Synthesis, crystal structure and polymorphism of a μ-oxo bridged binuclear iron(III) complex of 2,2′∶ 6′,2″∶6″,2‴-quaterpyridine
Calderazzo, Fausto; Labella, Luca; Marchetti, Fabio; Journal of the Chemical Society, Dalton Transactions  (1998) 1485–; doi:10.1039/a707623a

data_7027832
_publ_section_title
;
 Synthesis, crystal structure and polymorphism of a \m-oxo bridged
 binuclear iron(III) complex of 2,2&#x2032;&#x2236;
 6&#x2032;,2&#x2033;&#x2236;6&#x2033;,2&#x2034;-quaterpyridine
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_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1485
_journal_paper_doi               10.1039/a707623a
_journal_year                    1998
_chemical_formula_moiety         '[(Fe(C20H14N4)(H2O))2(\m-O)](ClO4)4.2H2O'
_chemical_formula_sum            'C40 H36 Cl4 Fe2 N8 O21'
_chemical_formula_weight         1218.27
_chemical_name_systematic
; 
bis-2,2':6',2'':6'',2''-quaterpyridine-bis-aquo-\m-oxo-diiron(III)
perchlorate dihydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.175(2)
_cell_length_b                   16.4630(10)
_cell_length_c                   20.949(3)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.28
_cell_measurement_theta_min      5.00
_cell_volume                     4888.7(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3995
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        2.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.8346
_exptl_absorpt_correction_T_min  0.8078
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            ruby-red
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       prism
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          '0.44 mm'
_exptl_crystal_size_mid          '0.32 mm'
_exptl_crystal_size_min          '0.12 mm'
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_goodness_of_fit_obs   1.120
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.1770
_refine_ls_R_factor_obs          0.1069
_refine_ls_shift/esd_max         -0.012
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2489P)^2^+4.9688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3759
_refine_ls_wR_factor_obs         0.2976
_reflns_number_observed          1673
_reflns_number_total             3189
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a707623sup1.cif
_cod_data_source_block           1O-RT
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2489P)^2^+4.9688P] 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^)+(0.2489P)^2^+4.9688P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'Pbca '
_cod_database_code               7027832