Crystal structures of morpholinium hydrogen bromanilate at 130, 145 and 180K
Gotoh, Kazuma; Tahara, Yuki; Ishida, Hiroyuki; Acta Crystallographica Section E 71 (2015) 1226–1229; doi:10.1107/S2056989015017272

data_2241103
_publ_section_title
;
 Crystal structures of morpholinium hydrogen bromanilate at 130, 145 and
 180K
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1226
_journal_page_last               1229
_journal_paper_doi               10.1107/S2056989015017272
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C4 H10 N O +, C6 H Br2 O4 -'
_chemical_formula_moiety         'C4 H10 N O +, C6 H Br2 O4 -'
_chemical_formula_sum            'C10 H11 Br2 N O5'
_chemical_formula_weight         385.01
_chemical_name_common
;
Morpholinium hydrogen bromanilate
;
_chemical_name_systematic
;
Morpholin-4-ium 2,5-dibromo-4-hydroxy-3,6-dioxocyclohexa-1,4-dien-1-olate
;
_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   mixed
_cell_angle_alpha                93.5208(7)
_cell_angle_beta                 112.9139(7)
_cell_angle_gamma                115.9757(7)
_cell_formula_units_Z            2
_cell_length_a                   8.62046(19)
_cell_length_b                   9.2129(2)
_cell_length_c                   9.4257(2)
_cell_measurement_reflns_used    15996
_cell_measurement_temperature    130.0(10)
_cell_measurement_theta_max      30.11
_cell_measurement_theta_min      3.00
_cell_volume                     595.05(2)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 2012)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2010) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>, 1994)
;
_diffrn_ambient_temperature      130.0(10)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPIDII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18162
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.026
_diffrn_reflns_theta_min         3.005
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.844
_exptl_absorpt_correction_T_max  0.292
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(NUMABS; Higashi, 1999)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.368
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3468
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+0.3723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0456
_reflns_number_gt                3183
_reflns_number_total             3468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5788sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        595.05(3)
_cod_database_code               2241103
_shelx_hkl_checksum              35705
_shelx_res_checksum              5173
_cod_database_fobs_code 2241103