Fe-Catalyzed Conversion of N<sub>2</sub> to N(SiMe<sub>3</sub>)<sub>3</sub> via an Fe-Hydrazido Resting State.
Piascik, Adam D.; Li, Ruohao; Wilkinson, Harry J.; Green, Jennifer C.; Ashley, Andrew E.; Journal of the American Chemical Society 140 (2018) 10691–10694; doi:10.1021/jacs.8b06999

data_4132858
_publ_section_title
;
 Fe-Catalyzed Conversion of N<sub>2</sub> to
 N(SiMe<sub>3</sub>)<sub>3</sub> via an Fe-Hydrazido Resting State.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10691
_journal_page_last               10694
_journal_paper_doi               10.1021/jacs.8b06999
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C29 H75 Fe N2 P4 Si3, C32 H12 B F24'
_chemical_formula_sum            'C61 H87 B F24 Fe N2 P4 Si3'
_chemical_formula_weight         1579.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2018-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                94.728(4)
_cell_angle_beta                 105.621(5)
_cell_angle_gamma                95.118(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9577(6)
_cell_length_b                   16.1735(5)
_cell_length_c                   20.8289(13)
_cell_measurement_reflns_used    4911
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      26.4920
_cell_measurement_theta_min      2.7950
_cell_volume                     3840.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -40.00  54.00   1.00   14.48    --  -13.18  77.00-120.00   94
  2  \w    -79.00  13.00   1.00   14.48    --  -13.18 -77.00 120.00   92
  3  \w     -2.00  82.00   1.00   14.48    --   14.43  57.00  30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0208946000
_diffrn_orient_matrix_UB_12      -0.0425765000
_diffrn_orient_matrix_UB_13      -0.0005703000
_diffrn_orient_matrix_UB_21      0.0145659000
_diffrn_orient_matrix_UB_22      -0.0095954000
_diffrn_orient_matrix_UB_23      -0.0303901000
_diffrn_orient_matrix_UB_31      0.0565393000
_diffrn_orient_matrix_UB_32      -0.0076222000
_diffrn_orient_matrix_UB_33      0.0184935000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1397
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15931
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         2.284
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.377
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         15931
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.0790
_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^)+(0.1097P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8944
_reflns_number_total             15931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06999_si_002.cif
_cod_data_source_block           ash1809
_cod_database_code               4132858
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C61 H83 B F24 Fe N2 P4 Si3'
_chemical_oxdiff_usercomment     AP-477
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7712(10)
 0.2288(10)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(F24) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F17)
\\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F22) \\sim Ueq,
Uanis(F2A) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F3A)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F11A) \\sim Ueq,
Uanis(F5A) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F4A)
\\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F19) \\sim Ueq,
Uanis(F23) \\sim Ueq, Uanis(F12B) \\sim Ueq, Uanis(F11B) \\sim Ueq, Uanis(F10B)
\\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F3B) \\sim Ueq,
Uanis(F5B) \\sim Ueq, Uanis(F4B) \\sim Ueq, Uanis(F6B) \\sim Ueq, Uanis(F15A)
\\sim Ueq, Uanis(F14A) \\sim Ueq, Uanis(F13B) \\sim Ueq, Uanis(F14B) \\sim Ueq,
Uanis(F15B) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Fixed Sof: F6A(0.66667) F12A(0.66667) F2A(0.66667) F3A(0.66667) F10A(0.66667)
 F11A(0.66667) F5A(0.66667) F1A(0.66667) F13A(0.75) F4A(0.66667) F12B(0.33333)
 F11B(0.33333) F10B(0.33333) H9AA(0.5) H9AB(0.5) H9BC(0.5) H9BD(0.5) C10B(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) C10A(0.5) H10D(0.5) H10E(0.5) H10F(0.5)
 F1B(0.33333) F2B(0.33333) F3B(0.33333) F5B(0.33333) F4B(0.33333) F6B(0.33333)
 F15A(0.75) F14A(0.75) F13B(0.25) F14B(0.25) F15B(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C16(H16A,H16B), C15(H15A,H15B), C11(H11A,H11B),
 C13(H13A,H13B), C17(H17A,H17B), C7(H7A,H7B), C19(H19A,H19B), C1(H1A,H1B),
 C6(H6A,H6B), C9(H9AA,H9AB), C9(H9BC,H9BD)
5.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C39(H39), C49(H49), C33(H33), C43(H43), C59(H59), C31(H31),
 C41(H41), C55(H55), C35(H35), C57(H57), C47(H47)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C22(H22A,H22B,H22C), C4(H4A,H4B,H4C), C12(H12A,H12B,
 H12C), C26(H26A,H26B,H26C), C18(H18A,H18B,H18C), C29(H29A,H29B,H29C), C14(H14A,
 H14B,H14C), C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C2(H2A,H2B,H2C), C25(H25A,
 H25B,H25C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C),
 C21(H21A,H21B,H21C), C10B(H10A,H10B,H10C), C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              84972
_shelx_hkl_checksum              67788
_olex2_date_sample_data_collection 2018-02-22
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.062
_oxdiff_exptl_absorpt_empirical_full_min 0.920