Crystal structures of the dioxane hemisolvates of <i>N</i>-(7-bromomethyl-1,8-naphthyridin-2-yl)acetamide and bis[<i>N</i>-(7-dibromomethyl-1,8-naphthyridin-2-yl)acetamide]
Rosin, Robert; Seichter, Wilhelm; Mazik, Monika; Acta Crystallographica Section E 73 (2017) 1409–1413; doi:10.1107/S2056989017012208

data_2242300
_publ_section_title
;
 Crystal structures of the dioxane hemisolvates of
 <i>N</i>-(7-bromomethyl-1,8-naphthyridin-2-yl)acetamide and
 bis[<i>N</i>-(7-dibromomethyl-1,8-naphthyridin-2-yl)acetamide]
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1409
_journal_page_last               1413
_journal_paper_doi               10.1107/S2056989017012208
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C11 H10 Br N3 O, 0.5C4 H8 O2'
_chemical_formula_moiety         'C11 H10 Br N3 O, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C13 H14 Br N3 O2'
_chemical_formula_weight         324.19
_chemical_name_systematic
;
<i>N</i>-(7-Bromomethyl-1,8-naphthyridin-2-yl)acetamide dioxane hemisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 106.310(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8863(10)
_cell_length_b                   7.6256(7)
_cell_length_c                   16.5300(15)
_cell_measurement_reflns_used    1901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      3.31
_cell_volume                     1317.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9345
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.703
_diffrn_reflns_theta_min         1.949
_exptl_absorpt_coefficient_mu    3.123
_exptl_absorpt_correction_T_max  0.8351
_exptl_absorpt_correction_T_min  0.4168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       needle
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.850
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2493
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+4.7912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                1965
_reflns_number_total             2493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5386sup1.cif
_cod_data_source_block           I
_cod_database_code               2242300
_cod_database_fobs_code          2242300
_shelx_estimated_absorpt_t_min   0.417
_shelx_estimated_absorpt_t_max   0.835
_shelx_hkl_checksum              57351
_shelx_res_checksum              32357
_shelxl_version_number           .2013