(4<i>S</i>,5<i>R</i>,6<i>R</i>)-Methyl 4-hydroxy-4,5-isopropylidenedioxy-4,5,6,7-tetrahydro-1,2,3-triazolo[1,5-<i>a</i>]pyridine-3-carboxylate
Jenkinson, Sarah F.; Fenton, Jennifer R.; Booth, K. Victoria; Fleet, George W. J.; Watkin, David J.; Acta Crystallographica Section E 65 (2009) o610–o611; doi:10.1107/S1600536809006357

data_2221139
_publ_section_title
;(4<i>S</i>,5<i>R</i>,6<i>R</i>)-Methyl
 4-hydroxy-4,5-isopropylidenedioxy-4,5,6,7-tetrahydro-1,2,3-triazolo[1,5-<i>a</i>]pyridine-3-carboxylate
;
_journal_coeditor_code           LH2778
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o610
_journal_page_last               o611
_journal_paper_doi               10.1107/S1600536809006357
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C11 H15 N3 O5'
_chemical_formula_moiety         'C11 H15 N3 O5'
_chemical_formula_sum            'C11 H15 N3 O5'
_chemical_formula_weight         269.26
_chemical_name_systematic
;
(4<i>S</i>,5<i>R</i>,6<i>R</i>)-Methyl
4-hydroxy-4,5-isopropylidenedioxy-4,5,6,7-tetrahydro-1,2,3-
triazolo[1,5-<i>a</i>]pyridine-3-carboxylate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 96.2740(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0587(3)
_cell_length_b                   7.3797(3)
_cell_length_c                   10.9785(5)
_cell_measurement_reflns_used    1565
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     648.99(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>,  1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9525
_diffrn_reflns_theta_full        27.498
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         5.228
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.31
_refine_ls_extinction_coef       12E1(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9645
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1595
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.000083
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method = Modified Sheldrick
w=1/[\s^2^(F^2^)+(0.04P)^2^+0.06P], where P=[max(Fo^2^,0)+2Fc^2^]/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0815
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                1219
_reflns_number_total             1595
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2778.cif
_cod_data_source_block           I
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2221139
_cod_database_fobs_code          2221139