Dinuclear lanthanoid(III) dithiocarbamato complexes bridged by (E)-N-benzylidenepicolinohydrazonate: Syntheses, crystal structures and spectroscopic properties
Yakubu, Abdallah; Suzuki, Takayoshi; Kita, Masakazu; Inorganica Chimica Acta 498 (2019) 119124–; doi:10.1016/j.ica.2019.119124

data_1565742
_publ_section_title
;
 Dinuclear lanthanoid(III) dithiocarbamato complexes bridged by
 (E)-N-benzylidenepicolinohydrazonate: Syntheses, crystal structures and
 spectroscopic properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119124
_journal_paper_doi               10.1016/j.ica.2019.119124
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C40 H48 Cl4 N10 O2 Pr2 S8'
_chemical_formula_sum            'C40 H48 Cl4 N10 O2 Pr2 S8'
_chemical_formula_weight         1380.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                74.5353(18)
_cell_angle_beta                 72.3561(15)
_cell_angle_gamma                73.3711(19)
_cell_formula_units_Z            4
_cell_length_a                   16.3680(7)
_cell_length_b                   18.5418(9)
_cell_length_c                   19.8671(9)
_cell_measurement_reflns_used    19333
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.02
_cell_volume                     5397.7(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      188(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53851
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.018
_exptl_absorpt_coefficient_mu    2.336
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         4.216
_refine_diff_density_min         -1.893
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1189
_refine_ls_number_reflns         24643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1024P)^2^+1.4802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.2270
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9656
_reflns_number_total             24643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2a_Pr_Me2dtc_bphz.cif
_cod_data_source_block           '[Pr2(Me2dtc)4(bphz)2]'
_cod_database_code               1565742
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.652
_shelx_estimated_absorpt_t_max   0.800