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_7058938
_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         'C8 H22 Cu N20 O, 2(C6 H2 N3 O9)'
_chemical_formula_sum            'C20 H26 Cu N26 O19'
_chemical_formula_weight         998.21
_chemical_name_common
;
monoaqua tetrakis(1-amino-5-methyl-tetrazolyl)copper(II) trinitrophloglucinate
;
_chemical_name_systematic
;
monoaqua tetrakis(1-amino-5-methyl-tetrazolyl)copper(II) trinitrophloglucinate
;
_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   mixed
_audit_creation_date             2018-07-24
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-08-26 deposited with the CCDC.    2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.152(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8633(3)
_cell_length_b                   16.3608(8)
_cell_length_c                   32.863(2)
_cell_measurement_reflns_used    2439
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      25.2180
_cell_measurement_theta_min      4.3300
_cell_volume                     3687.6(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 0.992
_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    -90.00   3.00   1.00   37.50    --  -20.29 -57.00  30.00   93
  2  \w    -44.00  50.00   1.00   37.50    --  -20.29  57.00-180.00   94
  3  \w    -13.00  25.00   1.00   37.50    --  -20.29 -99.00-180.00   38
  4  \w    -49.00  52.00   1.00   37.50    --   21.39 -77.00 -60.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0013936000
_diffrn_orient_matrix_UB_12      0.0260275000
_diffrn_orient_matrix_UB_13      -0.0172555000
_diffrn_orient_matrix_UB_21      0.0355988000
_diffrn_orient_matrix_UB_22      -0.0324674000
_diffrn_orient_matrix_UB_23      -0.0119700000
_diffrn_orient_matrix_UB_31      -0.0970956000
_diffrn_orient_matrix_UB_32      -0.0122489000
_diffrn_orient_matrix_UB_33      -0.0049888000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_sigmaI/netI    0.1182
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20880
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         4.175
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99225
_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    1.798
_exptl_crystal_description       rod
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         7501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0348P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4672
_reflns_number_total             7501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03937f2.cif
_cod_data_source_block           nx281
_cod_database_code               7058938
_shelx_estimated_absorpt_t_min   0.807
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2013-4
_shelx_res_checksum              64465