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_7714305
_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         'C30 H28 N15 O11 Tb, 5.5(H2O)'
_chemical_formula_sum            'C30 H39 N15 O16.5 Tb'
_chemical_formula_weight         1032.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-26
_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                90
_cell_angle_beta                 100.863(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5550(4)
_cell_length_b                   24.2497(5)
_cell_length_c                   20.6085(5)
_cell_measurement_reflns_used    20700
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.9320
_cell_measurement_theta_min      2.2160
_cell_volume                     9106.7(4)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.775
_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    -38.00  23.00   0.50   10.00    --   -7.10 -92.00 113.00  122
  2  \w    -21.00  39.00   0.50   10.00    --    4.91 -99.00  60.00  120
  3  \w    -20.00  26.00   0.50   10.00    --   -7.10 -99.00   0.00   92
  4  \w    -31.00  35.00   0.50   10.00    --   -7.10  92.00-133.00  132
;
_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      0.0160432000
_diffrn_orient_matrix_UB_12      0.0264858000
_diffrn_orient_matrix_UB_13      -0.0007271000
_diffrn_orient_matrix_UB_21      0.0041342000
_diffrn_orient_matrix_UB_22      -0.0045861000
_diffrn_orient_matrix_UB_23      -0.0330932000
_diffrn_orient_matrix_UB_31      -0.0352265000
_diffrn_orient_matrix_UB_32      0.0115075000
_diffrn_orient_matrix_UB_33      -0.0115663000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.775
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            72262
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.775
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.928
_diffrn_reflns_theta_min         2.158
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.925
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       plate
_exptl_crystal_F_000             4168
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.299
_refine_diff_density_min         -2.250
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1169
_refine_ls_number_reflns         22350
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0513P)^2^+43.1879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15374
_reflns_number_total             28828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02876c2.cif
_cod_data_source_block           Tb
_cod_depositor_comments
;

2024-09-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C60 H78 N30 O33 Tb2'
_cod_original_formula_weight         2065.38
_cod_original_formula_moiety         '2(C30 H28 N15 O11 Tb), 11(H2O)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7714305
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C N O Tb'
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H12A-H11B
 1.82 with sigma of 0.01
 H25B-H27A
 1.82 with sigma of 0.01
 H27A-H25B
 1.9 with sigma of 0.01
 H21A-H30A
 1.9 with sigma of 0.01
3.a Free rotating group:
 O15(H15A,H15B), O33(H33A,H33B), O29(H29D,H29E), O12(H12A,H12B), O27(H27A,
 H27B), O31(H31A,H31B), O30(H30A,H30B), O13(H13A,H13B), O32(H32A,H32B),
 O28(H28A,H28B), O14(H14A,H14B)
3.b Rotating group:
 O11(H11A,H11B), O10(H10A,H10B), O26(H26B,H26C), O25(H25A,H25B)
3.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C10(H10), C26(H26), C14(H14), C17(H17), C30(H30), N1(H1), C24(H24),
 N6(H6), N11(H11), C11(H11C), C1(H1A), C21(H21), C4(H4), C6(H6A), N18(H18),
 C44(H44), C46(H46), C50(H50), C31(H31), C40(H40), C60(H60), N26(H26A),
 C41(H41), N21(H21A), C51(H51), C56(H56), C36(H36), C34(H34), C54(H54)
3.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C59(H59A,H59B,
 H59C), C39(H39A,H39B,H39C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              28659
_shelx_fab_checksum              98150
_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 94.880
_oxdiff_exptl_absorpt_empirical_full_min 0.325