Synthesis, Structural Authentication, and Structurally Defined Metalation Reactions of Lithium and Sodium DA-Zincate Bases (DA = diisopropylamide) with Phenylacetylene†
Clegg, William; García-Álvarez, Joaquín; García-Álvarez, Pablo; Graham, David V.; Harrington, Ross W.; Hevia, Eva; Kennedy, Alan R.; Mulvey, Robert E.; Russo, Luca; Organometallics 27 (2008) 2654–; doi:10.1021/om8001813

data_4071483
_publ_section_title
;
 Synthesis, Structural Authentication, and Structurally Defined Metalation
 Reactions of Lithium and Sodium DA-Zincate Bases (DA = diisopropylamide)
 with Phenylacetylene&#x2020;
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2654
_journal_paper_doi               10.1021/om8001813
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C18 H30 N2 Zn'
_chemical_formula_sum            'C18 H30 N2 Zn'
_chemical_formula_weight         339.81
_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                61.934(9)
_cell_angle_beta                 85.505(7)
_cell_angle_gamma                89.357(7)
_cell_formula_units_Z            4
_cell_length_a                   10.4058(4)
_cell_length_b                   14.1317(15)
_cell_length_c                   14.986(3)
_cell_measurement_reflns_used    8888
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     1937.8(5)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21170
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         5.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.6352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                4665
_reflns_number_total             6743
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8001813-file001.cif
_cod_data_source_block           rem448_compound8
_cod_original_cell_volume        1937.7(4)
_cod_database_code               4071483