#------------------------------------------------------------------------------
#$Date: 2021-11-20 01:56:39 +0200 (Sat, 20 Nov 2021) $
#$Revision: 270764 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/88/7708892.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_7708892
loop_
_publ_author_name
'Wu, Jianfeng'
'Demeshko, Serhiy'
'Dechert, Sebastian'
'Meyer, Franc'
_publ_section_title
;
 Macrocycle Based Dinuclear Dysprosium(III) Single Molecule Magnets with
 Local D5h Coordination Geometry
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02815D
_journal_year                    2021
_chemical_formula_moiety         'C26 H40 Cl4 Dy2 N10'
_chemical_formula_sum            'C26 H40 Cl4 Dy2 N10'
_chemical_formula_weight         959.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-16 deposited with the CCDC.	2021-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.837(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9524(3)
_cell_length_b                   11.7805(5)
_cell_length_c                   15.8173(6)
_cell_measurement_reflns_used    13782
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.865
_cell_measurement_theta_min      2.175
_cell_volume                     1626.46(11)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2015)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2015)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2015)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13782
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.865
_diffrn_reflns_theta_min         2.175
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.923
_exptl_absorpt_correction_T_max  0.8004
_exptl_absorpt_correction_T_min  0.6557
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2015)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.882
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3450
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0293
_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)+(0.0357P)²+2.0961P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2911
_reflns_number_total             3450
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02815d2.cif
_cod_data_source_block           Dy2starCl-jwu9
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7708892
_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_min   0.506
_shelx_estimated_absorpt_t_max   0.639
loop_
_space_group_symop_operation_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_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 0.52095(2) 0.32338(2) 0.57531(2) 0.02451(8) Uani 1 1 d . . . . .
Cl1 Cl 0.34687(14) 0.21599(10) 0.44548(8) 0.0373(3) Uani 1 1 d . . . . .
Cl2 Cl 0.71015(13) 0.41128(11) 0.70835(8) 0.0368(3) Uani 1 1 d . . . . .
N1 N 0.6635(4) 0.4140(3) 0.4779(2) 0.0262(8) Uani 1 1 d . . . . .
N2 N 0.6569(4) 0.5158(3) 0.4390(2) 0.0247(7) Uani 1 1 d . . . . .
N3 N 0.7410(4) 0.2106(3) 0.5524(2) 0.0298(8) Uani 1 1 d D . . . .
N4 N 0.5427(5) 0.1365(3) 0.6581(2) 0.0345(9) Uani 1 1 d D . . . .
N5 N 0.6757(6) 0.6978(3) 0.3402(3) 0.0456(12) Uani 1 1 d . . . . .
C1 C 0.8647(5) 0.4251(4) 0.4123(3) 0.0264(9) Uani 1 1 d . . . . .
C2 C 0.7881(5) 0.3571(4) 0.4622(3) 0.0272(9) Uani 1 1 d . . . . .
C3 C 0.7766(5) 0.5240(4) 0.3990(3) 0.0253(9) Uani 1 1 d . . . . .
C4 C 1.0104(5) 0.3983(4) 0.3834(3) 0.0380(11) Uani 1 1 d . . . . .
H4A H 1.070465 0.467929 0.383761 0.057 Uiso 1 1 calc R U . . .
H4B H 0.985128 0.366776 0.324623 0.057 Uiso 1 1 calc R U . . .
H4C H 1.070437 0.342777 0.423105 0.057 Uiso 1 1 calc R U . . .
C5 C 0.8190(5) 0.2425(4) 0.4979(3) 0.0299(10) Uani 1 1 d . . . . .
C6 C 0.9331(7) 0.1688(5) 0.4659(5) 0.0567(16) Uani 1 1 d . . . . .
H6A H 0.922262 0.180396 0.403524 0.085 Uiso 1 1 calc R U . . .
H6B H 0.913805 0.088851 0.477067 0.085 Uiso 1 1 calc R U . . .
H6C H 1.037224 0.189170 0.496524 0.085 Uiso 1 1 calc R U . . .
C7A C 0.7748(16) 0.0982(11) 0.5945(11) 0.039(5) Uani 0.698(8) 1 d D . P A 1
H7A H 0.886619 0.084185 0.609044 0.047 Uiso 0.698(8) 1 calc R U P A 1
H7B H 0.724560 0.037165 0.555313 0.047 Uiso 0.698(8) 1 calc R U P A 1
C8A C 0.7121(7) 0.1012(6) 0.6770(4) 0.0340(18) Uani 0.698(8) 1 d D . P A 1
H8A H 0.773085 0.155498 0.718634 0.041 Uiso 0.698(8) 1 calc R U P A 1
H8B H 0.723269 0.025156 0.704256 0.041 Uiso 0.698(8) 1 calc R U P A 1
C9A C 0.4553(9) 0.0375(6) 0.6168(5) 0.0385(19) Uani 0.698(8) 1 d D . P A 1
H9A H 0.471138 -0.026458 0.657429 0.058 Uiso 0.698(8) 1 calc R U P A 1
H9B H 0.490620 0.016669 0.564541 0.058 Uiso 0.698(8) 1 calc R U P A 1
H9C H 0.346095 0.056570 0.601071 0.058 Uiso 0.698(8) 1 calc R U P A 1
C12A C 0.3437(8) 0.2061(5) 0.7260(5) 0.0281(16) Uani 0.698(8) 1 d D . P A 1
H12A H 0.322563 0.234910 0.780940 0.034 Uiso 0.698(8) 1 calc R U P A 1
H12B H 0.269079 0.145081 0.704078 0.034 Uiso 0.698(8) 1 calc R U P A 1
C13A C 0.5051(9) 0.1584(6) 0.7427(4) 0.0303(16) Uani 0.698(8) 1 d D . P A 1
H13A H 0.578509 0.213412 0.776326 0.036 Uiso 0.698(8) 1 calc R U P A 1
H13B H 0.511073 0.087058 0.776350 0.036 Uiso 0.698(8) 1 calc R U P A 1
C7B C 0.761(3) 0.102(2) 0.603(2) 0.035(8) Uani 0.302(8) 1 d D . P A 2
H7C H 0.825995 0.116614 0.660886 0.042 Uiso 0.302(8) 1 calc R U P A 2
H7D H 0.814381 0.046707 0.572904 0.042 Uiso 0.302(8) 1 calc R U P A 2
C8B C 0.6092(19) 0.0525(13) 0.6120(11) 0.044(5) Uani 0.302(8) 1 d D . P A 2
H8C H 0.541817 0.037636 0.554452 0.053 Uiso 0.302(8) 1 calc R U P A 2
H8D H 0.625569 -0.019502 0.645054 0.053 Uiso 0.302(8) 1 calc R U P A 2
C9B C 0.603(3) 0.1584(16) 0.7496(9) 0.044(5) Uani 0.302(8) 1 d D . P A 2
H9D H 0.574629 0.095797 0.783815 0.066 Uiso 0.302(8) 1 calc R U P A 2
H9E H 0.559813 0.229470 0.765890 0.066 Uiso 0.302(8) 1 calc R U P A 2
H9F H 0.714699 0.164582 0.760965 0.066 Uiso 0.302(8) 1 calc R U P A 2
C12B C 0.274(2) 0.1879(10) 0.6825(14) 0.042(4) Uani 0.302(8) 1 d D . P A 2
H12C H 0.164529 0.175216 0.654805 0.050 Uiso 0.302(8) 1 calc R U P A 2
H12D H 0.287119 0.180323 0.746124 0.050 Uiso 0.302(8) 1 calc R U P A 2
C13B C 0.3746(15) 0.1035(13) 0.6488(11) 0.042(4) Uani 0.302(8) 1 d D . P A 2
H13C H 0.329542 0.090241 0.586524 0.050 Uiso 0.302(8) 1 calc R U P A 2
H13D H 0.371069 0.030554 0.679293 0.050 Uiso 0.302(8) 1 calc R U P A 2
C10 C 0.7868(5) 0.6269(4) 0.3477(3) 0.0277(9) Uani 1 1 d . . . . .
C11 C 0.9160(6) 0.6440(5) 0.3045(4) 0.0463(13) Uani 1 1 d . . . . .
H11A H 0.913554 0.584876 0.260606 0.069 Uiso 1 1 calc R U . . .
H11B H 1.013030 0.639565 0.347708 0.069 Uiso 1 1 calc R U . . .
H11C H 0.906897 0.718727 0.276653 0.069 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'
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
_geom_angle_publ_flag
N5 Dy1 N2 66.32(13) 3_666 3_666 ?
N5 Dy1 N1 157.66(13) 3_666 . ?
N2 Dy1 N1 91.34(11) 3_666 . ?
N5 Dy1 N3 136.00(13) 3_666 . ?
N2 Dy1 N3 157.67(12) 3_666 . ?
N1 Dy1 N3 66.33(12) . . ?
N5 Dy1 N4 67.26(13) 3_666 . ?
N2 Dy1 N4 133.57(13) 3_666 . ?
N1 Dy1 N4 135.08(12) . . ?
N3 Dy1 N4 68.76(13) . . ?
N5 Dy1 Cl2 90.98(13) 3_666 . ?
N2 Dy1 Cl2 93.43(8) 3_666 . ?
N1 Dy1 Cl2 89.92(9) . . ?
N3 Dy1 Cl2 86.31(9) . . ?
N4 Dy1 Cl2 88.08(9) . . ?
N5 Dy1 Cl1 90.22(13) 3_666 . ?
N2 Dy1 Cl1 92.28(8) 3_666 . ?
N1 Dy1 Cl1 91.14(9) . . ?
N3 Dy1 Cl1 88.86(9) . . ?
N4 Dy1 Cl1 87.12(9) . . ?
Cl2 Dy1 Cl1 174.17(4) . . ?
N2 N1 C2 108.0(4) . . ?
N2 N1 Dy1 134.4(3) . . ?
C2 N1 Dy1 117.3(3) . . ?
N1 N2 C3 108.4(3) . . ?
N1 N2 Dy1 133.9(3) . 3_666 ?
C3 N2 Dy1 117.6(3) . 3_666 ?
C5 N3 C7A 118.5(6) . . ?
C5 N3 C7B 126.3(12) . . ?
C5 N3 Dy1 120.8(3) . . ?
C7A N3 Dy1 120.3(5) . . ?
C7B N3 Dy1 112.8(11) . . ?
C8B N4 C9B 121.7(12) . . ?
C13A N4 C9A 109.5(5) . . ?
C8B N4 C13B 106.6(10) . . ?
C9B N4 C13B 106.3(11) . . ?
C13A N4 C8A 106.6(5) . . ?
C9A N4 C8A 106.0(5) . . ?
C8B N4 Dy1 109.2(7) . . ?
C9B N4 Dy1 109.2(8) . . ?
C13A N4 Dy1 108.0(3) . . ?
C9A N4 Dy1 118.9(3) . . ?
C13B N4 Dy1 102.0(6) . . ?
C8A N4 Dy1 107.1(3) . . ?
C10 N5 C12B 109.8(8) . 3_666 ?
C10 N5 C12A 120.8(4) . 3_666 ?
C10 N5 Dy1 121.4(3) . 3_666 ?
C12A N5 Dy1 117.7(3) 3_666 3_666 ?
C3 C1 C2 103.3(4) . . ?
C3 C1 C4 128.8(4) . . ?
C2 C1 C4 127.9(4) . . ?
N1 C2 C1 110.0(4) . . ?
N1 C2 C5 118.1(4) . . ?
C1 C2 C5 131.9(4) . . ?
N2 C3 C1 110.3(4) . . ?
N2 C3 C10 117.7(4) . . ?
C1 C3 C10 131.9(4) . . ?
N3 C5 C2 116.5(4) . . ?
N3 C5 C6 124.5(4) . . ?
C2 C5 C6 119.0(4) . . ?
N3 C7A C8A 106.6(9) . . ?
C7A C8A N4 111.9(7) . . ?
C13A C12A N5 110.7(5) . 3_666 ?
N4 C13A C12A 107.9(6) . . ?
N3 C7B C8B 112.3(16) . . ?
N4 C8B C7B 105.3(18) . . ?
N5 C12B C13B 105.7(11) 3_666 . ?
C12B C13B N4 116.7(12) . . ?
N5 C10 C3 116.3(4) . . ?
N5 C10 C11 122.6(4) . . ?
C3 C10 C11 121.1(4) . . ?
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 N5 2.447(4) 3_666 ?
Dy1 N2 2.452(3) 3_666 ?
Dy1 N1 2.453(4) . ?
Dy1 N3 2.469(4) . ?
Dy1 N4 2.547(4) . ?
Dy1 Cl2 2.6050(12) . ?
Dy1 Cl1 2.6123(12) . ?
N1 N2 1.343(5) . ?
N1 C2 1.371(5) . ?
N2 C3 1.364(5) . ?
N3 C5 1.281(6) . ?
N3 C7A 1.482(9) . ?
N3 C7B 1.490(14) . ?
N4 C8B 1.434(12) . ?
N4 C9B 1.451(14) . ?
N4 C13A 1.473(7) . ?
N4 C9A 1.473(8) . ?
N4 C13B 1.530(13) . ?
N4 C8A 1.536(7) . ?
N5 C10 1.284(6) . ?
N5 C12B 1.491(12) 3_666 ?
N5 C12A 1.525(7) 3_666 ?
C1 C3 1.397(6) . ?
C1 C2 1.405(6) . ?
C1 C4 1.508(6) . ?
C2 C5 1.465(6) . ?
C3 C10 1.474(6) . ?
C5 C6 1.511(7) . ?
C7A C8A 1.531(13) . ?
C12A C13A 1.518(9) . ?
C7B C8B 1.518(17) . ?
C12B C13B 1.517(15) . ?
C10 C11 1.481(7) . ?
