A perdeuterated cryoprotectant for neutron studies and a demonstration of its use for neutron powder diffraction onL-(−)-ephedrine hemihydrate
Krebs, Frederik C.; Jørgensen, Mikkel; Lebech, Bente; Frydenvang, Karla; Journal of Applied Crystallography 34 (2001) 203–; doi:10.1107/S0021889800018987

data_2300392
_publ_section_title
;
 A perdeuterated cryoprotectant for neutron studies and a demonstration of
 its use for neutron powder diffraction onL-(&#x2212;)-ephedrine
 hemihydrate
;
_journal_issue                   2
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              203
_journal_paper_doi               10.1107/S0021889800018987
_journal_volume                  34
_journal_year                    2001
_chemical_formula_sum            'C10 H16 N O1.5'
_chemical_formula_weight         174.24
_chemical_name_common            'L-(-)Ephedrine hemihydrate'
_chemical_name_systematic
; 
 (1R,2S)-(-)-2-(N-methylamino)-1-phenylpropan-1-ol hemihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.3188(4)
_cell_length_b                   11.2018(6)
_cell_length_c                   24.0156(14)
_cell_measurement_temperature    120(2)
_cell_volume                     1968.89(19)
_computing_cell_refinement       'SAINT Siemens'
_computing_data_collection       'SMART Siemens'
_computing_data_reduction        'SAINT Siemens'
_computing_molecular_graphics    'SHELXTL (Sheldrick)'
_computing_publication_material  'XCIF (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'omega scan, frame data integration'
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25990
_diffrn_reflns_theta_full        30.40
_diffrn_reflns_theta_max         30.40
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                4623
_reflns_number_total             5596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            do0003sup1.cif
_cod_data_source_block           Xray
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               2300392