Crystal structure of 3,4-dihydro-3-oxo-6-ethoxycarbonyl-2H-1,4-benzoxazine-2-acetate, C15H17NO6
Janina Karolak-Wojciechowska; Ma»gorzata Szczesio; Sabiha Alper-Hayta; Esin Aki; Ismail Yalçin; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 531–; doi:

data_8102775
_publ_section_title
;
 Crystal structure of
 3,4-dihydro-3-oxo-6-ethoxycarbonyl-2H-1,4-benzoxazine-2-acetate,
 C15H17NO6
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              531
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         'C15 H17 N O6'
_chemical_formula_sum            'C15 H17 N O6'
_chemical_formula_weight         307.30
_chemical_name_systematic
; 
3,4-Dihydro-3-oxo-6-ethoxycarbonyl-2<i>H</i>-1,4-benzoxazine-2-acetate

;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.681(4)
_cell_angle_beta                 84.982(3)
_cell_angle_gamma                84.376(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6096(3)
_cell_length_b                   8.3617(5)
_cell_length_c                   12.3169(5)
_cell_measurement_reflns_used    11151
_cell_measurement_temperature    290
_cell_measurement_theta_max      36.1632
_cell_measurement_theta_min      1.6770
_cell_volume                     767.60(6)
_computing_cell_refinement       'CrysAlis RED [4]'
_computing_data_collection       'CrysAlis CCD [4]'
_computing_data_reduction        'CrysAlis RED [4]'
_computing_molecular_graphics    'SHELXTL [5] and <i>Mercury</i> [6]'
_computing_publication_material  'PLATON [7]'
_computing_structure_refinement  'SHELXTL [5]'
_computing_structure_solution    'SHELXTL [5]'
_diffrn_ambient_temperature      290
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       \w
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_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            17686
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISMATIC
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.019(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2677
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+0.0812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1693
_reflns_number_gt                2152
_reflns_number_total             2677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3074.cff
_cod_data_source_block           s6
_cod_database_code               8102775