) 0.0160(2) Uani 1 1 d . . . . .
C1 C 0.7828(3) 0.0378(3) 0.4221(4) 0.057(3) Uani 1 1 d D . . . .
C2 C 0.7857(4) 0.0328(4) 0.4780(5) 0.097(5) Uani 1 1 d D U . . .
H2 H 0.7732 0.0022 0.4814 0.117 Uiso 0.52(3) 1 calc R U P A 1
H2A H 0.8123 0.0589 0.4848 0.117 Uiso 0.48(3) 1 calc R U P A 2
C3 C 0.8265(5) 0.0476(8) 0.4971(8) 0.094(11) Uani 0.52(3) 1 d D U P A 1
H3A H 0.8420 0.0406 0.4722 0.113 Uiso 0.52(3) 1 calc R U P A 1
H3B H 0.8403 0.0776 0.5014 0.113 Uiso 0.52(3) 1 calc R U P A 1
H3C H 0.8252 0.0347 0.5310 0.113 Uiso 0.52(3) 1 calc R U P A 1
C3' C 0.7964(12) 0.0051(11) 0.4984(10) 0.141(18) Uani 0.48(3) 1 d D U P A 2
H3D H 0.8144 0.0016 0.4736 0.169 Uiso 0.48(3) 1 calc R U P A 2
H3I H 0.8111 0.0158 0.5316 0.169 Uiso 0.48(3) 1 calc R U P A 2
H3F H 0.7714 -0.0215 0.5044 0.169 Uiso 0.48(3) 1 calc R U P A 2
C4 C 0.7593(4) 0.0408(4) 0.5106(4) 0.096(5) Uani 1 1 d D U . . .
H4A H 0.7645 0.0688 0.5039 0.144 Uiso 1 1 calc R U . . .
H4B H 0.7650 0.0383 0.5474 0.144 Uiso 1 1 calc R U . . .
H4C H 0.7304 0.0208 0.5027 0.144 Uiso 1 1 calc R U . . .
C5 C 0.9011(2) 0.1416(2) 0.3944(4) 0.034(2) Uani 1 1 d D . . . .
C6 C 0.9308(3) 0.1267(3) 0.4097(4) 0.055(3) Uani 1 1 d D . . . .
H6A H 0.9398 0.1352 0.4466 0.066 Uiso 0.60(2) 1 calc R U P B 1
H6B H 0.9165 0.0962 0.4041 0.066 Uiso 0.40(2) 1 calc R U P B 2
C7 C 0.9673(4) 0.1457(6) 0.3761(7) 0.144(8) Uani 1 1 d D U . . .
H7A H 0.9803 0.1758 0.3780 0.173 Uiso 1 1 calc R U . . .
H7B H 0.9871 0.1374 0.3879 0.173 Uiso 1 1 calc R U . . .
H7C H 0.9592 0.1366 0.3400 0.173 Uiso 1 1 calc R U . . .
C8 C 0.9128(7) 0.0830(5) 0.4061(12) 0.129(9) Uani 0.60(2) 1 d D U P B 1
H8A H 0.8882 0.0695 0.4283 0.154 Uiso 0.60(2) 1 calc R U P B 1
H8B H 0.9050 0.0743 0.3697 0.154 Uiso 0.60(2) 1 calc R U P B 1
H8C H 0.9329 0.0750 0.4177 0.154 Uiso 0.60(2) 1 calc R U P B 1
C8' C 0.9424(10) 0.1346(12) 0.4636(7) 0.129(9) Uani 0.40(2) 1 d D U P B 2
H8D H 0.9175 0.1217 0.4854 0.154 Uiso 0.40(2) 1 calc R U P B 2
H8I H 0.9601 0.1231 0.4725 0.154 Uiso 0.40(2) 1 calc R U P B 2
H8F H 0.9574 0.1645 0.4698 0.154 Uiso 0.40(2) 1 calc R U P B 2
C9 C 0.8530(3) 0.0834(3) 0.2488(4) 0.046(3) Uani 1 1 d D . . . .
H9A H 0.8598 0.0809 0.2121 0.055 Uiso 1 1 calc R U . . .
H9B H 0.8766 0.0875 0.2707 0.055 Uiso 1 1 calc R U . . .
C10 C 0.8173(4) 0.0454(3) 0.2639(7) 0.098(6) Uani 1 1 d D . . . .
H10A H 0.7988 0.0334 0.2333 0.118 Uiso 1 1 calc R U . . .
H10B H 0.8260 0.0256 0.2752 0.118 Uiso 1 1 calc R U . . .
C11 C 0.8903(2) 0.1565(3) 0.2577(3) 0.0299(19) Uani 1 1 d . . . . .
H11A H 0.9045 0.1621 0.2235 0.036 Uiso 1 1 calc R U . . .
H11B H 0.9066 0.1510 0.2836 0.036 Uiso 1 1 calc R U . . .
C12 C 0.8877(3) 0.1939(2) 0.2746(3) 0.0297(19) Uani 1 1 d . . . . .
H12A H 0.9157 0.2169 0.2831 0.036 Uiso 1 1 calc R U . . .
H12B H 0.8764 0.2029 0.2458 0.036 Uiso 1 1 calc R U . . .
C13 C 0.8278(3) 0.1252(3) 0.2076(3) 0.033(2) Uani 1 1 d . . . . .
H13A H 0.8337 0.1133 0.1764 0.040 Uiso 1 1 calc R U . . .
H13B H 0.8391 0.1550 0.2011 0.040 Uiso 1 1 calc R U . . .
C14 C 0.7822(2) 0.1051(3) 0.2144(3) 0.0244(17) Uani 1 1 d . . . . .
H14A H 0.7706 0.1150 0.1870 0.029 Uiso 1 1 calc R U . . .
H14B H 0.7698 0.0748 0.2103 0.029 Uiso 1 1 calc R U . . .
C15 C 0.8413(2) 0.1922(2) 0.4938(3) 0.0294(18) Uani 1 1 d . . . . .
H15A H 0.8200 0.2004 0.4915 0.035 Uiso 1 1 calc R U . . .
H15B H 0.8448 0.1873 0.5310 0.035 Uiso 1 1 calc R U . . .
C16 C 0.8279(2) 0.1530(2) 0.4626(3) 0.0276(18) Uani 1 1 d . . . . .
H16A H 0.8466 0.1420 0.4697 0.033 Uiso 1 1 calc R U . . .
H16B H 0.7995 0.1318 0.4726 0.033 Uiso 1 1 calc R U . . .
C17 C 0.8821(3) 0.2656(2) 0.4710(3) 0.0286(18) Uani 1 1 d . . . . .
H17A H 0.9108 0.2884 0.4659 0.034 Uiso 1 1 calc R U . . .
H17B H 0.8719 0.2701 0.5047 0.034 Uiso 1 1 calc R U . . .
C18 C 0.8552(2) 0.2654(2) 0.4270(3) 0.0246(17) Uani 1 1 d . . . . .
H18A H 0.8260 0.2445 0.4340 0.030 Uiso 1 1 calc R U . . .
H18B H 0.8574 0.2928 0.4241 0.030 Uiso 1 1 calc R U . . .
C19 C 0.9177(3) 0.2290(3) 0.4997(3) 0.0307(19) Uani 1 1 d . . . . .
H19A H 0.9420 0.2440 0.4766 0.037 Uiso 1 1 calc R U . . .
H19B H 0.9132 0.2008 0.5046 0.037 Uiso 1 1 calc R U . . .
C20 C 0.9283(3) 0.2506(3) 0.5528(4) 0.048(3) Uani 1 1 d . . . . .
H20A H 0.9547 0.2534 0.5651 0.058 Uiso 1 1 calc R U . . .
H20B H 0.9324 0.2787 0.5484 0.058 Uiso 1 1 calc R U . . .
C21 C 0.9905(2) 0.2895(2) 0.3073(3) 0.0222(16) Uani 1 1 d . . . . .
H21A H 1.0205 0.3001 0.3043 0.027 Uiso 1 1 calc R U . . .
H21B H 0.9769 0.2720 0.2764 0.027 Uiso 1 1 calc R U . . .
C22 C 0.9743(2) 0.2639(2) 0.3561(3) 0.0247(17) Uani 1 1 d . . . . .
H22A H 0.9716 0.2364 0.3504 0.030 Uiso 1 1 calc R U . . .
H22B H 0.9940 0.2775 0.3852 0.030 Uiso 1 1 calc R U . . .
C23 C 1.0139(2) 0.3599(2) 0.3398(3) 0.0248(17) Uani 1 1 d . . . . .
H23A H 1.0403 0.3596 0.3403 0.030 Uiso 1 1 calc R U . . .
H23B H 1.0191 0.3862 0.3238 0.030 Uiso 1 1 calc R U . . .
C24 C 0.9984(2) 0.3567(2) 0.3944(3) 0.0253(17) Uani 1 1 d . . . . .
H24A H 1.0000 0.3345 0.4133 0.030 Uiso 1 1 calc R U . . .
H24B H 1.0156 0.3831 0.4131 0.030 Uiso 1 1 calc R U . . .
C25 C 0.9767(2) 0.3367(2) 0.2554(3) 0.0253(17) Uani 1 1 d . . . . .
H25A H 0.9994 0.3403 0.2321 0.030 Uiso 1 1 calc R U . . .
H25B H 0.9770 0.3632 0.2574 0.030 Uiso 1 1 calc R U . . .
C26 C 0.9355(2) 0.3032(2) 0.2337(3) 0.0250(17) Uani 1 1 d . . . . .
H26A H 0.9273 0.3144 0.2039 0.030 Uiso 1 1 calc R U . . .
H26B H 0.9383 0.2798 0.2210 0.030 Uiso 1 1 calc R U . . .
C27 C 0.8499(2) 0.3633(2) 0.3565(3) 0.0238(17) Uani 1 1 d . . . . .
H27A H 0.8406 0.3553 0.3930 0.029 Uiso 1 1 calc R U . . .
H27B H 0.8277 0.3648 0.3373 0.029 Uiso 1 1 calc R U . . .
C28 C 0.8573(2) 0.3315(2) 0.3319(3) 0.0254(17) Uani 1 1 d . . . . .
H28A H 0.8346 0.3035 0.3408 0.030 Uiso 1 1 calc R U . . .
H28B H 0.8586 0.3346 0.2934 0.030 Uiso 1 1 calc R U . . .
C29 C 0.9000(2) 0.4204(2) 0.3013(3) 0.0241(17) Uani 1 1 d . . . . .
H29A H 0.9129 0.4508 0.3012 0.029 Uiso 1 1 calc R U . . .
H29B H 0.8748 0.4089 0.2795 0.029 Uiso 1 1 calc R U . . .
C30 C 0.9302(2) 0.4083(2) 0.2776(3) 0.0203(16) Uani 1 1 d . . . . .
H30A H 0.9155 0.3785 0.2689 0.024 Uiso 1 1 calc R U . . .
H30B H 0.9425 0.4242 0.2451 0.024 Uiso 1 1 calc R U . . .
C31 C 0.8805(2) 0.4331(2) 0.3872(3) 0.0201(16) Uani 1 1 d . . . . .
H31A H 0.8654 0.4186 0.4193 0.024 Uiso 1 1 calc R U . . .
H31B H 0.8624 0.4404 0.3670 0.024 Uiso 1 1 calc R U . . .
C32 C 0.9192(2) 0.4721(2) 0.4025(3) 0.0241(17) Uani 1 1 d . . . . .
H32A H 0.9370 0.4654 0.4241 0.029 Uiso 1 1 calc R U . . .
H32B H 0.9348 0.4868 0.3708 0.029 Uiso 1 1 calc R U . . .
C33 C 0.8026(6) 0.4494(8) 0.4571(10) 0.166(10) Uani 1 1 d . . . . .
H33A H 0.8023 0.4240 0.4673 0.199 Uiso 1 1 calc R U . . .
H33B H 0.8019 0.4509 0.4189 0.199 Uiso 1 1 calc R U . . .
H33C H 0.7784 0.4494 0.4718 0.199 Uiso 1 1 calc R U . . .
N1 N 0.84872(19) 0.1200(2) 0.2533(3) 0.0257(15) Uani 1 1 d . . . . .
N2 N 0.88134(19) 0.22563(19) 0.4722(2) 0.0248(14) Uani 1 1 d . . . . .
N3 N 0.98267(18) 0.32428(18) 0.3083(2) 0.0202(13) Uani 1 1 d . . . . .
N4 N 0.88832(18) 0.40487(18) 0.3559(2) 0.0191(13) Uani 1 1 d . . . . .
N5 N 0.91229(19) 0.38391(19) 0.4547(2) 0.0235(14) Uani 1 1 d . . . . .
N6 N 0.91822(19) 0.36863(19) 0.4927(3) 0.0236(14) Uani 1 1 d . . . . .
N7 N 0.9232(2) 0.3546(2) 0.5296(3) 0.0400(19) Uani 1 1 d . . . . .
O1 O 0.78140(18) 0.06933(17) 0.4070(2) 0.0374(14) Uani 1 1 d . . . . .
O2 O 0.7832(3) 0.0123(2) 0.3917(4) 0.077(3) Uani 1 1 d . . . . .
O3 O 0.86841(17) 0.11682(16) 0.3723(2) 0.0319(13) Uani 1 1 d . . . . .
O4 O 0.91268(15) 0.17913(15) 0.4033(2) 0.0262(12) Uani 1 1 d . . . . .
O5 O 0.79504(18) 0.05113(17) 0.3054(3) 0.0405(15) Uani 1 1 d . . . . .
H5 H 0.7969 0.0356 0.3358 0.061 Uiso 1 1 d R U . . .
O6 O 0.86171(15) 0.18378(14) 0.31938(18) 0.0184(11) Uani 1 1 d . . . . .
O7 O 0.99137(14) 0.43853(14) 0.40227(18) 0.0173(10) Uani 1 1 d . . . . .
O8 O 0.82928(15) 0.16277(14) 0.40883(18) 0.0196(11) Uani 1 1 d . . . . .
O9 O 0.86845(14) 0.25569(13) 0.37974(18) 0.0169(10) Uani 1 1 d . . . . .
O10 O 0.8980(3) 0.2298(3) 0.5913(3) 0.101(4) Uani 1 1 d . . . . .
H10 H 0.9066 0.2421 0.6200 0.121 Uiso 1 1 d R U . . .
O11 O 0.93543(14) 0.25905(14) 0.36942(19) 0.0184(11) Uani 1 1 d . . . . .
O12 O 0.95646(14) 0.34786(14) 0.39270(19) 0.0191(11) Uani 1 1 d . . . . .
O13 O 0.90497(15) 0.28950(15) 0.27305(19) 0.0214(11) Uani 1 1 d . . . . .
O14 O 0.89512(14) 0.33730(14) 0.3511(2) 0.0207(11) Uani 1 1 d . . . . .
O15 O 0.96175(14) 0.41732(14) 0.31531(18) 0.0175(10) Uani 1 1 d . . . . .
O16 O 0.90802(16) 0.49793(15) 0.43150(19) 0.0240(12) Uani 1 1 d . . . . .
H16 H 0.8841 0.4833 0.4436 0.029 Uiso 1 1 d R U . . .
O17 O 0.8360(3) 0.4811(4) 0.4747(4) 0.106(4) Uani 1 1 d . . . . .
H17 H 0.8297 0.4977 0.4881 0.127 Uiso 1 1 d R U . . .
O18 O 0.8348(4) 0.2515(6) 0.6007(6) 0.081(7) Uani 0.56(3) 1 d . U P C 1
O18' O 0.8464(7) 0.2867(9) 0.6298(10) 0.105(12) Uani 0.44(3) 1 d . U P C 2
O19 O 0.7784(7) 0.2393(8) 0.5297(10) 0.113(11) Uani 0.47(2) 1 d . . P D 1
O19' O 0.7190(10) 0.1749(11) 0.5152(15) 0.23(2) Uani 0.53(2) 1 d . U P D 2
O20 O 0.7142(13) 0.1229(13) 0.5415(16) 0.114(19) Uani 0.28(3) 1 d . U P E 1
O20' O 0.7344(15) 0.1259(15) 0.586(2) 0.10(2) Uani 0.22(3) 1 d . U P E 2
O21 O 0.7471(13) 0.2844(12) 0.3917(18) 0.090(9) Uani 0.258(19) 1 d . U P F 1
O21' O 0.7362(13) 0.2949(13) 0.3710(19) 0.090(9) Uani 0.242(19) 1 d . U P F 2
O22 O 0.815(2) 0.9553(17) 0.390(2) 0.190(12) Uani 0.35(3) 1 d . U P G 1
O22' O 0.7794(13) 0.9390(8) 0.4053(10) 0.190(12) Uani 0.65(3) 1 d . U P G 2
O23 O 0.7826(17) 0.3010(19) 0.493(2) 0.116(10) Uani 0.205(14) 1 d . U P H 1
O23' O 0.8162(12) 0.3524(13) 0.5280(15) 0.116(10) Uani 0.295(14) 1 d . U P H 2
O24 O 0.8546(14) 0.2084(13) 0.7154(15) 0.089(8) Uani 0.211(12) 1 d . U P I 1
O24' O 0.9001(10) 0.2404(9) 0.6945(11) 0.089(8) Uani 0.289(12) 1 d . U P I 2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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
O6 Dy1 O15 106.13(17) . 17
O6 Dy1 O7 93.26(16) . 17
O15 Dy1 O7 63.43(16) 17 17
O6 Dy1 O8 66.04(16) . .
O15 Dy1 O8 78.75(17) 17 .
O7 Dy1 O8 129.94(17) 17 .
O6 Dy1 O1 142.31(18) . .
O15 Dy1 O1 82.79(19) 17 .
O7 Dy1 O1 122.50(18) 17 .
O8 Dy1 O1 80.58(18) . .
O6 Dy1 O3 78.34(18) . .
O15 Dy1 O3 150.22(18) 17 .
O7 Dy1 O3 146.36(18) 17 .
O8 Dy1 O3 76.42(19) . .
O1 Dy1 O3 77.2(2) . .
O6 Dy1 O5 131.45(18) . .
O15 Dy1 O5 113.26(18) 17 .
O7 Dy1 O5 80.5(2) 17 .
O8 Dy1 O5 147.5(2) . .
O1 Dy1 O5 71.7(2) . .
O3 Dy1 O5 81.1(2) . .
O6 Dy1 N1 68.07(18) . .
O15 Dy1 N1 131.19(18) 17 .
O7 Dy1 N1 68.49(18) 17 .
O8 Dy1 N1 130.90(18) . .
O1 Dy1 N1 132.6(2) . .
O3 Dy1 N1 78.2(2) . .
O5 Dy1 N1 64.9(2) . .
O6 Dy1 Fe1 33.80(11) . .
O15 Dy1 Fe1 100.32(12) 17 .
O7 Dy1 Fe1 121.11(12) 17 .
O8 Dy1 Fe1 34.05(12) . .
O1 Dy1 Fe1 109.19(14) . .
O3 Dy1 Fe1 66.63(13) . .
O5 Dy1 Fe1 146.04(15) . .
N1 Dy1 Fe1 97.05(14) . .
O6 Fe1 O8 80.80(19) . .
O6 Fe1 O11 102.7(2) . .
O8 Fe1 O11 176.3(2) . .
O6 Fe1 O9 98.1(2) . .
O8 Fe1 O9 102.9(2) . .
O11 Fe1 O9 75.66(19) . .
O6 Fe1 O4 95.1(2) . .
O8 Fe1 O4 92.1(2) . .
O11 Fe1 O4 88.7(2) . .
O9 Fe1 O4 161.4(2) . .
O6 Fe1 N2 159.7(2) . .
O8 Fe1 N2 79.9(2) . .
O11 Fe1 N2 96.5(2) . .
O9 Fe1 N2 80.1(2) . .
O4 Fe1 N2 92.0(2) . .
O6 Fe1 Dy1 41.38(14) . .
O8 Fe1 Dy1 41.81(14) . .
O11 Fe1 Dy1 141.89(14) . .
O9 Fe1 Dy1 114.68(14) . .
O4 Fe1 Dy1 83.85(14) . .
N2 Fe1 Dy1 121.05(16) . .
O13 Fe2 O14 93.1(2) . .
O13 Fe2 O12 141.0(2) . .
O14 Fe2 O12 72.74(19) . .
O13 Fe2 O9 101.2(2) . .
O14 Fe2 O9 88.2(2) . .
O12 Fe2 O9 114.05(19) . .
O13 Fe2 O11 106.8(2) . .
O14 Fe2 O11 155.8(2) . .
O12 Fe2 O11 98.40(19) . .
O9 Fe2 O11 74.67(19) . .
O13 Fe2 N3 79.4(2) . .
O14 Fe2 N3 121.1(2) . .
O12 Fe2 N3 77.8(2) . .
O9 Fe2 N3 150.7(2) . .
O11 Fe2 N3 77.1(2) . .
O7 Fe3 O15 76.18(19) . .
O7 Fe3 O14 163.3(2) . .
O15 Fe3 O14 94.5(2) . .
O7 Fe3 O12 96.5(2) . .
O15 Fe3 O12 105.8(2) . .
O14 Fe3 O12 72.48(19) . .
O7 Fe3 N5 95.0(2) . .
O15 Fe3 N5 155.7(2) . .
O14 Fe3 N5 98.8(2) . .
O12 Fe3 N5 97.6(2) . .
O7 Fe3 N4 114.8(2) . .
O15 Fe3 N4 79.3(2) . .
O14 Fe3 N4 76.1(2) . .
O12 Fe3 N4 148.4(2) . .
N5 Fe3 N4 84.3(2) . .
O2 C1 O1 123.3(10) . .
O2 C1 C2 119.2(10) . .
O1 C1 C2 117.5(11) . .
C3' C2 C4 115.1(14) . .
C3 C2 C4 115.8(14) . .
C3' C2 C1 122.5(14) . .
C3 C2 C1 115.1(11) . .
C4 C2 C1 116.0(9) . .
C3 C2 H2 102.2 . .
C4 C2 H2 102.2 . .
C1 C2 H2 102.2 . .
C3' C2 H2A 98.5 . .
C4 C2 H2A 98.5 . .
C1 C2 H2A 98.5 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C3' H3D 109.5 . .
C2 C3' H3I 109.5 . .
H3D C3' H3I 109.5 . .
C2 C3' H3F 109.5 . .
H3D C3' H3F 109.5 . .
H3I C3' H3F 109.5 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O3 C5 O4 124.8(7) . .
O3 C5 C6 118.2(7) . .
O4 C5 C6 116.9(7) . .
C8 C6 C7 108.0(13) . .
C8' C6 C7 110.7(14) . .
C8 C6 C5 112.9(10) . .
C8' C6 C5 111.9(12) . .
C7 C6 C5 110.3(8) . .
C8 C6 H6A 108.5 . .
C7 C6 H6A 108.5 . .
C5 C6 H6A 108.5 . .
C8' C6 H6B 107.9 . .
C7 C6 H6B 107.9 . .
C5 C6 H6B 107.9 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C8' H8D 109.5 . .
C6 C8' H8I 109.5 . .
H8D C8' H8I 109.5 . .
C6 C8' H8F 109.5 . .
H8D C8' H8F 109.5 . .
H8I C8' H8F 109.5 . .
C10 C9 N1 115.1(8) . .
C10 C9 H9A 108.5 . .
N1 C9 H9A 108.5 . .
C10 C9 H9B 108.5 . .
N1 C9 H9B 108.5 . .
H9A C9 H9B 107.5 . .
O5 C10 C9 112.0(9) . .
O5 C10 H10A 109.2 . .
C9 C10 H10A 109.2 . .
O5 C10 H10B 109.2 . .
C9 C10 H10B 109.2 . .
H10A C10 H10B 107.9 . .
N1 C11 C12 110.7(6) . .
N1 C11 H11A 109.5 . .
C12 C11 H11A 109.5 . .
N1 C11 H11B 109.5 . .
C12 C11 H11B 109.5 . .
H11A C11 H11B 108.1 . .
O6 C12 C11 109.5(6) . .
O6 C12 H12A 109.8 . .
C11 C12 H12A 109.8 . .
O6 C12 H12B 109.8 . .
C11 C12 H12B 109.8 . .
H12A C12 H12B 108.2 . .
N1 C13 C14 112.9(7) . .
N1 C13 H13A 109.0 . .
C14 C13 H13A 109.0 . .
N1 C13 H13B 109.0 . .
C14 C13 H13B 109.0 . .
H13A C13 H13B 107.8 . .
O7 C14 C13 111.4(6) 17 .
O7 C14 H14A 109.4 17 .
C13 C14 H14A 109.4 . .
O7 C14 H14B 109.4 17 .
C13 C14 H14B 109.4 . .
H14A C14 H14B 108.0 . .
N2 C15 C16 108.9(6) . .
N2 C15 H15A 109.9 . .
C16 C15 H15A 109.9 . .
N2 C15 H15B 109.9 . .
C16 C15 H15B 109.9 . .
H15A C15 H15B 108.3 . .
O8 C16 C15 108.2(6) . .
O8 C16 H16A 110.1 . .
C15 C16 H16A 110.1 . .
O8 C16 H16B 110.1 . .
C15 C16 H16B 110.1 . .
H16A C16 H16B 108.4 . .
N2 C17 C18 109.5(6) . .
N2 C17 H17A 109.8 . .
C18 C17 H17A 109.8 . .
N2 C17 H17B 109.8 . .
C18 C17 H17B 109.8 . .
H17A C17 H17B 108.2 . .
O9 C18 C17 108.7(6) . .
O9 C18 H18A 110.0 . .
C17 C18 H18A 110.0 . .
O9 C18 H18B 110.0 . .
C17 C18 H18B 110.0 . .
H18A C18 H18B 108.3 . .
N2 C19 C20 116.9(7) . .
N2 C19 H19A 108.1 . .
C20 C19 H19A 108.1 . .
N2 C19 H19B 108.1 . .
C20 C19 H19B 108.1 . .
H19A C19 H19B 107.3 . .
O10 C20 C19 114.0(8) . .
O10 C20 H20A 108.8 . .
C19 C20 H20A 108.8 . .
O10 C20 H20B 108.8 . .
C19 C20 H20B 108.8 . .
H20A C20 H20B 107.7 . .
N3 C21 C22 110.8(6) . .
N3 C21 H21A 109.5 . .
C22 C21 H21A 109.5 . .
N3 C21 H21B 109.5 . .
C22 C21 H21B 109.5 . .
H21A C21 H21B 108.1 . .
O11 C22 C21 109.9(6) . .
O11 C22 H22A 109.7 . .
C21 C22 H22A 109.7 . .
O11 C22 H22B 109.7 . .
C21 C22 H22B 109.7 . .
H22A C22 H22B 108.2 . .
C24 C23 N3 109.5(6) . .
C24 C23 H23A 109.8 . .
N3 C23 H23A 109.8 . .
C24 C23 H23B 109.8 . .
N3 C23 H23B 109.8 . .
H23A C23 H23B 108.2 . .
O12 C24 C23 109.2(6) . .
O12 C24 H24A 109.8 . .
C23 C24 H24A 109.8 . .
O12 C24 H24B 109.8 . .
C23 C24 H24B 109.8 . .
H24A C24 H24B 108.3 . .
N3 C25 C26 109.0(6) . .
N3 C25 H25A 109.9 . .
C26 C25 H25A 109.9 . .
N3 C25 H25B 109.9 . .
C26 C25 H25B 109.9 . .
H25A C25 H25B 108.3 . .
O13 C26 C25 110.0(6) . .
O13 C26 H26A 109.7 . .
C25 C26 H26A 109.7 . .
O13 C26 H26B 109.7 . .
C25 C26 H26B 109.7 . .
H26A C26 H26B 108.2 . .
C28 C27 N4 111.0(6) . .
C28 C27 H27A 109.4 . .
N4 C27 H27A 109.4 . .
C28 C27 H27B 109.4 . .
N4 C27 H27B 109.4 . .
H27A C27 H27B 108.0 . .
O14 C28 C27 107.7(6) . .
O14 C28 H28A 110.2 . .
C27 C28 H28A 110.2 . .
O14 C28 H28B 110.2 . .
C27 C28 H28B 110.2 . .
H28A C28 H28B 108.5 . .
N4 C29 C30 111.8(6) . .
N4 C29 H29A 109.2 . .
C30 C29 H29A 109.2 . .
N4 C29 H29B 109.2 . .
C30 C29 H29B 109.2 . .
H29A C29 H29B 107.9 . .
O15 C30 C29 107.8(6) . .
O15 C30 H30A 110.1 . .
C29 C30 H30A 110.1 . .
O15 C30 H30B 110.1 . .
C29 C30 H30B 110.1 . .
H30A C30 H30B 108.5 . .
N4 C31 C32 113.5(6) . .
N4 C31 H31A 108.9 . .
C32 C31 H31A 108.9 . .
N4 C31 H31B 108.9 . .
C32 C31 H31B 108.9 . .
H31A C31 H31B 107.7 . .
O16 C32 C31 109.0(6) . .
O16 C32 H32A 109.9 . .
C31 C32 H32A 109.9 . .
O16 C32 H32B 109.9 . .
C31 C32 H32B 109.9 . .
H32A C32 H32B 108.3 . .
O17 C33 H33A 109.5 . .
O17 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
O17 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C9 N1 C11 108.4(6) . .
C9 N1 C13 112.0(7) . .
C11 N1 C13 108.9(6) . .
C9 N1 Dy1 111.0(5) . .
C11 N1 Dy1 106.5(4) . .
C13 N1 Dy1 109.9(4) . .
C19 N2 C17 111.8(6) . .
C19 N2 C15 112.8(6) . .
C17 N2 C15 111.0(6) . .
C19 N2 Fe1 110.6(5) . .
C17 N2 Fe1 104.3(4) . .
C15 N2 Fe1 105.8(4) . .
C21 N3 C25 112.9(6) . .
C21 N3 C23 112.6(6) . .
C25 N3 C23 112.8(6) . .
C21 N3 Fe2 107.1(4) . .
C25 N3 Fe2 101.9(4) . .
C23 N3 Fe2 108.7(4) . .
C31 N4 C29 110.9(6) . .
C31 N4 C27 107.8(6) . .
C29 N4 C27 110.8(6) . .
C31 N4 Fe3 119.0(4) . .
C29 N4 Fe3 105.2(4) . .
C27 N4 Fe3 102.8(4) . .
N6 N5 Fe3 126.2(5) . .
N7 N6 N5 177.9(8) . .
C1 O1 Dy1 137.0(7) . .
C5 O3 Dy1 136.8(5) . .
C5 O4 Fe1 127.8(5) . .
C10 O5 Dy1 124.5(5) . .
C10 O5 H5 106.1 . .
Dy1 O5 H5 106.6 . .
C12 O6 Fe1 122.8(4) . .
C12 O6 Dy1 123.5(4) . .
Fe1 O6 Dy1 104.8(2) . .
C14 O7 Fe3 127.8(4) 18_545 .
C14 O7 Dy1 121.5(4) 18_545 18_545
Fe3 O7 Dy1 110.4(2) . 18_545
C16 O8 Fe1 113.5(4) . .
C16 O8 Dy1 127.6(4) . .
Fe1 O8 Dy1 104.1(2) . .
C18 O9 Fe2 118.0(4) . .
C18 O9 Fe1 113.8(4) . .
Fe2 O9 Fe1 102.6(2) . .
C20 O10 H10 109.1 . .
C22 O11 Fe1 132.0(4) . .
C22 O11 Fe2 120.3(4) . .
Fe1 O11 Fe2 103.9(2) . .
C24 O12 Fe2 114.4(4) . .
C24 O12 Fe3 125.3(4) . .
Fe2 O12 Fe3 104.9(2) . .
C26 O13 Fe2 121.0(4) . .
C28 O14 Fe2 129.5(4) . .
C28 O14 Fe3 123.3(4) . .
Fe2 O14 Fe3 106.7(2) . .
C30 O15 Fe3 111.8(4) . .
C30 O15 Dy1 130.8(4) . 18_545
Fe3 O15 Dy1 110.0(2) . 18_545
C32 O16 H16 109.0 . .
C33 O17 H17 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O6 2.310(5) .
Dy1 O15 2.313(5) 17
Dy1 O7 2.318(5) 17
Dy1 O8 2.322(5) .
Dy1 O1 2.357(6) .
Dy1 O3 2.384(5) .
Dy1 O5 2.418(5) .
Dy1 N1 2.602(6) .
Dy1 Fe1 3.3782(11) .
Fe1 O6 1.944(5) .
Fe1 O8 1.951(5) .
Fe1 O11 1.981(5) .
Fe1 O9 2.027(5) .
Fe1 O4 2.030(5) .
Fe1 N2 2.260(6) .
Fe2 O13 1.901(5) .
Fe2 O14 1.990(5) .
Fe2 O12 2.016(5) .
Fe2 O9 2.022(5) .
Fe2 O11 2.031(5) .
Fe2 N3 2.265(6) .
Fe3 O7 1.964(5) .
Fe3 O15 1.982(5) .
Fe3 O14 1.999(5) .
Fe3 O12 2.020(5) .
Fe3 N5 2.031(6) .
Fe3 N4 2.308(6) .
C1 O2 1.237(14) .
C1 O1 1.264(12) .
C1 C2 1.454(15) .
C2 C3' 1.383(14) .
C2 C3 1.422(14) .
C2 C4 1.434(11) .
C2 H2 1.0000 .
C2 H2A 1.0000 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C3' H3D 0.9800 .
C3' H3I 0.9800 .
C3' H3F 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 O3 1.241(9) .
C5 O4 1.266(9) .
C5 C6 1.521(12) .
C6 C8 1.427(14) .
C6 C8' 1.430(15) .
C6 C7 1.461(13) .
C6 H6A 1.0000 .
C6 H6B 1.0000 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C8' H8D 0.9800 .
C8' H8I 0.9800 .
C8' H8F 0.9800 .
C9 C10 1.432(12) .
C9 N1 1.461(10) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 O5 1.431(12) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 N1 1.472(10) .
C11 C12 1.512(11) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 O6 1.426(8) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 N1 1.473(10) .
C13 C14 1.488(11) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 O7 1.421(8) 17
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 N2 1.496(10) .
C15 C16 1.514(11) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 O8 1.417(8) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 N2 1.480(10) .
C17 C18 1.507(11) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 O9 1.421(8) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 N2 1.479(10) .
C19 C20 1.528(11) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 O10 1.407(12) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 N3 1.470(9) .
C21 C22 1.504(10) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 O11 1.415(9) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C24 1.494(11) .
C23 N3 1.495(9) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 O12 1.431(9) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 N3 1.481(9) .
C25 C26 1.522(11) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 O13 1.412(9) .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C27 C28 1.489(10) .
C27 N4 1.498(9) .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C28 O14 1.407(9) .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C29 N4 1.490(9) .
C29 C30 1.534(10) .
C29 H29A 0.9900 .
C29 H29B 0.9900 .
C30 O15 1.429(8) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C31 N4 1.466(9) .
C31 C32 1.506(10) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
C32 O16 1.434(8) .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C33 O17 1.30(2) .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
N5 N6 1.203(9) .
N6 N7 1.139(9) .
O5 H5 0.9936 .
O7 C14 1.421(8) 18_545
O7 Dy1 2.319(5) 18_545
O10 H10 0.8399 .
O15 Dy1 2.313(5) 18_545
O16 H16 0.8402 .
O17 H17 0.8400 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O2 0.99 1.62 2.555(11) 155.5 .
O10 H10 O24' 0.84 1.92 2.66(3) 147.4 .
O16 H16 O17 0.84 1.93 2.680(11) 147.7 .
O17 H17 O19' 0.84 1.95 2.78(3) 169.4 2_655
