#------------------------------------------------------------------------------
#$Date: 2021-07-05 20:05:48 +0200 (lun 05 de jul de 2021) $
#$Revision: 267220 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/06/7060629.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_7060629
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 O3)'
_chemical_formula_sum            'C24 H36 Cl2 Cu N24 O6'
_chemical_formula_weight         891.21
_chemical_name_common
'hexakis(1-cyclopropyl-5H-tetrazolyl)copper(II) dichlorate'
_chemical_name_systematic
'hexakis(1-cyclopropyl-5H-tetrazolyl)copper(II) dichlorate'
_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   difmap
_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                   10.9182(10)
_cell_length_b                   10.9182(10)
_cell_length_c                   28.166(3)
_cell_measurement_reflns_used    2269
_cell_measurement_temperature    127(2)
_cell_measurement_theta_max      30.7420
_cell_measurement_theta_min      2.3000
_cell_volume                     2907.8(5)
_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  'Encifer 1.5.1, CCDC 2014'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      127(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00 -82.00   1.00   50.00    --  -28.86-178.00  30.00   26
  2  ω     45.00 100.00   1.00   50.00    --   29.64  57.00  60.00   55
  3  ω     43.00  74.00   1.00   50.00    --   29.64 -99.00-180.00   31
  4  ω     -4.00  41.00   1.00   50.00    --   29.64  82.00  51.00   45
  5  ω    -32.00  40.00   1.00   50.00    --   29.64 -77.00-150.00   72
  6  ω     -3.00  79.00   1.00   50.00    --   29.64  37.00-180.00   82
  7  ω    -38.00  53.00   1.00   50.00    --   29.64 -57.00 -90.00   91
  8  ω     44.00  95.00   1.00   50.00    --   29.64  57.00   0.00   51
  9  ω     87.00 112.00   1.00   50.00    --   29.64-178.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0169621000
_diffrn_orient_matrix_UB_12      -0.0386090000
_diffrn_orient_matrix_UB_13      -0.0215741000
_diffrn_orient_matrix_UB_21      0.0572538000
_diffrn_orient_matrix_UB_22      -0.0122326000
_diffrn_orient_matrix_UB_23      0.0035118000
_diffrn_orient_matrix_UB_31      -0.0454715000
_diffrn_orient_matrix_UB_32      -0.0632897000
_diffrn_orient_matrix_UB_33      0.0124462000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            7265
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.348
_diffrn_reflns_theta_min         2.272
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82974
_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    1.527
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1377
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0299
_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)+(0.0475P)²+1.1875P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1148
_reflns_number_total             1328
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj01675j2.cif
_cod_data_source_block           px178
_cod_depositor_comments
'Adding full bibliography for 7060620--7060640.cif.'
_cod_original_cell_volume        2907.8(6)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_database_code               7060629
_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   0.816
_shelx_estimated_absorpt_t_max   0.920
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 0.01588(16) Uani 1 6 d S T P . .
Cl1 Cl 0.666667 0.333333 0.48065(2) 0.0232(2) Uani 1 3 d S T P . .
O1 O 0.72579(16) 0.47772(14) 0.50025(5) 0.0366(4) Uani 1 1 d . . . . .
N4 N 0.18220(16) 0.12116(16) 0.54277(5) 0.0236(3) Uani 1 1 d . . . . .
N1 N 0.36097(17) 0.28257(16) 0.58042(5) 0.0248(3) Uani 1 1 d . . . . .
N2 N 0.33566(19) 0.15666(17) 0.59788(6) 0.0329(4) Uani 1 1 d . . . . .
N3 N 0.22738(18) 0.05991(17) 0.57516(6) 0.0306(4) Uani 1 1 d . . . . .
C1 C 0.2669(2) 0.2583(2) 0.54660(7) 0.0255(4) Uani 1 1 d . . . . .
C2 C 0.4847(2) 0.4139(2) 0.59421(7) 0.0279(4) Uani 1 1 d . . . . .
C3 C 0.5092(3) 0.4471(2) 0.64567(7) 0.0334(5) Uani 1 1 d . . . . .
C4 C 0.4622(3) 0.5271(2) 0.61475(8) 0.0342(5) Uani 1 1 d . . . . .
H2 H 0.560(3) 0.438(2) 0.5746(8) 0.037(6) Uiso 1 1 d . . . . .
H3A H 0.444(2) 0.380(2) 0.6652(7) 0.024(5) Uiso 1 1 d . . . . .
H1 H 0.267(2) 0.330(2) 0.5309(7) 0.023(5) Uiso 1 1 d . . . . .
H3B H 0.600(3) 0.487(2) 0.6555(7) 0.033(6) Uiso 1 1 d . . . . .
H4A H 0.371(3) 0.511(3) 0.6191(7) 0.038(6) Uiso 1 1 d . . . . .
H4B H 0.521(3) 0.615(3) 0.6072(8) 0.037(6) 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
_geom_angle_publ_flag
N4 Cu1 N4 91.10(5) 10_556 12_556 ?
N4 Cu1 N4 88.90(5) 10_556 3 ?
N4 Cu1 N4 180.00(6) 12_556 3 ?
N4 Cu1 N4 88.90(5) 10_556 2 ?
N4 Cu1 N4 88.90(5) 12_556 2 ?
N4 Cu1 N4 91.10(5) 3 2 ?
N4 Cu1 N4 91.10(5) 10_556 11_556 ?
N4 Cu1 N4 91.10(5) 12_556 11_556 ?
N4 Cu1 N4 88.90(5) 3 11_556 ?
N4 Cu1 N4 180.00(6) 2 11_556 ?
N4 Cu1 N4 180.00(9) 10_556 . ?
N4 Cu1 N4 88.90(5) 12_556 . ?
N4 Cu1 N4 91.10(5) 3 . ?
N4 Cu1 N4 91.10(5) 2 . ?
N4 Cu1 N4 88.90(5) 11_556 . ?
O1 Cl1 O1 106.92(6) 3_665 2_655 ?
O1 Cl1 O1 106.92(6) 3_665 . ?
O1 Cl1 O1 106.92(6) 2_655 . ?
C1 N4 N3 106.47(16) . . ?
C1 N4 Cu1 131.45(13) . . ?
N3 N4 Cu1 122.00(12) . . ?
C1 N1 N2 108.30(16) . . ?
C1 N1 C2 129.52(16) . . ?
N2 N1 C2 121.65(16) . . ?
N3 N2 N1 106.80(15) . . ?
N2 N3 N4 109.76(15) . . ?
N4 C1 N1 108.66(16) . . ?
N4 C1 H1 130.4(13) . . ?
N1 C1 H1 120.9(13) . . ?
N1 C2 C3 117.96(17) . . ?
N1 C2 C4 117.77(17) . . ?
C3 C2 C4 60.24(14) . . ?
N1 C2 H2 112.6(14) . . ?
C3 C2 H2 119.5(15) . . ?
C4 C2 H2 119.5(15) . . ?
C2 C3 C4 60.11(14) . . ?
C2 C3 H3A 115.1(13) . . ?
C4 C3 H3A 117.9(13) . . ?
C2 C3 H3B 115.8(14) . . ?
C4 C3 H3B 120.6(15) . . ?
H3A C3 H3B 115.5(19) . . ?
C2 C4 C3 59.64(14) . . ?
C2 C4 H4A 120.1(15) . . ?
C3 C4 H4A 117.7(15) . . ?
C2 C4 H4B 118.7(15) . . ?
C3 C4 H4B 120.3(16) . . ?
H4A C4 H4B 112(2) . . ?
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 N4 2.1275(16) 10_556 ?
Cu1 N4 2.1275(16) 12_556 ?
Cu1 N4 2.1275(16) 3 ?
Cu1 N4 2.1275(16) 2 ?
Cu1 N4 2.1275(16) 11_556 ?
Cu1 N4 2.1276(16) . ?
Cl1 O1 1.4796(14) 3_665 ?
Cl1 O1 1.4796(14) 2_655 ?
Cl1 O1 1.4796(14) . ?
N4 C1 1.313(2) . ?
N4 N3 1.361(2) . ?
N1 C1 1.327(3) . ?
N1 N2 1.352(2) . ?
N1 C2 1.447(3) . ?
N2 N3 1.294(2) . ?
C1 H1 0.90(2) . ?
C2 C3 1.486(3) . ?
C2 C4 1.493(3) . ?
C2 H2 0.91(2) . ?
C3 C4 1.495(3) . ?
C3 H3A 0.91(2) . ?
C3 H3B 0.91(2) . ?
C4 H4A 0.93(2) . ?
C4 H4B 0.87(3) . ?
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
? ? ? ? ? ? ? ?
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 -0.8(2) . . . . ?
C2 N1 N2 N3 -173.14(16) . . . . ?
N1 N2 N3 N4 0.4(2) . . . . ?
C1 N4 N3 N2 0.1(2) . . . . ?
Cu1 N4 N3 N2 -177.03(12) . . . . ?
N3 N4 C1 N1 -0.6(2) . . . . ?
Cu1 N4 C1 N1 176.15(11) . . . . ?
N2 N1 C1 N4 0.8(2) . . . . ?
C2 N1 C1 N4 172.39(17) . . . . ?
C1 N1 C2 C3 134.5(2) . . . . ?
N2 N1 C2 C3 -54.9(2) . . . . ?
C1 N1 C2 C4 65.3(3) . . . . ?
N2 N1 C2 C4 -124.10(19) . . . . ?
N1 C2 C3 C4 -107.7(2) . . . . ?
N1 C2 C4 C3 108.0(2) . . . . ?
