#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:59:00 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294586 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/67/7716705.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_7716705
loop_
_publ_author_name
'Oggianu, Mariangela'
'Bertolotti, Federica'
'Manna, Fabio'
'Congiu, Francesco'
'Cappai, Antonio'
'Melis, Claudio'
'Concas, Giorgio'
'Avarvari, Narcis'
'Masciocchi, Norberto'
'Mercuri, Maria Laura'
_publ_section_title
;
 Slow magnetic relaxation in a heteroleptic anilate-based DyIII
 metal-organic framework.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14265
_journal_page_last               14271
_journal_paper_doi               10.1039/d4dt01979b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C11 H8 Cl F2 N O10 Tb'
_chemical_formula_sum            'C11 H8 Cl F2 N O10 Tb'
_chemical_formula_weight         546.55
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-10-10T15:40:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                95.724(4)
_cell_angle_beta                 99.786(5)
_cell_angle_gamma                90.157(5)
_cell_formula_units_Z            2
_cell_length_a                   5.1017(3)
_cell_length_b                   10.7630(6)
_cell_length_c                   14.8712(8)
_cell_measurement_reflns_used    4057
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      71.815
_cell_measurement_theta_min      4.04
_cell_volume                     800.52(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, V2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector_area_resol_mean 5.199
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6434
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        71
_diffrn_reflns_theta_max         71.888
_diffrn_reflns_theta_min         3.031
_exptl_absorpt_coefficient_mu    24.02
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.42749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_description       needle
_exptl_crystal_F_000             522
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.952
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3081
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0790P)²+0.0433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0
_reflns_number_gt                2858
_reflns_number_total             3081
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01979b2.cif
_cod_data_source_block           mo43b
_cod_depositor_comments          'Adding full bibliography for 7716705.cif.'
_cod_database_code               7716705
_shelx_shelxl_version_number     2018/3
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_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
C1 C 0.1419(13) 0.6052(6) 0.0542(4) 0.0251(12) Uani 1 1 d . . . . .
C2 C -0.0597(12) 0.5265(6) 0.0913(4) 0.0230(12) Uani 1 1 d . . . . .
C3 C -0.1929(12) 0.4259(6) 0.0332(4) 0.0242(12) Uani 1 1 d D . . . .
C4 C -0.384(11) 0.342(5) 0.071(4) 0.047(19) Uani 0.5 1 d D U P A 2
C5 C 0.6595(14) 0.6266(6) 0.3523(4) 0.0264(13) Uani 1 1 d . . . . .
C6 C 0.5767(13) 0.5598(6) 0.4277(4) 0.0258(12) Uani 1 1 d . . . . .
C7 C 0.3729(13) 0.4726(6) 0.4112(4) 0.0260(13) Uani 1 1 d . . . . .
C8 C 0.7071(12) 0.5851(6) 0.5178(4) 0.0227(12) Uani 1 1 d . . . . .
C9 C 0.1488(13) 0.9077(6) 0.4556(5) 0.0254(13) Uani 1 1 d . . . . .
C10 C 0.2256(13) 0.9416(6) 0.5504(4) 0.0247(12) Uani 1 1 d D . . . .
C11 C 0.0954(12) 1.0343(6) 0.5969(4) 0.0230(12) Uani 1 1 d . . . . .
C12 C 0.466(7) 0.886(5) 0.605(3) 0.036(10) Uani 0.5 1 d D U P B 4
N1 N -0.537(3) 0.2938(14) 0.0961(10) 0.043(3) Uani 0.5 1 d . . P A 2
N2 N 0.618(4) 0.8392(17) 0.6387(13) 0.056(5) Uani 0.5 1 d . . P B 4
O1 O 0.2508(9) 0.6948(4) 0.1095(3) 0.0262(9) Uani 1 1 d . . . . .
O2 O -0.0941(10) 0.5587(4) 0.1713(3) 0.0294(10) Uani 1 1 d . . . . .
O3 O 0.4827(9) 0.6605(4) 0.2904(3) 0.0277(9) Uani 1 1 d . . . . .
O4 O 0.9028(9) 0.6454(5) 0.3570(3) 0.0305(10) Uani 1 1 d . . . . .
O5 O 0.2754(9) 0.8352(5) 0.4087(3) 0.0277(10) Uani 1 1 d . . . . .
O6 O 0.1601(9) 1.0768(4) 0.6802(3) 0.0268(9) Uani 1 1 d . . . . .
O7 O -0.2508(9) 0.8087(5) 0.1340(3) 0.0292(9) Uani 1 1 d . . . . .
H7A H -0.251462 0.861077 0.094554 0.044 Uiso 1 1 d R U . . .
H7B H -0.408898 0.778398 0.123861 0.044 Uiso 1 1 d R U . . .
O8 O 0.3096(9) 0.9306(4) 0.2205(3) 0.0290(10) Uani 1 1 d . . . . .
H8A H 0.457319 0.941301 0.257336 0.043 Uiso 1 1 d R U . . .
H8B H 0.224687 0.997163 0.230963 0.043 Uiso 1 1 d R U . . .
O9 O -0.227(3) 1.0108(12) 0.0446(10) 0.124(5) Uani 1 1 d . . . . .
H9A H -0.115923 1.058815 0.027802 0.187 Uiso 1 1 d R U . . .
H9B H -0.363719 1.055019 0.047043 0.187 Uiso 1 1 d R U . . .
O10 O 0.090(3) 1.1684(10) 0.1831(8) 0.102(3) Uani 1 1 d . . . . .
H10A H -0.033167 1.196495 0.210999 0.153 Uiso 1 1 d R U . . .
H10B H 0.214333 1.223335 0.197857 0.153 Uiso 1 1 d R U . . .
F1 F 0.9078(8) 0.6688(4) 0.5402(3) 0.0329(8) Uani 1 1 d . . . . .
F2 F 0.2489(8) 0.4381(4) 0.3258(3) 0.0336(9) Uani 1 1 d . . . . .
Cl1 Cl -0.424(3) 0.3443(9) 0.0729(6) 0.032(2) Uani 0.5 1 d . . P A 1
Cl2 Cl 0.4918(19) 0.8622(13) 0.6080(8) 0.036(2) Uani 0.5 1 d . . P B 3
Tb1 Tb 0.08105(6) 0.75158(3) 0.25326(2) 0.02241(16) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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
O1 C1 C3 125.3(6) . 2_565 ?
O1 C1 C2 115.1(5) . . ?
C3 C1 C2 119.6(6) 2_565 . ?
O2 C2 C3 125.2(6) . . ?
O2 C2 C1 116.3(6) . . ?
C3 C2 C1 118.5(6) . . ?
C1 C3 C2 121.9(6) 2_565 . ?
C1 C3 C4 119(2) 2_565 . ?
C2 C3 C4 119(2) . . ?
C1 C3 Cl1 120.0(6) 2_565 . ?
C2 C3 Cl1 118.1(6) . . ?
N1 C4 C3 172(6) . . ?
O4 C5 O3 124.6(6) . . ?
O4 C5 C6 116.5(6) . . ?
O3 C5 C6 118.9(6) . . ?
C7 C6 C8 117.3(6) . . ?
C7 C6 C5 122.2(6) . . ?
C8 C6 C5 120.5(6) . . ?
F2 C7 C6 120.8(6) . . ?
F2 C7 C8 117.8(6) . 2_666 ?
C6 C7 C8 121.4(6) . 2_666 ?
F1 C8 C6 121.4(6) . . ?
F1 C8 C7 117.3(6) . 2_666 ?
C6 C8 C7 121.2(6) . 2_666 ?
O5 C9 C10 124.2(6) . . ?
O5 C9 C11 115.8(6) . 2_576 ?
C10 C9 C11 119.9(6) . 2_576 ?
C11 C10 C9 121.6(6) . . ?
C11 C10 C12 117(2) . . ?
C9 C10 C12 121(2) . . ?
C11 C10 Cl2 121.0(7) . . ?
C9 C10 Cl2 117.4(6) . . ?
O6 C11 C10 126.2(6) . . ?
O6 C11 C9 115.4(5) . 2_576 ?
C10 C11 C9 118.3(6) . 2_576 ?
N2 C12 C10 173(5) . . ?
C1 O1 Tb1 119.4(4) . . ?
C2 O2 Tb1 122.1(4) . . ?
C5 O3 Tb1 147.7(4) . . ?
C5 O4 Tb1 123.4(4) . 1_655 ?
C9 O5 Tb1 121.0(4) . . ?
C11 O6 Tb1 121.1(4) . 2_576 ?
Tb1 O7 H7A 132.5 . . ?
Tb1 O7 H7B 123 . . ?
H7A O7 H7B 104.5 . . ?
Tb1 O8 H8A 109.7 . . ?
Tb1 O8 H8B 111.3 . . ?
H8A O8 H8B 104.3 . . ?
H9A O9 H9B 104.5 . . ?
H10A O10 H10B 104.4 . . ?
O3 Tb1 O4 91.37(17) . 1_455 ?
O3 Tb1 O7 146.39(15) . . ?
O4 Tb1 O7 111.81(18) 1_455 . ?
O3 Tb1 O8 88.61(17) . . ?
O4 Tb1 O8 149.42(16) 1_455 . ?
O7 Tb1 O8 83.23(17) . . ?
O3 Tb1 O2 89.56(17) . . ?
O4 Tb1 O2 73.99(16) 1_455 . ?
O7 Tb1 O2 74.84(17) . . ?
O8 Tb1 O2 136.58(16) . . ?
O3 Tb1 O5 72.15(15) . . ?
O4 Tb1 O5 70.67(17) 1_455 . ?
O7 Tb1 O5 137.38(16) . . ?
O8 Tb1 O5 80.29(16) . . ?
O2 Tb1 O5 139.40(17) . . ?
O3 Tb1 O6 136.40(16) . 2_576 ?
O4 Tb1 O6 81.46(16) 1_455 2_576 ?
O7 Tb1 O6 73.33(15) . 2_576 ?
O8 Tb1 O6 77.64(16) . 2_576 ?
O2 Tb1 O6 128.32(16) . 2_576 ?
O5 Tb1 O6 64.86(15) . 2_576 ?
O3 Tb1 O1 72.53(15) . . ?
O4 Tb1 O1 136.01(16) 1_455 . ?
O7 Tb1 O1 73.91(15) . . ?
O8 Tb1 O1 72.67(15) . . ?
O2 Tb1 O1 65.47(15) . . ?
O5 Tb1 O1 135.51(15) . . ?
O6 Tb1 O1 137.75(16) 2_576 . ?
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
C1 O1 1.264(8) . ?
C1 C3 1.378(9) 2_565 ?
C1 C2 1.536(9) . ?
C2 O2 1.247(8) . ?
C2 C3 1.410(9) . ?
C3 C4 1.53(2) . ?
C3 Cl1 1.685(11) . ?
C4 N1 1.08(3) . ?
C5 O4 1.246(8) . ?
C5 O3 1.257(8) . ?
C5 C6 1.507(9) . ?
C6 C7 1.373(10) . ?
C6 C8 1.391(9) . ?
C7 F2 1.334(8) . ?
C7 C8 1.395(9) 2_666 ?
C8 F1 1.339(8) . ?
C9 O5 1.249(8) . ?
C9 C10 1.408(9) . ?
C9 C11 1.524(9) 2_576 ?
C10 C11 1.392(9) . ?
C10 C12 1.51(2) . ?
C10 Cl2 1.751(12) . ?
C11 O6 1.265(8) . ?
C12 N2 1.01(3) . ?
O1 Tb1 2.463(4) . ?
O2 Tb1 2.389(5) . ?
O3 Tb1 2.280(5) . ?
O4 Tb1 2.310(5) 1_655 ?
O5 Tb1 2.437(4) . ?
O6 Tb1 2.443(4) 2_576 ?
O7 Tb1 2.365(5) . ?
O7 H7A 0.8528 . ?
O7 H7B 0.8529 . ?
O8 Tb1 2.382(5) . ?
O8 H8A 0.8532 . ?
O8 H8B 0.8531 . ?
O9 H9A 0.85 . ?
O9 H9B 0.85 . ?
O10 H10A 0.8517 . ?
O10 H10B 0.8502 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 -0.1(8) . . . . ?
C3 C1 C2 O2 179.1(6) 2_565 . . . ?
O1 C1 C2 C3 179.0(6) . . . . ?
C3 C1 C2 C3 -1.7(10) 2_565 . . . ?
O2 C2 C3 C1 -179.2(6) . . . 2_565 ?
C1 C2 C3 C1 1.8(10) . . . 2_565 ?
O2 C2 C3 C4 -4(3) . . . . ?
C1 C2 C3 C4 177(3) . . . . ?
O2 C2 C3 Cl1 1.8(11) . . . . ?
C1 C2 C3 Cl1 -177.3(7) . . . . ?
O4 C5 C6 C7 -141.4(6) . . . . ?
O3 C5 C6 C7 39.5(9) . . . . ?
O4 C5 C6 C8 38.6(8) . . . . ?
O3 C5 C6 C8 -140.6(6) . . . . ?
C8 C6 C7 F2 -176.0(5) . . . . ?
C5 C6 C7 F2 3.9(9) . . . . ?
C8 C6 C7 C8 2.4(10) . . . 2_666 ?
C5 C6 C7 C8 -177.7(6) . . . 2_666 ?
C7 C6 C8 F1 -179.9(5) . . . . ?
C5 C6 C8 F1 0.2(9) . . . . ?
C7 C6 C8 C7 -2.3(10) . . . 2_666 ?
C5 C6 C8 C7 177.7(5) . . . 2_666 ?
O5 C9 C10 C11 172.0(6) . . . . ?
C11 C9 C10 C11 -4.8(11) 2_576 . . . ?
O5 C9 C10 C12 -3(3) . . . . ?
C11 C9 C10 C12 -180(2) 2_576 . . . ?
O5 C9 C10 Cl2 -8.2(11) . . . . ?
C11 C9 C10 Cl2 175.0(7) 2_576 . . . ?
C9 C10 C11 O6 -175.1(6) . . . . ?
C12 C10 C11 O6 0(2) . . . . ?
Cl2 C10 C11 O6 5.1(11) . . . . ?
C9 C10 C11 C9 4.7(11) . . . 2_576 ?
C12 C10 C11 C9 -180(2) . . . 2_576 ?
Cl2 C10 C11 C9 -175.1(7) . . . 2_576 ?
C3 C1 O1 Tb1 171.0(5) 2_565 . . . ?
C2 C1 O1 Tb1 -9.8(7) . . . . ?
C3 C2 O2 Tb1 -168.5(5) . . . . ?
C1 C2 O2 Tb1 10.6(8) . . . . ?
O4 C5 O3 Tb1 -134.6(7) . . . . ?
C6 C5 O3 Tb1 44.5(11) . . . . ?
O3 C5 O4 Tb1 1.3(9) . . . 1_655 ?
C6 C5 O4 Tb1 -177.8(4) . . . 1_655 ?
C10 C9 O5 Tb1 167.9(5) . . . . ?
C11 C9 O5 Tb1 -15.2(8) 2_576 . . . ?
C10 C11 O6 Tb1 176.5(5) . . . 2_576 ?
C9 C11 O6 Tb1 -3.4(7) 2_576 . . 2_576 ?
