#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/22/7202227.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_7202227
loop_
_publ_author_name
'Laus, Gerhard'
'Kahlenberg, Volker'
'Wurst, Klaus'
'Lörting, Thomas'
'Schottenberger, Herwig'
_publ_section_title
;
 Hydrogen bonding in the perhydrate and hydrates of
 1,4-diazabicyclo[2.2.2]octane (DABCO)
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1638
_journal_paper_doi               10.1039/b807303a
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C6 H12 N2, 1.7(H2O2), 0.3(H2O)'
_chemical_formula_sum            'C6 H16 N2 O3.7'
_chemical_formula_weight         176.2
_chemical_name_systematic
;
?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-10-06T16:43:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.0860(17)
_cell_length_b                   12.0860(17)
_cell_length_c                   12.0361(19)
_cell_measurement_reflns_used    5485
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.38
_cell_volume                     1758.1(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6709
_diffrn_reflns_theta_full        26.95
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         2.38
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS - Bruker Nonius area detector scaling and absorption correction - V2.06
R.H. Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.33
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath-shaped
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.055(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         948
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.1
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0759P)²+1.0460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                789
_reflns_number_total             948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807303a.txt
_cod_data_source_block           bisperhydrate_CCDC634612
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C6 H16 N2 O3.70 '
_cod_database_code               7202227
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7031(2) -0.0040(2) 0.6244(2) 0.0544(8) Uani 0.851(9) 1 d PD . .
H1 H 0.655(3) 0.054(3) 0.622(4) 0.082(10) Uiso 0.851(9) 1 d PD . .
O2 O 0.7876(2) 0.0556(2) 0.6844(3) 0.0644(10) Uani 0.851(9) 1 d PD . .
H2 H 0.775(4) 0.014(3) 0.746(2) 0.082(10) Uiso 0.851(9) 1 d PD . .
N1 N 0.56373(17) 0.16601(16) 0.61668(16) 0.0425(6) Uani 1 1 d . . .
C1 C 0.5353(3) 0.1974(2) 0.7309(2) 0.0600(8) Uani 1 1 d . . .
H1A H 0.6038 0.2103 0.774 0.072 Uiso 1 1 calc R . .
H1B H 0.4938 0.1365 0.7668 0.072 Uiso 1 1 calc R . .
C2 C 0.4620(2) 0.1411(2) 0.5562(3) 0.0603(8) Uani 1 1 d . . .
H2A H 0.4265 0.0746 0.5885 0.072 Uiso 1 1 calc R . .
H2B H 0.4795 0.1253 0.4775 0.072 Uiso 1 1 calc R . .
C3 C 0.6180(2) 0.2598(3) 0.5633(3) 0.0598(8) Uani 1 1 d . . .
H3A H 0.6421 0.2386 0.4877 0.072 Uiso 1 1 calc R . .
H3B H 0.6844 0.2811 0.6065 0.072 Uiso 1 1 calc R . .
OW O 0.7503(2) 0.0297(3) 0.6311(3) 0.082(7) Uiso 0.149(9) 1 d PR . .
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
O1 0.0495(14) 0.0465(12) 0.0674(16) 0.0006(10) 0.0031(10) 0.0054(11)
O2 0.0489(14) 0.0604(15) 0.084(2) 0.0088(13) 0.0040(13) -0.0031(11)
N1 0.0421(10) 0.0396(10) 0.0459(11) 0.0019(8) 0.0025(8) 0.0048(8)
C1 0.0724(19) 0.0601(17) 0.0474(14) 0.0040(13) 0.0010(14) 0.0200(14)
C2 0.0551(16) 0.0466(14) 0.079(2) -0.0150(14) -0.0109(14) -0.0010(12)
C3 0.0469(15) 0.0538(16) 0.079(2) 0.0089(14) 0.0153(14) 0.0023(12)
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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
_geom_angle_publ_flag
O2 O1 H1 95(3) . . ?
O1 O2 H2 90(3) . . ?
C3 N1 C2 108.6(2) . . ?
C3 N1 C1 108.5(2) . . ?
C2 N1 C1 108.8(2) . . ?
N1 C1 C1 110.21(13) . 2_655 ?
N1 C1 H1A 109.6 . . ?
C1 C1 H1A 109.6 2_655 . ?
N1 C1 H1B 109.6 . . ?
C1 C1 H1B 109.6 2_655 . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C3 109.9(2) . 2_655 ?
N1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 2_655 . ?
N1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 2_655 . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C2 110.3(2) . 2_655 ?
N1 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 2_655 . ?
N1 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 2_655 . ?
H3A C3 H3B 108.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 O2 1.443(4) . ?
O1 H1 0.912(10) . ?
O2 H2 0.908(10) . ?
N1 C3 1.459(4) . ?
N1 C2 1.460(3) . ?
N1 C1 1.467(3) . ?
C1 C1 1.531(6) 2_655 ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 C3 1.541(4) 2_655 ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
