3-[2,6-Bis(diethylcarbamoyl)pyridin-4-yl]-<i>N</i>-(<i>tert</i>-butoxycarbonyl)alanine methyl ester: a chiral tridentate ligand that causes a diastereomeric excess of its lanthanide complexes in solution
Muller, Gilles; Schmidt, Boris; Jiřiček, Jan; Bünzli, Jean-Claude G.; Schenk, Kurt J.; Acta Crystallographica Section C 59 (2003) o353–o356; doi:10.1107/S0108270103006656

data_2013353
_publ_section_title
;3-[2,6-Bis(diethylcarbamoyl)pyridin-4-yl]-<i>N</i>-(<i>tert</i>-butoxycarbonyl)alanine
 methyl ester: a chiral tridentate ligand that causes a diastereomeric excess
 of its lanthanide complexes in solution
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o353
_journal_page_last               o356
_journal_paper_doi               10.1107/S0108270103006656
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C24 H38 N4 O6'
_chemical_formula_moiety         'C24 H38 N4 O6'
_chemical_formula_sum            'C24 H38 N4 O6'
_chemical_formula_weight         478.58
_chemical_name_systematic
;
L^4^ is
3-[2,6-bis(diethylcarbamoyl)pyridin-4-yl]-N-(tert-butoxycarbonyl)alanine
methyl ester
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.144(2)
_cell_length_b                   13.047(3)
_cell_length_c                   18.429(4)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      13.75
_cell_volume                     2652.2(10)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1997)'
_computing_data_reduction        IPDS
_computing_molecular_graphics    'SHELXTL (Bruker, 1996)'
_computing_publication_material  'SHELXTL, PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 6.7
_diffrn_measured_fraction_theta_full 0.9307
_diffrn_measured_fraction_theta_max 0.9307
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38694
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         6220
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      3.073
_refine_ls_restrained_S_obs      3.248
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0576
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                5570
_reflns_number_total             6220
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1603.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2013353
_cod_database_fobs_code          2013353