Hydrogen-bonded bilayers in piperazinium(2+) bis(mandelate) bis(methanol) solvate
Farrell, Dorcas M. M.; Ferguson, George; Lough, Alan J.; Glidewell, Christopher; Acta Crystallographica Section C 57 (2001) 955–957; doi:10.1107/S0108270101007922

data_2012163
_publ_section_title
;
 Hydrogen-bonded bilayers in piperazinium(2+) bis(mandelate)
 bis(methanol) solvate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              955
_journal_page_last               957
_journal_paper_doi               10.1107/S0108270101007922
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C4 H12 N2 2+ , 2C8 H7 O3 - , 2C H4 O'
_chemical_formula_sum            'C22 H34 N2 O8'
_chemical_formula_weight         454.51
_chemical_name_systematic
;
Piperazinium(2+) bis(mandelate) bis(methanol) solvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7360(2)
_cell_length_b                   10.2394(4)
_cell_length_c                   29.7822(11)
_cell_measurement_reflns_used    2290
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.74
_cell_volume                     2359.11(14)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2000)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'SHELXL97 and  PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .089
_diffrn_reflns_av_sigmaI/netI    .094
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            11737
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    .097
_exptl_absorpt_correction_T_max  .988
_exptl_absorpt_correction_T_min  .973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .12
_refine_diff_density_max         .19
_refine_diff_density_min         -.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2074
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      .909
_refine_ls_R_factor_all          .127
_refine_ls_R_factor_gt           .048
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0694P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .133
_reflns_number_gt                1077
_reflns_number_total             2074
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1483.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'Pb c a'
_cod_database_code               2012163
_cod_database_fobs_code          2012163