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_4309488
_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         'Mg, 4(C H3), N2 C2 H4, 2(H N Si C9 H21)'
_chemical_formula_sum            'C24 H60 Mg N4 Si2'
_chemical_formula_weight         485.236
_chemical_name_common            Mg-TMEDA-NHSi(iPr)3
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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_TMEDA_HNSi(iPr)3_e246_westerhausen
_audit_creation_date             28-Oct-00
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_audit_update_record             28-Feb-05
_cell_angle_alpha                90
_cell_angle_beta                 102.449(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9300(12)
_cell_length_b                   10.2952(6)
_cell_length_c                   19.9613(15)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.1
_cell_volume                     3196.7(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 0.951
_diffrn_measured_fraction_theta_max 0.951
_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      0.019142
_diffrn_orient_matrix_UB_12      -0.049359
_diffrn_orient_matrix_UB_13      0.036469
_diffrn_orient_matrix_UB_21      -0.090497
_diffrn_orient_matrix_UB_22      -0.010123
_diffrn_orient_matrix_UB_23      0.033802
_diffrn_orient_matrix_UB_31      -0.007131
_diffrn_orient_matrix_UB_32      -0.040161
_diffrn_orient_matrix_UB_33      -0.031117
_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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11057
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         2.09
_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    0.147
_exptl_absorpt_correction_T_max  0.9768
_exptl_absorpt_correction_T_min  0.9598
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.00818(13)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0791P)^2^+0.4154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                2259
_reflns_number_total             2980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0503277si20050303_041028_2.cif
_cod_data_source_block           e246
_cod_original_cell_volume        3196.9(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4309488