Synthesis and Characterization of the Monomeric Vicinal Dianion Li~2~(THF)~3~[ArNC(SiMe~3~)~2~] and the Aluminum and Lithium Derivatives of the Amido Ligand [ArNCH(SiMe~3~)~2~]^-^
Cheng, Xiaoyan; Zhang, Jianying; Song, Haibin; Cui, Chunming; Organometallics 27 (2008) 678–682; doi:10.1021/om700972a

data_4083494
_publ_section_title
;
 Synthesis and Characterization of the Monomeric Vicinal Dianion
 Li~2~(THF)~3~[ArNC(SiMe~3~)~2~] and the Aluminum and Lithium Derivatives
 of the Amido Ligand [ArNCH(SiMe~3~)~2~]^-^
;
_journal_coden_ASTM              ORGND7
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              678
_journal_page_last               682
_journal_paper_doi               10.1021/om700972a
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C54 H110 Al2 Li2 N2 O4 Si4'
_chemical_formula_sum            'C54 H110 Al2 Li2 N2 O4 Si4'
_chemical_formula_weight         1031.64
_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                 95.577(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.225(2)
_cell_length_b                   17.355(3)
_cell_length_c                   14.270(3)
_cell_measurement_reflns_used    9474
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.9
_cell_volume                     3259.7(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40743
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.9633
_exptl_absorpt_correction_T_min  0.9514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         7782
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0634P)^2^+1.8124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                6577
_reflns_number_total             7782
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4070735
_cod_data_source_file            om700972a-file003.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;

2025-01-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C27 H55 Al Li N O2 Si2'
_cod_original_formula_weight         515.82
_cod_original_formula_moiety         'C27 H55 Al Li N O2 Si2'
_cod_original_formula_units_Z            4
_cod_database_code               4083494