#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006637.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006637
loop_
_publ_author_name
'Morosin, B.'
'Dunn, R. G.'
'Assink, R.'
'Massis, T. M.'
'Fronabarger, J.'
'Duesler, E. N.'
_publ_section_title
;
 The Secondary Explosive
 Tetraammine-<i>cis</i>-bis(5-nitro-2<i>H</i>-tetrazolato-<i>N</i>^2^)cobalt(III)
 Perchlorate at 293 and 213 K
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1609
_journal_page_last               1611
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Co (C N5 O2)2 (N H3)4] Cl O4'
_chemical_formula_structural
;
 Co(NH~3~)~4~(N~5~CO~2~)~2~ClO~4~
;
_chemical_formula_sum            'C2 H12 Cl Co N14 O8'
_chemical_formula_weight         454.59
_chemical_name_common
;
 Tetraammine-cis-bis(5-nitrotetrazolato)cobalt(III)
 Perchlorate
;
_chemical_name_systematic
;
 tetraammine-cis-bis(5-nitro-2H-tetrazolato-N^2^)cobalt(III)
 perchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.68(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.946(7)
_cell_length_b                   10.542(5)
_cell_length_c                   14.820(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      8
_cell_volume                     1472.0(15)
_computing_cell_refinement       SHELXTL-Plus
_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1991)'
_computing_data_reduction        SHELXTL-Plus
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL (Sheldrick, 1994)'
_computing_structure_solution    SHELXTL-Plus
_diffrn_ambient_temperature      213(5)
_diffrn_measurement_device       'Siemens P3 diffractometer'
_diffrn_measurement_method       \q-2\q
_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  0.024
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3709
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.427
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.03
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         1749
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_obs          0.041
_refine_ls_shift/esd_max         0.020
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0733P)^2^+2.7371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.116
_refine_ls_wR_factor_obs         0.1093
_reflns_number_observed          1431
_reflns_number_total             1749
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    bk1330.cif
_[local]_cod_data_source_block   2
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_cod_database_code               2006637
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co 0.0166(4) 0.0144(6) 0.0134(3) 0.0000(3) 0.0044(3) 0.0011(2)
N1 0.016(2) 0.021(2) 0.016(2) 0.003(2) 0.005(2) -0.001(2)
N2 0.031(3) 0.033(3) 0.025(3) -0.003(2) 0.010(2) 0.007(2)
N3 0.023(2) 0.024(2) 0.024(2) 0.000(3) 0.007(2) -0.002(3)
N4 0.029(3) 0.018(2) 0.027(3) 0.000(2) 0.004(2) -0.001(2)
N5 0.017(2) 0.020(2) 0.017(2) 0.002(2) 0.009(2) -0.001(2)
N6 0.030(3) 0.027(3) 0.044(3) -0.002(2) 0.023(2) -0.004(2)
N7 0.030(3) 0.027(3) 0.050(3) 0.002(2) 0.027(3) -0.007(2)
N8 0.020(2) 0.023(5) 0.023(2) 0.004(2) 0.001(2) -0.006(2)
N9 0.019(2) 0.017(2) 0.016(2) 0.000(2) 0.006(2) -0.003(2)
N10 0.020(2) 0.015(2) 0.012(2) -0.001(2) 0.005(2) 0.001(2)
N11 0.031(2) 0.028(3) 0.018(2) -0.002(3) 0.004(2) 0.006(3)
N12 0.026(3) 0.031(2) 0.014(2) 0.001(2) -0.002(2) 0.005(2)
N13 0.018(2) 0.021(3) 0.032(3) 0.006(2) -0.002(2) -0.001(2)
N14 0.016(2) 0.020(2) 0.016(2) 0.000(2) 0.002(2) -0.001(2)
C1 0.017(3) 0.018(3) 0.018(3) 0.000(2) 0.006(2) 0.002(2)
C2 0.016(3) 0.022(3) 0.014(3) 0.003(2) -0.001(2) -0.003(2)
Cl 0.0344(8) 0.0261(8) 0.0349(8) -0.0057(7) 0.0135(7) -0.0005(6)
O1 0.027(2) 0.023(2) 0.037(2) -0.004(2) 0.012(2) 0.000(2)
O2 0.048(3) 0.028(2) 0.049(3) 0.012(2) 0.022(2) -0.011(2)
O3 0.027(2) 0.047(3) 0.038(3) 0.001(2) -0.017(2) -0.001(2)
O4 0.024(2) 0.028(2) 0.047(3) -0.004(2) 0.008(2) 0.005(2)
O5 0.053(3) 0.039(3) 0.061(3) -0.017(2) 0.020(2) 0.006(2)
O6 0.053(3) 0.067(4) 0.097(5) -0.004(3) 0.035(3) 0.032(3)
O7 0.207(9) 0.049(4) 0.167(8) 0.007(5) 0.128(7) -0.017(4)
O8 0.158(8) 0.269(12) 0.081(6) -0.146(8) -0.078(5) 0.108(7)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Co 0.32374(7) -0.22293(6) 0.55971(5) 0.0149(3) Uani d D 1 Co
N1 0.3818(4) -0.1555(4) 0.4561(3) 0.0178(9) Uani d D 1 N
N2 0.2660(5) -0.2932(4) 0.6638(3) 0.0292(12) Uani d D 1 N
N3 0.1308(4) -0.2509(6) 0.4739(3) 0.0240(8) Uani d D 1 N
N4 0.3867(5) -0.3904(4) 0.5334(3) 0.0261(11) Uani d D 1 N
N5 0.2672(4) -0.0556(4) 0.5845(3) 0.0173(10) Uani d . 1 N
N6 0.1629(5) -0.0327(5) 0.6205(4) 0.0309(12) Uani d . 1 N
N7 0.1526(5) 0.0924(5) 0.6286(4) 0.0322(12) Uani d . 1 N
N8 0.2800(5) 0.2717(5) 0.5927(3) 0.0233(14) Uani d . 1 N
N9 0.3246(4) 0.0512(4) 0.5669(3) 0.0171(9) Uani d . 1 N
N10 0.5119(4) -0.1916(4) 0.6478(3) 0.0159(9) Uani d . 1 N
N11 0.5583(5) -0.2390(6) 0.7355(3) 0.0267(10) Uani d . 1 N
N12 0.6907(5) -0.1981(4) 0.7778(3) 0.0262(11) Uani d . 1 N
N13 0.8480(5) -0.0600(4) 0.7266(3) 0.0261(11) Uani d . 1 N
N14 0.6105(4) -0.1190(4) 0.6306(3) 0.0183(10) Uani d . 1 N
C1 0.2510(6) 0.1373(5) 0.5950(4) 0.0173(12) Uani d . 1 C
C2 0.7167(5) -0.1270(5) 0.7116(4) 0.0188(11) Uani d . 1 C
Cl 0.0912(2) 0.39257(14) 0.35539(10) 0.0312(4) Uani d . 1 Cl
O1 0.3643(4) 0.3040(4) 0.5517(3) 0.0288(9) Uani d . 1 O
O2 0.2199(5) 0.3448(4) 0.6315(3) 0.0404(12) Uani d . 1 O
O3 0.9392(4) -0.0716(4) 0.8052(3) 0.0439(12) Uani d . 1 O
O4 0.8618(4) 0.0023(4) 0.6614(3) 0.0340(10) Uani d . 1 O
O5 0.0710(5) 0.2704(4) 0.3904(3) 0.0504(13) Uani d . 1 O
O6 0.2355(5) 0.4106(5) 0.3606(4) 0.070(2) Uani d . 1 O
O7 0.0734(10) 0.4794(6) 0.4226(6) 0.124(3) Uani d . 1 O
O8 0.0017(10) 0.4147(11) 0.2696(6) 0.197(6) Uani d . 1 O
H1 0.359(4) -0.0801(18) 0.448(2) 0.063(7) Uiso d D 1 H
H2 0.343(4) -0.195(3) 0.4067(11) 0.063(7) Uiso d D 1 H
H3 0.4685(16) -0.162(4) 0.4688(15) 0.063(7) Uiso d D 1 H
H4 0.3370(15) -0.307(4) 0.7097(14) 0.063(7) Uiso d D 1 H
H5 0.223(4) -0.360(2) 0.6462(13) 0.063(7) Uiso d D 1 H
H6 0.214(4) -0.242(2) 0.679(2) 0.063(7) Uiso d D 1 H
H7 0.0750(13) -0.244(5) 0.5043(11) 0.063(7) Uiso d D 1 H
H8 0.112(2) -0.197(3) 0.432(2) 0.063(7) Uiso d D 1 H
H9 0.1254(17) -0.322(2) 0.451(3) 0.063(7) Uiso d D 1 H
H10 0.470(2) -0.3861(13) 0.535(3) 0.063(7) Uiso d D 1 H
H11 0.379(5) -0.4407(14) 0.574(2) 0.063(7) Uiso d D 1 H
H12 0.337(3) -0.414(2) 0.4802(17) 0.063(7) Uiso d D 1 H
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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_site_symmetry_1
_geom_angle
N5 Co N10 . 89.6(2)
N5 Co N1 . 89.7(2)
N10 Co N1 . 90.2(2)
N5 Co N4 . 178.0(2)
N10 Co N4 . 89.2(2)
N1 Co N4 . 88.7(2)
N5 Co N3 . 88.7(2)
N10 Co N3 . 177.8(2)
N1 Co N3 . 91.1(2)
N4 Co N3 . 92.5(2)
N5 Co N2 . 91.1(2)
N10 Co N2 . 89.8(2)
N1 Co N2 . 179.2(2)
N4 Co N2 . 90.5(2)
N3 Co N2 . 88.9(2)
Co N1 H1 . 110.0(6)
Co N1 H2 . 110.0(6)
H1 N1 H2 . 108.9(8)
Co N1 H3 . 110.1(6)
H1 N1 H3 . 109.0(8)
H2 N1 H3 . 108.9(8)
Co N2 H4 . 109.1(7)
Co N2 H5 . 109.2(7)
H4 N2 H5 . 109.9(8)
Co N2 H6 . 109.0(7)
H4 N2 H6 . 109.8(8)
H5 N2 H6 . 109.9(8)
Co N3 H7 . 109.0(6)
Co N3 H8 . 109.0(6)
H7 N3 H8 . 109.6(8)
Co N3 H9 . 109.2(6)
H7 N3 H9 . 109.9(8)
H8 N3 H9 . 110.1(8)
Co N4 H10 . 109.1(7)
Co N4 H11 . 109.2(7)
H10 N4 H11 . 109.6(8)
Co N4 H12 . 109.3(7)
H10 N4 H12 . 109.7(8)
H11 N4 H12 . 109.9(8)
N9 N5 N6 . 111.4(4)
N9 N5 Co . 124.8(3)
N6 N5 Co . 123.8(3)
N7 N6 N5 . 107.9(4)
C1 N7 N6 . 103.5(4)
O2 N8 O1 . 124.7(5)
O2 N8 C1 . 118.3(5)
O1 N8 C1 . 117.0(4)
C1 N9 N5 . 101.8(4)
N11 N10 N14 . 110.9(4)
N11 N10 Co . 123.6(3)
N14 N10 Co . 125.5(3)
N10 N11 N12 . 108.6(4)
C2 N12 N11 . 103.4(4)
O4 N13 O3 . 124.7(5)
O4 N13 C2 . 118.2(4)
O3 N13 C2 . 117.1(5)
C2 N14 N10 . 102.3(4)
N9 C1 N7 . 115.3(5)
N9 C1 N8 . 122.2(5)
N7 C1 N8 . 122.4(5)
N14 C2 N12 . 114.8(5)
N14 C2 N13 . 122.1(5)
N12 C2 N13 . 123.1(5)
O8 Cl O7 4_565 111.7(8)
O8 Cl O6 4_565 112.7(5)
O7 Cl O6 . 103.2(5)
O8 Cl O5 4_565 112.3(4)
O7 Cl O5 . 105.4(4)
O6 Cl O5 . 110.9(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co N5 . 1.923(4)
Co N10 . 1.937(4)
Co N1 . 1.940(4)
Co N4 . 1.954(4)
Co N3 . 1.955(4)
Co N2 . 1.956(4)
N1 H1 . 0.824(14)
N1 H2 . 0.825(14)
N1 H3 . 0.824(14)
N2 H4 . 0.821(14)
N2 H5 . 0.820(14)
N2 H6 . 0.821(14)
N3 H7 . 0.822(14)
N3 H8 . 0.821(14)
N3 H9 . 0.819(14)
N4 H10 . 0.822(14)
N4 H11 . 0.820(14)
N4 H12 . 0.821(14)
N5 N9 . 1.325(6)
N5 N6 . 1.332(6)
N6 N7 . 1.331(7)
N7 C1 . 1.320(7)
N8 O2 . 1.225(6)
N8 O1 . 1.231(5)
N8 C1 . 1.449(7)
N9 C1 . 1.315(7)
N10 N11 . 1.329(6)
N10 N14 . 1.331(6)
N11 N12 . 1.336(6)
N12 C2 . 1.325(7)
N13 O4 . 1.211(6)
N13 O3 . 1.233(6)
N13 C2 . 1.438(7)
N14 C2 . 1.323(6)
Cl O8 4_565 1.319(6)
Cl O7 . 1.406(7)
Cl O6 . 1.425(5)
Cl O5 . 1.427(5)
O8 Cl 4_666 1.319(6)