Oxo-, Hydroxo-, and Peroxo-Bridged Fe(III) Phosphonate Cages
Sanjit Konar; Nattamai Bhuvanesh; Abraham Clearfield; Journal of the American Chemical Society 128 (2006) 9604–9605; doi:10.1021/ja063388s

data_4110791
_publ_section_title
;
 Oxo-, Hydroxo-, and Peroxo-Bridged Fe(III) Phosphonate Cages
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9604
_journal_page_last               9605
_journal_paper_doi               10.1021/ja063388s
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C65.1 H113.65 Fe6 N2.55 O28 P2'
_chemical_formula_weight         1777.18
_chemical_name_systematic
; 
 ? 
;
_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                 100.269(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0253(18)
_cell_length_b                   23.845(3)
_cell_length_c                   24.665(3)
_cell_measurement_reflns_used    6697
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      2.39
_cell_volume                     9274.1(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55939
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      0
_exptl_crystal_description       cubic
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.391
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         20794
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          1.677
_refine_ls_shift/su_mean         0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1802P)^2^+13.3505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2344
_refine_ls_wR_factor_ref         0.2968
_reflns_number_gt                12242
_reflns_number_total             20794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063388ssi20060519_110612.cif
_cod_data_source_block           3
_cod_original_cell_volume        9274.1(18)
_cod_original_formula_sum        'C65.10 H113.65 Fe6 N2.55 O28 P2'
_cod_database_code               4110791