Pressure-Induced Hydration of 1,4-Diazabicyclo[2.2.2]octane Hydroiodide (dabcoHI)
Olejniczak, Anna; Katrusiak, Andrzej; Crystal Growth & Design 11 (2011) 2250–; doi:10.1021/cg101653x

data_4500534
_publ_section_title
;
 Pressure-Induced Hydration of 1,4-Diazabicyclo[2.2.2]octane Hydroiodide
 (dabcoHI)
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2250
_journal_paper_doi               10.1021/cg101653x
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C6 H13 N2, H2 O, I'
_chemical_formula_sum            'C6 H15 I N2 O'
_chemical_formula_weight         258.10
_chemical_name_common
;
dabcoHI hydarte
;
_chemical_name_systematic
;
1,4-diazabicyclo[2.2.2]octanium iodide hydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7310(11)
_cell_length_b                   8.2648(14)
_cell_length_c                   9.6593(17)
_cell_measurement_pressure       1400000
_cell_measurement_reflns_used    5363
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      3.24
_cell_volume                     856.7(2)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2002)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2002)'
_computing_molecular_graphics
;X-Seed (Barbour, 2001) 
and POV-Ray (Persistence of Vision, 2004)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.395
_diffrn_measured_fraction_theta_max 0.395
_diffrn_measurement_device_type  'Kuma KM4CCD \k geometry'
_diffrn_measurement_method
;HP omega scans - for more details see:
A. Budzianowski, A. Katrusiak in High-Pressure Crystallography
(Eds.: A. Katrusiak, P. F. McMillan),
Dordrecht: Kluwer Acad. Publ., 2004 pp.157-168
;
_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  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5363
_diffrn_reflns_theta_full        29.19
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    3.679
_exptl_absorpt_correction_T_max  0.40
_exptl_absorpt_correction_T_min  0.19
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Katrusiak, A. (2003). REDSHABS - Program for correcting
reflections intensities for DAC absorption, gasket shadowing
and sample crystal absorption. Adam Mickiewicz University, Pozna\'n.
Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         490
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0473P)^2^+2.4868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                472
_reflns_number_total             490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101653x_si_002.cif
_cod_data_source_block           dabcoHIH2Ob
_cod_original_sg_symbol_H-M      'P n m a '
_cod_database_code               4500534