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_4333809
_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),30(H2O),2(C2 H6 O),14(C F3 O3 S)
;
_chemical_formula_sum            'C238 H434 F42 Fe36 N44 O302 P44 S14'
_chemical_formula_weight         13364.2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
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_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   28.6989(3)
_cell_length_b                   28.6989(3)
_cell_length_c                   132.1838(12)
_cell_measurement_reflns_used    39448
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.49
_cell_measurement_theta_min      3.08
_cell_volume                     94284.3(16)
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.2273
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       117
_diffrn_reflns_limit_l_min       -106
_diffrn_reflns_number            106988
_diffrn_reflns_theta_full        43.50
_diffrn_reflns_theta_max         43.50
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    8.847
_exptl_absorpt_correction_T_max  0.8429
_exptl_absorpt_correction_T_min  0.7772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             40680
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.586
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         7830
_refine_ls_number_restraints     1991
_refine_ls_restrained_S_all      2.123
_refine_ls_R_factor_all          0.1698
_refine_ls_R_factor_gt           0.1480
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4356
_refine_ls_wR_factor_ref         0.4606
_reflns_number_gt                6237
_reflns_number_total             7830
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic3020145_si_002_2.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4333809