Ethylenediammonium bis(2-carboxylato-3,4,5,6-tetrahydro-2,6,6-trimethyl-2<i>H</i>-pyran-5-carboxylic acid) dihydrate [ethylenediammonium bis(hydrogen cineolate) dihydrate]
Barnes, John C.; Acta Crystallographica Section E 59 (2003) o731–o733; doi:10.1107/S1600536803007669

data_2201915
_publ_section_title
;Ethylenediammonium
 bis(2-carboxylato-3,4,5,6-tetrahydro-2,6,6-trimethyl-2<i>H</i>-pyran-5-carboxylic
 acid) dihydrate [ethylenediammonium bis(hydrogen cineolate) dihydrate]
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o731
_journal_page_last               o733
_journal_paper_doi               10.1107/S1600536803007669
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '2C10 H15 O5 1+, C2 H10 N2 2-, 2H2 O'
_chemical_formula_moiety         '2C10 H15 O5 1+, C2 H10 N2 2-, 2H2 O'
_chemical_formula_sum            'C22 H44 N2 O12'
_chemical_formula_weight         528.60
_chemical_name_common
;
Ethylenediammonium bis(hydrogen cineolate) dihydrate
;
_chemical_name_systematic
;
Ethylenediammonium
bis(tetrahydro-2,6,6-trimethyl-1,4-pyran-2-carboxylate-
5-carboxylic acid) dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 102.938(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.5948(14)
_cell_length_b                   7.9327(4)
_cell_length_c                   12.8480(9)
_cell_measurement_reflns_used    5796
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2641.7(3)
_computing_cell_refinement       'DENZO and COLLECT'
_computing_data_collection
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)
;
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 1999) '
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Enraf--Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w scans to fill Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enraf--Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7946
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0487P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                1936
_reflns_number_total             2939
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cm6039.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2201915
_cod_database_fobs_code          2201915