[Li{CH(Me)P(Ph)2(NCO2Me)}2(THF)2]: Crystal, Solution, and Calculated Structure of aN-Delocalized Lithium Phosphazene
Ignacio Fernández; Julia María Álvarez Gutíerrez; Nikolaus Kocher; Dirk Leusser; Dietmar Stalke; Javier González; Fernando López Ortiz; Journal of the American Chemical Society 124 (2002) 15184–15185; doi:10.1021/ja027469+

data_4115404
_publ_contact_author             'Prof. Dr. D. Stalke'
_publ_contact_author_email       dstalke@chemie.uni-wuerzburg.de
_publ_section_title
;
 [Li{CH(Me)P(Ph)2(NCO2Me)}2(THF)2]: Crystal, Solution, and Calculated
 Structure of aN-Delocalized Lithium Phosphazene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15184
_journal_page_last               15185
_journal_paper_doi               10.1021/ja027469+
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C48 H66 Li2 N2 O8 P2'
_chemical_formula_weight         874.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.460(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.435(3)
_cell_length_b                   16.162(3)
_cell_length_c                   10.858(2)
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.50
_cell_volume                     2318.5(8)
_computing_cell_refinement       'SAINT-NT V6/6.0'
_computing_data_collection       'SMART-NT V5.6'
_computing_data_reduction        'SAINT-NT V6/6.0'
_computing_molecular_graphics    SHELXTL-97
_computing_publication_material  SHELXTL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex with D8 Goniometr'
_diffrn_measurement_method       '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  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21576
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7835
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2.0 (Sheldrick 2000)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       blocks
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4106
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0768P)^2^+3.2398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                3140
_reflns_number_total             4106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0274692B_s2.cif
_cod_data_source_block           8
_cod_original_cell_volume        2318.4(8)
_cod_database_code               4115404