New monocyclic and acyclic hNK-2 antagonists retaining the β-turn feature. X-ray and molecular modelling studies
Altamura, Maria R.; Dapporto Paolo; Fedi, Valentina; Giolitti, Alessandro; Guerri, Annalisa; Guidi, Antonio; Paoli, Paola; Rossi, Patrizia; Acta Crystallographica, Section B 62 (2006) 889–896; doi:10.1107/S0108768106018167

data_2100619
_publ_section_title
;
New monocyclic and acyclic hNK-2 antagonists retaining the \b-turn
feature. X-ray and molecular modelling studies
;
_journal_coeditor_code           GP5007
_journal_date_accepted           2006-05-16
_journal_date_recd_electronic    2006-02-28
_journal_issue                   4
_journal_name_full               'Acta Crystallographica, Section B'
_journal_page_first              889
_journal_page_last               896
_journal_paper_category          FA
_journal_paper_doi               10.1107/S0108768106018167
_journal_volume                  62
_journal_year                    2006
_chemical_formula_sum            'C37 H48 N4 O4 S'
_chemical_formula_weight         644.85
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.152(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0346(8)
_cell_length_b                   9.8834(7)
_cell_length_c                   25.617(2)
_cell_measurement_reflns_used    4501
_cell_measurement_temperature    298
_cell_measurement_theta_max      57.1
_cell_measurement_theta_min      1.7
_cell_volume                     3517.4(4)
_computing_cell_refinement       'SMART, Siemens (1995)'
_computing_data_collection       'SMART, Siemens (1995)'
_computing_data_reduction        'SAINT, Siemens (1995)'
_computing_molecular_graphics    'ORTEP-3 (Farruggia, 1997)'
_computing_publication_material  'PARST-97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir97 (Altomare, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'three circles SMART CCD'
_diffrn_measurement_method       'intensity from \w scans'
_diffrn_radiation_monochromator  'Goebel mirrors'
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13267
_diffrn_reflns_theta_full        57.06
_diffrn_reflns_theta_max         57.06
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipedon
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.180
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         7090
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0748
_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^)+(0.1097P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1868
_reflns_number_gt                5160
_reflns_number_total             7090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gp5007.cif
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C37 H48 N4 O4 S1'
_cod_database_code               2100619