Bis[2,6-bis(1<i>H</i>-pyrazol-1-yl)pyridine]decakis(μ~2~-3-nitrobenzoato)bis(3-nitrobenzoato)tetradysprosium(III): a linear tetranuclear dysprosium compound based on mixed N- and O-donor ligands
Hua, Rong; Wu, Xiao-Liu; Li, Jin-Ying; Acta Crystallographica Section E 70 (2014) m162–m163; doi:10.1107/S1600536814006060

data_2239294
_publ_section_title
;
 Bis[2,6-bis(1<i>H</i>-pyrazol-1-yl)pyridine]decakis(\m~2~-3-nitrobenzoato)bis(3-nitrobenzoato)tetradysprosium(III):
 a linear tetranuclear dysprosium compound based on mixed N- and O-donor
 ligands
;
_journal_coeditor_code           SU2704
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m162
_journal_page_last               m163
_journal_paper_doi               10.1107/S1600536814006060
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Dy4 (C7 H4 N O4)12 (C11 H9 N5)2]'
_chemical_formula_moiety         'C106 H66 Dy4 N22 O48'
_chemical_formula_sum            'C106 H66 Dy4 N22 O48'
_chemical_formula_weight         3065.81
_chemical_name_systematic
Bis[2,6-bis(1<i>H</i>-pyrazol-1-yl)pyridine]decakis(\m~2~-3-nitrobenzoato)bis(3-nitrobenzoato)tetradysprosium(III)
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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                100.443(2)
_cell_angle_beta                 111.7540(10)
_cell_angle_gamma                99.695(2)
_cell_formula_units_Z            1
_cell_length_a                   14.2514(3)
_cell_length_b                   14.9274(5)
_cell_length_c                   14.9616(3)
_cell_measurement_reflns_used    9289
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      2.56
_cell_volume                     2808.88(13)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX2 CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42971
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    2.736
_exptl_absorpt_correction_T_max  0.6244
_exptl_absorpt_correction_T_min  0.6107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.669
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         11020
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0235P)^2^+2.1975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                9747
_reflns_number_total             11020
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su2704sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        2808.87(12)
_cod_database_code               2239294
_cod_database_fobs_code          2239294