#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:41:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179984 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/78/7027831.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027831
loop_
_publ_author_name
'Calderazzo, Fausto'
'Labella, Luca'
'Marchetti, Fabio'
_publ_section_title
;
 Synthesis, crystal structure and polymorphism of a μ-oxo bridged
 binuclear iron(III) complex of 2,2′∶
 6′,2″∶6″,2‴-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-μ-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       '2θ/ω 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/[σ²(Fo²)+(0.0469P)²+2.4163P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Fe Fe 0.98745(8) 0.37955(7) 0.45501(6) 0.0138(2) Uani 1 d .
O1 O 1.0000 0.5000 0.5000 0.021(2) Uani 1 d S
OW1 O 0.9841(5) 0.2323(4) 0.4714(4) 0.0222(12) Uani 1 d .
HW1A H 0.9329(61) 0.2159(55) 0.4573(55) 0.017(25) Uiso 1 d .
HW1B H 1.0324(95) 0.1887(85) 0.4337(81) 0.109(43) Uiso 1 d .
N1 N 1.1583(4) 0.3572(4) 0.5308(4) 0.0180(13) Uani 1 d .
N2 N 1.0656(4) 0.3718(4) 0.3360(4) 0.0148(11) Uani 1 d .
N3 N 0.8646(4) 0.3890(4) 0.3166(3) 0.0122(11) Uani 1 d .
N4 N 0.8359(4) 0.3734(4) 0.4987(4) 0.0159(12) Uani 1 d .
C1 C 1.1995(6) 0.3579(5) 0.6335(5) 0.022(2) Uani 1 d .
H1 H 1.1534(6) 0.3652(5) 0.6753(5) 0.027 Uiso 1 calc R
C2 C 1.3084(6) 0.3479(5) 0.6781(5) 0.021(2) Uani 1 d .
H2 H 1.3352(6) 0.3489(5) 0.7490(5) 0.025 Uiso 1 calc R
C3 C 1.3768(6) 0.3366(5) 0.6163(5) 0.023(2) Uani 1 d .
H3 H 1.4501(6) 0.3288(5) 0.6451(5) 0.028 Uiso 1 calc R
C4 C 1.3358(5) 0.3370(5) 0.5110(5) 0.0185(15) Uani 1 d .
H4 H 1.3808(5) 0.3292(5) 0.4681(5) 0.022 Uiso 1 calc R
C5 C 1.2252(5) 0.3493(4) 0.4705(5) 0.0177(15) Uani 1 d .
C6 C 1.1724(5) 0.3568(4) 0.3593(5) 0.0169(15) Uani 1 d .
C7 C 1.2251(6) 0.3503(5) 0.2826(5) 0.023(2) Uani 1 d .
H7 H 1.2988(6) 0.3397(5) 0.2986(5) 0.027 Uiso 1 calc R
C8 C 1.1661(6) 0.3598(5) 0.1820(5) 0.026(2) Uani 1 d .
H8 H 1.2003(6) 0.3556(5) 0.1298(5) 0.031 Uiso 1 calc R
C9 C 1.0565(5) 0.3754(5) 0.1582(5) 0.0198(15) Uani 1 d .
H9 H 1.0163(5) 0.3823(5) 0.0906(5) 0.024 Uiso 1 calc R
C10 C 1.0082(5) 0.3806(5) 0.2385(4) 0.0147(13) Uani 1 d .
C11 C 0.8904(5) 0.3921(5) 0.2268(4) 0.0162(14) Uani 1 d .
C12 C 0.8127(5) 0.4021(4) 0.1345(5) 0.0191(15) Uani 1 d .
H12 H 0.8313(5) 0.4063(4) 0.0728(5) 0.023 Uiso 1 calc R
C13 C 0.7065(6) 0.4055(5) 0.1377(5) 0.022(2) Uani 1 d .
H13 H 0.6527(6) 0.4106(5) 0.0768(5) 0.026 Uiso 1 calc R
C14 C 0.6788(5) 0.4015(5) 0.2288(5) 0.0197(15) Uani 1 d .
H14 H 0.6072(5) 0.4033(5) 0.2302(5) 0.024 Uiso 1 calc R
C15 C 0.7611(5) 0.3947(4) 0.3190(4) 0.0152(14) Uani 1 d .
C16 C 0.7459(5) 0.3936(5) 0.4235(5) 0.0160(14) Uani 1 d .
C17 C 0.6506(6) 0.4136(5) 0.4469(5) 0.020(2) Uani 1 d .
H17 H 0.5891(6) 0.4270(5) 0.3949(5) 0.024 Uiso 1 calc R
C18 C 0.6464(6) 0.4135(5) 0.5482(5) 0.022(2) Uani 1 d .
H18 H 0.5829(6) 0.4289(5) 0.5647(5) 0.026 Uiso 1 calc R
C19 C 0.7376(6) 0.3905(5) 0.6241(5) 0.027(2) Uani 1 d .
H19 H 0.7362(6) 0.3886(5) 0.6924(5) 0.033 Uiso 1 calc R
C20 C 0.8310(6) 0.3702(5) 0.5965(5) 0.025(2) Uani 1 d .
H20 H 0.8925(6) 0.3539(5) 0.6472(5) 0.030 Uiso 1 calc R
OW2 O 0.8090(6) 0.1331(4) 0.4502(5) 0.040(2) Uani 1 d .
HW2A H 0.7471(71) 0.1367(63) 0.4365(61) 0.037(28) Uiso 1 d .
HW2B H 0.8314(74) 0.0857(69) 0.4922(66) 0.055(30) Uiso 1 d .
Cl1 Cl 1.09673(13) 0.04716(11) 0.34095(11) 0.0185(4) Uani 1 d .
O2 O 1.0865(5) 0.1502(3) 0.3311(4) 0.0373(14) Uani 1 d .
O3 O 1.0660(4) 0.0041(4) 0.2414(3) 0.0272(12) Uani 1 d .
O4 O 1.0286(5) 0.0131(4) 0.4019(4) 0.045(2) Uani 1 d .
O5 O 1.2050(4) 0.0231(4) 0.3922(4) 0.045(2) Uani 1 d .
Cl2 Cl 0.51199(14) 0.17285(12) 0.36028(12) 0.0228(4) Uani 1 d .
O6 O 0.6014(4) 0.1920(4) 0.4482(3) 0.0334(13) Uani 1 d .
O7 O 0.5439(4) 0.1046(4) 0.2942(3) 0.0351(13) Uani 1 d .
O8 O 0.4244(5) 0.1338(5) 0.3958(4) 0.056(2) Uani 1 d .
O9 O 0.4787(5) 0.2602(4) 0.3047(4) 0.044(2) Uani 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
O1 Fe OW1 154.6(2) .
O1 Fe N3 102.98(15) .
OW1 Fe N3 97.1(2) .
O1 Fe N2 106.91(15) .
OW1 Fe N2 93.4(2) .
N3 Fe N2 74.0(2) .
O1 Fe N4 87.19(14) .
OW1 Fe N4 83.5(2) .
N3 Fe N4 74.2(2) .
N2 Fe N4 147.4(2) .
O1 Fe N1 89.07(14) .
OW1 Fe N1 81.8(2) .
N3 Fe N1 148.0(2) .
N2 Fe N1 74.1(2) .
N4 Fe N1 136.6(2) .
Fe O1 Fe 180.0 3_766
C5 N1 C1 119.0(6) .
C5 N1 Fe 117.1(4) .
C1 N1 Fe 123.7(5) .
C10 N2 C6 120.7(5) .
C10 N2 Fe 119.7(4) .
C6 N2 Fe 119.6(4) .
C11 N3 C15 120.3(5) .
C11 N3 Fe 119.8(4) .
C15 N3 Fe 119.9(4) .
C20 N4 C16 119.5(6) .
C20 N4 Fe 123.1(4) .
C16 N4 Fe 116.0(4) .
N1 C1 C2 121.8(6) .
C3 C2 C1 119.1(6) .
C2 C3 C4 119.7(6) .
C3 C4 C5 118.4(6) .
N1 C5 C4 121.8(6) .
N1 C5 C6 114.5(6) .
C4 C5 C6 123.6(6) .
N2 C6 C7 120.7(6) .
N2 C6 C5 114.5(6) .
C7 C6 C5 124.8(6) .
C8 C7 C6 118.7(6) .
C7 C8 C9 120.6(6) .
C8 C9 C10 117.9(6) .
N2 C10 C9 121.4(6) .
N2 C10 C11 113.4(5) .
C9 C10 C11 125.1(5) .
N3 C11 C12 121.7(6) .
N3 C11 C10 112.9(5) .
C12 C11 C10 125.4(6) .
C13 C12 C11 117.5(6) .
C14 C13 C12 121.5(6) .
C13 C14 C15 118.0(6) .
N3 C15 C14 120.9(6) .
N3 C15 C16 113.9(5) .
C14 C15 C16 125.1(6) .
N4 C16 C17 120.6(6) .
N4 C16 C15 114.6(5) .
C17 C16 C15 124.8(6) .
C16 C17 C18 119.9(6) .
C19 C18 C17 119.2(6) .
C18 C19 C20 118.6(6) .
N4 C20 C19 122.1(6) .
O5 Cl1 O3 110.6(3) .
O5 Cl1 O4 108.3(3) .
O3 Cl1 O4 110.1(3) .
O5 Cl1 O2 109.4(4) .
O3 Cl1 O2 109.4(3) .
O4 Cl1 O2 109.0(4) .
O9 Cl2 O7 109.1(3) .
O9 Cl2 O8 110.0(4) .
O7 Cl2 O8 109.7(4) .
O9 Cl2 O6 109.8(3) .
O7 Cl2 O6 109.6(3) .
O8 Cl2 O6 108.6(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe O1 1.7758(10) .
Fe OW1 2.063(5) .
Fe N3 2.115(5) .
Fe N2 2.118(5) .
Fe N4 2.191(5) .
Fe N1 2.194(6) .
O1 Fe 1.7758(10) 3_766
N1 C5 1.342(8) .
N1 C1 1.351(8) .
N2 C10 1.338(7) .
N2 C6 1.347(8) .
N3 C11 1.344(7) .
N3 C15 1.348(8) .
N4 C20 1.343(8) .
N4 C16 1.356(8) .
C1 C2 1.383(10) .
C2 C3 1.377(10) .
C3 C4 1.384(9) .
C4 C5 1.399(9) .
C5 C6 1.484(8) .
C6 C7 1.389(9) .
C7 C8 1.380(9) .
C8 C9 1.383(10) .
C9 C10 1.392(8) .
C10 C11 1.496(9) .
C11 C12 1.387(9) .
C12 C13 1.384(10) .
C13 C14 1.374(9) .
C14 C15 1.394(8) .
C15 C16 1.480(8) .
C16 C17 1.379(9) .
C17 C18 1.387(9) .
C18 C19 1.380(9) .
C19 C20 1.384(10) .
Cl1 O5 1.426(5) .
Cl1 O3 1.432(4) .
Cl1 O4 1.437(5) .
Cl1 O2 1.443(5) .
Cl2 O9 1.434(5) .
Cl2 O7 1.438(5) .
Cl2 O8 1.447(6) .
Cl2 O6 1.447(5) .
