Asymmetric total synthesis of sperabillins B and D via lithium amide conjugate addition
Davies, Stephen G.; Haggitt, Jane R.; Ichihara, Osamu; Kelly, Richard J.; Leech, Michael A.; Price Mortimer, Anne J.; Roberts, Paul M.; Smith, Andrew D.; Organic & Biomolecular Chemistry 2 (2004) 2630–2649; doi:10.1039/b404962d

data_7153517
_publ_section_title
;
 Asymmetric total synthesis of sperabillins B and D via lithium amide
 conjugate addition
;
_journal_issue                   18
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              2630
_journal_page_last               2649
_journal_paper_doi               10.1039/b404962d
_journal_volume                  2
_journal_year                    2004
_chemical_absolute_configuration unk
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C8 H16 N2 O5 '
_chemical_formula_sum            'C8 H16 N2 O5'
_chemical_formula_weight         220.23
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-15-03
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.804(1)
_cell_length_b                   11.033(1)
_cell_length_c                   15.991(1)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1024.0(2)
_computing_cell_refinement
;
USER DEFINED 6
;
_computing_data_collection
;
DATA COLLECTION
;
_computing_data_reduction
;
USER DEFINED 5
;
_computing_molecular_graphics
;
CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
USER DEFINED 7
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type
;
Unknown
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1196
_diffrn_reflns_theta_full        25.320
_diffrn_reflns_theta_max         26.513
_diffrn_reflns_theta_min         2.243
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             472.000
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1159
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000202
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin,
1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

1.59 -1.68 1.19 -0.593
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0311
_refine_ls_wR_factor_gt          0.0309
_refine_ls_wR_factor_ref         0.0309
_reflns_limit_h_max              7
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                1159
_reflns_number_total             1196
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b404962dsup1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1023.99225(4)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        ' C8 H16 N2 O5 '
_cod_database_code               7153517