Anomalous Staudinger reaction at intramolecular frustrated P-B Lewis pair frameworks
Annika Stute; Lukas Heletta; Roland Frohlich; Constantin G. Daniliuc; Gerald Kehr; Gerhard Erker; Chem.Commun. 48 (2012) 11739–; doi:10.1039/c2cc36782c

data_7108636
_publ_section_title
;
 Anomalous Staudinger reaction at intramolecular frustrated P-B Lewis pair
 frameworks
;
_journal_name_full               Chem.Commun.
_journal_page_first              11739
_journal_paper_doi               10.1039/c2cc36782c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C44.5 H45 B Cl2 F10 N3 P'
_chemical_formula_weight         924.52
_chemical_name_systematic
;
?
;
_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                78.9260(10)
_cell_angle_beta                 84.7730(10)
_cell_angle_gamma                74.6400(10)
_cell_formula_units_Z            2
_cell_length_a                   10.36170(10)
_cell_length_b                   12.65120(10)
_cell_length_c                   19.2962(2)
_cell_measurement_reflns_used    6183
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     2391.57(4)
_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 0.926
_diffrn_measured_fraction_theta_max 0.926
_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  0.071
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23344
_diffrn_reflns_theta_full        66.96
_diffrn_reflns_theta_max         66.96
_diffrn_reflns_theta_min         4.43
_exptl_absorpt_coefficient_mu    2.168
_exptl_absorpt_correction_T_max  0.8123
_exptl_absorpt_correction_T_min  0.3561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         7889
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1302P)^2^+1.5459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2084
_reflns_number_gt                6945
_reflns_number_total             7889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc36782c.txt
_cod_data_source_block           erk6440
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C44.50 H45 B Cl2 F10 N3 P'
_cod_database_code               7108636