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#$Date: 2016-03-23 03:26:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179246 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/66/4316645.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4316645
loop_
_publ_author_name
'Pablo Alborés'
'Eva Rentschler'
_publ_contact_author_address
;INQUIMAE-FCEN-Universidad de Buenos Aires
Ciudad  Universitaria- Pabellon 2- 3 piso
C1428EHA Buenos Aires- Argentina
;
_publ_contact_author_email       albores@qi.fcen.uba.ar
_publ_contact_author_name        'Pablo Albores'
_publ_section_title
;
 cis-2,2'-Bipyrimidine-Bridged Polynuclear Complex: A Stairway-like
 Mixed-Valent {Fe4} Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8953
_journal_page_last               8961
_journal_paper_doi               10.1021/ic1013472
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C24 H26 Cl10 Fe4 N12 O4'
_chemical_formula_weight         1124.47
_chemical_name_systematic
;
 ?
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.8550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4691(3)
_cell_length_b                   11.7690(5)
_cell_length_c                   22.9889(10)
_cell_measurement_temperature    173(2)
_cell_volume                     2006.37(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21602
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    2.133
_exptl_absorpt_correction_T_max  0.9008
_exptl_absorpt_correction_T_min  0.7756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4563
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0301P)²+2.5053P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                3788
_reflns_number_total             4563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1013472_si_001.cif
_cod_data_source_block           pa_442_1_0m
_cod_original_cell_volume        2006.37(25)
_cod_database_code               4316645
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4991(4) 0.3898(2) 0.75264(12) 0.0211(6) Uani 1 1 d . . .
H1 H 0.4680 0.4354 0.7840 0.025 Uiso 1 1 calc R . .
C2 C 0.5801(4) 0.0071(2) 0.48404(11) 0.0163(5) Uani 1 1 d . . .
C3 C 0.6119(4) 0.2975(2) 0.76462(12) 0.0206(6) Uani 1 1 d . . .
H3 H 0.6605 0.2798 0.8037 0.025 Uiso 1 1 calc R . .
C4 C 0.4044(4) 0.3755(2) 0.59465(12) 0.0167(5) Uani 1 1 d . . .
C5 C 0.2330(4) 0.4917(2) 0.53159(12) 0.0199(6) Uani 1 1 d . . .
H5 H 0.1566 0.5560 0.5243 0.024 Uiso 1 1 calc R . .
C6 C 0.8327(4) 0.1069(3) 0.47164(13) 0.0236(6) Uani 1 1 d . . .
H6 H 0.9144 0.1674 0.4820 0.028 Uiso 1 1 calc R . .
C7 C 0.7444(4) -0.0522(3) 0.41297(13) 0.0248(6) Uani 1 1 d . . .
H7 H 0.7648 -0.1037 0.3826 0.030 Uiso 1 1 calc R . .
C8 C 0.2772(4) 0.4282(2) 0.48481(13) 0.0227(6) Uani 1 1 d . . .
H8 H 0.2314 0.4471 0.4457 0.027 Uiso 1 1 calc R . .
C9 C 0.4775(4) 0.3471(2) 0.65548(11) 0.0168(5) Uani 1 1 d . . .
C10 C 0.8638(4) 0.0353(3) 0.42648(13) 0.0268(7) Uani 1 1 d . . .
H10 H 0.9644 0.0461 0.4054 0.032 Uiso 1 1 calc R . .
C11 C 0.3903(4) 0.3364(2) 0.49706(12) 0.0233(6) Uani 1 1 d . . .
H11 H 0.4220 0.2908 0.4658 0.028 Uiso 1 1 calc R . .
C12 C 0.6515(4) 0.2320(2) 0.71838(12) 0.0219(6) Uani 1 1 d . . .
H12 H 0.7295 0.1686 0.7256 0.026 Uiso 1 1 calc R . .
N1 N 0.5819(3) 0.25588(19) 0.66295(10) 0.0182(5) Uani 1 1 d . . .
N2 N 0.4566(3) 0.31006(19) 0.55236(10) 0.0186(5) Uani 1 1 d . . .
N3 N 0.4329(3) 0.4162(2) 0.69747(10) 0.0182(5) Uani 1 1 d . . .
N4 N 0.6900(3) 0.09330(19) 0.50135(10) 0.0187(5) Uani 1 1 d . . .
N5 N 0.2951(3) 0.46495(19) 0.58707(10) 0.0171(5) Uani 1 1 d . . .
N6 N 0.4003(3) 0.06690(19) 0.55839(10) 0.0183(5) Uani 1 1 d . . .
Cl1 Cl 0.07402(11) 0.68671(7) 0.61619(3) 0.03061(18) Uani 1 1 d . . .
Cl2 Cl 0.28425(10) 0.63971(6) 0.76035(3) 0.02457(16) Uani 1 1 d . . .
Cl3 Cl 0.74451(10) 0.00756(6) 0.63647(3) 0.02561(16) Uani 1 1 d . . .
Cl4 Cl 0.90261(11) 0.29419(6) 0.58145(3) 0.02893(17) Uani 1 1 d . . .
Cl5 Cl 0.53565(10) 0.65034(7) 0.64774(3) 0.02942(17) Uani 1 1 d . . .
Fe1 Fe 0.26842(5) 0.56765(3) 0.668812(17) 0.01702(10) Uani 1 1 d . . .
Fe2 Fe 0.64398(5) 0.17281(3) 0.583682(16) 0.01522(9) Uani 1 1 d . . .
O1 O 0.0604(3) 0.46014(19) 0.68293(9) 0.0271(5) Uani 1 1 d D . .
O1W O 0.0575(4) 0.3949(2) 0.79186(11) 0.0374(6) Uani 1 1 d D . .
H1A H 0.017(5) 0.412(3) 0.6601(14) 0.045 Uiso 1 1 d D . .
H1B H 0.047(5) 0.436(3) 0.7163(10) 0.045 Uiso 1 1 d D . .
H1WA H 0.063(5) 0.3271(18) 0.8009(17) 0.045 Uiso 1 1 d D . .
H1WB H -0.022(4) 0.427(3) 0.8085(16) 0.045 Uiso 1 1 d 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'
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'
O O 0.0106 0.0060 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C3 121.2(3) . . ?
N6 C2 N4 126.8(2) 3_656 . ?
N6 C2 C2 117.0(3) 3_656 3_656 ?
N4 C2 C2 116.2(3) . 3_656 ?
C12 C3 C1 118.0(3) . . ?
N5 C4 N2 126.1(2) . . ?
N5 C4 C9 117.0(2) . . ?
N2 C4 C9 116.9(2) . . ?
N5 C5 C8 121.7(3) . . ?
N4 C6 C10 121.7(3) . . ?
N6 C7 C10 121.7(3) 3_656 . ?
C11 C8 C5 117.5(3) . . ?
N1 C9 N3 126.4(2) . . ?
N1 C9 C4 116.8(2) . . ?
N3 C9 C4 116.8(2) . . ?
C7 C10 C6 117.7(3) . . ?
N2 C11 C8 121.4(3) . . ?
N1 C12 C3 121.4(3) . . ?
C9 N1 C12 116.5(2) . . ?
C9 N1 Fe2 115.97(18) . . ?
C12 N1 Fe2 127.20(19) . . ?
C4 N2 C11 116.7(2) . . ?
C4 N2 Fe2 114.52(18) . . ?
C11 N2 Fe2 128.77(19) . . ?
C9 N3 C1 116.6(2) . . ?
C9 N3 Fe1 116.85(18) . . ?
C1 N3 Fe1 126.51(19) . . ?
C2 N4 C6 115.9(2) . . ?
C2 N4 Fe2 115.50(17) . . ?
C6 N4 Fe2 127.53(19) . . ?
C4 N5 C5 116.6(2) . . ?
C4 N5 Fe1 115.29(17) . . ?
C5 N5 Fe1 127.52(19) . . ?
C2 N6 C7 116.2(2) 3_656 3_656 ?
C2 N6 Fe2 113.61(18) 3_656 . ?
C7 N6 Fe2 128.71(19) 3_656 . ?
O1 Fe1 N3 82.01(9) . . ?
O1 Fe1 Cl2 92.32(7) . . ?
N3 Fe1 Cl2 93.41(6) . . ?
O1 Fe1 Cl1 90.96(7) . . ?
N3 Fe1 Cl1 162.44(6) . . ?
Cl2 Fe1 Cl1 102.98(3) . . ?
O1 Fe1 N5 86.88(8) . . ?
N3 Fe1 N5 73.56(8) . . ?
Cl2 Fe1 N5 166.94(6) . . ?
Cl1 Fe1 N5 90.08(6) . . ?
O1 Fe1 Cl5 166.77(7) . . ?
N3 Fe1 Cl5 86.53(6) . . ?
Cl2 Fe1 Cl5 94.95(3) . . ?
Cl1 Fe1 Cl5 98.14(3) . . ?
N5 Fe1 Cl5 83.54(6) . . ?
N1 Fe2 N4 176.37(9) . . ?
N1 Fe2 N2 75.67(8) . . ?
N4 Fe2 N2 101.04(8) . . ?
N1 Fe2 N6 102.83(9) . . ?
N4 Fe2 N6 74.99(8) . . ?
N2 Fe2 N6 81.80(8) . . ?
N1 Fe2 Cl3 91.50(6) . . ?
N4 Fe2 Cl3 91.11(6) . . ?
N2 Fe2 Cl3 157.09(7) . . ?
N6 Fe2 Cl3 82.72(6) . . ?
N1 Fe2 Cl4 90.17(7) . . ?
N4 Fe2 Cl4 91.50(6) . . ?
N2 Fe2 Cl4 92.18(7) . . ?
N6 Fe2 Cl4 163.73(6) . . ?
Cl3 Fe2 Cl4 106.99(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.342(3) . ?
C1 C3 1.382(4) . ?
C2 N6 1.329(3) 3_656 ?
C2 N4 1.335(4) . ?
C2 C2 1.486(5) 3_656 ?
C3 C12 1.373(4) . ?
C4 N5 1.331(3) . ?
C4 N2 1.335(3) . ?
C4 C9 1.478(4) . ?
C5 N5 1.342(3) . ?
C5 C8 1.382(4) . ?
C6 N4 1.342(4) . ?
C6 C10 1.378(4) . ?
C7 N6 1.342(4) 3_656 ?
C7 C10 1.374(4) . ?
C8 C11 1.380(4) . ?
C9 N1 1.326(3) . ?
C9 N3 1.334(3) . ?
C11 N2 1.344(4) . ?
C12 N1 1.347(3) . ?
N1 Fe2 2.166(2) . ?
N2 Fe2 2.201(2) . ?
N3 Fe1 2.220(2) . ?
N4 Fe2 2.175(2) . ?
N5 Fe1 2.263(2) . ?
N6 C2 1.329(3) 3_656 ?
N6 C7 1.342(4) 3_656 ?
N6 Fe2 2.225(2) . ?
Cl1 Fe1 2.2618(8) . ?
Cl2 Fe1 2.2588(8) . ?
Cl3 Fe2 2.3668(8) . ?
Cl4 Fe2 2.4081(8) . ?
Cl5 Fe1 2.3230(8) . ?
Fe1 O1 2.059(2) . ?
