3-Methoxy-3-oxopropanaminium chloride
Gruber, Tobias; Schofield, Christopher J.; Thompson, Amber L.; Acta Crystallographica Section E 68 (2012) o595–; doi:10.1107/S1600536812003297

data_2233922
_publ_section_title
;
 3-Methoxy-3-oxopropanaminium chloride
;
_journal_coeditor_code           LH5384
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o595
_journal_paper_doi               10.1107/S1600536812003297
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C4 H10 N O2 +, Cl -'
_chemical_formula_moiety         'C4 H10 N O2 +, Cl -'
_chemical_formula_sum            'C4 H10 Cl N O2'
_chemical_formula_weight         139.58
_chemical_name_systematic
;
3-Methoxy-3-oxopropanaminium chloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 99.4638(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8469(2)
_cell_length_b                   5.32630(10)
_cell_length_c                   13.2804(2)
_cell_measurement_reflns_used    1729
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     687.04(2)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material
'CRYSTALS (Betteridge <i>et al.</i>, 2003) and PLATON (Spek, 2009)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14336
_diffrn_reflns_theta_full        27.484
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         5.158
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1563
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.0008315
_refine_ls_shift/su_mean         0.0000573
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994; Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are: 37.6 62.5 38.0 16.9 4.31
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0803
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                1413
_reflns_number_total             1563
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5384.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C4 H10 Cl1 N1 O2'
_cod_database_code               2233922
_cod_database_fobs_code          2233922