s-Block-Metal-Mediated Hydroamination of Diphenylbutadiyne with Primary Arylamines Using a Dipotassium Tetrakis(amino)calciate Precatalyst
Younis, Fadi M.; Krieck, Sven; Görls, Helmar; Westerhausen, Matthias; Organometallics 34 (2015) 3577–; doi:10.1021/acs.organomet.5b00449

data_4086038
_publ_section_title
;
 s-Block-Metal-Mediated Hydroamination of Diphenylbutadiyne with Primary
 Arylamines Using a Dipotassium Tetrakis(amino)calciate Precatalyst
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3577
_journal_paper_doi               10.1021/acs.organomet.5b00449
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C42 H35 N'
_chemical_formula_sum            'C42 H35 N'
_chemical_formula_weight         553.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90.509(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1588(2)
_cell_length_b                   21.6115(2)
_cell_length_c                   12.8659(2)
_cell_measurement_temperature    133(2)
_cell_volume                     3102.60(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18937
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0510P)^2^+2.3661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                5873
_reflns_number_total             7121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00449_si_002.cif
_cod_data_source_block           FO4803
_cod_depositor_comments
'Adding full bibliography for 4086038--4086042.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4086038