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_4338052
_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_formula_moiety
'C60 H58 Fe N9 P, 2(C F3 O3 S), 0.78(C4 H10 O), C2 H3 N'
_chemical_formula_sum            'C67.12 H68.8 F6 Fe N10 O6.78 P S2'
_chemical_formula_weight         1388.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                88.1913(14)
_cell_angle_beta                 64.9341(17)
_cell_angle_gamma                61.0812(19)
_cell_formula_units_Z            2
_cell_length_a                   15.3998(3)
_cell_length_b                   15.6626(3)
_cell_length_c                   17.9588(3)
_cell_measurement_reflns_used    31172
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9920
_cell_measurement_theta_min      3.2460
_cell_volume                     3351.41(15)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 16.1500
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9059
_diffrn_measurement_details
;
  1 omega   15.00   60.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -99.0000  -60.0000 45

  2 omega  -11.00   87.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909   77.0000  120.0000 98

  3 omega   16.00   87.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000   30.0000 71

  4 omega  -51.00  -13.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -57.0000 -120.0000 38

  5 omega  -11.00   14.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909   77.0000  -30.0000 25

  6 omega   42.00   69.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909   77.0000  -30.0000 27

  7 omega  -34.00   48.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -77.0000 -180.0000 82

  8 omega  -50.00   35.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -57.0000  -90.0000 85

  9 omega  -35.00   -8.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -57.0000  -30.0000 27

 10 omega  -86.00  -52.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -      -18.4034  -57.0000  -60.0000 34

 11 omega   -3.00   87.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000  -90.0000 90

 12 omega   35.00   94.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  178.0000  150.0000 59

 13 omega   35.00   94.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  178.0000    0.0000 59

 14 omega  -51.00   38.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -57.0000    0.0000 89

 15 omega   -3.00   87.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000    0.0000 90

 16 omega   35.00   94.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  178.0000 -120.0000 59

 17 omega  -54.00   32.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -37.0000 -150.0000 86

 18 omega  -86.00  -33.00   1.0000    5.7400
omega____ theta____ kappa____ phi______ frames
    -      -18.4034  142.0000   63.0887 53
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0298253000
_diffrn_orient_matrix_UB_12      0.0466637000
_diffrn_orient_matrix_UB_13      -0.0090886000
_diffrn_orient_matrix_UB_21      -0.0261478000
_diffrn_orient_matrix_UB_22      -0.0188545000
_diffrn_orient_matrix_UB_23      -0.0130158000
_diffrn_orient_matrix_UB_31      -0.0443526000
_diffrn_orient_matrix_UB_32      0.0166765000
_diffrn_orient_matrix_UB_33      0.0417677000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74982
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1445
_exptl_crystal_size_max          0.5061
_exptl_crystal_size_mid          0.3565
_exptl_crystal_size_min          0.1765
_refine_diff_density_max         1.889
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         16362
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+4.4094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                13651
_reflns_number_total             16362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403126p_si_002.cif
_cod_data_source_block           '[4](OTf)2'
_cod_depositor_comments
'Adding full bibliography for 4338051--4338054.cif.'
_cod_original_cell_volume        3351.42(10)
_cod_original_formula_sum        'C67.12 H68.80 F6 Fe N10 O6.78 P S2'
_cod_database_code               4338052
_chemical_oxdiff_formula
'Fe P C48 N6 H39 N2 C10 H16 (Me C N)2 (C F3 S O3)2 Et2 O'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H8A(0.021) H8B(0.021) H7A(0.023) H7B(0.023) H4A(0.031) H4B(0.031)
 H4C(0.031) H6(0.027) H7(0.033) H8(0.036) H9(0.037) H10(0.029) H12(0.024)
 H13(0.031) H14(0.035) H15(0.034) H16(0.026) H20A(0.039) H20B(0.039)
 H20C(0.039) H22(0.033) H23(0.042) H24(0.038) H25(0.033) H26(0.027) H28(0.03)
 H29(0.041) H30(0.042) H31(0.036) H32(0.025) H36A(0.035) H36B(0.035)
 H36C(0.035) H38(0.035) H39(0.048) H40(0.051) H41(0.051) H42(0.037) H44(0.023)
 H45(0.028) H46(0.028) H47(0.031) H48(0.028) H51(0.027) H53(0.031) H54(0.027)
 H56A(0.069) H56B(0.069) H56C(0.069) H56D(0.05) H56E(0.05) H56F(0.05)
 H57A(0.069) H57B(0.069) H57C(0.069) H57D(0.08) H57E(0.08) H57F(0.08)
 H58A(0.072) H58B(0.072) H58C(0.072) H58D(0.082) H58E(0.082) H58F(0.082)
 H60A(0.048) H60B(0.048) H60C(0.048) H64A(0.044) H64B(0.044) H64C(0.044)
 H65A(0.146) H65B(0.146) H66A(0.139) H66B(0.139) H66C(0.139) H67A(0.074)
 H67B(0.074) H68A(0.077) H68B(0.077) H68C(0.077)
 Fixed X: H8A(0.2591) H8B(0.1981) H7A(0.5522) H7B(0.5261) H4A(0.2053)
 H4B(0.229) H4C(0.1029) H6(0.0824) H7(-0.0854) H8(-0.2567) H9(-0.2617) H10(-
 0.0948) H12(0.0473) H13(-0.0138) H14(0.0026) H15(0.0754) H16(0.1414)
 H20A(0.4512) H20B(0.3178) H20C(0.3727) H22(0.2241) H23(0.2084) H24(0.3378)
 H25(0.4867) H26(0.5075) H28(0.2146) H29(0.2122) H30(0.3784) H31(0.5474)
 H32(0.5495) H36A(0.5907) H36B(0.6991) H36C(0.5794) H38(0.7109) H39(0.8779)
 H40(1.0442) H41(1.0443) H42(0.8783) H44(0.5511) H45(0.606) H46(0.7419)
 H47(0.8275) H48(0.7738) H51(0.175) H53(0.4521) H54(0.5605) H56A(0.2081)
 H56B(0.1116) H56C(0.1153) H56D(0.1088) H56E(0.0649) H56F(0.0615) H57A(0.3455)
 H57B(0.2556) H57C(0.3562) H57D(0.3544) H57E(0.2304) H57F(0.2703) H58A(0.106)
 H58B(0.112) H58C(0.2067) H58D(0.2009) H58E(0.1713) H58F(0.2994) H60A(0.393)
 H60B(0.2626) H60C(0.3053) H64A(0.9613) H64B(0.8797) H64C(0.9312) H65A(0.797)
 H65B(0.8597) H66A(0.8859) H66B(0.9365) H66C(0.9787) H67A(0.8205) H67B(0.8252)
 H68A(0.6712) H68B(0.6155) H68C(0.6997)
 Fixed Y: H8A(0.2365) H8B(0.223) H7A(0.0336) H7B(0.0933) H4A(0.5603)
 H4B(0.5888) H4C(0.628) H6(0.5134) H7(0.6052) H8(0.6557) H9(0.6117) H10(0.52)
 H12(0.3269) H13(0.2133) H14(0.1215) H15(0.1467) H16(0.2564) H20A(0.5479)
 H20B(0.6141) H20C(0.5756) H22(0.6057) H23(0.6632) H24(0.5621) H25(0.4039)
 H26(0.347) H28(0.3529) H29(0.2459) H30(0.102) H31(0.0621) H32(0.1646)
 H36A(0.3943) H36B(0.3446) H36C(0.4265) H38(0.2311) H39(0.1601) H40(0.0318)
 H41(-0.0225) H42(0.0497) H44(0.0407) H45(-0.1275) H46(-0.2322) H47(-0.1701)
 H48(-0.0016) H51(0.1003) H53(-0.1766) H54(-0.1114) H56A(-0.0462) H56B(-0.0622)
 H56C(0.0348) H56D(0.0432) H56E(-0.032) H56F(0.0372) H57A(-0.2348) H57B(-
 0.2303) H57C(-0.2179) H57D(-0.1974) H57E(-0.1706) H57F(-0.0939) H58A(-0.007)
 H58B(-0.109) H58C(-0.1114) H58D(-0.118) H58E(-0.1708) H58F(-0.2125) H60A(-
 0.0935) H60B(-0.0169) H60C(-0.0541) H64A(-0.2033) H64B(-0.2448) H64C(-0.2159)
 H65A(0.4274) H65B(0.3678) H66A(0.2885) H66B(0.221) H66C(0.2943) H67A(0.2414)
 H67B(0.1911) H68A(0.1966) H68B(0.3021) H68C(0.2015)
 Fixed Z: H8A(0.4078) H8B(0.3677) H7A(0.216) H7B(0.2936) H4A(0.0831)
 H4B(0.1544) H4C(0.1732) H6(0.0583) H7(0.0501) H8(0.1679) H9(0.2946)
 H10(0.3039) H12(0.3662) H13(0.3932) H14(0.2827) H15(0.1464) H16(0.1185)
 H20A(0.3161) H20B(0.3714) H20C(0.272) H22(0.5138) H23(0.6402) H24(0.6862)
 H25(0.6043) H26(0.476) H28(0.5281) H29(0.6218) H30(0.6003) H31(0.4837)
 H32(0.3863) H36A(-0.0201) H36B(-0.0056) H36C(0.0688) H38(-0.1316) H39(-0.2581)
 H40(-0.263) H41(-0.141) H42(-0.0134) H44(0.0191) H45(0.0112) H46(0.0509)
 H47(0.0937) H48(0.1011) H51(0.4504) H53(0.3602) H54(0.2807) H56A(0.5769)
 H56B(0.5802) H56C(0.5532) H56D(0.5668) H56E(0.5719) H56F(0.5044) H57A(0.3929)
 H57B(0.4832) H57C(0.4753) H57D(0.5005) H57E(0.5663) H57F(0.5688) H58A(0.4233)
 H58B(0.4451) H58C(0.359) H58D(0.3765) H58E(0.4534) H58F(0.3862) H60A(0.1344)
 H60B(0.164) H60C(0.2327) H64A(0.1727) H64B(0.2189) H64C(0.2677) H65A(0.0912)
 H65B(0.1447) H66A(-0.0046) H66B(0.052) H66C(0.0099) H67A(0.205) H67B(0.1258)
 H68A(0.2009) H68B(0.26) H68C(0.2761)
;