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_4085762
_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         'C37 H46 Fe Si'
_chemical_formula_sum            'C37 H46 Fe Si'
_chemical_formula_weight         574.68
_chemical_name_common            'Compound 3'
_chemical_name_systematic
;
 ?
;
_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     direct
_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                95.5940(10)
_cell_angle_beta                 104.4630(10)
_cell_angle_gamma                107.3250(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7703(3)
_cell_length_b                   11.2002(3)
_cell_length_c                   17.3519(5)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      2.48
_cell_volume                     1548.10(8)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19556
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.487
_diffrn_reflns_theta_min         1.938
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
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_refine_ls_matrix_type           full
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_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0511
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+3.0642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4977
_reflns_number_total             5699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00184_si_003.cif
_cod_data_source_block           ps1_74_0m
_cod_depositor_comments
'Adding full bibliography for 4085759--4085762.cif.'
_cod_database_code               4085762
_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 Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C17(H17), C16(H16), C24(H24), C22(H22), C18(H18), C33(H33)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C37(H37A,H37B,
 H37C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C12(H12A,
 H12B,H12C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              34971
_shelx_hkl_checksum              37290
_olex2_submission_special_instructions 'No special instructions were received'