Synthesis and Comparison of Copper(II) Complexes with various N-Aminotetrazole Ligands Involving Trinitrophenol Anions
Stierstorfer, Joerg; Wurzenberger, Maximilian Hans Horst; Lommel, Marcus; Gruhne, Michael S.; Szimhardt, Norbert; Bissinger, Benjamin; New Journal of Chemistry 43 (2019) 18193–18202; doi:10.1039/C9NJ03937F

data_7058946
_publ_section_title
;
 Synthesis and Comparison of Copper(II) Complexes with various
 N-Aminotetrazole Ligands Involving Trinitrophenol Anions
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18193
_journal_page_last               18202
_journal_paper_doi               10.1039/C9NJ03937F
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         ' C9 H9 N5'
_chemical_formula_sum            'C9 H9 N5'
_chemical_formula_weight         187.21
_chemical_name_common            '1-amino-5-methyl-tetrazole benzhydrazone'
_chemical_name_systematic
' (E)-1-phenyl-N-(5-methyl-1H-tetrazol-1-yl)methanimine '
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_date             2018-11-27
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-24 deposited with the CCDC.    2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.862(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5832(8)
_cell_length_b                   7.4944(4)
_cell_length_c                   11.9045(8)
_cell_measurement_reflns_used    3593
_cell_measurement_temperature    129(2)
_cell_measurement_theta_max      32.2000
_cell_measurement_theta_min      3.9080
_cell_volume                     905.05(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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      129(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 0.936
_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    -83.00 -57.00   1.00   10.00    --  -28.86-178.00  30.00   26
  2  \w    -98.00 -17.00   1.00   10.00    --  -28.86 -57.00   0.00   81
  3  \w    -17.00  40.00   1.00   10.00    --  -28.86  57.00 150.00   57
  4  \w     -3.00  97.00   1.00   10.00    --   30.11  77.00-120.00  100
  5  \w    -24.00   1.00   1.00   10.00    --   30.11 -99.00-120.00   25
  6  \w    -23.00  67.00   1.00   10.00    --   30.11 -99.00 120.00   90
  7  \w    -25.00  73.00   1.00   10.00    --   30.11 -99.00 -30.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0276361000
_diffrn_orient_matrix_UB_12      -0.0309942000
_diffrn_orient_matrix_UB_13      -0.0640954000
_diffrn_orient_matrix_UB_21      0.0613638000
_diffrn_orient_matrix_UB_22      0.0134223000
_diffrn_orient_matrix_UB_23      0.0015232000
_diffrn_orient_matrix_UB_31      0.0189952000
_diffrn_orient_matrix_UB_32      -0.0884268000
_diffrn_orient_matrix_UB_33      0.0227118000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9657
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.222
_diffrn_reflns_theta_min         3.380
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.335
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0673P)^2^+0.2054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2511
_reflns_number_total             2995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03937f2.cif
_cod_data_source_block           nx457
_cod_original_cell_volume        905.05(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7058946
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              18475