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_7714303
_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 Dy2 Mn N36 O24, H12 Mn O6, 4(H2O)'
_chemical_formula_sum            'C54 H70 Dy2 Mn2 N36 O34'
_chemical_formula_weight         2202.34
_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_block_doi                 10.5517/ccdc.csd.cc26m253
_audit_creation_date             2019-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-13 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                112.2770(10)
_cell_angle_beta                 94.1640(10)
_cell_angle_gamma                108.0530(10)
_cell_formula_units_Z            1
_cell_length_a                   11.6378(2)
_cell_length_b                   13.8140(2)
_cell_length_c                   15.5581(2)
_cell_measurement_reflns_used    14764
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.5170
_cell_measurement_theta_min      3.1470
_cell_volume                     2148.59(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.949
_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    -39.00 -13.00   0.50    0.15    --  -45.62  38.00  70.00   52
  2  \w    -69.00 -44.00   0.50    0.59    -- -102.00  61.00 120.00   50
  3  \w    -68.00 -43.00   0.50    0.59    -- -102.00  61.00  60.00   50
  4  \w   -100.00 -74.00   0.50    0.59    -- -102.00 125.00   0.00   52
  5  \w    -58.00 -32.00   0.50    0.59    -- -102.00 125.00   0.00   52
  6  \w    -80.00 -54.00   0.50    0.59    -- -102.00  77.00 -60.00   52
  7  \w    -96.00 -70.00   0.50    0.59    -- -102.00  77.00 -30.00   52
  8  \w    -24.00  30.00   0.50    0.15    --  -45.62  19.00 -90.00  108
  9  \w    -12.00  30.00   0.50    0.15    --  -45.62  19.00-150.00   84
 10  \w    -27.00  27.00   0.50    0.15    --   45.62 -38.00 -84.00  108
 11  \w     80.00 108.00   0.50    0.59    --  106.06 -94.00-180.00   56
 12  \w     64.00 117.00   0.50    0.59    --  106.06-125.00-180.00  106
 13  \w     54.00 114.00   0.50    0.59    --  106.06-125.00-150.00  120
 14  \w     37.00  67.00   0.50    0.59    --  106.06 -61.00   0.00   60
 15  \w     40.00  90.00   0.50    0.59    --  106.06 -94.00  60.00  100
 16  \w     59.00 117.00   0.50    0.59    --  106.06-125.00   0.00  116
 17  \w     49.00 102.00   0.50    0.59    --  106.06 -94.00   0.00  106
 18  \w     34.00  72.00   0.50    0.59    --  106.06 -61.00 120.00   76
 19  \w     34.00  71.00   0.50    0.59    --  106.06 -61.00  60.00   74
 20  \w     33.00  72.00   0.50    0.59    --  106.06 -61.00  90.00   78
 21  \w     43.00  92.00   0.50    0.15    --   45.62-125.00 150.00   98
 22  \w     33.00  67.00   0.50    0.59    --  106.06 -61.00 -60.00   68
 23  \w     40.00  73.00   0.50    0.59    --  106.06 -61.00-150.00   66
 24  \w     94.00 175.00   0.50    0.59    --  106.06  45.00   0.00  162
 25  \w    100.00 175.00   0.50    0.59    --  106.06  38.00  70.00  150
 26  \w     80.00 178.00   0.50    0.59    --  106.06 125.00  60.00  196
 27  \w     33.00  98.00   0.50    0.15    --   45.62  38.00  70.00  130
 28  \w    -18.00  69.00   0.50    0.15    --   45.62 -77.00  60.00  174
 29  \w    -90.00 -47.00   0.50    0.59    -- -102.00  77.00-120.00   86
 30  \w   -113.00 -37.00   0.50    0.59    -- -102.00 125.00-150.00  152
 31  \w   -118.00 -32.00   0.50    0.15    --  -45.62 -38.00 -84.00  172
 32  \w   -117.00 -80.00   0.50    0.59    -- -102.00 125.00  90.00   74
 33  \w   -174.00 -87.00   0.50    0.59    -- -102.00 -38.00 -84.00  174
 34  \w   -123.00 -80.00   0.50    0.59    -- -102.00 -77.00   0.00   86
 35  \w   -110.00 -85.00   0.50    0.15    --  -45.62-125.00   0.00   50
 36  \w   -163.00-136.00   0.50    0.59    -- -102.00 -77.00   0.00   54
 37  \w   -172.00-146.00   0.50    0.59    -- -102.00 -30.00-150.00   52
 38  \w   -126.00 -98.00   0.50    0.59    -- -102.00 -30.00-150.00   56
 39  \w   -166.00 -87.00   0.50    0.59    -- -102.00 -45.00-180.00  158
;
_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      -0.0228634000
_diffrn_orient_matrix_UB_12      0.0692791000
_diffrn_orient_matrix_UB_13      -0.0525156000
_diffrn_orient_matrix_UB_21      -0.1369669000
_diffrn_orient_matrix_UB_22      -0.0364296000
_diffrn_orient_matrix_UB_23      0.0068312000
_diffrn_orient_matrix_UB_31      0.0324266000
_diffrn_orient_matrix_UB_32      0.1031425000
_diffrn_orient_matrix_UB_33      0.0959506000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26284
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.045
_diffrn_reflns_theta_min         3.144
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.383
_exptl_absorpt_correction_T_max  0.141
_exptl_absorpt_correction_T_min  0.095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Tangerine
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.060
_refine_diff_density_min         -1.830
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8628
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0506
_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^)+(0.1000P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7901
_reflns_number_total             9088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02876c2.cif
_cod_data_source_block           Mn-Dy
_cod_database_code               7714303
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Co'
_shelx_estimated_absorpt_t_max   1.00
_shelx_estimated_absorpt_t_min   0.52
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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,H) groups
2. Restrained distances
 H13-N13
 0.9 with sigma of 0.01
3.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B)
3.b Rotating group:
 O11(H11A,H11B), O17(H17A,H17B), 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              67893
_shelx_fab_checksum              67067
_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 1.814
_oxdiff_exptl_absorpt_empirical_full_min 0.631