#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:40:04 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180150 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/47/7104744.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_7104744
loop_
_publ_author_name
'Duriska, Martin B'
'Neville, Suzanne M'
'Batten, Stuart R'
_publ_section_title
;
 Variable length ligands: a new class of bridging ligands for
 supramolecular chemistry and crystal engineering.
;
_journal_issue                   37
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5579
_journal_page_last               5581
_journal_paper_doi               10.1039/b910994c
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C28 H38 Fe N8 O4 S4, 2(C H4 O)'
_chemical_formula_sum            'C30 H46 Fe N8 O6 S4'
_chemical_formula_weight         798.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '9 November 2005'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.378(1)
_cell_angle_beta                 94.538(1)
_cell_angle_gamma                96.319(1)
_cell_formula_units_Z            1
_cell_length_a                   9.8825(8)
_cell_length_b                   10.0056(8)
_cell_length_c                   10.1091(6)
_cell_measurement_reflns_used    254
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.396
_cell_measurement_theta_min      2.765
_cell_volume                     960.89(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker X8 Apex II'
_diffrn_measurement_method       'phi and omega 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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8845
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.9075
_exptl_absorpt_correction_T_min  0.8793
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0417
_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)+(0.0506P)²+0.8027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                3447
_reflns_number_total             3927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910994c.txt
_cod_data_source_block           D
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7104744
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.5000 0.5000 0.5000 0.01963(13) Uani 1 2 d S . .
S1 S 0.30948(7) 0.55546(6) 0.05202(6) 0.03281(17) Uani 1 1 d . . .
O1 O 0.34357(17) 1.06187(16) 1.03464(16) 0.0261(4) Uani 1 1 d . . .
N1 N 0.1752(2) 1.1083(2) 0.8050(2) 0.0241(4) Uani 1 1 d . . .
C1 C 0.3463(3) 1.0806(3) 1.1790(2) 0.0307(5) Uani 1 1 d . . .
H1A H 0.2993 1.1609 1.2179 0.037 Uiso 1 1 calc R . .
H1B H 0.4421 1.0985 1.2220 0.037 Uiso 1 1 calc R . .
H1 H 0.155(3) 1.115(3) 0.717(3) 0.037 Uiso 1 1 d . . .
S2 S 0.10697(6) 0.15048(6) 0.50090(6) 0.02883(16) Uani 1 1 d . . .
O2 O -0.13571(17) 1.06578(17) 0.85037(17) 0.0279(4) Uani 1 1 d . . .
N2 N 0.37437(19) 0.65722(19) 0.60078(19) 0.0220(4) Uani 1 1 d . . .
C2 C 0.3719(3) 1.1868(3) 0.9939(3) 0.0317(6) Uani 1 1 d . . .
H2A H 0.4714 1.2197 1.0114 0.038 Uiso 1 1 calc R . .
H2B H 0.3231 1.2589 1.0470 0.038 Uiso 1 1 calc R . .
O3 O 0.0196(4) 0.4308(6) 0.1624(5) 0.167(3) Uani 1 1 d . . .
H3 H 0.0825 0.4712 0.1290 0.201 Uiso 1 1 calc R . .
N3 N 0.4202(2) 0.5192(2) 0.3028(2) 0.0288(5) Uani 1 1 d . . .
C3 C 0.3257(2) 1.1614(3) 0.8441(3) 0.0286(5) Uani 1 1 d . . .
H3A H 0.3797 1.0933 0.7926 0.034 Uiso 1 1 calc R . .
H3B H 0.3461 1.2490 0.8156 0.034 Uiso 1 1 calc R . .
N4 N 0.3380(2) 0.3398(2) 0.4997(2) 0.0293(5) Uani 1 1 d . . .
C4 C 0.0866(3) 1.2026(3) 0.8865(3) 0.0329(6) Uani 1 1 d . . .
H4A H 0.1268 1.2999 0.8965 0.040 Uiso 1 1 calc R . .
H4B H 0.0874 1.1856 0.9792 0.040 Uiso 1 1 calc R . .
C5 C -0.0605(3) 1.1838(3) 0.8233(3) 0.0349(6) Uani 1 1 d . . .
H5A H -0.1033 1.2673 0.8613 0.042 Uiso 1 1 calc R . .
H5B H -0.0626 1.1726 0.7232 0.042 Uiso 1 1 calc R . .
C6 C -0.2752(3) 1.0482(3) 0.7942(3) 0.0304(5) Uani 1 1 d . . .
H6A H -0.2806 1.0408 0.6945 0.037 Uiso 1 1 calc R . .
H6B H -0.3197 1.1290 0.8369 0.037 Uiso 1 1 calc R . .
C7 C 0.1333(2) 0.9588(2) 0.8073(2) 0.0251(5) Uani 1 1 d . . .
H7A H 0.1355 0.9525 0.9037 0.030 Uiso 1 1 calc R . .
H7B H 0.0377 0.9302 0.7647 0.030 Uiso 1 1 calc R . .
C8 C 0.2224(2) 0.8585(2) 0.7345(2) 0.0239(5) Uani 1 1 d . . .
C9 C 0.2628(3) 0.8587(3) 0.6059(3) 0.0293(5) Uani 1 1 d . . .
H9 H 0.2381 0.9271 0.5605 0.035 Uiso 1 1 calc R . .
C10 C 0.3396(3) 0.7581(2) 0.5441(2) 0.0274(5) Uani 1 1 d . . .
H10 H 0.3687 0.7613 0.4574 0.033 Uiso 1 1 calc R . .
C11 C 0.3339(2) 0.6564(2) 0.7249(2) 0.0265(5) Uani 1 1 d . . .
H11 H 0.3568 0.5847 0.7665 0.032 Uiso 1 1 calc R . .
C12 C 0.2605(2) 0.7554(2) 0.7947(3) 0.0266(5) Uani 1 1 d . . .
H12 H 0.2364 0.7526 0.8833 0.032 Uiso 1 1 calc R . .
C13 C 0.3763(2) 0.5351(2) 0.1987(2) 0.0246(5) Uani 1 1 d . . .
C14 C 0.2434(2) 0.2616(2) 0.5016(2) 0.0226(5) Uani 1 1 d . . .
C15 C 0.0402(4) 0.4751(5) 0.3076(5) 0.0805(13) Uani 1 1 d . . .
H15A H -0.0294 0.4230 0.3467 0.121 Uiso 1 1 calc R . .
H15B H 0.0329 0.5743 0.3360 0.121 Uiso 1 1 calc R . .
H15C H 0.1315 0.4583 0.3401 0.121 Uiso 1 1 calc R . .
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'
S S 0.1246 0.1234 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Fe1 N4 180.00(8) . 2_666 ?
N4 Fe1 N3 91.72(8) . . ?
N4 Fe1 N3 88.28(8) 2_666 . ?
N4 Fe1 N3 88.28(8) . 2_666 ?
N4 Fe1 N3 91.72(8) 2_666 2_666 ?
N3 Fe1 N3 180.000(1) . 2_666 ?
N4 Fe1 N2 89.63(7) . . ?
N4 Fe1 N2 90.37(7) 2_666 . ?
N3 Fe1 N2 90.47(7) . . ?
N3 Fe1 N2 89.53(7) 2_666 . ?
N4 Fe1 N2 90.37(7) . 2_666 ?
N4 Fe1 N2 89.63(7) 2_666 2_666 ?
N3 Fe1 N2 89.53(7) . 2_666 ?
N3 Fe1 N2 90.47(7) 2_666 2_666 ?
N2 Fe1 N2 180.000(1) . 2_666 ?
C2 O1 C1 113.55(18) . . ?
C4 N1 C3 111.55(18) . . ?
C4 N1 C7 111.11(19) . . ?
C3 N1 C7 115.52(18) . . ?
C4 N1 H1 104.0(18) . . ?
C3 N1 H1 106.9(19) . . ?
C7 N1 H1 106.9(19) . . ?
O1 C1 C6 108.04(19) . 2_577 ?
O1 C1 H1A 110.1 . . ?
C6 C1 H1A 110.1 2_577 . ?
O1 C1 H1B 110.1 . . ?
C6 C1 H1B 110.1 2_577 . ?
H1A C1 H1B 108.4 . . ?
C5 O2 C6 111.36(19) . . ?
C10 N2 C11 117.26(19) . . ?
C10 N2 Fe1 121.98(15) . . ?
C11 N2 Fe1 120.72(15) . . ?
O1 C2 C3 108.73(19) . . ?
O1 C2 H2A 109.9 . . ?
C3 C2 H2A 109.9 . . ?
O1 C2 H2B 109.9 . . ?
C3 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
C15 O3 H3 109.5 . . ?
C13 N3 Fe1 177.19(19) . . ?
C2 C3 N1 114.5(2) . . ?
C2 C3 H3A 108.6 . . ?
N1 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
N1 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C14 N4 Fe1 174.40(19) . . ?
N1 C4 C5 114.0(2) . . ?
N1 C4 H4A 108.8 . . ?
C5 C4 H4A 108.8 . . ?
N1 C4 H4B 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.6 . . ?
O2 C5 C4 110.6(2) . . ?
O2 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
O2 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
O2 C6 C1 108.4(2) . 2_577 ?
O2 C6 H6A 110.0 . . ?
C1 C6 H6A 110.0 2_577 . ?
O2 C6 H6B 110.0 . . ?
C1 C6 H6B 110.0 2_577 . ?
H6A C6 H6B 108.4 . . ?
C8 C7 N1 114.39(19) . . ?
C8 C7 H7A 108.7 . . ?
N1 C7 H7A 108.7 . . ?
C8 C7 H7B 108.7 . . ?
N1 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C12 C8 C9 117.5(2) . . ?
C12 C8 C7 118.7(2) . . ?
C9 C8 C7 123.7(2) . . ?
C8 C9 C10 119.5(2) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 123.1(2) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C11 C12 123.0(2) . . ?
N2 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C8 C12 C11 119.5(2) . . ?
C8 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
N3 C13 S1 178.3(2) . . ?
N4 C14 S2 178.7(2) . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
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 N4 2.137(2) . ?
Fe1 N4 2.137(2) 2_666 ?
Fe1 N3 2.144(2) . ?
Fe1 N3 2.144(2) 2_666 ?
Fe1 N2 2.2232(18) . ?
Fe1 N2 2.2232(18) 2_666 ?
S1 C13 1.640(3) . ?
O1 C2 1.411(3) . ?
O1 C1 1.425(3) . ?
N1 C4 1.507(3) . ?
N1 C3 1.512(3) . ?
N1 C7 1.514(3) . ?
N1 H1 0.91(3) . ?
C1 C6 1.491(4) 2_577 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
S2 C14 1.649(2) . ?
O2 C5 1.418(3) . ?
O2 C6 1.425(3) . ?
N2 C10 1.333(3) . ?
N2 C11 1.348(3) . ?
C2 C3 1.502(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O3 C15 1.423(6) . ?
O3 H3 0.8400 . ?
N3 C13 1.158(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N4 C14 1.156(3) . ?
C4 C5 1.514(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C1 1.491(4) 2_577 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.510(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C12 1.384(3) . ?
C8 C9 1.390(3) . ?
C9 C10 1.390(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.386(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 S1 0.84 2.55 3.372(4) 165.8 .
N1 H1 S2 0.91(3) 2.32(3) 3.227(2) 175(3) 1_565
