Oxidative Dehydrocoupling of N-H Bonds Using a Redox-Active Main Group Superbase
R.J.Less; V.Naseri; M.McPartlin; D.S.Wright; Chem.Commun. 47 (2011) 6129–; doi:10.1039/c1cc00053e

data_7106420
_publ_section_title
;
 Oxidative Dehydrocoupling of N-H Bonds Using a Redox-Active Main Group
 Superbase
;
_journal_coden_Cambridge         0182
_journal_name_full               Chem.Commun.
_journal_page_first              6129
_journal_paper_doi               10.1039/c1cc00053e
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         '2(C24 H50 Li2 N9), C30 H22 N10 Sn7'
_chemical_formula_sum            'C78 H122 Li4 N28 Sn7'
_chemical_formula_weight         2310.63
_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                97.486(1)
_cell_angle_beta                 104.430(1)
_cell_angle_gamma                103.962(1)
_cell_formula_units_Z            2
_cell_length_a                   13.8673(1)
_cell_length_b                   18.7128(2)
_cell_length_c                   20.1729(3)
_cell_measurement_reflns_used    52773
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.00
_cell_volume                     4817.84(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56150
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.839
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.328
_refine_diff_density_min         -3.333
_refine_diff_density_rms         0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     997
_refine_ls_number_reflns         22770
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                15857
_reflns_number_total             22770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc00053e.txt
_cod_data_source_block           dw1008
_cod_original_cell_volume        4817.83(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106420