Synthesis and Structural Elucidation of Alkyl, Amido, and Mixed Alkyl−Amido “Highly-Coordinated” Zincates
Armstrong, David R.; Dougan, Christine; Graham, David V.; Hevia, Eva; Kennedy, Alan R.; Organometallics 27 (2008) 6063–; doi:10.1021/om800786n

data_4072347
_publ_section_title
;
 Synthesis and Structural Elucidation of Alkyl, Amido, and Mixed
 Alkyl&#x2212;Amido &#x201C;Highly-Coordinated&#x201D; Zincates
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6063
_journal_paper_doi               10.1021/om800786n
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C24 H68 Li2 N10 Zn2'
_chemical_formula_weight         641.50
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_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                 95.742(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.156(2)
_cell_length_b                   11.9022(8)
_cell_length_c                   18.1773(15)
_cell_measurement_reflns_used    3467
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.52
_cell_volume                     3693.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega 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  0.1211
_diffrn_reflns_av_sigmaI/netI    0.2291
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17518
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'small fragment'
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.937
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5711
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.1901
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1849
_refine_ls_wR_factor_ref         0.2103
_reflns_number_gt                2307
_reflns_number_total             5711
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800786n_si_001.cif
_cod_data_source_block           new
_cod_original_cell_volume        3693.0(6)
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4072347