Ethyl 4-(2-bromomethyl-5,5-dimethyl-1,3-dioxan-2-yl)-5-methylisoxazole-3-carboxylate
Twamley, Brendan; Szabon-Watola, Monika; Sharma, Shikha; Natale, Nicholas R.; Acta Crystallographica Section E 63 (2007) o2258–o2260; doi:10.1107/S1600536807014845

data_2213536
_publ_section_title
;Ethyl
 4-(2-bromomethyl-5,5-dimethyl-1,3-dioxan-2-yl)-5-methylisoxazole-3-carboxylate
;
_journal_coeditor_code           SG2153
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2258
_journal_page_last               o2260
_journal_paper_doi               10.1107/S1600536807014845
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C14 H20 Br N O5'
_chemical_formula_moiety         'C14 H20 Br N O5'
_chemical_formula_sum            'C14 H20 Br N O5'
_chemical_formula_weight         362.22
_chemical_melting_point          122
_chemical_name_systematic
;Ethyl
5-methyl-4-(2-bromomethyl-5,5-dimethyl-1,3-dioxan-2-yl)isoxazole-3-carboxylate
;
_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                68.299(3)
_cell_angle_beta                 72.618(3)
_cell_angle_gamma                68.573(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9698(5)
_cell_length_b                   9.3913(5)
_cell_length_c                   11.1474(6)
_cell_measurement_reflns_used    8230
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.43
_cell_volume                     797.51(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'publCIF (Westrip, 2007)'
_computing_structure_refinement  'XL in SHELXTL'
_computing_structure_solution    'XS in SHELXTL (Bruker, 2003)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker--Siemens SMART APEX'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13695
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    2.597
_exptl_absorpt_correction_T_max  0.8598
_exptl_absorpt_correction_T_min  0.5516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0471P)^2^+1.3295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                2712
_reflns_number_total             2891
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg2153.cif
_cod_data_source_block           I
_cod_database_code               2213536
_cod_database_fobs_code          2213536