A facile preparation of two new isostructural metal-organochalcogen clusters from simple starting materials: Sonochemical synthesis, X-ray structures and spectroscopic remarks
Maisy I.P.R. Modestoa; Simone Finotoa; Gleison Antonio Casagrandea; Cristiano Raminellib; Ernesto Schulz Langc; Davi F. Backc; Samuel Leite Oliveirad; Marco Antonio U. Martines; Inorganica Chimica Acta 392 (2012) 103–107; doi:10.1016/j.ica.2012.05.032

data_1512462
_publ_section_title
;
 A facile preparation of two new isostructural metal-organochalcogen
 clusters from simple starting materials: Sonochemical synthesis, X-ray
 structures and spectroscopic remarks
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              103
_journal_page_last               107
_journal_paper_doi               10.1016/j.ica.2012.05.032
_journal_volume                  392
_journal_year                    2012
_chemical_formula_moiety         'C87 H75 Hg8 I2 N3 S Te12'
_chemical_formula_sum            'C87 H75 Hg8 I2 N3 S Te12'
_chemical_formula_weight         4584.28
_chemical_name_common            'cluster of mercury and tellurium'
_chemical_name_systematic
;
        Diphenyl ditelluride iodide mercury (II) complex . pyridine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2011-01-31T14:39:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 113.487(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.0591(15)
_cell_length_b                   13.9742(6)
_cell_length_c                   27.4368(13)
_cell_measurement_reflns_used    9633
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.3645
_cell_measurement_theta_min      2.432
_cell_volume                     10570.0(9)
_computing_cell_refinement       'BRUKER SANT'
_computing_data_collection       'BRUKER APEX-II'
_computing_data_reduction        'BRUKER SOFTWARE'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'X8 APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1414
_diffrn_reflns_av_unetI/netI     0.1726
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            89688
_diffrn_reflns_theta_full        26.1
_diffrn_reflns_theta_max         26.1
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    15.463
_exptl_absorpt_correction_T_max  0.4616
_exptl_absorpt_correction_T_min  0.3361
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8016
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       0.000019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         20880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1869
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                9320
_reflns_number_total             20880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-103-107-1.cif
_cod_data_source_block           teste1
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1512462