1-Oxo-<i>N</i>-(2-pyridyl)-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane-4-carboxamide
Guo-Feng Chen; Jing Hu; Guo-Chun Ma; Acta Crystallographica Section E 63 (2007) o4894–o4894; doi:10.1107/S160053680706120X

data_2216425
_publ_section_title
1-Oxo-<i>N</i>-(2-pyridyl)-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane-4-carboxamide
_journal_coeditor_code           DN2280
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4894
_journal_page_last               o4894
_journal_paper_doi               10.1107/S160053680706120X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C10 H11 N2 O5 P'
_chemical_formula_moiety         'C10 H11 N2 O5 P'
_chemical_formula_sum            'C10 H11 N2 O5 P'
_chemical_formula_weight         270.18
_chemical_melting_point          504.0(10)
_chemical_name_systematic
;
1-Oxo-N-(2-pyridyl)-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane-4-carboxamide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.427(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.915(3)
_cell_length_b                   11.960(6)
_cell_length_c                   17.678(8)
_cell_measurement_reflns_used    1990
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.87
_cell_volume                     1250.6(11)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997)
and PLATON (Spek, 2003)
;
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6101
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.4588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                1533
_reflns_number_total             2190
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2280.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_cell_volume        1250.5(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C10 H11 N2 O5 P '
_cod_database_code               2216425
_cod_database_fobs_code          2216425