Tailoring the properties of 3d transition metal complexes with different N-cycloalkyl-substituted tetrazoles
Braun, Vanessa; Wurzenberger, Maximilian H. H.; Weippert, Valentin; Stierstorfer, Jörg; New Journal of Chemistry 45 (2021) 11042–11050; doi:10.1039/D1NJ01675J

data_7060623
_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         'C15 H24 Cu N14 O6'
_chemical_formula_sum            'C15 H24 Cu N14 O6'
_chemical_formula_weight         560.02
_chemical_name_common
'dinitrato tris(1-cyclobutyl-5H-tetrazolyl) copper(II)'
_chemical_name_systematic
'dinitrato tris(1-cyclobutyl-5H-tetrazolyl) copper(II)'
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_audit_creation_date             2020-05-29
_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                 102.235(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4489(4)
_cell_length_b                   13.0298(5)
_cell_length_c                   17.6353(7)
_cell_measurement_reflns_used    8379
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      31.8950
_cell_measurement_theta_min      2.5390
_cell_volume                     2346.46(16)
_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      105(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  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -103.00 -46.00   1.00   12.00    --  -28.70 153.00 109.00   57
  2  \w    -54.00  37.00   1.00   12.00    --  -28.70  77.00 -30.00   91
  3  \w    -61.00  30.00   1.00   12.00    --  -28.70  77.00  60.00   91
  4  \w     39.00 102.00   1.00   12.00    --   29.64 178.00-150.00   63
  5  \w    -21.00  12.00   1.00   12.00    --   29.64 110.00 -88.81   33
  6  \w      6.00  82.00   1.00   12.00    --   29.64  57.00  30.00   76
  7  \w    -41.00  -1.00   1.00   12.00    --   29.64 -57.00-180.00   40
  8  \w      6.00 100.00   1.00   12.00    --   29.64  57.00 120.00   94
  9  \w    -33.00  -4.00   1.00   12.00    --   29.64 130.00  68.25   29
 10  \w     -3.00 103.00   1.00   12.00    --   29.64  37.00 -30.00  106
 11  \w      6.00 100.00   1.00   12.00    --   29.64  57.00-150.00   94
 12  \w    -43.00  59.00   1.00   12.00    --   29.64 -37.00-150.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0522833000
_diffrn_orient_matrix_UB_12      -0.0350506000
_diffrn_orient_matrix_UB_13      0.0010553000
_diffrn_orient_matrix_UB_21      0.0182433000
_diffrn_orient_matrix_UB_22      0.0055921000
_diffrn_orient_matrix_UB_23      0.0408972000
_diffrn_orient_matrix_UB_31      -0.0419517000
_diffrn_orient_matrix_UB_32      -0.0412392000
_diffrn_orient_matrix_UB_33      0.0046261000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23149
_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         30.501
_diffrn_reflns_theta_min         1.959
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83647
_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    1.585
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.198
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.381(9)
_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     422
_refine_ls_number_reflns         7161
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0269
_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/[\s^2^(Fo^2^)+(0.0276P)^2^+0.4941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6720
_reflns_number_total             7161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01675j2.cif
_cod_data_source_block           px206
_cod_depositor_comments
'Adding full bibliography for 7060620--7060640.cif.'
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               7060623
_shelx_estimated_absorpt_t_min   0.700
_shelx_estimated_absorpt_t_max   0.827
_shelx_res_checksum              23603