#------------------------------------------------------------------------------
#$Date: 2019-11-25 23:01:00 +0200 (Mon, 25 Nov 2019) $
#$Revision: 242010 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/19/4131930.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_4131930
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         '	C6 H12 Cu N12, 2(Cl O3)'
_chemical_formula_sum            'C6 H12 Cl2 Cu N12 O6'
_chemical_formula_weight         482.72
_chemical_name_common
'tris(4-amino-1,2,4-triazolyl) copper(II) chlorate'
_chemical_name_systematic
;
tris(4-amino-1,2,4-triazolyl) copper(II) chlorate
;
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date
;
'Mon May 22 14:20:31 2017'
;
_audit_creation_method           SHELXL-2013
_audit_update_record             11.07.2017
_cell_angle_alpha                90
_cell_angle_beta                 91.559(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5622(16)
_cell_length_b                   15.5713(18)
_cell_length_c                   7.7338(15)
_cell_measurement_reflns_used    693
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      23.4030
_cell_measurement_theta_min      4.6880
_cell_volume                     1632.6(4)
_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      143(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   41.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000    0.0000 28

#__ type_ start__ end____ width___ exp.time_
  2 omega   60.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -30.0000 47

#__ type_ start__ end____ width___ exp.time_
  3 omega   58.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  150.0000 48

#__ type_ start__ end____ width___ exp.time_
  4 omega   -1.00  102.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  -30.0000 103

#__ type_ start__ end____ width___ exp.time_
  5 omega   38.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000  -90.0000 30

#__ type_ start__ end____ width___ exp.time_
  6 omega  -25.00   73.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  150.0000 98

#__ type_ start__ end____ width___ exp.time_
  7 omega  -33.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932    0.0000  150.0000 128

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0148423000
_diffrn_orient_matrix_UB_12      0.0018458000
_diffrn_orient_matrix_UB_13      -0.0886371000
_diffrn_orient_matrix_UB_21      0.0404466000
_diffrn_orient_matrix_UB_22      0.0273354000
_diffrn_orient_matrix_UB_23      -0.0167763000
_diffrn_orient_matrix_UB_31      0.0296618000
_diffrn_orient_matrix_UB_32      -0.0363639000
_diffrn_orient_matrix_UB_33      -0.0170867000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1095
_diffrn_reflns_av_sigmaI/netI    0.2080
_diffrn_reflns_av_unetI/netI     0.1081
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6915
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.996
_diffrn_reflns_theta_min         4.204
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68997
_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    1.964
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.212
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0849P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1166
_reflns_number_total             1844
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b13230_si_002.cif
_cod_data_source_block           mx232
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4131930
_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   0.782
_shelx_estimated_absorpt_t_max   0.846
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.5000 0.0000 0.0175(4) Uani 1 4 d S T P . .
Cu2 Cu 0.5000 0.5000 0.5000 0.0232(4) Uani 1 4 d S T P . .
N1 N 0.4420(3) 0.4027(4) 0.1709(7) 0.0277(12) Uani 1 1 d . . . . .
N2 N 0.4390(3) 0.4066(3) 0.3464(7) 0.0243(11) Uani 1 1 d . . . . .
N3 N 0.3707(4) 0.2881(3) 0.2651(7) 0.0289(12) Uani 1 1 d . . . . .
N4 N 0.3220(4) 0.2073(3) 0.2680(8) 0.0363(14) Uani 1 1 d . . . . .
H4A H 0.2613 0.2155 0.2636 0.044 Uiso 1 1 d R U . . .
H4B H 0.3445 0.1974 0.1457 0.044 Uiso 1 1 d R U . . .
N9 N 0.3693(5) 0.5000 -0.1355(8) 0.0215(15) Uani 1 2 d S T P . .
N10 N 0.3612(5) 0.5000 -0.3117(9) 0.0266(17) Uani 1 2 d S T P . .
N11 N 0.2150(5) 0.5000 -0.2091(10) 0.0270(17) Uani 1 2 d S T P . .
N12 N 0.1107(7) 0.5000 -0.2074(16) 0.059(4) Uani 1 2 d S T P . .
C1 C 0.3956(5) 0.3360(4) 0.4023(9) 0.0309(15) Uani 1 1 d . . . . .
H1 H 0.3842 0.3219 0.5197 0.037 Uiso 1 1 calc R U . . .
C2 C 0.3998(4) 0.3307(5) 0.1249(8) 0.0313(15) Uani 1 1 d . . . . .
H2 H 0.3910 0.3112 0.0091 0.038 Uiso 1 1 calc R U . . .
C5 C 0.2666(7) 0.5000 -0.3498(12) 0.033(2) Uani 1 2 d S T P . .
H5 H 0.2391 0.5000 -0.4641 0.040 Uiso 1 2 calc R U P . .
C6 C 0.2802(7) 0.5000 -0.0756(13) 0.041(3) Uani 1 2 d S T P . .
H6 H 0.2642 0.5000 0.0433 0.050 Uiso 1 2 calc R U P . .
Cl1 Cl 0.10133(16) 0.35430(12) 0.2477(3) 0.0536(6) Uani 1 1 d . . . . .
O1 O 0.1059(3) 0.2589(3) 0.2471(7) 0.0403(12) Uani 1 1 d . . . . .
O2A O 0.1720(8) 0.3818(7) 0.3847(17) 0.041(3) Uani 0.487(13) 1 d . . P A 1
O3A O 0.1772(7) 0.3765(6) 0.0850(13) 0.037(3) Uani 0.487(13) 1 d . . P A 1
O2B O 0.1855(6) 0.3928(6) 0.2571(17) 0.039(3) Uani 0.513(13) 1 d . . P A 2
O3B O 0.0317(7) 0.3737(7) 0.1087(13) 0.050(4) Uani 0.513(13) 1 d . . P A 2
H12A H 0.093(7) 0.467(7) -0.146(13) 0.09(4) Uiso 1 1 d . . . . .
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'
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'
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
N9 Cu1 N9 180.0(3) . 5_665
N9 Cu1 N1 89.35(18) . .
N9 Cu1 N1 90.65(18) 5_665 .
N9 Cu1 N1 89.35(18) . 6_565
N9 Cu1 N1 90.65(18) 5_665 6_565
N1 Cu1 N1 88.5(3) . 6_565
N9 Cu1 N1 90.65(18) . 2_655
N9 Cu1 N1 89.35(18) 5_665 2_655
N1 Cu1 N1 91.5(3) . 2_655
N1 Cu1 N1 180.0 6_565 2_655
N9 Cu1 N1 90.65(18) . 5_665
N9 Cu1 N1 89.35(18) 5_665 5_665
N1 Cu1 N1 180.0 . 5_665
N1 Cu1 N1 91.5(3) 6_565 5_665
N1 Cu1 N1 88.5(3) 2_655 5_665
N2 Cu2 N2 180.0 . 5_666
N2 Cu2 N2 91.0(3) . 6_565
N2 Cu2 N2 89.0(3) 5_666 6_565
N2 Cu2 N2 89.0(3) . 2_656
N2 Cu2 N2 91.0(3) 5_666 2_656
N2 Cu2 N2 180.0 6_565 2_656
N2 Cu2 N10 87.67(18) . 5_665
N2 Cu2 N10 92.33(18) 5_666 5_665
N2 Cu2 N10 87.67(18) 6_565 5_665
N2 Cu2 N10 92.33(18) 2_656 5_665
N2 Cu2 N10 92.33(18) . 1_556
N2 Cu2 N10 87.67(18) 5_666 1_556
N2 Cu2 N10 92.33(18) 6_565 1_556
N2 Cu2 N10 87.67(18) 2_656 1_556
N10 Cu2 N10 180.0 5_665 1_556
C2 N1 N2 106.6(5) . .
C2 N1 Cu1 126.7(4) . .
N2 N1 Cu1 126.6(4) . .
C1 N2 N1 108.3(5) . .
C1 N2 Cu2 125.4(4) . .
N1 N2 Cu2 126.2(4) . .
C1 N3 C2 107.1(6) . .
C1 N3 N4 126.2(6) . .
C2 N3 N4 126.7(6) . .
N3 N4 H4A 108.9 . .
N3 N4 H4B 88.2 . .
H4A N4 H4B 107.9 . .
C6 N9 N10 107.7(7) . .
C6 N9 Cu1 128.2(6) . .
N10 N9 Cu1 124.1(5) . .
C5 N10 N9 106.1(7) . .
C5 N10 Cu2 129.8(6) . 1_554
N9 N10 Cu2 124.1(5) . 1_554
C5 N11 C6 106.4(8) . .
C5 N11 N12 124.4(8) . .
C6 N11 N12 129.2(8) . .
N11 N12 H12A 110(8) . .
N2 C1 N3 108.0(6) . .
N2 C1 H1 126.0 . .
N3 C1 H1 126.0 . .
N1 C2 N3 110.0(6) . .
N1 C2 H2 125.0 . .
N3 C2 H2 125.0 . .
N10 C5 N11 110.9(8) . .
N10 C5 H5 124.6 . .
N11 C5 H5 124.6 . .
N9 C6 N11 108.9(8) . .
N9 C6 H6 125.5 . .
N11 C6 H6 125.5 . .
O2B Cl1 O3B 120.3(7) . .
O2B Cl1 O1 115.3(5) . .
O3B Cl1 O1 103.5(5) . .
O2A Cl1 O1 105.4(5) . .
O2A Cl1 O3A 94.6(7) . .
O1 Cl1 O3A 100.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N9 2.034(7) .
Cu1 N9 2.034(7) 5_665
Cu1 N1 2.172(6) .
Cu1 N1 2.172(6) 6_565
Cu1 N1 2.172(6) 2_655
Cu1 N1 2.172(6) 5_665
Cu2 N2 2.039(5) .
Cu2 N2 2.039(5) 5_666
Cu2 N2 2.039(5) 6_565
Cu2 N2 2.039(5) 2_656
Cu2 N10 2.411(7) 5_665
Cu2 N10 2.411(7) 1_556
N1 C2 1.304(9) .
N1 N2 1.361(7) .
N2 C1 1.325(9) .
N3 C1 1.333(8) .
N3 C2 1.339(9) .
N3 N4 1.421(7) .
N4 H4A 0.8325 .
N4 H4B 1.0142 .
N9 C6 1.306(11) .
N9 N10 1.364(9) .
N10 C5 1.308(11) .
N10 Cu2 2.411(7) 1_554
N11 C5 1.310(12) .
N11 C6 1.342(11) .
N11 N12 1.414(11) .
N12 H12A 0.74(10) .
C1 H1 0.9500 .
C2 H2 0.9500 .
C5 H5 0.9500 .
C6 H6 0.9500 .
Cl1 O2B 1.290(9) .
Cl1 O3B 1.443(9) .
Cl1 O2A 1.473(10) .
Cl1 O1 1.486(5) .
Cl1 O3A 1.683(10) .
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
C2 N1 N2 C1 0.6(6) . .
Cu1 N1 N2 C1 178.2(4) . .
C2 N1 N2 Cu2 176.2(4) . .
Cu1 N1 N2 Cu2 -6.3(6) . .
C6 N9 N10 C5 0.000(1) . .
Cu1 N9 N10 C5 180.000(1) . .
C6 N9 N10 Cu2 180.0 . 1_554
Cu1 N9 N10 Cu2 0.000(0) . 1_554
N1 N2 C1 N3 -0.4(7) . .
Cu2 N2 C1 N3 -176.0(4) . .
C2 N3 C1 N2 0.1(7) . .
N4 N3 C1 N2 -179.5(5) . .
N2 N1 C2 N3 -0.6(7) . .
Cu1 N1 C2 N3 -178.1(4) . .
C1 N3 C2 N1 0.3(7) . .
N4 N3 C2 N1 179.9(5) . .
N9 N10 C5 N11 0.000(1) . .
Cu2 N10 C5 N11 180.000(1) 1_554 .
C6 N11 C5 N10 0.000(1) . .
N12 N11 C5 N10 180.000(1) . .
N10 N9 C6 N11 0.000(1) . .
Cu1 N9 C6 N11 180.000(0) . .
C5 N11 C6 N9 0.000(0) . .
N12 N11 C6 N9 180.000(0) . .
