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_4125002
_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         'C52 H74 B2 N5 Sn1'
_chemical_formula_sum            'C52 H74 B2 N5 Sn'
_chemical_formula_weight         909.50
_chemical_melting_point          ?
_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     other
_cell_angle_alpha                90
_cell_angle_beta                 105.3860(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4712(2)
_cell_length_b                   14.5386(2)
_cell_length_c                   18.7150(2)
_cell_measurement_reflns_used    11831
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5108.04(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            106092
_diffrn_reflns_theta_full        26.659
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         5.184
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.87
_refine_diff_density_min         -1.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9265
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         11602
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.0031251
_refine_ls_shift/su_mean         0.0000830
_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: 
 76.2 125. 76.3 33.0 8.33 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1302
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1298
_reflns_limit_h_max              25
_reflns_limit_h_min              0
_reflns_limit_k_max              0
_reflns_limit_k_min              -18
_reflns_limit_l_max              23
_reflns_limit_l_min              -24
_reflns_number_gt                9836
_reflns_number_total             11614
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0576
_oxford_refine_ls_scale          0.3695(4)
_oxford_reflns_number_all        11614
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 003apek15
_cod_data_source_file            ja6b00710_si_002.cif
_cod_data_source_block           1a-NH3
_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.

'_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.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

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

 Adding full bibliography for 4125002--4125015.cif.
;
_cod_original_cell_volume        5108.04(5)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C52 H74 B2 N5 Sn1'
_cod_database_code               4125002