4-Carboxypiperidinium 1-carboxycyclobutane-1-carboxylate
Belandria, Lusbely M.; Mora, Asiloé J.; Delgado, Gerzon E.; Briceño, Alexander; Acta Crystallographica Section C 68 (2012) o88–o91; doi:10.1107/S0108270111054977

data_2018386
_publ_section_title
;
 4-Carboxypiperidinium 1-carboxycyclobutane-1-carboxylate
;
_journal_coeditor_code           SF3160
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o88
_journal_page_last               o91
_journal_paper_doi               10.1107/S0108270111054977
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C6 H12 N O2 + , C6 H7 O4 -'
_chemical_formula_moiety         'C6 H12 N O2 +, C6 H7 O4 -'
_chemical_formula_sum            'C12 H19 N O6'
_chemical_formula_weight         273.28
_chemical_melting_point          555.3
_chemical_name_systematic
;
4-Carboxypiperidinium 1-carboxycyclobutane-1-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 91.060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.027(2)
_cell_length_b                   20.776(5)
_cell_length_c                   8.949(2)
_cell_measurement_reflns_used    2561
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      1.96
_cell_volume                     1306.3(6)
_computing_cell_refinement       'CrystalStructure (Rigaku/MSC, 2004)'
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1998)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2008 (Burla <i>et al.</i>, 2007)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_device
;
Mercury (2x2 bin mode)
;
_diffrn_measurement_device_type  'Rigaku AFC-7S Mercury'
_diffrn_measurement_method       '\w '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14962
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Jacobson, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lamellar
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.299
_refine_ls_extinction_coef       0.028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0657P)^2^+0.6501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                2026
_reflns_number_total             2561
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3160.cif
_cod_data_source_block           I
_cod_original_cell_volume        1306.2(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018386
_cod_database_fobs_code          2018386