Ring-fused gem-dibromocyclopropanes as precursors to enantiomerically pure D- and L-series 3-deoxy- and 2-amino-2,3-dideoxyaldohexose derivatives
Banwell, Martin G.; Ebenbeck, Wolfgang; Edwards, Alison J.; Journal of the Chemical Society, Perkin Transactions 1  (2001) 114–; doi:10.1039/b008146i

data_7213439
_publ_section_title
;
 Ring-fused gem-dibromocyclopropanes as precursors to enantiomerically
 pure D- and L-series 3-deoxy- and 2-amino-2,3-dideoxyaldohexose
 derivatives
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              114
_journal_paper_doi               10.1039/b008146i
_journal_year                    2001
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C21 H34 Br1 N1 O4 '
_chemical_formula_sum            'C21 H34 Br N O4'
_chemical_formula_weight         444.41
_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'
_audit_creation_method           'texsan v1.8 + CRYSTALS_ver_12-03-99'
_cell_angle_alpha                90
_cell_angle_beta                 108.29(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.023(2)
_cell_length_b                   11.832(2)
_cell_length_c                   10.575(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1190.8(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  CRYSTALS_ver_12-03-99
_computing_structure_refinement  CRYSTALS_ver_12-03-99
_computing_structure_solution
;
'DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      193.2
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.10128
_diffrn_orient_matrix_UB_12      0.01614
_diffrn_orient_matrix_UB_13      0.01255
_diffrn_orient_matrix_UB_21      -0.02249
_diffrn_orient_matrix_UB_22      0.01179
_diffrn_orient_matrix_UB_23      -0.09811
_diffrn_orient_matrix_UB_31      -0.01668
_diffrn_orient_matrix_UB_32      0.08212
_diffrn_orient_matrix_UB_33      0.01162
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  7.75
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4932
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.73
_diffrn_standards_decay_%        -4.33
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.54
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.24
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rect
_exptl_crystal_F_000             467.56
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.78
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details 'Flack, 3532 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.016(17)
_refine_ls_extinction_coef       10.4(16)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0910
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3396
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.000341
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 
 5.89    -5.48     4.81    -2.28    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0421
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                3396
_reflns_number_total             3532
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            b008146isup1.cif
_cod_data_source_block           mbwe1z
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1190.8
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        ' C21 H34 Br1 N1 O4 '
_cod_database_code               7213439