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_4125010
_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         'C55 H77 B2 K1 N5 Sn1'
_chemical_formula_sum            'C55 H77 B2 K N5 Sn'
_chemical_formula_weight         987.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 117.1098(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.85850(10)
_cell_length_b                   43.5512(2)
_cell_length_c                   19.19370(10)
_cell_measurement_reflns_used    29515
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     13288.00(12)
_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 0.988
_diffrn_measured_fraction_theta_max 0.986
_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  0.050
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            295537
_diffrn_reflns_theta_full        25.585
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         5.108
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4168
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         0.86
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9674
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         30117
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.0032234
_refine_ls_shift/su_mean         0.0000296
_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: 
 12.3 17.7 8.82 2.40 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1812
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1812
_reflns_limit_h_max              20
_reflns_limit_h_min              -23
_reflns_limit_k_max              56
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                19623
_reflns_number_total             30133
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.98
_oxford_diffrn_Wilson_scale      96.05
_oxford_refine_ls_r_factor_ref   0.0941
_oxford_refine_ls_scale          0.11652(3)
_oxford_reflns_number_all        30117
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'Compound X At 13:55 on 5/ 6'
_cod_data_source_file            ja6b00710_si_002.cif
_cod_data_source_block           9
_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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4125002--4125015.cif.
;
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C55 H77 B2 K1 N5 Sn1'
_cod_database_code               4125010
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE N   (   2,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 243,X'S) H   ( 242,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 323,X'S) H   ( 322,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) H   ( 393,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 402,X'S) H   ( 401,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) H   ( 463,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) H   ( 473,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) H   ( 533,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) H   ( 543,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) H   ( 612,X'S) H   ( 613,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) H   ( 623,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 683,X'S) H   ( 682,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) H   ( 692,X'S) H   ( 693,X'S) 
RIDE N   (  70,X'S) H   ( 701,X'S) H   ( 702,X'S) 
RIDE N   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE N   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) H   ( 832,X'S) H   ( 833,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) H   ( 842,X'S) H   ( 843,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) H   ( 902,X'S) H   ( 903,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) 
RIDE C   (  97,X'S) H   ( 971,X'S) H   ( 972,X'S) H   ( 973,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) H   ( 982,X'S) H   ( 983,X'S) 
RIDE C   (  99,X'S) H   ( 991,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1043,X'S) H   (1042,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) H   (1052,X'S) H   (1053,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) 
RIDE C   ( 121,X'S) H   (1213,X'S) H   (1212,X'S) H   (1211,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) H   (1222,X'S) H   (1223,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) 
RIDE C   ( 127,X'S) H   (1271,X'S) 
RIDE C   ( 128,X'S) H   (1283,X'S) H   (1282,X'S) H   (1281,X'S) 
RIDE C   ( 129,X'S) H   (1291,X'S) H   (1292,X'S) H   (1293,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) H   (1332,X'S) H   (1333,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) 
RIDE C   ( 165,X'S) H   (1651,X'S) 
RIDE C   ( 162,X'S) H   (1623,X'S) H   (1622,X'S) H   (1621,X'S) 
RIDE C   ( 141,X'S) H   (1411,X'S) H   (1412,X'S) H   (1413,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) H   (1142,X'S) H   (1143,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) H   (1172,X'S) H   (1173,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;