#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:01:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179713 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/15/7001508.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_7001508
loop_
_publ_author_name
'Ballmann, Joachim'
'Sun, Xianru'
'Dechert, Sebastian'
'Schneider, Benjamin'
'Meyer, Franc'
_publ_section_title
;
 A convenient ligand exchange pathway to [2Fe--2S] ferredoxin analogues
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              4908
_journal_page_last               4917
_journal_paper_doi               10.1039/b901242g
_journal_year                    2009
_chemical_formula_moiety         'C32 H36 Fe2 S6 2-, 2(C8 H20 N +)'
_chemical_formula_sum            'C48 H76 Fe2 N2 S6'
_chemical_formula_weight         985.17
_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                 105.673(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8071(4)
_cell_length_b                   16.8841(4)
_cell_length_c                   13.2627(4)
_cell_measurement_reflns_used    30798
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      2.00
_cell_volume                     2545.64(13)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30798
_diffrn_reflns_theta_full        26.72
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.7829
_exptl_absorpt_correction_T_min  0.5982
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0323P)²+1.3634P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                4954
_reflns_number_total             5385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901242g.txt
_cod_data_source_block           4c-ab44
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7001508
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
Fe1 Fe 0.478754(18) 0.565043(12) 0.436997(16) 0.02104(6) Uani 1 1 d . . .
S1 S 0.53058(4) 0.55989(2) 0.60913(3) 0.02592(9) Uani 1 1 d . . .
S2 S 0.30374(3) 0.63525(2) 0.38994(3) 0.02764(9) Uani 1 1 d . . .
S3 S 0.60552(3) 0.63542(2) 0.36599(3) 0.02714(9) Uani 1 1 d . . .
C1 C 0.26914(14) 0.64508(9) 0.25105(12) 0.0271(3) Uani 1 1 d . . .
C2 C 0.20859(14) 0.58462(10) 0.18588(13) 0.0304(3) Uani 1 1 d . . .
C3 C 0.17972(16) 0.59478(12) 0.07750(14) 0.0391(4) Uani 1 1 d . . .
H3 H 0.1421 0.5541 0.0339 0.080 Uiso 1 1 calc R . .
C4 C 0.20620(18) 0.66455(13) 0.03390(14) 0.0440(4) Uani 1 1 d . . .
H4 H 0.1858 0.6708 -0.0384 0.080 Uiso 1 1 calc R . .
C5 C 0.26274(17) 0.72439(11) 0.09821(15) 0.0401(4) Uani 1 1 d . . .
H5 H 0.2783 0.7717 0.0685 0.080 Uiso 1 1 calc R . .
C6 C 0.29741(14) 0.71617(10) 0.20686(14) 0.0316(3) Uani 1 1 d . . .
C7 C 0.17206(16) 0.50950(10) 0.22983(14) 0.0363(4) Uani 1 1 d . . .
H7A H 0.2408 0.4815 0.2687 0.080 Uiso 1 1 calc R . .
H7B H 0.1284 0.4768 0.1735 0.080 Uiso 1 1 calc R . .
H7C H 0.1238 0.5224 0.2753 0.080 Uiso 1 1 calc R . .
C8 C 0.36297(17) 0.78206(10) 0.27365(16) 0.0401(4) Uani 1 1 d . . .
H8A H 0.3656 0.8273 0.2305 0.080 Uiso 1 1 calc R . .
H8B H 0.4416 0.7650 0.3074 0.080 Uiso 1 1 calc R . .
H8C H 0.3236 0.7960 0.3257 0.080 Uiso 1 1 calc R . .
C9 C 0.67924(13) 0.56888(8) 0.30192(12) 0.0233(3) Uani 1 1 d . . .
C10 C 0.63897(13) 0.55857(9) 0.19268(12) 0.0261(3) Uani 1 1 d . . .
C11 C 0.70737(15) 0.51484(10) 0.14165(12) 0.0301(3) Uani 1 1 d . . .
H11 H 0.6816 0.5080 0.0695 0.080 Uiso 1 1 calc R . .
C12 C 0.81319(15) 0.48143(9) 0.19715(13) 0.0311(3) Uani 1 1 d . . .
H12 H 0.8598 0.4545 0.1620 0.080 Uiso 1 1 calc R . .
C13 C 0.84897(14) 0.48846(9) 0.30503(13) 0.0283(3) Uani 1 1 d . . .
H13 H 0.9187 0.4645 0.3421 0.080 Uiso 1 1 calc R . .
C14 C 0.78283(13) 0.53059(9) 0.35928(12) 0.0245(3) Uani 1 1 d . . .
C15 C 0.52300(14) 0.59275(11) 0.13166(13) 0.0336(4) Uani 1 1 d . . .
H15A H 0.5053 0.5748 0.0604 0.080 Uiso 1 1 calc R . .
H15B H 0.5276 0.6495 0.1333 0.080 Uiso 1 1 calc R . .
H15C H 0.4622 0.5757 0.1623 0.080 Uiso 1 1 calc R . .
C16 C 0.81989(14) 0.53305(10) 0.47675(12) 0.0317(3) Uani 1 1 d . . .
H16A H 0.8208 0.5870 0.4999 0.080 Uiso 1 1 calc R . .
H16B H 0.8972 0.5108 0.5019 0.080 Uiso 1 1 calc R . .
H16C H 0.7654 0.5030 0.5036 0.080 Uiso 1 1 calc R . .
N1 N 0.43892(11) 0.74389(7) 0.78431(9) 0.0222(2) Uani 1 1 d . . .
C21 C 0.34506(13) 0.68467(9) 0.73138(13) 0.0278(3) Uani 1 1 d . . .
H21A H 0.3612 0.6667 0.6672 0.080 Uiso 1 1 calc R . .
H21B H 0.3502 0.6390 0.7768 0.080 Uiso 1 1 calc R . .
C22 C 0.22077(14) 0.71696(10) 0.70545(14) 0.0345(4) Uani 1 1 d . . .
H22A H 0.2030 0.7336 0.7687 0.080 Uiso 1 1 calc R . .
H22B H 0.1665 0.6764 0.6722 0.080 Uiso 1 1 calc R . .
H22C H 0.2141 0.7614 0.6590 0.080 Uiso 1 1 calc R . .
C23 C 0.43052(15) 0.81908(9) 0.71982(13) 0.0298(3) Uani 1 1 d . . .
H23A H 0.3604 0.8478 0.7232 0.080 Uiso 1 1 calc R . .
H23B H 0.4978 0.8523 0.7514 0.080 Uiso 1 1 calc R . .
C24 C 0.42609(19) 0.80599(12) 0.60561(14) 0.0437(4) Uani 1 1 d . . .
H24A H 0.4950 0.7777 0.6011 0.080 Uiso 1 1 calc R . .
H24B H 0.4231 0.8563 0.5712 0.080 Uiso 1 1 calc R . .
H24C H 0.3573 0.7758 0.5723 0.080 Uiso 1 1 calc R . .
C25 C 0.55984(13) 0.70754(9) 0.79658(12) 0.0265(3) Uani 1 1 d . . .
H25A H 0.5662 0.6920 0.7279 0.080 Uiso 1 1 calc R . .
H25B H 0.6188 0.7479 0.8231 0.080 Uiso 1 1 calc R . .
C26 C 0.58788(15) 0.63641(10) 0.86819(13) 0.0335(4) Uani 1 1 d . . .
H26A H 0.5892 0.6520 0.9381 0.080 Uiso 1 1 calc R . .
H26B H 0.6634 0.6156 0.8677 0.080 Uiso 1 1 calc R . .
H26C H 0.5288 0.5965 0.8442 0.080 Uiso 1 1 calc R . .
C27 C 0.42102(14) 0.76469(10) 0.89023(12) 0.0291(3) Uani 1 1 d . . .
H27A H 0.3452 0.7904 0.8793 0.080 Uiso 1 1 calc R . .
H27B H 0.4187 0.7160 0.9285 0.080 Uiso 1 1 calc R . .
C28 C 0.51448(16) 0.81799(13) 0.95653(14) 0.0422(4) Uani 1 1 d . . .
H28A H 0.5902 0.7935 0.9670 0.080 Uiso 1 1 calc R . .
H28B H 0.4989 0.8265 1.0231 0.080 Uiso 1 1 calc R . .
H28C H 0.5138 0.8679 0.9217 0.080 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'
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
S1 Fe1 S1 103.335(14) 3_666 . ?
S1 Fe1 S3 111.837(16) 3_666 . ?
S1 Fe1 S3 114.556(17) . . ?
S1 Fe1 S2 116.328(17) 3_666 . ?
S1 Fe1 S2 106.116(16) . . ?
S3 Fe1 S2 104.879(16) . . ?
S1 Fe1 Fe1 51.815(12) 3_666 3_666 ?
S1 Fe1 Fe1 51.520(12) . 3_666 ?
S3 Fe1 Fe1 129.417(16) . 3_666 ?
S2 Fe1 Fe1 125.524(15) . 3_666 ?
Fe1 S1 Fe1 76.665(14) 3_666 . ?
C1 S2 Fe1 105.34(5) . . ?
C9 S3 Fe1 109.06(5) . . ?
C2 C1 C6 120.03(15) . . ?
C2 C1 S2 120.35(12) . . ?
C6 C1 S2 119.53(13) . . ?
C3 C2 C1 119.17(15) . . ?
C3 C2 C7 119.09(16) . . ?
C1 C2 C7 121.73(15) . . ?
C4 C3 C2 120.99(18) . . ?
C5 C4 C3 119.55(17) . . ?
C4 C5 C6 121.75(16) . . ?
C5 C6 C1 118.44(16) . . ?
C5 C6 C8 119.80(15) . . ?
C1 C6 C8 121.76(15) . . ?
C10 C9 C14 120.05(13) . . ?
C10 C9 S3 119.90(11) . . ?
C14 C9 S3 119.90(11) . . ?
C11 C10 C9 119.02(14) . . ?
C11 C10 C15 120.23(14) . . ?
C9 C10 C15 120.74(14) . . ?
C12 C11 C10 120.91(15) . . ?
C13 C12 C11 119.58(14) . . ?
C12 C13 C14 121.42(15) . . ?
C13 C14 C9 118.77(14) . . ?
C13 C14 C16 120.25(14) . . ?
C9 C14 C16 120.96(13) . . ?
C21 N1 C27 108.30(11) . . ?
C21 N1 C23 111.22(12) . . ?
C27 N1 C23 108.89(11) . . ?
C21 N1 C25 109.31(11) . . ?
C27 N1 C25 110.83(11) . . ?
C23 N1 C25 108.30(11) . . ?
C22 C21 N1 114.18(12) . . ?
C24 C23 N1 114.82(13) . . ?
C26 C25 N1 115.32(12) . . ?
C28 C27 N1 114.50(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 S1 2.1908(4) 3_666 ?
Fe1 S1 2.1998(4) . ?
Fe1 S3 2.3024(4) . ?
Fe1 S2 2.3169(4) . ?
Fe1 Fe1 2.7232(4) 3_666 ?
S1 Fe1 2.1908(4) 3_666 ?
S2 C1 1.7835(16) . ?
S3 C9 1.7724(15) . ?
C1 C2 1.402(2) . ?
C1 C6 1.415(2) . ?
C2 C3 1.395(2) . ?
C2 C7 1.507(2) . ?
C3 C4 1.385(3) . ?
C4 C5 1.373(3) . ?
C5 C6 1.395(2) . ?
C6 C8 1.500(3) . ?
C9 C10 1.408(2) . ?
C9 C14 1.411(2) . ?
C10 C11 1.397(2) . ?
C10 C15 1.505(2) . ?
C11 C12 1.387(2) . ?
C12 C13 1.383(2) . ?
C13 C14 1.392(2) . ?
C14 C16 1.501(2) . ?
N1 C21 1.5167(18) . ?
N1 C27 1.5171(18) . ?
N1 C23 1.5189(19) . ?
N1 C25 1.5218(18) . ?
C21 C22 1.515(2) . ?
C23 C24 1.518(2) . ?
C25 C26 1.511(2) . ?
C27 C28 1.509(2) . ?
