#------------------------------------------------------------------------------
#$Date: 2021-07-05 20:05:48 +0200 (lun 05 de jul de 2021) $
#$Revision: 267220 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/06/7060635.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_7060635
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         'C5 H8 Cu N10'
_chemical_formula_sum            'C5 H8 Cu N10'
_chemical_formula_weight         271.75
_chemical_name_common
'diazido 1-cyclobutyl-5H-tetrazolyl copper(II)'
_chemical_name_systematic
'diazido 1-cyclobutyl-5H-tetrazolyl copper(II)'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_date             2020-06-19
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.305(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1598(14)
_cell_length_b                   6.2457(3)
_cell_length_c                   10.8574(5)
_cell_measurement_reflns_used    1395
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      27.3230
_cell_measurement_theta_min      2.8050
_cell_volume                     1004.40(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (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      106(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_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     13.00  78.00   1.00   25.00    --   21.23  57.00  60.00   65
  2  ω     -9.00  36.00   1.00   25.00    --   21.23  77.00  30.00   45
  3  ω    -11.00  27.00   1.00   25.00    --   21.23  77.00 150.00   38
  4  ω    -47.00  34.00   1.00   25.00    --   21.23 -57.00 150.00   81
  5  ω    -40.00  97.00   1.00   25.00    --   21.23  19.00 -30.00  137
  6  ω     23.00  64.00   1.00   25.00    --   21.23 -99.00 -90.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0027156000
_diffrn_orient_matrix_UB_12      0.0121211000
_diffrn_orient_matrix_UB_13      -0.0656579000
_diffrn_orient_matrix_UB_21      -0.0465888000
_diffrn_orient_matrix_UB_22      0.0248373000
_diffrn_orient_matrix_UB_23      -0.0087053000
_diffrn_orient_matrix_UB_31      0.0107995000
_diffrn_orient_matrix_UB_32      0.1101245000
_diffrn_orient_matrix_UB_33      0.0091758000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         2.750
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.166
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       platelet
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.461
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0450
_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)+(0.0395P)²+0.9872P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1547
_reflns_number_total             2055
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj01675j2.cif
_cod_data_source_block           px234
_cod_depositor_comments
'Adding full bibliography for 7060620--7060640.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7060635
_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   0.479
_shelx_estimated_absorpt_t_max   0.950
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.03919(4) 0.04591(7) 0.14243(4) 0.01502(17) Uani 1 1 d . . . . .
N1 N 0.2681(2) 0.0725(5) 0.4202(3) 0.0170(8) Uani 1 1 d . . . . .
N2 N 0.3058(3) 0.0237(6) 0.3221(3) 0.0233(8) Uani 1 1 d . . . . .
N3 N 0.2406(3) 0.0058(6) 0.2245(3) 0.0248(9) Uani 1 1 d . . . . .
N4 N 0.1601(2) 0.0403(5) 0.2568(3) 0.0131(7) Uani 1 1 d . . . . .
N6 N -0.0143(2) 0.1763(5) 0.2784(3) 0.0154(7) Uani 1 1 d . . . . .
N7 N -0.0563(2) 0.0569(5) 0.3320(3) 0.0169(7) Uani 1 1 d . . . . .
N9 N -0.0776(2) 0.0528(5) 0.0150(3) 0.0161(7) Uani 1 1 d . . . . .
N10 N -0.1503(2) 0.0702(5) 0.0429(3) 0.0155(7) Uani 1 1 d . . . . .
N11 N -0.2177(3) 0.0885(6) 0.0718(3) 0.0265(9) Uani 1 1 d . . . . .
C1 C 0.1799(3) 0.0819(6) 0.3793(4) 0.0171(9) Uani 1 1 d . . . . .
H1 H 0.137301 0.113421 0.429557 0.021 Uiso 1 1 calc R U . . .
C2 C 0.3215(3) 0.1000(6) 0.5479(4) 0.0211(10) Uani 1 1 d . . . . .
H2 H 0.280907 0.140466 0.605705 0.025 Uiso 1 1 calc R U . . .
C3 C 0.4022(3) 0.2520(7) 0.5678(4) 0.0288(11) Uani 1 1 d . . . . .
H3A H 0.390340 0.394454 0.600894 0.035 Uiso 1 1 calc R U . . .
H3B H 0.430395 0.265097 0.493907 0.035 Uiso 1 1 calc R U . . .
C4 C 0.4513(3) 0.0939(7) 0.6701(4) 0.0290(11) Uani 1 1 d . . . . .
H4A H 0.514880 0.065402 0.666284 0.035 Uiso 1 1 calc R U . . .
H4B H 0.445831 0.131029 0.756847 0.035 Uiso 1 1 calc R U . . .
C5 C 0.3845(3) -0.0803(7) 0.6071(4) 0.0274(11) Uani 1 1 d . . . . .
H5A H 0.407267 -0.169606 0.545211 0.033 Uiso 1 1 calc R U . . .
H5B H 0.360176 -0.170027 0.667296 0.033 Uiso 1 1 calc R U . . .
N8 N -0.0971(3) -0.0537(5) 0.3840(3) 0.0274(9) 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'
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'
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
_geom_angle_publ_flag
N4 Cu1 N9 175.22(13) . . ?
N4 Cu1 N6 90.63(13) . . ?
N9 Cu1 N6 93.64(13) . . ?
N4 Cu1 N9 97.47(13) . 3 ?
N9 Cu1 N9 78.06(15) . 3 ?
N6 Cu1 N9 170.00(13) . 3 ?
C1 N1 N2 108.4(3) . . ?
C1 N1 C2 129.2(3) . . ?
N2 N1 C2 122.4(4) . . ?
N3 N2 N1 106.8(3) . . ?
N2 N3 N4 110.4(3) . . ?
C1 N4 N3 105.5(3) . . ?
C1 N4 Cu1 127.3(3) . . ?
N3 N4 Cu1 127.1(3) . . ?
N7 N6 Cu1 116.3(2) . . ?
N8 N7 N6 178.8(4) . . ?
N10 N9 Cu1 123.2(3) . . ?
N10 N9 Cu1 133.2(3) . 3 ?
Cu1 N9 Cu1 101.94(15) . 3 ?
N11 N10 N9 178.4(4) . . ?
N1 C1 N4 109.0(4) . . ?
N1 C1 H1 125.5 . . ?
N4 C1 H1 125.5 . . ?
N1 C2 C3 118.2(3) . . ?
N1 C2 C5 118.9(3) . . ?
C3 C2 C5 89.3(3) . . ?
N1 C2 H2 109.6 . . ?
C3 C2 H2 109.6 . . ?
C5 C2 H2 109.6 . . ?
C2 C3 C4 87.3(3) . . ?
C2 C3 H3A 114.1 . . ?
C4 C3 H3A 114.1 . . ?
C2 C3 H3B 114.1 . . ?
C4 C3 H3B 114.1 . . ?
H3A C3 H3B 111.3 . . ?
C5 C4 C3 87.8(3) . . ?
C5 C4 H4A 114.0 . . ?
C3 C4 H4A 114.0 . . ?
C5 C4 H4B 114.0 . . ?
C3 C4 H4B 114.0 . . ?
H4A C4 H4B 111.2 . . ?
C2 C5 C4 87.6(3) . . ?
C2 C5 H5A 114.0 . . ?
C4 C5 H5A 114.0 . . ?
C2 C5 H5B 114.0 . . ?
C4 C5 H5B 114.0 . . ?
H5A C5 H5B 111.2 . . ?
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 1.983(3) . ?
Cu1 N9 2.002(3) . ?
Cu1 N6 2.002(3) . ?
Cu1 N9 2.016(3) 3 ?
N1 C1 1.318(5) . ?
N1 N2 1.346(5) . ?
N1 C2 1.459(5) . ?
N2 N3 1.292(5) . ?
N3 N4 1.357(5) . ?
N4 C1 1.326(5) . ?
N6 N7 1.208(4) . ?
N7 N8 1.152(5) . ?
N9 N10 1.209(5) . ?
N10 N11 1.137(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.527(6) . ?
C2 C5 1.527(6) . ?
C2 H2 1.0000 . ?
C3 C4 1.553(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.544(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
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 N8 0.95 2.27 3.096(5) 145.5 3_556
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 0.4(4) . . . . ?
C2 N1 N2 N3 178.5(3) . . . . ?
N1 N2 N3 N4 -0.5(4) . . . . ?
N2 N3 N4 C1 0.5(4) . . . . ?
N2 N3 N4 Cu1 176.9(3) . . . . ?
N2 N1 C1 N4 -0.1(4) . . . . ?
C2 N1 C1 N4 -178.0(3) . . . . ?
N3 N4 C1 N1 -0.2(4) . . . . ?
Cu1 N4 C1 N1 -176.6(2) . . . . ?
C1 N1 C2 C3 -130.8(4) . . . . ?
N2 N1 C2 C3 51.5(5) . . . . ?
C1 N1 C2 C5 122.9(5) . . . . ?
N2 N1 C2 C5 -54.8(5) . . . . ?
N1 C2 C3 C4 -143.9(4) . . . . ?
C5 C2 C3 C4 -21.1(3) . . . . ?
C2 C3 C4 C5 20.9(3) . . . . ?
N1 C2 C5 C4 143.5(4) . . . . ?
C3 C2 C5 C4 21.2(3) . . . . ?
C3 C4 C5 C2 -20.8(3) . . . . ?
