Cleavage of P–S bonds and oxygenation by a trinuclear iron carboxylate: Synthesis and structures of iron clusters containing group 15/16 anions
Mitkina, Tatiana V.; Lan, Yanhua; Mereacre, Valeriu; Shi, Weifeng; Powell, Annie K.; Rothenberger, Alexander; Dalton Transactions  (2008) 1136–1139; doi:10.1039/b717583c

data_7003621
_publ_section_title
;
 Cleavage of P--S bonds and oxygenation by a trinuclear iron
 carboxylate: Synthesis and structures of iron clusters containing
 group 15/16 anions
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1136
_journal_page_last               1139
_journal_paper_doi               10.1039/b717583c
_journal_year                    2008
_chemical_formula_sum            'C90 H148 Fe9 O44 P3'
_chemical_formula_weight         2529.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.34(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.606(3)
_cell_length_b                   28.593(6)
_cell_length_c                   26.961(5)
_cell_measurement_reflns_used    27678
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      52.59
_cell_measurement_theta_min      2.80
_cell_volume                     12030(4)
_computing_cell_refinement       'stoe x-area'
_computing_data_collection       'stoe x-area'
_computing_data_reduction        'stoe x-area'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'stoe ipds 2'
_diffrn_measurement_method       rotation
_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  0.1115
_diffrn_reflns_av_sigmaI/netI    0.1619
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            69741
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.22
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5276
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1309
_refine_ls_number_reflns         26260
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.1874
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.2093
_reflns_number_gt                10098
_reflns_number_total             26260
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717583c.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7003621