(<i>R</i>)-Methyl {[(2-carboxybicyclo[2.2.2]octan-1-yl)ammonio]methyl}phosphonate dichloromethane 0.25-solvate
Todorov, Petar; Calmes, Monique; Shivachev, Boris L.; Nikolova, Rosica P.; Acta Crystallographica Section E 67 (2011) o2152–o2153; doi:10.1107/S1600536811029503

data_2231171
_publ_section_title
;
 (<i>R</i>)-Methyl
 {[(2-carboxybicyclo[2.2.2]octan-1-yl)ammonio]methyl}phosphonate
 dichloromethane 0.25-solvate
;
_journal_coeditor_code           IS2751
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2152
_journal_page_last               o2153
_journal_paper_doi               10.1107/S1600536811029503
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C11 H20 N O5 P, 0.25C H2 Cl2'
_chemical_formula_moiety         'C11 H20 N O5 P, 0.25(C H2 Cl2)'
_chemical_formula_sum            'C11.25 H20.5 Cl0.5 N O5 P'
_chemical_formula_weight         298.48
_chemical_name_systematic
;
(<i>R</i>)-Methyl
{[(2-carboxybicyclo[2.2.2]octan-1-yl)ammonio]methyl}phosphonate
dichloromethane 0.25-solvate
;
_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   geom
_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            8
_cell_length_a                   9.3520(2)
_cell_length_b                   12.7553(3)
_cell_length_c                   24.1148(8)
_cell_measurement_reflns_used    5494
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      62.5517
_cell_measurement_theta_min      3.4622
_cell_volume                     2876.60(13)
_computing_cell_refinement
;
<i>CrysAlis PRO</i> (Agilent, 2010)
;
_computing_data_collection
;
<i>CrysAlis PRO</i> (Agilent, 2010)
;
_computing_data_reduction
;
<i>CrysAlis PRO</i> (Agilent, 2010)
;
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
WinGX (Farrugia, 1999) and <i>Mercury</i> (Macrae <i>et al.</i>,
2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290
_diffrn_detector_area_resol_mean 10.3974
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Agilent SuperNova Dual diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11759
_diffrn_reflns_theta_full        62.64
_diffrn_reflns_theta_max         62.64
_diffrn_reflns_theta_min         3.67
_exptl_absorpt_coefficient_mu    2.703
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_correction_T_min  0.151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i>; Agilent, 2010)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.335
_refine_ls_abs_structure_details 'Flack (1983), 1914 Friedel paris'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0704
_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^)+(0.1029P)^2^+1.5603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.2046
_reflns_number_gt                3305
_reflns_number_total             4532
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            is2751.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C11.25 H20.5 Cl0.5 N1 O5 P1'
_cod_database_code               2231171
_cod_database_fobs_code          2231171