Silane‒Allyl Coupling Reactions of Cp*(iPr2MeP)Fe(η3-C3H5) and Synthetic Access to the Hydrido‒Dinitrogen Complex Cp*(iPr2MeP)FeH(N2)
Smith, Patrick W.; Tilley, T. Don; Organometallics 34 (2015) 2134–; doi:10.1021/acs.organomet.5b00184

data_4085759
_publ_section_title
;
 Silane--Allyl Coupling Reactions of Cp*(iPr2MeP)Fe(\h3-C3H5) and
 Synthetic Access to the Hydrido--Dinitrogen Complex Cp*(iPr2MeP)FeH(N2)
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2134
_journal_paper_doi               10.1021/acs.organomet.5b00184
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C31 H44 Fe Si'
_chemical_formula_sum            'C31 H44 Fe Si'
_chemical_formula_weight         500.60
_chemical_name_common            'Compound 2'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.23 svn.r3118 for OlexSys, GUI svn.r4975)
;
_cell_angle_alpha                93.8800(10)
_cell_angle_beta                 93.4510(10)
_cell_angle_gamma                107.7960(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3942(6)
_cell_length_b                   9.3342(7)
_cell_length_c                   18.0496(13)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.56
_cell_volume                     1338.61(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.978
_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  0.0215
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_laue_measured_fraction_full 0.981
_diffrn_reflns_laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20883
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.335
_diffrn_reflns_theta_min         2.270
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0467P)^2^+1.3436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4395
_reflns_number_total             4780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00184_si_002.cif
_cod_data_source_block           ps1_84_0m
_cod_depositor_comments
'Adding full bibliography for 4085759--4085762.cif.'
_cod_database_code               4085759
_shelxl_version_number           2014-3
_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.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C15(H15), C25(H25), C13(H13)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C31(H31A,H31B,H31C), C17(H17A,H17B,
 H17C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C9(H9A,H9B,H9C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              68497
_shelx_hkl_checksum              16919
_olex2_submission_special_instructions 'No special instructions were received'