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_7108637
_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            'C30 H10 B F20 N P'
_chemical_formula_weight         806.17
_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   'at N from difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.764(2)
_cell_angle_beta                 78.902(3)
_cell_angle_gamma                89.099(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1955(5)
_cell_length_b                   11.4489(5)
_cell_length_c                   14.1284(5)
_cell_measurement_reflns_used    4256
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     1483.74(11)
_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 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_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  0.067
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16479
_diffrn_reflns_theta_full        66.56
_diffrn_reflns_theta_max         66.56
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    2.259
_exptl_absorpt_correction_T_max  0.9353
_exptl_absorpt_correction_T_min  0.6608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         4959
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0768P)^2^+1.4055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                3735
_reflns_number_total             4959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc36782c.txt
_cod_data_source_block           erk6352
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108637