#------------------------------------------------------------------------------
#$Date: 2019-11-25 23:01:00 +0200 (Mon, 25 Nov 2019) $
#$Revision: 242010 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/19/4131934.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_4131934
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         '3(C5 H8 Cu0.33 N8), 2(Cl O3)'
_chemical_formula_sum            'C15 H24 Cl2 Cu N24 O6'
_chemical_formula_weight         771.02
_chemical_name_common
'tris(ditetrazolylpropyl) copper(II) chlorate'
_chemical_name_systematic
;
tris(ditetrazolylpropyl) copper(II) chlorate'
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date
;
'Mon Aug 01 09:15:29 2016'
;
_audit_creation_method           SHELXL-2013
_audit_update_record             01.08.2016
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.9642(2)
_cell_length_b                   10.9642(2)
_cell_length_c                   14.3772(4)
_cell_measurement_reflns_used    3051
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.4310
_cell_measurement_theta_min      5.1330
_cell_volume                     1496.78(6)
_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      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -77.00  -34.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   60.0000 43

#__ type_ start__ end____ width___ exp.time_
  2 omega   53.00   89.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -90.0000 36

#__ type_ start__ end____ width___ exp.time_
  3 omega   75.00  112.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000  120.0000 37

#__ type_ start__ end____ width___ exp.time_
  4 omega  -22.00   73.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
  5 omega   16.00  101.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000   60.0000 85

#__ type_ start__ end____ width___ exp.time_
  6 omega  -22.00   75.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 97

#__ type_ start__ end____ width___ exp.time_
  7 omega   32.00  102.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  -60.0000 70

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0591992000
_diffrn_orient_matrix_UB_12      0.0690020000
_diffrn_orient_matrix_UB_13      -0.0021587000
_diffrn_orient_matrix_UB_21      0.0331525000
_diffrn_orient_matrix_UB_22      -0.0174113000
_diffrn_orient_matrix_UB_23      0.0357781000
_diffrn_orient_matrix_UB_31      0.0313359000
_diffrn_orient_matrix_UB_32      -0.0227392000
_diffrn_orient_matrix_UB_33      -0.0338848000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10648
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         4.293
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82300
_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    1.711
_exptl_crystal_description       block
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0289
_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)+(0.0430P)²+0.7522P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                825
_reflns_number_total             989
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b13230_si_002.cif
_cod_data_source_block           lx365
_cod_original_cell_volume        1496.78(8)
_cod_database_code               4131934
_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   0.763
_shelx_estimated_absorpt_t_max   0.908
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu Cu 0.0000 0.0000 0.0000 0.02331(19) Uani 1 6 d S T P
N1 N 0.04132(18) 0.17669(18) 0.08369(11) 0.0335(4) Uani 1 1 d . . .
N2 N 0.1638(2) 0.2505(2) 0.13184(13) 0.0415(5) Uani 1 1 d . . .
N3 N 0.1702(2) 0.3611(2) 0.16775(13) 0.0427(5) Uani 1 1 d . . .
N4 N 0.05109(19) 0.35955(19) 0.14377(12) 0.0375(4) Uani 1 1 d . . .
C1 C -0.0254(2) 0.2468(2) 0.09282(16) 0.0382(5) Uani 1 1 d . . .
C2 C 0.0308(3) 0.4798(3) 0.1642(2) 0.0539(7) Uani 1 1 d . . .
C3 C -0.0645(5) 0.4658(5) 0.2259(3) 0.0370(9) Uani 0.5 1 d . . P
Cl1 Cl 0.6667 0.3333 0.99549(5) 0.0325(2) Uani 1 3 d S T P
O1 O 0.53289(17) 0.31354(17) 1.03221(12) 0.0495(4) Uani 1 1 d . . .
H1 H -0.103(3) 0.229(3) 0.0715(16) 0.040(7) Uiso 1 1 d . . .
H2A H 0.116(4) 0.555(4) 0.160(3) 0.098(13) Uiso 1 1 d . . .
H2B H 0.020(4) 0.509(4) 0.116(3) 0.084(12) Uiso 1 1 d . . .
H3A H -0.149(5) 0.394(5) 0.207(3) 0.040(13) Uiso 0.5 1 d . . P
H3B H -0.069(5) 0.543(5) 0.220(3) 0.045(13) Uiso 0.5 1 d . . P
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
N1 Cu N1 180.0 . 7
N1 Cu N1 88.83(6) . 9
N1 Cu N1 91.17(6) 7 9
N1 Cu N1 91.17(6) . 3
N1 Cu N1 88.83(6) 7 3
N1 Cu N1 180.00(11) 9 3
N1 Cu N1 91.17(6) . 2
N1 Cu N1 88.83(6) 7 2
N1 Cu N1 88.83(6) 9 2
N1 Cu N1 91.17(6) 3 2
N1 Cu N1 88.83(6) . 8
N1 Cu N1 91.17(6) 7 8
N1 Cu N1 91.17(6) 9 8
N1 Cu N1 88.83(6) 3 8
N1 Cu N1 180.00(19) 2 8
C1 N1 N2 105.99(18) . .
C1 N1 Cu 131.74(15) . .
N2 N1 Cu 121.79(13) . .
N3 N2 N1 109.71(17) . .
N2 N3 N4 106.90(18) . .
C1 N4 N3 108.32(18) . .
C1 N4 C2 129.9(2) . .
N3 N4 C2 121.3(2) . .
N1 C1 N4 109.1(2) . .
N1 C1 H1 129.4(17) . .
N4 C1 H1 121.5(17) . .
C3 C2 N4 119.6(3) . .
C3 C2 C3 55.1(4) . 5
N4 C2 C3 112.4(3) . 5
C3 C2 H2A 124(3) . .
N4 C2 H2A 105(2) . .
C3 C2 H2A 78(3) 5 .
C3 C2 H2B 111(3) . .
N4 C2 H2B 108(3) . .
C3 C2 H2B 138(3) 5 .
H2A C2 H2B 82(3) . .
C2 C3 C3 74.6(4) . 5
C2 C3 C2 116.6(4) . 5
C3 C3 C2 50.3(3) 5 5
C2 C3 H3A 108(3) . .
C3 C3 H3A 156(3) 5 .
C2 C3 H3A 112(3) 5 .
C2 C3 H3B 104(3) . .
C3 C3 H3B 95(3) 5 .
C2 C3 H3B 109(3) 5 .
H3A C3 H3B 107(4) . .
O1 Cl1 O1 107.84(8) . 3_665
O1 Cl1 O1 107.84(8) . 2_655
O1 Cl1 O1 107.84(8) 3_665 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N1 2.1279(18) .
Cu N1 2.1280(18) 7
Cu N1 2.1280(18) 9
Cu N1 2.1280(18) 3
Cu N1 2.1280(18) 2
Cu N1 2.1280(18) 8
N1 C1 1.307(3) .
N1 N2 1.360(3) .
N2 N3 1.287(3) .
N3 N4 1.342(3) .
N4 C1 1.316(3) .
N4 C2 1.472(3) .
C1 H1 0.83(2) .
C2 C3 1.320(5) .
C2 H2A 0.89(4) .
C2 H2B 0.79(4) .
C3 C2 1.654(6) 5
C3 H3A 0.91(5) .
C3 H3B 0.88(5) .
Cl1 O1 1.4693(16) .
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
C1 N1 N2 N3 -0.5(2) . .
Cu N1 N2 N3 172.48(13) . .
N1 N2 N3 N4 0.5(2) . .
N2 N3 N4 C1 -0.3(2) . .
N2 N3 N4 C2 -172.8(2) . .
N2 N1 C1 N4 0.3(2) . .
Cu N1 C1 N4 -171.68(13) . .
N3 N4 C1 N1 0.0(2) . .
C2 N4 C1 N1 171.6(2) . .
C1 N4 C2 C3 77.2(4) . .
N3 N4 C2 C3 -112.1(4) . .
C1 N4 C2 C3 138.6(3) . 5
N3 N4 C2 C3 -50.7(3) . 5
N4 C2 C3 C3 97.9(3) . 5
N4 C2 C3 C2 69.4(5) . 5
C3 C2 C3 C2 -28.5(4) 5 5
