Stereochemistry of electrophilic attack at 34e^-^ dimetallic complexes: the case of diiron dithiolato carbonyls + MeS^+^
Olsen, Matthew T.; Gray, Danielle L.; Rauchfuss, Thomas B.; Gioia, Luca De; Zampella, Giuseppe; Chemical Communications (Cambridge, United Kingdom) 47 (2011) 6554–6556; doi:10.1039/c1cc10858a

data_7112694
_publ_section_title
;
 Stereochemistry of electrophilic attack at 34e^-^ dimetallic
 complexes: the case of diiron dithiolato carbonyls + MeS^+^
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   23
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              6554
_journal_page_last               6556
_journal_paper_doi               10.1039/c1cc10858a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C95 H84 B2 Cl6 F48 Fe4 O8 P4 S6'
_chemical_formula_weight         3039.58
_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                105.661(5)
_cell_angle_beta                 91.642(5)
_cell_angle_gamma                99.204(5)
_cell_formula_units_Z            2
_cell_length_a                   17.3263(15)
_cell_length_b                   18.5078(16)
_cell_length_c                   20.1683(18)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      2.47
_cell_volume                     6129.5(9)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
;
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5
(Bruker, 2005 & 2007)
;
_computing_molecular_graphics
;
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994)
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  sba26masq
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            146429
_diffrn_reflns_theta_full        25.43
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.9322
_exptl_absorpt_correction_T_min  0.6684
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3044
_exptl_crystal_id                sba26masq
_exptl_crystal_preparation
;
The data crystal was mounted using ??oil (Parantone-N, Exxon) to a
??0.3 mm cryo-loop (Hampton Research)??
??0.2 mm Kapton micromount (Thorne, 2003)??
with the (??) scattering
planes roughly normal to the spindle axis.
;
_exptl_crystal_size_max          0.639
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
The solvent accessible voids contained 3 highly disordered dichloromethane
molecuels each. Their positions were poorly determined so they were squeezed ou
The void electron count removed is consistent with 2.5 DCM/void.
;
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1960
_refine_ls_number_reflns         22515
_refine_ls_number_restraints     5458
_refine_ls_restrained_S_all      1.710
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+2.8775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                16588
_reflns_number_total             22515
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7106491
_cod_data_source_file            c1cc10858a.txt
_cod_data_source_block           o
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 
;
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7112694