#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316440.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_4316440
loop_
_publ_author_name
'Ghulam Abbas'
'Yanhua Lan'
'George E. Kostakis'
'Wolfgang Wernsdorfer'
'Christopher E. Anson'
'Annie K. Powell'
_publ_contact_author
; 
Annie K. Powell
;
_publ_contact_author_email       annie.powell@kit.edu
_publ_contact_author_phone       '+49 721 608 2135'
_publ_section_title
;
 Series of Isostructural Planar Lanthanide Complexes
 [LnIII4(μ3-OH)2(mdeaH)2(piv)8] with Single Molecule Magnet Behavior for
 the Dy4 Analogue
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8067
_journal_page_last               8072
_journal_paper_doi               10.1021/ic1011605
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C50 H98 Dy4 N2 O22'
_chemical_formula_weight         1729.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.759(1)
_cell_angle_beta                 98.639(1)
_cell_angle_gamma                102.900(1)
_cell_formula_units_Z            1
_cell_length_a                   11.6333(6)
_cell_length_b                   12.5247(7)
_cell_length_c                   12.7437(7)
_cell_measurement_reflns_used    6633
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.17
_cell_volume                     1651.03(16)
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2003)'
_computing_molecular_graphics    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13701
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    4.542
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.706
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         7209
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0497P)²+4.7917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                5848
_reflns_number_total             7209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011605_si_002_2.cif
_cod_data_source_block           ga15
_cod_original_cell_volume        1651.03(15)
_cod_database_code               4316440
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.39751(2) 0.33379(2) 0.39442(2) 0.02316(9) Uani 1 1 d . . .
Dy2 Dy 0.72761(2) 0.42015(2) 0.43747(2) 0.02337(9) Uani 1 1 d . . .
O1 O 0.5643(4) 0.4983(4) 0.4232(4) 0.0235(9) Uani 1 1 d D . .
H1 H 0.548(6) 0.513(6) 0.362(4) 0.028 Uiso 1 1 d D . .
N1 N 0.7487(5) 0.2111(5) 0.4017(5) 0.0312(12) Uani 1 1 d . . .
C1 C 0.7057(7) 0.1859(7) 0.4969(7) 0.0430(18) Uani 1 1 d . . .
H1A H 0.7624 0.2412 0.5714 0.052 Uiso 1 1 calc R . .
H1B H 0.7037 0.1039 0.4884 0.052 Uiso 1 1 calc R . .
C2 C 0.5787(6) 0.2001(6) 0.4952(7) 0.0374(16) Uani 1 1 d . . .
H2A H 0.5174 0.1281 0.4362 0.045 Uiso 1 1 calc R . .
H2B H 0.5610 0.2097 0.5710 0.045 Uiso 1 1 calc R . .
O2 O 0.5715(4) 0.3020(4) 0.4700(4) 0.0269(9) Uani 1 1 d . . .
C3 C 0.8776(7) 0.2152(7) 0.4118(8) 0.047(2) Uani 1 1 d . . .
H3A H 0.8843 0.1334 0.3851 0.056 Uiso 1 1 calc R . .
H3B H 0.9233 0.2573 0.4934 0.056 Uiso 1 1 calc R . .
C4 C 0.9326(7) 0.2792(6) 0.3394(7) 0.0395(17) Uani 1 1 d . . .
H4A H 1.0209 0.2883 0.3512 0.047 Uiso 1 1 calc R . .
H4B H 0.8929 0.2340 0.2566 0.047 Uiso 1 1 calc R . .
O3 O 0.9110(4) 0.3965(4) 0.3790(5) 0.0365(11) Uani 1 1 d D . .
H3 H 0.947(7) 0.451(6) 0.360(7) 0.044 Uiso 1 1 d D . .
C5 C 0.6715(9) 0.1171(7) 0.2908(7) 0.053(2) Uani 1 1 d . . .
H5A H 0.6850 0.0408 0.2841 0.079 Uiso 1 1 calc R . .
H5B H 0.6929 0.1372 0.2269 0.079 Uiso 1 1 calc R . .
H5C H 0.5856 0.1113 0.2884 0.079 Uiso 1 1 calc R . .
O4 O 0.7153(4) 0.5399(4) 0.6390(4) 0.0254(9) Uani 1 1 d . . .
O5 O 0.8669(4) 0.4653(4) 0.6224(4) 0.0289(10) Uani 1 1 d . . .
C6 C 0.8032(5) 0.5135(5) 0.6847(6) 0.0261(13) Uani 1 1 d . A .
C7 C 0.8276(6) 0.5317(6) 0.8104(6) 0.0325(15) Uani 1 1 d D . .
C8A C 0.9579(10) 0.6187(11) 0.8685(12) 0.061(4) Uiso 0.66 1 d PD A 1
H8A1 H 1.0164 0.5845 0.8312 0.092 Uiso 0.66 1 calc PR A 1
H8A2 H 0.9783 0.6319 0.9502 0.092 Uiso 0.66 1 calc PR A 1
H8A3 H 0.9614 0.6944 0.8606 0.092 Uiso 0.66 1 calc PR A 1
C9A C 0.8320(10) 0.4172(8) 0.8255(10) 0.038(2) Uiso 0.66 1 d PD A 1
H9A1 H 0.8897 0.3849 0.7854 0.057 Uiso 0.66 1 calc PR A 1
H9A2 H 0.7509 0.3593 0.7933 0.057 Uiso 0.66 1 calc PR A 1
H9A3 H 0.8582 0.4334 0.9076 0.057 Uiso 0.66 1 calc PR A 1
C10A C 0.7405(11) 0.5835(11) 0.8718(12) 0.062(4) Uiso 0.66 1 d PD A 1
H10A H 0.7615 0.5922 0.9523 0.093 Uiso 0.66 1 calc PR A 1
H10B H 0.6575 0.5306 0.8347 0.093 Uiso 0.66 1 calc PR A 1
H10C H 0.7457 0.6615 0.8686 0.093 Uiso 0.66 1 calc PR A 1
C8B C 0.8638(19) 0.6617(12) 0.8853(19) 0.050(6) Uiso 0.34 1 d PD A 2
H8B1 H 0.8095 0.6994 0.8544 0.074 Uiso 0.34 1 calc PR A 2
H8B2 H 0.9478 0.6992 0.8867 0.074 Uiso 0.34 1 calc PR A 2
H8B3 H 0.8576 0.6713 0.9636 0.074 Uiso 0.34 1 calc PR A 2
C9B C 0.914(2) 0.471(2) 0.845(3) 0.086(10) Uiso 0.34 1 d PD A 2
H9B1 H 0.8877 0.3875 0.7935 0.130 Uiso 0.34 1 calc PR A 2
H9B2 H 0.9159 0.4778 0.9243 0.130 Uiso 0.34 1 calc PR A 2
H9B3 H 0.9957 0.5092 0.8409 0.130 Uiso 0.34 1 calc PR A 2
C10B C 0.7006(15) 0.474(2) 0.823(3) 0.071(8) Uiso 0.34 1 d PD A 2
H10D H 0.6438 0.5163 0.8052 0.106 Uiso 0.34 1 calc PR A 2
H10E H 0.7069 0.4792 0.9024 0.106 Uiso 0.34 1 calc PR A 2
H10F H 0.6707 0.3907 0.7702 0.106 Uiso 0.34 1 calc PR A 2
O6 O 0.7126(5) 0.7285(4) 0.4866(5) 0.0452(14) Uani 1 1 d . . .
O7 O 0.8204(4) 0.6017(4) 0.4356(4) 0.0332(11) Uani 1 1 d . . .
C11 C 0.7777(6) 0.6841(6) 0.4259(6) 0.0318(15) Uani 1 1 d . B .
C12 C 0.8022(7) 0.7306(7) 0.3349(7) 0.0460(19) Uani 1 1 d D . .
C13A C 0.8792(14) 0.8634(11) 0.4015(13) 0.056(4) Uiso 0.55 1 d PD B 1
H13A H 0.8983 0.8993 0.3464 0.084 Uiso 0.55 1 calc PR B 1
H13B H 0.9549 0.8679 0.4507 0.084 Uiso 0.55 1 calc PR B 1
H13C H 0.8326 0.9064 0.4492 0.084 Uiso 0.55 1 calc PR B 1
C14A C 0.6891(14) 0.7299(17) 0.2587(16) 0.082(6) Uiso 0.55 1 d PD B 1
H14A H 0.7119 0.7615 0.2017 0.123 Uiso 0.55 1 calc PR B 1
H14B H 0.6467 0.7794 0.3057 0.123 Uiso 0.55 1 calc PR B 1
H14C H 0.6353 0.6484 0.2192 0.123 Uiso 0.55 1 calc PR B 1
C15A C 0.8771(13) 0.6681(14) 0.2627(13) 0.035(4) Uiso 0.55 1 d PD B 1
H15A H 0.8909 0.7014 0.2047 0.052 Uiso 0.55 1 calc PR B 1
H15B H 0.8336 0.5832 0.2243 0.052 Uiso 0.55 1 calc PR B 1
H15C H 0.9556 0.6792 0.3121 0.052 Uiso 0.55 1 calc PR B 1
C13B C 0.8184(18) 0.8620(12) 0.3684(18) 0.062(6) Uiso 0.45 1 d PD B 2
H13D H 0.8338 0.8843 0.3040 0.092 Uiso 0.45 1 calc PR B 2
H13E H 0.8875 0.9071 0.4354 0.092 Uiso 0.45 1 calc PR B 2
H13F H 0.7444 0.8797 0.3874 0.092 Uiso 0.45 1 calc PR B 2
C14B C 0.6751(15) 0.6664(19) 0.2456(19) 0.078(7) Uiso 0.45 1 d PD B 2
H14D H 0.6758 0.6887 0.1789 0.118 Uiso 0.45 1 calc PR B 2
H14E H 0.6113 0.6904 0.2816 0.118 Uiso 0.45 1 calc PR B 2
H14F H 0.6589 0.5803 0.2205 0.118 Uiso 0.45 1 calc PR B 2
C15B C 0.898(2) 0.694(2) 0.276(3) 0.113(16) Uiso 0.45 1 d PD B 2
H15D H 0.9067 0.7298 0.2191 0.170 Uiso 0.45 1 calc PR B 2
H15E H 0.8735 0.6075 0.2377 0.170 Uiso 0.45 1 calc PR B 2
H15F H 0.9754 0.7214 0.3333 0.170 Uiso 0.45 1 calc PR B 2
O8 O 0.4501(4) 0.2939(4) 0.2152(4) 0.0344(11) Uani 1 1 d . . .
O9 O 0.6518(4) 0.3408(4) 0.2424(4) 0.0354(11) Uani 1 1 d . . .
C16 C 0.5450(6) 0.3000(6) 0.1788(6) 0.0309(15) Uani 1 1 d . C .
C17 C 0.5311(7) 0.2560(7) 0.0485(6) 0.0431(19) Uani 1 1 d D . .
C18A C 0.6261(11) 0.1950(11) 0.0153(12) 0.066(4) Uiso 0.72 1 d PD C 1
H18A H 0.7073 0.2498 0.0571 0.099 Uiso 0.72 1 calc PR C 1
H18B H 0.6185 0.1708 -0.0676 0.099 Uiso 0.72 1 calc PR C 1
H18C H 0.6141 0.1247 0.0349 0.099 Uiso 0.72 1 calc PR C 1
C19A C 0.5522(10) 0.3673(9) 0.0184(10) 0.049(3) Uiso 0.72 1 d PD C 1
H19A H 0.6330 0.4221 0.0621 0.073 Uiso 0.72 1 calc PR C 1
H19B H 0.4900 0.4067 0.0382 0.073 Uiso 0.72 1 calc PR C 1
H19C H 0.5471 0.3437 -0.0641 0.073 Uiso 0.72 1 calc PR C 1
C20A C 0.4033(9) 0.1751(9) -0.0187(10) 0.047(3) Uiso 0.72 1 d PD C 1
H20A H 0.3984 0.1493 -0.1013 0.070 Uiso 0.72 1 calc PR C 1
H20B H 0.3440 0.2186 0.0002 0.070 Uiso 0.72 1 calc PR C 1
H20C H 0.3856 0.1056 0.0019 0.070 Uiso 0.72 1 calc PR C 1
C18B C 0.515(4) 0.1219(17) 0.012(4) 0.097(14) Uiso 0.28 1 d PD C 2
H18D H 0.4760 0.0929 0.0641 0.145 Uiso 0.28 1 calc PR C 2
H18E H 0.5955 0.1083 0.0160 0.145 Uiso 0.28 1 calc PR C 2
H18F H 0.4650 0.0793 -0.0668 0.145 Uiso 0.28 1 calc PR C 2
C19B C 0.650(3) 0.310(4) 0.022(5) 0.16(3) Uiso 0.28 1 d PD C 2
H19D H 0.6438 0.2740 -0.0605 0.234 Uiso 0.28 1 calc PR C 2
H19E H 0.7180 0.2954 0.0649 0.234 Uiso 0.28 1 calc PR C 2
H19F H 0.6641 0.3960 0.0453 0.234 Uiso 0.28 1 calc PR C 2
C20B C 0.426(4) 0.270(5) -0.028(7) 0.47(12) Uiso 0.28 1 d PD C 2
H20D H 0.3483 0.2229 -0.0245 0.699 Uiso 0.28 1 calc PR C 2
H20E H 0.4335 0.2431 -0.1079 0.699 Uiso 0.28 1 calc PR C 2
H20F H 0.4282 0.3541 -0.0016 0.699 Uiso 0.28 1 calc PR C 2
O10 O 0.3426(4) 0.1210(4) 0.3079(4) 0.0350(11) Uani 1 1 d . . .
O11 O 0.2060(4) 0.2058(4) 0.2661(5) 0.0441(14) Uani 1 1 d . . .
C21 C 0.2374(6) 0.1132(6) 0.2583(6) 0.0350(16) Uani 1 1 d . . .
C22 C 0.1469(7) -0.0081(6) 0.1865(6) 0.0387(17) Uani 1 1 d . . .
C23 C 0.1794(9) -0.1032(7) 0.2234(9) 0.067(3) Uani 1 1 d . . .
H23A H 0.1754 -0.0859 0.3035 0.100 Uiso 1 1 calc R . .
H23B H 0.2620 -0.1041 0.2166 0.100 Uiso 1 1 calc R . .
H23C H 0.1217 -0.1809 0.1739 0.100 Uiso 1 1 calc R . .
C24 C 0.0181(7) -0.0050(8) 0.1976(8) 0.057(2) Uani 1 1 d . . .
H24A H 0.0136 0.0100 0.2773 0.085 Uiso 1 1 calc R . .
H24B H -0.0406 -0.0815 0.1464 0.085 Uiso 1 1 calc R . .
H24C H -0.0009 0.0584 0.1762 0.085 Uiso 1 1 calc R . .
C25 C 0.1518(9) -0.0320(8) 0.0611(8) 0.059(2) Uani 1 1 d . . .
H25A H 0.2339 -0.0334 0.0528 0.089 Uiso 1 1 calc R . .
H25B H 0.1314 0.0310 0.0398 0.089 Uiso 1 1 calc R . .
H25C H 0.0932 -0.1087 0.0105 0.089 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'
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'
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
O2 Dy1 O6 94.29(18) . 2_666 ?
O2 Dy1 O4 152.00(15) . 2_666 ?
O6 Dy1 O4 97.05(17) 2_666 2_666 ?
O2 Dy1 O8 90.21(16) . . ?
O6 Dy1 O8 150.15(17) 2_666 . ?
O4 Dy1 O8 92.50(16) 2_666 . ?
O2 Dy1 O1 71.85(15) . . ?
O6 Dy1 O1 135.12(16) 2_666 . ?
O4 Dy1 O1 82.12(14) 2_666 . ?
O8 Dy1 O1 74.15(16) . . ?
O2 Dy1 O11 133.93(16) . . ?
O6 Dy1 O11 76.0(2) 2_666 . ?
O4 Dy1 O11 73.85(15) 2_666 . ?
O8 Dy1 O11 79.70(18) . . ?
O1 Dy1 O11 143.42(18) . . ?
O2 Dy1 O10 79.49(15) . . ?
O6 Dy1 O10 75.98(17) 2_666 . ?
O4 Dy1 O10 128.13(15) 2_666 . ?
O8 Dy1 O10 75.88(17) . . ?
O1 Dy1 O10 137.94(15) . . ?
O11 Dy1 O10 54.44(16) . . ?
O2 Dy1 O1 87.48(14) . 2_666 ?
O6 Dy1 O1 70.94(16) 2_666 2_666 ?
O4 Dy1 O1 72.34(14) 2_666 2_666 ?
O8 Dy1 O1 138.82(16) . 2_666 ?
O1 Dy1 O1 66.10(17) . 2_666 ?
O11 Dy1 O1 128.47(16) . 2_666 ?
O10 Dy1 O1 143.30(16) . 2_666 ?
O2 Dy2 O9 94.22(17) . . ?
O2 Dy2 O7 149.24(15) . . ?
O9 Dy2 O7 91.78(18) . . ?
O2 Dy2 O1 73.04(15) . . ?
O9 Dy2 O1 79.70(15) . . ?
O7 Dy2 O1 78.44(15) . . ?
O2 Dy2 O3 134.69(16) . . ?
O9 Dy2 O3 80.81(18) . . ?
O7 Dy2 O3 76.06(16) . . ?
O1 Dy2 O3 147.19(17) . . ?
O2 Dy2 O5 94.09(15) . . ?
O9 Dy2 O5 157.60(15) . . ?
O7 Dy2 O5 91.65(16) . . ?
O1 Dy2 O5 122.65(14) . . ?
O3 Dy2 O5 78.57(16) . . ?
O2 Dy2 O4 75.39(15) . . ?
O9 Dy2 O4 150.80(15) . . ?
O7 Dy2 O4 84.82(16) . . ?
O1 Dy2 O4 71.19(14) . . ?
O3 Dy2 O4 125.89(16) . . ?
O5 Dy2 O4 51.59(13) . . ?
O2 Dy2 N1 67.15(16) . . ?
O9 Dy2 N1 82.83(18) . . ?
O7 Dy2 N1 143.60(17) . . ?
O1 Dy2 N1 134.88(16) . . ?
O3 Dy2 N1 67.55(17) . . ?
O5 Dy2 N1 81.32(16) . . ?
O4 Dy2 N1 116.27(16) . . ?
Dy2 O1 Dy1 101.72(16) . . ?
Dy2 O1 Dy1 106.50(16) . 2_666 ?
Dy1 O1 Dy1 113.90(17) . 2_666 ?
Dy2 O1 H1 115(5) . . ?
Dy1 O1 H1 104(5) . . ?
Dy1 O1 H1 116(5) 2_666 . ?
C3 N1 C1 110.7(6) . . ?
C3 N1 C5 110.6(6) . . ?
C1 N1 C5 108.5(6) . . ?
C3 N1 Dy2 109.5(4) . . ?
C1 N1 Dy2 102.5(4) . . ?
C5 N1 Dy2 114.8(4) . . ?
N1 C1 C2 109.8(6) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
O2 C2 C1 109.7(6) . . ?
O2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
O2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C2 O2 Dy2 123.8(4) . . ?
C2 O2 Dy1 125.9(4) . . ?
Dy2 O2 Dy1 106.97(17) . . ?
N1 C3 C4 110.3(6) . . ?
N1 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
O3 C4 C3 106.0(6) . . ?
O3 C4 H4A 110.5 . . ?
C3 C4 H4A 110.5 . . ?
O3 C4 H4B 110.5 . . ?
C3 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
C4 O3 Dy2 121.0(4) . . ?
C4 O3 H3 121(6) . . ?
Dy2 O3 H3 115(6) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 O4 Dy1 156.7(4) . 2_666 ?
C6 O4 Dy2 91.9(4) . . ?
Dy1 O4 Dy2 102.43(16) 2_666 . ?
C6 O5 Dy2 96.0(4) . . ?
O5 C6 O4 119.1(6) . . ?
O5 C6 C7 119.9(5) . . ?
O4 C6 C7 120.9(6) . . ?
C9B C7 C8B 112.4(11) . . ?
C9B C7 C6 114.6(14) . . ?
C10A C7 C6 114.0(7) . . ?
C8B C7 C6 110.5(11) . . ?
C10A C7 C9A 110.6(7) . . ?
C6 C7 C9A 111.0(6) . . ?
C9B C7 C10B 108.5(11) . . ?
C8B C7 C10B 107.2(10) . . ?
C6 C7 C10B 102.9(12) . . ?
C10A C7 C8A 108.5(7) . . ?
C6 C7 C8A 106.7(7) . . ?
C9A C7 C8A 105.5(7) . . ?
C7 C8A H8A1 109.5 . . ?
C7 C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7 C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C7 C9A H9A1 109.5 . . ?
C7 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C7 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C7 C10A H10A 109.5 . . ?
C7 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C7 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C7 C8B H8B1 109.5 . . ?
C7 C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7 C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C7 C9B H9B1 109.5 . . ?
C7 C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C7 C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C7 C10B H10D 109.5 . . ?
C7 C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C7 C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C11 O6 Dy1 132.6(5) . 2_666 ?
C11 O7 Dy2 131.4(4) . . ?
O6 C11 O7 124.0(7) . . ?
O6 C11 C12 116.2(6) . . ?
O7 C11 C12 119.8(6) . . ?
C11 C12 C15B 116.4(16) . . ?
C11 C12 C14A 113.9(11) . . ?
C11 C12 C15A 112.4(8) . . ?
C14A C12 C15A 110.2(9) . . ?
C11 C12 C13B 115.2(10) . . ?
C15B C12 C13B 111.1(12) . . ?
C11 C12 C13A 105.4(8) . . ?
C14A C12 C13A 106.7(9) . . ?
C15A C12 C13A 107.6(9) . . ?
C11 C12 C14B 99.1(11) . . ?
C15B C12 C14B 108.0(11) . . ?
C13B C12 C14B 105.5(10) . . ?
C12 C13A H13A 109.5 . . ?
C12 C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C12 C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C12 C14A H14A 109.5 . . ?
C12 C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
C12 C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C12 C15A H15A 109.5 . . ?
C12 C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
C12 C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C12 C13B H13D 109.5 . . ?
C12 C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C12 C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C12 C14B H14D 109.5 . . ?
C12 C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C12 C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C12 C15B H15D 109.5 . . ?
C12 C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C12 C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C16 O8 Dy1 137.9(4) . . ?
C16 O9 Dy2 133.0(4) . . ?
O8 C16 O9 124.5(6) . . ?
O8 C16 C17 118.1(6) . . ?
O9 C16 C17 117.4(6) . . ?
C18A C17 C20A 111.1(7) . . ?
C18A C17 C16 110.5(7) . . ?
C20A C17 C16 112.2(7) . . ?
C16 C17 C20B 120(4) . . ?
C16 C17 C19B 110(2) . . ?
C20B C17 C19B 108.0(16) . . ?
C16 C17 C18B 103.6(18) . . ?
C20B C17 C18B 107.6(16) . . ?
C19B C17 C18B 106.9(14) . . ?
C18A C17 C19A 108.8(7) . . ?
C20A C17 C19A 107.6(7) . . ?
C16 C17 C19A 106.5(7) . . ?
C17 C18A H18A 109.5 . . ?
C17 C18A H18B 109.5 . . ?
H18A C18A H18B 109.5 . . ?
C17 C18A H18C 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C17 C19A H19A 109.5 . . ?
C17 C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
C17 C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C17 C20A H20A 109.5 . . ?
C17 C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
C17 C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C17 C18B H18D 109.5 . . ?
C17 C18B H18E 109.5 . . ?
H18D C18B H18E 109.5 . . ?
C17 C18B H18F 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
C17 C19B H19D 109.5 . . ?
C17 C19B H19E 109.5 . . ?
H19D C19B H19E 109.5 . . ?
C17 C19B H19F 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C17 C20B H20D 109.5 . . ?
C17 C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
C17 C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C21 O10 Dy1 92.4(4) . . ?
C21 O11 Dy1 92.3(4) . . ?
O10 C21 O11 120.7(6) . . ?
O10 C21 C22 120.0(6) . . ?
O11 C21 C22 119.3(6) . . ?
C23 C22 C21 111.0(6) . . ?
C23 C22 C24 110.1(7) . . ?
C21 C22 C24 109.9(6) . . ?
C23 C22 C25 111.2(7) . . ?
C21 C22 C25 106.0(6) . . ?
C24 C22 C25 108.6(7) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
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 O2 2.284(4) . ?
Dy1 O6 2.343(5) 2_666 ?
Dy1 O4 2.370(4) 2_666 ?
Dy1 O8 2.372(5) . ?
Dy1 O1 2.373(4) . ?
Dy1 O11 2.397(5) . ?
Dy1 O10 2.402(5) . ?
Dy1 O1 2.447(4) 2_666 ?
Dy2 O2 2.258(4) . ?
Dy2 O9 2.286(5) . ?
Dy2 O7 2.299(5) . ?
Dy2 O1 2.334(4) . ?
Dy2 O3 2.410(5) . ?
Dy2 O5 2.458(4) . ?
Dy2 O4 2.543(4) . ?
Dy2 N1 2.576(5) . ?
O1 Dy1 2.447(4) 2_666 ?
O1 H1 0.86(4) . ?
N1 C3 1.473(9) . ?
N1 C1 1.481(10) . ?
N1 C5 1.487(10) . ?
C1 C2 1.525(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O2 1.434(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.534(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.475(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O3 H3 0.85(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
O4 C6 1.263(7) . ?
O4 Dy1 2.370(4) 2_666 ?
O5 C6 1.263(7) . ?
C6 C7 1.513(9) . ?
C7 C9B 1.487(14) . ?
C7 C10A 1.499(11) . ?
C7 C8B 1.504(13) . ?
C7 C9A 1.521(10) . ?
C7 C10B 1.552(14) . ?
C7 C8A 1.553(11) . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
O6 C11 1.246(8) . ?
O6 Dy1 2.343(5) 2_666 ?
O7 C11 1.276(8) . ?
C11 C12 1.498(10) . ?
C12 C15B 1.500(14) . ?
C12 C14A 1.509(13) . ?
C12 C15A 1.510(11) . ?
C12 C13B 1.512(13) . ?
C12 C13A 1.563(12) . ?
C12 C14B 1.573(13) . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
O8 C16 1.257(8) . ?
O9 C16 1.263(8) . ?
C16 C17 1.531(10) . ?
C17 C18A 1.511(11) . ?
C17 C20A 1.525(11) . ?
C17 C20B 1.532(17) . ?
C17 C19B 1.537(17) . ?
C17 C18B 1.543(16) . ?
C17 C19A 1.546(11) . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
O10 C21 1.257(8) . ?
O11 C21 1.269(8) . ?
C21 C22 1.520(9) . ?
C22 C23 1.519(11) . ?
C22 C24 1.533(11) . ?
C22 C25 1.536(12) . ?
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 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
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
O3 H3 O5 0.85(4) 2.13(6) 2.777(7) 133(7) 2_766
