#------------------------------------------------------------------------------
#$Date: 2019-11-22 23:40:59 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231584 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/60/4346020.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_4346020
loop_
_publ_author_name
'Luan, Fang'
'Liu, Tianqi'
'Yan, Pengfei'
'Zou, Xiaoyan'
'Li, Yuxin'
'Li, Guangming'
_publ_section_title
;
 Single-molecule magnet of a tetranuclear dysprosium complex disturbed by
 a salen-type ligand and chloride counterions.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3485
_journal_page_last               3490
_journal_paper_doi               10.1021/acs.inorgchem.5b00061
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
' 2(C88 H100 Cl2 Dy4 N8 O18), 3(C2 H6 O), 0.5(O2), 2(Cl), 2(O)  '
_chemical_formula_sum            'C182 H218 Cl6 Dy8 N16 O42'
_chemical_formula_weight         4814.44
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 132.218(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   18.4659(5)
_cell_length_b                   16.3855(4)
_cell_length_c                   25.4416(7)
_cell_measurement_temperature    293(2)
_cell_volume                     5701.0(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25349
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    2.722
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs(Sheldrick,1996)
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.492
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         10036
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0828P)²+26.7060P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                6814
_reflns_number_total             10036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00061_si_002.cif
_cod_data_source_block           lf1
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4346020
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Dy1 Dy 0.59645(2) -0.53800(2) 0.001064(16) 0.02885(9) Uani 1 1 d .
Dy2 Dy 0.35417(2) -0.55065(2) -0.164087(16) 0.03339(10) Uani 1 1 d .
Cl1 Cl 0.2719(2) -0.4031(3) -0.21563(15) 0.1077(12) Uani 1 1 d .
O1 O 0.4664(3) -0.6315(3) -0.0625(2) 0.0362(13) Uani 1 1 d .
O2 O 0.2878(3) -0.6879(3) -0.1535(3) 0.0426(15) Uani 1 1 d .
O3 O 0.5175(3) -0.5428(3) -0.1170(2) 0.0366(14) Uani 1 1 d .
O4 O 0.3843(4) -0.4933(4) -0.2455(3) 0.0510(17) Uani 1 1 d .
O5 O 0.2212(3) -0.5901(3) -0.2760(2) 0.0443(16) Uani 1 1 d .
O6 O 0.3801(3) -0.6741(3) -0.2138(3) 0.0475(17) Uani 1 1 d .
O7 O 0.2831(3) -0.5243(3) -0.1113(2) 0.0341(13) Uani 1 1 d .
O8 O 0.3381(3) -0.5932(3) 0.0035(2) 0.0401(14) Uani 1 1 d .
O9 O 0.4514(3) -0.4609(3) -0.0654(2) 0.0307(13) Uani 1 1 d .
H91 H 0.4959 -0.4268 -0.0514 0.037 Uiso 1 1 d R
N1 N 0.6658(4) -0.6693(4) 0.0576(3) 0.0387(18) Uani 1 1 d .
N2 N 0.7179(4) -0.5902(4) -0.0038(3) 0.0395(17) Uani 1 1 d .
N3 N 0.0350(4) -0.5673(4) -0.3868(3) 0.047(2) Uani 1 1 d .
H311 H 0.0797 -0.5530 -0.3404 0.057 Uiso 1 1 d R
N4 N -0.0080(4) -0.5178(5) -0.3017(3) 0.049(2) Uani 1 1 d .
C1 C 0.4514(5) -0.7010(4) -0.0440(4) 0.035(2) Uani 1 1 d .
C2 C 0.3535(5) -0.7321(5) -0.0916(4) 0.044(2) Uani 1 1 d .
C3 C 0.3299(6) -0.8043(6) -0.0765(5) 0.071(3) Uani 1 1 d .
H3 H 0.2663 -0.8244 -0.1077 0.085 Uiso 1 1 calc R
C4 C 0.4043(7) -0.8454(6) -0.0137(6) 0.086(4) Uani 1 1 d .
H4 H 0.3894 -0.8918 -0.0016 0.104 Uiso 1 1 calc R
C5 C 0.4994(6) -0.8181(6) 0.0307(5) 0.072(3) Uani 1 1 d .
H5 H 0.5480 -0.8481 0.0712 0.087 Uiso 1 1 calc R
C6 C 0.5248(5) -0.7467(5) 0.0165(4) 0.044(2) Uani 1 1 d .
C7 C 0.6280(5) -0.7304(5) 0.0601(4) 0.048(3) Uani 1 1 d .
H7 H 0.6708 -0.7698 0.0936 0.057 Uiso 1 1 calc R
C8 C 0.7719(5) -0.6651(6) 0.0987(4) 0.057(3) Uani 1 1 d .
H8 H 0.7928 -0.6149 0.1265 0.068 Uiso 1 1 calc R
C9 C 0.8387(6) -0.7295(6) 0.1532(5) 0.059(3) Uani 1 1 d .
H9A H 0.8291 -0.7330 0.1862 0.071 Uiso 1 1 calc R
H9B H 0.8213 -0.7819 0.1296 0.071 Uiso 1 1 calc R
C10 C 0.9442(6) -0.7127(7) 0.1937(5) 0.081(4) Uani 1 1 d .
H10A H 0.9658 -0.6678 0.2262 0.098 Uiso 1 1 calc R
H10B H 0.9824 -0.7604 0.2217 0.098 Uiso 1 1 calc R
C11 C 0.9630(7) -0.6924(8) 0.1479(5) 0.086(4) Uani 1 1 d .
H11A H 0.9590 -0.7422 0.1253 0.103 Uiso 1 1 calc R
H11B H 1.0294 -0.6722 0.1773 0.103 Uiso 1 1 calc R
C12 C 0.8945(5) -0.6298(6) 0.0904(4) 0.059(3) Uani 1 1 d .
H12A H 0.9108 -0.5760 0.1115 0.071 Uiso 1 1 calc R
H12B H 0.9028 -0.6294 0.0566 0.071 Uiso 1 1 calc R
C13 C 0.7897(5) -0.6491(6) 0.0524(4) 0.058(3) Uani 1 1 d .
H13 H 0.7757 -0.7006 0.0275 0.070 Uiso 1 1 calc R
C14 C 0.7176(5) -0.5785(6) -0.0529(4) 0.052(3) Uani 1 1 d .
H14 H 0.7708 -0.5993 -0.0454 0.062 Uiso 1 1 calc R
C15 C 0.6445(5) -0.5367(5) -0.1194(4) 0.048(2) Uani 1 1 d .
C16 C 0.6677(6) -0.5120(7) -0.1600(5) 0.066(3) Uani 1 1 d .
H16 H 0.7310 -0.5201 -0.1413 0.079 Uiso 1 1 calc R
C17 C 0.6014(6) -0.4769(7) -0.2250(5) 0.073(3) Uani 1 1 d .
H17 H 0.6216 -0.4585 -0.2480 0.087 Uiso 1 1 calc R
C18 C 0.5039(6) -0.4679(6) -0.2581(5) 0.068(3) Uani 1 1 d .
H18 H 0.4579 -0.4459 -0.3034 0.082 Uiso 1 1 calc R
C19 C 0.4779(5) -0.4935(5) -0.2200(4) 0.044(2) Uani 1 1 d .
C20 C 0.5475(5) -0.5242(5) -0.1499(4) 0.039(2) Uani 1 1 d .
C21 C 0.3095(6) -0.4639(6) -0.3180(4) 0.063(3) Uani 1 1 d .
H21A H 0.3277 -0.4111 -0.3221 0.095 Uiso 1 1 calc R
H21B H 0.2481 -0.4600 -0.3298 0.095 Uiso 1 1 calc R
H21C H 0.3033 -0.5012 -0.3499 0.095 Uiso 1 1 calc R
C22 C 0.1921(5) -0.7216(5) -0.2035(4) 0.055(3) Uani 1 1 d .
H22A H 0.1946 -0.7725 -0.2209 0.083 Uiso 1 1 calc R
H22B H 0.1501 -0.6843 -0.2424 0.083 Uiso 1 1 calc R
H22C H 0.1671 -0.7305 -0.1809 0.083 Uiso 1 1 calc R
C23 C 0.2149(5) -0.6533(5) -0.3116(4) 0.042(2) Uani 1 1 d .
C24 C 0.2994(5) -0.7020(5) -0.2791(4) 0.047(2) Uani 1 1 d .
C25 C 0.2934(6) -0.7696(6) -0.3134(5) 0.062(3) Uani 1 1 d .
H25 H 0.3493 -0.8005 -0.2920 0.074 Uiso 1 1 calc R
C26 C 0.2066(7) -0.7929(6) -0.3789(5) 0.075(4) Uani 1 1 d .
H26 H 0.2042 -0.8396 -0.4008 0.090 Uiso 1 1 calc R
C27 C 0.1232(7) -0.7469(6) -0.4117(5) 0.069(3) Uani 1 1 d .
H27 H 0.0645 -0.7627 -0.4558 0.083 Uiso 1 1 calc R
C28 C 0.1269(5) -0.6763(5) -0.3786(4) 0.046(2) Uani 1 1 d .
C29 C 0.0387(5) -0.6326(5) -0.4117(4) 0.048(3) Uani 1 1 d .
H29 H -0.0193 -0.6530 -0.4539 0.058 Uiso 1 1 calc R
C30 C -0.0544(5) -0.5201(5) -0.4166(4) 0.047(2) Uani 1 1 d .
H30 H -0.1067 -0.5585 -0.4329 0.056 Uiso 1 1 calc R
C31 C -0.0867(6) -0.4699(6) -0.4801(4) 0.061(3) Uani 1 1 d .
H31A H -0.0335 -0.4348 -0.4653 0.074 Uiso 1 1 calc R
H31B H -0.1025 -0.5063 -0.5166 0.074 Uiso 1 1 calc R
C32 C -0.1755(6) -0.4184(7) -0.5098(5) 0.070(3) Uani 1 1 d .
H32A H -0.2304 -0.4537 -0.5283 0.084 Uiso 1 1 calc R
H32B H -0.1934 -0.3850 -0.5485 0.084 Uiso 1 1 calc R
C33 C -0.1531(7) -0.3635(6) -0.4518(5) 0.073(3) Uani 1 1 d .
H33A H -0.1016 -0.3255 -0.4360 0.087 Uiso 1 1 calc R
H33B H -0.2109 -0.3321 -0.4711 0.087 Uiso 1 1 calc R
C34 C -0.1213(6) -0.4130(7) -0.3887(4) 0.064(3) Uani 1 1 d .
H34A H -0.1750 -0.4474 -0.4035 0.077 Uiso 1 1 calc R
H34B H -0.1052 -0.3762 -0.3522 0.077 Uiso 1 1 calc R
C35 C -0.0327(5) -0.4661(6) -0.3580(4) 0.050(3) Uani 1 1 d .
H35 H 0.0232 -0.4308 -0.3388 0.060 Uiso 1 1 calc R
C36 C 0.0785(5) -0.5150(5) -0.2420(4) 0.041(2) Uani 1 1 d .
H36 H 0.1233 -0.4814 -0.2372 0.049 Uiso 1 1 calc R
C37 C 0.1120(5) -0.5613(5) -0.1803(4) 0.038(2) Uani 1 1 d .
C38 C 0.0453(5) -0.6024(6) -0.1808(4) 0.051(3) Uani 1 1 d .
H38 H -0.0207 -0.6025 -0.2219 0.062 Uiso 1 1 calc R
C39 C 0.0752(6) -0.6419(6) -0.1225(5) 0.063(3) Uani 1 1 d .
H39 H 0.0296 -0.6707 -0.1249 0.075 Uiso 1 1 calc R
C40 C 0.1715(6) -0.6408(6) -0.0595(5) 0.058(3) Uani 1 1 d .
H40 H 0.1903 -0.6665 -0.0193 0.069 Uiso 1 1 calc R
C41 C 0.2390(5) -0.6010(5) -0.0570(4) 0.039(2) Uani 1 1 d .
C42 C 0.2114(5) -0.5615(4) -0.1169(4) 0.037(2) Uani 1 1 d .
C43 C 0.3793(6) -0.6495(5) 0.0609(4) 0.052(3) Uani 1 1 d .
H43A H 0.3484 -0.6421 0.0793 0.078 Uiso 1 1 calc R
H43B H 0.4482 -0.6395 0.0978 0.078 Uiso 1 1 calc R
H43C H 0.3689 -0.7044 0.0438 0.078 Uiso 1 1 calc R
C44 C 0.4658(6) -0.7252(6) -0.1743(5) 0.065(3) Uani 1 1 d .
H44A H 0.4509 -0.7777 -0.1668 0.098 Uiso 1 1 calc R
H44B H 0.5177 -0.7003 -0.1293 0.098 Uiso 1 1 calc R
H44C H 0.4857 -0.7316 -0.2005 0.098 Uiso 1 1 calc R
O10 O -0.3645(11) -0.6359(13) -0.5836(8) 0.134(7) Uiso 0.50 1 d PD
H10 H -0.3097 -0.6335 -0.5699 0.200 Uiso 0.50 1 calc PR
C45 C -0.3611(14) -0.6107(15) -0.5333(10) 0.093(8) Uiso 0.50 1 d PD
H45A H -0.3608 -0.6577 -0.5101 0.112 Uiso 0.50 1 calc PR
H45B H -0.3003 -0.5814 -0.4983 0.112 Uiso 0.50 1 calc PR
C46 C -0.4231(16) -0.5702(15) -0.5524(12) 0.090(8) Uiso 0.50 1 d P
H46A H -0.4198 -0.5206 -0.5708 0.135 Uiso 0.50 1 calc PR
H46B H -0.4192 -0.5577 -0.5137 0.135 Uiso 0.50 1 calc PR
H46C H -0.4838 -0.5974 -0.5892 0.135 Uiso 0.50 1 calc PR
Cl2 Cl 0.1863(4) -0.2890(4) -0.4471(2) 0.100(2) Uani 0.50 1 d P
O13 O -0.002(3) -0.532(2) -0.014(2) 0.121(14) Uiso 0.25 1 d P
O14 O 0.103(3) -0.288(3) -0.377(2) 0.136(15) Uiso 0.25 1 d P
O11 O 0.5079(11) -0.694(2) -0.2940(14) 0.127(14) Uiso 0.25 1 d PD
H99 H 0.4558 -0.6624 -0.3356 0.152 Uiso 0.25 1 d PRD
C47 C 0.6278(12) -0.686(3) -0.2893(13) 0.089(15) Uiso 0.25 1 d PD
H47A H 0.6917 -0.7092 -0.2610 0.134 Uiso 0.25 1 calc PR
H47B H 0.6334 -0.6272 -0.2844 0.134 Uiso 0.25 1 calc PR
H47C H 0.5897 -0.6999 -0.3382 0.134 Uiso 0.25 1 calc PR
C48 C 0.5909(14) -0.709(3) -0.2711(16) 0.104(18) Uiso 0.25 1 d PD
H48A H 0.6353 -0.6959 -0.2209 0.125 Uiso 0.25 1 calc PR
H48B H 0.5929 -0.7681 -0.2736 0.125 Uiso 0.25 1 calc PR
O12 O -0.237(3) -0.520(3) -0.287(3) 0.18(2) Uiso 0.25 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1890 4.4100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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
O3 Dy1 O9 135.50(16) . 3_645
O3 Dy1 O7 147.16(18) . 3_645
O9 Dy1 O7 70.37(17) 3_645 3_645
O3 Dy1 O1 67.68(19) . .
O9 Dy1 O1 77.44(18) 3_645 .
O7 Dy1 O1 144.97(19) 3_645 .
O3 Dy1 O9 70.30(18) . .
O9 Dy1 O9 73.88(18) 3_645 .
O7 Dy1 O9 109.46(16) 3_645 .
O1 Dy1 O9 73.26(16) . .
O3 Dy1 N1 111.4(2) . .
O9 Dy1 N1 82.8(2) 3_645 .
O7 Dy1 N1 88.76(17) 3_645 .
O1 Dy1 N1 73.56(17) . .
O9 Dy1 N1 142.72(19) . .
O3 Dy1 N2 73.96(18) . .
O9 Dy1 N2 144.77(18) 3_645 .
O7 Dy1 N2 92.69(18) 3_645 .
O1 Dy1 N2 106.37(19) . .
O9 Dy1 N2 141.3(2) . .
N1 Dy1 N2 65.7(2) . .
O3 Dy1 O8 82.58(17) . 3_645
O9 Dy1 O8 117.56(17) 3_645 3_645
O7 Dy1 O8 65.29(17) 3_645 3_645
O1 Dy1 O8 146.08(15) . 3_645
O9 Dy1 O8 81.84(16) . 3_645
N1 Dy1 O8 135.27(18) . 3_645
N2 Dy1 O8 79.2(2) . 3_645
O3 Dy1 Dy2 42.04(13) . .
O9 Dy1 Dy2 93.46(9) 3_645 .
O7 Dy1 Dy2 151.24(12) 3_645 .
O1 Dy1 Dy2 41.40(11) . .
O9 Dy1 Dy2 41.94(11) . .
N1 Dy1 Dy2 113.35(13) . .
N2 Dy1 Dy2 112.71(13) . .
O8 Dy1 Dy2 105.09(10) 3_645 .
O3 Dy1 Dy1 103.35(13) . 3_645
O9 Dy1 Dy1 37.23(10) 3_645 3_645
O7 Dy1 Dy1 90.06(13) 3_645 3_645
O1 Dy1 Dy1 71.55(13) . 3_645
O9 Dy1 Dy1 36.65(13) . 3_645
N1 Dy1 Dy1 115.03(17) . 3_645
N2 Dy1 Dy1 177.18(13) . 3_645
O8 Dy1 Dy1 101.42(13) 3_645 3_645
Dy2 Dy1 Dy1 64.473(10) . 3_645
O3 Dy1 Dy2 153.86(13) . 3_645
O9 Dy1 Dy2 34.71(10) 3_645 3_645
O7 Dy1 Dy2 37.24(13) 3_645 3_645
O1 Dy1 Dy2 112.16(15) . 3_645
O9 Dy1 Dy2 84.45(12) . 3_645
N1 Dy1 Dy2 92.71(16) . 3_645
N2 Dy1 Dy2 127.69(13) . 3_645
O8 Dy1 Dy2 87.37(13) 3_645 3_645
Dy2 Dy1 Dy2 119.603(11) . 3_645
Dy1 Dy1 Dy2 55.129(10) 3_645 3_645
O3 Dy1 H91 73.2 . .
O9 Dy1 H91 82.7 3_645 .
O7 Dy1 H91 95.6 3_645 .
O1 Dy1 H91 93.7 . .
O9 Dy1 H91 21.0 . .
N1 Dy1 H91 162.5 . .
N2 Dy1 H91 130.8 . .
O8 Dy1 H91 61.1 3_645 .
Dy2 Dy1 H91 57.9 . .
Dy1 Dy1 H91 48.2 3_645 .
Dy2 Dy1 H91 80.8 3_645 .
O5 Dy2 O1 129.02(18) . .
O5 Dy2 O9 156.14(17) . .
O1 Dy2 O9 72.82(16) . .
O5 Dy2 O3 125.6(2) . .
O1 Dy2 O3 66.13(18) . .
O9 Dy2 O3 68.46(17) . .
O5 Dy2 O7 102.07(19) . .
O1 Dy2 O7 84.18(17) . .
O9 Dy2 O7 67.43(16) . .
O3 Dy2 O7 132.27(15) . .
O5 Dy2 O6 64.24(17) . .
O1 Dy2 O6 77.42(17) . .
O9 Dy2 O6 137.97(15) . .
O3 Dy2 O6 72.68(17) . .
O7 Dy2 O6 137.91(18) . .
O5 Dy2 O4 74.89(19) . .
O1 Dy2 O4 124.46(18) . .
O9 Dy2 O4 101.58(18) . .
O3 Dy2 O4 61.03(16) . .
O7 Dy2 O4 146.20(17) . .
O6 Dy2 O4 72.00(19) . .
O5 Dy2 O2 72.68(18) . .
O1 Dy2 O2 62.50(15) . .
O9 Dy2 O2 119.31(17) . .
O3 Dy2 O2 120.50(16) . .
O7 Dy2 O2 69.12(17) . .
O6 Dy2 O2 68.80(19) . .
O4 Dy2 O2 136.96(18) . .
O5 Dy2 Cl1 82.15(15) . .
O1 Dy2 Cl1 146.73(14) . .
O9 Dy2 Cl1 74.69(12) . .
O3 Dy2 Cl1 107.83(15) . .
O7 Dy2 Cl1 76.97(14) . .
O6 Dy2 Cl1 133.90(14) . .
O4 Dy2 Cl1 69.26(15) . .
O2 Dy2 Cl1 131.59(13) . .
O5 Dy2 Dy1 161.32(15) . .
O1 Dy2 Dy1 41.28(11) . .
O9 Dy2 Dy1 41.53(10) . .
O3 Dy2 Dy1 40.10(12) . .
O7 Dy2 Dy1 93.12(9) . .
O6 Dy2 Dy1 97.17(9) . .
O4 Dy2 Dy1 98.39(10) . .
O2 Dy2 Dy1 103.35(9) . .
Cl1 Dy2 Dy1 112.18(7) . .
O5 Dy2 Dy1 136.52(16) . 3_645
O1 Dy2 Dy1 68.61(13) . 3_645
O9 Dy2 Dy1 33.87(13) . 3_645
O3 Dy2 Dy1 97.63(12) . 3_645
O7 Dy2 Dy1 35.05(9) . 3_645
O6 Dy2 Dy1 145.59(12) . 3_645
O4 Dy2 Dy1 132.87(13) . 3_645
O2 Dy2 Dy1 90.13(13) . 3_645
Cl1 Dy2 Dy1 80.47(7) . 3_645
Dy1 Dy2 Dy1 60.398(11) . 3_645
C1 O1 Dy1 132.5(4) . .
C1 O1 Dy2 129.2(4) . .
Dy1 O1 Dy2 97.32(19) . .
C2 O2 C22 115.3(6) . .
C2 O2 Dy2 116.6(4) . .
C22 O2 Dy2 128.1(5) . .
C20 O3 Dy1 131.1(4) . .
C20 O3 Dy2 128.7(4) . .
Dy1 O3 Dy2 97.9(2) . .
C19 O4 C21 114.8(7) . .
C19 O4 Dy2 119.0(4) . .
C21 O4 Dy2 126.1(5) . .
C23 O5 Dy2 127.0(4) . .
C24 O6 C44 116.3(6) . .
C24 O6 Dy2 116.5(5) . .
C44 O6 Dy2 126.0(5) . .
C42 O7 Dy1 113.0(4) . 3_645
C42 O7 Dy2 133.9(4) . .
Dy1 O7 Dy2 107.71(17) 3_645 .
C41 O8 C43 118.0(6) . .
C41 O8 Dy1 110.0(4) . 3_645
C43 O8 Dy1 130.8(4) . 3_645
Dy1 O9 Dy1 106.12(18) 3_645 .
Dy1 O9 Dy2 111.42(19) 3_645 .
Dy1 O9 Dy2 96.52(17) . .
Dy1 O9 H91 115.4 3_645 .
Dy1 O9 H91 74.8 . .
Dy2 O9 H91 133.0 . .
C7 N1 C8 121.6(6) . .
C7 N1 Dy1 130.8(5) . .
C8 N1 Dy1 107.4(5) . .
C14 N2 C13 117.4(7) . .
C14 N2 Dy1 126.6(5) . .
C13 N2 Dy1 115.5(6) . .
C29 N3 C30 126.6(6) . .
C29 N3 H311 124.2 . .
C30 N3 H311 104.9 . .
C36 N4 C35 118.1(8) . .
O1 C1 C6 124.6(6) . .
O1 C1 C2 116.7(6) . .
C6 C1 C2 118.6(7) . .
O2 C2 C3 124.0(6) . .
O2 C2 C1 114.8(7) . .
C3 C2 C1 121.1(7) . .
C4 C3 C2 118.3(8) . .
C4 C3 H3 120.8 . .
C2 C3 H3 120.8 . .
C5 C4 C3 121.0(10) . .
C5 C4 H4 119.5 . .
C3 C4 H4 119.5 . .
C4 C5 C6 121.7(8) . .
C4 C5 H5 119.2 . .
C6 C5 H5 119.2 . .
C5 C6 C1 119.1(7) . .
C5 C6 C7 117.1(7) . .
C1 C6 C7 123.1(8) . .
N1 C7 C6 127.2(7) . .
N1 C7 H7 116.4 . .
C6 C7 H7 116.4 . .
C13 C8 N1 110.6(6) . .
C13 C8 C9 112.6(9) . .
N1 C8 C9 119.8(8) . .
C13 C8 H8 104.0 . .
N1 C8 H8 104.0 . .
C9 C8 H8 104.0 . .
C10 C9 C8 112.9(9) . .
C10 C9 H9A 109.0 . .
C8 C9 H9A 109.0 . .
C10 C9 H9B 109.0 . .
C8 C9 H9B 109.0 . .
H9A C9 H9B 107.8 . .
C11 C10 C9 112.9(8) . .
C11 C10 H10A 109.0 . .
C9 C10 H10A 109.0 . .
C11 C10 H10B 109.0 . .
C9 C10 H10B 109.0 . .
H10A C10 H10B 107.8 . .
C10 C11 C12 115.6(9) . .
C10 C11 H11A 108.4 . .
C12 C11 H11A 108.4 . .
C10 C11 H11B 108.4 . .
C12 C11 H11B 108.4 . .
H11A C11 H11B 107.4 . .
C13 C12 C11 110.9(9) . .
C13 C12 H12A 109.5 . .
C11 C12 H12A 109.5 . .
C13 C12 H12B 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 108.0 . .
C8 C13 N2 111.0(7) . .
C8 C13 C12 114.4(7) . .
N2 C13 C12 114.6(8) . .
C8 C13 H13 105.3 . .
N2 C13 H13 105.3 . .
C12 C13 H13 105.3 . .
N2 C14 C15 127.6(8) . .
N2 C14 H14 116.2 . .
C15 C14 H14 116.2 . .
C20 C15 C16 116.8(7) . .
C20 C15 C14 123.9(9) . .
C16 C15 C14 119.1(8) . .
C17 C16 C15 122.8(9) . .
C17 C16 H16 118.6 . .
C15 C16 H16 118.6 . .
C16 C17 C18 121.5(10) . .
C16 C17 H17 119.2 . .
C18 C17 H17 119.2 . .
C17 C18 C19 117.0(8) . .
C17 C18 H18 121.5 . .
C19 C18 H18 121.5 . .
O4 C19 C18 125.1(7) . .
O4 C19 C20 112.6(8) . .
C18 C19 C20 122.2(8) . .
O3 C20 C15 122.7(7) . .
O3 C20 C19 118.0(7) . .
C15 C20 C19 119.2(8) . .
O4 C21 H21A 109.5 . .
O4 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
O4 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
O2 C22 H22A 109.5 . .
O2 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
O2 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
O5 C23 C28 122.6(7) . .
O5 C23 C24 118.8(6) . .
C28 C23 C24 118.6(7) . .
O6 C24 C25 127.0(7) . .
O6 C24 C23 113.2(7) . .
C25 C24 C23 119.8(7) . .
C24 C25 C26 121.7(8) . .
C24 C25 H25 119.1 . .
C26 C25 H25 119.1 . .
C25 C26 C27 119.8(9) . .
C25 C26 H26 120.1 . .
C27 C26 H26 120.1 . .
C26 C27 C28 120.1(8) . .
C26 C27 H27 120.0 . .
C28 C27 H27 120.0 . .
C23 C28 C27 120.0(8) . .
C23 C28 C29 120.9(8) . .
C27 C28 C29 118.9(7) . .
N3 C29 C28 123.5(7) . .
N3 C29 H29 118.3 . .
C28 C29 H29 118.3 . .
N3 C30 C31 109.1(8) . .
N3 C30 C35 109.1(6) . .
C31 C30 C35 112.1(7) . .
N3 C30 H30 108.8 . .
C31 C30 H30 108.8 . .
C35 C30 H30 108.8 . .
C32 C31 C30 110.4(9) . .
C32 C31 H31A 109.6 . .
C30 C31 H31A 109.6 . .
C32 C31 H31B 109.6 . .
C30 C31 H31B 109.6 . .
H31A C31 H31B 108.1 . .
C31 C32 C33 110.1(7) . .
C31 C32 H32A 109.6 . .
C33 C32 H32A 109.6 . .
C31 C32 H32B 109.6 . .
C33 C32 H32B 109.6 . .
H32A C32 H32B 108.1 . .
C34 C33 C32 111.6(9) . .
C34 C33 H33A 109.3 . .
C32 C33 H33A 109.3 . .
C34 C33 H33B 109.3 . .
C32 C33 H33B 109.3 . .
H33A C33 H33B 108.0 . .
C33 C34 C35 111.4(9) . .
C33 C34 H34A 109.4 . .
C35 C34 H34A 109.4 . .
C33 C34 H34B 109.4 . .
C35 C34 H34B 109.4 . .
H34A C34 H34B 108.0 . .
N4 C35 C34 110.8(8) . .
N4 C35 C30 109.0(7) . .
C34 C35 C30 109.9(6) . .
N4 C35 H35 109.0 . .
C34 C35 H35 109.0 . .
C30 C35 H35 109.0 . .
N4 C36 C37 123.7(8) . .
N4 C36 H36 118.1 . .
C37 C36 H36 118.1 . .
C38 C37 C42 118.2(7) . .
C38 C37 C36 120.6(6) . .
C42 C37 C36 121.1(7) . .
C39 C38 C37 120.9(7) . .
C39 C38 H38 119.5 . .
C37 C38 H38 119.5 . .
C38 C39 C40 121.7(9) . .
C38 C39 H39 119.1 . .
C40 C39 H39 119.1 . .
C41 C40 C39 118.9(9) . .
C41 C40 H40 120.6 . .
C39 C40 H40 120.6 . .
C40 C41 O8 124.9(7) . .
C40 C41 C42 121.1(6) . .
O8 C41 C42 114.0(7) . .
O7 C42 C41 118.2(6) . .
O7 C42 C37 122.7(7) . .
C41 C42 C37 119.2(8) . .
O8 C43 H43A 109.5 . .
O8 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
O8 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
O6 C44 H44A 109.5 . .
O6 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
O6 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
C45 O10 H10 109.5 . .
C46 C45 O10 114(2) . .
C46 C45 H45A 108.8 . .
O10 C45 H45A 108.8 . .
C46 C45 H45B 108.8 . .
O10 C45 H45B 108.8 . .
H45A C45 H45B 107.7 . .
C45 C46 H46A 109.5 . .
C45 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
C45 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C48 O11 H99 128.5 . .
C48 C47 H47A 109.5 . .
C48 C47 H47B 109.5 . .
H47A C47 H47B 109.5 . .
C48 C47 H47C 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C47 C48 O11 130(3) . .
C47 C48 H48A 104.9 . .
O11 C48 H48A 104.9 . .
C47 C48 H48B 104.9 . .
O11 C48 H48B 104.9 . .
H48A C48 H48B 105.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O3 2.294(5) .
Dy1 O9 2.323(6) 3_645
Dy1 O7 2.340(4) 3_645
Dy1 O1 2.347(4) .
Dy1 O9 2.355(4) .
Dy1 N1 2.421(6) .
Dy1 N2 2.479(7) .
Dy1 O8 2.508(5) 3_645
Dy1 Dy2 3.5285(4) .
Dy1 Dy1 3.7393(7) 3_645
Dy1 Dy2 3.8809(5) 3_645
Dy1 H91 2.2849 .
Dy2 O5 2.271(4) .
Dy2 O1 2.352(4) .
Dy2 O9 2.374(4) .
Dy2 O3 2.385(5) .
Dy2 O7 2.465(6) .
Dy2 O6 2.596(6) .
Dy2 O4 2.652(6) .
Dy2 O2 2.660(5) .
Dy2 Cl1 2.682(4) .
Dy2 Dy1 3.8809(5) 3_645
O1 C1 1.330(9) .
O2 C2 1.381(9) .
O2 C22 1.422(8) .
O3 C20 1.314(10) .
O4 C19 1.379(9) .
O4 C21 1.455(9) .
O5 C23 1.329(10) .
O6 C24 1.364(8) .
O6 C44 1.442(9) .
O7 C42 1.375(10) .
O7 Dy1 2.340(4) 3_645
O8 C41 1.395(8) .
O8 C43 1.437(9) .
O8 Dy1 2.508(5) 3_645
O9 Dy1 2.323(6) 3_645
O9 H91 0.8495 .
N1 C7 1.246(11) .
N1 C8 1.477(10) .
N2 C14 1.261(12) .
N2 C13 1.478(10) .
N3 C29 1.269(11) .
N3 C30 1.490(10) .
N3 H311 0.9041 .
N4 C36 1.266(8) .
N4 C35 1.448(11) .
C1 C6 1.402(9) .
C1 C2 1.433(9) .
C2 C3 1.400(13) .
C3 C4 1.395(12) .
C3 H3 0.9300 .
C4 C5 1.376(12) .
C4 H4 0.9300 .
C5 C6 1.397(13) .
C5 H5 0.9300 .
C6 C7 1.446(10) .
C7 H7 0.9300 .
C8 C13 1.445(14) .
C8 C9 1.503(11) .
C8 H8 0.9800 .
C9 C10 1.495(13) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.460(17) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.518(13) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.504(11) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 H13 0.9800 .
C14 C15 1.444(11) .
C14 H14 0.9300 .
C15 C20 1.408(11) .
C15 C16 1.418(14) .
C16 C17 1.357(12) .
C16 H16 0.9300 .
C17 C18 1.392(13) .
C17 H17 0.9300 .
C18 C19 1.403(14) .
C18 H18 0.9300 .
C19 C20 1.416(10) .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 C28 1.402(9) .
C23 C24 1.422(11) .
C24 C25 1.367(12) .
C25 C26 1.380(11) .
C25 H25 0.9300 .
C26 C27 1.382(13) .
C26 H26 0.9300 .
C27 C28 1.405(13) .
C27 H27 0.9300 .
C28 C29 1.426(11) .
C29 H29 0.9300 .
C30 C31 1.532(13) .
C30 C35 1.536(12) .
C30 H30 0.9800 .
C31 C32 1.520(13) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 C33 1.529(15) .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
C33 C34 1.521(14) .
C33 H33A 0.9700 .
C33 H33B 0.9700 .
C34 C35 1.527(12) .
C34 H34A 0.9700 .
C34 H34B 0.9700 .
C35 H35 0.9800 .
C36 C37 1.454(11) .
C36 H36 0.9300 .
C37 C38 1.396(12) .
C37 C42 1.412(9) .
C38 C39 1.352(13) .
C38 H38 0.9300 .
C39 C40 1.379(10) .
C39 H39 0.9300 .
C40 C41 1.370(12) .
C40 H40 0.9300 .
C41 C42 1.400(11) .
C43 H43A 0.9600 .
C43 H43B 0.9600 .
C43 H43C 0.9600 .
C44 H44A 0.9600 .
C44 H44B 0.9600 .
C44 H44C 0.9600 .
O10 C45 1.305(17) .
O10 H10 0.8200 .
C45 C46 1.11(3) .
C45 H45A 0.9700 .
C45 H45B 0.9700 .
C46 H46A 0.9600 .
C46 H46B 0.9600 .
C46 H46C 0.9600 .
O13 O13 1.24(7) 3_545
O11 C48 1.245(17) .
O11 H99 0.9720 .
C47 C48 1.119(19) .
C47 H47A 0.9600 .
C47 H47B 0.9600 .
C47 H47C 0.9600 .
C48 H48A 0.9700 .
C48 H48B 0.9700 .
