Regioselective Metalation of a Tertiary Phosphine. Synthesis and Structural Characterization of an Unusual Tetrameric Lithium Phosphinomethanide
Izod, Keith; O'Shaughnessy, Paul; Clegg, William; Liddle, Stephen T.; Organometallics 20 (2001) 648–; doi:10.1021/om000876e

data_4077240
_publ_section_title
;
 Regioselective Metalation of a Tertiary Phosphine. Synthesis and
 Structural Characterization of an Unusual Tetrameric Lithium
 Phosphinomethanide
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              648
_journal_paper_doi               10.1021/om000876e
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C97 H128 Li4 N8 P4'
_chemical_formula_weight         1557.71
_chemical_name_systematic
;
 ?
;
_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                113.890(2)
_cell_angle_beta                 92.138(2)
_cell_angle_gamma                90.708(2)
_cell_formula_units_Z            2
_cell_length_a                   16.6255(7)
_cell_length_b                   16.8352(7)
_cell_length_c                   19.2871(8)
_cell_measurement_reflns_used    24030
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.15
_cell_volume                     4930.2(4)
_computing_cell_refinement       'Siemens Saint'
_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 0.985
_diffrn_measured_fraction_theta_max 0.889
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42846
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.9622
_exptl_absorpt_correction_T_min  0.7992
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.00150(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         22464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0543P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                14152
_reflns_number_total             22464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000876e.cif
_cod_data_source_block           ki58
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077240