4-{[3,5-Bis(methoxycarbonyl)-4,5-dihydro-1<i>H</i>-pyrazol-5-yl]methylamino}pyridine 1-oxide monohydrate
Hostetler, Katherine J.; Poole, James S.; Fanwick, Phillip E.; Acta Crystallographica Section E 62 (2006) o3015–o3016; doi:10.1107/S1600536806021970

data_2209426
_publ_section_title
;4-{[3,5-Bis(methoxycarbonyl)-4,5-dihydro-1<i>H</i>-pyrazol-5-yl]methylamino}pyridine
 1-oxide monohydrate
;
_journal_coeditor_code           BV2013
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3015
_journal_page_last               o3016
_journal_paper_doi               10.1107/S1600536806021970
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C13 H16 N4 O5, H2 O1'
_chemical_formula_moiety         'C13 H16 N4 O5, H2 O1'
_chemical_formula_sum            'C13 H18 N4 O6'
_chemical_formula_weight         326.31
_chemical_name_systematic
;4-{[3,5-Bis(methoxycarbonyl)-4,5-dihydro-1H-pyrazol-5-yl)]methylamino}pyridine
1-oxide
 monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                104.435(6)
_cell_angle_beta                 94.885(6)
_cell_angle_gamma                103.676(6)
_cell_formula_units_Z            2
_cell_length_a                   6.0678(7)
_cell_length_b                   8.7476(9)
_cell_length_c                   15.0449(18)
_cell_measurement_reflns_used    8766
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     742.57(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and PLATON (Spek, 2003)'
_computing_publication_material  'Please supply'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>,  2003)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.9841
_diffrn_measured_fraction_theta_max 0.9163
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8766
_diffrn_reflns_theta_full        27.83
_diffrn_reflns_theta_max         27.83
_diffrn_reflns_theta_min         2.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.9691
_exptl_absorpt_correction_T_min  0.9360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.064
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0806P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.122
_refine_ls_wR_factor_ref         0.131
_reflns_number_gt                1906
_reflns_number_total             2559
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            bv2013.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc' 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:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
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_database_code               2209426
_cod_database_fobs_code          2209426