Magnetic investigation in di- and tetranuclear lanthanide complexes
Wu, Jianfeng; Liu, Dan; Yang, Qianqian; Ge, Yan; Tang, Jinkui; Qi, Zhenhui; New Journal of Chemistry 45 (2021) 2200–2207; doi:10.1039/D0NJ04247A

data_7060172
_publ_section_title
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 Magnetic investigation in di- and tetranuclear lanthanide complexes
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_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2200
_journal_page_last               2207
_journal_paper_doi               10.1039/D0NJ04247A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C56 H55.958 Dy4 N15.979 O9, 3(Cl O4)'
_chemical_formula_sum            'C56 H57 Cl3 Dy4 N16 O21'
_chemical_formula_weight         2046.52
_space_group_crystal_system      tetragonal
_space_group_IT_number           124
_space_group_name_Hall           '-P 4 2c'
_space_group_name_H-M_alt        'P 4/m c c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-11 deposited with the CCDC.	2020-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6051(5)
_cell_length_b                   11.6051(5)
_cell_length_c                   25.651(3)
_cell_measurement_reflns_used    3239
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      62.41
_cell_measurement_theta_min      4.18
_cell_volume                     3454.6(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.874
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8562
_diffrn_reflns_point_group_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.658
_diffrn_reflns_theta_min         5.390
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    24.532
_exptl_absorpt_correction_T_max  0.018
_exptl_absorpt_correction_T_min  0.012
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.394
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       0.00024(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1409
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1587
_refine_ls_R_factor_gt           0.1185
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+194.5445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2509
_refine_ls_wR_factor_ref         0.2773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                969
_reflns_number_total             1409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04247a2.cif
_cod_data_source_block           Dy4
_cod_depositor_comments
'Adding full bibliography for 7060172--7060173.cif.'
_cod_database_code               7060172
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.096
_shelx_estimated_absorpt_t_min   0.084
_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
2. Restrained distances
 Cl1-O4
 1.48 with sigma of 0.02
 O5-Cl2
 1.48 with sigma of 0.02
 O6-Cl2
 1.48 with sigma of 0.02
 C2-C1
 1.45 with sigma of 0.02
 O3-Cl1
 1.48 with sigma of 0.02
 C6-C8
 1.45 with sigma of 0.02
 C8-N3
 1.42 with sigma of 0.02
 C7-N2
 1.45 with sigma of 0.02
 N2-N3
 1.42 with sigma of 0.02
 O6-O5
 2.35 with sigma of 0.04
 O3-O4
 2.35 with sigma of 0.04
 C7-C6
 2.5 with sigma of 0.04
 C7-N3
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(Cl1) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C8)=Sof(H8)=1-FVAR(1)
 Sof(N2)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
 Fixed Sof: O3(0.75) O6(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8)
6.c Fitted hexagon refined as free rotating group:
 N1(C2,C3,C4,C5,C6)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              76766
_shelx_fab_checksum              93293
_olex2_submission_special_instructions 'No special instructions were received'