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_7058937
_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         'C10 H11 Cu N13 O8'
_chemical_formula_sum            'C10 H11 Cu N13 O8'
_chemical_formula_weight         504.86
_chemical_name_common
'bis(1-amino-5-methyltetrazolyl) copper(II) styphnate'
_chemical_name_systematic
;
bis(1-amino-5-methyltetrazolyl) copper(II) styphnate
;
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_audit_creation_date             2018-07-11
_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                   14.6007(14)
_cell_length_b                   15.0584(14)
_cell_length_c                   8.0850(7)
_cell_measurement_reflns_used    1307
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      24.9710
_cell_measurement_theta_min      4.6170
_cell_volume                     1777.6(3)
_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 0.931
_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    -25.00  17.00   1.00   42.00    --  -21.75 -99.00 120.00   42
  2  \w    -99.00 -34.00   1.00   42.00    --  -21.75-179.00 -90.00   65
  3  \w    -41.00  18.00   1.00   42.00    --  -21.75  38.00 120.00   59
  4  \w    -25.00  23.00   1.00   42.00    --  -21.75 -99.00 -90.00   48
  5  \w     -7.00  80.00   1.00   42.00    --   22.84  38.00 -90.00   87
  6  \w     39.00  92.00   1.00   42.00    --   22.84  57.00 -60.00   53
  7  \w    -48.00   7.00   1.00   42.00    --   22.84 -57.00 150.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0434705000
_diffrn_orient_matrix_UB_12      0.0203713000
_diffrn_orient_matrix_UB_13      -0.0097226000
_diffrn_orient_matrix_UB_21      0.0201345000
_diffrn_orient_matrix_UB_22      0.0422373000
_diffrn_orient_matrix_UB_23      0.0138618000
_diffrn_orient_matrix_UB_31      0.0081048000
_diffrn_orient_matrix_UB_32      0.0044687000
_diffrn_orient_matrix_UB_33      -0.0860613000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_sigmaI/netI    0.1610
_diffrn_reflns_av_unetI/netI     0.1287
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13583
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.441
_diffrn_reflns_theta_min         4.293
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92714
_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            green
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_description       needle
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.537
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 892 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4360
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0102P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.833
_reflns_number_gt                2894
_reflns_number_total             4360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03937f2.cif
_cod_data_source_block           nx263
_cod_database_code               7058937
_shelx_estimated_absorpt_t_min   0.540
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              55597