Acidic and anionic forms of 1,3-cyclic dihydroxyacetone phosphate (cDHAP) dimethyl acetal
Ślepokura, Katarzyna; Mitaszewska, Irmina; Acta Crystallographica Section C 67 (2011) o161–o165; doi:10.1107/S0108270111011723

data_2018071
_publ_section_title
;
 Acidic and anionic forms of 1,3-cyclic dihydroxyacetone phosphate
 (cDHAP) dimethyl acetal
;
_journal_coeditor_code           MX3045
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o161
_journal_page_last               o165
_journal_paper_doi               10.1107/S0108270111011723
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C6 H14 N + , C5 H10 O6 P -'
_chemical_formula_moiety         'C5 H10 O6 P, C6 H14 N'
_chemical_formula_sum            'C11 H24 N O6 P'
_chemical_formula_weight         297.28
_chemical_name_common
;
cyclic dihydroxyacetone phosphate (cDHAP) dimethyl acetal
cyclohexylammonium salt
;
_chemical_name_systematic
;
cyclohexylammonium 5,5-dimethoxy-2-oxo-1,3,2-dioxaphosphinane-2-olate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.678(2)
_cell_length_b                   8.877(2)
_cell_length_c                   24.930(6)
_cell_measurement_reflns_used    5357
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      76.42
_cell_measurement_theta_min      3.54
_cell_volume                     1477.9(7)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'XP (Bruker, 1998)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur PX \k-geometry diffractometer
with an Onyx CCD camera
;
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11210
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         76.23
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    1.863
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.209
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                1876
_reflns_number_total             2803
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            mx3045.cif
_cod_data_source_block           5j
_cod_database_code               2018071
_cod_database_fobs_code          2018071