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_1514660
_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            'C39.5 H30 B Cl F10 N P'
_chemical_formula_weight         785.88
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.4210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   39.1199(4)
_cell_length_b                   16.3061(2)
_cell_length_c                   23.4811(4)
_cell_measurement_reflns_used    12881
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     14853.0(3)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.042
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68796
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    2.034
_exptl_absorpt_correction_T_max  0.7109
_exptl_absorpt_correction_T_min  0.5621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6416
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         12969
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0715P)^2^+24.4007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                11402
_reflns_number_total             12969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc00082f.txt
_cod_data_source_block           erk6623
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C39.50 H30 B Cl F10 N P'
_cod_database_code               1514660