Non-Heme Mononitrosyldiiron Complexes: Importance of Iron Oxidation State in Controlling the Nature of the Nitrosylated Products
Amit Majumdar; Stephen J. Lippard; Inorganic Chemistry 52 (2013) 13292–13294; doi:10.1021/ic4019508

data_4336835
_publ_contact_author_address
;Department of Chemistry, Room 18-498
Massachusetts Institute of Technology
77 Massachusetts Avenue
Cambridge, MA 02139-4307
;
_publ_contact_author_email       lippard@mit.edu
_publ_contact_author_name        'S. J. Lippard'
_publ_section_title
;
 Non-Heme Mononitrosyldiiron Complexes: Importance of Iron Oxidation State
 in Controlling the Nature of the Nitrosylated Products
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13292
_journal_page_last               13294
_journal_paper_doi               10.1021/ic4019508
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C49 H64 Fe2 N13 O5, 3(B F4)'
_chemical_formula_sum            'C49 H64 B3 F12 Fe2 N13 O5'
_chemical_formula_weight         1287.26
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-06-19
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                67.6430(10)
_cell_angle_beta                 73.8330(10)
_cell_angle_gamma                76.6920(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6754(5)
_cell_length_b                   14.8013(6)
_cell_length_c                   18.9609(7)
_cell_measurement_reflns_used    18135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.21
_cell_volume                     3375.6(2)
_computing_data_reduction        'SAINT v7.46A (Bruker, 2008)'
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54938
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0539 before and 0.0403 after correction.
The Ratio of minimum to maximum transmission is 0.8968.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.663
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         12837
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0891
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1695P)^2^+6.8667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2648
_refine_ls_wR_factor_ref         0.2796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10205
_reflns_number_total             12837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4019508_si_002_3.cif
_cod_data_source_block           113
_cod_database_code               4336835
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C44-C46B
 2.42 with sigma of 0.04
 N11A-C44 \\sim N11B-C44
 with sigma of 0.02
 N11A-C45A \\sim N11A-C46A \\sim N11B-C45B \\sim N11B-C46B
 with sigma of 0.02
 F6-B2 \\sim F8-B2
 with sigma of 0.02
 F10B-B3B \\sim F9B-B3B \\sim F12B-B3B \\sim F11B-B3B \\sim F12A-B3A 
\\sim F11A-B3A \\sim F10A-B3A ~
 F9A-B3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C20) = Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C16)
Uanis(C45A) = Uanis(C45B) = Uanis(C46A) = Uanis(C46B)
Uanis(N11A) = Uanis(N11B)
Uanis(C44) = Uanis(C46A) = Uanis(C46B) = Uanis(C45A) = Uanis(C45B)
 = Uanis(N11A) = Uanis(N11B)
Uanis(F10B) = Uanis(F10A)
Uanis(F12B) = Uanis(F12A)
Uanis(F9A) = Uanis(F9B)
Uanis(F11B) = Uanis(F11A)
Uanis(F5) = Uanis(F9A) = Uanis(F9B) = Uanis(F11A) = Uanis(F11B) =
 Uanis(F10A) = Uanis(F10B) = Uanis(F12A) = Uanis(F12B) = 
Uanis(B3A) = Uanis(B3B)
Uanis(C21) = Uanis(C22)
Uanis(F2) = Uanis(F4)
Uanis(F6) = Uanis(F7)
4. others
 Sof(H44A)=Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46B)=Sof(H46D)=
 Sof(H46E)=Sof(H46F)=Sof(N11B)=1-FVAR(1)
 Sof(H44)=Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46A)=Sof(H46A)=
 Sof(H46B)=Sof(H46C)=Sof(N11A)=FVAR(1)
 Sof(B3B)=Sof(F9B)=Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(2)
 Sof(B3A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C13(H13A,H13B), C21(H21A,H21B),
 C23(H23A,H23B), C24(H24A,H24B), C32(H32A,H32B), C34(H34A,H34B), C42(H42A,H42B)
5.c Me refined with riding coordinates:
 C45A(H45A,H45B,H45C), C45B(H45D,H45E,H45F), C46A(H46A,H46B,H46C), C46B(H46D,
 H46E,H46F)
5.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C16(H16), C17(H17), C18(H18), C19(H19),
 C27(H27), C28(H28), C29(H29), C30(H30), C37(H37), C38(H38), C39(H39), C40(H40),
  C44(H44), C44(H44A), C47(H47)
5.e Tetrahedral OH refined with riding coordinates:
 O4(H4)
5.f Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C43(H43A,H43B,
 H43C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.829
_shelx_res_checksum              33144
_shelxl_version_number           2013-3