Use of the di-2-pyridyl ketone/3,5-di-tert-butylcatechol “blend” in iron(III) chemistry: a cationic tetranuclear cluster and an anionic trinuclear complex
Athanassios K. Boudalis; Françoise Dahan; Azzedine Bousseksou; Jean-Pierre Tuchagues; Spyros P. Perlepes; Dalton Trans.  (2003) 3411–3418; doi:10.1039/b305873e

data_7013253
_publ_section_title
;
 Use of the di-2-pyridyl ketone/3,5-di-tert-butylcatechol
 &#x201C;blend&#x201D; in iron(III) chemistry: a cationic tetranuclear
 cluster and an anionic trinuclear complex
;
_journal_issue                   17
_journal_name_full               'Dalton Trans.'
_journal_page_first              3411
_journal_page_last               3418
_journal_paper_doi               10.1039/b305873e
_journal_year                    2003
_chemical_formula_sum            'C86 H117 Fe3 N6 O12'
_chemical_formula_weight         1594.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 112.586(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.495(2)
_cell_length_b                   18.6521(13)
_cell_length_c                   23.326(3)
_cell_measurement_temperature    160(2)
_cell_volume                     8634.8(17)
_computing_cell_refinement       'STOE-IPDS software (Stoe, 2.93, 1997)'
_computing_data_collection       'STOE-IPDS software (Stoe, 2.93, 1997)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Imaging Plate Detector System'
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67360
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Dark-Red
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             3396
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         17043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                10336
_reflns_number_total             17043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305873e.txt
_cod_data_source_block           (2)
_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.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.0000P] 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^)+(0.0615P)^2^+0.0000P] 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        8634.8(16)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7013253