Synthesis, Structure, and Stability of Adducts between Phosphide and Amide Anions and the Lewis Acids Borane, Tris(pentafluorophenyl)borane, and Tris(pentafluorophenyl)alane
Anna-Marie Fuller; Andrew J. Mountford; Matthew L. Scott; Simon J. Coles; Peter N. Horton; David L. Hughes; Michael B. Hursthouse; Simon J. Lancaster; Inorganic Chemistry 48 (2009) 11474–11482; doi:10.1021/ic901799q

data_4303766
_publ_contact_author_address
;Wolfson Materials and Catalysis Centre,
School of Chemisrty,
University of East Anglia,
Norwich,
NR4 7TJ
;
_publ_contact_author_email       S.Lancasterr@uea.ac.uk
_publ_contact_author_fax         '44 1603 592003'
_publ_contact_author_name        'S. J. Lancaster'
_publ_contact_author_phone       '44 1603 592009'
_publ_section_title
;
Synthesis, Structure, and Stability of Adducts between Phosphide and Amide
Anions and the Lewis Acids Borane, Tris(pentafluorophenyl)borane, and
Tris(pentafluorophenyl)alane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11474
_journal_page_last               11482
_journal_paper_doi               10.1021/ic901799q
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C8 H16 Li O4, C36 H2 B2 F30 P'
_chemical_formula_sum            'C44 H18 B2 F30 Li O4 P'
_chemical_formula_weight         1240.11
_chemical_name_systematic        '[Li(C8H16O4)].[H2P{B(C6F5)3}2]'
_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
_cell_angle_alpha                62.10(13)
_cell_angle_beta                 84.68(10)
_cell_angle_gamma                89.27(10)
_cell_formula_units_Z            2
_cell_length_a                   12.465(13)
_cell_length_b                   14.37(3)
_cell_length_c                   14.461(14)
_cell_measurement_reflns_used    9641
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2278(6)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source
;
'Bruker-Nonius FR591 rotating anode'
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1233
_diffrn_reflns_av_sigmaI/netI    0.1414
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42972
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.9954
_exptl_absorpt_correction_T_min  0.9685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Cut Blade'
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         10370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1821
_refine_ls_R_factor_gt           0.0919
_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^)+(0.0270P)^2^+4.2807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1620
_reflns_number_gt                5853
_reflns_number_total             10370
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic901799q_si_001_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;

2021-05-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2279(5)
_cod_original_formula_moiety     'C16 H32 Li2 O8, 2(C36 H2 B2 F30 P)'
_cod_original_formula_sum        'C88 H36 B4 F60 Li2 O8 P2'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     2480.22
_cod_database_code               4303766