Cocrystallization of Photosensitive Energetic Copper(II) Perchlorate Complexes with the Nitrogen-rich Ligand 1,2-Di(1H-tetrazol-5-yl)ethane.
Evers, Jürgen; Gospodinov, Ivan; Joas, Manuel; Klapötke, Thomas M; Stierstorfer, Jörg; Inorganic chemistry 53 (2014) 11749–11756; doi:10.1021/ic5020175

data_4341303
_publ_section_title
;
 Cocrystallization of Photosensitive Energetic Copper(II) Perchlorate
 Complexes with the Nitrogen-rich Ligand 1,2-Di(1H-tetrazol-5-yl)ethane.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11749
_journal_page_last               11756
_journal_paper_doi               10.1021/ic5020175
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C8 H16 Cu N16 O2, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C8 H20 Cl2 Cu N16 O12'
_chemical_formula_weight         666.84
_chemical_name_common
'[Cu(dt-5-e)~2~(H~2~O)~2~](ClO~4~)~2~ * 2 H~2~O'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Fri Jun 27 13:50:58 2014'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.72730(10)
_cell_length_b                   21.9914(4)
_cell_length_c                   15.9205(3)
_cell_measurement_reflns_used    15858
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.3620
_cell_measurement_theta_min      4.3670
_cell_volume                     2355.32(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33668
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.26
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.263
_refine_diff_density_max         3.800
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.403(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4785
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+1.8242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                4627
_reflns_number_total             4785
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5020175_si_002.cif
_cod_data_source_block           ix252
_cod_depositor_comments
'Adding full bibliography for 4341302--4341305.cif.'
_cod_database_code               4341303