Electrophile-promoted Fe-to-N<sub>2</sub> hydride migration in highly reduced Fe(N<sub>2</sub>)(H) complexes.
Deegan, Meaghan M.; Peters, Jonas C.; Chemical science 9 (2018) 6264–6270; doi:10.1039/c8sc02380h

data_1549633
_publ_section_title
;
 Electrophile-promoted Fe-to-N<sub>2</sub> hydride migration in highly
 reduced Fe(N<sub>2</sub>)(H) complexes.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              6264
_journal_page_last               6270
_journal_paper_doi               10.1039/c8sc02380h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety
'C41 H64 B Fe N P3, C32 H12 B F24, 1.24(C5 H12)'
_chemical_formula_sum            'C79.22 H90.92 B2 F24 Fe N P3'
_chemical_formula_weight         1683.40
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-30 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.8630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.577(3)
_cell_length_b                   15.5573(16)
_cell_length_c                   38.526(4)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.39
_cell_volume                     16232(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            249578
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.670
_diffrn_reflns_theta_min         1.415
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0595 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.9209. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       plate
_exptl_crystal_F_000             6962
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.549
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2297
_refine_ls_number_reflns         34202
_refine_ls_number_restraints     783
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+64.7430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.1984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25101
_reflns_number_total             34202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02380h2.cif
_cod_data_source_block           tBuNCB-Hcation
_cod_depositor_comments
'Adding full bibliography for 1549629--1549633.cif.'
_cod_database_code               1549633
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.916
_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
C163 \\sim C165 \\sim C158 \\sim C161 \\sim C159 \\sim C157 \\sim C166 \\sim
C164 \\sim C162 \\sim C160: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
F8A \\sim F7A \\sim F9A \\sim C97 \\sim F7B \\sim F8B \\sim F9B: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
F24A \\sim F22A \\sim C114 \\sim F23A \\sim F24B \\sim F23B \\sim F22B: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
F41A \\sim F40A \\sim F42A \\sim C138 \\sim F41B \\sim F40B \\sim F42B: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
F31A \\sim F32A \\sim F33A \\sim C129 \\sim F32B \\sim F31B \\sim F33B: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
F5A \\sim F4A \\sim F6A \\sim C89 \\sim F5B \\sim F6B \\sim F4B: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C147 \\sim C148 \\sim C149 \\sim C150 \\sim C151: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C163, C165, C158, C161, C159, C157, C166, C164, C162, C160
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F8A, F7A, F9A, C97, F7B, F8B, F9B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F24A, F22A, C114, F23A, F24B, F23B, F22B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F41A, F40A, F42A, C138, F41B, F40B, F42B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F35A, F36A, F34A, C130, F34B, F35B, F36B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F31A, F32A, F33A, C129, F32B, F31B, F33B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F25A, F27A, F26A, C121, F26B, F27B, F25B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F5A, F4A, F6A, C89, F5B, F6B, F4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C151, C150, C149, C148, C147
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F7B)=Sof(F8B)=Sof(F9B)=1-FVAR(1)
 Sof(F8A)=Sof(F7A)=Sof(F9A)=FVAR(1)
 Sof(F5B)=Sof(F6B)=Sof(F4B)=1-FVAR(2)
 Sof(F5A)=Sof(F4A)=Sof(F6A)=FVAR(2)
 Sof(F34B)=Sof(F35B)=Sof(F36B)=1-FVAR(3)
 Sof(F35A)=Sof(F36A)=Sof(F34A)=FVAR(3)
 Sof(F26B)=Sof(F27B)=Sof(F25B)=1-FVAR(4)
 Sof(F25A)=Sof(F27A)=Sof(F26A)=FVAR(4)
 Sof(F24B)=Sof(F23B)=Sof(F22B)=1-FVAR(5)
 Sof(F24A)=Sof(F22A)=Sof(F23A)=FVAR(5)
 Sof(C158)=Sof(H15R)=Sof(H15S)=Sof(H15T)=Sof(C166)=Sof(H16K)=Sof(H16L)=
 Sof(H16M)=Sof(C164)=Sof(H16N)=Sof(H16O)=Sof(C162)=Sof(H16P)=Sof(H16Q)=
 Sof(C160)=Sof(H16R)=Sof(H16S)=1-FVAR(6)
 Sof(C163)=Sof(H16D)=Sof(H16E)=Sof(C165)=Sof(H16F)=Sof(H16G)=Sof(H16H)=
 Sof(C161)=Sof(H16I)=Sof(H16J)=Sof(C159)=Sof(H15M)=Sof(H15N)=Sof(C157)=
 Sof(H15O)=Sof(H15P)=Sof(H15Q)=FVAR(6)
 Sof(F41B)=Sof(F40B)=Sof(F42B)=1-FVAR(7)
 Sof(F41A)=Sof(F40A)=Sof(F42A)=FVAR(7)
 Sof(F32B)=Sof(F31B)=Sof(F33B)=1-FVAR(8)
 Sof(F31A)=Sof(F32A)=Sof(F33A)=FVAR(8)
 Sof(C150)=Sof(H15U)=Sof(H15V)=Sof(C149)=Sof(H14D)=Sof(H14E)=Sof(C151)=
 Sof(H15W)=Sof(H15X)=Sof(H15Y)=Sof(C148)=Sof(H14F)=Sof(H14G)=Sof(C147)=
 Sof(H14H)=Sof(H14I)=Sof(H14J)=FVAR(9)
5.a Ternary CH refined with riding coordinates:
 C39(H39), C56(H56), C36(H36), C12(H12), C15(H15), C53(H53), C68(H68),
 C80(H80), C77(H77), C27(H27), C24(H24), C65(H65)
5.b Secondary CH2 refined with riding coordinates:
 C154(H15A,H15B), C155(H15C,H15D), C153(H15E,H15F), C163(H16D,H16E), C161(H16I,
 H16J), C159(H15M,H15N), C164(H16N,H16O), C162(H16P,H16Q), C160(H16R,H16S),
 C150(H15U,H15V), C149(H14D,H14E), C148(H14F,H14G)
5.c Aromatic/amide H refined with riding coordinates:
 C120(H120), C144(H144), C19(H19), C94(H94), C116(H116), C134(H134), C34(H34),
 C92(H92), C104(H104), C118(H118), C75(H75), C31(H31), C48(H48), C63(H63),
 C102(H102), C136(H136), C74(H74), C33(H33), C96(H96), C50(H50), C88(H88),
 C73(H73), C132(H132), C22(H22), C108(H108), C21(H21), C51(H51), C128(H128),
 C10(H10), C142(H142), C72(H72), C20(H20), C124(H124), C140(H140), C32(H32),
 C60(H60), C7(H7), C62(H62), C100(H100), C86(H86), C84(H84), C49(H49),
 C112(H112), C61(H61), C9(H9), C110(H110), C126(H126), C8(H8)
5.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C58(H58A,H58B,H58C), C44(H44A,H44B,H44C), C3(H3A,H3B,
 H3C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C37(H37A,H37B,H37C), C45(H45A,
 H45B,H45C), C81(H81A,H81B,H81C), C29(H29A,H29B,H29C), C54(H54A,H54B,H54C),
 C41(H41A,H41B,H41C), C38(H38A,H38B,H38C), C5(H5A,H5B,H5C), C57(H57A,H57B,H57C),
  C26(H26A,H26B,H26C), C16(H16A,H16B,H16C), C67(H67A,H67B,H67C), C55(H55A,H55B,
 H55C), C79(H79A,H79B,H79C), C69(H69A,H69B,H69C), C82(H82A,H82B,H82C), C28(H28A,
 H28B,H28C), C70(H70A,H70B,H70C), C17(H17A,H17B,H17C), C46(H46A,H46B,H46C),
 C78(H78A,H78B,H78C), C66(H66A,H66B,H66C), C156(H15G,H15H,H15I), C152(H15J,H15K,
 H15L), C4(H4A,H4B,H4C), C165(H16F,H16G,H16H), C158(H15R,H15S,H15T), C157(H15O,
 H15P,H15Q), C166(H16K,H16L,H16M), C25(H25A,H25B,H25C), C151(H15W,H15X,H15Y),
 C147(H14H,H14I,H14J)
;
_shelx_res_checksum              16668
_olex2_submission_special_instructions 'No special instructions were received'