Synthesis, molecular and electronic structure of an incomplete cuboidal Re3S4 cluster with an unusual quadruplet ground state
Sergey Konchenko; Rosa Llusar; Pavel Petrov; Aleksandr Virovets; Artem Bogomyakov; Carlos Gomez Garcia; Victor Polo; Che. Commun. 48 (2012) 2713–; doi:10.1039/c2cc17287a

data_1501648
_publ_section_title
;
 Synthesis, molecular and electronic structure of an incomplete cuboidal
 Re3S4 cluster with an unusual quadruplet ground state
;
_journal_name_full               'Che. Commun.'
_journal_page_first              2713
_journal_paper_doi               10.1039/c2cc17287a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C82.5 H81 Br2.6 Cl10.4 P6 Re3 S4'
_chemical_formula_weight         2521.58
_chemical_name_systematic
;
?
;
_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                80.5320(10)
_cell_angle_beta                 72.6390(10)
_cell_angle_gamma                83.4320(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6395(3)
_cell_length_b                   15.3991(3)
_cell_length_c                   22.8431(5)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.6227
_cell_measurement_theta_min      2.4379
_cell_volume                     4506.04(17)
_computing_cell_refinement       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_collection       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction        'Apex2 V.1.27 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.771
_diffrn_measurement_device_type  'Bruker X8Apex CCD detector'
_diffrn_measurement_method       'combined omega- and phi-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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            47320
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.57
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.723
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.779722
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2446
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.747
_refine_diff_density_min         -3.012
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1032
_refine_ls_number_reflns         23261
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0401P)^2^+61.1813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1290
_reflns_number_gt                17767
_reflns_number_total             23261
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc17287a.txt
_cod_data_source_block           2Br*4.5CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C82.50 H81 Br2.60 Cl10.40 P6 Re3 S4'
_cod_database_code               1501648