Low temperature activation of S8, Sered and α-Te with [Cp(BIG)Fe(CO)2] radicals.
Heinl, S.; Scheer, M.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16139–16142; doi:10.1039/c4dt01764a

data_7031724
_publ_section_title
;
 Low temperature activation of S8, Sered and \a-Te with [Cp(BIG)Fe(CO)2]
 radicals.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16139
_journal_page_last               16142
_journal_paper_doi               10.1039/c4dt01764a
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'see text'
_chemical_formula_moiety
'C110 H130 Fe2 Se4, 2(C H2 Cl2), 0.75(C2 H3 N)'
_chemical_formula_sum            'C113.5 H136.25 Cl4 Fe2 N0.75 Se4'
_chemical_formula_weight         2080.43
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                90.382(1)
_cell_angle_beta                 92.790(1)
_cell_angle_gamma                112.446(2)
_cell_formula_units_Z            4
_cell_length_a                   22.1190(4)
_cell_length_b                   22.2233(5)
_cell_length_c                   23.0616(3)
_cell_measurement_reflns_used    26843
_cell_measurement_temperature    128(7)
_cell_measurement_theta_max      70.7490
_cell_measurement_theta_min      3.5250
_cell_volume                     10460.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.12a (release 12-09-2013 CrysAlis171 .NET)
(compiled Sep 12 2013,13:51:24)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.12a (release 12-09-2013 CrysAlis171 .NET)
(compiled Sep 12 2013,13:51:24)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.12a (release 12-09-2013 CrysAlis171 .NET)
(compiled Sep 12 2013,13:51:24)
;
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      128(7)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'SuperNova,Single source at offset,Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38150
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        70.82
_diffrn_reflns_theta_max         70.82
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    5.090
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.12a (release 12-09-2013 CrysAlis171 .NET)
(compiled Sep 12 2013,13:51:24)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.1860
_exptl_crystal_size_mid          0.1328
_exptl_crystal_size_min          0.0875
_platon_squeeze_details
;
With the aid of PLATON three solvent accessible area was found, but it was
impossible to refine any reasonable molecules from difference Fourier peaks.
Therefore the midpoints, the sizes and the numbers of electrons in the voids
were refined and the contribution to the calculated structure factors of
the disordered solvent is taken into account by back-Fourier transformation
with the program SQUEEZE (Sluis and Spek, 1990). The voids are found around 
(0.365  0.335  0.910), (0.500  0.000  0.000) and (0.635  0.665  0.089) 
the sizes are 91, 117 and 91 \%A^3^, 
and 23, 30 and 23 e^-^ respectively were detected.(Whole Cell)
This electron number corresponds roughly to three acetonitrile molecules.
;
_refine_diff_density_max         1.614
_refine_diff_density_min         -1.528
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2350
_refine_ls_number_reflns         38150
_refine_ls_number_restraints     339
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0569
_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^)+(0.1140P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1683
_reflns_number_gt                27797
_reflns_number_total             38150
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c4dt01764a2.cif
_cod_data_source_block           6b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031718--7031724.cif.
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_cod_database_code               7031724