On the control of secondary carbanion structure utilising ligand effects during directed metallation.
Wheatley, Andrew E. H.; Clayden, Jonathan; Hillier, Ian H.; Campbell Smith, Alison; Vincent, Mark A.; Taylor, Laurence J.; Haywood, Joanna; Beilstein journal of organic chemistry 8 (2012) 50–60; doi:10.3762/bjoc.8.5

data_4029724
_publ_section_title
;
 On the control of secondary carbanion structure utilising ligand effects
 during directed metallation.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              50
_journal_page_last               60
_journal_paper_doi               10.3762/bjoc.8.5
_journal_volume                  8
_journal_year                    2012
_chemical_formula_moiety         'C25 H47 Li N4 O'
_chemical_formula_sum            'C25 H47 Li N4 O'
_chemical_formula_weight         426.61
_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                 102.643(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6194(2)
_cell_length_b                   29.1721(8)
_cell_length_c                   10.0296(3)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      1
_cell_volume                     2746.24(13)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14239
_diffrn_reflns_theta_full        24.40
_diffrn_reflns_theta_max         24.40
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                2591
_reflns_number_total             4461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-8-5-S1.cif
_cod_data_source_block           e:\crysta~1\aw1211\aw1112
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4029724