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_4336837
_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   constr
_audit_creation_date             2013-05-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                76.9090(10)
_cell_angle_beta                 79.8750(10)
_cell_angle_gamma                66.8620(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7306(7)
_cell_length_b                   13.5070(7)
_cell_length_c                   21.6669(12)
_cell_measurement_reflns_used    23123
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.33
_cell_volume                     3321.2(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-Axs,2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-Axs,2009)'
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53478
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.699
_diffrn_reflns_theta_min         1.665
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0541 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.8984.
The \l/2 correction factor is 0.0015.

;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.494
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         12602
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0901
_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^)+(0.1633P)^2^+6.7955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2625
_refine_ls_wR_factor_ref         0.2797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9612
_reflns_number_total             12602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4019508_si_002_5.cif
_cod_data_source_block           105
_cod_database_code               4336837
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4
 0.82 with sigma of 0.02
 F6A-B2A \\sim F8A-B2A \\sim F5A-B2A \\sim F7A-B2A \\sim F8B-B2B \\sim F6B-B2B 
\\sim F7B-B2B \\sim F5B-B2B
 with sigma of 0.02
 F10A-B3A \\sim F12A-B3A \\sim F9A-B3A \\sim F11A-B3A \\sim F10B-B3B 
\\sim F11B-B3B \\sim F9B-B3B ~
 F12B-B3B
 with sigma of 0.02
 C12A-C11 \\sim C12B-C11
 with sigma of 0.02
 F3A-B1A \\sim F1A-B1A \\sim F2A-B1A \\sim F4A-B1A \\sim F4B-B1B 
\\sim F3B-B1B \\sim F1B-B1B \\sim F2B-B1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F5A) = Uanis(F5B)
Uanis(F7B) = Uanis(F7A)
Uanis(F5A) = Uanis(F5B) = Uanis(F7A) = Uanis(F7B) = Uanis(F6A) = Uanis(F6B) 
= Uanis(F8B) = Uanis(F8A)
Uanis(B2B) = Uanis(B2A)
Uanis(B3A) = Uanis(B3B)
Uanis(F10B) = Uanis(F12A) = Uanis(F11B)
Uanis(F9A) = Uanis(F9B)
Uanis(F9A) = Uanis(F9B) = Uanis(F10A) = Uanis(F12A) = Uanis(F11B) = Uanis(F12B)
= Uanis(F10B) = Uanis(B3B) = Uanis(B3A) = Uanis(F11A)
Uanis(C43A) = Uanis(C43B)
Uanis(C22A) = Uanis(C22B)
Uanis(C11) = Uanis(C12B) = Uanis(C12A)
Uanis(F2A) = Uanis(F2B)
Uanis(B1A) = Uanis(B1B)
Uanis(F1B) = Uanis(F1A) = Uanis(B1A) = Uanis(B1B)
Uanis(F3B) = Uanis(F3A)
4. others
 Sof(B1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(1)
 Sof(B1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=FVAR(1)
 Sof(B2B)=Sof(F5B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=1-FVAR(2)
 Sof(B2A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=FVAR(2)
 Sof(B3B)=Sof(F9B)=Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(3)
 Sof(B3A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(3)
 Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(4)
 Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(4)
 Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(5)
 Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(5)
 Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(6)
 Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(6)
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), C11(H11C,H11D), C13(H13A,H13B),
 C21(H21A,H21B), C21(H21C,H21D), C23(H23A,H23B), C24(H24A,H24B), C32(H32A,H32B),
  C34(H34A,H34B), C42(H42A,H42B), C42(H42C,H42D)
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), C47(H47)
5.d Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C12B(H12D,H12E,H12F), C22A(H22A,H22B,H22C), C22B(H22D,
 H22E,H22F), C33(H33A,H33B,H33C), C43A(H43A,H43B,H43C), C43B(H43D,H43E,H43F),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C)
;
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.827
_shelx_res_checksum              55209
_shelxl_version_number           2013-3