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_7715893
_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 Mn N3 Na2 O9 S, 2[C2H3N]'
_chemical_formula_sum            'C34 H36 F3 Mn N5 Na2 O9 S'
_chemical_formula_weight         848.66
_chemical_name_systematic        exp_603
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-02-28 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                104.826(4)
_cell_angle_beta                 106.697(4)
_cell_angle_gamma                105.433(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6556(5)
_cell_length_b                   13.3317(5)
_cell_length_c                   13.5391(6)
_cell_measurement_reflns_used    7299
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.0210
_cell_measurement_theta_min      4.1350
_cell_volume                     1812.26(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 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 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_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    -25.00  17.00   1.00    6.61    --  -33.50  57.00 120.00   42
  2  \w   -106.00 -47.00   1.00    6.61    --  -33.50-178.00 120.00   59
  3  \w    -44.00 -17.00   1.00    6.61    --  -33.50 -57.00 150.00   27
  4  \w   -101.00 -63.00   1.00    6.61    --  -33.50 -57.00 150.00   38
  5  \w      2.00  74.00   1.00    6.61    --   36.21 -99.00   0.00   72
  6  \w     58.00  91.00   1.00    6.61    --   36.21-130.00 -78.00   33
  7  \w     37.00 103.00   1.00    6.61    --   36.21  57.00 -60.00   66
  8  \w      7.00 107.00   1.00    6.61    --   36.21  19.00  90.00  100
  9  \w    -31.00  53.00   1.00    6.61    --   36.21 -57.00 150.00   84
 10  \w      5.00  57.00   1.00    6.61    --   36.21 -77.00  90.00   52
 11  \w    151.00 176.00   1.00   26.44    --  108.00  45.00 -60.00   25
 12  \w     91.00 117.00   1.00   26.44    --  108.00  61.00  90.00   26
 13  \w    104.00 176.00   1.00   26.44    --  108.00  45.00 120.00   72
 14  \w     92.00 119.00   1.00   26.44    --  108.00  45.00 -60.00   27
 15  \w     43.00 106.00   1.00   26.44    --  108.00-111.00   0.00   63
 16  \w     44.00 124.00   1.00   26.44    --  108.00 -45.00 150.00   80
 17  \w     64.00 108.00   1.00   26.44    --  108.00-111.00 150.00   44
 18  \w    101.00 127.00   1.00   26.44    --  108.00 -77.00 150.00   26
 19  \w     42.00 118.00   1.00   26.44    --  108.00 -45.00  60.00   76
 20  \w     42.00  71.00   1.00   26.44    --  108.00 -94.00  30.00   29
 21  \w     77.00 103.00   1.00   26.44    --  108.00 -94.00  30.00   26
 22  \w     63.00 107.00   1.00   26.44    --  108.00-111.00-120.00   44
 23  \w     39.00 124.00   1.00   26.44    --  108.00 -30.00 -60.00   85
 24  \w     45.00  89.00   1.00   26.44    --  108.00 -94.00 -60.00   44
 25  \w     59.00 104.00   1.00   26.44    --  108.00 -61.00   0.00   45
 26  \w    148.00 173.00   1.00   26.44    --  108.00  61.00  90.00   25
 27  \w     52.00  77.00   1.00   26.44    --  108.00 -77.00 150.00   25
 28  \w     73.00 178.00   1.00   26.44    --  108.00  15.00-120.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0114227000
_diffrn_orient_matrix_UB_12      -0.0999692000
_diffrn_orient_matrix_UB_13      -0.0948026000
_diffrn_orient_matrix_UB_21      0.0793724000
_diffrn_orient_matrix_UB_22      -0.0381520000
_diffrn_orient_matrix_UB_23      0.0848596000
_diffrn_orient_matrix_UB_31      -0.1247841000
_diffrn_orient_matrix_UB_32      -0.0711382000
_diffrn_orient_matrix_UB_33      0.0049286000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12129
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.132
_diffrn_reflns_theta_min         3.653
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.417
_exptl_absorpt_correction_T_max  0.146
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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 orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.696
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.337
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6974
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0951P)^2^+0.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6397
_reflns_number_total             6974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03760f2.cif
_cod_data_source_block           exp_603
_cod_depositor_comments
'Adding full bibliography for 7715892--7715896.cif.'
_cod_original_cell_volume        1812.26(14)
_cod_database_code               7715893
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         MnUC29H30N3O6I2
_shelx_estimated_absorpt_t_max   0.318
_shelx_estimated_absorpt_t_min   0.149
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Rigid bond restraints
 S1, O7, O8, O9
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
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)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11131
_shelx_fab_checksum              46709
_olex2_submission_original_sample_id exp_603
_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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.758