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_4303769
_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         'C16 H32 Li O8, C22 H13 B2 F15 P'
_chemical_formula_structural
;
'[Li{C8H16O4}2][{H3B}PH{C(CH3)3}{B(C6F5)3}]'
;
_chemical_formula_sum            'C38 H45 B2 F15 Li O8 P'
_chemical_formula_weight         974.27
_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                99.750(17)
_cell_angle_beta                 96.41(2)
_cell_angle_gamma                91.167(17)
_cell_formula_units_Z            2
_cell_length_a                   8.545(2)
_cell_length_b                   15.851(5)
_cell_length_c                   16.004(3)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2121.3(9)
_computing_cell_refinement       'DENZO, COLLECT'
_computing_data_reduction        'DENZO, COLLECT'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48265
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  0.9928
_exptl_absorpt_correction_T_min  0.9786
_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    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0052(7)
_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   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         9718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0446P)^2^+1.8056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                6586
_reflns_number_total             9718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901799q_si_001_5.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2121.4(9)
_cod_database_code               4303769