Regioselective Metalation of a Tertiary Phosphine. Solution and Solid-State Structures of an Unusual Aminobenzyllithium Complex
Clegg, William; Izod, Keith; McFarlane, William; O'Shaughnessy, Paul; Organometallics 18 (1999) 3950–; doi:10.1021/om9904910

data_4077822
_publ_section_title
;
 Regioselective Metalation of a Tertiary Phosphine. Solution and
 Solid-State Structures of an Unusual Aminobenzyllithium Complex
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3950
_journal_paper_doi               10.1021/om9904910
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C45 H60 Li2 N4 P2'
_chemical_formula_weight         732.79
_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                70.298(2)
_cell_angle_beta                 81.523(2)
_cell_angle_gamma                68.833(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7384(6)
_cell_length_b                   13.1535(8)
_cell_length_c                   19.0431(12)
_cell_measurement_reflns_used    8477
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.24
_cell_volume                     2140.7(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14392
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         9388
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0677P)^2^+1.1521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1603
_reflns_number_gt                6732
_reflns_number_total             9388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9904910.cif
_cod_data_source_block           ki22
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077822