Substituted 2-Methylene-1,3-oxazolidines, -1,3-thiazolidines, -1,3-benzothiazines, -1,3-oxazines, and Substituted Imidazopyrimidinediones from Cl(CH~2~)~n~NCO and Cl(CH~2~)~n~NCS and Active Methylene Compound
Ahmad Basheer; Zvi Rappoport; Journal of Organic Chemistry 71 (2006) 9743–9750; doi:10.1021/jo061835g

data_4022190
_publ_section_title
;
 Substituted 2-Methylene-1,3-oxazolidines, -1,3-thiazolidines,
 -1,3-benzothiazines, -1,3-oxazines, and Substituted
 Imidazopyrimidinediones from Cl(CH~2~)~n~NCO and
 Cl(CH~2~)~n~NCS and Active Methylene Compound
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9743
_journal_page_last               9750
_journal_paper_doi               10.1021/jo061835g
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C10 H13 Cl N4 O3'
_chemical_formula_sum            'C10 H13 Cl N4 O3'
_chemical_formula_weight         272.69
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.1910(10)
_cell_angle_beta                 84.771(2)
_cell_angle_gamma                87.873(2)
_cell_formula_units_Z            2
_cell_length_a                   4.9308(4)
_cell_length_b                   9.6974(9)
_cell_length_c                   13.0845(12)
_cell_measurement_reflns_used    2159
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.92
_cell_measurement_theta_min      2.25
_cell_volume                     582.40(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6816
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.9737
_exptl_absorpt_correction_T_min  0.8945
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0941P)^2^+0.2707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1652
_reflns_number_gt                2204
_reflns_number_total             2704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo061835gsi20060906_044958.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
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_cod_database_code               4022190