Predictable electronic tuning of Fe<sup>II</sup> and Ru<sup>II</sup> complexes <i>via</i> choice of azine: correlation of ligand p<i>K</i><sub>a</sub> with <i>E</i><sub>pa</sub>(M<sup>III/II</sup>) of complex.
Robb, Matthew G.; Bondì, Luca; Rodríguez-Jiménez, Santiago; Garden, Anna L.; Jerabek, Paul; Brooker, Sally; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1999–2007; doi:10.1039/d3dt03484d

data_7714785
_publ_section_title
;
 Predictable electronic tuning of Fe<sup>II</sup> and Ru<sup>II</sup>
 complexes <i>via</i> choice of azine: correlation of ligand
 p<i>K</i><sub>a</sub> with <i>E</i><sub>pa</sub>(M<sup>III/II</sup>) of
 complex.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1999
_journal_page_last               2007
_journal_paper_doi               10.1039/d3dt03484d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C57 H45 N15 Ru, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C61 H51 F12 N17 P2 Ru'
_chemical_formula_weight         1413.19
_chemical_name_common            'Ru(II) complex of pyrazine-triazole ligand'
_chemical_name_systematic        '[Ru(Lpyrazine)3](PF6)2.2MeCN'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-03-21 deposited with the CCDC.	2023-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.352(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2893(5)
_cell_length_b                   17.5489(6)
_cell_length_c                   18.9097(6)
_cell_measurement_reflns_used    8123
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.9560
_cell_measurement_theta_min      4.0790
_cell_volume                     6042.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1725
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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   -129.00 -34.00   1.00   10.00    --  -41.79 178.00 150.00   95
  2  \w    -67.00  32.00   1.00   10.00    --  -41.79  40.00 102.00   99
  3  \w   -116.00 -17.00   1.00   10.00    --  -41.79 -38.00 120.00   99
  4  \w     57.00 131.00   1.00   10.00    --   41.79 178.00-180.00   74
  5  \w     39.00 118.00   1.00   40.00    --  112.00-125.00  30.00   79
  6  \w     30.00 110.00   1.00   40.00    --  112.00 -95.00-150.00   80
  7  \w     84.00 178.00   1.00   40.00    --  112.00  30.00 150.00   94
  8  \w     79.00 178.00   1.00   40.00    --  112.00  77.00   0.00   99
  9  \w     58.00 135.00   1.00   40.00    --  112.00 -45.00 -30.00   77
 10  \w     73.00 117.00   1.00   40.00    --  112.00-125.00 -60.00   44
 11  \w     50.00 117.00   1.00   40.00    --  112.00-125.00  90.00   67
 12  \w    130.00 156.00   1.00   40.00    --  112.00 125.00 -60.00   26
 13  \w     39.00 128.00   1.00   40.00    --  112.00 -45.00-150.00   89
;
_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      0.0752674000
_diffrn_orient_matrix_UB_12      0.0234376000
_diffrn_orient_matrix_UB_13      0.0369185000
_diffrn_orient_matrix_UB_21      0.0177676000
_diffrn_orient_matrix_UB_22      -0.0842174000
_diffrn_orient_matrix_UB_23      0.0169337000
_diffrn_orient_matrix_UB_31      0.0342130000
_diffrn_orient_matrix_UB_32      -0.0079029000
_diffrn_orient_matrix_UB_33      -0.0710884000
_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  0.1303
_diffrn_reflns_av_unetI/netI     0.1339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35206
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.297
_diffrn_reflns_theta_min         4.085
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       needle
_exptl_crystal_F_000             2872
_exptl_crystal_preparation       'redox and theoretical (DFT) study'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: vapour diffusion of diethyl ether into acetonitrile solution'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.662
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         12393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0741
_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^)+(0.0945P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.1992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7878
_reflns_number_total             12393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03484d3.cif
_cod_data_source_block           mgr40
_cod_depositor_comments
'Adding full bibliography for 7714784--7714786.cif.'
_cod_database_code               7714785
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.748
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), C20(H20), C50(H50), C12(H12), C49(H49), C7(H7), C41(H41),
 C2(H2), C39(H39), C40(H40), C21(H21), C26(H26), C27(H27), C30(H30), C22(H22),
 C19(H19), C55(H55), C46(H46), C45(H45), C57(H57), C56(H56), C31(H31), C8(H8),
 C15(H15), C53(H53), C34(H34), C38(H38), C54(H54), C11(H11), C16(H16), C36(H36),
  C18(H18), C35(H35), C37(H37), C17(H17)
2.b Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C29(H29A,H29B,H29C), C202(H20A,H20B,H20C), C10(H10A,H10B,
 H10C), C102(H10D,H10E,H10F)
;
_shelx_res_checksum              17564
_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 4.667
_oxdiff_exptl_absorpt_empirical_full_min 0.377