#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:14:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179100 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/62/4306273.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_4306273
loop_
_publ_author_name
'Pablo Alborés'
'Eva Rentschler'
_publ_contact_author_address
;Institute of Inorganic and Analytical Chemistry
University of Mainz
Mainz
Germany
D-55128
;
_publ_contact_author_email       albores@uni-mainz.de
_publ_contact_author_fax         '+49 6131 / 39-23922'
_publ_contact_author_name        'Dr.Pablo Albores'
_publ_contact_author_phone       '+49 6131 / 39-25377'
_publ_section_title
;
Structural and Magnetic Characterization of a μ-1,5-Dicyanamide-Bridged
Iron Basic Carboxylate [Fe3O(O2C(CH3)3)6] 1D Chain
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7960
_journal_page_last               7962
_journal_paper_doi               10.1021/ic801113d
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C40 H74 Fe3 N3 O16'
_chemical_formula_weight         1020.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2ab'
_symmetry_space_group_name_H-M   'P b n m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.461(7)
_cell_length_b                   19.034(9)
_cell_length_c                   20.510(10)
_cell_measurement_temperature    173(2)
_cell_volume                     5645(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.3249
_diffrn_reflns_av_sigmaI/netI    0.3056
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54191
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8261
_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    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.772
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6922
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.2385
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0455P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                1988
_reflns_number_total             6922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801113d_si_001_1.cif
_cod_data_source_block           2
_cod_original_cell_volume        5645(8)
_cod_database_code               4306273
loop_
_symmetry_equiv_pos_as_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_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
Fe1 Fe 0.03041(7) 0.11329(5) 0.2500 0.0383(4) Uani 1 2 d S . .
Fe2 Fe -0.10761(7) 0.25144(5) 0.2500 0.0375(3) Uani 1 2 d S . .
Fe3 Fe 0.11794(7) 0.27380(5) 0.2500 0.0401(4) Uani 1 2 d S . .
O1 O 0.0119(3) 0.2133(2) 0.2500 0.0322(13) Uani 1 2 d S . .
O6 O -0.0828(3) 0.32492(19) 0.3188(2) 0.0507(12) Uani 1 1 d . . .
O4 O -0.1525(3) 0.1896(2) 0.3228(2) 0.0536(13) Uani 1 1 d . . .
C1 C -0.0105(5) 0.3515(3) 0.3391(3) 0.0453(17) Uani 1 1 d . . .
C10 C -0.1183(5) 0.1373(3) 0.3485(4) 0.0547(19) Uani 1 1 d . . .
O2 O 0.1263(3) 0.1151(2) 0.3192(2) 0.0771(16) Uani 1 1 d . . .
O7 O 0.0673(3) 0.3372(3) 0.3178(3) 0.099(2) Uani 1 1 d . . .
C6 C 0.1787(4) 0.1601(4) 0.3406(3) 0.0536(19) Uani 1 1 d . . .
O3 O 0.1840(3) 0.2209(3) 0.3184(3) 0.0886(18) Uani 1 1 d . . .
C2 C -0.0131(5) 0.4070(3) 0.3937(3) 0.062(2) Uani 1 1 d . . .
O5 O -0.0607(3) 0.0981(2) 0.3214(3) 0.097(2) Uani 1 1 d . . .
C7 C 0.2422(6) 0.1418(4) 0.3977(4) 0.087(3) Uani 1 1 d . . .
C11 C -0.1446(5) 0.1208(4) 0.4190(5) 0.089(3) Uani 1 1 d . . .
C3 C -0.1102(5) 0.4152(3) 0.4200(3) 0.094(3) Uani 1 1 d . . .
H3A H -0.1523 0.4270 0.3842 0.140 Uiso 1 1 calc R . .
H3B H -0.1112 0.4528 0.4526 0.140 Uiso 1 1 calc R . .
H3C H -0.1299 0.3710 0.4402 0.140 Uiso 1 1 calc R . .
C5 C 0.0522(7) 0.3884(5) 0.4456(4) 0.212(7) Uani 1 1 d . . .
H5A H 0.0339 0.3435 0.4651 0.318 Uiso 1 1 calc R . .
H5B H 0.0519 0.4251 0.4791 0.318 Uiso 1 1 calc R . .
H5C H 0.1145 0.3841 0.4272 0.318 Uiso 1 1 calc R . .
C12 C -0.1010(8) 0.1792(6) 0.4602(4) 0.178(5) Uani 1 1 d . . .
H12A H -0.0336 0.1774 0.4558 0.266 Uiso 1 1 calc R . .
H12B H -0.1179 0.1725 0.5061 0.266 Uiso 1 1 calc R . .
H12C H -0.1236 0.2250 0.4452 0.266 Uiso 1 1 calc R . .
C4 C 0.0124(6) 0.4770(4) 0.3615(4) 0.135(4) Uani 1 1 d . . .
H4A H -0.0341 0.4889 0.3285 0.203 Uiso 1 1 calc R . .
H4B H 0.0732 0.4729 0.3407 0.203 Uiso 1 1 calc R . .
H4C H 0.0144 0.5141 0.3946 0.203 Uiso 1 1 calc R . .
C8 C 0.3383(5) 0.1554(5) 0.3792(5) 0.171(6) Uani 1 1 d . . .
H8A H 0.3453 0.2049 0.3670 0.256 Uiso 1 1 calc R . .
H8B H 0.3550 0.1256 0.3421 0.256 Uiso 1 1 calc R . .
H8C H 0.3790 0.1448 0.4161 0.256 Uiso 1 1 calc R . .
C9 C 0.2291(6) 0.0675(4) 0.4185(4) 0.158(5) Uani 1 1 d . . .
H9A H 0.1648 0.0604 0.4319 0.236 Uiso 1 1 calc R . .
H9B H 0.2703 0.0573 0.4553 0.236 Uiso 1 1 calc R . .
H9C H 0.2438 0.0361 0.3822 0.236 Uiso 1 1 calc R . .
O8 O -0.2424(3) 0.2899(2) 0.2500 0.0524(17) Uani 1 2 d S . .
N2 N 0.2635(5) -0.1613(4) 0.2500 0.069(3) Uani 1 2 d S . .
N1 N 0.0525(5) 0.0033(4) 0.2500 0.055(2) Uani 1 2 d S . .
C17 C 0.1934(8) -0.1349(5) 0.2500 0.103(5) Uani 1 2 d S . .
C16 C 0.0849(7) -0.0504(5) 0.2500 0.086(4) Uani 1 2 d S . .
N3 N 0.1144(7) -0.1092(5) 0.2801(7) 0.126(10) Uani 0.50 1 d P . .
C13 C -0.1089(8) 0.0494(6) 0.4411(5) 0.255(8) Uani 1 1 d . . .
H13A H -0.0416 0.0478 0.4360 0.382 Uiso 1 1 calc R . .
H13B H -0.1372 0.0124 0.4144 0.382 Uiso 1 1 calc R . .
H13C H -0.1251 0.0420 0.4870 0.382 Uiso 1 1 calc R . .
C14 C -0.2477(6) 0.1233(5) 0.4275(4) 0.140(4) Uani 1 1 d . . .
H14A H -0.2634 0.1128 0.4729 0.209 Uiso 1 1 calc R . .
H14B H -0.2767 0.0885 0.3988 0.209 Uiso 1 1 calc R . .
H14C H -0.2704 0.1703 0.4163 0.209 Uiso 1 1 calc R . .
C15 C 0.2176(9) 0.1934(6) 0.4534(5) 0.232(7) Uani 1 1 d . . .
H15A H 0.2263 0.2418 0.4384 0.348 Uiso 1 1 calc R . .
H15B H 0.2580 0.1845 0.4909 0.348 Uiso 1 1 calc R . .
H15C H 0.1530 0.1864 0.4663 0.348 Uiso 1 1 calc R . .
O1S O -0.3984(6) 0.2412(5) 0.3080(5) 0.092(4) Uani 0.509(6) 1 d PDU A 1
C1S C -0.4458(11) 0.1812(8) 0.2924(11) 0.172(11) Uani 0.509(6) 1 d PDU A 1
H1S1 H -0.4575 0.1529 0.3320 0.207 Uiso 0.509(6) 1 calc PR A 1
H1S2 H -0.5060 0.1930 0.2721 0.207 Uiso 0.509(6) 1 calc PR A 1
C2S C -0.3922(11) 0.1452(7) 0.2500 0.194(9) Uani 1 2 d SDU A 1
H2S1 H -0.4015 0.0946 0.2564 0.291 Uiso 0.50 1 calc PR A 1
H2S2 H -0.3271 0.1569 0.2576 0.291 Uiso 0.50 1 calc PR A 1
H2S3 H -0.4091 0.1579 0.2053 0.291 Uiso 0.50 1 calc PR A 1
C3S C -0.4363(9) 0.2896(9) 0.3667(7) 0.179(11) Uani 0.509(6) 1 d PDU A 1
H3S1 H -0.5042 0.2944 0.3621 0.215 Uiso 0.509(6) 1 calc PR A 1
H3S2 H -0.4241 0.2653 0.4085 0.215 Uiso 0.509(6) 1 calc PR A 1
C4S C -0.3966(8) 0.3579(10) 0.3695(8) 0.31(2) Uani 0.509(6) 1 d PDU A 1
H4S1 H -0.4207 0.3829 0.4076 0.459 Uiso 0.509(6) 1 calc PR A 1
H4S2 H -0.4126 0.3839 0.3298 0.459 Uiso 0.509(6) 1 calc PR A 1
H4S3 H -0.3292 0.3539 0.3729 0.459 Uiso 0.509(6) 1 calc PR A 1
O2S O -0.3280(7) 0.3918(5) 0.3188(5) 0.091(4) Uani 0.491(6) 1 d PDU A 2
C8S C -0.3216(11) 0.4570(8) 0.2903(9) 0.123(8) Uani 0.491(6) 1 d PDU A 2
H8S1 H -0.3223 0.4924 0.3257 0.148 Uiso 0.491(6) 1 calc PR A 2
H8S2 H -0.3785 0.4643 0.2642 0.148 Uiso 0.491(6) 1 calc PR A 2
C7S C -0.2461(9) 0.4723(6) 0.2500 0.120(5) Uani 1 2 d SDU A 2
H7S1 H -0.2270 0.5211 0.2567 0.180 Uiso 0.50 1 calc PR A 2
H7S2 H -0.2638 0.4655 0.2043 0.180 Uiso 0.50 1 calc PR A 2
H7S3 H -0.1947 0.4409 0.2607 0.180 Uiso 0.50 1 calc PR A 2
C5S C -0.4363(9) 0.2896(9) 0.3667(7) 0.232(5) Uani 0.491(6) 1 d PDU A 2
H5S1 H -0.4785 0.2832 0.4036 0.348 Uiso 0.491(6) 1 calc PR A 2
H5S2 H -0.3872 0.2542 0.3687 0.348 Uiso 0.491(6) 1 calc PR A 2
H5S3 H -0.4707 0.2843 0.3258 0.348 Uiso 0.491(6) 1 calc PR A 2
C6S C -0.3966(8) 0.3579(10) 0.3695(8) 0.233(6) Uani 0.491(6) 1 d PDU A 2
H6S1 H -0.3646 0.3604 0.4121 0.280 Uiso 0.491(6) 1 calc PR A 2
H6S2 H -0.4495 0.3908 0.3724 0.280 Uiso 0.491(6) 1 calc PR A 2
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'
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'
O O 0.0106 0.0060 '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'
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
O1 Fe1 O2 94.60(15) . . ?
O1 Fe1 O2 94.60(15) . 6_556 ?
O2 Fe1 O2 91.3(3) . 6_556 ?
O1 Fe1 O5 92.96(14) . 6_556 ?
O2 Fe1 O5 172.28(17) . 6_556 ?
O2 Fe1 O5 86.5(2) 6_556 6_556 ?
O1 Fe1 O5 92.96(14) . . ?
O2 Fe1 O5 86.5(2) . . ?
O2 Fe1 O5 172.28(17) 6_556 . ?
O5 Fe1 O5 94.7(3) 6_556 . ?
O1 Fe1 N1 179.4(2) . . ?
O2 Fe1 N1 84.95(17) . . ?
O2 Fe1 N1 84.95(17) 6_556 . ?
O5 Fe1 N1 87.48(17) 6_556 . ?
O5 Fe1 N1 87.48(17) . . ?
O1 Fe2 O4 94.05(14) . 6_556 ?
O1 Fe2 O4 94.05(14) . . ?
O4 Fe2 O4 96.0(3) 6_556 . ?
O1 Fe2 O6 96.00(15) . . ?
O4 Fe2 O6 169.35(16) 6_556 . ?
O4 Fe2 O6 86.79(17) . . ?
O1 Fe2 O6 96.00(15) . 6_556 ?
O4 Fe2 O6 86.79(17) 6_556 6_556 ?
O4 Fe2 O6 169.35(16) . 6_556 ?
O6 Fe2 O6 88.6(2) . 6_556 ?
O1 Fe2 O8 177.80(19) . . ?
O4 Fe2 O8 84.49(14) 6_556 . ?
O4 Fe2 O8 84.49(14) . . ?
O6 Fe2 O8 85.57(14) . . ?
O6 Fe2 O8 85.57(14) 6_556 . ?
O1 Fe3 O3 94.63(16) . . ?
O1 Fe3 O3 94.63(16) . 6_556 ?
O3 Fe3 O3 90.6(3) . 6_556 ?
O1 Fe3 O7 94.02(16) . 6_556 ?
O3 Fe3 O7 171.32(19) . 6_556 ?
O3 Fe3 O7 89.5(2) 6_556 6_556 ?
O1 Fe3 O7 94.02(16) . . ?
O3 Fe3 O7 89.5(2) . . ?
O3 Fe3 O7 171.32(19) 6_556 . ?
O7 Fe3 O7 89.2(4) 6_556 . ?
O1 Fe3 N2 178.8(2) . 7_665 ?
O3 Fe3 N2 84.56(18) . 7_665 ?
O3 Fe3 N2 84.56(18) 6_556 7_665 ?
O7 Fe3 N2 86.80(19) 6_556 7_665 ?
O7 Fe3 N2 86.80(19) . 7_665 ?
Fe2 O1 Fe3 120.3(2) . . ?
Fe2 O1 Fe1 120.8(2) . . ?
Fe3 O1 Fe1 118.9(2) . . ?
C1 O6 Fe2 132.1(4) . . ?
C10 O4 Fe2 131.5(4) . . ?
O6 C1 O7 124.1(6) . . ?
O6 C1 C2 120.4(6) . . ?
O7 C1 C2 115.4(6) . . ?
O4 C10 O5 124.2(7) . . ?
O4 C10 C11 118.0(6) . . ?
O5 C10 C11 117.7(7) . . ?
C6 O2 Fe1 134.5(4) . . ?
C1 O7 Fe3 135.9(4) . . ?
O2 C6 O3 123.7(6) . . ?
O2 C6 C7 119.3(7) . . ?
O3 C6 C7 117.0(7) . . ?
C6 O3 Fe3 134.7(4) . . ?
C5 C2 C3 111.4(7) . . ?
C5 C2 C4 111.7(7) . . ?
C3 C2 C4 106.7(6) . . ?
C5 C2 C1 110.2(6) . . ?
C3 C2 C1 110.6(6) . . ?
C4 C2 C1 106.1(5) . . ?
C10 O5 Fe1 133.0(4) . . ?
C8 C7 C9 111.2(8) . . ?
C8 C7 C6 109.5(7) . . ?
C9 C7 C6 111.1(6) . . ?
C8 C7 C15 107.3(8) . . ?
C9 C7 C15 111.1(9) . . ?
C6 C7 C15 106.5(7) . . ?
C14 C11 C13 109.3(7) . . ?
C14 C11 C10 110.6(7) . . ?
C13 C11 C10 112.3(7) . . ?
C14 C11 C12 108.8(8) . . ?
C13 C11 C12 110.1(9) . . ?
C10 C11 C12 105.8(6) . . ?
C17 N2 Fe3 170.6(8) . 7_655 ?
C16 N1 Fe1 164.0(7) . . ?
N2 C17 N3 153.4(6) . 6_556 ?
N2 C17 N3 153.4(6) . . ?
N3 C17 N3 52.8(13) 6_556 . ?
N1 C16 N3 152.5(6) . . ?
N1 C16 N3 152.5(6) . 6_556 ?
N3 C16 N3 54.4(13) . 6_556 ?
N3 N3 C16 62.8(7) 6_556 . ?
N3 N3 C17 63.6(6) 6_556 . ?
C16 N3 C17 110.5(10) . . ?
C1S O1S C3S 118.7(12) . . ?
C2S C1S O1S 106.6(15) . . ?
C4S C3S O1S 114.5(11) . . ?
O2S C8S C7S 119.4(13) . . ?
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
Fe1 O1 1.922(4) . ?
Fe1 O2 1.984(4) . ?
Fe1 O2 1.984(4) 6_556 ?
Fe1 O5 1.990(4) 6_556 ?
Fe1 O5 1.990(4) . ?
Fe1 N1 2.118(7) . ?
Fe2 O1 1.875(4) . ?
Fe2 O4 2.010(4) 6_556 ?
Fe2 O4 2.010(4) . ?
Fe2 O6 2.018(4) . ?
Fe2 O6 2.018(4) 6_556 ?
Fe2 O8 2.082(5) . ?
Fe3 O1 1.918(4) . ?
Fe3 O3 1.973(4) . ?
Fe3 O3 1.973(4) 6_556 ?
Fe3 O7 1.982(4) 6_556 ?
Fe3 O7 1.982(4) . ?
Fe3 N2 2.113(7) 7_665 ?
O6 C1 1.234(6) . ?
O4 C10 1.230(7) . ?
C1 O7 1.237(7) . ?
C1 C2 1.540(8) . ?
C10 O5 1.248(7) . ?
C10 C11 1.528(9) . ?
O2 C6 1.225(7) . ?
C6 O3 1.248(7) . ?
C6 C7 1.527(9) . ?
C2 C5 1.466(9) . ?
C2 C3 1.512(9) . ?
C2 C4 1.533(9) . ?
C7 C8 1.464(11) . ?
C7 C9 1.489(9) . ?
C7 C15 1.548(11) . ?
C11 C14 1.502(10) . ?
C11 C13 1.524(10) . ?
C11 C12 1.532(11) . ?
N2 C17 1.133(11) . ?
N2 Fe3 2.113(7) 7_655 ?
N1 C16 1.124(10) . ?
C17 N3 1.386(13) 6_556 ?
C17 N3 1.386(13) . ?
C16 N3 1.348(12) . ?
C16 N3 1.348(12) 6_556 ?
N3 N3 1.23(3) 6_556 ?
O1S C1S 1.370(15) . ?
O1S C3S 1.611(14) . ?
C1S C2S 1.353(15) . ?
C3S C4S 1.42(2) . ?
O2S C8S 1.375(14) . ?
C8S C7S 1.399(14) . ?
