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_7027831
_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
;
_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           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                 105.360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.912(2)
_cell_length_b                   13.913(4)
_cell_length_c                   13.545(2)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      9.96
_cell_measurement_theta_min      9.62
_cell_volume                     2346.4(8)
_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'
_diffrn_ambient_temperature      153(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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.1217
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5145
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  0.7076
_exptl_absorpt_correction_T_min  0.6871
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            ruby-red
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          '0.31 mm'
_exptl_crystal_size_mid          '0.20 mm'
_exptl_crystal_size_min          '0.14 mm'
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_obs          0.0634
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+2.4163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1436
_refine_ls_wR_factor_obs         0.1166
_reflns_number_observed          2551
_reflns_number_total             4129
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a707623sup1.cif
_cod_data_source_block           1M-LT
_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 2.4.2 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^)+(0.0469P)^2^+2.4163P] 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^)+(0.0469P)^2^+2.4163P] 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      'P2(1)/n  '
_cod_database_code               7027831