Reactivity of highly Lewis acidic diborane(4) towards pyridine and isocyanide: formation of boraalkene-pyridine complex and <i>ortho</i>-functionalized pyridine derivatives.
Katsuma, Yuhei; Asakawa, Hiroki; Yamashita, Makoto; Chemical science 9 (2018) 1301–1310; doi:10.1039/c7sc04759b

data_1548441
_publ_section_title
;
 Reactivity of highly Lewis acidic diborane(4) towards pyridine and
 isocyanide: formation of boraalkene-pyridine complex and
 <i>ortho</i>-functionalized pyridine derivatives.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1301
_journal_page_last               1310
_journal_paper_doi               10.1039/c7sc04759b
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C39 H37 B2 F3 N2 O2'
_chemical_formula_sum            'C39 H37 B2 F3 N2 O2'
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-11-03 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;
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_cell_angle_gamma                90
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_cell_length_c                   32.930(8)
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_cell_measurement_theta_max      30.6400
_cell_measurement_theta_min      1.8553
_cell_volume                     11280(5)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    'Yadokari-XG 2009(Wakita Nemoto et al.)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      93(2)
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_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
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_diffrn_reflns_Laue_measured_fraction_full 0.971
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_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       39
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_diffrn_reflns_point_group_measured_fraction_full 0.971
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_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.112
_exptl_absorpt_coefficient_mu    0.080
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       Platelet
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_refine_diff_density_min         -0.459
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_refine_ls_abs_structure_details
;
 Flack x determined using 6557 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0961
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_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+10.3332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2177
_refine_ls_wR_factor_ref         0.2235
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                17996
_reflns_number_total             19805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04759b3.cif
_cod_data_source_block           5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 

2019-07-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1548427--1548445.cif.
;
_cod_original_cell_volume        11279(5)
_cod_original_formula_moiety     'C117 H141 B6 F9 N6 O6'
_cod_original_formula_sum        'C117 H141 B6 F9 N6 O6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1963.21
_cod_database_code               1548441
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2014-3
_shelx_res_checksum              86618