New Bonding Modes for Boraamidinate Ligands in Heavy Group 15 Complexes: Fluxional Behavior of the 1:2 Complexes, LiM[PhB(NtBu)2]2 (M = As, Sb, Bi)
Jari Konu; Maravanji S. Balakrishna; Tristram Chivers; Thomas W. Swaddle; Inorganic Chemistry 46 (2007) 2627–2636; doi:10.1021/ic0622757

data_4307789
_publ_contact_author             'Professor Tristram Chivers'
_publ_contact_author_email       chivers@ucalgary.ca
_publ_section_title
;
New Bonding Modes for Boraamidinate Ligands in Heavy Group 15 Complexes:
Fluxional Behavior of the 1:2 Complexes, LiM[PhB(NtBu)2]2 (M = As, Sb, Bi)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2627
_journal_page_last               2636
_journal_paper_doi               10.1021/ic0622757
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C14 H23 As B Cl N2'
_chemical_formula_sum            'C14 H23 As B Cl N2'
_chemical_formula_weight         340.52
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.16(3)
_cell_angle_beta                 96.76(3)
_cell_angle_gamma                99.49(3)
_cell_formula_units_Z            2
_cell_length_a                   6.0002(12)
_cell_length_b                   10.653(2)
_cell_length_c                   13.411(3)
_cell_measurement_reflns_used    5606
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.67
_cell_volume                     835.9(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'WinGX v1.70-01 (L. J. Farrugia)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'phi\omega scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Enraf Nonius FR590D, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5606
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.182
_exptl_absorpt_correction_T_max  0.9577
_exptl_absorpt_correction_T_min  0.4469
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.941
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.019(4)
_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   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0494P)^2^+4.6571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                2598
_reflns_number_total             2944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0622757si20070112_014747_1.cif
_cod_data_source_block           compound_1a
_cod_database_code               4307789