Ligand Exchange Reaction Between an Alkylzinc Primary Amide and a Dialkylmagnesium Compound: Crystal Structures of [(thf)MeMg-μ-N(H)SiiPr3]2 and (tmeda)Mg[N(H)SiiPr3]2
Matthias Westerhausen; Tobias Bollwein; Nikolaos Makropoulos; Holger Piotrowski; Inorganic Chemistry 44 (2005) 6439–6444; doi:10.1021/ic0503277

data_4309487
_publ_contact_author_address
;
Institut fuer Anorganische und Analytische Chemie
Friedrich-Schiller-Universitaet
August-Bebel-Str. 2
D-07743 Jena
Bundesrepublik Deutschland
;
_publ_contact_author_email       m.we@uni-jena.de
_publ_contact_author_name        'Matthias Westerhausen'
_publ_section_title
;
Ligand Exchange Reaction Between an Alkylzinc Primary Amide and a
Dialkylmagnesium Compound: Crystal Structures of
[(thf)MeMg-\m-N(H)SiiPr3]2 and (tmeda)Mg[N(H)SiiPr3]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6439
_journal_page_last               6444
_journal_paper_doi               10.1021/ic0503277
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety
;
Mg2, 2(C H3), 2(N H Si C9 H21), 2(C4 H8 O)
;
_chemical_formula_sum            'C28 H66 Mg2 N2 O2 Si2'
_chemical_formula_weight         567.617
_chemical_name_common            'Mg{(CH3)[NH(Si(iPr)3)]} * x THF'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Piotrowski, H.'
_audit_block_code                Mg_CH3_NHSi(iPr)3_THF_d097_makropoulos
_audit_creation_date             11-Nov-99
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_audit_update_record             28-Feb-05
_cell_angle_alpha                90
_cell_angle_beta                 95.021(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8237(16)
_cell_length_b                   20.3413(12)
_cell_length_c                   9.0722(6)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.0
_cell_volume                     3644.2(4)
_computing_cell_refinement       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_collection       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_reduction        'Stoe IPDS software (Darmstadt, Germany)'
_computing_molecular_graphics
;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
 Plot Program for Crystal Structure Illustrations, Oak Ridge National
 Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
 Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
 Germany, 1995).
;
_computing_publication_material
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
--- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)
;
_diffrn_ambient_temperature      200(3)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'image-plate area detector'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_diffrn_orient_matrix_type
;first index: i in a~i~^*^, second: diffractometer xyz
 e.g. UB_21,UB_22,UB_23 are the xyz components of b^*^
;
_diffrn_orient_matrix_UB_11      -0.007416
_diffrn_orient_matrix_UB_12      0.023943
_diffrn_orient_matrix_UB_13      -0.044000
_diffrn_orient_matrix_UB_21      -0.048515
_diffrn_orient_matrix_UB_22      -0.006419
_diffrn_orient_matrix_UB_23      0.004684
_diffrn_orient_matrix_UB_31      -0.008958
_diffrn_orient_matrix_UB_32      0.100634
_diffrn_orient_matrix_UB_33      0.045126
_diffrn_radiation_collimation    '0.5 mm collimator'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20720
_diffrn_reflns_theta_full        23.96
_diffrn_reflns_theta_max         23.96
_diffrn_reflns_theta_min         2.00
_diffrn_source_current           50_mA
_diffrn_source_power             2.75_kW
_diffrn_source_type              'Spellman DF4 Series'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.9669
_exptl_absorpt_correction_T_min  0.9443
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.03459(11)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         5516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                4206
_reflns_number_total             5516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0503277si20050303_041028_1.cif
_cod_data_source_block           d097
_cod_database_code               4309487