An unusually water-poor 5,5′-azobistetrazolate of dysprosium: stabilization of a nitrogen-rich heterocycle by a minimum of hydrogen bonds
Knoll, Christian; Müller, Danny; Giester, Gerald; Ofner, Johannes; Lendl, Bernhard; Weinberger, Peter; Steinhauser, Georg; New Journal of Chemistry 37 (2013) 3840–; doi:10.1039/c3nj00492a

data_7053238
_publ_section_title
;
 An unusually water-poor 5,5&#x2032;-azobistetrazolate of dysprosium:
 stabilization of a nitrogen-rich heterocycle by a minimum of hydrogen
 bonds
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3840
_journal_paper_doi               10.1039/c3nj00492a
_journal_volume                  37
_journal_year                    2013
_chemical_formula_sum            'C6 H32 Dy2 N30 O16'
_chemical_formula_weight         1105.62
_chemical_name_common            'octaaquadysprosium 5,5'-azobis[tetrazolide]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.060(10)
_cell_angle_beta                 80.190(10)
_cell_angle_gamma                67.970(10)
_cell_formula_units_Z            1
_cell_length_a                   8.0770(10)
_cell_length_b                   9.4350(10)
_cell_length_c                   12.681(2)
_cell_measurement_temperature    200(2)
_cell_volume                     841.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14171
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    4.517
_exptl_absorpt_correction_T_max  0.323
_exptl_absorpt_correction_T_min  0.281
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow-brownish
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         7322
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+0.2567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0431
_reflns_number_gt                6637
_reflns_number_total             7322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00492a.txt
_cod_data_source_block           ck070a
_cod_original_cell_volume        841.11(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7053238