Enabling and Probing Oxidative Addition and Reductive Elimination at a Group 14 Metal Center: Cleavage and Functionalization of E-H Bonds by a Bis(boryl)stannylene.
Protchenko, Andrey V.; Bates, Joshua I.; Saleh, Liban M. A.; Blake, Matthew P.; Schwarz, Andrew D.; Kolychev, Eugene L.; Thompson, Amber L.; Jones, Cameron; Mountford, Philip; Aldridge, Simon; Journal of the American Chemical Society 138 (2016) 4555–4564; doi:10.1021/jacs.6b00710

data_4125003
_publ_section_title
;
 Enabling and Probing Oxidative Addition and Reductive Elimination at a
 Group 14 Metal Center: Cleavage and Functionalization of E-H Bonds by a
 Bis(boryl)stannylene.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4555
_journal_page_last               4564
_journal_paper_doi               10.1021/jacs.6b00710
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C56 H83 B2 N5 Sn1, 0.25(C6H14)'
_chemical_formula_sum            'C57.5 H86.5 B2 N5 Sn'
_chemical_formula_weight         988.16
_chemical_melting_point          ?
_chemical_name_systematic
;
Sn{B(NArCH)2}2NtBu
;
_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                 102.8998(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3402(2)
_cell_length_b                   12.8395(1)
_cell_length_c                   22.8290(3)
_cell_measurement_reflns_used    17222
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      3
_cell_volume                     5811.51(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.984
_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  0.026
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34404
_diffrn_reflns_theta_full        73.030
_diffrn_reflns_theta_max         76.073
_diffrn_reflns_theta_min         3.975
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.770
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2106
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.31
_refine_diff_density_min         -1.30
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0373
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         10355
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.0012059
_refine_ls_shift/su_mean         0.0000500
_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: 
 0.849E-01 -13.4 -9.18 -2.93 -7.08 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0292
_refine_ls_wR_factor_gt          0.0274
_refine_ls_wR_factor_ref         0.0269
_reflns_limit_h_max              24
_reflns_limit_h_min              -25
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                10758
_reflns_number_total             11964
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.86
_oxford_diffrn_Wilson_scale      0.28
_oxford_refine_ls_r_factor_ref   0.0353
_oxford_refine_ls_scale          2.2852(14)
_oxford_reflns_number_all        11964
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title MPB183
_cod_data_source_file            ja6b00710_si_002.cif
_cod_data_source_block           1a-NH2tBu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4125002--4125015.cif.
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C57.50 H86.50 B2 N5 Sn1'
_cod_database_code               4125003