Synthesis, Structural and Magnetochemical Studies of Iron Phosphonate Cages Based on {Fe3O}7+ Core
Khanra, Sumit; Konar, Sanjit; Clearfield, Abraham; Helliwell, Madeleine; McInnes, Eric J. L.; Tolis, Evangelos; Tuna, Floriana; Winpenny, Richard E. P.; Inorganic Chemistry 48 (2009) 5338–5349; doi:10.1021/ic9003214

data_4338600
_publ_section_title
;
 Synthesis, Structural and Magnetochemical Studies of Iron Phosphonate
 Cages Based on {Fe3O}7+ Core
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5338
_journal_page_last               5349
_journal_paper_doi               10.1021/ic9003214
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C97 H148.5 Fe9 N5.5 O46.5 P6'
_chemical_formula_weight         2824.18
_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                 98.365(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7176(6)
_cell_length_b                   31.6232(12)
_cell_length_c                   27.2512(12)
_cell_measurement_temperature    100(2)
_cell_volume                     13400.9(9)
_computing_cell_refinement
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) 
(compiled Apr 27 2007,17:53:11) 
;
_computing_data_collection
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) 
(compiled Apr 27 2007,17:53:11) 
;
_computing_data_reduction
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) 
(compiled Apr 27 2007,17:53:11) 
;
_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      100(2)
_diffrn_measured_fraction_theta_full 0.807
_diffrn_measured_fraction_theta_max 0.807
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_sigmaI/netI    0.1560
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52533
_diffrn_reflns_theta_full        23.71
_diffrn_reflns_theta_max         23.71
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             5860
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1447
_refine_ls_number_reflns         16421
_refine_ls_number_restraints     680
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1670
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+91.7263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.2451
_reflns_number_gt                8167
_reflns_number_total             16421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9003214_si_001.cif
_cod_data_source_block           testorepw790
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C97 H148.50 Fe9 N5.50 O46.50 P6'
_cod_database_code               4338600