Functional Mononitrosyl Diiron(II) Complex Mediates the Reduction of NO to N<sub>2</sub>O with Relevance for Flavodiiron NO Reductases.
Jana, Manish; Pal, Nabhendu; White, Corey J.; Kupper, Claudia; Meyer, Franc; Lehnert, Nicolai; Majumdar, Amit; Journal of the American Chemical Society 139 (2017) 14380–14383; doi:10.1021/jacs.7b08855

data_4131689
_publ_section_title
;
 Functional Mononitrosyl Diiron(II) Complex Mediates the Reduction of NO
 to N<sub>2</sub>O with Relevance for Flavodiiron NO Reductases.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14380
_journal_page_last               14383
_journal_paper_doi               10.1021/jacs.7b08855
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C52 H70 Fe2 N14 O5, 3(B F4)'
_chemical_formula_sum            'C52 H70 B3 F12 Fe2 N14 O5'
_chemical_formula_weight         1343.35
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                85.169(5)
_cell_angle_beta                 85.229(6)
_cell_angle_gamma                70.914(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6141(17)
_cell_length_b                   16.5066(18)
_cell_length_c                   17.648(3)
_cell_measurement_reflns_used    4218
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.32
_cell_volume                     3180.4(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker-Axs,2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker D8VENTURE with PHOTON II Detector'
_diffrn_measurement_method       'phi, omega and kappa scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.1658
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21347
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.116
_diffrn_reflns_theta_min         2.249
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1460 before and 0.0746 after correction.
The Ratio of minimum to maximum transmission is 0.8207.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.147
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         10864
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1718
_refine_ls_R_factor_gt           0.1082
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2867
_refine_ls_wR_factor_ref         0.3495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5781
_reflns_number_total             10864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08855_si_003.cif
_cod_data_source_block           Mononitrosyl1
_cod_original_cell_volume        3180.5(8)
_cod_database_code               4131689
_shelxl_version_number           2014-3
_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
 N13-C48 \\sim N13-C49B \\sim N13-C49A
 with sigma of 0.02
 N14-C51 \\sim N14-C52B \\sim N14-C52A
 with sigma of 0.02
 F5-B2 \\sim F6-B2 \\sim F8A-B2 \\sim F8B-B2 \\sim F7A-B2 \\sim F7B-B2
 with sigma of 0.02
 F9-B3 \\sim F11B-B3 \\sim F11A-B3 \\sim F12B-B3 \\sim F12A-B3 \\sim F10-B3
 with sigma of 0.02
 F3-B1 \\sim F2A-B1 \\sim F4B-B1 \\sim F1-B1 \\sim F4A-B1 \\sim F2B-B1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C51) = Uanis(C52B) = Uanis(C52A)
Uanis(C48) = Uanis(C49B) = Uanis(C49A)
Uanis(F5) = Uanis(F8B) = Uanis(F8A) = Uanis(F7A) = Uanis(F7B)
Uanis(F10) = Uanis(F12A) = Uanis(F12B) = Uanis(F11A) = Uanis(F11B)
Uanis(F3) = Uanis(F1) = Uanis(F2B) = Uanis(F2A) = Uanis(F4A) = Uanis(F4B)
Uanis(Fe1) = Uanis(N12)
4. Others
 Sof(C49B)=Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(C52B)=Sof(H52D)=Sof(H52E)=
 Sof(H52F)=1-FVAR(1)
 Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C52A)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=FVAR(1)
 Sof(F2B)=Sof(F4B)=Sof(F7B)=Sof(F8B)=Sof(F11B)=Sof(F12B)=1-FVAR(2)
 Sof(F2A)=Sof(F4A)=Sof(F7A)=Sof(F8A)=Sof(F11A)=Sof(F12A)=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), C50(H50)
5.d 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),
 C49A(H49A,H49B,H49C), C49B(H49D,H49E,H49F), C51(H51A,H51B,H51C), C52A(H52A,
 H52B,H52C), C52B(H52D,H52E,H52F)
;
_shelx_res_checksum              66210
_shelx_hkl_checksum              2309
_shelx_fab_checksum              89630
_olex2_submission_special_instructions 'No special instructions were received'