Functional Models for the Mono- and Di-nitrosyl Intermediates of FNORs: Semireduction versus Superreduction of NO.
Jana, Manish; White, Corey J.; Pal, Nabhendu; Demeshko, Serhiy; Kupper, Claudia; Meyer, Franc; Lehnert, Nicolai; Majumdar, Amit; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13795

data_4134567
_publ_section_title
;
 Functional Models for the Mono- and Di-nitrosyl Intermediates of FNORs:
 Semireduction versus Superreduction of NO.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13795
_journal_year                    2020
_chemical_formula_moiety         'C52 H71 Fe2 N13 O5, C3 H7 N O, 3(B F4)'
_chemical_formula_sum            'C55 H78 B3 F12 Fe2 N14 O6'
_chemical_formula_weight         1403.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                85.673(5)
_cell_angle_beta                 84.727(5)
_cell_angle_gamma                69.969(4)
_cell_formula_units_Z            2
_cell_length_a                   11.489(4)
_cell_length_b                   16.691(6)
_cell_length_c                   17.688(6)
_cell_measurement_reflns_used    3188
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.41
_cell_measurement_theta_min      2.15
_cell_volume                     3169.7(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.7-1 (Bruker-Axs,2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_unetI/netI     0.1303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.568
_diffrn_reflns_theta_min         1.157
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1574 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.7931.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0037(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         11764
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.0786
_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^)+(0.0936P)^2^+6.1955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6537
_reflns_number_total             11764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13795_si_002.cif
_cod_data_source_block           mixedvalence
_cod_original_cell_volume        3169.8(18)
_cod_database_code               4134567
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.888
_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
 N14-O6B
 2.3 with sigma of 0.04
 N13B-C52B \\sim N13B-C51B \\sim N13A-C51A \\sim N13A-C52A
 with sigma of 0.02
 N13B-C50B \\sim N13A-C50A
 with sigma of 0.02
 O5-C50A \\sim O5-C50B
 with sigma of 0.02
 N14-C53A \\sim N14-C53B \\sim N14-C54B \\sim N14-C54A
 with sigma of 0.02
 N14-C55B \\sim N14-C55B
 with sigma of 0.02
 O6A-C55A \\sim O6B-C55B
 with sigma of 0.02
 N14-C55A \\sim N14-C55B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C49) = Uanis(C48)
Uanis(O5) = Uanis(C50A) = Uanis(C50B) = Uanis(C51A) = Uanis(C51B) = Uanis(N13A)
= Uanis(N13B) = Uanis(C52A) = Uanis(C52B)
Uanis(F6) = Uanis(F5)
Uanis(F8A) = Uanis(F8B)
Uanis(F11A) = Uanis(F11B) = Uanis(F12A) = Uanis(F12B) = Uanis(F10) = Uanis(F9)
Uanis(F2) = Uanis(F1A) = Uanis(F1B) = Uanis(F3A) = Uanis(F3B) = Uanis(F4)
Uanis(N14) = Uanis(C53A) = Uanis(C53B) = Uanis(C54B) = Uanis(C54A) =
Uanis(C55A) = Uanis(C55B) = Uanis(O6B) = Uanis(O6A)
4. Others
 Sof(C50B)=Sof(H50B)=Sof(C51B)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52B)=
 Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(N13B)=Sof(C53B)=Sof(H53D)=Sof(H53E)=
 Sof(H53F)=Sof(C54B)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C55B)=Sof(H55B)=Sof(O6B)=
 1-FVAR(1)
 Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52A)=
 Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(N13A)=Sof(C53A)=Sof(H53A)=Sof(H53B)=
 Sof(H53C)=Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C55A)=Sof(H55A)=Sof(O6A)=
 FVAR(1)
 Sof(F11B)=Sof(F12B)=Sof(F1B)=Sof(F3B)=Sof(F8B)=1-FVAR(2)
 Sof(F11A)=Sof(F12A)=Sof(F1A)=Sof(F3A)=Sof(F8A)=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 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), C50A(H50A), C50B(H50B), C55A(H55A), C55B(H55B)
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), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C51A(H51A,H51B,H51C), C51B(H51D,H51E,H51F), C52A(H52A,H52B,H52C),
 C52B(H52D,H52E,H52F), C53A(H53A,H53B,H53C), C53B(H53D,H53E,H53F), C54A(H54A,
 H54B,H54C), C54B(H54D,H54E,H54F)
;
_shelx_res_checksum              84449
_shelx_hkl_checksum              58534
_olex2_submission_special_instructions 'No special instructions were received'