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#$Date: 2016-03-24 01:34:15 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179536 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/05/4500534.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_4500534
loop_
_publ_author_name
'Olejniczak, Anna'
'Katrusiak, Andrzej'
_publ_section_title
;
 Pressure-Induced Hydration of 1,4-Diazabicyclo[2.2.2]octane Hydroiodide
 (dabcoHI)
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & 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 κ 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, Poznań.
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/[σ²(Fo²)+(0.0473P)²+2.4868P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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
I1 I 0.55458(4) 0.7500 0.32715(7) 0.0290(3) Uani 1 2 d S
O1W O 0.8490(5) 0.7500 0.4807(9) 0.0347(18) Uani 1 2 d SD
H1W H 0.779(8) 0.7500 0.420(11) 0.042 Uiso 1 2 d SD
H2W H 0.830(10) 0.7500 0.582(8) 0.042 Uiso 1 2 d SD
N2 N 0.8939(7) 0.2500 0.4527(10) 0.027(2) Uani 1 2 d S
H2N H 0.9486 0.2500 0.5247 0.033 Uiso 1 2 calc SR
C4 C 0.6763(6) 0.2500 0.3750(12) 0.038(3) Uani 1 2 d S
H4A H 0.6231 0.1552 0.3767 0.046 Uiso 0.50 1 calc PR
H4B H 0.6231 0.3448 0.3767 0.046 Uiso 0.50 1 calc PR
C3 C 0.7620(6) 0.2500 0.5098(12) 0.072(5) Uani 1 2 d SR
H3A H 0.7497 0.1540 0.5659 0.087 Uiso 0.50 1 d PR
H3B H 0.7497 0.3460 0.5659 0.087 Uiso 0.50 1 d PR
N1 N 0.7496(6) 0.2500 0.2448(10) 0.0242(18) Uani 1 2 d S
C2 C 0.9181(7) 0.1057(11) 0.3648(11) 0.042(2) Uani 1 1 d .
H2A H 0.9065 0.0078 0.4187 0.051 Uiso 1 1 calc R
H2B H 1.0033 0.1077 0.3314 0.051 Uiso 1 1 calc R
C1 C 0.8279(5) 0.1074(9) 0.2427(9) 0.0287(16) Uani 1 1 d .
H1A H 0.8747 0.1048 0.1568 0.034 Uiso 1 1 calc R
H1B H 0.7759 0.0115 0.2460 0.034 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
H1W O1W H2W 116(9) . .
C2 N2 C2 106.7(11) . 7_565
C2 N2 C3 111.7(5) . .
C2 N2 C3 111.7(5) 7_565 .
C2 N2 H2N 108.9 . .
C2 N2 H2N 108.9 7_565 .
C3 N2 H2N 108.9 . .
N1 C4 C3 112.8(4) . .
N1 C4 H4A 109.0 . .
C3 C4 H4A 109.0 . .
N1 C4 H4B 109.0 . .
C3 C4 H4B 109.0 . .
H4A C4 H4B 107.8 . .
N2 C3 C4 103.9(5) . .
N2 C3 H3A 109.2 . .
C4 C3 H3A 112.2 . .
N2 C3 H3B 109.2 . .
C4 C3 H3B 112.2 . .
H3A C3 H3B 109.8 . .
C1 N1 C1 109.1(7) 7_565 .
C1 N1 C4 108.7(6) 7_565 .
C1 N1 C4 108.7(6) . .
N2 C2 C1 108.8(6) . .
N2 C2 H2A 109.9 . .
C1 C2 H2A 109.9 . .
N2 C2 H2B 109.9 . .
C1 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
N1 C1 C2 111.4(6) . .
N1 C1 H1A 109.4 . .
C2 C1 H1A 109.4 . .
N1 C1 H1B 109.4 . .
C2 C1 H1B 109.4 . .
H1A C1 H1B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1W H1W 0.95(7) .
O1W H2W 1.00(7) .
N2 C2 1.487(11) .
N2 C2 1.487(11) 7_565
N2 C3 1.520(11) .
N2 H2N 0.9100 .
C4 N1 1.483(13) .
C4 C3 1.5937 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
N1 C1 1.447(8) 7_565
N1 C1 1.447(8) .
C2 C1 1.527(10) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 N2 C3 C4 -59.7(6) . .
C2 N2 C3 C4 59.7(6) 7_565 .
N1 C4 C3 N2 0.0 . .
C3 C4 N1 C1 -59.3(4) . 7_565
C3 C4 N1 C1 59.3(4) . .
C2 N2 C2 C1 -61.6(10) 7_565 .
C3 N2 C2 C1 60.7(10) . .
C1 N1 C1 C2 57.9(11) 7_565 .
C4 N1 C1 C2 -60.4(8) . .
N2 C2 C1 N1 2.2(10) . .
