Four-centre hydrogen bonds: a triethanolamine–triethanolamine oxide complex
Kemmitt, Tim; Gainsford, Graeme J.; Steel, Peter J.; Wikaira, Jan; Acta Crystallographica Section E 58 (2002) o851–o852; doi:10.1107/S1600536802012175

data_2201632
_publ_section_title
;
 Four-centre hydrogen bonds: a triethanolamine--triethanolamine oxide
 complex
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o851
_journal_page_last               o852
_journal_paper_doi               10.1107/S1600536802012175
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C6 H15 N O4, C6 H15 N O3'
_chemical_formula_moiety         'C6 H15 N O4, C6 H15 N O3'
_chemical_formula_sum            'C12 H30 N2 O7'
_chemical_formula_weight         314.38
_space_group_IT_number           146
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.065(5)
_cell_length_b                   12.065(5)
_cell_length_c                   9.633(8)
_cell_measurement_reflns_used    330
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      21.9
_cell_measurement_theta_min      2.9
_cell_volume                     1214.4(12)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction
'SAINT (Siemens, 1996) and SADABS (Sheldrick, 1996)'
_computing_molecular_graphics    'ORTEP-3 in WinGX (Farrugia, 1997, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      168(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.759
_diffrn_measured_fraction_theta_max 0.759
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \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  0.211
_diffrn_reflns_av_sigmaI/netI    0.170
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1170
_diffrn_reflns_theta_full        26.4
_diffrn_reflns_theta_max         26.4
_diffrn_reflns_theta_min         2.9
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.30
_refine_ls_abs_structure_details 'not determined'
_refine_ls_extinction_coef       0.016(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   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         422
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.097
_refine_ls_R_factor_gt           0.061
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.038P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.113
_refine_ls_wR_factor_ref         0.134
_reflns_number_gt                299
_reflns_number_total             422
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6067.cif
_cod_data_source_block           I
_cod_original_cell_volume        1214.4(13)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               2201632
_cod_database_fobs_code          2201632