Boron and Aluminum Complexes of Sterically Demanding Phosphinimines and Phosphinimides
Silke Courtenay; Denise Walsh; Sarah Hawkeswood; Pingrong Wei; Anjan Kumar Das; Douglas W. Stephan; Inorganic Chemistry 46 (2007) 3623–3631; doi:10.1021/ic0700351

data_4308069
_publ_section_title
;
Boron and Aluminum Complexes of Sterically Demanding Phosphinimines and
Phosphinimides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3623
_journal_page_last               3631
_journal_paper_doi               10.1021/ic0700351
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C24 H54 B2 F4 N2 P2'
_chemical_formula_weight         530.25
_space_group_IT_number           205
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.298(4)
_cell_length_b                   14.298(4)
_cell_length_c                   14.298(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     2923.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0763
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3111
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.300355
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0588
_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^)+(0.1109P)^2^+0.6850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1757
_reflns_number_gt                469
_reflns_number_total             644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0700351si20070111_011533_6.cif
_cod_data_source_block           '[(?-t-Bu3PN)2BF2]2'
_cod_original_cell_volume        2922.9(16)
_cod_database_code               4308069