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_1564575
_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         'C153 H119 Ho7 N36 O32, 4(H1 O1), 4.5(H2 O)'
_chemical_formula_sum            'C153 H132 Ho7 N36 O40.5'
_chemical_formula_weight         4277.45
_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                   21.8289(4)
_cell_length_b                   21.8289(4)
_cell_length_c                   20.8477(5)
_cell_measurement_reflns_used    23185
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.4130
_cell_measurement_theta_min      2.1500
_cell_volume                     8603.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9584
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -40.00  62.00   1.00    3.50    --  -11.59  57.00 -90.00  102
  2  \w    -17.00  76.00   1.00    3.50    --   11.74  77.00  30.00   93
  3  \w     36.00  63.00   1.00    3.50    --   11.74 178.00 120.00   27
  4  \w    -78.00  12.00   1.00    3.50    --  -11.59 -57.00 120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0358326000
_diffrn_orient_matrix_UB_12      0.0275535000
_diffrn_orient_matrix_UB_13      0.0004028000
_diffrn_orient_matrix_UB_21      -0.0001834000
_diffrn_orient_matrix_UB_22      -0.0008858000
_diffrn_orient_matrix_UB_23      0.0340130000
_diffrn_orient_matrix_UB_31      0.0111363000
_diffrn_orient_matrix_UB_32      -0.0254498000
_diffrn_orient_matrix_UB_33      -0.0007457000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73871
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.596
_diffrn_reflns_theta_min         2.106
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.263
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       block
_exptl_crystal_F_000             4190
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.931
_refine_diff_density_min         -2.241
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         7925
_refine_ls_number_restraints     1815
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0499P)^2^+62.7599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6391
_reflns_number_total             7925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            7.cif
_cod_data_source_block           lhm-1
_cod_original_cell_volume        8603.0(4)
_cod_original_formula_sum        'C153 H132 Ho7 N36 O40.50'
_cod_database_code               1564575
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.695
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H5 of O5, H0AA of O0AA, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups, H7A of O7
2. Restrained distances
 N4-C17 = N3-C15 = N3-C16
 1.47 with sigma of 0.01
 N4-C15 = C17-C16
 1.36 with sigma of 0.01
 C30-C29 \\sim C30A-C29 \\sim C30-C31 \\sim C31A-C30A \\sim C31-C26 \\sim
C31A-C26A \\sim C26A-C27 ~
 C26-C27
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C25A \\sim C26 \\sim C26A \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim
C30A \\sim C31 \\sim C31A \\sim C32 \\sim C33 \\sim C33A \\sim C34 \\sim C34A
\\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N6A \\sim N7 \\sim
N8 \\sim O1 \\sim O3 \\sim O4 \\sim O0AA \\sim O5 \\sim O6 \\sim O7 \\sim O8
\\sim O9 \\sim O2: within 3.8A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C30A) = Uanis(C30)
Uanis(C31A) = Uanis(C31)
4. Others
 Sof(N6A)=Sof(H6AA)=Sof(C25A)=Sof(C26A)=Sof(H27A)=Sof(C30A)=Sof(H30A)=
 Sof(C31A)=Sof(H31A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=1-FVAR(1)
 Sof(N6)=Sof(H6)=Sof(C25)=Sof(C26)=Sof(H27)=Sof(C30)=Sof(H30)=Sof(C31)=
 Sof(H31)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=FVAR(1)
 Fixed Sof: O1(0.5) N1(0.5) H1(0.5) C5(0.5) C6(0.5) H6C(0.5) C7(0.5) H7(0.5)
 O7(0.6666) H7A(0.6666) O8(0.5) H8A(0.5) H8B(0.5) O9(0.25) H9A(0.25) H9B(0.25)
 O2(0.5)
5.a Riding coordinates:
 O7(H7A), O8(H8A,H8B), O9(H9A,H9B)
5.b Rotating group:
 O6(H6A,H6B)
5.c Ternary CH refined with riding coordinates:
 O0AA(H0AA), O5(H5)
5.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N6(H6), N6A(H6AA), C3(H3), C6(H6C), C7(H7), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C23(H23), C24(H24),
  C27(H27), C27(H27A), C28(H28), C30(H30), C30A(H30A), C31(H31), C31A(H31A),
 C32(H32), C33(H33), C33A(H33A), C34(H34), C34A(H34A)
;
_shelx_fab_checksum              96450
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.159
_oxdiff_exptl_absorpt_empirical_full_min 0.863