Two new soluble iron‒oxo complexes: [Fe~2~(μ-O)(μ-O~2~CCF~3~)~2~(O~2~CCF~3~)~2~(C~10~H~8~N~2~)~2~] and [Fe~4~(μ~3~-O)~2~(μ-O~2~CCF~3~)~6~(O~2~CCF~3~)~2~(C~10~H~8~N~2~)~2~]·CF~3~CO~2~H
Bacsa, John; Zhao, Hanhua; Kim R. Dunbar; Acta Crystallographica Section C 59 (2003) m561–m564; doi:10.1107/S0108270103025691

data_2013575
_publ_section_title
;Two new soluble iron--oxo complexes:
 [Fe~2~(\m-O)(\m-O~2~CCF~3~)~2~(O~2~CCF~3~)~2~(C~10~H~8~N~2~)~2~] and
 [Fe~4~(\m~3~-O)~2~(\m-O~2~CCF~3~)~6~(O~2~CCF~3~)~2~(C~10~H~8~N~2~)~2~]&#x00B7;CF~3~CO~2~H
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m561
_journal_page_last               m564
_journal_paper_doi               10.1107/S0108270103025691
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'[Fe4 O2 (C2 F3 O2)8 (C10 H8 N2)2], C2 H F3 O2'
_chemical_formula_moiety         'C36 H16 F24 Fe4 N4 O18, C2 H F3 O2'
_chemical_formula_sum            'C38 H17 F27 Fe4 N4 O20'
_chemical_formula_weight         1585.96
_chemical_name_systematic
;
bis(2,2'-bipyridine)di-\m~3~-oxo-hexa-\m-trifluoroacetato-
bis(trifluoroacetato)tetrairon(III) trifluoroacetic acid solvate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.733(3)
_cell_length_b                   19.015(4)
_cell_length_c                   22.222(4)
_cell_measurement_reflns_used    2413
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.619
_cell_measurement_theta_min      2.313
_cell_volume                     5378(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT '
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24224
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.93
_diffrn_reflns_theta_min         2.84
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.8027
_exptl_absorpt_correction_T_min  0.6701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.602
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         10470
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+19.8269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                7787
_reflns_number_total             10470
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1034.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_sg_symbol_H-M      'P 21/n'
_cod_database_code               2013575