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_7027830
_publ_contact_author
;
        Fausto Calderazzo
        Dipartimento di Chimica e Chimica Industriale
        Universita' di Pisa
        Via Risorgimento, 35
        56126 Pisa
        Italy
;
_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                 105.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.080(3)
_cell_length_b                   14.045(3)
_cell_length_c                   13.778(3)
_cell_measurement_reflns_used    17
_cell_measurement_temperature    296
_cell_measurement_theta_max      10.1
_cell_measurement_theta_min      8.4
_cell_volume                     2438.8(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3472
_diffrn_reflns_theta_max         21.25
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        4.07
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.6546
_exptl_absorpt_correction_T_min  0.6136
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            ruby-red
_exptl_crystal_density_diffrn    1.659
_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         1.683
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.120
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         2702
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_obs          0.0868
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1440P)^2^+14.0219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2740
_refine_ls_wR_factor_obs         0.2260
_reflns_number_observed          1711
_reflns_number_total             2703
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a707623sup1.cif
_cod_data_source_block           1M-RT
_cod_depositor_comments
;
The following automatic conversions were performed:
'_publ_contact_autor' tag replaced with '_publ_contact_author'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_cell_measurement_temperature' value '296 K' was changed to '296' -
the value should be numeric and without a unit
designator.

'_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^)+(0.1440P)^2^+14.0219P] 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^)+(0.1440P)^2^+14.0219P] 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        2438.8(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027830