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_1564574
_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 Gd7 N36 O32), 6(H2 O), 2(Cl)'
_chemical_formula_sum            'C153 H117 Cl2 Gd7 N36 O38'
_chemical_formula_weight         4239.38
_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                   21.9624(4)
_cell_length_b                   21.9624(4)
_cell_length_c                   20.8625(11)
_cell_measurement_reflns_used    9362
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.348
_cell_measurement_theta_min      2.353
_cell_volume                     8714.8(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      150.05
_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  0.0712
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -27
_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            110964
_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         26.388
_diffrn_reflns_theta_min         2.227
_exptl_absorpt_coefficient_mu    2.736
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0986 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission is 0.3623.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             4146
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.071
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6117
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0425P)^2^+44.7831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4793
_reflns_number_total             6117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6.cif
_cod_data_source_block           222_sq
_cod_original_cell_volume        8714.8(6)
_cod_database_code               1564574
_shelx_estimated_absorpt_t_max   0.753
_shelx_estimated_absorpt_t_min   0.515
_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
 C16-C17
 2.1 with sigma of 0.02
 C17-C15
 2.1 with sigma of 0.02
 H7B-H6A
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6 \\sim C5 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
N3 \\sim C17 \\sim N4: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O1 \\sim C1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C34B) = Uanis(C34A) = Uanis(C33A) = Uanis(C33B)
4. Others
 Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=1-FVAR(1)
 Sof(C33B)=Sof(H33B)=Sof(C34B)=Sof(H34B)=FVAR(1)
 Fixed Sof: C3(0.5) C4(0.5)
5.a Free rotating group:
 O7(H7A,H7B)
5.b Rotating group:
 O6(H6A,H6B)
5.c Aromatic/amide H refined with riding coordinates:
 N6(H6), C28(H28), C21(H21), C27(H27), C15(H15), N1(H1), C20(H20), C24(H24),
 C7(H7), C32(H32), C16(H16), C13(H13), C14(H14), C30(H30), C31(H31), C11(H11),
 C10(H10), C17(H17), C33B(H33B), C34B(H34B), C33A(H33A), C34A(H34A)
;