#------------------------------------------------------------------------------
#$Date: 2021-07-05 21:05:48 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267220 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/06/7060627.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_7060627
loop_
_publ_author_name
'Braun, Vanessa'
'Wurzenberger, Maximilian H. H.'
'Weippert, Valentin'
'Stierstorfer, Jörg'
_publ_section_title
;
 Tailoring the properties of 3d transition metal complexes with different
 N-cycloalkyl-substituted tetrazoles
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11042
_journal_page_last               11050
_journal_paper_doi               10.1039/D1NJ01675J
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C24 H36 Cu N24, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 Cu N24 O8'
_chemical_formula_weight         923.21
_chemical_name_common
'hexakis(1-cyclopropyl)tetrazole copper(II) perchlorate'
_chemical_name_systematic
'hexakis(1-cyclopropyl)tetrazole copper(II) perchlorate'
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_date             2020-05-08
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.7417(15)
_cell_length_b                   10.7417(15)
_cell_length_c                   29.826(5)
_cell_measurement_reflns_used    1599
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.3040
_cell_measurement_theta_min      2.2780
_cell_volume                     2980.4(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00 -39.00   1.00   25.00    --  -20.37-178.00 120.00   26
  2  ω     23.00  50.00   1.00   25.00    --  -20.37  57.00-150.00   27
  3  ω    -49.00  40.00   1.00   25.00    --   21.39 -57.00 -60.00   89
  4  ω     -9.00  36.00   1.00   25.00    --   21.39  77.00  60.00   45
  5  ω    -10.00  26.00   1.00   25.00    --   21.39  77.00 -60.00   36
  6  ω     -1.00  92.00   1.00   25.00    --   21.39  37.00-150.00   93
  7  ω      4.00  92.00   1.00   25.00    --   21.39  57.00  90.00   88
  8  ω     33.00  64.00   1.00   25.00    --   21.39 -99.00-180.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0625424000
_diffrn_orient_matrix_UB_12      -0.0028348000
_diffrn_orient_matrix_UB_13      -0.0097772000
_diffrn_orient_matrix_UB_21      -0.0379852000
_diffrn_orient_matrix_UB_22      -0.0712740000
_diffrn_orient_matrix_UB_23      -0.0112092000
_diffrn_orient_matrix_UB_31      -0.0164940000
_diffrn_orient_matrix_UB_32      -0.0006169000
_diffrn_orient_matrix_UB_33      -0.0370889000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.1733
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            7345
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         2.048
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             1425
_exptl_crystal_size_max          0.458
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0405
_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)+(0.0423P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1124
_reflns_number_total             1363
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj01675j2.cif
_cod_data_source_block           px179
_cod_depositor_comments
'Adding full bibliography for 7060620--7060640.cif.'
_cod_original_cell_volume        2980.4(10)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_database_code               7060627
_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   0.722
_shelx_estimated_absorpt_t_max   0.962
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.000000 0.000000 0.500000 0.0183(2) Uani 1 6 d S T P . .
N1 N 0.1844(2) 0.1182(2) 0.54115(7) 0.0267(5) Uani 1 1 d . . . . .
N2 N 0.2233(2) 0.0521(2) 0.57272(8) 0.0341(6) Uani 1 1 d . . . . .
N3 N 0.3287(2) 0.1470(2) 0.59662(8) 0.0362(6) Uani 1 1 d . . . . .
N4 N 0.3586(2) 0.2772(2) 0.58074(7) 0.0274(5) Uani 1 1 d . . . . .
C1 C 0.2707(3) 0.2575(2) 0.54717(9) 0.0274(6) Uani 1 1 d . . . . .
H1 H 0.269574 0.331534 0.530072 0.033 Uiso 1 1 calc R U . . .
C2 C 0.4823(3) 0.4087(3) 0.59670(9) 0.0305(6) Uani 1 1 d . . . . .
H2 H 0.570996 0.448015 0.577859 0.037 Uiso 1 1 calc R U . . .
C3 C 0.5049(3) 0.4289(3) 0.64600(10) 0.0353(7) Uani 1 1 d . . . . .
H3A H 0.605038 0.477844 0.657212 0.042 Uiso 1 1 calc R U . . .
H3B H 0.433888 0.352192 0.665786 0.042 Uiso 1 1 calc R U . . .
C4 C 0.4567(3) 0.5165(3) 0.62013(9) 0.0353(7) Uani 1 1 d . . . . .
H4A H 0.355907 0.493892 0.623936 0.042 Uiso 1 1 calc R U . . .
H4B H 0.527082 0.619563 0.615361 0.042 Uiso 1 1 calc R U . . .
Cl1 Cl 0.666667 0.333333 0.49056(4) 0.0243(3) Uani 1 3 d S T P . .
O1 O 0.666667 0.333333 0.44273(12) 0.0516(10) Uani 1 3 d S T P . .
O2 O 0.70482(19) 0.47336(18) 0.50722(7) 0.0408(5) Uani 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
_geom_angle_publ_flag
N1 Cu1 N1 89.95(8) . 11_556 ?
N1 Cu1 N1 90.05(8) . 2 ?
N1 Cu1 N1 180.00(9) 11_556 2 ?
N1 Cu1 N1 180.00(9) . 10_556 ?
N1 Cu1 N1 90.05(8) 11_556 10_556 ?
N1 Cu1 N1 89.95(8) 2 10_556 ?
N1 Cu1 N1 89.95(8) . 12_556 ?
N1 Cu1 N1 90.05(8) 11_556 12_556 ?
N1 Cu1 N1 89.95(8) 2 12_556 ?
N1 Cu1 N1 90.05(8) 10_556 12_556 ?
N1 Cu1 N1 90.05(8) . 3 ?
N1 Cu1 N1 89.95(8) 11_556 3 ?
N1 Cu1 N1 90.05(8) 2 3 ?
N1 Cu1 N1 89.95(8) 10_556 3 ?
N1 Cu1 N1 180.00(8) 12_556 3 ?
C1 N1 N2 105.8(2) . . ?
C1 N1 Cu1 132.14(17) . . ?
N2 N1 Cu1 121.56(15) . . ?
N3 N2 N1 110.19(19) . . ?
N2 N3 N4 106.4(2) . . ?
C1 N4 N3 108.6(2) . . ?
C1 N4 C2 129.7(2) . . ?
N3 N4 C2 121.2(2) . . ?
N4 C1 N1 109.0(2) . . ?
N4 C1 H1 125.5 . . ?
N1 C1 H1 125.5 . . ?
N4 C2 C3 117.9(2) . . ?
N4 C2 C4 118.3(2) . . ?
C3 C2 C4 60.26(18) . . ?
N4 C2 H2 116.2 . . ?
C3 C2 H2 116.2 . . ?
C4 C2 H2 116.2 . . ?
C2 C3 C4 59.98(17) . . ?
C2 C3 H3A 117.8 . . ?
C4 C3 H3A 117.8 . . ?
C2 C3 H3B 117.8 . . ?
C4 C3 H3B 117.8 . . ?
H3A C3 H3B 114.9 . . ?
C2 C4 C3 59.76(17) . . ?
C2 C4 H4A 117.8 . . ?
C3 C4 H4A 117.8 . . ?
C2 C4 H4B 117.8 . . ?
C3 C4 H4B 117.8 . . ?
H4A C4 H4B 114.9 . . ?
O1 Cl1 O2 110.24(9) . 3_665 ?
O1 Cl1 O2 110.24(9) . 2_655 ?
O2 Cl1 O2 108.69(9) 3_665 2_655 ?
O1 Cl1 O2 110.25(9) . . ?
O2 Cl1 O2 108.69(9) 3_665 . ?
O2 Cl1 O2 108.68(9) 2_655 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.128(2) . ?
Cu1 N1 2.128(2) 11_556 ?
Cu1 N1 2.128(2) 2 ?
Cu1 N1 2.128(2) 10_556 ?
Cu1 N1 2.128(2) 12_556 ?
Cu1 N1 2.128(2) 3 ?
N1 C1 1.320(3) . ?
N1 N2 1.364(3) . ?
N2 N3 1.294(3) . ?
N3 N4 1.354(3) . ?
N4 C1 1.319(3) . ?
N4 C2 1.453(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.488(4) . ?
C2 C4 1.492(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.496(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
Cl1 O1 1.427(4) . ?
Cl1 O2 1.4355(17) 3_665 ?
Cl1 O2 1.4355(18) 2_655 ?
Cl1 O2 1.4356(17) . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 O2 0.95 2.26 3.209(3) 172.8 10_666
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.3(3) . . . . ?
Cu1 N1 N2 N3 -173.07(15) . . . . ?
N1 N2 N3 N4 0.5(3) . . . . ?
N2 N3 N4 C1 -0.6(3) . . . . ?
N2 N3 N4 C2 -173.2(2) . . . . ?
N3 N4 C1 N1 0.4(3) . . . . ?
C2 N4 C1 N1 172.2(2) . . . . ?
N2 N1 C1 N4 -0.1(3) . . . . ?
Cu1 N1 C1 N4 171.62(16) . . . . ?
C1 N4 C2 C3 140.7(3) . . . . ?
N3 N4 C2 C3 -48.5(3) . . . . ?
C1 N4 C2 C4 71.3(3) . . . . ?
N3 N4 C2 C4 -117.9(3) . . . . ?
N4 C2 C3 C4 -108.4(2) . . . . ?
N4 C2 C4 C3 107.8(2) . . . . ?
