2,2-Dimethyl-5-nitroso-1,3-dioxan-5-yl benzoate, 2,2-dimethyl-5-nitroso-1,3-dioxan-5-yl 4-chlorobenzoate and 5-nitroso-1,3-dioxan-5-yl 4-chlorobenzoate
Calvet, Géraldine; Blanchard, Nicolas; Kouklovsky, Cyrille; Guillot, Régis; Acta Crystallographica Section C 63 (2007) o365–o368; doi:10.1107/S0108270107021804

data_2015979
_publ_section_title
;
 2,2-Dimethyl-5-nitroso-1,3-dioxan-5-yl benzoate,
 2,2-dimethyl-5-nitroso-1,3-dioxan-5-yl 4-chlorobenzoate and
 5-nitroso-1,3-dioxan-5-yl 4-chlorobenzoate
;
_journal_coeditor_code           GA3047
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o365
_journal_page_last               o368
_journal_paper_doi               10.1107/S0108270107021804
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C13 H15 N O5'
_chemical_formula_moiety         'C13 H15 N O5'
_chemical_formula_sum            'C13 H15 N O5'
_chemical_formula_weight         265.26
_chemical_name_systematic
;
2,2-Dimethyl-5-nitroso-1,3-dioxan-5-yl benzoate
;
_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                 100.495(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.2809(5)
_cell_length_b                   21.9393(19)
_cell_length_c                   9.6452(9)
_cell_measurement_reflns_used    6252
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      2.34
_cell_volume                     1306.9(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT  (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3.2 (Brueggemann & Schmid, 1990)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Bruker SMART APEX II area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21059
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.405
_refine_ls_extinction_coef       0.069(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+0.3535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                2914
_reflns_number_total             3401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ga3047.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2015979
_cod_database_fobs_code          2015979