Hydrogen bonding in 2-(hydroxymethyl)-1,3-propanediol and <i>N</i>,<i>N</i>'-bis[2-hydroxy-1,1-bis(hydroxymethyl)ethyl]malonamide
Fernandes, Christiane; Wardell, James L.; Skakle, Janet M. S.; Acta Crystallographica Section C 58 (2002) o499–o502; doi:10.1107/S0108270102011800

data_2012901
_publ_section_title
;
 Hydrogen bonding in 2-(hydroxymethyl)-1,3-propanediol and
 <i>N</i>,<i>N</i>'-bis[2-hydroxy-1,1-bis(hydroxymethyl)ethyl]malonamide
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o499
_journal_page_last               o502
_journal_paper_doi               10.1107/S0108270102011800
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C4 H10 O3'
_chemical_formula_moiety         'C4 H10 O3'
_chemical_formula_sum            'C4 H10 O3'
_chemical_formula_weight         106.12
_chemical_name_systematic
;
2-(hydroxymethyl)-1,2-propanediol
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 107.911(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.8066(3)
_cell_length_b                   9.5179(6)
_cell_length_c                   6.1346(4)
_cell_measurement_reflns_used    1123
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     267.05(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
;ORTEX in OSCAIL (McArdle, 1994, 2000) and ORTEP-3 for Windows (Farrugia,
 1997)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Enraf-Nonius KappaCCD'
_diffrn_measurement_method       \f-\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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2166
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             116
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.157
_refine_ls_extinction_coef       0.21(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0523P)^2^+0.0278P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                504
_reflns_number_total             629
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1567.cif
_cod_data_source_block           VI
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2012901
_cod_database_fobs_code          2012901