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_4122329
_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_absolute_configuration ad
_chemical_formula_moiety         'C58 H82 B2 N4 Sn1'
_chemical_formula_sum            'C58 H82 B2 N4 Sn'
_chemical_formula_weight         975.63
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-04-24
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.11301(14)
_cell_length_b                   18.55311(17)
_cell_length_c                   19.57819(18)
_cell_measurement_reflns_used    36307
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     5489.59(9)
_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 0.997
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59242
_diffrn_reflns_theta_full        76.475
_diffrn_reflns_theta_max         76.475
_diffrn_reflns_theta_min         3.282
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.982
_exptl_absorpt_correction_T_max  0.45
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.67
_refine_diff_density_min         -1.09
_refine_ls_abs_structure_details 'Flack (1983), 5141 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.024(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         11062
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.0038069
_refine_ls_shift/su_mean         0.0000387
_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: 
 62.0 -83.9 75.1 -27.7 15.5 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0223
_refine_ls_wR_factor_gt          0.0217
_refine_ls_wR_factor_ref         0.0216
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                11162
_reflns_number_total             11451
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.58
_oxford_diffrn_Wilson_scale      0.17
_oxford_refine_ls_r_factor_ref   0.0201
_oxford_refine_ls_scale          3.3225(17)
_oxford_reflns_number_all        11408
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'ADS_352 in P2(1)2(1)2(1)'
_cod_data_source_file            ja5062467_si_002.cif
_cod_data_source_block           ADS_352
_cod_depositor_comments
'Adding full bibliography for 4122328--4122335.cif.'
_cod_original_cell_volume        5489.60(9)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C58 H82 B2 N4 Sn1'
_cod_database_code               4122329
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 103,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) H   ( 223,X'S) 
RIDE C   (  23,X'S) H   ( 233,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 253,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 262,X'S) H   ( 261,X'S) H   ( 263,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 363,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 392,X'S) H   ( 391,X'S) H   ( 393,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 482,X'S) H   ( 481,X'S) H   ( 483,X'S) 
RIDE C   (  49,X'S) H   ( 493,X'S) H   ( 491,X'S) H   ( 492,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 513,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 522,X'S) H   ( 521,X'S) H   ( 523,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) 
RIDE C   (  56,X'S) H   ( 562,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 573,X'S) H   ( 572,X'S) 
RIDE C   (  58,X'S) H   ( 582,X'S) H   ( 581,X'S) H   ( 583,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.01000 = 
CONT C(9) TO C(10) 
CONT C(9) TO C(11) 
CONT C(38) TO C(39) 
CONT C(38) TO C(40) 
CONT C(24) TO C(25) 
CONT C(24) TO C(26) 
CONT C(50) TO C(51) 
CONT C(50) TO C(52) 
DIST 0, 0.01 = MEAN 
CONT C(9) TO C(10) 
CONT C(9) TO C(11) 
CONT C(38) TO C(39) 
CONT C(38) TO C(40) 
CONT C(24) TO C(25) 
CONT C(24) TO C(26) 
CONT C(50) TO C(51) 
CONT C(50) TO C(52) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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