A Series of Iron Nitrosyl Complexes {Fe-NO}<sup>6-9</sup> and a Fleeting {Fe-NO}<sup>10</sup> Intermediate en Route to a Metalacyclic Iron Nitrosoalkane.
Keilwerth, Martin; Hohenberger, Johannes; Heinemann, Frank W.; Sutter, Jörg; Scheurer, Andreas; Fang, Huayi; Bill, Eckhard; Neese, Frank; Ye, Shengfa; Meyer, Karsten; Journal of the American Chemical Society 141 (2019) 17217–17235; doi:10.1021/jacs.9b08053

data_4133705
_publ_section_title
;
 A Series of Iron Nitrosyl Complexes {Fe-NO}<sup>6-9</sup> and a Fleeting
 {Fe-NO}<sup>10</sup> Intermediate en Route to a Metalacyclic Iron
 Nitrosoalkane.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17217
_journal_page_last               17235
_journal_paper_doi               10.1021/jacs.9b08053
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety
'3(C14 H17 Fe0.33 N2.67 O0.33), B F4, 2.67(C H Cl3)'
_chemical_formula_sum            'C44.67 H53.67 B Cl8 F4 Fe N8 O'
_chemical_formula_weight         1144.88
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   18.6911(8)
_cell_length_b                   18.6911(8)
_cell_length_c                   39.1469(19)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.66
_cell_measurement_theta_min      2.18
_cell_volume                     11844.0(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_collection       'Bruker APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa ImuS Duo Photon II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS high brilliance micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            82495
_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         27.101
_diffrn_reflns_theta_min         2.179
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0748 after correction.
The Ratio of minimum to maximum transmission is 0.8715.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       plate
_exptl_crystal_F_000             5298
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         11632
_refine_ls_number_restraints     665
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0980P)^2^+53.4544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2002
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8696
_reflns_number_total             11632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08053_si_002.cif
_cod_data_source_block           mk1901
_cod_original_cell_volume        11844.0(12)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4133705
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.896
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80(4)
 0.20(4)
2. 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
3. Restrained distances
 N9-C29 \\sim N9-C29A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C30-N10 \\sim C30A-N10A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N9 \\sim C29 \\sim C30 \\sim N10 \\sim C31 \\sim N11 \\sim C32 \\sim C33 \\sim
C29A \\sim C30A \\sim N10A \\sim C31A \\sim N11A \\sim C29 \\sim C30 \\sim N10
\\sim C31 \\sim N11 \\sim C32 \\sim C33 \\sim C29A \\sim C30A \\sim N10A \\sim
C31A \\sim N11A \\sim C32A \\sim C33A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim
C42 \\sim C34A \\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39A \\sim
C40A \\sim C41A \\sim C42A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Cl11 \\sim Cl12 \\sim Cl13 \\sim Cl14 \\sim Cl15 \\sim Cl16: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Cl21 \\sim Cl22 \\sim Cl23 \\sim Cl24 \\sim Cl25 \\sim Cl26: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40A) \\sim Ueq, Uanis(C41A) \\sim Ueq, Uanis(C42A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl11) \\sim Ueq, Uanis(Cl12) \\sim Ueq, Uanis(Cl13) \\sim Ueq,
Uanis(Cl14) \\sim Ueq, Uanis(Cl15) \\sim Ueq, Uanis(Cl16) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
5. Same fragment restrains
{C1, C2, N2, C3, N3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C29, C30, N10, C31, N11, C32, C33}
{C1, C2, N2, C3, N3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C29A, C30A, N10A, C31A, N11A, C32A, C33A}
6. Others
 Sof(H10A)=Sof(Cl14)=Sof(Cl15)=Sof(Cl16)=1-FVAR(1)
 Sof(H100)=Sof(Cl11)=Sof(Cl12)=Sof(Cl13)=FVAR(1)
 Sof(H20A)=Sof(Cl24)=Sof(Cl25)=Sof(Cl26)=1-FVAR(2)
 Sof(H200)=Sof(Cl21)=Sof(Cl22)=Sof(Cl23)=FVAR(2)
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(N10A)=
 Sof(C31A)=Sof(N11A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=
 Sof(C35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41A)=Sof(H41D)=Sof(H41E)=
 Sof(H41F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(3)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(N10)=Sof(C31)=
 Sof(N11)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(C35)=Sof(C36)=
 Sof(H36)=Sof(C37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C100(H100), C100(H10A), C200(H200), C200(H20A), C300(H300), C400(H400)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C15(H15A,H15B), C16(H16A,H16B), C29(H29A,H29B),
 C30(H30A,H30B), C29A(H29C,H29D), C30A(H30C,H30D)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C10(H10), C18(H18), C19(H19), C22(H22), C24(H24),
 C32(H32), C33(H33), C32A(H32A), C33A(H33A), C36(H36), C38(H38), C36A(H36A),
 C38A(H38A)
7.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C40A(H40D,H40E,H40F), C41A(H41D,H41E,H41F),
 C42A(H42D,H42E,H42F)
;
_shelx_res_checksum              63101
_shelx_hkl_checksum              42736
_olex2_submission_special_instructions 'No special instructions were received'