Remarkable coordination behavior of alkyl isocyanides toward unsaturated vicinal frustrated P/B Lewis pairs
Ekkert, Olga; Miera, Greco González; Wiegand, Thomas; Eckert, Hellmut; Schirmer, Birgitta; Petersen, Jeffrey L.; Daniliuc, Constantin G.; Fröhlich, Roland; Grimme, Stefan; Kehr, Gerald; Erker, Gerhard; Chemical Science 4 (2013) 2657–; doi:10.1039/c3sc00082f

data_1514658
_publ_section_title
;
 Remarkable coordination behavior of alkyl isocyanides toward unsaturated
 vicinal frustrated P/B Lewis pairs
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              2657
_journal_paper_doi               10.1039/c3sc00082f
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C39 H29 B F10 N P'
_chemical_formula_weight         743.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.693(3)
_cell_angle_beta                 95.330(5)
_cell_angle_gamma                112.360(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1806(5)
_cell_length_b                   10.4896(3)
_cell_length_c                   17.7612(8)
_cell_measurement_reflns_used    5265
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     1732.34(13)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20969
_diffrn_reflns_theta_full        66.74
_diffrn_reflns_theta_max         66.74
_diffrn_reflns_theta_min         4.74
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_T_max  0.9308
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         5917
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0479P)^2^+0.7991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                5387
_reflns_number_total             5917
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc00082f.txt
_cod_data_source_block           erk6519
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1514658