New lithium-zincate approaches for the selective functionalisation of pyrazine: direct dideprotozincation vs. nucleophilic alkylation
Sharon E. Baillie; Victoria L. Blair; David C. Blakemore; Duncan Hay; Alan R. Kennedy; David C. Pryde; Eva Hevia; Chem.Commun. 48 (2012) 1985–; doi:10.1039/c2cc16959b

data_7107344
_publ_section_title
;
 New lithium-zincate approaches for the selective functionalisation of
 pyrazine: direct dideprotozincation vs. nucleophilic alkylation
;
_journal_name_full               Chem.Commun.
_journal_page_first              1985
_journal_paper_doi               10.1039/c2cc16959b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C46 H88 Li2 N4 O4 Zn2'
_chemical_formula_weight         905.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.038(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3706(4)
_cell_length_b                   16.5165(4)
_cell_length_c                   17.8453(6)
_cell_measurement_reflns_used    13335
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.35
_cell_measurement_theta_min      2.70
_cell_volume                     4944.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32501
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro. Absorption correction using spherical harmonics
implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.773
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         32506
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0846
_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^)+(0.1099P)^2^+15.8182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2390
_reflns_number_gt                21835
_reflns_number_total             32506
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc16959b.txt
_cod_data_source_block           savep21
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7107344