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_1514657
_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            'C44 H26 B F15 N P'
_chemical_formula_weight         895.44
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.896(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8351(8)
_cell_length_b                   11.5678(8)
_cell_length_c                   30.569(3)
_cell_measurement_reflns_used    7613
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     4787.2(6)
_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 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.059
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            33705
_diffrn_reflns_theta_full        67.11
_diffrn_reflns_theta_max         67.11
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.9146
_exptl_absorpt_correction_T_min  0.6968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         8139
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1181P)^2^+2.4834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1936
_refine_ls_wR_factor_ref         0.2077
_reflns_number_gt                6278
_reflns_number_total             8139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc00082f.txt
_cod_data_source_block           erk6523
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1514657