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_2013574
_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          '[Fe2 O (C2 F3 O2)4 (C10 H8 N2)2]'
_chemical_formula_moiety         'C28 H16 F12 Fe2 N4 O9'
_chemical_formula_sum            'C28 H16 F12 Fe2 N4 O9'
_chemical_formula_weight         892.15
_chemical_name_systematic
;
di-\m-trifluoroacetato-\m~3~-oxo-bis[(2,2'-bipyridine-
\k^2^N,N')(trifluoroacetato-\kO)iron(III)]
;
_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                 98.046(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3902(16)
_cell_length_b                   16.751(3)
_cell_length_c                   18.960(3)
_cell_measurement_reflns_used    1562
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.327
_cell_measurement_theta_min      2.323
_cell_volume                     3267.4(9)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23339
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.9415
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.581
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         6984
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0535P)^2^+2.838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                5087
_reflns_number_total             6984
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1034.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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               2013574