Gilman-Type versus Lipshutz-Type Reagents: Competition in Lithiocuprate Chemistry
Haywood, Joanna; Morey, James V.; Wheatley, Andrew E. H.; Liu, Ching-Yuan; Yasuike, Shuji; Kurita, Jyoji; Uchiyama, Masanobu; Raithby, Paul R.; Organometallics 28 (2009) 38–; doi:10.1021/om801101u

data_4068796
_publ_section_title
;
 Gilman-Type versus Lipshutz-Type Reagents: Competition in Lithiocuprate
 Chemistry
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              38
_journal_paper_doi               10.1021/om801101u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C27 H47 Cu Li N O3'
_chemical_formula_sum            'C27 H47 Cu Li N O3'
_chemical_formula_weight         504.14
_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                77.32(3)
_cell_angle_beta                 72.54(3)
_cell_angle_gamma                85.82(3)
_cell_formula_units_Z            2
_cell_length_a                   10.556(2)
_cell_length_b                   11.664(2)
_cell_length_c                   11.939(2)
_cell_measurement_reflns_used    12952
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     1368.0(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14539
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         4.35
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         6192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0589P)^2^+1.0606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                5511
_reflns_number_total             6192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801101u_si_002.cif
_cod_data_source_block           aw0708
_cod_original_cell_volume        1367.9(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068796