Pressure induced transformations of 1,4-diazabicyclo[2.2.2]octane (dabco) hydroiodide: diprotonation of dabco, its N-methylation and co-crystallization with methanol
Olejniczak, Anna; Katrusiak, Andrzej; CrystEngComm 12 (2010) 2528–; doi:10.1039/c001379j

data_7212551
_publ_section_title
;
 Pressure induced transformations of 1,4-diazabicyclo[2.2.2]octane (dabco)
 hydroiodide: diprotonation of dabco, its N-methylation and
 co-crystallization with methanol
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              2528
_journal_paper_doi               10.1039/c001379j
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C6 H14 N2, 3(C H4 O), 2(I)'
_chemical_formula_sum            'C9 H26 I2 N2 O3'
_chemical_formula_weight         464.12
_chemical_name_common
;1,4-diazabicyclo(2.2.2)octane dihydroiodide trimethanol
cocrystal
;
_chemical_name_systematic
;
1,4-diazabicyclo[2.2.2]octane dihydroiodide trimethanol cocrystal
;
_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                 95.02(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.385(3)
_cell_length_b                   7.782(5)
_cell_length_c                   12.82(8)
_cell_measurement_pressure       1800000
_cell_measurement_reflns_used    639
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      2.78
_cell_volume                     734(5)
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.135
_diffrn_measured_fraction_theta_max 0.135
_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  0.0847
_diffrn_reflns_av_sigmaI/netI    0.0951
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            639
_diffrn_reflns_theta_full        28.92
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    4.284
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.52
_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    2.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.386
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         281
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.374
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0316P)^2^+23.9176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                195
_reflns_number_total             281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c001379j.txt
_cod_data_source_block           dabcoHI18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7212551