Generation of Cationic Two-Coordinate Group-13 Ligand Systems by Spontaneous Halide Ejection: Remarkably Nucleophile-Resistant (Dimethylamino)borylene Complexes
David A. Addy; Glesni A. Pierce; Dragoslav Vidovic; Dibyendu Mallick; Eluvathingal D. Jemmis; Jose M. Goicoechea; Simon Aldridge; Journal of the American Chemical Society 132 (2010) 4586–4588; doi:10.1021/ja101192e

data_4102222
_publ_contact_author             'Simon Aldridge'
_publ_contact_author_email       simon.aldridge@chem.ox.ac.uk
_publ_section_title
;
 Generation of Cationic Two-Coordinate Group-13 Ligand Systems by
 Spontaneous Halide Ejection: Remarkably Nucleophile-Resistant
 (Dimethylamino)borylene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4586
_journal_page_last               4588
_journal_paper_doi               10.1021/ja101192e
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C80.00 H83.00 B4 Cl16 F1.00 Fe2 N2 P4.00'
_chemical_formula_sum            'C80 H83 B4 Cl16 F Fe2 N2 P4'
_chemical_formula_weight         1937.63
_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
_audit_creation_date             09-12-16
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                76.5761(5)
_cell_angle_beta                 76.9145(5)
_cell_angle_gamma                80.9145(5)
_cell_formula_units_Z            2
_cell_length_a                   13.65660(10)
_cell_length_b                   14.8733(2)
_cell_length_c                   23.5763(3)
_cell_measurement_reflns_used    17498
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4508.87(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            61514
_diffrn_reflns_theta_full        26.582
_diffrn_reflns_theta_max         27.404
_diffrn_reflns_theta_min         5.089
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            pale_orange
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1980.007
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.64
_refine_diff_density_min         -1.19
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         18487
_refine_ls_number_restraints     457
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.003515
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 23.0 33.8 16.1 3.99 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1459
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1459
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              19
_reflns_limit_k_min              -18
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                14571
_reflns_number_total             20220
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.84
_oxford_diffrn_Wilson_scale      18.18
_oxford_refine_ls_r_factor_ref   0.0720
_oxford_refine_ls_scale          0.24994(13)
_oxford_reflns_number_all        18487
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 089dadv09
_cod_data_source_file            ja101192e_si_001_1.cif
_cod_data_source_block           4a1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C80.00 H83.00 B4 Cl16 F1.00 Fe2 N2 P4.00'
_cod_database_code               4102222