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#$Date: 2016-03-22 12:11:15 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178939 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/68/4116895.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_4116895
loop_
_publ_author_name
'Dongwhan Lee'
'Stephen J. Lippard'
_publ_section_title
;
 Structural and Functional Models of the Dioxygen-Activating Centers of
 Non-Heme Diiron Enzymes Ribonucleotide Reductase and Soluble Methane
 Monooxygenase
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12153
_journal_page_last               12154
_journal_paper_doi               10.1021/ja9831094
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C47 H42 Cl2 Fe O5'
_chemical_formula_weight         813.56
_chemical_name_common            '[Fe2(m-O2CAr)2(O2CAr)2(THF)2]'
_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_method           SHELXL-97
_cell_angle_alpha                107.5490(10)
_cell_angle_beta                 98.4140(10)
_cell_angle_gamma                105.7620(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7768(3)
_cell_length_b                   14.2356(3)
_cell_length_c                   15.1219(4)
_cell_measurement_temperature    188(2)
_cell_volume                     2061.87(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      188(2)
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.855
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0728
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12551
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.733806
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         8751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.384
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                5805
_reflns_number_total             8751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9831094_1.cif
_cod_data_source_block           sir
_cod_database_code               4116895
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 0.87293(4) -0.46309(3) 1.09179(3) 0.03150(13) Uani 1 1 d . . .
O1 O 0.78476(19) -0.45102(16) 1.20308(13) 0.0402(5) Uani 1 1 d . . .
O1T O 0.7376(2) -0.40411(16) 1.03202(14) 0.0467(5) Uani 1 1 d . . .
O2 O 0.95592(19) -0.50446(15) 1.22212(13) 0.0401(5) Uani 1 1 d . . .
O3 O 1.03631(19) -0.36830(15) 1.08513(14) 0.0433(5) Uani 1 1 d . . .
O4 O 0.80089(19) -0.60120(14) 0.98287(13) 0.0408(5) Uani 1 1 d . . .
C1 C 1.0479(4) 0.0088(3) 1.3230(3) 0.0687(11) Uani 1 1 d . . .
H1A H 0.9732 0.0085 1.2773 0.103 Uiso 1 1 calc R . .
H1B H 1.1232 0.0082 1.2937 0.103 Uiso 1 1 calc R . .
H1C H 1.0745 0.0718 1.3806 0.103 Uiso 1 1 calc R . .
C1C C 0.5100(3) -0.5047(3) 0.6419(2) 0.0551(8) Uani 1 1 d . . .
H1C1 H 0.4980 -0.4474 0.6914 0.083 Uiso 1 1 calc R . .
H1C2 H 0.4264 -0.5434 0.5924 0.083 Uiso 1 1 calc R . .
H1C3 H 0.5800 -0.4762 0.6131 0.083 Uiso 1 1 calc R . .
C1T C 0.6766(4) -0.4342(3) 0.9334(2) 0.0630(10) Uani 1 1 d . . .
H1TA H 0.6361 -0.5113 0.9038 0.076 Uiso 1 1 calc R . .
H1TB H 0.7432 -0.4103 0.8993 0.076 Uiso 1 1 calc R . .
C2 C 1.0064(3) -0.0865(2) 1.3498(2) 0.0501(8) Uani 1 1 d . . .
C2C C 0.5493(3) -0.5773(2) 0.68626(19) 0.0406(7) Uani 1 1 d . . .
C2T C 0.5721(4) -0.3844(3) 0.9277(3) 0.0795(13) Uani 1 1 d . . .
H2TA H 0.5746 -0.3541 0.8768 0.095 Uiso 1 1 calc R . .
H2TB H 0.4826 -0.4362 0.9137 0.095 Uiso 1 1 calc R . .
C3 C 0.9035(3) -0.1049(2) 1.3937(2) 0.0522(8) Uani 1 1 d . . .
H3B H 0.8580 -0.0557 1.4075 0.063 Uiso 1 1 calc R . .
C3C C 0.4553(3) -0.6489(2) 0.7081(2) 0.0427(7) Uani 1 1 d . . .
H3CA H 0.3659 -0.6495 0.6976 0.051 Uiso 1 1 calc R . .
C3T C 0.6036(5) -0.3011(4) 1.0230(3) 0.0851(14) Uani 1 1 d . . .
H3TA H 0.5271 -0.3124 1.0523 0.102 Uiso 1 1 calc R . .
H3TB H 0.6240 -0.2316 1.0168 0.102 Uiso 1 1 calc R . .
C4 C 0.8643(3) -0.1927(2) 1.4181(2) 0.0479(8) Uani 1 1 d . . .
H4A H 0.7939 -0.2020 1.4493 0.057 Uiso 1 1 calc R . .
C4C C 0.4874(3) -0.7195(2) 0.74480(19) 0.0387(7) Uani 1 1 d . . .
H4CA H 0.4197 -0.7693 0.7567 0.046 Uiso 1 1 calc R . .
C4T C 0.7227(4) -0.3076(3) 1.0833(2) 0.0604(10) Uani 1 1 d . . .
H4TA H 0.8032 -0.2482 1.0928 0.072 Uiso 1 1 calc R . .
H4TB H 0.7081 -0.3061 1.1467 0.072 Uiso 1 1 calc R . .
C5 C 0.9267(3) -0.2679(2) 1.39763(19) 0.0390(7) Uani 1 1 d . . .
C5C C 0.6196(3) -0.7182(2) 0.76467(18) 0.0331(6) Uani 1 1 d . . .
C6 C 1.0329(3) -0.2482(2) 1.3554(2) 0.0497(8) Uani 1 1 d . . .
H6A H 1.0803 -0.2961 1.3428 0.060 Uiso 1 1 calc R . .
C6C C 0.7149(3) -0.6442(2) 0.74589(19) 0.0363(6) Uani 1 1 d . . .
H6CA H 0.8053 -0.6403 0.7601 0.044 Uiso 1 1 calc R . .
C7 C 1.0705(3) -0.1599(3) 1.3315(2) 0.0554(9) Uani 1 1 d . . .
H7A H 1.1422 -0.1494 1.3017 0.067 Uiso 1 1 calc R . .
C7C C 0.6800(3) -0.5755(2) 0.70657(19) 0.0392(7) Uani 1 1 d . . .
H7CA H 0.7469 -0.5263 0.6934 0.047 Uiso 1 1 calc R . .
C8 C 0.8830(3) -0.3636(2) 1.4213(2) 0.0407(7) Uani 1 1 d . . .
C8C C 0.6526(3) -0.7980(2) 0.79949(18) 0.0344(6) Uani 1 1 d . . .
C9 C 0.8704(3) -0.3532(3) 1.5141(2) 0.0515(8) Uani 1 1 d . . .
H9A H 0.8871 -0.2856 1.5597 0.062 Uiso 1 1 calc R . .
C9C C 0.5757(3) -0.9030(2) 0.7527(2) 0.0442(7) Uani 1 1 d . . .
H9CA H 0.5006 -0.9221 0.7013 0.053 Uiso 1 1 calc R . .
C10 C 0.8346(4) -0.4384(3) 1.5402(2) 0.0638(10) Uani 1 1 d . . .
H10A H 0.8300 -0.4293 1.6044 0.077 Uiso 1 1 calc R . .
C10C C 0.6068(3) -0.9800(2) 0.7799(2) 0.0520(8) Uani 1 1 d . . .
H10B H 0.5529 -1.0512 0.7477 0.062 Uiso 1 1 calc R . .
C11 C 0.8050(3) -0.5378(3) 1.4745(2) 0.0555(9) Uani 1 1 d . . .
H11A H 0.7795 -0.5963 1.4939 0.067 Uiso 1 1 calc R . .
C11C C 0.7157(3) -0.9533(2) 0.8534(2) 0.0466(7) Uani 1 1 d . . .
H11B H 0.7369 -1.0069 0.8709 0.056 Uiso 1 1 calc R . .
C12 C 0.8120(3) -0.5536(2) 1.3792(2) 0.0429(7) Uani 1 1 d . . .
C12C C 0.7965(3) -0.8489(2) 0.90348(19) 0.0366(6) Uani 1 1 d . . .
C13 C 0.8536(3) -0.4648(2) 1.35462(19) 0.0358(6) Uani 1 1 d . . .
C13C C 0.7631(3) -0.7712(2) 0.87571(18) 0.0320(6) Uani 1 1 d . . .
C14 C 0.8664(3) -0.4757(2) 1.25334(19) 0.0340(6) Uani 1 1 d . . .
C14C C 0.8488(3) -0.6585(2) 0.92856(18) 0.0320(6) Uani 1 1 d . . .
C15 C 0.7706(3) -0.6621(2) 1.3095(2) 0.0425(7) Uani 1 1 d . . .
C15C C 0.9115(3) -0.8239(2) 0.9843(2) 0.0370(6) Uani 1 1 d . . .
C16 C 0.8103(3) -0.7377(3) 1.3344(3) 0.0616(9) Uani 1 1 d . . .
H16A H 0.8643 -0.7195 1.3967 0.074 Uiso 1 1 calc R . .
C16C C 1.0009(3) -0.8792(2) 0.9737(2) 0.0441(7) Uani 1 1 d . . .
H16B H 0.9905 -0.9305 0.9133 0.053 Uiso 1 1 calc R . .
C17 C 0.7721(4) -0.8394(3) 1.2696(3) 0.0696(11) Uani 1 1 d . . .
H17A H 0.8000 -0.8896 1.2889 0.084 Uiso 1 1 calc R . .
C17C C 1.1039(3) -0.8605(2) 1.0497(2) 0.0479(8) Uani 1 1 d . . .
H17B H 1.1642 -0.8983 1.0401 0.058 Uiso 1 1 calc R . .
C18 C 0.6953(4) -0.8696(3) 1.1784(3) 0.0610(10) Uani 1 1 d . . .
C18C C 1.1216(3) -0.7881(2) 1.1394(2) 0.0436(7) Uani 1 1 d . . .
C19 C 0.6617(5) -0.9792(3) 1.1053(3) 0.0910(15) Uani 1 1 d . . .
H19A H 0.7074 -1.0184 1.1330 0.136 Uiso 1 1 calc R . .
H19B H 0.6906 -0.9744 1.0479 0.136 Uiso 1 1 calc R . .
H19C H 0.5653 -1.0152 1.0882 0.136 Uiso 1 1 calc R . .
C19C C 1.2313(4) -0.7714(3) 1.2240(2) 0.0625(10) Uani 1 1 d . . .
H19D H 1.2067 -0.8301 1.2464 0.094 Uiso 1 1 calc R . .
H19E H 1.2431 -0.7062 1.2759 0.094 Uiso 1 1 calc R . .
H19F H 1.3146 -0.7670 1.2042 0.094 Uiso 1 1 calc R . .
C20 C 0.6507(3) -0.7956(3) 1.1544(3) 0.0550(8) Uani 1 1 d . . .
H20A H 0.5935 -0.8149 1.0930 0.066 Uiso 1 1 calc R . .
C20C C 1.0348(3) -0.7314(2) 1.1497(2) 0.0456(7) Uani 1 1 d . . .
H20B H 1.0465 -0.6797 1.2101 0.055 Uiso 1 1 calc R . .
C21 C 0.6883(3) -0.6937(2) 1.2187(2) 0.0457(7) Uani 1 1 d . . .
H21A H 0.6571 -0.6445 1.2002 0.055 Uiso 1 1 calc R . .
C21C C 0.9317(3) -0.7484(2) 1.0743(2) 0.0403(7) Uani 1 1 d . . .
H21B H 0.8739 -0.7084 1.0837 0.048 Uiso 1 1 calc R . .
C10S C 1.5019(5) 0.1605(5) 1.4943(3) 0.0999(17) Uani 1 1 d . . .
Cl1A Cl 1.4559(5) 0.2406(4) 1.4312(3) 0.0644(11) Uani 0.434(3) 1 d P A 1
Cl2A Cl 1.6322(4) 0.1349(3) 1.4877(3) 0.1248(15) Uani 0.434(3) 1 d P A 1
Cl1 Cl 1.3733(2) 0.06171(15) 1.48742(13) 0.0776(7) Uani 0.566(3) 1 d P A 2
Cl2 Cl 1.4624(8) 0.2383(6) 1.4330(5) 0.169(3) Uani 0.566(3) 1 d P 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'
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'
Fe Fe 0.3463 0.8444 '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'
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
O3 Fe1 O4 114.33(9) . .
O3 Fe1 O1 128.66(9) . .
O4 Fe1 O1 116.11(8) . .
O3 Fe1 O1T 98.57(9) . .
O4 Fe1 O1T 92.79(8) . .
O1 Fe1 O1T 88.02(8) . .
O3 Fe1 O2 99.84(8) . .
O4 Fe1 O2 103.69(7) . .
O1 Fe1 O2 59.52(7) . .
O1T Fe1 O2 147.40(7) . .
C14 O1 Fe1 96.21(16) . .
C1T O1T C4T 108.9(2) . .
C1T O1T Fe1 126.86(19) . .
C4T O1T Fe1 122.22(18) . .
C14 O2 Fe1 82.70(16) . .
C14C O3 Fe1 156.64(19) 2_747 .
C14C O4 Fe1 135.98(18) . .
O1T C1T C2T 106.9(3) . .
C3 C2 C7 117.0(3) . .
C3 C2 C1 121.7(3) . .
C7 C2 C1 121.2(3) . .
C3C C2C C7C 117.5(3) . .
C3C C2C C1C 120.7(3) . .
C7C C2C C1C 121.8(3) . .
C3T C2T C1T 105.6(3) . .
C2 C3 C4 122.1(3) . .
C4C C3C C2C 122.0(3) . .
C2T C3T C4T 106.5(3) . .
C3 C4 C5 120.9(3) . .
C3C C4C C5C 120.5(3) . .
O1T C4T C3T 106.0(3) . .
C6 C5 C4 117.0(3) . .
C6 C5 C8 121.7(3) . .
C4 C5 C8 121.2(3) . .
C6C C5C C4C 117.6(3) . .
C6C C5C C8C 122.0(2) . .
C4C C5C C8C 120.3(2) . .
C7 C6 C5 121.1(3) . .
C5C C6C C7C 121.0(3) . .
C6 C7 C2 121.8(3) . .
C2C C7C C6C 121.3(3) . .
C9 C8 C13 118.2(3) . .
C9 C8 C5 118.8(3) . .
C13 C8 C5 123.1(2) . .
C9C C8C C13C 118.7(3) . .
C9C C8C C5C 119.3(2) . .
C13C C8C C5C 121.9(2) . .
C10 C9 C8 121.0(3) . .
C10C C9C C8C 121.1(3) . .
C9 C10 C11 120.7(3) . .
C11C C10C C9C 119.9(3) . .
C10 C11 C12 120.9(3) . .
C10C C11C C12C 121.7(3) . .
C13 C12 C11 117.5(3) . .
C13 C12 C15 123.5(3) . .
C11 C12 C15 119.0(3) . .
C11C C12C C13C 117.9(3) . .
C11C C12C C15C 119.6(3) . .
C13C C12C C15C 122.5(2) . .
C12 C13 C8 121.6(3) . .
C12 C13 C14 120.5(2) . .
C8 C13 C14 117.9(2) . .
C8C C13C C12C 120.7(2) . .
C8C C13C C14C 120.5(2) . .
C12C C13C C14C 118.8(2) . .
O2 C14 O1 121.3(3) . .
O2 C14 C13 121.4(3) . .
O1 C14 C13 117.2(2) . .
O4 C14C O3 126.1(2) . 2_747
O4 C14C C13C 117.4(2) . .
O3 C14C C13C 116.5(2) 2_747 .
C16 C15 C21 117.1(3) . .
C16 C15 C12 120.5(3) . .
C21 C15 C12 122.3(3) . .
C16C C15C C21C 117.4(3) . .
C16C C15C C12C 120.4(3) . .
C21C C15C C12C 122.1(3) . .
C15 C16 C17 120.9(3) . .
C17C C16C C15C 121.0(3) . .
C18 C17 C16 122.0(3) . .
C16C C17C C18C 121.6(3) . .
C17 C18 C20 117.3(3) . .
C17 C18 C19 121.8(4) . .
C20 C18 C19 120.9(4) . .
C17C C18C C20C 117.6(3) . .
C17C C18C C19C 121.4(3) . .
C20C C18C C19C 121.0(3) . .
C21 C20 C18 121.0(3) . .
C21C C20C C18C 121.6(3) . .
C20 C21 C15 121.5(3) . .
C20C C21C C15C 120.8(3) . .
Cl2A C10S Cl1 114.9(4) . .
Cl2A C10S Cl2 117.7(5) . .
Cl1 C10S Cl2 114.0(4) . .
Cl2A C10S Cl1A 119.4(4) . .
Cl1 C10S Cl1A 112.6(3) . .
Cl2 C10S Cl1A 1.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O3 1.9428(19) .
Fe1 O4 2.0061(18) .
Fe1 O1 2.0363(19) .
Fe1 O1T 2.0941(19) .
Fe1 O2 2.3455(19) .
O1 C14 1.268(3) .
O1T C1T 1.419(4) .
O1T C4T 1.424(4) .
O2 C14 1.246(3) .
O3 C14C 1.260(3) 2_747
O4 C14C 1.247(3) .
C1 C2 1.503(5) .
C1C C2C 1.507(4) .
C1T C2T 1.490(5) .
C2 C3 1.379(5) .
C2 C7 1.385(5) .
C2C C3C 1.384(4) .
C2C C7C 1.387(4) .
C2T C3T 1.485(5) .
C3 C4 1.385(4) .
C3C C4C 1.380(4) .
C3T C4T 1.504(5) .
C4 C5 1.395(4) .
C4C C5C 1.406(4) .
C5 C6 1.394(4) .
C5 C8 1.484(4) .
C5C C6C 1.387(4) .
C5C C8C 1.490(4) .
C6 C7 1.383(5) .
C6C C7C 1.392(4) .
C8 C9 1.396(4) .
C8 C13 1.405(4) .
C8C C9C 1.392(4) .
C8C C13C 1.406(4) .
C9 C10 1.363(5) .
C9C C10C 1.382(4) .
C10 C11 1.380(5) .
C10C C11C 1.370(4) .
C11 C12 1.407(4) .
C11C C12C 1.401(4) .
C12 C13 1.401(4) .
C12 C15 1.484(4) .
C12C C13C 1.409(4) .
C12C C15C 1.486(4) .
C13 C14 1.523(4) .
C13C C14C 1.506(4) .
C14C O3 1.260(3) 2_747
C15 C16 1.388(4) .
C15 C21 1.389(4) .
C15C C16C 1.399(4) .
C15C C21C 1.400(4) .
C16 C17 1.389(5) .
C16C C17C 1.381(4) .
C17 C18 1.374(6) .
C17C C18C 1.383(4) .
C18 C20 1.389(5) .
C18 C19 1.523(5) .
C18C C20C 1.388(4) .
C18C C19C 1.521(4) .
C20 C21 1.388(4) .
C20C C21C 1.382(4) .
C10S Cl2A 1.552(6) .
C10S Cl1 1.649(6) .
C10S Cl2 1.741(8) .
C10S Cl1A 1.812(7) .
