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_4122332
_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         '2(C110 H154 B4 In2 N8), 0.5(C6 H14)'
_chemical_formula_sum            'C223 H315 B8 In4 N16'
_chemical_formula_weight         3765.85
_chemical_name_systematic
;
[{In{B(NArCH)2}}2{C6H10}]. 0.25(C6H14)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.4557(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.8417(3)
_cell_length_b                   13.13430(10)
_cell_length_c                   45.0886(4)
_cell_measurement_reflns_used    54571
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     22946.9(3)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_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  0.029
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            47495
_diffrn_reflns_theta_full        74.081
_diffrn_reflns_theta_max         76.372
_diffrn_reflns_theta_min         3.334
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.545
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8004
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.

PLATON
PLATON, A Multipurpose Crystallographic Tool, A. L. Spek. Utrecht, 
the Netherlands, 1998.; A. Spek, J. Appl. Cryst. (2003), 36, 7-13.

SQUEEZE
A. Spek, J. Appl. Cryst. (2003), 36, 7-13; 
P. van der Sluis & A. L. Spek, Acta Cryst. (1990). A46, 194-201.

MCE
J. Rohlicek & M. Husak, J. Appl. Cryst. (2007), 40, 600-601.

;
_refine_diff_density_max         1.47
_refine_diff_density_min         -1.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0376
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2422
_refine_ls_number_reflns         39980
_refine_ls_number_restraints     479
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.0073598
_refine_ls_shift/su_mean         0.0000827
_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: 
 -0.835 -16.7 -7.18 -5.79 -4.78 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0257
_refine_ls_wR_factor_gt          0.0244
_refine_ls_wR_factor_ref         0.0240
_reflns_limit_h_max              48
_reflns_limit_h_min              -50
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              56
_reflns_limit_l_min              0
_reflns_number_gt                42044
_reflns_number_total             47495
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.15
_oxford_diffrn_Wilson_scale      0.32
_oxford_refine_ls_r_factor_ref   0.0371
_oxford_refine_ls_scale          0.8249(3)
_oxford_reflns_number_all        47308
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja5062467_si_004.cif
_cod_data_source_block           MPB175
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4122328--4122335.cif.
;
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4122332