High-Nuclearity Mixed-Chelate Ferric Complexes from a New Family of Polynuclear Precursors
Colette Boskovic; Hans U. Güdel; Gaël Labat; Antonia Neels; Wolfgang Wernsdorfer; Boujemaa Moubaraki; Keith S. Murray; Inorganic Chemistry 44 (2005) 3181–3189; doi:10.1021/ic048411u

data_4308813
_publ_contact_author_email       C.BOSKOVIC@UNIMELB.EDU.AU
_publ_contact_author_name        'Colette Boskovic'
_publ_section_title
;
High-Nuclearity Mixed-Chelate Ferric Complexes from a New Family of
Polynuclear Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3181
_journal_page_last               3189
_journal_paper_doi               10.1021/ic048411u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C92 H119 Fe11 N10 O39'
_chemical_formula_weight         2603.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.091(10)
_cell_angle_beta                 112.105(9)
_cell_angle_gamma                103.271(10)
_cell_formula_units_Z            2
_cell_length_a                   17.7648(12)
_cell_length_b                   19.763(2)
_cell_length_c                   20.5964(19)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.15
_cell_volume                     5794.9(13)
_computing_cell_refinement       'CELL (Stoe IPDS Software, 2000)'
_computing_data_collection       'EXPOSE (Stoe IPDS Software, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS Software, 2000)'
_computing_molecular_graphics    'PLATON99 (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_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  0.1058
_diffrn_reflns_av_sigmaI/netI    0.2163
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45911
_diffrn_reflns_theta_full        25.90
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.288
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DIFABS (PLATON99, Spek, 1999)'
_exptl_crystal_colour            dark-orange
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2678
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.712
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1224
_refine_ls_number_reflns         21037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.712
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                8851
_reflns_number_total             21037
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic048411usi20041117_071619_2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5794.7(9)
_cod_database_code               4308813