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_1564042
_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(Cl O4)'
_chemical_formula_sum            'C28 H30 Cl2 Fe N6 O8'
_chemical_formula_weight         705.33
_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
_cell_angle_alpha                67.053(2)
_cell_angle_beta                 78.5550(10)
_cell_angle_gamma                69.178(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4312(2)
_cell_length_b                   12.5054(2)
_cell_length_c                   12.8166(2)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    293
_cell_measurement_theta_max      31.9690
_cell_measurement_theta_min      3.0890
_cell_volume                     1573.16(5)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.952
_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   20.00    --   29.89  54.00  30.00  624
  2  \w    -69.00 118.20   0.30   20.00    --   29.89  54.00-180.00  624
  3  \w    -69.00 118.20   0.30   20.00    --   29.89  54.00 150.00  624
  4  \w    -69.00  60.00   0.30   20.00    --   29.89  54.00 -60.00  430
  5  \w    -69.00 118.20   0.30   20.00    --   29.89  54.00 -90.00  624
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35533
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.789
_diffrn_reflns_theta_min         2.487
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84403
_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    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         11108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0591
_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^)+(0.1139P)^2^+0.4530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8166
_reflns_number_total             11108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            enfeac-rt.cif
_cod_data_source_block           enfeac-rt
_cod_database_code               1564042
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.061) H6B(0.061) H3A(0.063) H3B(0.063) H1(0.06) H4(0.058)
 H15(0.063) H3(0.067) H27A(0.062) H27B(0.062) H12(0.081) H2(0.067) H16(0.077)
 H13A(0.072) H13B(0.072) H8(0.077) H28A(0.068) H28B(0.068) H10(0.095)
 H26(0.078) H9(0.096) H14A(0.083) H14B(0.083) H18(0.068) H17(0.082) H11(0.101)
 H25(0.098) H24(0.097) H22(0.093) H23(0.114)
 Fixed X: H6A(0.4933) H6B(0.5456) H3A(0.3328) H3B(0.4575) H1(0.2312)
 H4(0.1484) H15(0.0607) H3(0.1166) H27A(0.4516) H27B(0.5241) H12(0.3697)
 H2(0.152) H16(-0.1158) H13A(0.2407) H13B(0.3442) H8(0.0102) H28A(0.6006)
 H28B(0.4679) H10(0.0931) H26(0.4164) H9(-0.0542) H14A(0.4954) H14B(0.4182)
 H18(0.0394) H17(-0.1276) H11(0.3018) H25(0.4313) H24(0.3046) H22(0.1226)
 H23(0.1465)
 Fixed Y: H6A(0.0697) H6B(0.166) H3A(0.4141) H3B(0.3541) H1(0.2072) H4(-
 0.0806) H15(0.3498) H3(-0.0864) H27A(0.3107) H27B(0.3387) H12(-0.0979)
 H2(0.0642) H16(0.5151) H13A(0.2588) H13B(0.1311) H8(0.0858) H28A(0.131)
 H28B(0.1192) H10(-0.1834) H26(0.5724) H9(-0.0328) H14A(0.2001) H14B(0.3104)
 H18(0.637) H17(0.6623) H11(-0.2157) H25(0.6869) H24(0.6954) H22(0.4998)
 H23(0.6073)
 Fixed Z: H6A(0.8054) H6B(0.7335) H3A(0.555) H3B(0.5946) H1(1.0006) H4(0.9128)
 H15(0.6386) H3(1.1003) H27A(0.9462) H27B(0.8254) H12(0.6476) H2(1.1418)
 H16(0.6197) H13A(0.5063) H13B(0.5241) H8(0.7049) H28A(0.9028) H28B(0.9582)
 H10(0.5816) H26(0.7927) H9(0.6414) H14A(0.5373) H14B(0.4399) H18(0.787)
 H17(0.6903) H11(0.5836) H25(0.8919) H24(1.051) H22(1.0014) H23(1.1046)
;
_shelx_res_checksum              60998
_shelx_hkl_checksum              79801
_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
;