Tuning valence tautomerism in a family of dinuclear cobalt complexes incorporating a conjugated bridging bis(dioxolene) ligand with weak communication.
Fischer, Tristan E.; Janetzki, Jett T.; M Zahir, F Zahra; Gable, Robert W.; Starikova, Alyona A.; Boskovic, Colette; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3104–3117; doi:10.1039/d3dt04162j

data_7714944
_publ_section_title
;
 Tuning valence tautomerism in a family of dinuclear cobalt complexes
 incorporating a conjugated bridging bis(dioxolene) ligand with weak
 communication.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3104
_journal_page_last               3117
_journal_paper_doi               10.1039/d3dt04162j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C52 H48 Co2 N10 O6, 2(F6 P), 2(C2 H3 N), 2(C7 H8)'
_chemical_formula_sum            'C70 H70 Co2 F12 N12 O6 P2'
_chemical_formula_weight         1583.18
_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
_audit_creation_date             2023-08-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-11-21 deposited with the CCDC.	2024-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                93.436(2)
_cell_angle_beta                 101.986(2)
_cell_angle_gamma                111.088(2)
_cell_formula_units_Z            1
_cell_length_a                   8.6957(2)
_cell_length_b                   10.8984(2)
_cell_length_c                   20.7669(4)
_cell_measurement_reflns_used    10623
_cell_measurement_temperature    99(3)
_cell_measurement_theta_max      75.0500
_cell_measurement_theta_min      2.3010
_cell_volume                     1776.57(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      98.99(10)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    -19.00   7.00   0.50    1.40    --   48.20 -19.00  90.00   52
  2  \w     30.00  70.00   0.50    1.40    --   48.20 -93.00 133.00   80
  3  \w     52.00  95.00   0.50    1.40    --   48.20-125.00  30.00   86
  4  \w     46.00  71.00   0.50    5.61    --  107.75 -93.00 133.00   50
  5  \w     64.00 106.00   0.50    5.61    --  107.75 -94.00 120.00   84
  6  \w     81.00 107.00   0.50    5.61    --  107.75-125.00  60.00   52
  7  \w     84.00 110.00   0.50    5.61    --  107.75-125.00  30.00   52
  8  \w     81.00 107.00   0.50    5.61    --  107.75-107.00  84.72   52
  9  \w     78.00 103.00   0.50    5.61    --  107.75 -94.00  90.00   50
 10  \w     49.00  97.00   0.50    5.61    --  107.75 -94.00  60.00   96
 11  \w     40.00  66.00   0.50    5.61    --  107.75-125.00  60.00   52
 12  \w     37.00 106.00   0.50    5.61    --  107.75 -94.00  30.00  138
 13  \w     77.00 112.00   0.50    5.61    --  107.75-125.00 -30.00   70
 14  \w     81.00 106.00   0.50    5.61    --  107.75 -94.00 -60.00   50
 15  \w     80.00 105.00   0.50    5.61    --  107.75 -94.00 -90.00   50
 16  \w     58.00  84.00   0.50    5.61    --  107.75 -94.00-120.00   52
 17  \w     72.00 104.00   0.50    5.61    --  107.75 -94.00-180.00   64
 18  \w     58.00  84.00   0.50    5.61    --  107.75-125.00-150.00   52
 19  \w     41.00  66.00   0.50    5.61    --  107.75 -94.00-180.00   50
 20  \w     37.00 106.00   0.50    5.61    --  107.75 -94.00-150.00  138
 21  \w     36.00  76.00   0.50    5.61    --  107.75 -94.00 -60.00   80
 22  \w     60.00 104.00   0.50    5.61    --  107.75 -94.00 -30.00   88
 23  \w     37.00  78.00   0.50    5.61    --  107.75-125.00  30.00   82
 24  \w     35.00  72.00   0.50    5.61    --  107.75 -94.00  90.00   74
 25  \w     41.00  67.00   0.50    5.61    --  107.75 -61.00  90.00   52
 26  \w     37.00 104.00   0.50    5.61    --  107.75 -94.00 150.00  134
 27  \w     36.00  69.00   0.50    5.61    --  107.75 -61.00 150.00   66
 28  \w     40.00  65.00   0.50    5.61    --  107.75-107.00  84.72   50
 29  \w     35.00  60.00   0.50    5.61    --  107.75 -61.00  30.00   50
 30  \w     42.00  67.00   0.50    5.61    --  107.75 -61.00  60.00   50
 31  \w     35.00  60.00   0.50    5.61    --  107.75 -61.00   0.00   50
 32  \w     35.00  68.00   0.50    5.61    --  107.75 -61.00 -60.00   66
 33  \w     41.00  67.00   0.50    5.61    --  107.75 -61.00-120.00   52
 34  \w     40.00  65.00   0.50    5.61    --  107.75 -61.00-150.00   50
 35  \w     35.00  61.00   0.50    5.61    --  107.75 -94.00 -90.00   52
 36  \w     40.00  66.00   0.50    5.61    --  107.75-125.00 -30.00   52
 37  \w     42.00  69.00   0.50    5.61    --  107.75 -61.00 -90.00   54
 38  \w     95.00 129.00   0.50    5.61    --  107.75  15.00-120.00   68
 39  \w    138.00 175.00   0.50    5.61    --  107.75  15.00 -90.00   74
 40  \w    144.00 176.00   0.50    5.61    --  107.75  15.00-120.00   64
 41  \w    142.00 168.00   0.50    5.61    --  107.75  77.00-180.00   52
 42  \w    147.00 177.00   0.50    5.61    --  107.75  77.00-150.00   60
 43  \w    110.00 136.00   0.50    5.61    --  107.75  93.00-114.00   52
 44  \w    113.00 143.00   0.50    5.61    --  107.75  77.00-150.00   60
 45  \w     94.00 127.00   0.50    5.61    --  107.75  15.00 -90.00   66
 46  \w    102.00 174.00   0.50    5.61    --  107.75  45.00 -30.00  144
 47  \w    134.00 161.00   0.50    5.61    --  107.75 125.00 -30.00   54
 48  \w    110.00 172.00   0.50    5.61    --  107.75  61.00  90.00  124
 49  \w    142.00 175.00   0.50    5.61    --  107.75  77.00 120.00   66
 50  \w    114.00 140.00   0.50    5.61    --  107.75  45.00 150.00   52
 51  \w    122.00 153.00   0.50    5.61    --  107.75  77.00  90.00   62
 52  \w     97.00 123.00   0.50    5.61    --  107.75 125.00 -30.00   52
 53  \w     94.00 174.00   0.50    5.61    --  107.75  15.00-180.00  160
 54  \w    -11.00  22.00   0.50    1.40    --   48.20 -93.00 133.00   66
 55  \w    -62.00  24.00   0.50    1.40    --  -48.20  57.00 120.00  172
 56  \w    -77.00  12.00   0.50    1.40    --  -48.20  93.00-114.00  178
 57  \w    -17.00  26.00   0.50    1.40    --  -48.20  19.00-120.00   86
 58  \w    -43.00  25.00   0.50    1.40    --  -48.20  37.00-180.00  136
 59  \w    -70.00 -45.00   0.50    5.61    --  -86.25  93.00-114.00   50
 60  \w   -152.00-113.00   0.50    5.61    --  -86.25 -61.00-180.00   78
 61  \w   -137.00-111.00   0.50    5.61    --  -86.25 -61.00 -90.00   52
 62  \w   -156.00-131.00   0.50    5.61    --  -86.25-125.00   0.00   50
 63  \w   -145.00-120.00   0.50    5.61    --  -86.25 -93.00 133.00   50
 64  \w   -159.00-108.00   0.50    5.61    --  -86.25 -61.00-120.00  102
 65  \w    -24.00   3.00   0.50    1.40    --   48.20 -19.00-120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30037
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.290
_diffrn_reflns_theta_min         4.396
_exptl_absorpt_coefficient_mu    4.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       plate
_exptl_crystal_F_000             814
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0084(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1596P)^2^+0.0441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6264
_reflns_number_total             7308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04162j3.cif
_cod_data_source_block           tf1-038-mecn-tol_redabs2
_cod_depositor_comments
'Adding full bibliography for 7714944--7714946.cif.'
_cod_database_code               7714944
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.346
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C13(H13A,H13B), C7(H7A,H7B)
1.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C6(H6), C22(H22), C5(H5), C12(H12), C3(H3), C18(H18), C25(H25),
 C17(H17), C11(H11), C16(H16), C4(H4), C9(H9), C15(H15), C10(H10), C34(H34),
 C30(H30), C33(H33), C32(H32), C31(H31)
1.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              62037
_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
- B-factor correction
;