In Search of the [PhB(μ-NtBu)2]2As. Radical: Experimental and Computational Investigations of the Redox Chemistry of Group 15 Bis-boraamidinates
Jari Konu; Heikki M. Tuononen; Tristram Chivers; Andrea M. Corrente; René T. Boeré; Tracey L. Roemmele; Inorganic Chemistry 47 (2008) 3823–3831; doi:10.1021/ic702435e

data_4304848
_publ_contact_author             'Professor Tristram Chivers'
_publ_contact_author_email       chivers@ucalgary.ca
_publ_section_title
;
In Search of the [PhB(\m-NtBu)2]2As. Radical: Experimental and
Computational Investigations of the Redox Chemistry of Group 15
Bis-boraamidinates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3823
_journal_page_last               3831
_journal_paper_doi               10.1021/ic702435e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C30 H39 B Cl N2 P'
_chemical_formula_sum            'C30 H39 B Cl N2 P'
_chemical_formula_weight         504.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 115.22(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.876(3)
_cell_length_b                   12.416(3)
_cell_length_c                   15.917(4)
_cell_measurement_reflns_used    15549
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.27
_cell_volume                     2838.4(13)
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15549
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_correction_T_min  0.9691
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0476P)^2^+1.3432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                3679
_reflns_number_total             4804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702435e-file002_2.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        2838.6(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4304848