Novel Rectangular [Fe4(μ4-OHO)(μ-OH)2]7+ versus "Butterfly" [Fe4(μ3-O)2]8+ Core Topology in the FeIII/RCO2-/phen Reaction Systems (R = Me, Ph; phen = 1,10-Phenanthroline): Preparation and Properties of [Fe4(OHO)(OH)2(O2CMe)4(phen)4](ClO4)3, [Fe4O2(O2CPh)7(phen)2](ClO4), and [Fe4O2(O2CPh)8(phen)2]
Athanassios K. Boudalis; Nikolia Lalioti; Georgios A. Spyroulias; Catherine P. Raptopoulou; Aris Terzis; Azzedine Bousseksou; Vassilis Tangoulis; Jean-Pierre Tuchagues; Spyros P. Perlepes; Inorganic Chemistry 41 (2002) 6474–6487; doi:10.1021/ic025795k

data_4318948
_publ_section_title
;
 Novel Rectangular [Fe4(\m4-OHO)(\m-OH)2]7+ versus "Butterfly"
 [Fe4(\m3-O)2]8+ Core Topology in the FeIII/RCO2-/phen Reaction Systems (R
 = Me, Ph; phen = 1,10-Phenanthroline): Preparation and Properties of
 [Fe4(OHO)(OH)2(O2CMe)4(phen)4](ClO4)3, [Fe4O2(O2CPh)7(phen)2](ClO4), and
 [Fe4O2(O2CPh)8(phen)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6474
_journal_page_last               6487
_journal_paper_doi               10.1021/ic025795k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C77 H57 Cl Fe4 N6 O20'
_chemical_formula_weight         1645.14
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.416(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.532(2)
_cell_length_b                   35.908(3)
_cell_length_c                   11.591(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      27
_cell_measurement_theta_min      12
_cell_volume                     7664.9(12)
_computing_cell_refinement
;
Program LEAST (UCLA Crystallographic package, C.E.Strouse 1994)
;
_computing_data_collection
;
Program COLLECT (UCLA Crystallographic package, C.E.Strouse 1994)
;
_computing_data_reduction
;
Program REDUCE (UCLA Crystallographic package, C.E.Strouse 1994)
;
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
;
P21 Nicolet diffractometer upgraded by Crystal Logic
;
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7860
_diffrn_reflns_theta_max         48.74
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        -1.8
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.905
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            'green-red dichroic'
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      1.40
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.090
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         7370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_obs          0.0737
_refine_ls_shift/esd_max         0.029
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+32.2473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2174
_refine_ls_wR_factor_obs         0.1897
_reflns_number_observed          5328
_reflns_number_total             7370
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic025795k-2_s2_1.cif
_cod_data_source_block           COMPOUND2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+32.2473P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+32.2473P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7665(1)
_cod_database_code               4318948