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_4338053
_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
'C58 H55 Fe N8 P, 0.8(C2 H4 Cl2), C F3 O3 S, C24 H20 B, 0.84(C5 H12)'
_chemical_formula_sum            'C88.82 H88.32 B Cl1.6 F3 Fe N8 O3 P S'
_chemical_formula_weight         1559.11
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-06
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0089(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6939(4)
_cell_length_b                   18.3202(4)
_cell_length_c                   22.2057(4)
_cell_measurement_reflns_used    21765
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.0050
_cell_measurement_theta_min      3.4590
_cell_volume                     8006.8(3)
_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 0.9978
_diffrn_measured_fraction_theta_max 0.8929
_diffrn_measurement_details
;
  1 omega   10.00   36.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -57.0000  -60.0000 26

  2 omega  -53.00   15.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -37.0000   30.0000 68

  3 omega   45.00   72.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0909  178.0000   60.0000 27

  4 omega   -7.00   87.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0909   37.0000 -180.0000 94

  5 omega  -90.00  -65.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.4034  148.0000   13.6885 25

  6 omega  -86.00  -61.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.4034  142.0000 -108.8839 25

  7 omega   34.00   95.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0909 -178.0000  -90.0000 61

  8 omega  -12.00   54.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0909   77.0000  -90.0000 66

  9 omega   -8.00   91.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0909   37.0000   60.0000 99
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0345156000
_diffrn_orient_matrix_UB_12      -0.0106664000
_diffrn_orient_matrix_UB_13      -0.0015002000
_diffrn_orient_matrix_UB_21      -0.0101183000
_diffrn_orient_matrix_UB_22      -0.0370968000
_diffrn_orient_matrix_UB_23      -0.0023790000
_diffrn_orient_matrix_UB_31      -0.0021355000
_diffrn_orient_matrix_UB_32      0.0032652000
_diffrn_orient_matrix_UB_33      -0.0318267000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77363
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.917
_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    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3270
_exptl_crystal_size_max          0.4544
_exptl_crystal_size_mid          0.3418
_exptl_crystal_size_min          0.0746
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         19234
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0962
_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^)+(0.0696P)^2^+24.7018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2375
_reflns_number_gt                13891
_reflns_number_total             19234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403126p_si_002.cif
_cod_data_source_block           '[4](OTf)(BPh4)'
_cod_depositor_comments
'Adding full bibliography for 4338051--4338054.cif.'
_cod_original_formula_sum        'C88.82 H88.32 B Cl1.60 F3 Fe N8 O3 P S'
_cod_database_code               4338053
_chemical_oxdiff_formula         'Fe C86 H82 N8 B P C F3 S O3 C2 H4 Cl2'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{Cl1, Cl1A}
2. Others
 Fixed Uiso: H7A(0.048) H7B(0.048) H8A(0.058) H8B(0.058) H4A(0.078) H4B(0.078)
 H4C(0.078) H6(0.074) H7(0.109) H8(0.136) H9(0.123) H10(0.084) H12(0.066)
 H13(0.089) H14(0.094) H15(0.102) H16(0.083) H20A(0.071) H20B(0.071)
 H20C(0.071) H22(0.042) H23(0.047) H24(0.052) H25(0.072) H26(0.069) H22A(0.078)
 H23A(0.091) H24A(0.068) H25A(0.057) H26A(0.048) H28(0.093) H29(0.136)
 H30(0.093) H31(0.11) H32(0.095) H36A(0.068) H36B(0.068) H36C(0.068) H38(0.049)
 H39(0.057) H40(0.048) H41(0.052) H42(0.046) H38A(0.049) H39A(0.06) H40A(0.06)
 H41A(0.064) H42A(0.057) H44(0.07) H45(0.101) H46(0.112) H47(0.1) H48(0.062)
 H51(0.046) H53(0.063) H54(0.054) H56A(0.116) H56B(0.116) H56C(0.116)
 H57A(0.087) H57B(0.087) H57C(0.087) H58A(0.127) H58B(0.127) H58C(0.127)
 H56D(0.369) H56E(0.369) H56F(0.369) H57D(0.215) H57E(0.215) H57F(0.215)
 H58D(0.32) H58E(0.32) H58F(0.32) H84A(0.078) H84B(0.078) H85A(0.083)
 H85B(0.083) H84C(0.103) H84D(0.103) H85C(0.067) H85D(0.067) H61(0.057)
 H62(0.056) H63(0.052) H64(0.054) H65(0.046) H67(0.077) H68(0.085) H69(0.063)
 H70(0.047) H71(0.042) H73(0.047) H74(0.053) H75(0.055) H76(0.058) H77(0.049)
 H79(0.049) H80(0.052) H81(0.049) H82(0.048) H83(0.044) H86A(0.196) H86B(0.196)
 H86C(0.196) H87A(0.143) H87B(0.143) H88A(0.151) H88B(0.151) H89A(0.11)
 H89B(0.11) H90A(0.519) H90B(0.519) H90C(0.519)
 Fixed X: H7A(0.3765) H7B(0.3904) H8A(0.4459) H8B(0.4195) H4A(0.1224)
 H4B(0.1555) H4C(0.1323) H6(0.203) H7(0.2001) H8(0.2701) H9(0.3399) H10(0.349)
 H12(0.4348) H13(0.5496) H14(0.5854) H15(0.5053) H16(0.3902) H20A(0.1317)
 H20B(0.1473) H20C(0.1183) H22(0.3145) H23(0.3128) H24(0.2704) H25(0.2244)
 H26(0.2289) H22A(0.2195) H23A(0.2122) H24A(0.2719) H25A(0.3117) H26A(0.3165)
 H28(0.3951) H29(0.5104) H30(0.5858) H31(0.5473) H32(0.4316) H36A(0.0562)
 H36B(0.0422) H36C(0.0616) H38(0.1633) H39(0.1005) H40(0.0218) H41(0.0135)
 H42(0.0773) H38A(0.0977) H39A(0.0331) H40A(0.0411) H41A(0.0982) H42A(0.1603)
 H44(0.2733) H45(0.3676) H46(0.4431) H47(0.4252) H48(0.3332) H51(0.5627)
 H53(0.6181) H54(0.5051) H56A(0.6487) H56B(0.7238) H56C(0.6594) H57A(0.6917)
 H57B(0.7412) H57C(0.6636) H58A(0.7187) H58B(0.7706) H58C(0.7145) H56D(0.7112)
 H56E(0.7557) H56F(0.6801) H57D(0.6659) H57E(0.7403) H57F(0.6761) H58D(0.6898)
 H58E(0.762) H58F(0.7243) H84A(0.5922) H84B(0.5256) H85A(0.5554) H85B(0.545)
 H84C(0.6558) H84D(0.7092) H85C(0.642) H85D(0.6745) H61(0.0616) H62(0.0805)
 H63(0.148) H64(0.197) H65(0.1777) H67(0.1398) H68(0.1125) H69(0.0281) H70(-
 0.0273) H71(0.0005) H73(0.1455) H74(0.243) H75(0.3176) H76(0.2921) H77(0.1954)
 H79(-0.02) H80(-0.1224) H81(-0.1383) H82(-0.0527) H83(0.047) H86A(0.4521)
 H86B(0.4129) H86C(0.378) H87A(0.4338) H87B(0.4297) H88A(0.5288) H88B(0.5232)
 H89A(0.5092) H89B(0.5377) H90A(0.632) H90B(0.6045) H90C(0.6027)
 Fixed Y: H7A(0.3419) H7B(0.2945) H8A(0.5082) H8B(0.5106) H4A(0.2482)
 H4B(0.2352) H4C(0.3154) H6(0.1187) H7(0.0077) H8(-0.0116) H9(0.0808)
 H10(0.1897) H12(0.3498) H13(0.3207) H14(0.2107) H15(0.1296) H16(0.1576)
 H20A(0.5236) H20B(0.6094) H20C(0.5728) H22(0.7333) H23(0.8415) H24(0.8447)
 H25(0.7412) H26(0.6292) H22A(0.7144) H23A(0.8172) H24A(0.8162) H25A(0.7086)
 H26A(0.605) H28(0.6822) H29(0.7032) H30(0.6163) H31(0.5017) H32(0.4787)
 H36A(0.4423) H36B(0.4166) H36C(0.3577) H38(0.5167) H39(0.5217) H40(0.4296)
 H41(0.3286) H42(0.3229) H38A(0.5233) H39A(0.5252) H40A(0.4273) H41A(0.3221)
 H42A(0.3187) H44(0.338) H45(0.3428) H46(0.44) H47(0.5317) H48(0.526)
 H51(0.5004) H53(0.298) H54(0.2622) H56A(0.5287) H56B(0.5023) H56C(0.4643)
 H57A(0.4333) H57B(0.4871) H57C(0.5094) H58A(0.3459) H58B(0.3853) H58C(0.3303)
 H56D(0.3218) H56E(0.3878) H56F(0.3747) H57D(0.5101) H57E(0.5108) H57F(0.5353)
 H58D(0.4333) H58E(0.4366) H58F(0.3599) H84A(0.8287) H84B(0.8047) H85A(0.6822)
 H85B(0.7226) H84C(0.6819) H84D(0.7432) H85C(0.77) H85D(0.6895) H61(0.5325)
 H62(0.5315) H63(0.4406) H64(0.3527) H65(0.3541) H67(0.5807) H68(0.6911)
 H69(0.6988) H70(0.5921) H71(0.4811) H73(0.2961) H74(0.2495) H75(0.3264)
 H76(0.4504) H77(0.4976) H79(0.4236) H80(0.3602) H81(0.2765) H82(0.2593)
 H83(0.3275) H86A(0.6505) H86B(0.576) H86C(0.6527) H87A(0.5797) H87B(0.6654)
 H88A(0.588) H88B(0.6731) H89A(0.5946) H89B(0.674) H90A(0.6302) H90B(0.6099)
 H90C(0.5503)
 Fixed Z: H7A(0.7749) H7B(0.7222) H8A(0.6758) H8B(0.7378) H4A(0.5745)
 H4B(0.5106) H4C(0.5296) H6(0.5898) H7(0.5389) H8(0.4581) H9(0.4259) H10(0.48)
 H12(0.5642) H13(0.5711) H14(0.6149) H15(0.6505) H16(0.6432) H20A(0.5141)
 H20B(0.5128) H20C(0.5721) H22(0.5841) H23(0.5287) H24(0.4321) H25(0.3876)
 H26(0.4409) H22A(0.5663) H23A(0.5024) H24A(0.4137) H25A(0.3782) H26A(0.4394)
 H28(0.6108) H29(0.6157) H30(0.5906) H31(0.5634) H32(0.5574) H36A(0.6858)
 H36B(0.7531) H36C(0.7033) H38(0.8763) H39(0.9644) H40(0.9825) H41(0.9207)
 H42(0.8335) H38A(0.8365) H39A(0.9238) H40A(0.9931) H41A(0.9668) H42A(0.8781)
 H44(0.8767) H45(0.9427) H46(0.9376) H47(0.8676) H48(0.8001) H51(0.7194)
 H53(0.7731) H54(0.7712) H56A(0.7976) H56B(0.8167) H56C(0.8456) H57A(0.6658)
 H57B(0.7034) H57C(0.6899) H58A(0.8071) H58B(0.7637) H58C(0.7362) H56D(0.7044)
 H56E(0.6798) H56F(0.6531) H57D(0.6792) H57E(0.7106) H57F(0.748) H58D(0.8304)
 H58E(0.7995) H58F(0.807) H84A(0.7472) H84B(0.709) H85A(0.7225) H85B(0.7855)
 H84C(0.6844) H84D(0.704) H85C(0.7862) H85D(0.7872) H61(0.2504) H62(0.1487)
 H63(0.1073) H64(0.1709) H65(0.2731) H67(0.3299) H68(0.3726) H69(0.4437)
 H70(0.4718) H71(0.4293) H73(0.3635) H74(0.4097) H75(0.4645) H76(0.4716)
 H77(0.4229) H79(0.2711) H80(0.2753) H81(0.3533) H82(0.4265) H83(0.4244)
 H86A(1.0853) H86B(1.0696) H86C(1.0534) H87A(0.9764) H87B(0.9733) H88A(1.0028)
 H88B(0.9962) H89A(0.8987) H89B(0.9103) H90A(0.9365) H90B(0.87) H90C(0.9226)
;