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_7708054
_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         'C76 H58 Cl4 N8 O6 Tb2, 3[C2H4Cl2]'
_chemical_formula_sum            'C82 H70 Cl10 N8 O6 Tb2'
_chemical_formula_weight         1935.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-28 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                68.8760(10)
_cell_angle_beta                 87.5280(10)
_cell_angle_gamma                85.8270(10)
_cell_formula_units_Z            1
_cell_length_a                   11.7936(9)
_cell_length_b                   11.8409(9)
_cell_length_c                   14.1346(10)
_cell_measurement_reflns_used    6727
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.34
_cell_volume                     1836.0(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.979
_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  0.0159
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10456
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.978
_exptl_absorpt_coefficient_mu    2.338
_exptl_absorpt_correction_T_max  0.8255
_exptl_absorpt_correction_T_min  0.7716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       block
_exptl_crystal_F_000             966
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.102
_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     436
_refine_ls_number_reflns         7361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+1.4021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6662
_reflns_number_total             7361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01514a2.cif
_cod_data_source_block           gf20191128b_0m_sq
_cod_database_code               7708054
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.767
_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.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C18(H18),
 C20(H20), C21(H21), C23(H23), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
  C32(H32), C34(H34), C36(H36), C37(H37)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              83101
_shelx_hkl_checksum              67652
_shelx_fab_checksum              63779
_olex2_submission_special_instructions 'No special instructions were received'