Heterobimetallic 3d-4f complexes supported by a Schiff-base tripodal ligand.
Neumann, Till; Thompson, Benedict C.; Hebron, Denny; Graycon, Daniel M.; Collauto, Alberto; Roessler, Maxie M.; Wilson, Daniel W. N.; Musgrave, Rebecca A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9921–9932; doi:10.1039/d3dt03760f

data_7715895
_publ_section_title
;
 Heterobimetallic 3d-4f complexes supported by a Schiff-base tripodal
 ligand.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9921
_journal_page_last               9932
_journal_paper_doi               10.1039/d3dt03760f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C30 H30 F3 La N3 Na O9 S, C2 H3 N'
_chemical_formula_sum            'C32 H33 F3 La N4 Na O9 S'
_chemical_formula_weight         868.597
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-11-10 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.815(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0670(1)
_cell_length_b                   13.0765(1)
_cell_length_c                   16.7696(1)
_cell_measurement_reflns_used    39389
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3290
_cell_measurement_theta_min      4.3450
_cell_volume                     3448.65(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9914
_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    -75.00  33.00   1.00    1.50    --  -42.37  75.00  36.00  108
  2  \w     97.00 136.00   1.00    6.00    --  103.86 -75.00 -90.00   39
  3  \w     29.00  73.00   1.00    6.00    --  103.86 -75.00 -90.00   44
  4  \w    115.00 140.00   1.00    6.00    --  103.86  75.00  36.00   25
  5  \w     -4.00  22.00   1.00    1.50    --   34.00  92.00 163.67   26
  6  \w     -3.00  22.00   1.00    1.50    --   34.00  90.00  28.46   25
  7  \w     -3.00  23.00   1.00    1.50    --   34.00  90.00 -34.54   26
  8  \w   -121.00 -10.00   1.00    1.50    --  -42.37 -19.00  30.00  111
  9  \w    -67.00  24.00   1.00    1.50    --  -42.37  38.00-150.00   91
 10  \w    -89.00 -18.00   1.00    1.50    --  -42.37 -38.00-150.00   71
 11  \w     -3.00  50.00   1.00    1.50    --   42.37 -75.00 -90.00   53
 12  \w     55.00  82.00   1.00    1.50    --   42.37  38.00 -90.00   27
 13  \w     35.00  85.00   1.00    1.50    --   42.37-125.00-180.00   50
 14  \w     19.00  47.00   1.00    1.50    --   42.37  38.00 -90.00   28
 15  \w     16.00  41.00   1.00    1.50    --   50.00  81.00  82.68   25
 16  \w     16.00  42.00   1.00    1.50    --   50.00  82.00   5.80   26
 17  \w     16.00  41.00   1.00    1.50    --   50.00  82.00 138.38   25
 18  \w     16.00  41.00   1.00    1.50    --   50.00  81.00-143.17   25
 19  \w     16.00  41.00   1.00    1.50    --   50.00  81.00 -83.09   25
 20  \w     31.00  57.00   1.00    1.50    --   62.00  71.00 176.92   26
 21  \w     35.00  68.00   1.00    1.50    --   66.00  71.00 -41.92   33
 22  \w     39.00  65.00   1.00    1.50    --   70.00  70.00-154.80   26
 23  \w     39.00  65.00   1.00    1.50    --   70.00  70.00  35.74   26
 24  \w     39.00  65.00   1.00    1.50    --   70.00  69.00 -67.53   26
 25  \w     39.00  65.00   1.00    1.50    --   70.00  71.00  95.98   26
 26  \w     39.00  65.00   1.00    1.50    --   70.00  71.00  -6.20   26
 27  \w     39.00  65.00   1.00    1.50    --   70.00  71.00-107.57   26
 28  \w     40.00  65.00   1.00    1.50    --   70.00  71.00 142.52   25
 29  \w     44.00  70.00   1.00    6.00    --   74.00  65.00  72.08   26
 30  \w     51.00  77.00   1.00    6.00    --   82.00  69.00 -36.23   26
 31  \w     51.00  99.00   1.00    6.00    --   82.00  71.00 154.05   48
 32  \w     54.00  81.00   1.00    6.00    --   82.00  62.00  94.82   27
 33  \w     51.00  77.00   1.00    6.00    --   82.00  69.00 -70.41   26
 34  \w     55.00  81.00   1.00    6.00    --   86.00  71.00 104.25   26
 35  \w     55.00  81.00   1.00    6.00    --   86.00  69.00 -15.47   26
 36  \w     56.00  83.00   1.00    6.00    --   86.00  67.00-146.62   27
 37  \w     62.00  89.00   1.00    6.00    --   90.00  62.00-169.83   27
 38  \w     59.00  85.00   1.00    6.00    --   90.00  71.00-116.52   26
 39  \w     64.00  90.00   1.00    6.00    --   94.00  67.00   2.23   26
 40  \w    104.00 130.00   1.00    6.00    --   94.00  67.00   2.23   26
 41  \w     74.00 102.00   1.00    6.00    --  103.86  67.00 -77.58   28
 42  \w    150.00 177.00   1.00    6.00    --  103.86  66.00 128.42   27
 43  \w    113.00 177.00   1.00    6.00    --  103.86  66.00 -60.44   64
 44  \w     75.00 109.00   1.00    6.00    --  103.86  66.00 128.42   34
 45  \w     74.00 105.00   1.00    6.00    --  103.86  66.00 -60.44   31
 46  \w     73.00 170.00   1.00    6.00    --  103.86  71.00-165.43   97
 47  \w     29.00 135.00   1.00    6.00    --  103.86 -77.00  90.00  106
 48  \w     75.00 177.00   1.00    6.00    --  103.86  60.00  80.37  102
 49  \w     75.00 173.00   1.00    6.00    --  103.86  61.00 150.00   98
 50  \w     74.00 136.00   1.00    6.00    --  103.86  63.00  23.49   62
 51  \w    114.00 176.00   1.00    6.00    --  103.86  61.00 120.00   62
 52  \w     31.00 113.00   1.00    6.00    --  103.86-125.00 -90.00   82
 53  \w     75.00 102.00   1.00    6.00    --  103.86  61.00 120.00   27
 54  \w     76.00 172.00   1.00    6.00    --  103.86  61.00-120.00   96
 55  \w     47.00 107.00   1.00    6.00    --  103.86-106.00 -23.52   60
 56  \w    114.00 176.00   1.00    6.00    --  103.86  61.00 -90.00   62
 57  \w     46.00 112.00   1.00    6.00    --  103.86-125.00  90.00   66
 58  \w     78.00 174.00   1.00    6.00    --  103.86  61.00 -30.00   96
 59  \w     78.00 104.00   1.00    6.00    --  103.86  61.00 -90.00   26
 60  \w     74.00 162.00   1.00    6.00    --  103.86  70.00  39.19   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0246463000
_diffrn_orient_matrix_UB_12      0.0787698000
_diffrn_orient_matrix_UB_13      0.0691546000
_diffrn_orient_matrix_UB_21      0.0773604000
_diffrn_orient_matrix_UB_22      0.0325502000
_diffrn_orient_matrix_UB_23      -0.0351379000
_diffrn_orient_matrix_UB_31      -0.0548016000
_diffrn_orient_matrix_UB_32      0.0813545000
_diffrn_orient_matrix_UB_33      -0.0528177000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9914
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59489
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9914
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         72.58
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.929
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       block
_exptl_crystal_F_000             1749.496
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.3340
_refine_diff_density_min         -0.9522
_refine_diff_density_rms         0.0768
_refine_ls_d_res_high            0.8080
_refine_ls_d_res_low             12.7325
_refine_ls_goodness_of_fit_ref   1.0522
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     465
_refine_ls_number_reflns         6788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0522
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.3768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0508
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -19
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -12
_reflns_number_gt                6650
_reflns_number_total             6788
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt03760f2.cif
_cod_data_source_block           exp_3229
_cod_depositor_comments
'Adding full bibliography for 7715892--7715896.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7715895
_chemical_oxdiff_formula         'C31 H33 F3 La N5 Na O9 S'
_chemical_oxdiff_usercomment     'TN022 MeCN Et2O'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16), C17(H17), C18(H18),
 C22(H22), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C13(H13a,H13b,H13c), C21(H21a,H21b,H21c), C29(H29a,H29b,
 H29c), C32(H32a,H32b,H32c)
;
_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 2.343
_oxdiff_exptl_absorpt_empirical_full_min 0.550