Amine-Chelated Aryllithium Reagents Structure and Dynamics
Hans J. Reich; Wayne S. Goldenberg; Birgir Ö. Gudmundsson; Aaron W. Sanders; Klaus J. Kulicke; Katya Simon; Ilia A. Guzei; Journal of the American Chemical Society 123 (2001) 8067–8079; doi:10.1021/ja010489b

data_4115651
_publ_section_title
;
 Amine-Chelated Aryllithium Reagents Structure and Dynamics
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8067
_journal_page_last               8079
_journal_paper_doi               10.1021/ja010489b
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C30 H48 Li2 N2 O2'
_chemical_formula_weight         482.58
_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-97
_cell_angle_alpha                117.115(2)
_cell_angle_beta                 102.521(2)
_cell_angle_gamma                98.701(2)
_cell_formula_units_Z            1
_cell_length_a                   8.8594(9)
_cell_length_b                   9.8398(10)
_cell_length_c                   10.4018(11)
_cell_measurement_temperature    173(2)
_cell_volume                     754.58(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3067
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.9736
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0524
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1616
_reflns_number_gt                2120
_reflns_number_total             3067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010489b.cif
_cod_data_source_block           rei02
_cod_original_cell_volume        754.58(13)
_cod_database_code               4115651