Spin frustration and concealed asymmetry: structure and magnetic spectrum of [Fe3O(O2CPh)6(py)3]ClO4·py †
Sowrey, Frank E.; Tilford, Claire; Wocadlo, Sigrid; Anson, Christopher E.; Powell, Annie K.; Bennington, Stephen M.; Montfrooij, Wouter; Jayasooriya, Upali A.; Cannon, Roderick D.; Journal of the Chemical Society, Dalton Transactions  (2001) 862–; doi:10.1039/b008121n

data_7010325
_publ_section_title
;
 Spin frustration and concealed asymmetry: structure and magnetic
 spectrum of [Fe3O(O2CPh)6(py)3]ClO4&#x00B7;py&#x200A;&#x2020;
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              862
_journal_paper_doi               10.1039/b008121n
_journal_year                    2001
_chemical_formula_sum            'C62 H50 Cl Fe3 N4 O17'
_chemical_formula_weight         1326.06
_chemical_name_systematic
; 
Hexakis(O,O'-\m-benzoate)(\m3-oxo)tris(pyridine)triiron(III)
perchlorate pyridine solvate 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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            2
_cell_length_a                   13.541(3)
_cell_length_b                   13.541(3)
_cell_length_c                   19.136(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      12.34
_cell_measurement_theta_min      10.96
_cell_volume                     3038.7(12)
_computing_cell_refinement       'AFC7R Control Software (MSC, 1994)'
_computing_data_collection       'AFC7R Control Software (MSC, 1994)'
_computing_data_reduction        'TEXSAN 1.6 (MSC, 1996)'
_computing_molecular_graphics    'XP in SHELXTL/PC 5.03 (Siemens, 1995)'
_computing_publication_material  'XCIF in SHELXTL/PC 5.03 (Siemens, 1995)'
_computing_structure_refinement  'XL in SHELXTL/PC 5.03 (Siemens, 1995)'
_computing_structure_solution    'XS in SHELXTL/PC 5.03 (Siemens, 1995)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1687
_diffrn_reflns_theta_full        23.16
_diffrn_reflns_theta_max         23.16
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1477
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                798
_reflns_number_total             1477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008121n.txt
_cod_data_source_block           clair1
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               7010325