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_4071481
_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         'C52 H70 N4 Na2 Zn2'
_chemical_formula_sum            'C52 H70 N4 Na2 Zn2'
_chemical_formula_weight         927.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   22.420(3)
_cell_length_b                   22.883(3)
_cell_length_c                   41.069(6)
_cell_measurement_reflns_used    7027
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.35
_cell_volume                     21070(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            74668
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7872
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+108.1183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                6239
_reflns_number_total             9282
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8001813-file001.cif
_cod_data_source_block           rem383_compound6
_cod_original_cell_volume        21069(5)
_cod_database_code               4071481