Oxidative Bond Formation and Reductive Bond Cleavage at Main Group Metal Centers: Reactivity of Five-Valence-Electron MX2 Radicals.
Protchenko, Andrey V.; Dange, Deepak; Blake, Matthew P.; Schwarz, Andrew D.; Jones, Cameron; Mountford, Philip; Aldridge, Simon; Journal of the American Chemical Society 136 (2014) 10902–10905; doi:10.1021/ja5062467

data_4122328
_publ_section_title
;
 Oxidative Bond Formation and Reductive Bond Cleavage at Main Group Metal
 Centers: Reactivity of Five-Valence-Electron MX2 Radicals.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10902
_journal_page_last               10905
_journal_paper_doi               10.1021/ja5062467
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C52 H73 B2 Ga1 N4 O1'
_chemical_formula_sum            'C52 H73 B2 Ga N4 O'
_chemical_formula_weight         861.52
_chemical_name_systematic
;
Ga{B(L)}2(OH)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 93.8759(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9473(2)
_cell_length_b                   14.8095(2)
_cell_length_c                   21.5138(3)
_cell_measurement_reflns_used    25192
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      3
_cell_volume                     5069.33(12)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55308
_diffrn_reflns_theta_full        75.529
_diffrn_reflns_theta_max         77.071
_diffrn_reflns_theta_min         3.626
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         9432
_refine_ls_number_restraints     277
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.0011286
_refine_ls_shift/su_mean         0.0000216
_refine_ls_structure_factor_coef F
_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: 
 10.9 6.18 9.36 1.95 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0513
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0490
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                9716
_reflns_number_total             10635
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.52
_oxford_diffrn_Wilson_scale      0.14
_oxford_refine_ls_r_factor_ref   0.0395
_oxford_refine_ls_scale          2.896(4)
_oxford_reflns_number_all        10598
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja5062467_si_009.cif
_cod_data_source_block           MPB138
_cod_depositor_comments
'Adding full bibliography for 4122328--4122335.cif.'
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C52 H73 B2 Ga1 N4 O1'
_cod_database_code               4122328