Betaine 0.77-perhydrate 0.23-hydrate and common structural motifs in crystals of amino acid perhydrates
Minkov, Vasily S.; Kapustin, Evgeny A.; Boldyreva, Elena V.; Acta Crystallographica Section C 69 (2013) 416–420; doi:10.1107/S0108270113005386

data_2018909
_publ_section_title
;
 Betaine 0.77-perhydrate 0.23-hydrate and common structural motifs in
 crystals of amino acid perhydrates
;
_journal_coeditor_code           KU3089
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              416
_journal_page_last               420
_journal_paper_doi               10.1107/S0108270113005386
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C5 H11 N O2 , 0.77H2 O2 , 0.23H2 O'
_chemical_formula_moiety         'C5 H11 N O2, 0.77(H2 O2), 0.23(H2 O)'
_chemical_formula_sum            'C5 H13 N O3.77'
_chemical_formula_weight         147.44
_chemical_name_common            'Betaine 0.77-perhydrate 0.23-hydrate'
_chemical_name_systematic
;
2-(Trimethylazaniumyl)acetate 0.77-perhydrate 0.23-hydrate
;
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5819(2)
_cell_length_b                   6.78424(14)
_cell_length_c                   11.7152(3)
_cell_measurement_reflns_used    4289
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      31.8685
_cell_measurement_theta_min      2.1211
_cell_volume                     761.56(3)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008) and ORTEP-3 (Farrugia,
2012)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Gemini Ultra R'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13549
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.9862
_exptl_absorpt_correction_T_min  0.8802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             320.5
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.101
_refine_diff_density_min         -0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2325
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0808
_reflns_number_gt                2054
_reflns_number_total             2325
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ku3089.cif
_cod_data_source_block           I_295K
_cod_database_code               2018909
_cod_database_fobs_code          2018909