A Tetrameric Lithiated Phosphazene Containing a Lithium Atom Bound Exclusively to Four sp3-Hybridized Carbanionic Centers: A Key Intermediate for Understanding Structure−Reactivity Relationships of Phosphazenyllithium Compounds
Ruiz Gómez, Gloria; Fernández, Ignacio; López Ortiz, Fernando; Price, Richard D.; Davidson, Matthew G.; Mahon, Mary F.; Howard, Judith A. K.; Organometallics 26 (2007) 514–; doi:10.1021/om0608354

data_4072571
_publ_section_title
;
 A Tetrameric Lithiated Phosphazene Containing a Lithium Atom Bound
 Exclusively to Four sp3-Hybridized Carbanionic Centers:&#x00A0; A Key
 Intermediate for Understanding Structure&#x2212;Reactivity Relationships
 of Phosphazenyllithium Compounds
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              514
_journal_paper_doi               10.1021/om0608354
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C109.6 H98.4 Li4 N4 P4'
_chemical_formula_weight         1623.16
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 104.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.763(4)
_cell_length_b                   20.181(4)
_cell_length_c                   25.127(5)
_cell_measurement_temperature    150(2)
_cell_volume                     9211(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29115
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SHELXTL'
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3424
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00069(19)
_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   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7191
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+55.6938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2391
_refine_ls_wR_factor_ref         0.2622
_reflns_number_gt                4467
_reflns_number_total             7191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0608354si20061121_065918.cif
_cod_data_source_block           c:\x-ray\propos~1\davidson\lithum\lithium
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4072571