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_7715892
_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 Co F3 N3 Na2 O9 S'
_chemical_formula_sum            'C30 H30 Co F3 N3 Na2 O9 S'
_chemical_formula_weight         770.54
_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             2023-08-23
_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                104.532(3)
_cell_angle_beta                 106.887(3)
_cell_angle_gamma                105.274(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7547(5)
_cell_length_b                   13.2058(5)
_cell_length_c                   13.4600(4)
_cell_measurement_reflns_used    7704
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.1540
_cell_measurement_theta_min      4.2180
_cell_volume                     1803.26(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.974
_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   -103.00  33.00   1.00    5.00    --  -33.50   0.00 -60.00  136
  2  \w     44.00  75.00   1.00    5.00    --   36.21 -99.00 -60.00   31
  3  \w     20.00 103.00   1.00    5.00    --   36.21  57.00 -30.00   83
  4  \w     69.00 104.00   1.00    5.00    --   36.21 178.00 -30.00   35
  5  \w     29.00  99.00   1.00    5.00    --   36.21  57.00 120.00   70
  6  \w     73.00  98.00   1.00    5.00    --   36.21 178.00 120.00   25
  7  \w      4.00  57.00   1.00    5.00    --   36.21 -99.00  60.00   53
  8  \w      2.00  51.00   1.00    5.00    --   36.21 -37.00-180.00   49
  9  \w    -33.00  -7.00   1.00    5.00    --   36.21 -37.00-180.00   26
 10  \w     23.00  75.00   1.00    5.00    --   36.21 -99.00 150.00   52
 11  \w    102.00 175.00   1.00   20.00    --  108.00  77.00  90.00   73
 12  \w     93.00 155.00   1.00   20.00    --  108.00  45.00   0.00   62
 13  \w     64.00 105.00   1.00   20.00    --  108.00-111.00  30.00   41
 14  \w    104.00 178.00   1.00   20.00    --  108.00 111.00-180.00   74
 15  \w     91.00 149.00   1.00   20.00    --  108.00  45.00 150.00   58
 16  \w     82.00 108.00   1.00   20.00    --  108.00 -30.00  90.00   26
 17  \w     38.00  64.00   1.00   20.00    --  108.00 -30.00  90.00   26
 18  \w     66.00 121.00   1.00   20.00    --  108.00 -45.00 -90.00   55
 19  \w     64.00 109.00   1.00   20.00    --  108.00-111.00-120.00   45
 20  \w     66.00 123.00   1.00   20.00    --  108.00 -45.00   0.00   57
 21  \w     79.00 107.00   1.00   20.00    --  108.00-111.00 120.00   28
 22  \w    110.00 177.00   1.00   20.00    --  108.00 111.00  30.00   67
 23  \w    114.00 146.00   1.00   20.00    --  108.00 111.00  60.00   32
 24  \w     43.00 116.00   1.00   20.00    --  108.00 -45.00 120.00   73
 25  \w     51.00 112.00   1.00   20.00    --  108.00 -77.00  90.00   61
 26  \w     92.00 160.00   1.00   20.00    --  108.00  45.00-120.00   68
 27  \w     52.00  96.00   1.00   20.00    --  108.00-111.00 -30.00   44
;
_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      0.0322522000
_diffrn_orient_matrix_UB_12      0.1184988000
_diffrn_orient_matrix_UB_13      0.0810637000
_diffrn_orient_matrix_UB_21      0.1291457000
_diffrn_orient_matrix_UB_22      -0.0011646000
_diffrn_orient_matrix_UB_23      0.0694240000
_diffrn_orient_matrix_UB_31      0.0623647000
_diffrn_orient_matrix_UB_32      0.0518230000
_diffrn_orient_matrix_UB_33      -0.0705385000
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12391
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.154
_diffrn_reflns_theta_min         3.671
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.115
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0504P)^2^+1.3549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6401
_reflns_number_total             6933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03760f2.cif
_cod_data_source_block           exp_542
_cod_depositor_comments
'Adding full bibliography for 7715892--7715896.cif.'
_cod_original_cell_volume        1803.25(12)
_cod_database_code               7715892
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H30 Co F3 N4 Na2 O9 S'
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.220
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C4(H4A,H4B), C5(H5A,H5B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C18(H18), C22(H22), C16(H16), C10(H10), C8(H8), C17(H17),
 C26(H26), C9(H9), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C21(H21A,H21B,H21C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 87 electrons were 
found in a volume of 283\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C2H3N] per Asymmetric Unit 
which account for 44 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              59581
_shelx_fab_checksum              27960
_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 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.837