Methyl [hydroxy(phenyl)phosphonomethyl]phosphonate methanol solvate
Dupont, Nathalie; Retailleau, Pascal; Migianu-Griffoni, Evelyne; Barbey, Carole; Acta Crystallographica Section E 64 (2008) o1874–o1875; doi:10.1107/S160053680802285X

data_2219676
_publ_section_title
;
 Methyl [hydroxy(phenyl)phosphonomethyl]phosphonate methanol solvate
;
_journal_coeditor_code           PK2106
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1874
_journal_page_last               o1875
_journal_paper_doi               10.1107/S160053680802285X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C8 H12 O7 P2, C H4 O'
_chemical_formula_moiety         'C8 H12 O7 P2, C H4 O'
_chemical_formula_sum            'C9 H16 O8 P2'
_chemical_formula_weight         314.16
_chemical_name_common            'hydroxy-bisphonic acid'
_chemical_name_systematic
;
Methyl [hydroxy(phenyl)phosphonomethyl]phosphonate methanol solvate
;
_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
_cell_angle_alpha                90.
_cell_angle_beta                 92.654(3)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   6.3085(5)
_cell_length_b                   6.9871(6)
_cell_length_c                   28.147(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      0.41
_cell_volume                     1239.34(17)
_computing_cell_refinement       'HKL (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'COLLECT (Hooft, 1998)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek (2003)'
_computing_publication_material
'WinGX (Farrugia, 1999) and CrystalBuilder (Welter, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            3837
_diffrn_reflns_theta_full        25.92
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         3.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2375
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0456P)^2^+3.3095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                1943
_reflns_number_total             2375
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2106.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C9 H16 O8 P2 '
_cod_database_code               2219676
_cod_database_fobs_code          2219676