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_7058943
_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         '2(C16 H14 Cu N16 O14), H2 O'
_chemical_formula_sum            'C32 H30 Cu2 N32 O29'
_chemical_formula_weight         1453.96
_chemical_name_common
'di(1-amino-5-methyltetrazolyl) dipicrato copper(II) semihydrate'
_chemical_name_systematic
;
di(1-amino-5-methyltetrazolyl) dipicrato copper(II) semihydrate
;
_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   mixed
_audit_creation_date             2018-06-28
_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                 103.280(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5743(8)
_cell_length_b                   15.0908(7)
_cell_length_c                   22.2088(10)
_cell_measurement_reflns_used    3351
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      25.0670
_cell_measurement_theta_min      4.3870
_cell_volume                     5406.3(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -12.00  94.00   1.00   10.00    --   21.39  77.00-180.00  106
  2  \w    -12.00  94.00   1.00   10.00    --   21.39  77.00  60.00  106
  3  \w    -12.00  93.00   1.00   10.00    --   21.39  77.00 -60.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0245185000
_diffrn_orient_matrix_UB_12      0.0073354000
_diffrn_orient_matrix_UB_13      0.0218349000
_diffrn_orient_matrix_UB_21      0.0158851000
_diffrn_orient_matrix_UB_22      0.0437109000
_diffrn_orient_matrix_UB_23      0.0049540000
_diffrn_orient_matrix_UB_31      -0.0328542000
_diffrn_orient_matrix_UB_32      0.0156537000
_diffrn_orient_matrix_UB_33      -0.0239958000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_sigmaI/netI    0.1368
_diffrn_reflns_av_unetI/netI     0.1085
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29193
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         4.159
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94737
_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    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         10570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0382P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6322
_reflns_number_total             10570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03937f2.cif
_cod_data_source_block           nx243
_cod_database_code               7058943
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.860
_shelxl_version_number           2013-4
_shelx_res_checksum              15716