Cyclopentanes from N-amino-glyconolactams. A synthesis of mannostatin A
Hu, Guixian; Zimmermann, Martin; Ramana, Chepuri Venkata; Vasella, Andrea; Chemical Communications (Cambridge, United Kingdom)  (2003) 952–953; doi:10.1039/b301213a

data_7104079
_publ_section_title
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 Cyclopentanes from N-amino-glyconolactams. A synthesis of mannostatin A
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_journal_coden_ASTM              CHCOFS
_journal_issue                   8
_journal_name_full
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 Chemical Communications (Cambridge, United Kingdom)
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_journal_page_first              952
_journal_page_last               953
_journal_paper_doi               10.1039/b301213a
_journal_year                    2003
_chemical_formula_sum            'C28 H36 O7 Si'
_chemical_formula_weight         512.66
_chemical_melting_point          435.2(8)
_chemical_name_common
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1R-(1,2,3,4/5)-1,5-di-O-benzoyl-4-O-tert-Butyldimethylsilyl-
2,3-O-isopropylidene-cyclopentane-1,2,3,4,5-pentol
;
_chemical_name_systematic
; 
1R-(1,2,3,4/5)-1,5-di-O-benzoyl-4-O-tert-
Butyldimethylsilyl-2,3-O-
isopropylidene-cyclopentane-1,2,3,4,5-pentol
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.00(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.3780(10)
_cell_length_b                   19.449(5)
_cell_length_c                   11.752(3)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      19.7
_cell_volume                     1420.4(6)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        MolEN
_computing_molecular_graphics    'Ortep, Pluto'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.676
_diffrn_measured_fraction_theta_max 0.676
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       \o/2\p
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2283
_diffrn_reflns_theta_full        68.93
_diffrn_reflns_theta_max         68.93
_diffrn_reflns_theta_min         3.86
_diffrn_standards_interval_time  10000s
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         1842
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1632
_reflns_number_gt                1842
_reflns_number_total             2627
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            b301213a.txt
_cod_data_source_block           v230501
_cod_depositor_comments
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'_chemical_melting_point' value '434.5&#x0096;436' was changed to 
'435.2(8)' - the average value was taken and precision was estimated.

Adriana Da\<skevi\<c, 2007-06-14 
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_cod_original_sg_symbol_H-M      P21
_cod_database_code               7104079