#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:50:36 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179542 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/11/4501124.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4501124
loop_
_publ_author_name
'Andrzejewski, Michał'
'Olejniczak, Anna'
'Katrusiak, Andrzej'
_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 & 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, Poznań.
 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/[σ²(Fo²)+(0.0852P)²+0.4723P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br1 Br 0.2500 0.56635(8) 0.5945(3) 0.0305(10) Uani 1 2 d S
N1 N 0.0794(10) 0.2500 0.182(3) 0.039(6) Uani 1 2 d S
H1N H -0.0455 0.2500 0.1839 0.046 Uiso 1 2 calc SR
C1 C 0.1461(13) 0.2500 0.431(4) 0.031(7) Uani 1 2 d S
H1A H 0.1008 0.1780 0.5130 0.038 Uiso 0.50 1 calc PR
H1B H 0.1008 0.3220 0.5130 0.038 Uiso 0.50 1 calc PR
C2 C 0.1427(9) 0.3619(6) 0.058(2) 0.028(5) Uani 1 1 d .
H2A H 0.0970 0.4344 0.1373 0.033 Uiso 1 1 calc R
H2B H 0.0970 0.3623 -0.1033 0.033 Uiso 1 1 calc R
O1W O 0.2500 0.7500 0.135(3) 0.030(6) Uani 1 4 d SD
H1W H 0.2500 0.6745(5) 0.218(5) 0.036 Uiso 1 2 d SD
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0209(6) 0.0253(10) 0.045(3) -0.0023(4) 0.000 0.000
N1 0.013(3) 0.018(5) 0.09(2) 0.000 -0.007(6) 0.000
C1 0.019(4) 0.034(8) 0.04(3) 0.000 -0.002(7) 0.000
C2 0.026(3) 0.025(5) 0.032(18) 0.010(3) 0.006(4) 0.001(3)
O1W 0.026(5) 0.045(8) 0.02(2) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 N1 C2 110.8(12) 7_565 .
C2 N1 C1 110.4(8) 7_565 .
C2 N1 C1 110.4(8) . .
C2 N1 H1N 108.4 7_565 .
C2 N1 H1N 108.4 . .
C1 N1 H1N 108.4 . .
N1 C1 C1 109.0(5) . 2
N1 C1 H1A 109.9 . .
C1 C1 H1A 109.9 2 .
N1 C1 H1B 109.9 . .
C1 C1 H1B 109.9 2 .
H1A C1 H1B 108.3 . .
N1 C2 C2 108.1(4) . 8_655
N1 C2 H2A 110.1 . .
C2 C2 H2A 110.1 8_655 .
N1 C2 H2B 110.1 . .
C2 C2 H2B 110.1 8_655 .
H2A C2 H2B 108.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C2 1.485(11) 7_565
N1 C2 1.485(11) .
N1 C1 1.49(2) .
N1 H1N 0.9100 .
C1 C1 1.513(18) 2
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C2 1.563(13) 8_655
C2 H2A 0.9700 .
C2 H2B 0.9700 .
O1W H1W 0.950(11) .
