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_4336833
_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         '3(B F4), C53.21 H72.82 Fe2 N14 O5'
_chemical_formula_sum            'C53.2 H72.79 B3 F12 Fe2 N14 O5'
_chemical_formula_weight         1360.57
_chemical_name_systematic
;
 ?
;
_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             2013-06-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                97.4430(10)
_cell_angle_beta                 92.3440(10)
_cell_angle_gamma                110.6450(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1536(7)
_cell_length_b                   16.1353(10)
_cell_length_c                   17.5569(10)
_cell_measurement_reflns_used    19826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.73
_cell_measurement_theta_min      2.35
_cell_volume                     3180.8(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-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50938
_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         25.818
_diffrn_reflns_theta_min         1.658
_diffrn_source                   'Fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0623 before and 0.0341 after correction.
The Ratio of minimum to maximum transmission is 0.8795.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Green-brown
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       Block
_exptl_crystal_F_000             1410
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.294
_refine_diff_density_min         -2.065
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         12205
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1744P)^2^+13.9890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2567
_refine_ls_wR_factor_ref         0.2768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10040
_reflns_number_total             12205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4019508_si_002_1.cif
_cod_data_source_block           104
_cod_original_formula_sum        'C53.20 H72.79 B3 F12 Fe2 N14 O5'
_cod_database_code               4336833
_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
2. Restrained distances
 F9B-F10B
 2.2 with sigma of 0.02
 F11A-F9A
 2.27 with sigma of 0.02
 F11A-F9A
 2.5 with sigma of 0.02
 F10A-F9A
 2.26 with sigma of 0.04
 F10B-F11B
 2.26 with sigma of 0.04
 F10A-F9A
 2.26 with sigma of 0.04
 F9B-F11B
 2.26 with sigma of 0.04
 F9A-F12A
 2.26 with sigma of 0.04
 F12B-F11B
 2.26 with sigma of 0.04
 F9B-F12B
 2.26 with sigma of 0.04
 F9B-F10B
 2.26 with sigma of 0.04
 F11B-F10B
 2.26 with sigma of 0.04
 O4-C47 \\sim O14B-C5B
 with sigma of 0.02
 N15B-C54B \\sim N15B-C53B
 with sigma of 0.02
 N13-C48 \\sim N15B-C54B \\sim N15B-C53B
 with sigma of 0.02
 F6-B2 \\sim F5-B2 \\sim F7-B2 \\sim F8A-B2 \\sim F8B-B2
 with sigma of 0.02
 N5-C21B \\sim N5-C21A
 with sigma of 0.02
 C12-C11 \\sim C22B-C21B \\sim C21A-C22A
 with sigma of 0.02
 N13-C47 \\sim N15B-C5B
 with sigma of 0.02
 N13-C48 \\sim N15B-C53B \\sim N15B-C54B
 with sigma of 0.02
 N13-C48 \\sim N15B-C54B \\sim N15B-C53B
 with sigma of 0.02
 F3-B1 \\sim F11A-B3A \\sim F10A-B3A \\sim F9A-B3A \\sim F12B-B3B 
\\sim F9B-B3B \\sim F10B-B3B \\sim F11B-
 B3B \\sim F12A-B3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C51) = Uanis(C52)
Uanis(C50) = Uanis(C51) = Uanis(C52)
Uanis(N14A) = Uanis(O14B)
Uanis(N15B) = Uanis(O5A) = Uanis(C5B)
Uanis(N15B) = Uanis(C53B) = Uanis(C54B)
Uanis(F8A) = Uanis(F8B) = Uanis(B2)
Uanis(F6) = Uanis(F7) = Uanis(F8B) = Uanis(F8A)
Uanis(F9A) = Uanis(B3A) = Uanis(B3B)
Uanis(F12A) = Uanis(F11B)
Uanis(F9A) = Uanis(F12A) = Uanis(B3A) = Uanis(B3B) = Uanis(F11B) = Uanis(F9B) 
= Uanis(F10B) = Uanis(F10A) = Uanis(F11A) = Uanis(F12B)
Uanis(F5) = Uanis(B3A) = Uanis(B3B) = Uanis(F11B) = Uanis(F10A) = Uanis(F10B) 
= Uanis(F11A) = Uanis(F9B) = Uanis(F12A) = Uanis(F12B) = Uanis(F9A)
Uanis(C21A) = Uanis(C21B) = Uanis(C22A)
Uanis(C21A) = Uanis(C21B) = Uanis(C22A) = Uanis(C22B)
Uanis(C33) = Uanis(C21B) = Uanis(C21A) = Uanis(C22A) = Uanis(C22B)
4. others
 Sof(C5B)=Sof(H5B)=Sof(C53B)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54B)=Sof(H54A)=
 Sof(H54B)=Sof(H54C)=Sof(N15B)=Sof(O14B)=1-FVAR(1)
 Sof(N14A)=Sof(O5A)=FVAR(1)
 Sof(F8B)=1-FVAR(2)
 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(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(4)
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=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), C21A(H21A,H21B),
 C21B(H21C,H21D), C23(H23A,H23B), C24(H24A,H24B), C32(H32A,H32B), C34(H34A,
 H34B), C42(H42A,H42B)
5.c Aromatic/amide H refined with riding coordinates:
 C5B(H5B), 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), C50(H50)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C33(H33A,
 H33B,H33C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C53B(H53A,H53B,H53C), C54B(H54A,H54B,H54C)
;
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.811
_shelx_res_checksum              74260
_shelxl_version_number           2013-3