LnIII/MnII-LnIII complexes derived from salicylic azo dye ligand: synthesis, structures, magnetic and fluorescent properties
Kuang, Xiao-Man; Li, You-Hong; Yang, Meng; Dong, Wen; Leng, Ji-Dong; Dalton Transactions  (2023) –; doi:10.1039/D3DT02876C

data_7714304
_publ_section_title
;
 LnIII/MnII-LnIII complexes derived from salicylic azo dye ligand:
 synthesis, structures, magnetic and fluorescent properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02876C
_journal_year                    2023
_chemical_formula_moiety         'C54 H50 Tb2 Mn N36 O24, H12 Mn O6, 4(H2O)'
_chemical_formula_sum            'C54 H70 Mn2 N36 O34 Tb2'
_chemical_formula_weight         2195.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-09 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                112.375(2)
_cell_angle_beta                 94.0318(19)
_cell_angle_gamma                108.238(2)
_cell_formula_units_Z            1
_cell_length_a                   11.6539(3)
_cell_length_b                   13.7912(3)
_cell_length_c                   15.5805(4)
_cell_measurement_reflns_used    17671
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9680
_cell_measurement_theta_min      2.1780
_cell_volume                     2147.49(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.793
_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    -10.00  78.00   0.50    3.42    --    4.91  53.00-174.00  176
  2  \w    -67.00  20.00   0.50    3.42    --    4.91 -53.00  41.00  174
  3  \w     14.00  39.00   0.50    3.42    --    4.91 -99.00   0.00   50
  4  \w    -20.00  39.00   0.50    3.42    --    4.91 -99.00 120.00  118
  5  \w    -23.00   9.00   0.50    3.42    --   -6.94 -57.00 -60.00   64
  6  \w    -52.00 -26.00   0.50    3.42    --   -6.94 -57.00 -60.00   52
  7  \w    -81.00   4.00   0.50    3.42    --   -6.94 -37.00-120.00  170
  8  \w     -6.00  23.00   0.50    3.42    --   -6.94 -99.00  30.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0295813000
_diffrn_orient_matrix_UB_12      -0.0439347000
_diffrn_orient_matrix_UB_13      0.0132515000
_diffrn_orient_matrix_UB_21      0.0286386000
_diffrn_orient_matrix_UB_22      -0.0341329000
_diffrn_orient_matrix_UB_23      -0.0298854000
_diffrn_orient_matrix_UB_31      0.0511063000
_diffrn_orient_matrix_UB_32      0.0219916000
_diffrn_orient_matrix_UB_33      0.0383831000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32022
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.933
_diffrn_reflns_theta_min         2.297
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.017
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       block
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.586
_refine_diff_density_min         -2.677
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         10787
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0605P)^2^+2.5755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9028
_reflns_number_total             13599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02876c2.cif
_cod_data_source_block           Mn-Tb
_cod_original_cell_volume        2147.48(10)
_cod_original_formula_sum        'C54 H70 Tb2 Mn2 N36 O34'
_cod_database_code               7714304
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C17-O6
 1.42 with sigma of 0.01
 N13-H13
 0.96 with sigma of 0.01
 O15-H15B
 0.8 with sigma of 0.01
 O17-H17B
 0.8 with sigma of 0.01
3.a Free rotating group:
 O15(H15A), O16(H16A,H16B)
3.b Rotating group:
 O11(H11A,H11B), O17(H17A), O10(H10B,H10A), O13(H13B,H13A), O12(H12A,H12B),
 O14(H14A,H14B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C3(H3), C5(H5), C12(H12), C18(H18), C27(H27), C21(H21), C14(H14),
 C23(H23)
3.d Idealised Me refined as rotating group:
 C17(H17C,H17D,H17E), C8(H8A,H8B,H8C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              32970
_shelx_fab_checksum              30074
_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 2.503
_oxdiff_exptl_absorpt_empirical_full_min 0.259