Stabilization of 3:1 Site-Differentiated Cubane-Type Clusters in the [Fe4S4]1+ Core Oxidation State by Tertiary Phosphine Ligation: Synthesis, Core Structural Diversity, and S= 1/2 Ground States
Liang Deng; Amit Majumdar; Wayne Lo; R. H. Holm; Inorganic Chemistry 49 (2010) 11118–11126; doi:10.1021/ic101702b

data_4317187
_publ_contact_author_address
;Departemnt of Chemistry and Chemical Biology
12 Oxford Street
Cambridge, MA 02138
United States of America
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_name        'Prof. Richard H. Holm'
_publ_section_title
;
 Stabilization of 3:1 Site-Differentiated Cubane-Type Clusters in the
 [Fe4S4]1+ Core Oxidation State by Tertiary Phosphine Ligation: Synthesis,
 Core Structural Diversity, and S= 1/2 Ground States
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11118
_journal_page_last               11126
_journal_paper_doi               10.1021/ic101702b
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C27 H63 Br Fe4 P3 S4'
_chemical_formula_sum            'C27 H63 Br Fe4 P3 S4'
_chemical_formula_weight         912.26
_chemical_name_systematic
; 
 ? 
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.874(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5180(5)
_cell_length_b                   13.3790(4)
_cell_length_c                   18.8744(6)
_cell_measurement_reflns_used    22947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.967
_cell_measurement_theta_min      2.205
_cell_volume                     3881.7(2)
_computing_cell_refinement       'Bruker Saint v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX SMART (Bruker, 2009)'
_computing_data_reduction        'Bruker Saint v7.23A (Bruker, 2005)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            83523
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.6913
_exptl_absorpt_correction_T_min  0.4272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            Black-brown
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0369P)^2^+8.8746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                6180
_reflns_number_total             7607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101702b_si_001_08.cif
_cod_data_source_block           '[Fe4S4(PPri3)3(Br)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4317187