Synthesis and investigation of L-fuco- and D-glucurono-azafagomine
Jensen, Henrik H.; Jensen, Astrid; Hazell, Rita G.; Bols, Mikael; Journal of the Chemical Society, Perkin Transactions 1  (2002) 1190–; doi:10.1039/b200884j

data_7204358
_publ_section_title
;
 Synthesis and investigation of L-fuco- and D-glucurono-azafagomine
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1190
_journal_paper_doi               10.1039/b200884j
_journal_year                    2002
_chemical_formula_sum            'C10 H18 N2 O3'
_chemical_formula_weight         214.27
_chemical_name_systematic
;                                   
(3S,4R,5S)-1-N-Acetyl-4,5-isopropylidene-3-methyl-hexahydropyridazine
;
_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_type_scat_source           IntTabIV
_cell_angle_alpha                90.000
_cell_angle_beta                 105.899(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   6.436(1)
_cell_length_b                   10.547(2)
_cell_length_c                   8.763(2)
_cell_measurement_reflns_used    3812
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.4
_cell_volume                     572.08(19)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;                                   
ORTEP-III (Burnett & Johnson,  1996), KRYSTAL                     
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;                                   
SIR97 (Altomare et al., 1997 ), KRYSTAL                            
;
_diffrn_ambient_temperature      120
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.078
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6253
_diffrn_reflns_reduction_process 6253
_diffrn_reflns_theta_max         30.5
_diffrn_reflns_theta_min         2.4
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
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_refine_diff_density_max         0.59(7)
_refine_diff_density_min         -0.36(7)
_refine_ls_extinction_coef       19(11)
_refine_ls_extinction_method
;                                   
Type 1 Lorentzian isotropic ( Becker and Coppens, 1974)           
;
_refine_ls_goodness_of_fit_ref   1.37
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
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_refine_ls_number_reflns         2811
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.0012
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;                                   
w= 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^- |F|}^2^                           
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.046
_reflns_number_gt                2811
_reflns_number_total             3168
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            b200884j.txt
_cod_data_source_block           compound_10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 15 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:
data name '_geom_bond_atom_site_label_D' replaced with
'_geom_hbond_atom_site_label_D' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_atom_site_label_H' replaced with
'_geom_hbond_atom_site_label_H' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_atom_site_label_a' replaced with
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'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_distance_DH' replaced with '_geom_hbond_distance_DH'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_HA' replaced with
'_geom_hbond_distance_HA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_DA' replaced with
'_geom_hbond_distance_DA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_angle_DHA' replaced with '_geom_hbond_angle_DHA' as
specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_site_symmetry_A' replaced with
'_geom_hbond_site_symmetry_A' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 

The following automatic conversions were performed:

data name '_exptl_aabsorpt_process_details' was replaced with
'_exptl_absorpt_process_details' as specified in the replacement file
'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_original_cell_volume        572.1(2)
_cod_original_sg_symbol_H-M      P21
_cod_original_formula_sum        C10H18N2O3
_cod_database_code               7204358