1,4-Diazabicyclo[2.2.2]octane (DABCO) 5-aminotetrazolates
Laus, Gerhard; Kahlenberg, Volker; Wurst, Klaus; Hummel, Michael; Schottenberger, Herwig; Crystals 2 (2012) 96–104; doi:10.3390/cryst2010096

data_1508428
_publ_section_title
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 1,4-Diazabicyclo[2.2.2]octane (DABCO) 5-aminotetrazolates
;
_journal_issue                   1
_journal_name_full               Crystals
_journal_page_first              96
_journal_page_last               104
_journal_paper_doi               10.3390/cryst2010096
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C6 H12 N2, 2(C6 H13 N2), 2(C H2 N5), 8(H2 O)'
_chemical_formula_sum            'C20 H58 N16 O8'
_chemical_formula_weight         650.82
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.390(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6856(3)
_cell_length_b                   8.8200(2)
_cell_length_c                   31.3885(8)
_cell_measurement_reflns_used    39249
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      1.0
_cell_volume                     3464.91(15)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15576
_diffrn_reflns_theta_full        23.10
_diffrn_reflns_theta_max         23.10
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0035(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         4769
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.6923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                3567
_reflns_number_total             4769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file
C20H58N16O8_P21_c_CCDC855699corr_crystals-02-00096-s001_DC173.CIF
_cod_data_source_block           s276c_chateigner_1508428
_cod_original_cell_volume        3464.91(14)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1508428