pH dependent catecholase activity of Fe(II) complexes of type [Fe(L)]X2 [L = N-(phenyl-pyridin-2-yl-methylene)-ethane-1,2-diamine; X = ClO4− (1), PF6− (2)]: Role of counter anion on turnover number
Chatterjee, Arnab; Kaur, Gurpreet; Joshi, Mayank; Choudhury, Angshuman Roy; Ghosh, Rajarshi; Inorganica Chimica Acta 513 (2020) 119933–; doi:10.1016/j.ica.2020.119933

data_1564043
_publ_section_title
;
 pH dependent catecholase activity of Fe(II) complexes of type [Fe(L)]X2
 [L&#x00A0;=&#x00A0;N-(phenyl-pyridin-2-yl-methylene)-ethane-1,2-diamine;
 X&#x00A0;=&#x00A0;ClO4&#x2212; (1), PF6&#x2212; (2)]: Role of counter
 anion on turnover number
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119933
_journal_paper_doi               10.1016/j.ica.2020.119933
_journal_volume                  513
_journal_year                    2020
_chemical_formula_moiety         'C28 H30 Fe N6, 2(F6 P)'
_chemical_formula_sum            'C28 H30 F12 Fe N6 P2'
_chemical_formula_weight         796.37
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                66.204(2)
_cell_angle_beta                 75.134(2)
_cell_angle_gamma                70.645(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8627(2)
_cell_length_b                   12.6978(2)
_cell_length_c                   12.9813(3)
_cell_measurement_reflns_used    8230
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.9880
_cell_measurement_theta_min      2.8790
_cell_volume                     1670.85(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_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    -69.00 118.20   0.30    6.00    --   29.89  54.00 120.00  624
  2  \w    -69.00 118.20   0.30    6.00    --   29.89  54.00-150.00  624
  3  \w    -69.00 118.20   0.30    6.00    --   29.89  54.00-150.00  624
  4  \w    -69.00 118.20   0.30    6.00    --   29.89  54.00   0.00  624
  5  \w    -69.00 100.20   0.30    6.00    --   29.89  54.00  30.00  564
  6  \w    -69.00 118.20   0.30    6.00    --   29.89  54.00 -60.00  624
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0617787000
_diffrn_orient_matrix_UB_12      -0.0032572000
_diffrn_orient_matrix_UB_13      -0.0041644000
_diffrn_orient_matrix_UB_21      -0.0051119000
_diffrn_orient_matrix_UB_22      -0.0214032000
_diffrn_orient_matrix_UB_23      0.0601793000
_diffrn_orient_matrix_UB_31      0.0160168000
_diffrn_orient_matrix_UB_32      -0.0593597000
_diffrn_orient_matrix_UB_33      0.0009562000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42298
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         2.700
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.401
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         9761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0660
_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^)+(0.1214P)^2^+0.7154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.2215
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7050
_reflns_number_total             9761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Fe-en-PF6IISERM.cif
_cod_data_source_block           en-fe-pf6-rt
_cod_database_code               1564043
_chemical_oxdiff_formula         'C20 H14 N6 P2 F12 Fe1'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), C13(H13A,H13B), C14(H14A,H14B), C27(H27A,H27B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C15(H15), C18(H18), C17(H17), C4(H4), C16(H16), C22(H22), C23(H23),
 C26(H26), C3(H3), C24(H24), C12(H12), C2(H2), C8(H8), C10(H10), C9(H9),
 C25(H25), C11(H11)
;
_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 1.206
_oxdiff_exptl_absorpt_empirical_full_min 0.781