Synthesis, crystal structures and reactions of sila- and germa-β-diketiminates
Farwell, James D.; Fernandes, Manuel A.; Hitchcock, Peter B.; Lappert, Michael F.; Layh, Marcus; Omondi, Bernard; Dalton Transactions  (2003) 1719–; doi:10.1039/b300817g

data_7012749
_publ_section_title
;
 Synthesis, crystal structures and reactions of sila- and
 germa-\b-diketiminates
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1719
_journal_paper_doi               10.1039/b300817g
_journal_year                    2003
_chemical_formula_sum            'C38.5 H58 Li N3 Si4'
_chemical_formula_weight         682.18
_chemical_name_common
;
(Li(NCR)(Si(SiMe3)(CRNSiMe3)2)) pentane solvate (R=C6H3Me2)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                80.74(3)
_cell_angle_beta                 81.55(2)
_cell_angle_gamma                67.29(2)
_cell_formula_units_Z            2
_cell_length_a                   12.324(3)
_cell_length_b                   12.837(4)
_cell_length_c                   15.253(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     2187.4(11)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7672
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    'riding ; but omitted for solvate'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+1.0339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1317
_reflns_number_observed          5897
_reflns_number_total             7672
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b300817g.txt
_cod_data_source_block           mfl(1b)-jan198
_cod_original_cell_volume        2187.4(10)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C38.50 H58 Li N3 Si4'
_cod_database_code               7012749