Successive syntheses and magnetic properties of homodinuclear lanthanide macrocyclic complexes
Li, Xiang; Liu, Yu-Han; Zhu, Guang-Zhou; Yang, Feng-Lei; Gao, Feng; Dalton Transactions  (2021) –; doi:10.1039/D1DT01514A

data_7708053
_publ_section_title
;
 Successive syntheses and magnetic properties of homodinuclear lanthanide
 macrocyclic complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01514A
_journal_year                    2021
_chemical_formula_moiety         'C56 H62 N4 O10 Tb2, 7[C2H4Cl2]'
_chemical_formula_sum            'C70 H90 Cl14 N4 O10 Tb2'
_chemical_formula_weight         1961.59
_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   mixed
_audit_creation_date             2021-07-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-28 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.0930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5727(13)
_cell_length_b                   13.8912(16)
_cell_length_c                   22.363(3)
_cell_measurement_reflns_used    4808
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.43
_cell_measurement_theta_min      2.31
_cell_volume                     3539.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19798
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.115
_diffrn_reflns_theta_min         2.759
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  0.8491
_exptl_absorpt_correction_T_min  0.7831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7762
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0396
_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/[\s^2^(Fo^2^)+(0.0575P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5693
_reflns_number_total             7762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01514a2.cif
_cod_data_source_block           gf20190429b_0m_sq
_cod_database_code               7708053
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.748
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1A-C2A \\sim C2A-C3A \\sim C3A-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim N1 \\sim O1 \\sim Tb1 \\sim C2 \\sim N2 \\sim O2 \\sim C3 \\sim O3
\\sim C4: within 3.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.5A
C3 \\sim C1A \\sim C1 \\sim C2A \\sim C2 \\sim C3A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
5.a Riding coordinates:
 C2A(H2AA,H2AB,H2AC), C1A(H1AA,H1AB,H1AC)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C21(H21), C26(H26)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C19(H19A,H19B,H19C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C3A(H3AA,H3AB,
 H3AC)
;
_shelx_res_checksum              45978
_shelx_hkl_checksum              11046
_shelx_fab_checksum              82574
_olex2_submission_special_instructions 'No special instructions were received'