#------------------------------------------------------------------------------
#$Date: 2016-04-28 05:16:30 +0300 (Thu, 28 Apr 2016) $
#$Revision: 182310 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/31/1543170.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_1543170
loop_
_publ_author_name
'Barrio, Jesús'
'Delgado, Esther'
'Hernández, Diego'
'Hernández, Elisa'
'Perles, Josefina'
'Zamora, Félix'
_publ_section_title
;
 Di-μ-dimethylformamide-κ⁴O:O-μ-tetrahydrofuran-κ²O:O-bis[(tetrahydrofuran-κO)sodium(I)]
 bis(μ-3,6-dichlorobenzene-1,2-dithiolato-κ³S,S':S)bis[(3,6-dichlorobenzene-1,2-dithiolato-κ²S,S')iron(III)]
;
_journal_coeditor_code           BH4005
_journal_issue                   4
_journal_name_full               IUCrData
_journal_page_first              x160643
_journal_paper_doi               10.1107/S241431461600643X
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac
'[Na2 (C3 H7 N O)2 (C4 H8 O)5] [Fe2 (C6 H2 Cl2 S2)4]'
_chemical_formula_moiety         'C24 H8 Cl8 Fe2 S8 2+, C26 H54 N2 Na2 O7 2-'
_chemical_formula_sum            'C50 H62 Cl8 Fe2 N2 Na2 O7 S8'
_chemical_formula_weight         1500.77
_chemical_name_systematic
;Di-μ-dimethylformamide-κ⁴O:O-μ-tetrahydrofuran-κ²O:O-bis[(tetrahydrofuran-κO)sodium(I)]
bis(μ-3,6-dichlorobenzene-1,2-dithiolato-κ³S,S':S)bis[(3,6-dichlorobenzene-1,2-dithiolato-κ²S,S')iron(III)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX3 v2015.5-2'
_cell_angle_alpha                90
_cell_angle_beta                 121.609(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.063(2)
_cell_length_b                   9.9393(6)
_cell_length_c                   25.645(3)
_cell_measurement_reflns_used    3584
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      22.1064
_cell_measurement_theta_min      2.2081
_cell_volume                     6309.0(10)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII'
_diffrn_measurement_method       'θ and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43114
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0.0(2)
_diffrn_standards_interval_time  908
_diffrn_standards_number         5765
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5762
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0854P)²+20.9273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                3785
_reflns_number_total             5765
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            bh4005sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        6309.0(9)
_cod_database_code               1543170
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
C C1 0.1205(2) 0.5476(6) 0.1796(2) 0.0255(13) Uani d 1
C C2 0.1666(2) 0.6228(6) 0.2206(3) 0.0324(14) Uani d 1
C C3 0.2126(2) 0.5608(7) 0.2674(3) 0.0382(16) Uani d 1
H H3 0.2437 0.6124 0.2942 0.046 Uiso calc 1
C C4 0.2125(2) 0.4236(7) 0.2746(3) 0.0370(16) Uani d 1
H H4 0.2438 0.38 0.3063 0.044 Uiso calc 1
C C5 0.1673(2) 0.3495(6) 0.2359(3) 0.0328(14) Uani d 1
C C6 0.1201(2) 0.4095(6) 0.1884(2) 0.0257(13) Uani d 1
C C7 -0.1128(2) 0.3851(6) -0.0270(2) 0.0248(13) Uani d 1
C C8 -0.1619(2) 0.3163(6) -0.0633(3) 0.0334(14) Uani d 1
C C9 -0.2079(2) 0.3846(7) -0.1069(3) 0.0377(16) Uani d 1
H H9 -0.2406 0.3363 -0.1316 0.045 Uiso calc 1
C C10 0.2067(2) 0.4793(7) 0.1147(3) 0.0387(17) Uani d 1
H H10 0.2386 0.433 0.1437 0.046 Uiso calc 1
C C11 0.1589(2) 0.4098(6) 0.0804(3) 0.0314(14) Uani d 1
C C12 0.1114(2) 0.4770(6) 0.0375(2) 0.0274(13) Uani d 1
Cl Cl1 0.16741(7) 0.79653(16) 0.21324(7) 0.0429(4) Uani d 1
Cl Cl2 0.16885(6) 0.17555(17) 0.24562(7) 0.0452(4) Uani d 1
Cl Cl3 -0.16552(6) 0.14461(18) -0.05570(7) 0.0456(4) Uani d 1
Cl Cl4 0.15827(6) 0.23673(17) 0.08984(7) 0.0393(4) Uani d 1
Fe Fe1 0.01139(3) 0.45371(7) 0.06272(3) 0.0205(2) Uani d 1
S S1 0.06380(5) 0.62436(14) 0.11780(6) 0.0229(3) Uani d 1
S S2 0.06183(5) 0.31766(14) 0.14040(6) 0.0267(3) Uani d 1
S S3 -0.05458(5) 0.30212(14) 0.02869(6) 0.0265(3) Uani d 1
S S4 0.04882(5) 0.39247(14) -0.00191(6) 0.0231(3) Uani d 1
C C13 0.0826(5) 1.1857(10) 0.3275(6) 0.105(4) Uani d 1
H H13A 0.0671 1.1971 0.283 0.126 Uiso calc 1
H H13B 0.0531 1.1929 0.3359 0.126 Uiso calc 1
C C14 0.1240(7) 1.2872(13) 0.3620(7) 0.148(6) Uani d 1
H H14A 0.1343 1.332 0.3351 0.177 Uiso calc 1
H H14B 0.11 1.3564 0.3779 0.177 Uiso calc 1
C C15 0.1627(3) 1.0772(10) 0.3994(4) 0.076(3) Uani d 1
H H15A 0.19 1.0432 0.3906 0.091 Uiso calc 1
H H15B 0.1674 1.0287 0.4356 0.091 Uiso calc 1
C C16 0.1703(6) 1.2210(14) 0.4120(7) 0.121(5) Uani d 1
H H16A 0.1728 1.2413 0.4512 0.146 Uiso calc 1
H H16B 0.2039 1.2518 0.4148 0.146 Uiso calc 1
C C17 0.1423(4) 0.6789(11) 0.4322(4) 0.082(3) Uani d 1
H H17A 0.1119 0.6231 0.4269 0.099 Uiso calc 1
H H17B 0.1475 0.7541 0.4601 0.099 Uiso calc 1
C C18 0.1906(3) 0.5988(9) 0.4591(4) 0.069(2) Uani d 1
H H18A 0.1826 0.5041 0.4635 0.083 Uiso calc 1
H H18B 0.218 0.634 0.4999 0.083 Uiso calc 1
C C19 0.2101(4) 0.6087(10) 0.4164(4) 0.081(3) Uani d 1
H H19A 0.2472 0.6455 0.4377 0.098 Uiso calc 1
H H19B 0.2103 0.5188 0.4 0.098 Uiso calc 1
C C20 0.1741(5) 0.6957(13) 0.3685(5) 0.112(4) Uani d 1
H H20A 0.1607 0.6507 0.3286 0.135 Uiso calc 1
H H20B 0.1936 0.7782 0.3695 0.135 Uiso calc 1
C C23 0.0411(3) 0.9659(7) 0.1732(3) 0.0423(16) Uani d 1
H H23 0.0786 0.9867 0.1968 0.051 Uiso calc 1
C C24 0.0492(3) 0.9917(7) 0.0845(3) 0.0398(16) Uani d 1
H H24A 0.0869 1.011 0.1158 0.06 Uiso calc 1
H H24B 0.0339 1.068 0.0563 0.06 Uiso calc 1
H H24C 0.0476 0.9109 0.0617 0.06 Uiso calc 1
C C25 -0.0394(3) 0.9425(6) 0.0737(3) 0.0408(16) Uani d 1
H H25A -0.0577 0.9574 0.0962 0.061 Uiso calc 1
H H25B -0.0447 0.849 0.0596 0.061 Uiso calc 1
H H25C -0.0546 1.0031 0.0383 0.061 Uiso calc 1
N N1 0.0182(2) 0.9694(5) 0.1138(2) 0.0317(12) Uani d 1
Na Na1 0.05894(11) 0.8688(3) 0.30354(12) 0.0485(7) Uani d 1
O O1 0.1100(2) 1.0542(6) 0.3483(3) 0.0744(17) Uani d 1
O O2 0.1294(2) 0.7314(6) 0.3744(3) 0.0757(18) Uani d 1
O O3 0.01874(19) 0.9381(4) 0.2015(2) 0.0431(11) Uani d 1
O O4 0 0.6850(7) 0.25 0.061(2) Uani d 1
C C21 0.0153(4) 0.5972(8) 0.2171(5) 0.080(3) Uani d 1
H H21A -0.0079 0.6157 0.1727 0.096 Uiso calc 1
H H21B 0.0532 0.6163 0.2295 0.096 Uiso calc 1
C C22 0.0109(9) 0.4696(10) 0.2273(8) 0.227(11) Uani d 1
H H22A 0.0464 0.424 0.2462 0.272 Uiso calc 1
H H22B -0.0148 0.423 0.1886 0.272 Uiso calc 1
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
N N 0.0061 0.0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C6 C1 C2 . . 119.2(5)
C6 C1 S1 . . 119.5(4)
C2 C1 S1 . . 121.4(5)
C3 C2 C1 . . 121.3(6)
C3 C2 Cl1 . . 118.2(5)
C1 C2 Cl1 . . 120.5(5)
C4 C3 C2 . . 119.2(6)
C5 C4 C3 . . 120.1(6)
C4 C5 C6 . . 122.0(6)
C4 C5 Cl2 . . 119.0(5)
C6 C5 Cl2 . . 119.1(5)
C1 C6 C5 . . 118.2(5)
C1 C6 S2 . . 119.3(4)
C5 C6 S2 . . 122.5(5)
C12 C7 C8 5_565 . 117.9(5)
C12 C7 S3 5_565 . 120.5(4)
C8 C7 S3 . . 121.6(5)
C9 C8 C7 . . 120.7(6)
C9 C8 Cl3 . . 118.9(5)
C7 C8 Cl3 . . 120.4(5)
C10 C9 C8 5_565 . 120.8(6)
C9 C10 C11 5_565 . 119.7(6)
C10 C11 C12 . . 120.7(6)
C10 C11 Cl4 . . 119.2(5)
C12 C11 Cl4 . . 120.1(5)
C11 C12 C7 . 5_565 120.1(5)
C11 C12 S4 . . 121.2(5)
C7 C12 S4 5_565 . 118.7(4)
S2 Fe1 S1 . . 89.09(6)
S2 Fe1 S3 . . 88.13(6)
S1 Fe1 S3 . . 158.23(7)
S2 Fe1 S4 . 5_565 163.07(7)
S1 Fe1 S4 . 5_565 86.93(6)
S3 Fe1 S4 . 5_565 89.48(6)
S2 Fe1 S4 . . 97.79(6)
S1 Fe1 S4 . . 102.52(6)
S3 Fe1 S4 . . 99.25(6)
S4 Fe1 S4 5_565 . 99.13(5)
C1 S1 Fe1 . . 104.4(2)
C6 S2 Fe1 . . 104.9(2)
C7 S3 Fe1 . . 105.5(2)
C12 S4 Fe1 . 5_565 105.7(2)
C12 S4 Fe1 . . 100.46(18)
Fe1 S4 Fe1 5_565 . 80.87(5)
C14 C13 O1 . . 106.0(11)
C16 C14 C13 . . 108.2(12)
O1 C15 C16 . . 109.1(9)
C14 C16 C15 . . 106.8(11)
O2 C17 C18 . . 111.1(7)
C17 C18 C19 . . 105.4(8)
C20 C19 C18 . . 106.8(8)
C19 C20 O2 . . 111.0(8)
O3 C23 N1 . . 126.0(7)
C23 N1 C25 . . 121.0(5)
C23 N1 C24 . . 121.9(6)
C25 N1 C24 . . 117.0(5)
O1 Na1 O3 . 2 98.5(2)
O1 Na1 O2 . . 90.4(3)
O3 Na1 O2 2 . 130.9(2)
O1 Na1 O3 . . 97.9(2)
O3 Na1 O3 2 . 87.03(19)
O2 Na1 O3 . . 139.6(2)
O1 Na1 O4 . . 175.4(2)
O3 Na1 O4 2 . 79.00(16)
O2 Na1 O4 . . 94.2(2)
O3 Na1 O4 . . 78.16(15)
O1 Na1 Na1 . 2 125.53(17)
O3 Na1 Na1 2 2 49.18(13)
O2 Na1 Na1 . 2 143.93(18)
O3 Na1 Na1 . 2 47.98(13)
O4 Na1 Na1 . 2 49.97(12)
C15 O1 C13 . . 107.9(7)
C15 O1 Na1 . . 134.7(6)
C13 O1 Na1 . . 116.8(6)
C17 O2 C20 . . 105.1(6)
C17 O2 Na1 . . 132.0(5)
C20 O2 Na1 . . 122.6(5)
C23 O3 Na1 . 2 147.1(4)
C23 O3 Na1 . . 128.0(4)
Na1 O3 Na1 2 . 82.83(18)
C21 O4 C21 2 . 105.3(8)
C21 O4 Na1 2 2 116.9(4)
C21 O4 Na1 . 2 118.5(4)
C21 O4 Na1 2 . 118.5(4)
C21 O4 Na1 . . 116.9(4)
Na1 O4 Na1 2 . 80.1(2)
C22 C21 O4 . . 112.1(7)
C21 C22 C22 . 2 105.3(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 C6 . 1.393(8)
C1 C2 . 1.407(8)
C1 S1 . 1.753(5)
C2 C3 . 1.388(8)
C2 Cl1 . 1.739(7)
C3 C4 . 1.376(9)
C4 C5 . 1.374(8)
C5 C6 . 1.402(7)
C5 Cl2 . 1.745(6)
C6 S2 . 1.742(5)
C7 C12 5_565 1.402(8)
C7 C8 . 1.407(8)
C7 S3 . 1.746(5)
C8 C9 . 1.390(9)
C8 Cl3 . 1.727(7)
C9 C10 5_565 1.371(9)
C10 C9 5_565 1.372(9)
C10 C11 . 1.377(8)
C11 C12 . 1.403(8)
C11 Cl4 . 1.739(7)
C12 C7 5_565 1.402(8)
C12 S4 . 1.764(6)
Fe1 S2 . 2.2101(16)
Fe1 S1 . 2.2219(15)
Fe1 S3 . 2.2256(15)
Fe1 S4 5_565 2.2296(15)
Fe1 S4 . 2.4885(16)
S4 Fe1 5_565 2.2296(15)
C13 C14 . 1.461(16)
C13 O1 . 1.477(12)
C14 C16 . 1.442(18)
C15 O1 . 1.419(10)
C15 C16 . 1.456(15)
C17 O2 . 1.425(9)
C17 C18 . 1.436(11)
C18 C19 . 1.473(12)
C19 C20 . 1.416(12)
C20 O2 . 1.428(10)
C23 O3 . 1.236(7)
C23 N1 . 1.303(8)
C24 N1 . 1.462(7)
C25 N1 . 1.458(8)
Na1 O1 . 2.265(6)
Na1 O3 2 2.298(5)
Na1 O2 . 2.336(6)
Na1 O3 . 2.341(5)
Na1 O4 . 2.385(6)
Na1 Na1 2 3.069(5)
O3 Na1 2 2.298(5)
O4 C21 2 1.438(7)
O4 C21 . 1.438(7)
O4 Na1 2 2.385(6)
C21 C22 . 1.315(11)
C22 C22 2 1.593(17)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C9 H9 Cl2 8_455 0.95 2.86 3.645(6) 141.0 y
C16 H16A Cl3 2_565 0.99 2.96 3.836(15) 148.4 y
C23 H23 Cl2 1_565 0.95 2.92 3.787(7) 152.2 y
C25 H25B S4 5_565 0.98 2.79 3.744(6) 165.3 y
C25 H25C S3 1_565 0.98 2.98 3.711(7) 132.0 y

_cod_database_fobs_code 1543170
