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#$Date: 2019-11-23 16:02:58 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233932 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/93/4349393.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_4349393
loop_
_publ_author_name
'Mazarakioti, Eleni C.'
'Regier, Jeffery'
'Cunha-Silva, Luís'
'Wernsdorfer, Wolfgang'
'Pilkington, Melanie'
'Tang, Jinkui'
'Stamatatos, Theocharis C.'
_publ_section_title
;
 Large Energy Barrier and Magnetization Hysteresis at 5 K for a Symmetric
 {Dy₂} Complex with Spherical Tricapped Trigonal Prismatic
 DyIII Ions.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3568
_journal_page_last               3578
_journal_paper_doi               10.1021/acs.inorgchem.7b00026
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C32 H28 Cl2 Dy2 N8 O20'
_chemical_formula_sum            'C32 H28 Cl2 Dy2 N8 O20'
_chemical_formula_weight         1240.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             '28 November 2016'
_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_cell_angle_alpha                66.309(2)
_cell_angle_beta                 74.672(2)
_cell_angle_gamma                81.563(3)
_cell_formula_units_Z            1
_cell_length_a                   8.5421(6)
_cell_length_b                   10.4051(8)
_cell_length_c                   12.8795(10)
_cell_measurement_reflns_used    7814
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.70
_cell_measurement_theta_min      2.47
_cell_volume                     1009.92(13)
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'omega/phi scans'
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8237
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.667
_exptl_absorpt_coefficient_mu    3.896
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_description       Plate
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4387
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0308
_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)+2.6044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3991
_reflns_number_total             4387
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic7b00026_si_002.cif
_cod_data_source_block           EM1246e
_cod_database_code               4349393
_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   0.652
_shelx_estimated_absorpt_t_max   0.860
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_adp
Dy1 Dy 0.53229(2) 0.45617(2) 0.31428(2) 0.01547(6) Uani 1 1 d . .
Cl1 Cl 0.93347(13) -0.03553(11) 0.90060(9) 0.0268(2) Uani 1 1 d . .
O1 O 0.5386(3) 0.2366(3) 0.3239(2) 0.0208(6) Uani 1 1 d . .
O2 O 0.5667(3) 0.3057(3) 0.5004(2) 0.0190(6) Uani 1 1 d . .
O3 O 0.6036(3) 0.3561(3) 0.6435(2) 0.0202(6) Uani 1 1 d . .
O4 O 0.8403(4) 0.4033(4) 0.3050(3) 0.0343(8) Uani 1 1 d . .
O5 O 0.7252(3) 0.5647(3) 0.3680(2) 0.0230(6) Uani 1 1 d . .
O6 O 0.9765(4) 0.5056(5) 0.3713(3) 0.0523(11) Uani 1 1 d . .
O7 O 0.6756(4) 0.4556(3) 0.1207(3) 0.0280(7) Uani 1 1 d . .
O8 O 0.6535(4) 0.6531(3) 0.1410(3) 0.0307(7) Uani 1 1 d . .
O9 O 0.7767(4) 0.6407(4) -0.0264(3) 0.0337(8) Uani 1 1 d . .
O10 O 0.2661(3) 0.3721(3) 0.4395(3) 0.0224(6) Uani 1 1 d D .
H1W H 0.261(5) 0.375(5) 0.508(2) 0.034 Uiso 1 1 d D U
H2W H 0.178(4) 0.409(5) 0.412(3) 0.034 Uiso 1 1 d D U
N1 N 0.6964(4) 0.0642(3) 0.4813(3) 0.0167(7) Uani 1 1 d D .
H1 H 0.644(5) 0.143(3) 0.455(4) 0.025 Uiso 1 1 d D U
N2 N 0.8514(4) 0.4899(4) 0.3485(3) 0.0274(8) Uani 1 1 d . .
N3 N 0.7043(4) 0.5850(4) 0.0744(3) 0.0236(8) Uani 1 1 d . .
N4 N 0.3300(4) 0.5346(4) 0.1879(3) 0.0264(8) Uani 1 1 d . .
C1 C 0.6231(4) 0.2778(4) 0.5884(3) 0.0144(7) Uani 1 1 d . .
C2 C 0.7218(4) 0.1421(4) 0.6308(3) 0.0151(8) Uani 1 1 d . .
C3 C 0.7803(5) 0.1161(4) 0.7285(3) 0.0180(8) Uani 1 1 d . .
H3 H 0.7591 0.1838 0.7633 0.022 Uiso 1 1 calc R U
C4 C 0.8689(5) -0.0063(4) 0.7761(3) 0.0178(8) Uani 1 1 d . .
C5 C 0.9043(5) -0.1064(4) 0.7260(4) 0.0213(9) Uani 1 1 d . .
H5 H 0.9662 -0.1902 0.7584 0.026 Uiso 1 1 calc R U
C6 C 0.8479(5) -0.0819(4) 0.6285(4) 0.0202(8) Uani 1 1 d . .
H6 H 0.8724 -0.1494 0.5935 0.024 Uiso 1 1 calc R U
C7 C 0.7556(4) 0.0398(4) 0.5803(3) 0.0154(8) Uani 1 1 d . .
C8 C 0.7162(5) -0.0172(4) 0.4222(3) 0.0180(8) Uani 1 1 d . .
H8 H 0.7722 -0.1057 0.4501 0.022 Uiso 1 1 calc R U
C9 C 0.6594(5) 0.0186(4) 0.3199(3) 0.0186(8) Uani 1 1 d . .
C10 C 0.6903(5) -0.0780(4) 0.2632(4) 0.0221(9) Uani 1 1 d . .
H10 H 0.7470 -0.1651 0.2953 0.027 Uiso 1 1 calc R U
C11 C 0.6400(5) -0.0479(5) 0.1641(4) 0.0255(9) Uani 1 1 d . .
H11 H 0.6613 -0.1134 0.1272 0.031 Uiso 1 1 calc R U
C12 C 0.5564(5) 0.0807(5) 0.1165(4) 0.0231(9) Uani 1 1 d . .
H12 H 0.5220 0.1015 0.0468 0.028 Uiso 1 1 calc R U
C13 C 0.5233(5) 0.1766(5) 0.1681(4) 0.0237(9) Uani 1 1 d . .
H13 H 0.4666 0.2629 0.1338 0.028 Uiso 1 1 calc R U
C14 C 0.5724(5) 0.1489(4) 0.2717(3) 0.0182(8) Uani 1 1 d . .
C15 C 0.2313(5) 0.5828(5) 0.1386(4) 0.0249(9) Uani 1 1 d . .
C16 C 0.1034(6) 0.6476(6) 0.0767(4) 0.0343(11) Uani 1 1 d . .
H16A H 0.0327 0.7087 0.1126 0.051 Uiso 1 1 calc R U
H16B H 0.0394 0.5744 0.0803 0.051 Uiso 1 1 calc R U
H16C H 0.1515 0.7034 -0.0048 0.051 Uiso 1 1 calc R U
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'
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'
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
O1 Dy1 O3 150.70(10) . 2_666
O1 Dy1 O2 72.86(10) . .
O3 Dy1 O2 99.57(10) 2_666 .
O1 Dy1 O8 124.36(10) . .
O3 Dy1 O8 79.13(10) 2_666 .
O2 Dy1 O8 142.37(10) . .
O1 Dy1 O10 76.78(10) . .
O3 Dy1 O10 74.03(10) 2_666 .
O2 Dy1 O10 70.99(10) . .
O8 Dy1 O10 140.93(11) . .
O1 Dy1 O7 72.55(10) . .
O3 Dy1 O7 127.31(10) 2_666 .
O2 Dy1 O7 130.20(10) . .
O8 Dy1 O7 51.82(10) . .
O10 Dy1 O7 131.93(10) . .
O1 Dy1 O5 128.42(10) . .
O3 Dy1 O5 72.18(9) 2_666 .
O2 Dy1 O5 72.16(9) . .
O8 Dy1 O5 71.73(10) . .
O10 Dy1 O5 123.92(9) . .
O7 Dy1 O5 104.15(10) . .
O1 Dy1 N4 91.20(11) . .
O3 Dy1 N4 77.70(11) 2_666 .
O2 Dy1 N4 142.38(11) . .
O8 Dy1 N4 74.67(12) . .
O10 Dy1 N4 72.27(11) . .
O7 Dy1 N4 72.32(11) . .
O5 Dy1 N4 138.18(11) . .
O1 Dy1 O4 83.39(11) . .
O3 Dy1 O4 121.84(10) 2_666 .
O2 Dy1 O4 71.53(10) . .
O8 Dy1 O4 77.40(11) . .
O10 Dy1 O4 141.31(10) . .
O7 Dy1 O4 69.89(10) . .
O5 Dy1 O4 50.05(10) . .
N4 Dy1 O4 141.71(11) . .
O1 Dy1 N3 98.38(10) . .
O3 Dy1 N3 103.44(10) 2_666 .
O2 Dy1 N3 143.15(10) . .
O8 Dy1 N3 25.98(10) . .
O10 Dy1 N3 143.26(10) . .
O7 Dy1 N3 25.84(10) . .
O5 Dy1 N3 87.95(10) . .
N4 Dy1 N3 71.45(11) . .
O4 Dy1 N3 71.92(10) . .
C14 O1 Dy1 149.2(3) . .
C1 O2 Dy1 151.3(3) . .
C1 O3 Dy1 149.4(3) . 2_666
N2 O4 Dy1 94.3(2) . .
N2 O5 Dy1 98.5(2) . .
N3 O7 Dy1 95.8(2) . .
N3 O8 Dy1 96.9(2) . .
Dy1 O10 H1W 107(3) . .
Dy1 O10 H2W 119(3) . .
H1W O10 H2W 114(3) . .
C8 N1 C7 127.9(4) . .
C8 N1 H1 116(3) . .
C7 N1 H1 116(3) . .
O6 N2 O4 123.9(4) . .
O6 N2 O5 119.2(4) . .
O4 N2 O5 116.9(3) . .
O9 N3 O7 122.4(4) . .
O9 N3 O8 122.1(4) . .
O7 N3 O8 115.5(3) . .
O9 N3 Dy1 179.3(3) . .
O7 N3 Dy1 58.3(2) . .
O8 N3 Dy1 57.1(2) . .
C15 N4 Dy1 170.3(4) . .
O3 C1 O2 124.1(4) . .
O3 C1 C2 117.1(3) . .
O2 C1 C2 118.8(3) . .
C3 C2 C7 118.3(3) . .
C3 C2 C1 116.5(3) . .
C7 C2 C1 125.2(3) . .
C4 C3 C2 121.2(4) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C3 C4 C5 120.7(4) . .
C3 C4 Cl1 119.2(3) . .
C5 C4 Cl1 120.1(3) . .
C6 C5 C4 118.8(4) . .
C6 C5 H5 120.6 . .
C4 C5 H5 120.6 . .
C5 C6 C7 121.4(4) . .
C5 C6 H6 119.3 . .
C7 C6 H6 119.3 . .
C6 C7 N1 121.4(4) . .
C6 C7 C2 119.5(4) . .
N1 C7 C2 119.1(3) . .
N1 C8 C9 124.2(4) . .
N1 C8 H8 117.9 . .
C9 C8 H8 117.9 . .
C8 C9 C10 118.8(4) . .
C8 C9 C14 122.1(4) . .
C10 C9 C14 119.1(4) . .
C11 C10 C9 121.1(4) . .
C11 C10 H10 119.5 . .
C9 C10 H10 119.5 . .
C10 C11 C12 119.6(4) . .
C10 C11 H11 120.2 . .
C12 C11 H11 120.2 . .
C13 C12 C11 121.5(4) . .
C13 C12 H12 119.3 . .
C11 C12 H12 119.3 . .
C12 C13 C14 120.7(4) . .
C12 C13 H13 119.6 . .
C14 C13 H13 119.6 . .
O1 C14 C13 121.8(4) . .
O1 C14 C9 120.1(4) . .
C13 C14 C9 118.0(4) . .
N4 C15 C16 178.4(5) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.231(3) .
Dy1 O3 2.305(3) 2_666
Dy1 O2 2.347(3) .
Dy1 O8 2.445(3) .
Dy1 O10 2.459(3) .
Dy1 O7 2.472(3) .
Dy1 O5 2.500(3) .
Dy1 N4 2.511(4) .
Dy1 O4 2.589(3) .
Dy1 N3 2.889(4) .
Cl1 C4 1.730(4) .
O1 C14 1.297(5) .
O2 C1 1.258(4) .
O3 C1 1.249(5) .
O3 Dy1 2.305(3) 2_666
O4 N2 1.263(5) .
O5 N2 1.265(5) .
O6 N2 1.229(5) .
O7 N3 1.266(5) .
O8 N3 1.275(5) .
O9 N3 1.217(4) .
O10 H1W 0.891(18) .
O10 H2W 0.883(18) .
N1 C8 1.316(5) .
N1 C7 1.411(5) .
N1 H1 0.856(19) .
N4 C15 1.127(6) .
C1 C2 1.509(5) .
C2 C3 1.388(5) .
C2 C7 1.416(5) .
C3 C4 1.381(5) .
C3 H3 0.9500 .
C4 C5 1.392(6) .
C5 C6 1.378(6) .
C5 H5 0.9500 .
C6 C7 1.395(5) .
C6 H6 0.9500 .
C8 C9 1.415(6) .
C8 H8 0.9500 .
C9 C10 1.423(6) .
C9 C14 1.431(6) .
C10 C11 1.357(6) .
C10 H10 0.9500 .
C11 C12 1.402(6) .
C11 H11 0.9500 .
C12 C13 1.367(6) .
C12 H12 0.9500 .
C13 C14 1.411(6) .
C13 H13 0.9500 .
C15 C16 1.448(6) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 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
O10 H1W O5 0.891(18) 1.96(2) 2.828(4) 164(5) 2_666
O10 H1W N2 0.891(18) 2.65(3) 3.435(5) 147(4) 2_666
O10 H2W O6 0.883(18) 1.95(2) 2.825(4) 170(4) 1_455
N1 H1 O1 0.856(19) 1.96(4) 2.638(4) 135(4) .
N1 H1 O2 0.856(19) 1.98(3) 2.672(4) 138(4) .
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
Dy1 O4 N2 O6 176.1(4) .
Dy1 O4 N2 O5 -4.6(4) .
Dy1 O5 N2 O6 -175.9(3) .
Dy1 O5 N2 O4 4.8(4) .
Dy1 O7 N3 O9 179.9(3) .
Dy1 O7 N3 O8 0.5(4) .
Dy1 O8 N3 O9 -180.0(3) .
Dy1 O8 N3 O7 -0.6(4) .
Dy1 O3 C1 O2 15.6(8) 2_666
Dy1 O3 C1 C2 -164.9(3) 2_666
Dy1 O2 C1 O3 52.8(7) .
Dy1 O2 C1 C2 -126.7(5) .
O3 C1 C2 C3 0.8(5) .
O2 C1 C2 C3 -179.7(3) .
O3 C1 C2 C7 179.5(4) .
O2 C1 C2 C7 -1.0(6) .
C7 C2 C3 C4 -0.2(6) .
C1 C2 C3 C4 178.5(3) .
C2 C3 C4 C5 1.1(6) .
C2 C3 C4 Cl1 -178.0(3) .
C3 C4 C5 C6 -0.7(6) .
Cl1 C4 C5 C6 178.4(3) .
C4 C5 C6 C7 -0.5(6) .
C5 C6 C7 N1 -179.3(4) .
C5 C6 C7 C2 1.4(6) .
C8 N1 C7 C6 0.1(6) .
C8 N1 C7 C2 179.5(4) .
C3 C2 C7 C6 -0.9(5) .
C1 C2 C7 C6 -179.6(3) .
C3 C2 C7 N1 179.7(3) .
C1 C2 C7 N1 1.1(6) .
C7 N1 C8 C9 -176.6(4) .
N1 C8 C9 C10 179.3(4) .
N1 C8 C9 C14 -0.7(6) .
C8 C9 C10 C11 -179.2(4) .
C14 C9 C10 C11 0.7(6) .
C9 C10 C11 C12 0.1(6) .
C10 C11 C12 C13 -0.4(6) .
C11 C12 C13 C14 -0.1(6) .
Dy1 O1 C14 C13 -47.5(7) .
Dy1 O1 C14 C9 133.5(4) .
C12 C13 C14 O1 -178.1(4) .
C12 C13 C14 C9 0.9(6) .
C8 C9 C14 O1 -2.2(6) .
C10 C9 C14 O1 177.9(3) .
C8 C9 C14 C13 178.8(4) .
C10 C9 C14 C13 -1.1(6) .
