Humidity Control of Isostructural Dehydration and Pressure-Induced Polymorphism in 1,4-Diazabicyclo[2.2.2]octane Dihydrobromide Monohydrate
Andrzejewski, Michał; Olejniczak, Anna; Katrusiak, Andrzej; Crystal Growth & Design 11 (2011) 4892–; doi:10.1021/cg200743n

data_4501124
_publ_section_title
;
 Humidity Control of Isostructural Dehydration and Pressure-Induced
 Polymorphism in 1,4-Diazabicyclo[2.2.2]octane Dihydrobromide Monohydrate
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4892
_journal_paper_doi               10.1021/cg200743n
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         '    C6 H14 N2, H2 O, 2(Br)'
_chemical_formula_sum            'C6 H16 Br2 N2 O'
_chemical_formula_weight         292.03
_chemical_name_common
;
dabco dihydrobromide monohydrate, dabco2HBr*H2O
;
_chemical_name_systematic
;
1,4-diazabicyclo[2.2.2]octane dihydrobromide monohydrate
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_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            2
_cell_length_a                   7.2844(19)
_cell_length_b                   10.918(4)
_cell_length_c                   5.663(4)
_cell_measurement_pressure       1500000
_cell_measurement_reflns_used    2039
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      3.36
_cell_volume                     450.4(4)
_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)

Mercury (2008)
;
_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 0.413
_diffrn_measured_fraction_theta_max 0.413
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.1222
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            2039
_diffrn_reflns_theta_full        29.19
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_min         3.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.947
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.49
_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    2.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.381
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         283
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0852P)^2^+0.4723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                253
_reflns_number_total             283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200743n_si_002.cif
_cod_data_source_block           dabco2HBr*H2Odelta
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pmmn
_cod_database_code               4501124