Lanthanide complexes based on the linear bifunctional ligand: Synthesis, structure regulation and magnetic properties
Lan, Hai-Ming; Yang, Ru-Xia; Yang, Li-Zhen; Zhu, Peng-Yin; Wang, Lu-Lu; Yu, Yu-Ming; Wang, Duo-Zhi; Inorganica Chimica Acta 508 (2020) 119593–; doi:10.1016/j.ica.2020.119593

data_1564576
_publ_section_title
;
 Lanthanide complexes based on the linear bifunctional ligand: Synthesis,
 structure regulation and magnetic properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119593
_journal_paper_doi               10.1016/j.ica.2020.119593
_journal_volume                  508
_journal_year                    2020
_chemical_formula_moiety         '1(C153 H102 Dy7 N33 O32)'
_chemical_formula_sum            'C153 H102 Dy7 N33 O32'
_chemical_formula_weight         4052.09
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   21.8806(5)
_cell_length_b                   21.8806(5)
_cell_length_c                   20.7765(11)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.399
_cell_measurement_theta_min      2.844
_cell_volume                     8614.3(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            105511
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.015
_diffrn_reflns_theta_min         2.104
_exptl_absorpt_coefficient_mu    3.072
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0993 before and 0.0684 after correction.
The Ratio of minimum to maximum transmission is 0.3732.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       block
_exptl_crystal_F_000             3938
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.900
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5811
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+65.9020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4475
_reflns_number_total             5811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            8.cif
_cod_data_source_block           222_sq
_cod_original_cell_volume        8614.3(6)
_cod_database_code               1564576
_shelx_estimated_absorpt_t_max   0.656
_shelx_estimated_absorpt_t_min   0.551
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N3-N4
 2.186 with sigma of 0.02
 C15-C17
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C15, N4, C16, C17, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: N4(0.25) N2(0.25) C7(0.5) C6(0.5)
6.a Rotating group:
 O9(H9A,H9B)
6.b Aromatic/amide H refined with riding coordinates:
 N6(H6), C21(H21), C28(H28), C15(H15), C24(H24), C27(H27), C20(H20), C32(H32),
 C16(H16), C13(H13), C14(H14), C30(H30), C31(H31), C10(H10), C11(H11), C17(H17),
  C3(H3), C33(H33), C34(H34)
;