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_7715896
_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         'C33 H33 Co F6 La N4 O12 S2'
_chemical_formula_sum            'C33 H33 Co F6 La N4 O12 S2'
_chemical_formula_weight         1053.611
_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             2023-08-22
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-11-10 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.320(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4835(1)
_cell_length_b                   12.9504(1)
_cell_length_c                   22.0541(2)
_cell_measurement_reflns_used    43763
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      72.3060
_cell_measurement_theta_min      3.9580
_cell_volume                     3844.55(5)
_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 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
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9896
_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    -30.00  -5.00   1.00    1.61    --   22.00 118.00-132.48   25
  2  \w   -115.00 -20.00   1.00    1.61    --  -42.37 -38.00   0.00   95
  3  \w    -87.00  -7.00   1.00    1.61    --  -42.37 125.00 -90.00   80
  4  \w   -115.00 -21.00   1.00    1.61    --  -42.37 -38.00  90.00   94
  5  \w   -111.00 -18.00   1.00    1.61    --  -42.37 -38.00-180.00   93
  6  \w   -116.00 -30.00   1.00    1.61    --  -42.37 -38.00 -90.00   86
  7  \w     27.00  98.00   1.00    1.61    --   42.37-125.00 150.00   71
  8  \w      8.00  33.00   1.00    1.61    --   42.37  83.00  46.93   25
  9  \w     16.00  41.00   1.00    1.61    --   50.00  81.00 -68.27   25
 10  \w     16.00  42.00   1.00    1.61    --   50.00  82.00  64.88   26
 11  \w     16.00  41.00   1.00    1.61    --   50.00  81.00   0.42   25
 12  \w     16.00  42.00   1.00    1.61    --   50.00  81.00-145.59   26
 13  \w     16.00  41.00   1.00    1.61    --   50.00  82.00 137.03   25
 14  \w     36.00  61.00   1.00    1.61    --   66.00  70.00 170.07   25
 15  \w     35.00  64.00   1.00    1.61    --   66.00  71.00  51.69   29
 16  \w     35.00  62.00   1.00    1.61    --   66.00  69.00  26.90   27
 17  \w     39.00  65.00   1.00    1.61    --   70.00  69.00-168.43   26
 18  \w     39.00  64.00   1.00    1.61    --   70.00  71.00  91.43   25
 19  \w    100.00 143.00   1.00    1.61    --   70.00  71.00 -91.52   43
 20  \w     40.00  65.00   1.00    1.61    --   70.00  71.00-153.39   25
 21  \w    106.00 132.00   1.00    1.61    --   70.00  71.00 -40.88   26
 22  \w    110.00 140.00   1.00    1.61    --   70.00  71.00-153.39   30
 23  \w     39.00  66.00   1.00    1.61    --   70.00  69.00 121.03   27
 24  \w     39.00  65.00   1.00    1.61    --   70.00  71.00 -40.88   26
 25  \w     98.00 143.00   1.00    1.61    --   70.00  66.00  -5.59   45
 26  \w     40.00  66.00   1.00    1.61    --   70.00  66.00  -5.59   26
 27  \w     39.00  65.00   1.00    1.61    --   70.00  71.00 -91.52   26
 28  \w     40.00  67.00   1.00    1.61    --   70.00  70.00 -69.74   27
 29  \w     44.00  71.00   1.00    6.43    --   74.00  66.00 147.25   27
 30  \w     43.00  69.00   1.00    6.43    --   74.00  69.00-118.36   26
 31  \w     48.00  74.00   1.00    6.43    --   78.00  68.00  -5.79   26
 32  \w     51.00  77.00   1.00    6.43    --   82.00  70.00  18.94   26
 33  \w     57.00  86.00   1.00    6.43    --   86.00  61.00  72.52   29
 34  \w     55.00  82.00   1.00    6.43    --   86.00  70.00 -67.16   27
 35  \w    113.00 139.00   1.00    6.43    --   86.00  70.00  32.61   26
 36  \w     55.00  81.00   1.00    6.43    --   86.00  70.00  32.61   26
 37  \w     59.00  85.00   1.00    6.43    --   90.00  70.00-116.78   26
 38  \w     61.00  87.00   1.00    6.43    --   90.00  63.00-141.49   26
 39  \w     59.00  85.00   1.00    6.43    --   90.00  71.00 161.07   26
 40  \w     94.00 167.00   1.00    6.43    --   94.00  71.00  88.84   73
 41  \w     63.00  89.00   1.00    6.43    --   94.00  71.00  88.84   26
 42  \w     64.00 167.00   1.00    6.43    --   94.00  64.00  -9.90  103
 43  \w    134.00 171.00   1.00    6.43    --   98.00  65.00 111.61   37
 44  \w     68.00  94.00   1.00    6.43    --   98.00  65.00 111.61   26
 45  \w     71.00 174.00   1.00    6.43    --  102.00  71.00 163.64  103
 46  \w    106.00 162.00   1.00    6.43    --  103.86  65.00-109.63   56
 47  \w     89.00 117.00   1.00    6.43    --  103.86 -61.00-150.00   28
 48  \w     74.00  99.00   1.00    6.43    --  103.86  65.00-109.63   25
 49  \w     33.00  64.00   1.00    6.43    --  103.86 -61.00-150.00   31
 50  \w     75.00 125.00   1.00    6.43    --  103.86  61.00 -30.00   50
 51  \w     75.00 172.00   1.00    6.43    --  103.86  71.00-155.95   97
 52  \w    148.00 174.00   1.00    6.43    --  103.86  61.00 -90.00   26
 53  \w     77.00 102.00   1.00    6.43    --  103.86  61.00 -90.00   25
 54  \w     80.00 106.00   1.00    6.43    --  103.86 -95.00  30.00   26
 55  \w     33.00  63.00   1.00    6.43    --  103.86 -95.00  30.00   30
 56  \w     75.00 153.00   1.00    6.43    --  103.86  61.00  30.00   78
 57  \w     29.00  71.00   1.00    6.43    --  103.86 -77.00-180.00   42
 58  \w    103.00 130.00   1.00    6.43    --  103.86 -61.00  30.00   27
 59  \w     37.00  73.00   1.00    6.43    --  103.86 -61.00  30.00   36
 60  \w     25.00 106.00   1.00    6.43    --  103.86 -95.00 -90.00   81
 61  \w     75.00 174.00   1.00    6.43    --  103.86  61.00 -60.00   99
 62  \w     32.00 106.00   1.00    6.43    --  103.86 -95.00 120.00   74
 63  \w     36.00 101.00   1.00    6.43    --  103.86 -95.00   0.00   65
 64  \w     75.00 141.00   1.00    6.43    --  103.86  61.00 137.17   66
 65  \w    111.00 175.00   1.00    6.43    --  103.86  61.00  60.00   64
 66  \w     76.00 108.00   1.00    6.43    --  103.86  61.00  60.00   32
 67  \w     48.00 108.00   1.00    6.43    --  103.86-109.00-124.81   60
;
_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      0.1141120000
_diffrn_orient_matrix_UB_12      -0.0010099000
_diffrn_orient_matrix_UB_13      0.0093976000
_diffrn_orient_matrix_UB_21      -0.0000675000
_diffrn_orient_matrix_UB_22      -0.1183804000
_diffrn_orient_matrix_UB_23      -0.0071219000
_diffrn_orient_matrix_UB_31      0.0088646000
_diffrn_orient_matrix_UB_32      0.0121243000
_diffrn_orient_matrix_UB_33      -0.0689378000
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.9999
_diffrn_reflns_Laue_measured_fraction_max 0.9896
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            71163
_diffrn_reflns_point_group_measured_fraction_full 0.9999
_diffrn_reflns_point_group_measured_fraction_max 0.9896
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         72.54
_diffrn_reflns_theta_min         3.75
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.729
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       block
_exptl_crystal_F_000             2099.288
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.4819
_refine_diff_density_min         -0.9890
_refine_diff_density_rms         0.0803
_refine_ls_d_res_high            0.8081
_refine_ls_d_res_low             11.7925
_refine_ls_goodness_of_fit_ref   1.0503
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0503
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+3.0656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0546
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -13
_reflns_number_gt                7322
_reflns_number_total             7553
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt03760f2.cif
_cod_data_source_block           exp_3105
_cod_depositor_comments
'Adding full bibliography for 7715892--7715896.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7715896
_chemical_oxdiff_formula         'C33 H33 Co F6 La N4 O12 S2'
_chemical_oxdiff_usercomment     TN001
_reflns_odcompleteness_completeness 99.94
_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), C33(H33a,H33b,H33c)
;
_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 1.873
_oxdiff_exptl_absorpt_empirical_full_min 0.723