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_1508370
_publ_section_title
;
 Supramolecular Hydrogen-Bond Motifs in Chiral and Racemic Molecular
 Salts: A Comparison of (S)-2-Methyl Piperizinium Hydrogen Phosphite
 Monohydrate, C5H14N2&#x00B7;HPO3&#x00B7;H2O and (R,S)-2-Methyl
 Piperizinium Hydrogen Phosphite 2.23 Hydrate,
 C5H14N2&#x00B7;HPO3&#x00B7;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_formula_moiety         'C5 H14 N2, H O3 P, 2.230(H2 O)'
_chemical_formula_sum            'C5 H19.47 N2 O5.24 P'
_chemical_formula_weight         222.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   31.075(2)
_cell_length_b                   31.075(2)
_cell_length_c                   6.1875(4)
_cell_measurement_reflns_used    2123
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.42
_cell_measurement_theta_min      2.27
_cell_volume                     5174.5(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            11694
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2167
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                1419
_reflns_number_total             2270
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file
C5H19.47N2O5.24P_crystals-01-00236-s001_R_3_DC114.cif
_cod_data_source_block           wh415a_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_sg_symbol_H-M      'R -3'
_cod_database_code               1508370