Dioxygen Reactivity of Biomimetic Fe(II) Complexes with Noninnocent Catecholate, o-Aminophenolate, and o-Phenylenediamine Ligands.
Bittner, Michael M.; Lindeman, Sergey V.; Popescu, Codrina V.; Fiedler, Adam T.; Inorganic chemistry 53 (2014) 4047–4061; doi:10.1021/ic403126p

data_4338051
_publ_section_title
;
 Dioxygen Reactivity of Biomimetic Fe(II) Complexes with Noninnocent
 Catecholate, o-Aminophenolate, and o-Phenylenediamine Ligands.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4047
_journal_page_last               4061
_journal_paper_doi               10.1021/ic403126p
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C58 H52 Fe N6 O2 P, C F3 O3 S, 2(C2 H4 Cl2)'
_chemical_formula_sum            'C63 H60 Cl4 F3 Fe N6 O5 P S'
_chemical_formula_weight         1298.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.1428(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.08589(16)
_cell_length_b                   21.47794(14)
_cell_length_c                   17.84876(18)
_cell_measurement_reflns_used    36281
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.5850
_cell_measurement_theta_min      3.6720
_cell_volume                     6166.58(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9419
_diffrn_measurement_details
;
  1 omega  -69.00   -8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -77.0000  150.0000 61

  2 omega  -75.00   38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987   77.0000   60.0000 113

  3 omega -116.00  -78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -77.0000  150.0000 38

  4 omega  -32.00    1.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   30.0000   30.0000 33

  5 omega   49.00   85.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -94.0000 -120.0000 36

  6 omega   39.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000  150.0000 50

  7 omega   29.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -94.0000 -180.0000 80

  8 omega   81.00  118.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -125.0000   30.0000 37

  9 omega   33.00   65.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -125.0000   30.0000 32

 10 omega   36.00  122.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -61.0000  -60.0000 86

 11 omega   79.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000 -150.0000 29

 12 omega  132.00  162.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000 -150.0000 30

 13 omega   77.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   30.0000  -60.0000 100

 14 omega  -70.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987   57.0000  -90.0000 103

 15 omega -115.00  -11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -57.0000 -120.0000 104

 16 omega -115.00  -11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -57.0000    0.0000 104

 17 omega   77.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   30.0000 -180.0000 101

 18 omega   32.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   30.0000 66

 19 omega   79.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000    0.0000 99

 20 omega   79.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000 -120.0000 99

 21 omega   73.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   77.0000   30.0000 105

 22 omega   79.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000   90.0000 99

 23 omega -115.00  -80.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987 -142.0000   38.0000 35
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0266578000
_diffrn_orient_matrix_UB_12      -0.0279038000
_diffrn_orient_matrix_UB_13      0.0757552000
_diffrn_orient_matrix_UB_21      0.0063404000
_diffrn_orient_matrix_UB_22      -0.0659461000
_diffrn_orient_matrix_UB_23      -0.0333376000
_diffrn_orient_matrix_UB_31      0.0918145000
_diffrn_orient_matrix_UB_32      -0.0035607000
_diffrn_orient_matrix_UB_33      0.0244810000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60871
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.76
_diffrn_reflns_theta_min         3.22
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.642
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.2228
_exptl_crystal_size_min          0.1842
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1532
_refine_ls_number_reflns         23500
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+2.2596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                23223
_reflns_number_total             23500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403126p_si_002.cif
_cod_data_source_block           '[3]OTf'
_cod_depositor_comments
'Adding full bibliography for 4338051--4338054.cif.'
_cod_database_code               4338051
_chemical_oxdiff_formula         'Fe C59 H51 N6 O5 P S F3 C2 H4 Cl2'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.035) H4A(0.044) H4B(0.044) H4C(0.044) H6(0.032) H7(0.036)
 H8(0.038) H9(0.041) H10(0.037) H12(0.039) H13(0.043) H14(0.048) H15(0.049)
 H16(0.035) H20A(0.048) H20B(0.048) H20C(0.048) H22(0.038) H23(0.048)
 H24(0.048) H25(0.05) H26(0.041) H28(0.032) H29(0.037) H30(0.038) H31(0.038)
 H32(0.034) H36A(0.043) H36B(0.043) H36C(0.043) H38(0.044) H39(0.052)
 H40(0.056) H41(0.05) H42(0.039) H44(0.035) H45(0.043) H46(0.039) H47(0.035)
 H48(0.028) H51(0.03) H53(0.039) H54(0.035) H56A(0.06) H56B(0.06) H56C(0.06)
 H57A(0.082) H57B(0.082) H57C(0.082) H58A(0.09) H58B(0.09) H58C(0.09)
 H1A(0.045) H4AA(0.045) H4AB(0.045) H4AC(0.045) H6A(0.035) H7A(0.042)
 H8A(0.041) H9A(0.039) H10A(0.031) H12A(0.046) H13A(0.054) H14A(0.046)
 H15A(0.065) H16A(0.059) H20D(0.041) H20E(0.041) H20F(0.041) H22A(0.041)
 H23A(0.058) H24A(0.06) H25A(0.052) H26A(0.041) H28A(0.038) H29A(0.045)
 H30A(0.05) H31A(0.044) H32A(0.034) H36D(0.046) H36E(0.046) H36F(0.046)
 H38A(0.036) H39A(0.038) H40A(0.042) H41A(0.04) H42A(0.034) H44A(0.041)
 H45A(0.049) H46A(0.05) H47A(0.046) H48A(0.035) H51A(0.032) H53A(0.038)
 H54A(0.039) H56D(0.124) H56E(0.124) H56F(0.124) H57D(0.059) H57E(0.059)
 H57F(0.059) H58D(0.081) H58E(0.081) H58F(0.081) H1SA(0.072) H1SB(0.072)
 H2SA(0.072) H2SB(0.072) H3SA(0.054) H3SB(0.054) H4SA(0.066) H4SB(0.066)
 H5SA(0.056) H5SB(0.056) H6SA(0.05) H6SB(0.05) H7SA(0.063) H7SB(0.063)
 H8SA(0.083) H8SB(0.083)
 Fixed X: H4A(0.043) H4B(0.0247) H4C(0.0513) H6(0.0625) H7(-0.0314) H8(-0.03)
 H9(0.0677) H10(0.1636) H12(0.2861) H13(0.3831) H14(0.4767) H15(0.4751)
 H16(0.3793) H20A(0.1949) H20B(0.1733) H20C(0.1409) H22(0.3527) H23(0.3545)
 H24(0.3379) H25(0.3261) H26(0.3269) H28(0.5214) H29(0.6619) H30(0.7092)
 H31(0.6138) H32(0.4703) H36A(0.1165) H36B(0.1564) H36C(0.1513) H38(0.4048)
 H39(0.4077) H40(0.3172) H41(0.218) H42(0.2122) H44(0.4161) H45(0.5482)
 H46(0.6664) H47(0.6519) H48(0.5201) H51(0.6625) H53(0.7087) H54(0.5669)
 H56A(0.7942) H56B(0.8842) H56C(0.8157) H57A(0.7878) H57B(0.8693) H57C(0.7813)
 H58A(0.8412) H58B(0.9003) H58C(0.8178) H4AA(0.4362) H4AB(0.4695) H4AC(0.4527)
 H6A(0.3355) H7A(0.427) H8A(0.5287) H9A(0.5393) H10A(0.4467) H12A(0.1386)
 H13A(0.0558) H14A(0.0461) H15A(0.1261) H16A(0.2062) H20D(0.3473) H20E(0.317)
 H20F(0.3676) H22A(0.101) H23A(0.1111) H24A(0.2123) H25A(0.3031) H26A(0.2917)
 H28A(-0.0273) H29A(-0.1544) H30A(-0.1652) H31A(-0.0467) H32A(0.0827)
 H36D(0.3137) H36E(0.2667) H36F(0.3177) H38A(0.0153) H39A(-0.0034) H40A(0.0904)
 H41A(0.2036) H42A(0.2208) H44A(-0.0077) H45A(-0.1488) H46A(-0.2378) H47A(-
 0.1851) H48A(-0.0432) H51A(-0.1524) H53A(-0.2206) H54A(-0.0846) H56D(-0.3296)
 H56E(-0.403) H56F(-0.335) H57D(-0.267) H57E(-0.3617) H57F(-0.2906) H58D(-
 0.3061) H58E(-0.3786) H58F(-0.2888) H1SA(-0.0506) H1SB(-0.014) H2SA(0.0719)
 H2SB(-0.0005) H3SA(0.5416) H3SB(0.5505) H4SA(0.5099) H4SB(0.4384) H5SA(-
 0.0761) H5SB(0.0142) H6SA(-0.0449) H6SB(-0.0549) H7SA(0.4388) H7SB(0.4779)
 H8SA(0.4846) H8SB(0.5415)
 Fixed Y: H4A(0.6725) H4B(0.7114) H4C(0.6397) H6(0.7926) H7(0.876) H8(0.9436)
 H9(0.931) H10(0.8488) H12(0.8532) H13(0.9331) H14(0.9315) H15(0.8481)
 H16(0.7667) H20A(0.4365) H20B(0.4828) H20C(0.4977) H22(0.3864) H23(0.3214)
 H24(0.3627) H25(0.4692) H26(0.5355) H28(0.54) H29(0.5577) H30(0.5818)
 H31(0.5915) H32(0.5754) H36A(0.5192) H36B(0.4627) H36C(0.4595) H38(0.413)
 H39(0.3444) H40(0.3546) H41(0.4345) H42(0.5038) H44(0.5626) H45(0.5712)
 H46(0.5667) H47(0.5547) H48(0.5414) H51(0.675) H53(0.752) H54(0.7449)
 H56A(0.6193) H56B(0.6446) H56C(0.6323) H57A(0.7766) H57B(0.734) H57C(0.7058)
 H58A(0.7377) H58B(0.7579) H58C(0.7968) H4AA(0.7779) H4AB(0.7081) H4AC(0.7359)
 H6A(0.5599) H7A(0.475) H8A(0.4638) H9A(0.5362) H10A(0.6216) H12A(0.6069)
 H13A(0.5171) H14A(0.4578) H15A(0.4821) H16A(0.5724) H20D(0.9264) H20E(0.9642)
 H20F(0.9006) H22A(0.9906) H23A(1.0539) H24A(1.0332) H25A(0.9501) H26A(0.8858)
 H28A(0.8417) H29A(0.8198) H30A(0.8118) H31A(0.8227) H32A(0.8403) H36D(0.9026)
 H36E(0.9655) H36F(0.9272) H38A(0.9757) H39A(1.0401) H40A(1.037) H41A(0.9685)
 H42A(0.902) H44A(0.8442) H45A(0.8273) H46A(0.8164) H47A(0.8227) H48A(0.8411)
 H51A(0.6884) H53A(0.6512) H54A(0.6729) H56D(0.7473) H56E(0.6973) H56F(0.7026)
 H57D(0.6348) H57E(0.6546) H57F(0.7067) H58D(0.5849) H58E(0.5872) H58F(0.5609)
 H1SA(0.7078) H1SB(0.7063) H2SA(0.6549) H2SB(0.6047) H3SA(0.7554) H3SB(0.6824)
 H4SA(0.7017) H4SB(0.716) H5SA(0.5617) H5SB(0.5497) H6SA(0.5514) H6SB(0.6165)
 H7SA(0.3517) H7SB(0.4199) H8SA(0.4038) H8SB(0.3554)
 Fixed Z: H4A(0.051) H4B(0.1256) H4C(0.1313) H6(0.0097) H7(0.0154) H8(0.1166)
 H9(0.2116) H10(0.2062) H12(0.0402) H13(0.0547) H14(0.1553) H15(0.2401)
 H16(0.2233) H20A(-0.0109) H20B(-0.0784) H20C(0.0043) H22(-0.0579) H23(-0.1626)
 H24(-0.2813) H25(-0.2975) H26(-0.1939) H28(0.0768) H29(0.0565) H30(-0.0634)
 H31(-0.1631) H32(-0.1411) H36A(0.2602) H36B(0.3063) H36C(0.2168) H38(0.3297)
 H39(0.4313) H40(0.5291) H41(0.5279) H42(0.4275) H44(0.4154) H45(0.4695)
 H46(0.3932) H47(0.2643) H48(0.211) H51(0.1874) H53(-0.0158) H54(-0.0458)
 H56A(0.1341) H56B(0.1115) H56C(0.0481) H57A(0.1958) H57B(0.1991) H57C(0.2234)
 H58A(0.0048) H58B(0.0728) H58C(0.0551) H4AA(0.6233) H4AB(0.6141) H4AC(0.6959)
 H6A(0.5414) H7A(0.5377) H8A(0.6309) H9A(0.727) H10A(0.7308) H12A(0.5257)
 H13A(0.5274) H14A(0.6343) H15A(0.7391) H16A(0.7385) H20D(0.5527) H20E(0.4804)
 H20F(0.4706) H22A(0.4097) H23A(0.3022) H24A(0.2129) H25A(0.2281) H26A(0.3325)
 H28A(0.5322) H29A(0.4764) H30A(0.3464) H31A(0.2726) H32A(0.3285) H36D(0.8247)
 H36E(0.8018) H36F(0.7401) H38A(0.8304) H39A(0.9341) H40A(1.0345) H41A(1.0304)
 H42A(0.9275) H44A(0.8894) H45A(0.9067) H46A(0.8039) H47A(0.6835) H48A(0.6648)
 H51A(0.6864) H53A(0.473) H54A(0.4322) H56D(0.5842) H56E(0.5777) H56F(0.5126)
 H57D(0.7174) H57E(0.7035) H57F(0.7071) H58D(0.5304) H58E(0.5916) H58F(0.6139)
 H1SA(-0.2134) H1SB(-0.1302) H2SA(-0.2183) H2SB(-0.2312) H3SA(0.2844)
 H3SB(0.3009) H4SA(0.4261) H4SB(0.366) H5SA(0.428) H5SB(0.3935) H6SA(0.2719)
 H6SB(0.3147) H7SA(0.0644) H7SB(0.0739) H8SA(0.2055) H8SB(0.1604)
;