#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:02:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179167 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/28/4312808.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_4312808
loop_
_publ_author_name
'Jane Kuzelka'
'Joshua R. Farrell'
'Stephen J. Lippard'
_publ_section_title
;
 Modeling the Syn Disposition of Nitrogen Donors at the Active Sites of
 Carboxylate-Bridged Diiron Enzymes. Enforcing Dinuclearity and Kinetic
 Stability with a 1,2-Diethynylbenzene-Based Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8652
_journal_page_last               8662
_journal_paper_doi               10.1021/ic034928e
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C62 H56 Fe N0 O6'
_chemical_formula_weight         952.92
_chemical_name_systematic
;

   ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.840(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.297(6)
_cell_length_b                   11.092(2)
_cell_length_c                   15.225(3)
_cell_measurement_reflns_used    978
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      3.40
_cell_volume                     5409.3(17)
_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      203(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15913
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.842267
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6117
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0477
_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)+(0.0934P)²+1.4936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1449
_reflns_number_gt                4836
_reflns_number_total             6117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034928esi20030806_110655_4.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5409.4(17)
_cod_database_code               4312808
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 0.5000 0.61079(3) 0.7500 0.02919(13) Uani 1 2 d S . .
O1 O 0.52865(4) 0.74866(13) 0.86803(9) 0.0318(3) Uani 1 1 d . . .
O2 O 0.47796(4) 0.62823(12) 0.85909(10) 0.0332(3) Uani 1 1 d . . .
O3 O 0.45288(4) 0.48406(13) 0.67838(11) 0.0421(4) Uani 1 1 d . . .
C1 C 0.50188(5) 0.71656(16) 0.89710(12) 0.0263(4) Uani 1 1 d . . .
C2 C 0.49619(5) 0.78830(16) 0.97494(11) 0.0254(4) Uani 1 1 d . . .
C3 C 0.52839(5) 0.79458(17) 1.06872(12) 0.0282(4) Uani 1 1 d . . .
C4 C 0.52283(6) 0.86594(18) 1.13810(13) 0.0323(4) Uani 1 1 d . . .
H4 H 0.5450(7) 0.8707(18) 1.2051(16) 0.033(5) Uiso 1 1 d . . .
C5 C 0.48653(6) 0.93146(19) 1.11466(13) 0.0337(4) Uani 1 1 d . . .
H5 H 0.4840(6) 0.981(2) 1.1629(16) 0.033(5) Uiso 1 1 d . . .
C6 C 0.45536(6) 0.92617(18) 1.02232(13) 0.0312(4) Uani 1 1 d . . .
H6 H 0.4316(7) 0.976(2) 1.0030(15) 0.033(5) Uiso 1 1 d . . .
C7 C 0.45897(5) 0.85407(17) 0.95077(12) 0.0272(4) Uani 1 1 d . . .
C8 C 0.42413(5) 0.85871(17) 0.85185(12) 0.0276(4) Uani 1 1 d . . .
C9 C 0.38285(6) 0.86446(18) 0.84106(14) 0.0323(4) Uani 1 1 d . . .
H9 H 0.3764(7) 0.857(2) 0.8958(18) 0.043(6) Uiso 1 1 d . . .
C10 C 0.35006(6) 0.88363(19) 0.75076(14) 0.0355(4) Uani 1 1 d . . .
H10 H 0.3219(8) 0.895(2) 0.7487(17) 0.045(6) Uiso 1 1 d . . .
C11 C 0.35698(5) 0.89619(18) 0.66796(13) 0.0335(4) Uani 1 1 d . A .
C12 C 0.39795(6) 0.88464(18) 0.67866(14) 0.0329(4) Uani 1 1 d . . .
H12 H 0.4040(7) 0.888(2) 0.6295(18) 0.041(6) Uiso 1 1 d . . .
C13 C 0.43081(5) 0.86740(17) 0.76836(13) 0.0292(4) Uani 1 1 d . . .
H13 H 0.4616(7) 0.862(2) 0.7794(16) 0.038(6) Uiso 1 1 d . . .
C14 C 0.56852(5) 0.72741(17) 1.09925(12) 0.0296(4) Uani 1 1 d . . .
C15 C 0.60634(6) 0.7884(2) 1.14355(14) 0.0375(4) Uani 1 1 d . . .
H15 H 0.6050(7) 0.870(2) 1.1458(17) 0.037(6) Uiso 1 1 d . . .
C16 C 0.64389(6) 0.7268(2) 1.17803(15) 0.0410(5) Uani 1 1 d . . .
H16 H 0.6673(8) 0.772(2) 1.2020(18) 0.055(7) Uiso 1 1 d . . .
C17 C 0.64580(6) 0.6026(2) 1.17148(14) 0.0368(5) Uani 1 1 d . . .
C18 C 0.60782(6) 0.5422(2) 1.12771(14) 0.0356(4) Uani 1 1 d . . .
H18 H 0.6077(7) 0.459(2) 1.1229(17) 0.044(6) Uiso 1 1 d . . .
C19 C 0.57005(6) 0.60265(18) 1.09175(13) 0.0316(4) Uani 1 1 d . . .
H19 H 0.5445(7) 0.560(2) 1.0656(16) 0.041(6) Uiso 1 1 d . . .
C20 C 0.32151(6) 0.9216(3) 0.56828(15) 0.0492(6) Uani 1 1 d . . .
C21 C 0.68694(6) 0.5315(2) 1.21215(16) 0.0480(6) Uani 1 1 d . . .
C22 C 0.33234(14) 1.0282(8) 0.5234(5) 0.133(4) Uani 0.811(9) 1 d PU A 1
C22A C 0.2970(7) 1.044(2) 0.5876(14) 0.123(11) Uani 0.189(9) 1 d PU A 2
C23 C 0.31665(17) 0.8070(6) 0.5049(3) 0.106(2) Uani 0.811(9) 1 d PU A 1
C23A C 0.2909(7) 0.826(2) 0.5401(15) 0.120(12) Uani 0.189(9) 1 d PU A 2
C24 C 0.28003(10) 0.9413(6) 0.5736(3) 0.083(2) Uani 0.811(9) 1 d PU A 1
C24A C 0.3409(7) 0.963(3) 0.4960(12) 0.113(10) Uani 0.189(9) 1 d PU A 2
C25 C 0.68723(9) 0.4449(3) 1.2914(2) 0.0651(8) Uani 1 1 d . . .
H25A H 0.7172(10) 0.403(3) 1.325(2) 0.075(9) Uiso 1 1 d . . .
H25B H 0.6906(9) 0.495(3) 1.356(2) 0.074(9) Uiso 1 1 d . . .
H25C H 0.6585(12) 0.379(3) 1.264(3) 0.108(13) Uiso 1 1 d . . .
C26 C 0.72515(8) 0.6147(3) 1.2563(3) 0.0699(9) Uani 1 1 d . . .
H26A H 0.7534(12) 0.564(4) 1.285(3) 0.103(11) Uiso 1 1 d . . .
H26B H 0.7274(10) 0.658(3) 1.324(3) 0.094(11) Uiso 1 1 d . . .
H26C H 0.7249(8) 0.678(3) 1.204(2) 0.064(8) Uiso 1 1 d . . .
C27 C 0.69065(10) 0.4583(4) 1.1306(3) 0.0755(10) Uani 1 1 d . . .
H27A H 0.7181(12) 0.424(4) 1.153(3) 0.101(11) Uiso 1 1 d . . .
H27B H 0.6655(10) 0.399(3) 1.101(2) 0.069(9) Uiso 1 1 d . . .
H27C H 0.6876(13) 0.518(4) 1.068(3) 0.126(15) Uiso 1 1 d . . .
C28 C 0.40980(6) 0.5171(2) 0.64765(17) 0.0444(5) Uani 1 1 d . . .
H28A H 0.4001 0.5656 0.5893 0.053 Uiso 1 1 calc R . .
H28B H 0.4058 0.5616 0.6979 0.053 Uiso 1 1 calc R . .
C29 C 0.38742(7) 0.3978(2) 0.62886(18) 0.0518(6) Uani 1 1 d . . .
H29A H 0.3588 0.4058 0.5808 0.062 Uiso 1 1 calc R . .
H29B H 0.3873 0.3650 0.6878 0.062 Uiso 1 1 calc R . .
C30 C 0.41265(8) 0.3191(2) 0.59185(18) 0.0529(6) Uani 1 1 d . . .
H30A H 0.4145 0.2374 0.6161 0.064 Uiso 1 1 calc R . .
H30B H 0.4000 0.3170 0.5217 0.064 Uiso 1 1 calc R . .
C31 C 0.45496(8) 0.3767(2) 0.6295(2) 0.0634(8) Uani 1 1 d . . .
H31A H 0.4759 0.3225 0.6737 0.076 Uiso 1 1 calc R . .
H31B H 0.4624 0.3955 0.5764 0.076 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'
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
O3 Fe1 O3 95.93(8) . 2_656 ?
O3 Fe1 O2 89.81(5) . . ?
O3 Fe1 O2 97.22(6) 2_656 . ?
O3 Fe1 O2 97.22(6) . 2_656 ?
O3 Fe1 O2 89.81(5) 2_656 2_656 ?
O2 Fe1 O2 169.52(7) . 2_656 ?
O3 Fe1 O1 149.54(5) . . ?
O3 Fe1 O1 92.76(6) 2_656 . ?
O2 Fe1 O1 60.10(5) . . ?
O2 Fe1 O1 111.98(5) 2_656 . ?
O3 Fe1 O1 92.76(6) . 2_656 ?
O3 Fe1 O1 149.54(5) 2_656 2_656 ?
O2 Fe1 O1 111.98(5) . 2_656 ?
O2 Fe1 O1 60.10(5) 2_656 2_656 ?
O1 Fe1 O1 94.38(7) . 2_656 ?
O3 Fe1 C1 119.73(6) . . ?
O3 Fe1 C1 97.56(6) 2_656 . ?
O2 Fe1 C1 30.29(5) . . ?
O2 Fe1 C1 141.07(6) 2_656 . ?
O1 Fe1 C1 29.91(5) . . ?
O1 Fe1 C1 103.30(5) 2_656 . ?
O3 Fe1 C1 97.56(6) . 2_656 ?
O3 Fe1 C1 119.73(6) 2_656 2_656 ?
O2 Fe1 C1 141.07(6) . 2_656 ?
O2 Fe1 C1 30.29(5) 2_656 2_656 ?
O1 Fe1 C1 103.30(5) . 2_656 ?
O1 Fe1 C1 29.91(5) 2_656 2_656 ?
C1 Fe1 C1 124.12(8) . 2_656 ?
C1 O1 Fe1 86.35(10) . . ?
C1 O2 Fe1 92.00(10) . . ?
C31 O3 C28 108.83(16) . . ?
C31 O3 Fe1 128.95(14) . . ?
C28 O3 Fe1 119.82(12) . . ?
O1 C1 O2 121.14(16) . . ?
O1 C1 C2 119.79(16) . . ?
O2 C1 C2 118.98(15) . . ?
O1 C1 Fe1 63.74(9) . . ?
O2 C1 Fe1 57.71(9) . . ?
C2 C1 Fe1 170.71(11) . . ?
C3 C2 C7 120.47(16) . . ?
C3 C2 C1 120.45(15) . . ?
C7 C2 C1 118.99(14) . . ?
C4 C3 C2 119.07(17) . . ?
C4 C3 C14 117.63(15) . . ?
C2 C3 C14 123.30(16) . . ?
C5 C4 C3 120.75(16) . . ?
C6 C5 C4 119.87(18) . . ?
C5 C6 C7 121.65(18) . . ?
C6 C7 C2 118.17(15) . . ?
C6 C7 C8 117.38(16) . . ?
C2 C7 C8 124.32(16) . . ?
C13 C8 C9 117.29(16) . . ?
C13 C8 C7 122.72(16) . . ?
C9 C8 C7 119.78(16) . . ?
C10 C9 C8 121.09(18) . . ?
C11 C10 C9 121.45(17) . . ?
C10 C11 C12 117.07(17) . . ?
C10 C11 C20 122.33(17) . . ?
C12 C11 C20 120.59(18) . . ?
C13 C12 C11 121.82(18) . . ?
C12 C13 C8 121.18(17) . . ?
C19 C14 C15 117.44(18) . . ?
C19 C14 C3 122.39(16) . . ?
C15 C14 C3 120.01(18) . . ?
C16 C15 C14 121.0(2) . . ?
C15 C16 C17 122.11(19) . . ?
C16 C17 C18 116.55(18) . . ?
C16 C17 C21 123.24(19) . . ?
C18 C17 C21 120.2(2) . . ?
C19 C18 C17 122.0(2) . . ?
C18 C19 C14 120.91(18) . . ?
C23A C20 C22 138.5(7) . . ?
C23A C20 C24 60.2(15) . . ?
C22 C20 C24 110.4(4) . . ?
C23A C20 C11 110.9(7) . . ?
C22 C20 C11 109.8(3) . . ?
C24 C20 C11 112.3(2) . . ?
C23A C20 C23 49.1(15) . . ?
C22 C20 C23 110.2(5) . . ?
C24 C20 C23 107.0(3) . . ?
C11 C20 C23 107.1(3) . . ?
C23A C20 C24A 119.5(17) . . ?
C22 C20 C24A 35.5(11) . . ?
C24 C20 C24A 134.6(7) . . ?
C11 C20 C24A 109.2(8) . . ?
C23 C20 C24A 77.0(13) . . ?
C23A C20 C22A 105.5(18) . . ?
C22 C20 C22A 72.0(12) . . ?
C24 C20 C22A 45.9(11) . . ?
C11 C20 C22A 103.8(6) . . ?
C23 C20 C22A 145.7(7) . . ?
C24A C20 C22A 106.5(15) . . ?
C27 C21 C17 109.45(19) . . ?
C27 C21 C26 108.3(2) . . ?
C17 C21 C26 112.1(2) . . ?
C27 C21 C25 109.2(3) . . ?
C17 C21 C25 109.30(18) . . ?
C26 C21 C25 108.5(2) . . ?
O3 C28 C29 103.71(18) . . ?
C28 C29 C30 103.50(18) . . ?
C31 C30 C29 105.03(19) . . ?
O3 C31 C30 107.1(2) . . ?
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 O3 2.0993(14) . ?
Fe1 O3 2.0993(14) 2_656 ?
Fe1 O2 2.1182(14) . ?
Fe1 O2 2.1182(14) 2_656 ?
Fe1 O1 2.2503(13) . ?
Fe1 O1 2.2503(13) 2_656 ?
Fe1 C1 2.5043(18) . ?
Fe1 C1 2.5043(18) 2_656 ?
O1 C1 1.251(2) . ?
O2 C1 1.264(2) . ?
O3 C31 1.423(3) . ?
O3 C28 1.438(2) . ?
C1 C2 1.509(2) . ?
C2 C3 1.404(2) . ?
C2 C7 1.410(2) . ?
C3 C4 1.398(3) . ?
C3 C14 1.492(2) . ?
C4 C5 1.383(3) . ?
C5 C6 1.375(3) . ?
C6 C7 1.400(3) . ?
C7 C8 1.492(2) . ?
C8 C13 1.390(3) . ?
C8 C9 1.397(3) . ?
C9 C10 1.392(3) . ?
C10 C11 1.388(3) . ?
C11 C12 1.391(3) . ?
C11 C20 1.534(3) . ?
C12 C13 1.384(3) . ?
C14 C19 1.391(3) . ?
C14 C15 1.392(3) . ?
C15 C16 1.384(3) . ?
C16 C17 1.385(3) . ?
C17 C18 1.393(3) . ?
C17 C21 1.536(3) . ?
C18 C19 1.384(3) . ?
C20 C23A 1.442(18) . ?
C20 C22 1.494(6) . ?
C20 C24 1.516(4) . ?
C20 C23 1.561(6) . ?
C20 C24A 1.59(2) . ?
C20 C22A 1.70(2) . ?
C21 C27 1.535(4) . ?
C21 C26 1.536(4) . ?
C21 C25 1.539(4) . ?
C28 C29 1.505(3) . ?
C29 C30 1.515(4) . ?
C30 C31 1.499(3) . ?
