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_7058949
_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         'C2 H5 N5'
_chemical_formula_sum            'C2 H5 N5'
_chemical_formula_weight         99.11
_chemical_name_common            1-amino-5-methyltetrazole
_chemical_name_systematic
;
1-amino-5-methyltetrazole
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_audit_creation_date             2018-05-24
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-10-24 deposited with the CCDC.    2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7191(4)
_cell_length_b                   7.7483(5)
_cell_length_c                   10.4586(7)
_cell_measurement_reflns_used    1511
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      31.3710
_cell_measurement_theta_min      4.6860
_cell_volume                     463.46(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      143(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.938
_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     44.00  95.20   0.80   10.00    --   29.79  77.00 120.00   64
  2  \w     55.00  99.00   0.80   10.00    --   29.79  57.00   0.00   55
  3  \w    -17.00  75.00   0.80   10.00    --   29.79 -99.00 -30.00  115
  4  \w     56.00 112.00   0.80   10.00    --   29.79-179.00 -90.00   70
  5  \w    -25.00  65.40   0.80   10.00    --   29.79 -99.00  90.00  113
  6  \w    -40.00  39.20   0.80   10.00    --   29.79 -57.00-150.00   99
  7  \w    -96.00 -72.00   0.80   10.00    --  -28.70 -57.00  90.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1213768000
_diffrn_orient_matrix_UB_12      0.0016440000
_diffrn_orient_matrix_UB_13      -0.0140435000
_diffrn_orient_matrix_UB_21      -0.0200347000
_diffrn_orient_matrix_UB_22      -0.0631980000
_diffrn_orient_matrix_UB_23      0.0477999000
_diffrn_orient_matrix_UB_31      -0.0161084000
_diffrn_orient_matrix_UB_32      0.0662215000
_diffrn_orient_matrix_UB_33      0.0459681000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4787
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.438
_diffrn_reflns_theta_min         4.429
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.134
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 469 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0482P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.649
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.887
_reflns_number_gt                1360
_reflns_number_total             1534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03937f2.cif
_cod_data_source_block           nx192
_cod_database_code               7058949
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              90474