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_4336836
_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             2013-05-31
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                67.4970(10)
_cell_angle_beta                 73.7200(10)
_cell_angle_gamma                76.6050(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7005(6)
_cell_length_b                   14.8640(7)
_cell_length_c                   18.9800(9)
_cell_measurement_reflns_used    17077
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.16
_cell_volume                     3393.8(3)
_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      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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            55416
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.56
_diffrn_source                   'Fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0513 before and 0.0417 after correction.
The Ratio of minimum to maximum transmission is 0.9212.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.931
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         12913
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0815
_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^)+(0.1607P)^2^+3.5736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2439
_refine_ls_wR_factor_ref         0.2602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9887
_reflns_number_total             12913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4019508_si_002_4.cif
_cod_data_source_block           101
_cod_database_code               4336836
_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
 C45B-C46B
 2.45 with sigma of 0.04
 C44-C45B
 2.45 with sigma of 0.04
 N11B-C46B \\sim N11B-C45B
 with sigma of 0.02
 F9A-B3A \\sim F10A-B3A \\sim F11A-B3A \\sim F12A-B3A \\sim F9B-B3B 
\\sim F11B-B3B \\sim F10B-B3B ~
 F12B-B3B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N11A) = Uanis(N11B)
Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20)
Uanis(C9) = Uanis(C8) = Uanis(C10)
Uanis(C44) = Uanis(C45B) = Uanis(C45A) = Uanis(C46A) = Uanis(C46B)
Uanis(F3A) = Uanis(F3B)
Uanis(F4A) = Uanis(F4B)
Uanis(B1) = Uanis(B3B) = Uanis(B3A)
Uanis(F1) = Uanis(F12B) = Uanis(F12A) = Uanis(F10B) = Uanis(F10A) = Uanis(F9A) 
= Uanis(F9B) = Uanis(F11A) = Uanis(F11B)
Uanis(F7) = Uanis(F5B) = Uanis(F5A) = Uanis(F8B) = Uanis(F8A)
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)
 Sof(F3B)=Sof(F4B)=1-FVAR(3)
 Sof(F3A)=Sof(F4A)=FVAR(3)
 Sof(F5B)=Sof(F8B)=1-FVAR(4)
 Sof(F5A)=Sof(F8A)=FVAR(4)
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 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.d Tetrahedral OH refined with riding coordinates:
 O2(H2)
5.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C43(H43A,H43B,
 H43C), C45A(H45A,H45B,H45C), C45B(H45D,H45E,H45F), C46A(H46A,H46B,H46C),
 C46B(H46D,H46E,H46F), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.815
_shelx_res_checksum              17516
_shelxl_version_number           2013-3