Synthesis, Structural Elucidation, and Diffusion-Ordered NMR Studies of Homoleptic Alkyllithium Magnesiates: Donor-Controlled Structural Variations in Mixed-Metal Chemistry
Baillie, Sharon E.; Clegg, William; Garc\?ía-Álvarez, Pablo; Hevia, Eva; Kennedy, Alan R.; Klett, Jan; Russo, Luca; Organometallics 31 (2012) 5131–; doi:10.1021/om300477m

data_4078870
_publ_section_title
;
 Synthesis, Structural Elucidation, and Diffusion-Ordered NMR Studies of
 Homoleptic Alkyllithium Magnesiates: Donor-Controlled Structural
 Variations in Mixed-Metal Chemistry
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              5131
_journal_paper_doi               10.1021/om300477m
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C21 H56 Li Mg N3 Si3'
_chemical_formula_weight         466.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.643(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8686(3)
_cell_length_b                   16.9877(7)
_cell_length_c                   19.5686(8)
_cell_measurement_reflns_used    8903
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.89
_cell_measurement_theta_min      2.73
_cell_volume                     3251.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 12.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       '\w scans'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27494
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.96
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         9417
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                5767
_reflns_number_total             9417
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om300477m_si_001.cif
_cod_data_source_block           jksha3_compound_6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4078870