Montanastatin, cyclo[‒(Val-<small>D</small>-Hyv-<small>D</small>-Val-Lac)~2~‒]
Mitsunobu Doi; Akiko Asano; Acta Crystallographica Section E 58 (2002) o935–o936; doi:10.1107/S1600536802013259

data_2201562
_publ_section_title
;
 Montanastatin,
 cyclo[--(Val-<small>D</small>-Hyv-<small>D</small>-Val-Lac)~2~--]
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o935
_journal_page_last               o936
_journal_paper_doi               10.1107/S1600536802013259
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C36 H60 N4 O12'
_chemical_formula_moiety         'C36 H60 N4 O12'
_chemical_formula_sum            'C36 H60 N4 O12'
_chemical_formula_weight         740.88
_chemical_name_common            mont2
_chemical_name_systematic
;
 Montanastatin: cyclo(-Val-D-Hyv-D-Val-Lac-)2,
 Hyv=alpha-hydroxyisovaleric acid, Lac=lactic acid
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.488(6)
_cell_length_b                   17.868(7)
_cell_length_c                   16.452(7)
_cell_measurement_reflns_used    3994
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.25
_cell_volume                     3965(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD'
_diffrn_measurement_method       \w
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13003
_diffrn_reflns_theta_full        28.60
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0.36
_diffrn_standards_interval_time  167
_diffrn_standards_number         144
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.8543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.217
_refine_ls_abs_structure_details '(Flack, 1983), 1912 Friedel pairs'
_refine_ls_abs_structure_Flack   0.1(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0472P)^2^+1.956P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                4545
_reflns_number_total             4717
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6157.cif
_cod_data_source_block           I
_cod_database_code               2201562
_cod_database_fobs_code          2201562