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_1564577
_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 H105 Er7 N36 O32)'
_chemical_formula_sum            'C153.01 H105 Er7 N36 O32'
_chemical_formula_weight         4130.71
_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                   21.7953(5)
_cell_length_b                   21.7953(5)
_cell_length_c                   20.9712(13)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.357
_cell_measurement_theta_min      2.366
_cell_volume                     8627.4(6)
_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      293(2)
_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  0.1031
_diffrn_reflns_av_unetI/netI     0.0307
_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       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            109495
_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         26.397
_diffrn_reflns_theta_min         2.106
_exptl_absorpt_coefficient_mu    3.442
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1199 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.3188.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             4014
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         3.023
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.201
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6066
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0865P)^2^+83.0658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4434
_reflns_number_total             6066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            9.cif
_cod_data_source_block           222_sq
_cod_original_cell_volume        8627.4(7)
_cod_database_code               1564577
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.396
_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
 C17-C16
 2.1 with sigma of 0.02
3. Rigid bond restraints
 N4, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C15, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O1, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C9 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C11 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N3 \\sim C15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C17 \\sim N4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N1 \\sim C8: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C5 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C1 \\sim O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C27) \\sim
Ueq, Uanis(C28) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C25) \\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(C15) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N8) \\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
Uanis(C34B) \\sim Ueq, Uanis(C33B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C33B) = Uanis(C34B) = Uanis(C33A) = Uanis(C34A)
5. Others
 Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=1-FVAR(1)
 Sof(C34B)=Sof(H34B)=Sof(C33B)=Sof(H33B)=FVAR(1)
 Fixed Sof: C7(0.5) C6(0.5)
6.a Rotating group:
 O6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C30(H30), C23(H23), C31(H31), C3(H3), C14(H14), C20(H20), C32(H32),
 C24(H24), C28(H28), C27(H27), C13(H13), C16(H16), C15(H15), N1(H1), C10(H10),
 C11(H11), C17(H17), C34B(H34B), C33B(H33B), C33A(H33A), C34A(H34A)
;