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_4135597
_publ_section_title
;
 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
'2(C44 H55 Fe N9), B F4, 3(C24 H20 B), 1.5(C2 H3 N), C4 H10 O'
_chemical_formula_sum            'C167 H184.5 B4 F4 Fe2 N19.5 O'
_chemical_formula_weight         2711.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.598(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.570(2)
_cell_length_b                   18.1960(10)
_cell_length_c                   47.439(9)
_cell_measurement_reflns_used    343
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     14996(3)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_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    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 0.50 \% and 100 sec per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1299
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            177728
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.836
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.06 (Bruker AXS, 2002) was used for absorption correction.
R(int) was 0.1424 before and 0.0558 after correction.
The Ratio of minimum to maximum transmission is 0.8921.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       plate
_exptl_crystal_F_000             5756
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2066
_refine_ls_number_reflns         28363
_refine_ls_number_restraints     2615
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0845P)^2^+13.1061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15380
_reflns_number_total             28363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11141_si_002.cif
_cod_data_source_block           cv0901
_cod_original_formula_sum        'C167 H184.50 B4 F4 Fe2 N19.50 O'
_cod_database_code               4135597
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.913
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups
2. Restrained distances
 C301-C302 = C304-C305 = C314-C315
 1.54 with sigma of 0.02
 C302-O303 = C304-O303 = C314-O313
 1.48 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C58 \\sim C59 \\sim C58A \\sim C59A \\sim C60 \\sim C61 \\sim C62 \\sim C63
\\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C60A \\sim C61A \\sim
C62A \\sim C63A \\sim C64A \\sim C65A \\sim C66A \\sim C67A \\sim C68A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C47 \\sim N11 \\sim C48 \\sim C49 \\sim N12 \\sim C47A \\sim N11A \\sim C48A
\\sim C49A \\sim N12A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
B1 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim B1A \\sim F11A \\sim F12A
\\sim F13A \\sim F14A: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C301 \\sim C302 \\sim O303 \\sim C304 \\sim C305 \\sim C311 \\sim C312 \\sim
O313 \\sim C314 \\sim C315: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C37) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C66A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C47) \\sim Ueq, Uanis(C47A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(B1) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13)
\\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(B1A) \\sim Ueq, Uanis(F11A) \\sim Ueq,
Uanis(F12A) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C301) \\sim Ueq, Uanis(C302) \\sim Ueq, Uanis(O303) \\sim Ueq,
Uanis(C304) \\sim Ueq, Uanis(C305) \\sim Ueq, Uanis(C311) \\sim Ueq,
Uanis(C312) \\sim Ueq, Uanis(O313) \\sim Ueq, Uanis(C314) \\sim Ueq,
Uanis(C315) \\sim Ueq, Uanis(N400) \\sim Ueq, Uanis(C401) \\sim Ueq,
Uanis(C402) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{B1, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as
{B1A, F11A, F12A, F13A, F14A}
{C311, C312, O313, C314, C315} sigma for 1-2: 0.02, 1-3: 0.04
as
{C301, C302, O303, C304, C305}
6. Others
 Sof(B1A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=1-FVAR(1)
 Sof(B1)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=FVAR(1)
 Sof(C47A)=Sof(N11A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(N12A)=
 Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C58A)=Sof(H58A)=
 Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(C61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=
 Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(C66A)=Sof(H66D)=Sof(H66E)=Sof(H66F)=
 Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C68A)=Sof(H68D)=Sof(H68E)=
 Sof(H68F)=Sof(C311)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C312)=Sof(H31G)=
 Sof(H31H)=Sof(O313)=Sof(C314)=Sof(H31I)=Sof(H31J)=Sof(C315)=Sof(H31K)=
 Sof(H31L)=Sof(H31M)=1-FVAR(2)
 Sof(C47)=Sof(N11)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(N12)=Sof(H45A)=
 Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=
 Sof(C60)=Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(C64)=Sof(H64)=Sof(C65)=
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C301)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(C302)=Sof(H30D)=Sof(H30E)=Sof(O303)=Sof(C304)=Sof(H30F)=Sof(H30G)=
 Sof(C305)=Sof(H30H)=Sof(H30I)=Sof(H30J)=FVAR(2)
 Fixed Sof: N400(0.5) C401(0.5) C402(0.5) H40D(0.5) H40E(0.5) H40F(0.5)
7.a Riding coordinates:
 N8(H8), N17(H17)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C12(H12A,
 H12B), C45(H45A,H45B), C45(H45C,H45D), C46(H46A,H46B), C46A(H46C,H46D),
 C50(H50A,H50B), C51(H51A,H51B), C55(H55A,H55B), C56(H56A,H56B), C302(H30D,
 H30E), C304(H30F,H30G), C312(H31G,H31H), C314(H31I,H31J)
7.c 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), C48(H48), C49(H49), C48A(H48A),
 C49A(H49A), C53(H53), C54(H54), C58(H58), C59(H59), C58A(H58A), C59A(H59A),
 C62(H62), C64(H64), C62A(H62A), C64A(H64A), C71(H71), C73(H73), C80(H80),
 C82(H82), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97),
  C98(H98), C99(H99), C100(H100), C102(H102), C103(H103), C104(H104),
 C105(H105), C106(H106), C108(H108), C109(H109), C110(H110), C111(H111),
 C112(H112), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C120(H120), C121(H121), C122(H122), C123(H123), C124(H124), C126(H126),
 C127(H127), C128(H128), C129(H129), C130(H130), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136), C138(H138), C139(H139), C140(H140),
 C141(H141), C142(H142), C144(H144), C145(H145), C146(H146), C147(H147),
 C148(H148), C150(H150), C151(H151), C152(H152), C153(H153), C154(H154),
 C156(H156), C157(H157), C158(H158), C159(H159), C160(H160)
7.d 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), C66(H66A,H66B,H66C),
 C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C66A(H66D,H66E,H66F), C67A(H67D,H67E,
 H67F), C68A(H68D,H68E,H68F), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C),
 C77(H77A,H77B,H77C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,
 H86C), C88(H88A,H88B,H88C), C202(H20A,H20B,H20C), C301(H30A,H30B,H30C),
 C305(H30H,H30I,H30J), C311(H31D,H31E,H31F), C315(H31K,H31L,H31M), C402(H40D,
 H40E,H40F)
;
_shelx_res_checksum              6726
_shelx_hkl_checksum              2186
_olex2_submission_special_instructions 'No special instructions were received'