An Unprecedented Fe36 Phosphonate Cage
Christine M. Beavers; Andrey V. Prosverin; John D. Cashion; Kim R. Dunbar; Anne F. Richards; Inorganic Chemistry 52 (2013) 1670–1672; doi:10.1021/ic3020145

data_4333808
_publ_contact_author_address
;Advanced Light Source
Lawrence Berkeley National Lab
One Cyclotron Rd
MS 7-222
Berkeley, CA 94720
;
_publ_contact_author_email       cmbeavers@lbl.gov
_publ_contact_author_name        'Christine M. Beavers'
_publ_contact_author_phone       (510)495-2448
_publ_section_title
;
 An Unprecedented Fe36 Phosphonate Cage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1670
_journal_page_last               1672
_journal_paper_doi               10.1021/ic3020145
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
;
C220 H272 Fe36 N44 O180 P44,6(OH),2.1(ClO4), 11.9(NO3), 47.9(H2O),10(C2 H6 O) 
;
_chemical_formula_sum            'C240 H385.8 Cl2.1 Fe36 N55.9 O264 P44'
_chemical_formula_weight         11726.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.999(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   43.6079(17)
_cell_length_b                   28.7572(10)
_cell_length_c                   50.5916(19)
_cell_measurement_reflns_used    9687
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      2.35
_cell_volume                     54383(4)
_computing_cell_refinement       'SAINT V7.60A (Bruker, 2009)'
_computing_data_collection       'Apex2 v2010.3 (Bruker, 2010)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
SHELXTL 5.1, XP (Sheldrick, 1994), 
WinCoot, (P.Emsley, B.Lohkamp W.G.Scott and K.Cowtand, 2010)
;
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.03320
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            150226
_diffrn_reflns_theta_full        26.69
_diffrn_reflns_theta_max         26.69
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    3.229
_exptl_absorpt_correction_T_max  0.9532
_exptl_absorpt_correction_T_min  0.6261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       plate
_exptl_crystal_F_000             23843
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.218
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.750
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1715
_refine_ls_number_reflns         18689
_refine_ls_number_restraints     15284
_refine_ls_restrained_S_all      3.859
_refine_ls_R_factor_all          0.2414
_refine_ls_R_factor_gt           0.1927
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4821
_refine_ls_wR_factor_ref         0.5115
_reflns_number_gt                12593
_reflns_number_total             18689
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic3020145_si_002_1.cif
_cod_data_source_block           1a
_cod_original_cell_volume        54383(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C240 H385.80 Cl2.10 Fe36 N55.90 O264 P44'
_cod_database_code               4333808