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_4125011
_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
'0.81(C108 H144 N8 Sn11), 0.19(C108 H144 N8 Sn10)'
_chemical_formula_sum            'C108 H144 N8 Sn10.81'
_chemical_formula_weight         2837.28
_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
_audit_creation_date             2015-03-12
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 94.4855(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6958(2)
_cell_length_b                   14.9348(1)
_cell_length_c                   33.1882(4)
_cell_measurement_reflns_used    39461
_cell_measurement_temperature    150
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     12203.2(2)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            108750
_diffrn_reflns_theta_full        25.668
_diffrn_reflns_theta_max         28.840
_diffrn_reflns_theta_min         3.131
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            metallic_dark_red
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5553.740
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.120
_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.
;
_refine_diff_density_max         4.63
_refine_diff_density_min         -2.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1350
_refine_ls_number_reflns         30192
_refine_ls_number_restraints     649
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.0031382
_refine_ls_shift/su_mean         0.0001118
_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: 
 235. 347. 193. 68.1 11.6 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0985
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0980
_reflns_limit_h_max              33
_reflns_limit_h_min              -33
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              43
_reflns_limit_l_min              0
_reflns_number_gt                24332
_reflns_number_total             30255
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.19
_oxford_diffrn_Wilson_scale      5.20
_oxford_refine_ls_r_factor_ref   0.0624
_oxford_refine_ls_scale          0.35158(13)
_oxford_reflns_number_all        30204
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title MPB205
_cod_data_source_file            ja6b00710_si_002.cif
_cod_data_source_block           cluster
_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_sg_symbol_H-M      'P 21/c '
_cod_database_code               4125011