Supramolecular Hydrogen-Bond Motifs in Chiral and Racemic Molecular Salts: A Comparison of (S)-2-Methyl Piperizinium Hydrogen Phosphite Monohydrate, C5H14N2 HPO3 H2O and (R,S)-2-Methyl Piperizinium Hydrogen Phosphite 2.23 Hydrate, C5H14N2 HPO3 2 23H2O
Harrison, William T. A.; Crystals 1 (2011) 236–243; doi:10.3390/cryst1040236

data_1508371
_publ_section_title
;
 Supramolecular Hydrogen-Bond Motifs in Chiral and Racemic Molecular
 Salts: A Comparison of (S)-2-Methyl Piperizinium Hydrogen Phosphite
 Monohydrate, C5H14N2 HPO3 H2O and (R,S)-2-Methyl Piperizinium Hydrogen
 Phosphite 2.23 Hydrate, C5H14N2 HPO3 2 23H2O
;
_journal_issue                   4
_journal_name_full               Crystals
_journal_page_first              236
_journal_page_last               243
_journal_paper_doi               10.3390/cryst1040236
_journal_volume                  1
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C5 H14 N2, H O3 P, H2 O'
_chemical_formula_sum            'C5 H17 N2 O4 P'
_chemical_formula_weight         200.18
_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   mixed
_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            4
_cell_length_a                   8.564(5)
_cell_length_b                   9.593(6)
_cell_length_c                   11.607(6)
_cell_measurement_reflns_used    237
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.21
_cell_measurement_theta_min      2.96
_cell_volume                     953.6(10)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_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  0.2468
_diffrn_reflns_av_sigmaI/netI    0.2079
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5970
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.785
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.785
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0035P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                507
_reflns_number_total             1104
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file
C5H17N2O4P_crystals-01-00236-s002_P212121_DC115.cif
_cod_data_source_block           wh426a_chateigner
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap and geom' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        953.6(9)
_cod_database_code               1508371