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_2242301
_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          '2C11 H9 Br2 N3 O, 0.5C4 H8 O2'
_chemical_formula_moiety         '2(C11 H9 Br2 N3 O), 0.5(C4 H8 O2)'
_chemical_formula_sum            'C24 H22 Br4 N6 O3'
_chemical_formula_weight         762.11
_chemical_name_systematic
;
Bis[<i>N</i>-(7-dibromomethyl-1,8-naphthyridin-2-yl)acetamide] dioxane
hemisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                88.777(3)
_cell_angle_beta                 81.057(2)
_cell_angle_gamma                64.928(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4065(5)
_cell_length_b                   9.5271(5)
_cell_length_c                   16.6464(10)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.36
_cell_volume                     1333.15(13)
_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 0.984
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32569
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.896
_diffrn_reflns_theta_min         2.363
_exptl_absorpt_coefficient_mu    6.077
_exptl_absorpt_correction_T_max  0.6111
_exptl_absorpt_correction_T_min  0.1948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.795
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5659
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+4.6947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                5247
_reflns_number_total             5659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5386sup1.cif
_cod_data_source_block           II
_cod_database_code               2242301
_cod_database_fobs_code          2242301
_shelx_estimated_absorpt_t_min   0.195
_shelx_estimated_absorpt_t_max   0.611
_shelx_hkl_checksum              98003
_shelx_res_checksum              95674
_shelxl_version_number           .2013