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_4336834
_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(C3 H7 N O), 3(B F4)'
_chemical_formula_sum            'C58 H85 B3 F12 Fe2 N16 O8'
_chemical_formula_weight         1506.54
_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             2013-06-11
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                68.9001(3)
_cell_angle_beta                 72.3877(4)
_cell_angle_gamma                75.8563(4)
_cell_formula_units_Z            2
_cell_length_a                   13.0188(4)
_cell_length_b                   15.2668(4)
_cell_length_c                   20.2175(5)
_cell_measurement_reflns_used    ****
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.21
_cell_volume                     3531.51(17)
_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      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0215
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58035
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.689
_diffrn_reflns_theta_min         1.527
_diffrn_source                   'Fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6555
_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    1.417
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.633
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         13399
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0932P)^2^+5.6829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11728
_reflns_number_total             13399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4019508_si_002_2.cif
_cod_data_source_block           112
_cod_database_code               4336834
_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
 F10A-F11A \\sim F11A-F12A \\sim F11B-F12B
 with sigma of 0.04
 B3-F9 \\sim B3-F10A \\sim B3-F11A \\sim B3-F12A \\sim B3-F10B \\sim B3-F11B 
\\sim B3-F12B
 with sigma of 0.02
 F10B-B3 \\sim F10A-B3 \\sim F9-B3 \\sim F11B-B3 \\sim F12A-B3 \\sim F12B-B3 
\\sim F11A-B3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4) = Uanis(O5)
Uanis(F10A) = Uanis(F10B) = Uanis(F12A) = Uanis(F12B) = Uanis(F11A) 
= Uanis(F11B) = Uanis(F9)
4. others
 Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(1)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(1)
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),
 C26(H26A,H26B), C27(H27A,H27B), C35(H35A,H35B), C37(H37A,H37B), C45(H45A,H45B)
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),
 C23(H23), C30(H30), C31(H31), C32(H32), C33(H33), C40(H40), C41(H41), C42(H42),
  C43(H43), C47(H47), C50(H50), C56(H56), C53(H53)
5.d Tetrahedral OH refined with riding coordinates:
 O5(H5)
5.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C36(H36A,H36B,H36C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C)
;
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.824
_shelx_res_checksum              28035
_shelxl_version_number           2013-3