Rigid backbone moiety of KNI-272, a highly selective HIV protease inhibitor: methanol, acetone and dimethylsulfoxide solvated forms of 3-[3-benzyl-2-hydroxy-9-(isoquinolin-5-yloxy)-6-methylsulfanylmethyl-5,8-dioxo-4,7-diazanonanoyl]-<i>N</i>-<i>tert</i>-butyl-1,3-thiazolidine-4-carboxamide
Doi, Mitsunobu; Kimura, Tooru; Ishida, Toshimasa; Kiso, Yoshiaki; Acta Crystallographica Section B 60 (2004) 433–437; doi:10.1107/S0108768104013047

data_2102581
_publ_section_title
;Rigid backbone moiety of KNI-272, a highly selective HIV protease inhibitor:
 methanol, acetone and dimethylsulfoxide solvated forms of
 3-[3-benzyl-2-hydroxy-9-(isoquinolin-5-yloxy)-6-methylsulfanylmethyl-5,8-dioxo-4,7-diazanonanoyl]-<i>N</i>-<i>tert</i>-butyl-1,3-thiazolidine-4-carboxamide
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              433
_journal_page_last               437
_journal_paper_doi               10.1107/S0108768104013047
_journal_volume                  60
_journal_year                    2004
_chemical_formula_moiety         'C33 H41 N5 O6 S2, 2(C3 H6 O)'
_chemical_formula_sum            'C39 H53 N5 O8 S2'
_chemical_formula_weight         783.98
_chemical_name_common            knia
_chemical_name_systematic
;
 HIV protease inhibitor KNI272: iQoa-Mta-Apns-Thz-tBu diacetone
;
_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                 98.9310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6395(7)
_cell_length_b                   13.2130(9)
_cell_length_c                   14.6921(10)
_cell_measurement_reflns_used    7940
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      2.6
_cell_volume                     2040.4(2)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINTPLUS (Bruker, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS, SMART APEX area detector'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'MacScience, M18XCE rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23703
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_count 23703
_diffrn_standards_interval_time  360
_diffrn_standards_number         498
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9507
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.218
_refine_ls_abs_structure_details 'Flack (1983), 4257 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8940
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.4323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                8718
_reflns_number_total             8940
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            og5001.cif
_cod_data_source_block           knia
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2102581