2-Diazo-1-(1,1-dioxothiomorpholin-4-yl)ethanone
Kaupang, Åsmund; Görbitz, Carl Henrik; Hansen, Tore; Acta Crystallographica Section E 67 (2011) o1844–o1845; doi:10.1107/S1600536811023774

data_2230862
_publ_section_title
;
 2-Diazo-1-(1,1-dioxothiomorpholin-4-yl)ethanone
;
_journal_coeditor_code           SI2361
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1844
_journal_page_last               o1845
_journal_paper_doi               10.1107/S1600536811023774
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C6 H9 N3 O3 S'
_chemical_formula_moiety         'C6 H9 N3 O3 S'
_chemical_formula_sum            'C6 H9 N3 O3 S'
_chemical_formula_weight         203.22
_chemical_melting_point_gt       438
_chemical_melting_point_lt       449
_chemical_name_common            'thiomorpholine-1,1-dioxide diazoacetamide'
_chemical_name_systematic
;
2-Diazo-1-(1,1-dioxothiomorpholin-4-yl)ethanone
;
_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                 95.171(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.2729(3)
_cell_length_b                   20.1349(11)
_cell_length_c                   7.8683(4)
_cell_measurement_reflns_used    5309
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      36.6310
_cell_measurement_theta_min      2.7890
_cell_volume                     831.97(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      105(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method
'Sets of exposures each taken over 0.5\% \w rotation'
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14742
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         36.76
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.9292
_exptl_absorpt_correction_T_min  0.8486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.713
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3951
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0728P)^2^+1.0103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1651
_reflns_number_gt                3029
_reflns_number_total             3951
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2361.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2230862
_cod_database_fobs_code          2230862