#------------------------------------------------------------------------------
#$Date: 2019-11-25 23:01:00 +0200 (Mon, 25 Nov 2019) $
#$Revision: 242010 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/19/4131929.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_4131929
loop_
_publ_author_name
'Wurzenberger, Maximilian H. H.'
'Szimhardt, Norbert'
'Stierstorfer, Jörg'
_publ_section_title
;
 Copper(II) Chlorate Complexes: The Renaissance of a Forgotten and
 Misjudged Energetic Anion.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3206
_journal_page_last               3209
_journal_paper_doi               10.1021/jacs.7b13230
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C10 H16 Cl2 Cu N16 O6'
_chemical_formula_sum            'C10 H16 Cl2 Cu N16 O6'
_chemical_formula_weight         590.83
_chemical_name_common
' dichlorato bis(1,2-ditetrazolyl)propane copper(II)'
_chemical_name_systematic
;
 dichlorato bis(1,2-ditetrazolyl)propane copper(II)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date
;
'Wed Apr 26 16:46:18 2017'
;
_audit_creation_method           SHELXL-2013
_audit_update_record             05.07.2017
_cell_angle_alpha                108.068(11)
_cell_angle_beta                 101.188(10)
_cell_angle_gamma                90.137(10)
_cell_formula_units_Z            1
_cell_length_a                   6.7837(8)
_cell_length_b                   8.1820(10)
_cell_length_c                   10.1959(12)
_cell_measurement_reflns_used    598
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.7160
_cell_measurement_theta_min      4.5480
_cell_volume                     526.60(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.775
_diffrn_measured_fraction_theta_max 0.777
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -81.00   12.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5028  -57.0000  150.0000 93

#__ type_ start__ end____ width___ exp.time_
  2 omega  -34.00   56.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5028   57.0000  -60.0000 90

#__ type_ start__ end____ width___ exp.time_
  3 omega  -17.00   72.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       12.5965   77.0000   60.0000 89

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0811162000
_diffrn_orient_matrix_UB_12      0.0302359000
_diffrn_orient_matrix_UB_13      0.0336672000
_diffrn_orient_matrix_UB_21      0.0652217000
_diffrn_orient_matrix_UB_22      0.0674580000
_diffrn_orient_matrix_UB_23      0.0511485000
_diffrn_orient_matrix_UB_31      -0.0240428000
_diffrn_orient_matrix_UB_32      0.0537382000
_diffrn_orient_matrix_UB_33      -0.0428907000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_Laue_measured_fraction_full 0.775
_diffrn_reflns_Laue_measured_fraction_max 0.777
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2222
_diffrn_reflns_point_group_measured_fraction_full 0.775
_diffrn_reflns_point_group_measured_fraction_max 0.777
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.219
_diffrn_reflns_theta_min         4.171
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       block
_exptl_crystal_F_000             299
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.889
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0073P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                987
_reflns_number_total             1471
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b13230_si_002.cif
_cod_data_source_block           mx192
_cod_original_cell_volume        526.60(11)
_cod_database_code               4131929
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.948
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5000 0.0000 0.5000 0.0209(3) Uani 1 2 d S . P
Cl1 Cl 0.1678(2) 0.33632(16) 0.59374(15) 0.0280(4) Uani 1 1 d . . .
O1 O 0.2046(5) 0.1630(4) 0.5020(3) 0.0257(9) Uani 1 1 d . . .
O2 O 0.2955(6) 0.4659(4) 0.5698(4) 0.0396(11) Uani 1 1 d . . .
O3 O 0.2334(6) 0.3407(4) 0.7418(4) 0.0369(11) Uani 1 1 d . . .
N1 N 0.7859(6) 0.4467(5) 0.7827(5) 0.0188(11) Uani 1 1 d . . .
N2 N 0.7950(7) 0.3516(5) 0.8701(5) 0.0250(12) Uani 1 1 d . . .
N3 N 0.7194(7) 0.1990(5) 0.7923(5) 0.0261(12) Uani 1 1 d . . .
N4 N 0.6632(6) 0.1948(5) 0.6552(4) 0.0175(11) Uani 1 1 d . . .
N5 N 0.7384(7) 0.1324(5) 0.1945(5) 0.0285(12) Uani 1 1 d . . .
N6 N 0.5515(7) 0.1891(5) 0.1859(4) 0.0214(11) Uani 1 1 d . . .
N7 N 0.4586(7) 0.1679(5) 0.2813(5) 0.0250(11) Uani 1 1 d . . .
N8 N 0.5866(6) 0.0915(4) 0.3559(4) 0.0186(11) Uani 1 1 d . . .
C1 C 0.7063(7) 0.3514(6) 0.6542(6) 0.0181(13) Uani 1 1 d . . .
H1 H 0.6833 0.3888 0.5734 0.022 Uiso 1 1 calc R U .
C2 C 0.8639(8) 0.6278(5) 0.8337(5) 0.0250(14) Uani 1 1 d . . .
H2A H 0.8409 0.6753 0.7541 0.030 Uiso 1 1 calc R U .
H2B H 1.0109 0.6345 0.8705 0.030 Uiso 1 1 calc R U .
C3 C 0.7630(8) 0.7348(6) 0.9486(5) 0.0262(14) Uani 1 1 d . . .
H3A H 0.8106 0.8569 0.9719 0.031 Uiso 1 1 calc R U .
H3B H 0.8096 0.7004 1.0338 0.031 Uiso 1 1 calc R U .
C4 C 0.4652(8) 0.2762(6) 0.0827(6) 0.0286(15) Uani 1 1 d . . .
H4A H 0.5124 0.2232 -0.0061 0.034 Uiso 1 1 calc R U .
H4B H 0.5153 0.3989 0.1197 0.034 Uiso 1 1 calc R U .
C5 C 0.7521(8) 0.0725(5) 0.3021(5) 0.0225(14) Uani 1 1 d . . .
H5 H 0.8676 0.0215 0.3372 0.027 Uiso 1 1 calc R U .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 '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
N4 Cu1 N4 180.0 . 2_656
N4 Cu1 N8 90.11(16) . 2_656
N4 Cu1 N8 89.89(16) 2_656 2_656
N4 Cu1 N8 89.89(16) . .
N4 Cu1 N8 90.11(16) 2_656 .
N8 Cu1 N8 180.00(10) 2_656 .
N4 Cu1 O1 88.69(13) . 2_656
N4 Cu1 O1 91.31(13) 2_656 2_656
N8 Cu1 O1 92.09(13) 2_656 2_656
N8 Cu1 O1 87.91(13) . 2_656
N4 Cu1 O1 91.31(13) . .
N4 Cu1 O1 88.69(13) 2_656 .
N8 Cu1 O1 87.90(13) 2_656 .
N8 Cu1 O1 92.10(13) . .
O1 Cu1 O1 180.0 2_656 .
O2 Cl1 O3 108.0(2) . .
O2 Cl1 O1 108.3(2) . .
O3 Cl1 O1 107.66(18) . .
Cl1 O1 Cu1 131.69(19) . .
C1 N1 N2 109.5(4) . .
C1 N1 C2 128.8(4) . .
N2 N1 C2 121.7(4) . .
N3 N2 N1 106.1(4) . .
N2 N3 N4 109.8(4) . .
C1 N4 N3 105.9(4) . .
C1 N4 Cu1 128.3(3) . .
N3 N4 Cu1 124.8(3) . .
C5 N5 N6 101.1(4) . .
N7 N6 N5 114.0(4) . .
N7 N6 C4 123.4(4) . .
N5 N6 C4 122.5(4) . .
N6 N7 N8 105.3(4) . .
N7 N8 C5 106.9(4) . .
N7 N8 Cu1 120.9(3) . .
C5 N8 Cu1 131.7(3) . .
N1 C1 N4 108.7(4) . .
N1 C1 H1 125.7 . .
N4 C1 H1 125.7 . .
N1 C2 C3 111.5(4) . .
N1 C2 H2A 109.3 . .
C3 C2 H2A 109.3 . .
N1 C2 H2B 109.3 . .
C3 C2 H2B 109.3 . .
H2A C2 H2B 108.0 . .
C2 C3 C4 116.9(4) . 2_666
C2 C3 H3A 108.1 . .
C4 C3 H3A 108.1 2_666 .
C2 C3 H3B 108.1 . .
C4 C3 H3B 108.1 2_666 .
H3A C3 H3B 107.3 . .
N6 C4 C3 112.8(4) . 2_666
N6 C4 H4A 109.0 . .
C3 C4 H4A 109.0 2_666 .
N6 C4 H4B 109.0 . .
C3 C4 H4B 109.0 2_666 .
H4A C4 H4B 107.8 . .
N5 C5 N8 112.8(4) . .
N5 C5 H5 123.6 . .
N8 C5 H5 123.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N4 2.004(4) .
Cu1 N4 2.004(4) 2_656
Cu1 N8 2.020(4) 2_656
Cu1 N8 2.020(4) .
Cu1 O1 2.410(3) 2_656
Cu1 O1 2.410(3) .
Cl1 O2 1.474(3) .
Cl1 O3 1.478(3) .
Cl1 O1 1.489(3) .
N1 C1 1.306(6) .
N1 N2 1.346(5) .
N1 C2 1.468(5) .
N2 N3 1.294(5) .
N3 N4 1.365(5) .
N4 C1 1.318(5) .
N5 C5 1.322(5) .
N5 N6 1.348(5) .
N6 N7 1.310(5) .
N6 C4 1.478(5) .
N7 N8 1.329(5) .
N8 C5 1.331(6) .
C1 H1 0.9500 .
C2 C3 1.512(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.516(6) 2_666
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C3 1.516(6) 2_666
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5 0.9500 .
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_4
O2 Cl1 O1 Cu1 64.9(3) .
O3 Cl1 O1 Cu1 -51.6(3) .
C1 N1 N2 N3 -0.2(5) .
C2 N1 N2 N3 -178.4(4) .
N1 N2 N3 N4 0.5(5) .
N2 N3 N4 C1 -0.6(5) .
N2 N3 N4 Cu1 -169.9(3) .
C5 N5 N6 N7 0.8(5) .
C5 N5 N6 C4 177.4(4) .
N5 N6 N7 N8 -1.0(5) .
C4 N6 N7 N8 -177.7(4) .
N6 N7 N8 C5 0.8(5) .
N6 N7 N8 Cu1 -171.3(3) .
N2 N1 C1 N4 -0.2(5) .
C2 N1 C1 N4 177.8(4) .
N3 N4 C1 N1 0.5(5) .
Cu1 N4 C1 N1 169.2(3) .
C1 N1 C2 C3 124.3(5) .
N2 N1 C2 C3 -57.9(6) .
N1 C2 C3 C4 -52.1(6) 2_666
N7 N6 C4 C3 -26.4(6) 2_666
N5 N6 C4 C3 157.2(4) 2_666
N6 N5 C5 N8 -0.2(5) .
N7 N8 C5 N5 -0.4(6) .
Cu1 N8 C5 N5 170.6(3) .
