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_7708051
_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 Dy2 N4 O10, 6[C2H4Cl2]'
_chemical_formula_sum            'C68 H86 Cl12 Dy2 N4 O10'
_chemical_formula_weight         1869.80
_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   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                90
_cell_angle_beta                 100.092(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.562(2)
_cell_length_b                   13.893(3)
_cell_length_c                   22.308(4)
_cell_measurement_reflns_used    5176
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      2.34
_cell_volume                     3527.9(12)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19386
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.313
_exptl_absorpt_coefficient_mu    2.618
_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    1.760
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         7206
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0683P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5563
_reflns_number_total             7206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01514a2.cif
_cod_data_source_block           gf20190429a_0m_sq
_cod_original_cell_volume        3527.7(12)
_cod_database_code               7708051
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.744
_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. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim C27 \\sim C28: within 3.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C9(H9), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C19(H19), C22(H22)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              41424
_shelx_hkl_checksum              11735
_shelx_fab_checksum              48386
_olex2_submission_special_instructions 'No special instructions were received'