Diverse Reactivity of ECp* (E = Al, Ga) toward Low-Coordinate Transition Metal Amides [TM(N(SiMe<sub>3</sub>)<sub>2</sub>)<sub>2</sub>] (TM = Fe, Co, Zn): Insertion, Cp* Transfer, and Orthometalation.
Weßing, Jana; Göbel, Christoph; Weber, Birgit; Gemel, Christian; Fischer, Roland A.; Inorganic chemistry 56 (2017) 3517–3525; doi:10.1021/acs.inorgchem.6b03127

data_4349382
_publ_section_title
;
 Diverse Reactivity of ECp* (E = Al, Ga) toward Low-Coordinate Transition
 Metal Amides [TM(N(SiMe<sub>3</sub>)<sub>2</sub>)<sub>2</sub>] (TM = Fe,
 Co, Zn): Insertion, Cp* Transfer, and Orthometalation.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3517
_journal_page_last               3525
_journal_paper_doi               10.1021/acs.inorgchem.6b03127
_journal_volume                  56
_journal_year                    2017
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C12 H36 Fe Ga2 N2 Si4, 2(C10 H15)'
_chemical_formula_sum            'C32 H66 Fe Ga2 N2 Si4'
_chemical_formula_weight         786.52
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3997(3)
_cell_length_b                   15.1616(2)
_cell_length_c                   16.9223(3)
_cell_measurement_reflns_used    5846
_cell_measurement_temperature    112
_cell_measurement_theta_max      76.0190
_cell_measurement_theta_min      3.9430
_cell_volume                     4207.66(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      112
_diffrn_detector_area_resol_mean 10.4372
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11783
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        67.68
_diffrn_reflns_theta_max         76.31
_diffrn_reflns_theta_min         3.97
_exptl_absorpt_coefficient_mu    5.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82481
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0366P)^2^+1.3813P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                4004
_reflns_number_total             4346
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic6b03127_si_001.cif
_cod_data_source_block           om1206
_cod_database_code               4349382
_shelx_res_checksum              37621
_shelx_hkl_checksum              78696