Synthesis and biological evaluation of quinaldopeptin.
Katayama, Katsushi; Okamura, Takuya; Sunadome, Takuya; Nakagawa, Koji; Takeda, Hiroshi; Shiro, Motoo; Matsuda, Akira; Ichikawa, Satoshi; The Journal of organic chemistry 79 (2014) 2580–2590; doi:10.1021/jo500039d

data_4037608
_publ_section_title
;
 Synthesis and biological evaluation of quinaldopeptin.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2580
_journal_page_last               2590
_journal_paper_doi               10.1021/jo500039d
_journal_volume                  79
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C60 H76 N16 O12'
_chemical_formula_sum            'C60 H76 N16 O12'
_chemical_formula_weight         1213.36
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 125.123(9)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   24.4859(5)
_cell_length_b                   11.3635(3)
_cell_length_c                   14.2600(10)
_cell_measurement_reflns_used    16281
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.31
_cell_measurement_theta_min      3.79
_cell_volume                     3245.3(4)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2000-2010)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku, 2000-2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla, 2005)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku VariMax with RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18842
_diffrn_reflns_theta_full        68.21
_diffrn_reflns_theta_max         68.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288.00
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.210
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2338 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.28(27)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5445
_refine_ls_number_restraints     394
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'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_ref         0.1826
_reflns_number_gt                3668
_reflns_number_total             5445
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo500039d_si_001.cif
_cod_data_source_block           RGK1904
_cod_original_cell_volume        3245.3(5)
_cod_database_code               4037608