#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:04:00 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224177 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/95/7049546.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_7049546
loop_
_publ_author_name
'Biswas, Sourav'
'Kumar, Pawan'
'Swain, Abinash'
'Gupta, Tulika'
'Kalita, Pankaj'
'Kundu, Subrata'
'Rajaraman, Gopalan'
'Chandrasekhar, Vadapalli'
_publ_section_title
;
 Phosphonate-assisted tetranuclear lanthanide assemblies: observation of
 the toroidic ground state in the TbIII analogue.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6421
_journal_page_last               6434
_journal_paper_doi               10.1039/c9dt00592g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C55.7 H67.4 Dy4 F6 N10 O20 P2, 2(Cl), 2(C H4 O), 0.3(H2 O)'
_chemical_formula_sum            'C57.7 H76 Cl2 Dy4 F6 N10 O22.3 P2'
_chemical_formula_weight         2163.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-22 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                112.8160(10)
_cell_angle_beta                 98.8770(10)
_cell_angle_gamma                108.9790(10)
_cell_formula_units_Z            1
_cell_length_a                   12.2754(8)
_cell_length_b                   12.9357(8)
_cell_length_c                   14.5715(9)
_cell_measurement_reflns_used    6923
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.38
_cell_volume                     1909.6(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12451
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.063
_diffrn_reflns_theta_max         25.063
_diffrn_reflns_theta_min         2.383
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0738 before and 0.0353 after correction.
The Ratio of minimum to maximum transmission is 0.8760.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       block
_exptl_crystal_F_000             1053
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6718
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0193P)²+1.9331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5542
_reflns_number_total             6718
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00592g2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
'Adding full bibliography for 7049546--7049548.cif.'
_cod_original_formula_sum        'C57.70 H76 Cl2 Dy4 F6 N10 O22.30 P2'
_cod_database_code               7049546
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.663
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O3-H3
 0.87 with sigma of 0.01
 O12-H12A = O12-H12B
 0.87 with sigma of 0.02
 C21-H5
 1.915796 with sigma of 0.02
 Dy1-H5
 2.969387 with sigma of 0.02
 C19-H4
 1.909474 with sigma of 0.02
 Dy1-H4
 2.976831 with sigma of 0.02
 Dy2-H3
 2.9126 with sigma of 0.02
 H12A-H12B
 1.38 with sigma of 0.04
 C22-H3
 1.914506 with sigma of 0.02
 Dy2-H12A \\sim Dy2-H12B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O12)
4. Others
 Fixed Sof: O3(0.85) H3(0.85) C22(0.85) H22A(0.85) H22B(0.85) H22C(0.85)
 O30(0.15) H30A(0.15) H30B(0.15) O12(0.15) H12A(0.15) H12B(0.15)
5.a Riding coordinates:
 O30(H30A,H30B), O12(H12A,H12B)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C21(H21A,H21B), C18(H18A,H18B), C20(H20A,H20B), C19(H19A,H19B)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3A), C9(H9), C2(H2), C15(H15), C14(H14), C4(H4A), C10(H10),
 C8(H8)
5.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C22(H22A,H22B,
 H22C), C29(H29A,H29B,H29C)
5.e Idealised tetrahedral OH refined as rotating group:
 O11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.25681(2) 0.29366(2) 0.85125(2) 0.01540(6) Uani 1 1 d D . . .
Dy2 Dy 0.55734(2) 0.51242(2) 0.82115(2) 0.01509(6) Uani 1 1 d D . . .
P1 P 0.43080(10) 0.60967(10) 1.02685(9) 0.0150(2) Uani 1 1 d . . . .
O8 O 0.5327(2) 0.6520(2) 1.1282(2) 0.0159(6) Uani 1 1 d . . . .
O7 O 0.4774(2) 0.6103(2) 0.9371(2) 0.0169(6) Uani 1 1 d . . . .
O2 O 0.3285(2) 0.3964(3) 0.7546(2) 0.0172(6) Uani 1 1 d . . . .
O10 O 0.3270(3) 0.2686(3) 1.1001(2) 0.0187(7) Uani 1 1 d . . . .
O3 O 0.5119(10) 0.3314(16) 0.6642(17) 0.0216(17) Uani 0.85 1 d D P A 1
H3 H 0.4388(16) 0.273(3) 0.633(3) 0.032 Uiso 0.85 1 d DR P B 1
O6 O 0.3392(2) 0.4792(2) 1.0009(2) 0.0159(6) Uani 1 1 d . . . .
O5 O 0.1306(3) 0.2980(3) 0.9615(2) 0.0199(7) Uani 1 1 d D . . .
H5 H 0.154(3) 0.3605(17) 1.0222(16) 0.030 Uiso 1 1 d DR . . .
F1 F 0.3000(3) -0.0238(3) 0.9427(3) 0.0567(10) Uani 1 1 d . . . .
O1 O 0.7578(3) 0.5333(3) 0.8412(2) 0.0198(7) Uani 1 1 d . . . .
N2 N 0.4326(3) 0.5478(3) 0.6899(3) 0.0156(8) Uani 1 1 d . . . .
O9 O 0.2860(3) 0.1684(3) 0.9245(2) 0.0198(7) Uani 1 1 d . . . .
N4 N 0.0940(3) 0.3005(3) 0.7236(3) 0.0181(8) Uani 1 1 d . . . .
O4 O 0.2363(3) 0.1141(3) 0.7102(2) 0.0234(7) Uani 1 1 d D . . .
H4 H 0.253(3) 0.1075(19) 0.6536(16) 0.035 Uiso 1 1 d DR . . .
N5 N 0.0308(3) 0.1133(3) 0.7741(3) 0.0194(8) Uani 1 1 d . . . .
F2 F 0.1712(4) 0.0029(3) 1.0198(4) 0.0771(13) Uani 1 1 d . . . .
N3 N 0.3073(3) 0.5107(3) 0.6690(3) 0.0160(8) Uani 1 1 d . . . .
F3 F 0.3553(4) 0.0785(3) 1.1093(3) 0.0841(14) Uani 1 1 d . . . .
C23 C 0.3023(4) 0.1787(4) 1.0154(4) 0.0197(10) Uani 1 1 d . . . .
N1 N 0.6569(3) 0.5860(3) 0.7034(3) 0.0151(8) Uani 1 1 d . . . .
C13 C 0.0510(4) 0.3829(4) 0.6074(3) 0.0197(10) Uani 1 1 d . . . .
H13 H 0.080442 0.435140 0.577107 0.024 Uiso 1 1 calc R . . .
C17 C -0.0631(4) 0.1553(4) 0.7490(4) 0.0231(10) Uani 1 1 d . . . .
H17A H -0.076573 0.203281 0.814560 0.028 Uiso 1 1 calc R . . .
H17B H -0.140773 0.082439 0.701992 0.028 Uiso 1 1 calc R . . .
C6 C 0.7737(4) 0.6043(4) 0.7148(3) 0.0182(10) Uani 1 1 d . . . .
C3 C 1.0111(4) 0.6351(4) 0.7457(4) 0.0250(11) Uani 1 1 d . . . .
H3A H 1.092842 0.644673 0.756544 0.030 Uiso 1 1 calc R . . .
C9 C 0.7811(4) 0.6854(4) 0.5916(3) 0.0211(10) Uani 1 1 d . . . .
H9 H 0.821895 0.717261 0.551646 0.025 Uiso 1 1 calc R . . .
C24 C 0.2857(5) 0.0592(4) 1.0211(4) 0.0295(12) Uani 1 1 d . . . .
C11 C 0.2654(4) 0.4320(4) 0.7039(3) 0.0164(9) Uani 1 1 d . . . .
C7 C 0.6041(4) 0.6202(4) 0.6407(3) 0.0176(9) Uani 1 1 d . . . .
C21 C 0.0405(4) 0.1922(4) 0.9602(4) 0.0242(11) Uani 1 1 d D . . .
H21A H -0.034380 0.204407 0.964746 0.029 Uiso 1 1 calc R . . .
H21B H 0.072011 0.181315 1.020972 0.029 Uiso 1 1 calc R . . .
C2 C 0.9455(4) 0.5874(4) 0.8017(4) 0.0233(10) Uani 1 1 d . . . .
H2 H 0.982916 0.565543 0.848892 0.028 Uiso 1 1 calc R . . .
C1 C 0.8271(4) 0.5723(4) 0.7884(3) 0.0198(10) Uani 1 1 d . . . .
C12 C 0.1312(4) 0.3725(4) 0.6777(3) 0.0174(9) Uani 1 1 d . . . .
C25 C 0.3555(4) 0.7132(4) 1.0535(3) 0.0205(10) Uani 1 1 d . . . .
C15 C -0.1118(4) 0.2388(4) 0.6261(3) 0.0212(10) Uani 1 1 d . . . .
H15 H -0.196131 0.189866 0.608301 0.025 Uiso 1 1 calc R . . .
C5 C 0.8417(4) 0.6535(4) 0.6590(3) 0.0186(10) Uani 1 1 d . . . .
C27 C 0.4435(5) 0.8386(4) 1.0710(4) 0.0360(13) Uani 1 1 d . . . .
H27A H 0.520818 0.866828 1.124074 0.054 Uiso 1 1 calc GR . . .
H27B H 0.408702 0.898581 1.095365 0.054 Uiso 1 1 calc GR . . .
H27C H 0.457796 0.831055 1.004815 0.054 Uiso 1 1 calc GR . . .
C18 C 0.0226(4) 0.0094(4) 0.6780(4) 0.0269(11) Uani 1 1 d . . . .
H18A H -0.000469 0.022595 0.616705 0.032 Uiso 1 1 calc R . . .
H18B H -0.041775 -0.068613 0.666500 0.032 Uiso 1 1 calc R . . .
C20 C 0.0124(4) 0.0778(4) 0.8574(3) 0.0237(10) Uani 1 1 d . . . .
H20A H 0.066353 0.038108 0.868225 0.028 Uiso 1 1 calc R . . .
H20B H -0.072867 0.017326 0.835468 0.028 Uiso 1 1 calc R . . .
C14 C -0.0727(4) 0.3159(4) 0.5820(3) 0.0225(10) Uani 1 1 d . . . .
H14 H -0.129738 0.322663 0.535202 0.027 Uiso 1 1 calc R . . .
C16 C -0.0257(4) 0.2340(4) 0.6968(3) 0.0168(9) Uani 1 1 d . . . .
C28 C 0.3157(5) 0.7283(5) 1.1497(4) 0.0348(13) Uani 1 1 d . . . .
H28A H 0.256012 0.648082 1.136818 0.052 Uiso 1 1 calc GR . . .
H28B H 0.278812 0.787252 1.164013 0.052 Uiso 1 1 calc GR . . .
H28C H 0.386537 0.759311 1.210423 0.052 Uiso 1 1 calc GR . . .
C4 C 0.9640(4) 0.6686(4) 0.6766(3) 0.0227(10) Uani 1 1 d . . . .
H4A H 1.012157 0.701406 0.640970 0.027 Uiso 1 1 calc R . . .
C10 C 0.4776(4) 0.5947(4) 0.6332(3) 0.0174(9) Uani 1 1 d . . . .
H10 H 0.429833 0.611851 0.588156 0.021 Uiso 1 1 calc R . . .
C8 C 0.6640(4) 0.6709(4) 0.5830(3) 0.0198(10) Uani 1 1 d . . . .
H8 H 0.623762 0.694587 0.538952 0.024 Uiso 1 1 calc R . . .
C26 C 0.2437(5) 0.6574(5) 0.9571(4) 0.0385(13) Uani 1 1 d . . . .
H26A H 0.269623 0.649652 0.895372 0.058 Uiso 1 1 calc GR . . .
H26B H 0.201212 0.711372 0.969669 0.058 Uiso 1 1 calc GR . . .
H26C H 0.188712 0.575385 0.944694 0.058 Uiso 1 1 calc GR . . .
C19 C 0.1411(4) -0.0024(4) 0.6859(4) 0.0284(11) Uani 1 1 d D . . .
H19A H 0.160048 -0.025451 0.741740 0.034 Uiso 1 1 calc R . . .
H19B H 0.134832 -0.068063 0.618487 0.034 Uiso 1 1 calc R . . .
C22 C 0.5899(5) 0.2910(5) 0.6091(5) 0.0335(14) Uani 0.85 1 d D P A 1
H22A H 0.586548 0.309495 0.549860 0.050 Uiso 0.85 1 calc GR P A 1
H22B H 0.562473 0.201619 0.582834 0.050 Uiso 0.85 1 calc GR P A 1
H22C H 0.673656 0.334354 0.657141 0.050 Uiso 0.85 1 calc GR P A 1
Cl1 Cl 0.26745(12) 0.11632(12) 0.51617(10) 0.0419(3) Uani 1 1 d . . . .
O11 O 0.7502(4) 0.3126(4) 0.3771(3) 0.0506(10) Uani 1 1 d . . . .
H11 H 0.738883 0.371232 0.372228 0.076 Uiso 1 1 calc GR . . .
C29 C 0.6777(6) 0.2027(5) 0.2854(5) 0.0639(19) Uani 1 1 d . . . .
H29A H 0.664262 0.132597 0.300142 0.096 Uiso 1 1 calc GR . . .
H29B H 0.718433 0.194995 0.231873 0.096 Uiso 1 1 calc GR . . .
H29C H 0.599257 0.202986 0.259517 0.096 Uiso 1 1 calc GR . . .
O30 O 0.617(2) 0.256(3) 0.5100(19) 0.052(7) Uani 0.15 1 d . P C 2
H30A H 0.628443 0.242206 0.449608 0.077 Uiso 0.15 1 d R P C 2
H30B H 0.659473 0.225416 0.535938 0.077 Uiso 0.15 1 d R P C 2
O12 O 0.513(5) 0.318(10) 0.668(10) 0.0216(17) Uani 0.15 1 d D P A 2
H12A H 0.580222 0.315212 0.654802 0.032 Uiso 0.15 1 d DR P A 2
H12B H 0.471112 0.311832 0.609872 0.032 Uiso 0.15 1 d DR P A 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'
Cl Cl 0.1484 0.1585 '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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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
O8 Dy1 O5 137.22(10) 2_667 .
O8 Dy1 N4 130.29(9) 2_667 .
O8 Dy1 N5 147.62(10) 2_667 .
O2 Dy1 O8 66.81(9) . 2_667
O2 Dy1 O5 138.56(10) . .
O2 Dy1 N4 64.15(10) . .
O2 Dy1 N5 120.67(10) . .
O6 Dy1 O8 80.30(9) . 2_667
O6 Dy1 O2 90.03(10) . .
O6 Dy1 O5 68.69(9) . .
O6 Dy1 O9 99.22(10) . .
O6 Dy1 N4 107.04(10) . .
O6 Dy1 O4 162.00(10) . .
O6 Dy1 N5 128.26(10) . .
O5 Dy1 N4 87.83(10) . .
O5 Dy1 N5 60.81(10) . .
O9 Dy1 O8 81.34(9) . 2_667
O9 Dy1 O2 144.84(10) . .
O9 Dy1 O5 75.60(10) . .
O9 Dy1 N4 141.26(10) . .
O9 Dy1 N5 79.24(10) . .
N4 Dy1 N5 62.18(10) . .
O4 Dy1 O8 82.02(10) . 2_667
O4 Dy1 O2 86.10(10) . .
O4 Dy1 O5 124.27(10) . .
O4 Dy1 O9 74.69(10) . .
O4 Dy1 N4 87.05(11) . .
O4 Dy1 N5 68.00(10) . .
O8 Dy2 P1 28.42(7) 2_667 2_667
O8 Dy2 O2 62.76(9) 2_667 .
O8 Dy2 O6 57.00(9) 2_667 2_667
O8 Dy2 N2 122.97(10) 2_667 .
O8 Dy2 N1 151.15(10) 2_667 .
O7 Dy2 P1 79.76(7) . 2_667
O7 Dy2 O8 81.35(9) . 2_667
O7 Dy2 O2 70.06(10) . .
O7 Dy2 O10 70.06(9) . 2_667
O7 Dy2 O3 144.3(3) . .
O7 Dy2 O6 75.46(9) . 2_667
O7 Dy2 O1 130.38(10) . .
O7 Dy2 N2 86.22(10) . .
O7 Dy2 N1 126.91(10) . .
O7 Dy2 O12 144(2) . .
O2 Dy2 P1 89.15(6) . 2_667
O2 Dy2 O6 113.43(8) . 2_667
O2 Dy2 N2 60.66(9) . .
O2 Dy2 N1 117.11(10) . .
O10 Dy2 P1 116.21(7) 2_667 2_667
O10 Dy2 O8 140.06(9) 2_667 2_667
O10 Dy2 O2 126.94(9) 2_667 .
O10 Dy2 O6 88.41(9) 2_667 2_667
O10 Dy2 N2 83.23(10) 2_667 .
O10 Dy2 N1 65.63(10) 2_667 .
O10 Dy2 O12 142(3) 2_667 .
O3 Dy2 P1 95.8(4) . 2_667
O3 Dy2 O8 78.9(4) . 2_667
O3 Dy2 O2 74.5(3) . .
O3 Dy2 O10 139.3(4) . 2_667
O3 Dy2 O6 116.3(3) . 2_667
O3 Dy2 N2 80.1(2) . .
O3 Dy2 N1 73.8(4) . .
O6 Dy2 P1 28.86(6) 2_667 2_667
O1 Dy2 P1 82.87(7) . 2_667
O1 Dy2 O8 103.32(9) . 2_667
O1 Dy2 O2 155.52(10) . .
O1 Dy2 O10 77.01(10) . 2_667
O1 Dy2 O3 83.3(3) . .
O1 Dy2 O6 67.41(9) . 2_667
O1 Dy2 N2 125.90(10) . .
O1 Dy2 N1 64.62(10) . .
O1 Dy2 O12 82.2(13) . .
N2 Dy2 P1 149.63(7) . 2_667
N2 Dy2 O6 161.55(9) . 2_667
N2 Dy2 N1 61.33(10) . .
N1 Dy2 P1 146.58(8) . 2_667
N1 Dy2 O6 129.18(10) . 2_667
O12 Dy2 O2 74.9(16) . .
O12 Dy2 O6 112.0(18) . 2_667
O12 Dy2 N2 84.1(16) . .
O12 Dy2 N1 77(3) . .
O8 P1 Dy2 50.01(10) . 2_667
O8 P1 C25 109.57(19) . .
O7 P1 Dy2 136.82(12) . 2_667
O7 P1 O8 113.22(16) . .
O7 P1 O6 112.51(16) . .
O7 P1 C25 107.26(17) . .
O6 P1 Dy2 55.80(11) . 2_667
O6 P1 O8 105.14(15) . .
O6 P1 C25 109.07(18) . .
C25 P1 Dy2 115.85(14) . 2_667
Dy1 O8 Dy2 112.65(10) 2_667 2_667
P1 O8 Dy1 126.58(15) . 2_667
P1 O8 Dy2 101.57(13) . 2_667
P1 O7 Dy2 142.66(16) . .
Dy1 O2 Dy2 112.19(11) . .
C11 O2 Dy1 124.6(2) . .
C11 O2 Dy2 118.3(2) . .
C23 O10 Dy2 136.5(3) . 2_667
Dy2 O3 H3 121(2) . .
C22 O3 Dy2 130.9(8) . .
C22 O3 H3 108(2) . .
Dy1 O6 Dy2 117.89(10) . 2_667
P1 O6 Dy1 131.98(15) . .
P1 O6 Dy2 95.33(13) . 2_667
Dy1 O5 H5 120.6(15) . .
C21 O5 Dy1 126.5(2) . .
C21 O5 H5 108.5(14) . .
C1 O1 Dy2 125.1(2) . .
N3 N2 Dy2 122.0(2) . .
C10 N2 Dy2 123.2(3) . .
C10 N2 N3 114.7(3) . .
C23 O9 Dy1 133.6(3) . .
C12 N4 Dy1 118.1(3) . .
C16 N4 Dy1 124.1(3) . .
C16 N4 C12 117.8(4) . .
Dy1 O4 H4 127.2(16) . .
C19 O4 Dy1 118.6(2) . .
C19 O4 H4 107.9(16) . .
C17 N5 Dy1 112.3(2) . .
C18 N5 Dy1 108.0(2) . .
C18 N5 C17 109.8(3) . .
C20 N5 Dy1 106.5(2) . .
C20 N5 C17 108.2(3) . .
C20 N5 C18 112.0(3) . .
C11 N3 N2 109.5(3) . .
O10 C23 O9 130.4(4) . .
O10 C23 C24 114.9(4) . .
O9 C23 C24 114.6(4) . .
C6 N1 Dy2 117.7(3) . .
C7 N1 Dy2 123.2(3) . .
C7 N1 C6 118.6(3) . .
C12 C13 H13 120.6 . .
C14 C13 H13 120.6 . .
C14 C13 C12 118.8(4) . .
N5 C17 H17A 109.4 . .
N5 C17 H17B 109.4 . .
N5 C17 C16 111.2(3) . .
H17A C17 H17B 108.0 . .
C16 C17 H17A 109.4 . .
C16 C17 H17B 109.4 . .
N1 C6 C1 115.7(3) . .
N1 C6 C5 122.9(4) . .
C5 C6 C1 121.4(4) . .
C2 C3 H3A 118.2 . .
C4 C3 H3A 118.2 . .
C4 C3 C2 123.5(4) . .
C5 C9 H9 119.7 . .
C8 C9 H9 119.7 . .
C8 C9 C5 120.6(4) . .
F1 C24 F2 105.4(4) . .
F1 C24 C23 115.3(4) . .
F2 C24 C23 109.4(4) . .
F3 C24 F1 108.3(4) . .
F3 C24 F2 104.6(4) . .
F3 C24 C23 113.0(4) . .
O2 C11 N3 126.6(4) . .
O2 C11 C12 116.9(3) . .
N3 C11 C12 116.4(4) . .
N1 C7 C10 114.0(3) . .
N1 C7 C8 122.7(4) . .
C8 C7 C10 123.3(4) . .
O5 C21 H21A 110.1 . .
O5 C21 H21B 110.1 . .
O5 C21 C20 108.1(3) . .
H21A C21 H21B 108.4 . .
C20 C21 H21A 110.1 . .
C20 C21 H21B 110.1 . .
C3 C2 H2 120.0 . .
C1 C2 C3 120.1(4) . .
C1 C2 H2 120.0 . .
O1 C1 C6 116.8(4) . .
O1 C1 C2 125.2(4) . .
C2 C1 C6 118.0(4) . .
N4 C12 C13 122.9(4) . .
N4 C12 C11 113.6(4) . .
C13 C12 C11 123.3(4) . .
C27 C25 P1 108.6(3) . .
C27 C25 C26 109.8(4) . .
C28 C25 P1 111.3(3) . .
C28 C25 C27 109.7(4) . .
C28 C25 C26 109.5(4) . .
C26 C25 P1 107.9(3) . .
C14 C15 H15 120.5 . .
C14 C15 C16 119.0(4) . .
C16 C15 H15 120.5 . .
C9 C5 C6 116.3(4) . .
C9 C5 C4 125.3(4) . .
C4 C5 C6 118.3(4) . .
C25 C27 H27A 109.5 . .
C25 C27 H27B 109.5 . .
C25 C27 H27C 109.5 . .
H27A C27 H27B 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
N5 C18 H18A 109.3 . .
N5 C18 H18B 109.3 . .
N5 C18 C19 111.7(4) . .
H18A C18 H18B 107.9 . .
C19 C18 H18A 109.3 . .
C19 C18 H18B 109.3 . .
N5 C20 C21 110.2(3) . .
N5 C20 H20A 109.6 . .
N5 C20 H20B 109.6 . .
C21 C20 H20A 109.6 . .
C21 C20 H20B 109.6 . .
H20A C20 H20B 108.1 . .
C13 C14 C15 118.9(4) . .
C13 C14 H14 120.6 . .
C15 C14 H14 120.6 . .
N4 C16 C17 116.2(4) . .
N4 C16 C15 122.7(4) . .
C15 C16 C17 121.2(4) . .
C25 C28 H28A 109.5 . .
C25 C28 H28B 109.5 . .
C25 C28 H28C 109.5 . .
H28A C28 H28B 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C3 C4 C5 118.7(4) . .
C3 C4 H4A 120.6 . .
C5 C4 H4A 120.6 . .
N2 C10 C7 117.6(4) . .
N2 C10 H10 121.2 . .
C7 C10 H10 121.2 . .
C9 C8 C7 118.7(4) . .
C9 C8 H8 120.7 . .
C7 C8 H8 120.7 . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26B 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
O4 C19 C18 109.2(4) . .
O4 C19 H19A 109.8 . .
O4 C19 H19B 109.8 . .
C18 C19 H19A 109.8 . .
C18 C19 H19B 109.8 . .
H19A C19 H19B 108.3 . .
O3 C22 H22A 109.5 . .
O3 C22 H22B 109.5 . .
O3 C22 H22C 109.5 . .
H22A C22 H22B 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C29 O11 H11 109.5 . .
O11 C29 H29A 109.5 . .
O11 C29 H29B 109.5 . .
O11 C29 H29C 109.5 . .
H29A C29 H29B 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
H30A O30 H30B 104.5 . .
Dy2 O12 H12A 111.6 . .
Dy2 O12 H12B 112.1 . .
H12A O12 H12B 102.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O8 2.382(3) 2_667
Dy1 O2 2.366(3) .
Dy1 O6 2.285(3) .
Dy1 O5 2.396(3) .
Dy1 O9 2.344(3) .
Dy1 N4 2.560(3) .
Dy1 O4 2.333(3) .
Dy1 N5 2.683(3) .
Dy2 P1 3.1912(10) 2_667
Dy2 O8 2.496(3) 2_667
Dy2 O7 2.255(3) .
Dy2 O2 2.524(3) .
Dy2 O10 2.391(3) 2_667
Dy2 O3 2.37(2) .
Dy2 O6 2.651(3) 2_667
Dy2 O1 2.344(3) .
Dy2 N2 2.539(3) .
Dy2 N1 2.549(3) .
Dy2 O12 2.44(13) .
P1 O8 1.550(3) .
P1 O7 1.508(3) .
P1 O6 1.547(3) .
P1 C25 1.820(4) .
O2 C11 1.295(5) .
O10 C23 1.228(5) .
O3 H3 0.868(10) .
O3 C22 1.44(2) .
O5 H5 0.857(9) .
O5 C21 1.444(5) .
F1 C24 1.312(5) .
O1 C1 1.340(5) .
N2 N3 1.397(4) .
N2 C10 1.290(5) .
O9 C23 1.256(5) .
N4 C12 1.351(5) .
N4 C16 1.339(5) .
O4 H4 0.857(9) .
O4 C19 1.441(5) .
N5 C17 1.480(5) .
N5 C18 1.479(5) .
N5 C20 1.477(5) .
F2 C24 1.349(6) .
N3 C11 1.304(5) .
F3 C24 1.311(6) .
C23 C24 1.529(6) .
N1 C6 1.347(5) .
N1 C7 1.329(5) .
C13 H13 0.9500 .
C13 C12 1.385(6) .
C13 C14 1.385(6) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C17 C16 1.493(5) .
C6 C1 1.433(6) .
C6 C5 1.424(5) .
C3 H3A 0.9500 .
C3 C2 1.402(6) .
C3 C4 1.362(6) .
C9 H9 0.9500 .
C9 C5 1.406(6) .
C9 C8 1.367(6) .
C11 C12 1.485(6) .
C7 C10 1.456(6) .
C7 C8 1.408(6) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C21 C20 1.530(6) .
C2 H2 0.9500 .
C2 C1 1.374(6) .
C25 C27 1.523(6) .
C25 C28 1.517(6) .
C25 C26 1.533(6) .
C15 H15 0.9500 .
C15 C14 1.385(6) .
C15 C16 1.392(6) .
C5 C4 1.418(6) .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C18 C19 1.502(6) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C14 H14 0.9500 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C4 H4A 0.9500 .
C10 H10 0.9500 .
C8 H8 0.9500 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
O11 H11 0.8400 .
O11 C29 1.392(7) .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
O30 H30A 0.8700 .
O30 H30B 0.8699 .
O12 H12A 0.8865 .
O12 H12B 0.8762 .
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_4
Dy1 O2 C11 N3 164.2(3) . .
Dy1 O2 C11 C12 -19.3(5) . .
Dy1 O5 C21 C20 -16.1(5) . .
Dy1 O9 C23 O10 -13.0(7) . .
Dy1 O9 C23 C24 165.4(3) . .
Dy1 N4 C12 C13 179.9(3) . .
Dy1 N4 C12 C11 4.0(5) . .
Dy1 N4 C16 C17 2.1(5) . .
Dy1 N4 C16 C15 -179.2(3) . .
Dy1 O4 C19 C18 50.8(4) . .
Dy1 N5 C17 C16 42.1(4) . .
Dy1 N5 C18 C19 33.6(4) . .
Dy1 N5 C20 C21 53.5(4) . .
Dy2 P1 O8 Dy1 129.9(2) 2_667 2_667
Dy2 P1 O7 Dy2 14.5(4) 2_667 .
Dy2 P1 O6 Dy1 -135.7(2) 2_667 .
Dy2 P1 C25 C27 123.7(3) 2_667 .
Dy2 P1 C25 C28 2.8(4) 2_667 .
Dy2 P1 C25 C26 -117.3(3) 2_667 .
Dy2 O2 C11 N3 11.0(5) . .
Dy2 O2 C11 C12 -172.4(3) . .
Dy2 O10 C23 O9 -33.4(7) 2_667 .
Dy2 O10 C23 C24 148.2(3) 2_667 .
Dy2 O1 C1 C6 0.6(5) . .
Dy2 O1 C1 C2 178.4(3) . .
Dy2 N2 N3 C11 -16.1(4) . .
Dy2 N2 C10 C7 4.2(5) . .
Dy2 N1 C6 C1 3.9(5) . .
Dy2 N1 C6 C5 -175.5(3) . .
Dy2 N1 C7 C10 -8.7(5) . .
Dy2 N1 C7 C8 174.2(3) . .
O8 P1 O7 Dy2 70.1(3) . .
O8 P1 O6 Dy1 -127.1(2) . .
O8 P1 O6 Dy2 8.60(15) . 2_667
O8 P1 C25 C27 69.5(3) . .
O8 P1 C25 C28 -51.3(4) . .
O8 P1 C25 C26 -171.5(3) . .
O7 P1 O8 Dy1 -2.6(2) . 2_667
O7 P1 O8 Dy2 -132.51(14) . 2_667
O7 P1 O6 Dy1 -3.5(3) . .
O7 P1 O6 Dy2 132.27(14) . 2_667
O7 P1 C25 C27 -53.8(4) . .
O7 P1 C25 C28 -174.6(3) . .
O7 P1 C25 C26 65.2(3) . .
O2 C11 C12 N4 8.6(5) . .
O2 C11 C12 C13 -167.2(4) . .
O10 C23 C24 F1 -158.0(4) . .
O10 C23 C24 F2 83.4(5) . .
O10 C23 C24 F3 -32.7(6) . .
O6 P1 O8 Dy1 120.60(18) . 2_667
O6 P1 O8 Dy2 -9.29(16) . 2_667
O6 P1 O7 Dy2 -49.0(3) . .
O6 P1 C25 C27 -175.9(3) . .
O6 P1 C25 C28 63.3(4) . .
O6 P1 C25 C26 -56.9(3) . .
O5 C21 C20 N5 -29.0(5) . .
N2 N3 C11 O2 3.0(6) . .
N2 N3 C11 C12 -173.5(3) . .
O9 C23 C24 F1 23.3(6) . .
O9 C23 C24 F2 -95.3(5) . .
O9 C23 C24 F3 148.7(4) . .
N5 C17 C16 N4 -30.4(5) . .
N5 C17 C16 C15 150.9(4) . .
N5 C18 C19 O4 -54.9(5) . .
N3 N2 C10 C7 -172.0(4) . .
N3 C11 C12 N4 -174.5(4) . .
N3 C11 C12 C13 9.7(6) . .
N1 C6 C1 O1 -3.0(6) . .
N1 C6 C1 C2 179.0(4) . .
N1 C6 C5 C9 1.4(6) . .
N1 C6 C5 C4 -179.8(4) . .
N1 C7 C10 N2 2.8(6) . .
N1 C7 C8 C9 0.1(7) . .
C17 N5 C18 C19 156.3(3) . .
C17 N5 C20 C21 -67.4(4) . .
C6 N1 C7 C10 179.3(4) . .
C6 N1 C7 C8 2.2(6) . .
C6 C5 C4 C3 0.2(6) . .
C3 C2 C1 O1 -176.6(4) . .
C3 C2 C1 C6 1.2(7) . .
C9 C5 C4 C3 179.0(4) . .
C7 N1 C6 C1 176.4(4) . .
C7 N1 C6 C5 -3.0(6) . .
C2 C3 C4 C5 -0.7(7) . .
C1 C6 C5 C9 -177.9(4) . .
C1 C6 C5 C4 0.9(6) . .
C12 N4 C16 C17 179.9(4) . .
C12 N4 C16 C15 -1.5(6) . .
C12 C13 C14 C15 -1.4(6) . .
C25 P1 O8 Dy1 -122.3(2) . 2_667
C25 P1 O8 Dy2 107.80(16) . 2_667
C25 P1 O7 Dy2 -168.9(3) . .
C25 P1 O6 Dy1 115.4(2) . .
C25 P1 O6 Dy2 -108.83(17) . 2_667
C5 C6 C1 O1 176.3(4) . .
C5 C6 C1 C2 -1.6(6) . .
C5 C9 C8 C7 -1.8(6) . .
C18 N5 C17 C16 -78.1(4) . .
C18 N5 C20 C21 171.4(4) . .
C20 N5 C17 C16 159.3(4) . .
C20 N5 C18 C19 -83.4(4) . .
C14 C13 C12 N4 -0.6(6) . .
C14 C13 C12 C11 174.9(4) . .
C14 C15 C16 N4 -0.5(6) . .
C14 C15 C16 C17 178.1(4) . .
C16 N4 C12 C13 2.0(6) . .
C16 N4 C12 C11 -173.9(4) . .
C16 C15 C14 C13 1.9(6) . .
C4 C3 C2 C1 0.0(7) . .
C10 N2 N3 C11 160.2(4) . .
C10 C7 C8 C9 -176.7(4) . .
C8 C9 C5 C6 1.0(6) . .
C8 C9 C5 C4 -177.7(4) . .
C8 C7 C10 N2 179.9(4) . .
