Morpholinium hydrogen chloranilate methanol monosolvate
Gotoh, Kazuma; Tahara, Yuki; Ishida, Hiroyuki; Acta Crystallographica Section E 67 (2011) o3335–; doi:10.1107/S1600536811047891

data_2232852
_publ_section_title
;
 Morpholinium hydrogen chloranilate methanol monosolvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3335
_journal_paper_doi               10.1107/S1600536811047891
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C4 H10 N O +, C6 H Cl2 O4 -, C H4 O'
_chemical_formula_moiety         'C4 H10 N O, C6 H Cl2 O4, C H4 O'
_chemical_formula_sum            'C11 H15 Cl2 N O6'
_chemical_formula_weight         328.15
_chemical_name_common
;
Morpholinium hydrogen chloranilate methanol monosolvate
;
_chemical_name_systematic
;
Morpholin-1-ium 2,5-dichloro-4-hydroxy-3,6-dioxocyclohexa-1,4-dien-1-olate
methanol monosolvate
;
_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
_cell_angle_alpha                107.8089(7)
_cell_angle_beta                 107.5510(7)
_cell_angle_gamma                110.2398(7)
_cell_formula_units_Z            2
_cell_length_a                   9.11845(17)
_cell_length_b                   9.39881(17)
_cell_length_c                   9.96935(18)
_cell_measurement_reflns_used    16546
_cell_measurement_temperature    170.0(10)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      3.6
_cell_volume                     679.25(2)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku/MSC, 2004)'
_computing_data_collection       'PROCESS-AUTO (Rigaku/MSC, 2004)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.0(10)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17817
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(NUMABS; Higashi, 1999)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0459P)^2^+0.1482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                3636
_reflns_number_total             3928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            lh5377.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C11 H15 Cl2 N O6 '
_cod_database_code               2232852
_cod_database_fobs_code          2232852