Catalytic Trimerization of Bis-silylated Diazomethane
Muhammad Farooq Ibad; Peter Langer; Fabian Reiß; Axel Schulz; Alexander Villinger; Journal of the American Chemical Society 134 (2012) 17757–17768; doi:10.1021/ja308104k

data_4118820
_publ_contact_author_address
;
Universit\"at Rostock
Institut f\"ur Chemie
Abteilung f\"ur Anorganische Chemie
Albert-Einstein-Strasse 3a 
18059 Rostock
Bundesrepublik Deutschland
;
_publ_contact_author_email
;
axel.schulz@uni-rostock.de, alexander.villinger@uni-rostock.de'
;
_publ_contact_author_fax         '+49 (0)381/498-6382'
_publ_contact_author_name        'Axel Schulz, Alexander Villinger'
_publ_contact_author_phone       '+49 (0)381/498-6400 or 6403'
_publ_section_title
;
 Catalytic Trimerization of Bis-silylated Diazomethane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17757
_journal_page_last               17768
_journal_paper_doi               10.1021/ja308104k
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C25 H18 B F15 N2 Si2'
_chemical_formula_sum            'C25 H18 B F15 N2 Si2'
_chemical_formula_weight         698.40
_chemical_name_systematic
;
bis(trimethylsilyl)aminoisonitrile tris(pentafluorophenyl)borane adduct
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Villinger, A.; Hering, C.'
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_cell_length_b                   11.5683(5)
_cell_length_c                   12.7373(6)
_cell_measurement_reflns_used    7833
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      51.792
_cell_measurement_theta_min      4.921
_cell_volume                     1413.67(11)
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_collection       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa Apex II-CCD-diffractometer'
_diffrn_measurement_method       'phi and psi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37661
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.9571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         8978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.0592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                5759
_reflns_number_total             8978
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja308104k_si_001_09.cif
_cod_data_source_block           ch_fr142_(me3si)2nncb(c6f5)3_2
_cod_original_cell_volume        1413.68(11)
_cod_database_code               4118820