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_7715894
_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 F6 La Mn N4 O12 S2'
_chemical_formula_sum            'C33 H33 F6 La Mn N4 O12 S2'
_chemical_formula_weight         1049.616
_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                 99.748(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0537(2)
_cell_length_b                   13.0153(2)
_cell_length_c                   19.0750(2)
_cell_measurement_reflns_used    8588
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.0810
_cell_measurement_theta_min      4.1400
_cell_volume                     3928.06(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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_temperature      150.15
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9794
_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    -93.00 -65.00   1.00    2.50    --  -33.50 -57.00 -30.00   28
  2  \w    -44.00 -19.00   1.00    2.50    --  -33.50 -57.00 -30.00   25
  3  \w   -104.00 -74.00   1.00    2.50    --  -33.50-178.00-150.00   30
  4  \w     23.00  58.00   1.00    2.50    --   36.21  57.00 120.00   35
  5  \w    -30.00  36.00   1.00    2.50    --   36.21 -19.00-150.00   66
  6  \w     35.00  75.00   1.00    2.50    --   36.21 -99.00   0.00   40
  7  \w     61.00 101.00   1.00    2.50    --   36.21  57.00 120.00   40
  8  \w     27.00  75.00   1.00    2.50    --   36.21 -99.00 150.00   48
  9  \w     72.00  99.00   1.00    2.50    --   36.21 178.00 -30.00   27
 10  \w     52.00 116.00   1.00   10.00    --  108.00 -45.00   0.00   64
 11  \w    109.00 172.00   1.00   10.00    --  108.00 111.00-180.00   63
 12  \w    106.00 176.00   1.00   10.00    --  108.00  77.00 -90.00   70
 13  \w     69.00 117.00   1.00   10.00    --  108.00 -45.00 150.00   48
 14  \w     39.00  90.00   1.00   10.00    --  108.00 -94.00-180.00   51
 15  \w    103.00 128.00   1.00   10.00    --  108.00 -30.00 150.00   25
 16  \w     40.00  66.00   1.00   10.00    --  108.00 -45.00 150.00   26
 17  \w     46.00  72.00   1.00   10.00    --  108.00 -30.00 150.00   26
 18  \w    105.00 176.00   1.00   10.00    --  108.00  45.00-120.00   71
 19  \w    107.00 172.00   1.00   10.00    --  108.00  30.00-180.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9794
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14963
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9794
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         71.97
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    12.744
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       block
_exptl_crystal_F_000             2098.393
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.1310
_refine_diff_density_min         -1.5581
_refine_diff_density_rms         0.1207
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             13.2620
_refine_ls_goodness_of_fit_ref   1.0491
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0491
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.9443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -19
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -13
_reflns_number_gt                6973
_reflns_number_total             7564
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt03760f2.cif
_cod_data_source_block           exp_548
_cod_depositor_comments
'Adding full bibliography for 7715892--7715896.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7715894
_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), C31(H31a,H31b,H31c)
;
_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
;