A solid state and theoretical study of the solvent effects controlling the mono- and di-lithiation of aromatic primary amines
Armstrong, David R.; Ball, Sarah C.; Barr, Donald; Clegg, William; Linton, David J.; Kerr, Lesley C.; Moncrieff, David; Raithby, Paul R.; Singer, Robert J.; Snaith, Ronald; Stalke, Dietmar; Wheatley, Andrew E. H.; Wright, Dominic S.; Journal of the Chemical Society, Dalton Transactions  (2002) 2505–; doi:10.1039/b107970k

data_7011139
_publ_section_title
;
 A solid state and theoretical study of the solvent effects controlling
 the mono- and di-lithiation of aromatic primary amines
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2505
_journal_paper_doi               10.1039/b107970k
_journal_year                    2002
_chemical_formula_sum            'C112 H154 Li20 N10 O10.5'
_chemical_formula_weight         1947.28
_chemical_name_systematic
; 
? 
;
_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
_cell_angle_alpha                111.47(5)
_cell_angle_beta                 105.16(5)
_cell_angle_gamma                65.89(4)
_cell_formula_units_Z            1
_cell_length_a                   14.854(9)
_cell_length_b                   17.152(9)
_cell_length_c                   14.186(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     3043(3)
_computing_cell_refinement       'Rigaku cntl software'
_computing_data_collection       'Rigaku cntl software'
_computing_data_reduction        TeXsan
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       omega/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9896
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0.04%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_description       Block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.168
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         5492
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.105
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.1660
_refine_ls_R_factor_obs          0.1121
_refine_ls_shift/esd_max         -0.601
_refine_ls_shift/esd_mean        0.054
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w3D1/[\s^2^(Fo^2^)+(0.2490P)^2^+2.0267P] where 
P3D(Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.3913
_refine_ls_wR_factor_obs         0.3197
_reflns_number_observed          3469
_reflns_number_total             5652
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b107970k.txt
_cod_data_source_block           rs9702
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3043.1(31)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C112 H154 Li20 N10 O10.50'
_cod_database_code               7011139