#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:12:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179444 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/41/4334199.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_4334199
loop_
_publ_author_name
'Matthew B. Chambers'
'Stanislav Groysman'
'Dino Villagrán'
'Daniel G. Nocera'
_publ_section_title
;
 Iron in a Trigonal Tris(alkoxide) Ligand Environment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3159
_journal_page_last               3169
_journal_paper_doi               10.1021/ic302634q
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C38 H79 O5 Fe K'
_chemical_formula_sum            'C38 H79 Fe K O5'
_chemical_formula_weight         710.981
_chemical_name_common            Fe(Ditox)3K(THF)2
_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                 122.4540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4202(11)
_cell_length_b                   15.8786(10)
_cell_length_c                   16.7830(10)
_cell_measurement_temperature    100(2)
_cell_volume                     4142.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43649
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.9073
_exptl_absorpt_correction_T_min  0.8262
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       Block
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5364
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          6.443
_refine_ls_shift/su_mean         0.281
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0490P)²+2.2318P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                4696
_reflns_number_total             5364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302634q_si_002_03.cif
_cod_data_source_block           cmpd_4_Fe(Ditox)3K(THF)2
_cod_database_code               4334199
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 0.689386(14) 0.7500 0.02532(8) Uani 1 2 d SU . .
K1 K 0.5000 0.90108(2) 0.7500 0.04035(11) Uani 1 2 d SU . .
O1 O 0.5000 0.57437(7) 0.7500 0.0317(3) Uani 1 2 d SU . .
C1 C 0.4935(2) 0.48802(14) 0.72587(18) 0.0307(6) Uani 0.50 1 d PDU A -1
C10 C 0.4715(2) 0.4739(2) 0.6246(2) 0.0488(7) Uani 0.50 1 d PDU A -1
H10A H 0.4125 0.4928 0.5796 0.073 Uiso 0.50 1 calc PR A -1
H10B H 0.4763 0.4138 0.6149 0.073 Uiso 0.50 1 calc PR A -1
H10C H 0.5115 0.5060 0.6148 0.073 Uiso 0.50 1 calc PR A -1
C11 C 0.4147(6) 0.4530(5) 0.7302(5) 0.0372(12) Uani 0.50 1 d PDU A -1
C12 C 0.3829(6) 0.3657(5) 0.6792(7) 0.0625(18) Uani 0.50 1 d PDU A -1
H12A H 0.4316 0.3266 0.7049 0.094 Uiso 0.50 1 calc PR A -1
H12B H 0.3580 0.3730 0.6114 0.094 Uiso 0.50 1 calc PR A -1
H12C H 0.3392 0.3428 0.6895 0.094 Uiso 0.50 1 calc PR A -1
C13 C 0.33899(19) 0.5144(2) 0.6787(3) 0.0494(8) Uani 0.50 1 d PDU A -1
H13A H 0.3277 0.5263 0.6157 0.074 Uiso 0.50 1 calc PR A -1
H13B H 0.3532 0.5670 0.7147 0.074 Uiso 0.50 1 calc PR A -1
H13C H 0.2877 0.4892 0.6727 0.074 Uiso 0.50 1 calc PR A -1
C14 C 0.4332(3) 0.4428(2) 0.8295(3) 0.0548(8) Uani 0.50 1 d PDU A -1
H14A H 0.3799 0.4286 0.8261 0.082 Uiso 0.50 1 calc PR A -1
H14B H 0.4564 0.4957 0.8644 0.082 Uiso 0.50 1 calc PR A -1
H14C H 0.4753 0.3976 0.8620 0.082 Uiso 0.50 1 calc PR A -1
C15 C 0.5865(6) 0.4486(6) 0.7971(5) 0.0441(14) Uani 0.50 1 d PDU A -1
C16 C 0.6259(2) 0.4827(3) 0.8979(3) 0.0677(11) Uani 0.50 1 d PU A -1
H16A H 0.5933 0.4613 0.9243 0.102 Uiso 0.50 1 calc PR A -1
H16B H 0.6236 0.5444 0.8962 0.102 Uiso 0.50 1 calc PR A -1
H16C H 0.6859 0.4643 0.9373 0.102 Uiso 0.50 1 calc PR A -1
C17 C 0.6477(3) 0.4791(3) 0.7664(4) 0.0657(11) Uani 0.50 1 d PU A -1
H17A H 0.7073 0.4662 0.8162 0.098 Uiso 0.50 1 calc PR A -1
H17B H 0.6413 0.5400 0.7556 0.098 Uiso 0.50 1 calc PR A -1
H17C H 0.6333 0.4504 0.7080 0.098 Uiso 0.50 1 calc PR A -1
C18 C 0.5901(6) 0.3509(6) 0.7990(9) 0.090(3) Uani 0.50 1 d PU A -1
H18A H 0.5588 0.3293 0.7342 0.135 Uiso 0.50 1 calc PR A -1
H18B H 0.5636 0.3292 0.8323 0.135 Uiso 0.50 1 calc PR A -1
H18C H 0.6502 0.3324 0.8318 0.135 Uiso 0.50 1 calc PR A -1
O2 O 0.50638(5) 0.76655(5) 0.84029(6) 0.03089(19) Uani 1 1 d U B .
C2 C 0.50680(8) 0.75764(9) 0.92436(10) 0.0360(3) Uani 1 1 d U . .
C20 C 0.49409(11) 0.66404(11) 0.93727(12) 0.0481(4) Uani 1 1 d U B .
H20A H 0.4339 0.6483 0.8926 0.072 Uiso 1 1 calc R . .
H20B H 0.5087 0.6545 1.0019 0.072 Uiso 1 1 calc R . .
H20C H 0.5316 0.6296 0.9255 0.072 Uiso 1 1 calc R . .
C21 C 0.42586(9) 0.80726(9) 0.91165(11) 0.0387(3) Uani 1 1 d U B .
C22 C 0.34750(9) 0.78882(10) 0.81148(11) 0.0414(3) Uani 1 1 d U . .
H22A H 0.2960 0.8151 0.8040 0.062 Uiso 1 1 calc R B .
H22B H 0.3388 0.7278 0.8026 0.062 Uiso 1 1 calc R . .
H22C H 0.3580 0.8119 0.7644 0.062 Uiso 1 1 calc R . .
C23 C 0.40037(11) 0.77892(13) 0.98137(13) 0.0543(4) Uani 1 1 d U . .
H23A H 0.4482 0.7897 1.0462 0.081 Uiso 1 1 calc R B .
H23B H 0.3872 0.7186 0.9733 0.081 Uiso 1 1 calc R . .
H23C H 0.3496 0.8105 0.9689 0.081 Uiso 1 1 calc R . .
C24 C 0.43557(11) 0.90357(10) 0.91966(14) 0.0542(4) Uani 1 1 d U . .
H24A H 0.3818 0.9289 0.9069 0.081 Uiso 1 1 calc R B .
H24B H 0.4485 0.9244 0.8737 0.081 Uiso 1 1 calc R . .
H24C H 0.4825 0.9188 0.9835 0.081 Uiso 1 1 calc R . .
C25 C 0.59969(10) 0.78640(13) 1.00895(12) 0.0529(4) Uani 1 1 d U B .
C26 C 0.60656(13) 0.79938(17) 1.10407(13) 0.0786(7) Uani 1 1 d U . .
H26A H 0.6669 0.8080 1.1543 0.118 Uiso 1 1 calc R B .
H26B H 0.5843 0.7495 1.1184 0.118 Uiso 1 1 calc R . .
H26C H 0.5728 0.8489 1.0998 0.118 Uiso 1 1 calc R . .
C27 C 0.66547(12) 0.71693(16) 1.02604(14) 0.0676(6) Uani 1 1 d U . .
H27A H 0.7239 0.7379 1.0697 0.101 Uiso 1 1 calc R B .
H27B H 0.6588 0.7016 0.9659 0.101 Uiso 1 1 calc R . .
H27C H 0.6553 0.6672 1.0534 0.101 Uiso 1 1 calc R . .
C28 C 0.63106(10) 0.86686(14) 0.98529(14) 0.0623(5) Uani 1 1 d U . .
H28A H 0.5892 0.9122 0.9690 0.093 Uiso 1 1 calc R B .
H28B H 0.6370 0.8559 0.9316 0.093 Uiso 1 1 calc R . .
H28C H 0.6869 0.8837 1.0402 0.093 Uiso 1 1 calc R . .
O1S O 0.6126(4) 1.0260(4) 0.7826(4) 0.0472(10) Uani 0.485(6) 1 d PU B 3
C1S C 0.6144(4) 1.1057(3) 0.8202(4) 0.0439(11) Uani 0.485(6) 1 d PU B 3
H1S1 H 0.583(5) 1.104(4) 0.853(4) 0.066 Uiso 0.48 1 calc P B 3
H1S2 H 0.586(3) 1.148(3) 0.769(3) 0.066 Uiso 0.48 1 calc P B 3
C6S C 0.7058(6) 1.1305(8) 0.8879(10) 0.106(5) Uani 0.485(6) 1 d PU B 3
H6S1 H 0.721(6) 1.126(6) 0.954(7) 0.159 Uiso 0.48 1 calc P B 3
H6S2 H 0.717(7) 1.189(6) 0.876(8) 0.159 Uiso 0.48 1 calc P B 3
C7S C 0.7538(6) 1.0662(7) 0.8660(9) 0.094(4) Uani 0.485(6) 1 d PU B 3
H7S1 H 0.785(6) 1.095(6) 0.841(7) 0.141 Uiso 0.48 1 calc P B 3
H7S2 H 0.796(6) 1.035(5) 0.924(6) 0.141 Uiso 0.48 1 calc P B 3
C4S C 0.6957(4) 1.0117(5) 0.8007(7) 0.0720(19) Uani 0.485(6) 1 d PU B 3
H4S1 H 0.714(6) 0.953(7) 0.824(6) 0.108 Uiso 0.48 1 calc P B 3
H4S2 H 0.694(4) 1.018(4) 0.741(4) 0.108 Uiso 0.48 1 calc P B 3
O2S O 0.6259(4) 1.0114(4) 0.8185(4) 0.0557(12) Uani 0.515(6) 1 d PU B 4
C5S C 0.6269(4) 1.0843(4) 0.8605(7) 0.0698(18) Uani 0.515(6) 1 d PU B 4
H5S1 H 0.638(4) 1.073(4) 0.924(4) 0.105 Uiso 0.52 1 calc P B 4
H5S2 H 0.571(6) 1.113(5) 0.822(5) 0.105 Uiso 0.52 1 calc P B 4
C2S C 0.6991(5) 1.1393(3) 0.8687(5) 0.0424(14) Uani 0.485(6) 1 d PU B 4
H2S1 H 0.675(3) 1.184(3) 0.820(3) 0.064 Uiso 0.52 1 calc P B 4
H2S2 H 0.733(3) 1.166(3) 0.932(4) 0.064 Uiso 0.52 1 calc P B 4
C3S C 0.7532(5) 1.0817(4) 0.8542(6) 0.0455(14) Uani 0.515(6) 1 d PU B 4
H3S1 H 0.814(3) 1.084(3) 0.908(4) 0.068 Uiso 0.52 1 calc P B 4
H3S2 H 0.751(3) 1.096(3) 0.796(3) 0.068 Uiso 0.52 1 calc P B 4
C8S C 0.7139(3) 0.9942(3) 0.8469(4) 0.0500(12) Uani 0.515(6) 1 d PU B 4
H8S1 H 0.716(4) 0.959(5) 0.799(4) 0.075 Uiso 0.52 1 calc P B 4
H8S2 H 0.745(3) 0.965(3) 0.908(4) 0.075 Uiso 0.52 1 calc P B 4
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'
K K 0.2009 0.2494 '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
O1 Fe1 O2 130.09(3) . .
O1 Fe1 O2 130.09(3) . 2_656
O2 Fe1 O2 99.82(6) . 2_656
O1 Fe1 K1 180.0 . .
O2 Fe1 K1 49.91(3) . .
O2 Fe1 K1 49.91(3) 2_656 .
O2 K1 O2 68.55(4) . 2_656
O2 K1 O2S 123.99(15) . 2_656
O2 K1 O2S 122.85(12) 2_656 2_656
O2 K1 O2S 122.85(12) . .
O2 K1 O2S 123.99(15) 2_656 .
O2S K1 O2S 96.4(3) 2_656 .
O2 K1 O1S 134.32(12) . .
O2 K1 O1S 120.88(13) 2_656 .
O2S K1 O1S 90.04(10) 2_656 .
O2S K1 O1S 12.03(13) . .
O2 K1 O1S 120.88(13) . 2_656
O2 K1 O1S 134.31(12) 2_656 2_656
O2S K1 O1S 12.03(13) 2_656 2_656
O2S K1 O1S 90.04(10) . 2_656
O1S K1 O1S 85.7(3) . 2_656
O2 K1 Fe1 34.27(2) . .
O2 K1 Fe1 34.27(2) 2_656 .
O2S K1 Fe1 131.80(14) 2_656 .
O2S K1 Fe1 131.80(14) . .
O1S K1 Fe1 137.16(13) . .
O1S K1 Fe1 137.16(13) 2_656 .
O2 K1 C28 109.29(4) . 2_656
O2 K1 C28 53.46(4) 2_656 2_656
O2S K1 C28 71.79(12) 2_656 2_656
O2S K1 C28 121.76(12) . 2_656
O1S K1 C28 110.05(11) . 2_656
O1S K1 C28 83.82(11) 2_656 2_656
Fe1 K1 C28 80.77(4) . 2_656
C1 O1 C1 29.07(19) . 2_656
C1 O1 Fe1 165.46(9) . .
C1 O1 Fe1 165.47(9) 2_656 .
O1 C1 C10 112.91(19) . .
O1 C1 C11 105.3(3) . .
C10 C1 C11 107.0(3) . .
O1 C1 C15 105.9(4) . .
C10 C1 C15 108.1(3) . .
C11 C1 C15 117.8(3) . .
C14 C11 C13 106.7(4) . .
C14 C11 C12 107.6(6) . .
C13 C11 C12 107.1(6) . .
C14 C11 C1 114.4(6) . .
C13 C11 C1 109.2(5) . .
C12 C11 C1 111.5(5) . .
C17 C15 C16 104.9(6) . .
C17 C15 C18 106.8(7) . .
C16 C15 C18 109.9(7) . .
C17 C15 C1 107.9(4) . .
C16 C15 C1 111.6(6) . .
C18 C15 C1 115.1(7) . .
C2 O2 Fe1 134.05(8) . .
C2 O2 K1 129.93(8) . .
Fe1 O2 K1 95.82(4) . .
O2 C2 C20 108.51(11) . .
O2 C2 C21 108.22(11) . .
C20 C2 C21 107.10(11) . .
O2 C2 C25 106.76(11) . .
C20 C2 C25 108.84(13) . .
C21 C2 C25 117.16(12) . .
C24 C21 C23 106.99(13) . .
C24 C21 C22 106.28(14) . .
C23 C21 C22 106.43(12) . .
C24 C21 C2 115.02(11) . .
C23 C21 C2 113.40(13) . .
C22 C21 C2 108.17(11) . .
C28 C25 C26 108.77(17) . .
C28 C25 C27 105.93(15) . .
C26 C25 C27 106.35(16) . .
C28 C25 C2 112.32(14) . .
C26 C25 C2 114.30(14) . .
C27 C25 C2 108.67(15) . .
C1S O1S C4S 106.6(5) . .
C1S O1S K1 125.6(4) . .
C4S O1S K1 123.5(4) . .
O1S C1S C6S 108.9(6) . .
C1S C6S C7S 101.8(7) . .
C4S C7S C6S 108.3(7) . .
C7S C4S O1S 111.5(7) . .
C5S O2S C8S 106.9(5) . .
C5S O2S K1 124.2(4) . .
C8S O2S K1 125.9(4) . .
O2S C5S C2S 107.7(5) . .
C3S C2S C5S 105.3(5) . .
C2S C3S C8S 104.0(5) . .
O2S C8S C3S 104.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.8263(12) .
Fe1 O2 1.9027(9) .
Fe1 O2 1.9028(9) 2_656
Fe1 K1 3.3614(5) .
K1 O2 2.5849(10) .
K1 O2 2.5850(10) 2_656
K1 O2S 2.627(6) 2_656
K1 O2S 2.627(6) .
K1 O1S 2.704(6) .
K1 O1S 2.704(6) 2_656
K1 C28 3.389(2) 2_656
O1 C1 1.416(2) .
O1 C1 1.416(2) 2_656
C1 C10 1.537(4) .
C1 C11 1.592(9) .
C1 C15 1.599(9) .
C11 C14 1.520(7) .
C11 C13 1.533(10) .
C11 C12 1.569(11) .
C15 C17 1.547(8) .
C15 C16 1.537(9) .
C15 C18 1.553(13) .
O2 C2 1.4139(16) .
C2 C20 1.538(2) .
C2 C21 1.5963(18) .
C2 C25 1.595(2) .
C21 C24 1.537(2) .
C21 C23 1.543(2) .
C21 C22 1.546(2) .
C25 C28 1.539(3) .
C25 C26 1.546(3) .
C25 C27 1.547(3) .
O1S C1S 1.408(8) .
O1S C4S 1.410(9) .
C1S C6S 1.491(11) .
C6S C7S 1.520(14) .
C7S C4S 1.355(12) .
O2S C5S 1.351(8) .
O2S C8S 1.449(8) .
C5S C2S 1.534(9) .
C2S C3S 1.467(12) .
C3S C8S 1.542(8) .
