Lithiation of Tris(alkyl- and arylamido)orthophosphates EP[N(H)R]3 (E = O, S, Se): Imido Substituent Effects and PE Bond Cleavage
Tristram Chivers; Mark Krahn; Gabriele Schatte; Masood Parvez; Inorganic Chemistry 42 (2003) 3994–4005; doi:10.1021/ic034151p

data_4313841
_publ_contact_author_address
; Department of Chemistry
    University of Calgary
    Calgary Alberta T2N 1N4
    Canada
;
_publ_contact_author_email       chivers@ucalgary.ca
_publ_contact_author_fax         '001 403 289 9488'
_publ_contact_author_name        'Dr Tristram Chivers'
_publ_contact_author_phone       '001 403 220 5741'
_publ_section_title
;
 Lithiation of Tris(alkyl- and arylamido)orthophosphates EP[N(H)R]3 (E =
 O, S, Se): Imido Substituent Effects and PE Bond Cleavage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3994
_journal_page_last               4005
_journal_paper_doi               10.1021/ic034151p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C40 H95 Li3 N9 O4 P3'
_chemical_formula_sum            'C40 H95 Li3 N9 O4 P3'
_chemical_formula_weight         879.98
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.940(3)
_cell_length_b                   19.282(3)
_cell_length_c                   27.461(3)
_cell_measurement_reflns_used    6773
_cell_measurement_temperature    193(2)
_cell_volume                     11088(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  WinGX-1.62
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25694
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  0.9415
_exptl_absorpt_correction_T_min  0.9226
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; SADABS, V 5.0, Software for Area-Detector Absorption
    Corrections; Bruker AXS Inc., Madison, WI, 1998.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         7767
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0651P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                4878
_reflns_number_total             7767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034151psi20030224_104900_5.cif
_cod_data_source_block           4
_cod_original_cell_volume        11088(2)
_cod_database_code               4313841