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_1501647
_publ_section_title
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 Synthesis, molecular and electronic structure of an incomplete cuboidal
 Re3S4 cluster with an unusual quadruplet ground state
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_journal_name_full               'Che. Commun.'
_journal_page_first              2713
_journal_paper_doi               10.1039/c2cc17287a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C84 H81 Br4 N3 P6 Re3 S4'
_chemical_formula_weight         2324.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.4630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   44.6606(12)
_cell_length_b                   13.7072(4)
_cell_length_c                   29.2555(8)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      31.5933
_cell_measurement_theta_min      2.3514
_cell_volume                     17714.4(9)
_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 0.995
_diffrn_measured_fraction_theta_max 0.885
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54964
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.62
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.140
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.647042
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9000
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         3.921
_refine_diff_density_min         -2.058
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         26356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+204.4582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                21811
_reflns_number_total             26356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc17287a.txt
_cod_data_source_block           1Br*3MeCN
_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 
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_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1501647