Ligand Tailoring Toward an Air-Stable Iron(V) Nitrido Complex.
Keilwerth, Martin; Grunwald, Liam; Mao, Weiqing; Heinemann, Frank W.; Sutter, Jörg; Bill, Eckhard; Meyer, Karsten; Journal of the American Chemical Society 143 (2021) 1458–1465; doi:10.1021/jacs.0c11141

data_4135595
_publ_section_title
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 Ligand Tailoring Toward an Air-Stable Iron(V) Nitrido Complex.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1458
_journal_page_last               1465
_journal_paper_doi               10.1021/jacs.0c11141
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'C39 H45 Fe N8, F6 P, 0.93(C6 H6)'
_chemical_formula_sum            'C44.56 H50.56 F6 Fe N8 P'
_chemical_formula_weight         899.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.670(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   46.429(2)
_cell_length_b                   16.3087(7)
_cell_length_c                   23.2775(13)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.40
_cell_volume                     17589.5(15)
_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-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1347
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            194053
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.753
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0987 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.9218.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       platelet
_exptl_crystal_F_000             7503
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.078
_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     1164
_refine_ls_number_reflns         17984
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0549P)^2^+67.5152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11968
_reflns_number_total             17984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11141_si_002.cif
_cod_data_source_block           wm2008
_cod_database_code               4135595
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.924
_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. Uiso/Uaniso restraints and constraints
F31 \\sim F32 \\sim F33 \\sim F31A \\sim F32A \\sim F33A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206 \\sim C211 \\sim
C212 \\sim C213: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Same fragment restrains
{C201, C202, C203} sigma for 1-2: 0.02, 1-3: 0.04
as
{C211, C212, C213}
4. Others
 Sof(F31A)=Sof(F32A)=Sof(F33A)=1-FVAR(1)
 Sof(F31)=Sof(F32)=Sof(F33)=FVAR(1)
 Sof(C211)=Sof(H211)=Sof(C212)=Sof(H212)=Sof(C213)=Sof(H213)=1-FVAR(2)
 Sof(C201)=Sof(H201)=Sof(C202)=Sof(H202)=Sof(C203)=Sof(H203)=Sof(C204)=
 Sof(H204)=Sof(C205)=Sof(H205)=Sof(C206)=Sof(H206)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C9(H9A,H9B), C40(H40A,H40B), C44(H44A,H44B),
 C48(H48A,H48B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C11(H11), C12(H12), C15(H15), C17(H17),
 C24(H24), C26(H26), C33(H33), C35(H35), C42(H42), C43(H43), C46(H46), C47(H47),
  C50(H50), C51(H51), C54(H54), C56(H56), C63(H63), C65(H65), C72(H72),
 C74(H74), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105),
 C106(H106), C201(H201), C202(H202), C203(H203), C204(H204), C205(H205),
 C206(H206), C211(H211), C212(H212), C213(H213)
5.c Fitted hexagon refined as free rotating group:
 C201(C202,C203,C204,C205,C206)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C)
;
_shelx_res_checksum              55116
_shelx_hkl_checksum              69624
_olex2_submission_special_instructions 'No special instructions were received'