#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:26:15 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223509 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234435.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_7234435
loop_
_publ_author_name
'Wang, Juan'
'Yang, Mingfang'
'Sun, Juan'
'Li, Hui'
'Liu, Jinjin'
'Wang, Qinglun'
'Li, Licun'
'Ma, Yue'
'Zhao, Bin'
'Cheng, Peng'
_publ_section_title
;
 Enhancing the energy barrier of dysprosium(iii) single-molecule magnets
 by tuning the magnetic interactions through different N-oxide bridging
 ligands
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              6219
_journal_paper_doi               10.1039/C9CE01378D
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C38 H14 F36 N4 O14 Tb2'
_chemical_formula_sum            'C38 H14 F36 N4 O14 Tb2'
_chemical_formula_weight         1752.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-03-05 deposited with the CCDC.    2019-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.26(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.080(4)
_cell_length_b                   12.930(3)
_cell_length_c                   22.428(5)
_cell_measurement_reflns_used    6678
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      25.0441
_cell_measurement_theta_min      1.8639
_cell_volume                     5925(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23123
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.864
_exptl_absorpt_coefficient_mu    2.541
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_description       block
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.249
_refine_diff_density_min         -2.105
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5234
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.303
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0671
_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)+(0.0968P)²+4.4963P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4148
_reflns_number_total             5234
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce01378d2.cif
_cod_data_source_block           shelxl_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7234434--7234439.cif.'
_cod_database_code               7234435
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Tb1 Tb 0.30438(2) 0.23560(3) 0.09029(2) 0.0621(2) Uani 1 1 d . U
O1 O 0.3562(3) 0.2193(5) 0.1929(3) 0.0793(11) Uani 1 1 d . U
O2 O 0.3650(3) 0.0788(5) 0.1023(3) 0.0767(12) Uani 1 1 d . U
O3 O 0.2330(3) 0.1063(5) 0.1070(3) 0.0821(11) Uani 1 1 d . U
O4 O 0.2289(3) 0.3101(5) 0.1381(3) 0.0807(11) Uani 1 1 d . U
O5 O 0.3527(3) 0.3986(5) 0.1178(3) 0.0780(11) Uani 1 1 d . U
O6 O 0.3880(3) 0.2591(4) 0.0386(3) 0.0747(11) Uani 1 1 d . U
O7 O 0.2386(3) 0.3445(5) 0.0096(3) 0.0746(11) Uani 1 1 d . U
N1 N 0.2269(4) 0.4464(6) 0.0194(4) 0.082(2) Uani 1 1 d . .
N2 N 0.2055(9) 0.6488(10) 0.0391(7) 0.160(6) Uani 1 1 d . .
C1 C 0.4104(7) 0.1878(12) 0.2943(6) 0.111(4) Uani 1 1 d . U
C2 C 0.3905(4) 0.1520(8) 0.2262(4) 0.083(3) Uani 1 1 d . .
C3 C 0.4091(5) 0.0565(8) 0.2074(4) 0.083(3) Uani 1 1 d . .
H3 H 0.4317 0.0103 0.2369 0.099 Uiso 1 1 calc R U
C4 C 0.3950(4) 0.0290(7) 0.1469(4) 0.071(2) Uani 1 1 d . .
C5 C 0.4205(7) -0.0742(10) 0.1315(5) 0.104(4) Uani 1 1 d . .
C6 C 0.1680(8) -0.0100(14) 0.1436(11) 0.155(6) Uani 1 1 d . U
C7 C 0.1956(5) 0.0984(11) 0.1443(6) 0.099(3) Uani 1 1 d . U
C8 C 0.1792(6) 0.1740(13) 0.1776(7) 0.119(4) Uani 1 1 d . U
H8 H 0.1558 0.1571 0.2064 0.143 Uiso 1 1 calc R U
C9 C 0.1945(6) 0.2733(11) 0.1720(6) 0.098(3) Uani 1 1 d . U
C10 C 0.1671(11) 0.3589(18) 0.2084(12) 0.168(7) Uani 1 1 d . U
C11 C 0.4204(9) 0.5407(12) 0.1512(8) 0.126(5) Uani 1 1 d . .
C12 C 0.4053(5) 0.4409(8) 0.1146(5) 0.090(3) Uani 1 1 d . U
C13 C 0.4478(5) 0.4063(10) 0.0821(5) 0.100(3) Uani 1 1 d . U
H13 H 0.4864 0.4428 0.0848 0.120 Uiso 1 1 calc R U
C14 C 0.4358(4) 0.3187(9) 0.0452(5) 0.084(3) Uani 1 1 d . .
C15 C 0.4824(7) 0.2864(17) 0.0082(8) 0.127(5) Uani 1 1 d . .
C16 C 0.2713(6) 0.5151(8) 0.0089(5) 0.108(4) Uani 1 1 d . .
H16 H 0.3077 0.4956 -0.0049 0.129 Uiso 1 1 calc R U
C17 C 0.2576(8) 0.6187(11) 0.0206(8) 0.153(7) Uani 1 1 d . .
H17 H 0.2870 0.6691 0.0149 0.184 Uiso 1 1 calc R U
C18 C 0.1627(9) 0.5734(13) 0.0468(7) 0.140(6) Uani 1 1 d . .
H18 H 0.1250 0.5925 0.0585 0.168 Uiso 1 1 calc R U
C19 C 0.1735(6) 0.4702(9) 0.0376(5) 0.101(4) Uani 1 1 d . .
H19 H 0.1446 0.4195 0.0440 0.122 Uiso 1 1 calc R U
F4 F 0.4601(4) -0.1218(6) 0.1762(3) 0.139(3) Uani 1 1 d . .
F6 F 0.4537(4) -0.0634(7) 0.0874(4) 0.152(3) Uani 1 1 d . .
F5 F 0.3715(4) -0.1367(6) 0.1078(4) 0.149(3) Uani 1 1 d . .
F3 F 0.4431(4) 0.1096(7) 0.3297(3) 0.158(3) Uani 1 1 d . U
F2 F 0.3621(5) 0.2080(10) 0.3162(4) 0.178(4) Uani 1 1 d . U
F1 F 0.4497(8) 0.2636(9) 0.3011(5) 0.204(6) Uani 1 1 d . U
F18 F 0.4568(6) 0.2711(10) -0.0474(6) 0.201(5) Uani 1 1 d . U
F15 F 0.4799(5) 0.5710(10) 0.1594(6) 0.216(6) Uani 1 1 d . .
F9 F 0.2090(6) -0.0821(9) 0.1439(7) 0.215(5) Uani 1 1 d . .
F16 F 0.5273(6) 0.3531(12) 0.0075(6) 0.242(6) Uani 1 1 d . U
F12 F 0.1958(7) 0.4433(11) 0.2141(7) 0.246(7) Uani 1 1 d . U
F14 F 0.3830(7) 0.6110(10) 0.1301(7) 0.263(7) Uani 1 1 d . U
F7 F 0.1445(8) -0.0277(11) 0.1898(7) 0.271(7) Uani 1 1 d . U
F13 F 0.4153(7) 0.5294(11) 0.2056(6) 0.244(6) Uani 1 1 d . U
F10 F 0.1116(6) 0.3902(13) 0.1682(7) 0.257(7) Uani 1 1 d . U
F11 F 0.1474(10) 0.3285(13) 0.2508(8) 0.328(11) Uani 1 1 d . U
F8 F 0.1209(6) -0.0235(10) 0.0977(9) 0.284(9) Uani 1 1 d . U
F17 F 0.5130(8) 0.2088(12) 0.0254(7) 0.244(7) Uani 1 1 d . 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'
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'
Tb Tb -0.1723 4.1537 '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 Tb1 O4 77.8(2) . .
O1 Tb1 O3 86.5(2) . .
O4 Tb1 O3 71.5(2) . .
O1 Tb1 O6 106.0(2) . .
O4 Tb1 O6 148.2(2) . .
O3 Tb1 O6 139.4(2) . .
O1 Tb1 O5 75.6(2) . .
O4 Tb1 O5 79.1(2) . .
O3 Tb1 O5 148.3(2) . .
O6 Tb1 O5 71.7(2) . .
O1 Tb1 O2 72.5(2) . .
O4 Tb1 O2 135.1(2) . .
O3 Tb1 O2 73.8(2) . .
O6 Tb1 O2 73.7(2) . .
O5 Tb1 O2 123.2(2) . .
O1 Tb1 O7 149.3(2) . 7
O4 Tb1 O7 117.2(2) . 7
O3 Tb1 O7 74.7(2) . 7
O6 Tb1 O7 75.9(2) . 7
O5 Tb1 O7 131.4(2) . 7
O2 Tb1 O7 79.0(2) . 7
O1 Tb1 O7 147.0(2) . .
O4 Tb1 O7 77.0(2) . .
O3 Tb1 O7 105.1(2) . .
O6 Tb1 O7 85.3(2) . .
O5 Tb1 O7 78.9(2) . .
O2 Tb1 O7 140.2(2) . .
O7 Tb1 O7 63.1(2) 7 .
C2 O1 Tb1 136.2(7) . .
C4 O2 Tb1 134.1(6) . .
C7 O3 Tb1 133.0(8) . .
C9 O4 Tb1 132.6(8) . .
C12 O5 Tb1 135.0(7) . .
C14 O6 Tb1 134.7(7) . .
N1 O7 Tb1 121.2(5) . 7
N1 O7 Tb1 121.9(5) . .
Tb1 O7 Tb1 116.9(2) 7 .
C19 N1 C16 125.3(10) . .
C19 N1 O7 118.3(9) . .
C16 N1 O7 116.4(9) . .
C17 N2 C18 117.0(13) . .
F2 C1 F1 111.0(13) . .
F2 C1 F3 105.5(14) . .
F1 C1 F3 106.3(12) . .
F2 C1 C2 113.4(11) . .
F1 C1 C2 111.1(13) . .
F3 C1 C2 109.1(10) . .
O1 C2 C3 126.9(9) . .
O1 C2 C1 110.8(9) . .
C3 C2 C1 122.3(9) . .
C4 C3 C2 121.6(9) . .
O2 C4 C3 128.1(9) . .
O2 C4 C5 114.7(9) . .
C3 C4 C5 117.1(8) . .
F4 C5 F5 108.3(12) . .
F4 C5 F6 105.4(11) . .
F5 C5 F6 105.4(11) . .
F4 C5 C4 116.2(10) . .
F5 C5 C4 110.2(10) . .
F6 C5 C4 110.7(11) . .
F8 C6 F9 108(2) . .
F8 C6 F7 104.8(14) . .
F9 C6 F7 105.4(17) . .
F8 C6 C7 111.1(15) . .
F9 C6 C7 114.7(12) . .
F7 C6 C7 112.5(19) . .
O3 C7 C8 126.4(12) . .
O3 C7 C6 111.3(13) . .
C8 C7 C6 122.2(12) . .
C7 C8 C9 123.5(12) . .
O4 C9 C8 127.2(12) . .
O4 C9 C10 112.8(13) . .
C8 C9 C10 120.1(12) . .
F11 C10 F12 118(3) . .
F11 C10 F10 102.4(17) . .
F12 C10 F10 97(2) . .
F11 C10 C9 115.3(19) . .
F12 C10 C9 116.3(13) . .
F10 C10 C9 103.5(19) . .
F14 C11 F13 105.2(18) . .
F14 C11 F15 110.1(16) . .
F13 C11 F15 102.2(16) . .
F14 C11 C12 113.2(14) . .
F13 C11 C12 111.6(14) . .
F15 C11 C12 113.7(14) . .
O5 C12 C13 126.5(11) . .
O5 C12 C11 114.2(11) . .
C13 C12 C11 119.3(11) . .
C12 C13 C14 122.7(9) . .
O6 C14 C13 126.5(9) . .
O6 C14 C15 112.7(12) . .
C13 C14 C15 120.8(11) . .
F17 C15 F18 105(2) . .
F17 C15 F16 103.1(14) . .
F18 C15 F16 103.5(15) . .
F17 C15 C14 115.5(14) . .
F18 C15 C14 114.6(12) . .
F16 C15 C14 113.9(17) . .
N1 C16 C17 114.2(13) . .
N2 C17 C16 124.1(16) . .
N2 C18 C19 122.3(16) . .
N1 C19 C18 117.0(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O1 2.301(7) .
Tb1 O4 2.335(6) .
Tb1 O3 2.340(6) .
Tb1 O6 2.355(7) .
Tb1 O5 2.357(6) .
Tb1 O2 2.376(6) .
Tb1 O7 2.431(6) 7
Tb1 O7 2.439(6) .
O1 C2 1.254(10) .
O2 C4 1.225(10) .
O3 C7 1.286(12) .
O4 C9 1.265(12) .
O5 C12 1.253(10) .
O6 C14 1.250(11) .
O7 N1 1.367(9) .
O7 Tb1 2.431(6) 7
N1 C19 1.326(13) .
N1 C16 1.352(14) .
N2 C17 1.33(2) .
N2 C18 1.37(2) .
C1 F2 1.263(15) .
C1 F1 1.268(18) .
C1 F3 1.363(15) .
C1 C2 1.551(14) .
C2 C3 1.392(13) .
C3 C4 1.363(13) .
C4 C5 1.511(14) .
C5 F4 1.292(13) .
C5 F5 1.316(15) .
C5 F6 1.351(14) .
C6 F8 1.25(2) .
C6 F9 1.271(18) .
C6 F7 1.275(19) .
C6 C7 1.517(19) .
C7 C8 1.328(18) .
C8 C9 1.337(18) .
C9 C10 1.57(2) .
C10 F11 1.20(2) .
C10 F12 1.24(2) .
C10 F10 1.35(3) .
C11 F14 1.219(19) .
C11 F13 1.260(18) .
C11 F15 1.284(18) .
C11 C12 1.520(17) .
C12 C13 1.363(15) .
C13 C14 1.390(15) .
C14 C15 1.492(16) .
C15 F17 1.20(2) .
C15 F18 1.247(19) .
C15 F16 1.283(19) .
C16 C17 1.408(18) .
C18 C19 1.377(17) .
