Synthesis and conformational analysis of a type VIb β-turn mimetic based on an eight-membered lactam
Derrer, Sam; Davies, John E.; Holmes, Andrew B.; Journal of the Chemical Society, Perkin Transactions 1  (2000) 2957–; doi:10.1039/b003791p

data_7213369
_publ_section_title
;
 Synthesis and conformational analysis of a type VIb \b-turn mimetic based
 on an eight-membered lactam
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2957
_journal_paper_doi               10.1039/b003791p
_journal_year                    2000
_chemical_formula_sum            'C11.5 H18.5 Cl1.5 N2 O4'
_chemical_formula_weight         301.96
_chemical_name_systematic
; 
 3(S)-(Acetyl-amino)-8(R)-carboxy-azacane-2-one methy 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                 90.93(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.955(2)
_cell_length_b                   18.210(5)
_cell_length_c                   10.141(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75
_cell_measurement_theta_min      15
_cell_volume                     1468.8(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega 2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4894
_diffrn_reflns_theta_max         60.06
_diffrn_reflns_theta_min         4.36
_diffrn_standards_decay_%        0%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.259
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4375
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_obs          0.0513
_refine_ls_shift/esd_max         0.029
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+0.3875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1419
_refine_ls_wR_factor_obs         0.1344
_reflns_number_observed          3844
_reflns_number_total             4375
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b003791psup1.cif
_cod_data_source_block           ah9605
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+0.3875P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+0.3875P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_original_formula_sum        'C11.50 H18.50 Cl1.50 N2 O4'
_cod_database_code               7213369