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_4133701
_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_formula_moiety         'C44 H54 Fe N8, 2(B F4), 2.73(C2 H3 N)'
_chemical_formula_sum            'C49.46 H62.18 B2 F8 Fe N10.73'
_chemical_formula_weight         1036.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.217(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2667(9)
_cell_length_b                   11.2967(6)
_cell_length_c                   24.8121(12)
_cell_measurement_reflns_used    9443
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.58
_cell_measurement_theta_min      2.19
_cell_volume                     5211.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            70739
_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         27.877
_diffrn_reflns_theta_min         2.110
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0643 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.8764.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.053(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         12308
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0713P)^2^+9.2100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                11099
_reflns_number_total             12308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08053_si_002.cif
_cod_data_source_block           mk1701
_cod_database_code               4133701
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.880
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.947(19)
 0.053(19)
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. Uiso/Uaniso restraints and constraints
F31 \\sim F32 \\sim F33 \\sim F34: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(B3) \\sim Ueq, Uanis(F31) \\sim Ueq, Uanis(F32) \\sim Ueq, Uanis(F33)
\\sim Ueq, Uanis(F34) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Same fragment restrains
{B1, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as
{B3, F31, F32, F33, F34}
5. Others
 1*[Sof(B1)+Sof(F11)+Sof(F12)+Sof(F13)+Sof(F14)]+1*[Sof(B2)+Sof(F21)+Sof(F22)+
 Sof(F23)+Sof(F24)]+1*[Sof(N200)+Sof(C201)+Sof(C202)+Sof(H20A)+Sof(H20B)+
 Sof(H20C)+Sof(N300)+Sof(C301)+Sof(C302)+Sof(H30A)+Sof(H30B)+Sof(H30C)+Sof(B3)+
 Sof(F31)+Sof(F32)+Sof(F33)+Sof(F34)]=2 with esd of 0.001
 Sof(B1)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=FVAR(1)
 Sof(B2)=Sof(F21)=Sof(F22)=Sof(F23)=Sof(F24)=FVAR(2)
 Sof(N200)=Sof(C201)=Sof(C202)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(N300)=
 Sof(C301)=Sof(C302)=Sof(H30A)=Sof(H30B)=Sof(H30C)=1-FVAR(3)
 Sof(B3)=Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C12(H12A,
 H12B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C14(H14), C15(H15), C18(H18), C20(H20),
 C27(H27), C29(H29), C36(H36), C38(H38)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C102(H10A,H10B,H10C),
 C202(H20A,H20B,H20C), C302(H30A,H30B,H30C)
;
_shelx_res_checksum              97064
_shelx_hkl_checksum              39934
_olex2_submission_special_instructions 'No special instructions were received'