Calciate-mediated intermolecular hydroamination of diphenylbutadiyne with secondary anilines
Carsten Glock; Helmar Gorls; Matthias Westerhausen; Chem.Commun. 48 (2012) 7094–; doi:10.1039/c2cc32790b

data_7107962
_publ_section_title
;
 Calciate-mediated intermolecular hydroamination of diphenylbutadiyne with
 secondary anilines
;
_journal_name_full               Chem.Commun.
_journal_page_first              7094
_journal_paper_doi               10.1039/c2cc32790b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C41 H31 N'
_chemical_formula_sum            'C41 H31 N'
_chemical_formula_weight         537.67
_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                78.709(2)
_cell_angle_beta                 71.546(2)
_cell_angle_gamma                89.447(1)
_cell_formula_units_Z            2
_cell_length_a                   10.0932(3)
_cell_length_b                   11.9758(3)
_cell_length_c                   13.0546(3)
_cell_measurement_reflns_used    9330
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.67
_cell_volume                     1465.53(7)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9330
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0332P)^2^+1.3917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1410
_reflns_number_gt                5588
_reflns_number_total             6589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32790b.txt
_cod_data_source_block           FO4297
_cod_database_code               7107962