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_1512463
_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 Br2 Hg8 N3 S Te12'
_chemical_formula_sum            'C87 H75 Br2 Hg8 N3 S Te12'
_chemical_formula_weight         4490.3
_chemical_name_systematic
;
 Chalcogenide Mercury Cluster
;
_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      2.4
_audit_creation_date             2011-03-30T04:09:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.1280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.5202(2)
_cell_length_b                   13.95040(10)
_cell_length_c                   27.2233(2)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.43
_cell_volume                     10385.31(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            94293
_diffrn_reflns_theta_full        27.15
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    15.913
_exptl_absorpt_correction_T_max  0.7853
_exptl_absorpt_correction_T_min  0.6579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7872
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.161
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       0.0000032(13)
_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   1.1
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         22965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0125P)^2^+77.3358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                15310
_reflns_number_total             22965
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2012-392-103-107-2.cif
_cod_data_source_block           teste1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        10385.30(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1512463