Reversible <i>chair</i> {łeftrightarrow} <i>skew</i> conformational interconversion of 1,3,2-dioxaphosphorinane ring in the solid state
Ślepokura, Katarzyna Anna; Acta Crystallographica Section B 72 (2016) 117–125; doi:10.1107/S2052520615020259

data_2107467
_publ_section_title
;
 Reversible <i>chair</i> {\/leftrightarrow} <i>skew</i> conformational
 interconversion of 1,3,2-dioxaphosphorinane ring in the solid state
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              117
_journal_page_last               125
_journal_paper_doi               10.1107/S2052520615020259
_journal_volume                  72
_journal_year                    2016
_chemical_formula_moiety         'C5 H10 O6 P, H4 N'
_chemical_formula_sum            'C5 H14 N O6 P'
_chemical_formula_weight         215.14
_chemical_melting_point          446(2)
_chemical_name_common
;
 ammonium salt of 
 1,3-cyclic dihydroxyacetone phosphate dimethyl acetal
;
_chemical_name_systematic
;
 ammonium 
 5,5-dimethoxy-2-oxo-1,3,2-dioxaphosphorinan-2-olate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                105.60(3)
_cell_angle_beta                 97.50(3)
_cell_angle_gamma                90.17(3)
_cell_formula_units_Z            24
_cell_length_a                   11.336(3)
_cell_length_b                   20.486(5)
_cell_length_c                   25.369(6)
_cell_measurement_reflns_used    15395
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.50
_cell_measurement_theta_min      2.22
_cell_volume                     5621(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type
;
Xcalibur PX kappa-geometry diffractometer with an Onyx 
CCD camera 
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            77940
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.229
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1568
_refine_ls_number_reflns         32235
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0160P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14062
_reflns_number_total             32235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wf5120sup1.cif
_cod_data_source_block           LTP_sl8lt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '444-448' was changed to '446(2)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 2107464--2107467.cif.

 Adding full bibliography for 2107464--2107467.cif.
;
_cod_database_code               2107467
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.983
_shelxl_version_number           2013-4
_shelx_res_checksum              18434
_shelx_hkl_checksum              73253