#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:18:00 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180033 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/27/7032715.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_7032715
loop_
_publ_author_name
'Grau, Michaela'
'Kyriacou, Andrew'
'Cabedo Martinez, Fernando'
'de Wispelaere, Irene M.'
'White, Andrew J. P.'
'Britovsek, George J. P.'
_publ_section_title
;
 Unraveling the origins of catalyst degradation in non-heme iron-based
 alkane oxidation.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17108
_journal_page_last               17119
_journal_paper_doi               10.1039/c4dt02067g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C28 H30 Fe2 N6 O6, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C34 H36 F6 Fe2 N8 O12 S2'
_chemical_formula_weight         1038.53
_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                104.096(3)
_cell_angle_beta                 109.381(4)
_cell_angle_gamma                98.362(4)
_cell_formula_units_Z            1
_cell_length_a                   9.0685(5)
_cell_length_b                   9.9914(4)
_cell_length_c                   13.1697(5)
_cell_measurement_reflns_used    4091
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.1256
_cell_measurement_theta_min      3.7426
_cell_volume                     1057.85(9)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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      173
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8131
_diffrn_reflns_theta_full        71.50
_diffrn_reflns_theta_max         72.27
_diffrn_reflns_theta_min         3.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.283
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.328
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4080
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0417
_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)+(0.0783P)²+0.0723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                3607
_reflns_number_total             4080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02067g2.cif
_cod_data_source_block           '[Fe(6')(OH)]2(OTf)2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7032713--7032715.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7032715
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 0.51880(4) 0.57483(4) 0.62256(3) 0.03504(14) Uani 1 1 d . . .
N1 N 0.5949(3) 0.5154(2) 0.76914(18) 0.0407(4) Uani 1 1 d . . .
C2 C 0.7466(3) 0.5791(3) 0.8417(2) 0.0474(6) Uani 1 1 d . . .
C3 C 0.8082(4) 0.5526(4) 0.9439(3) 0.0580(7) Uani 1 1 d . . .
H3A H 0.9153 0.5989 0.9964 0.070 Uiso 1 1 calc R . .
C4 C 0.7085(5) 0.4564(4) 0.9672(3) 0.0627(8) Uani 1 1 d . . .
H4A H 0.7475 0.4360 1.0367 0.075 Uiso 1 1 calc R . .
C5 C 0.5519(4) 0.3891(4) 0.8903(3) 0.0556(7) Uani 1 1 d . . .
H5A H 0.4836 0.3226 0.9061 0.067 Uiso 1 1 calc R . .
C6 C 0.4980(3) 0.4217(3) 0.7896(2) 0.0446(6) Uani 1 1 d . . .
C7 C 0.8324(4) 0.6781(3) 0.7979(3) 0.0540(7) Uani 1 1 d . . .
O8 O 0.7433(2) 0.6907(2) 0.70252(16) 0.0479(4) Uani 1 1 d . . .
O9 O 0.9751(3) 0.7376(4) 0.8500(2) 0.0814(8) Uani 1 1 d . . .
C10 C 0.3358(3) 0.3588(3) 0.6940(2) 0.0461(6) Uani 1 1 d . . .
H10A H 0.3392 0.2727 0.6393 0.055 Uiso 1 1 calc R . .
H10B H 0.2531 0.3310 0.7237 0.055 Uiso 1 1 calc R . .
N11 N 0.2941(3) 0.4674(2) 0.63665(19) 0.0400(4) Uani 1 1 d . . .
C12 C 0.2439(3) 0.5764(3) 0.7088(2) 0.0448(6) Uani 1 1 d . . .
H12A H 0.2955 0.5805 0.7890 0.054 Uiso 1 1 calc R . .
H12B H 0.1256 0.5479 0.6864 0.054 Uiso 1 1 calc R . .
C13 C 0.2901(3) 0.7212(3) 0.6980(2) 0.0430(5) Uani 1 1 d . . .
N14 N 0.4195(3) 0.7464(2) 0.67132(19) 0.0427(5) Uani 1 1 d . . .
C15 C 0.4782(4) 0.8775(3) 0.6714(3) 0.0534(7) Uani 1 1 d . . .
H15A H 0.5680 0.8940 0.6502 0.064 Uiso 1 1 calc R . .
C16 C 0.4118(5) 0.9891(3) 0.7013(4) 0.0679(9) Uani 1 1 d . . .
H16A H 0.4574 1.0822 0.7038 0.081 Uiso 1 1 calc R . .
C17 C 0.2776(5) 0.9623(4) 0.7276(4) 0.0685(9) Uani 1 1 d . . .
H17A H 0.2289 1.0373 0.7476 0.082 Uiso 1 1 calc R . .
C18 C 0.2141(4) 0.8271(3) 0.7250(3) 0.0566(7) Uani 1 1 d . . .
H18A H 0.1204 0.8070 0.7414 0.068 Uiso 1 1 calc R . .
C19 C 0.1641(3) 0.3998(3) 0.5234(3) 0.0473(6) Uani 1 1 d . . .
H19A H 0.0672 0.3537 0.5312 0.071 Uiso 1 1 calc R . .
H19B H 0.1991 0.3283 0.4774 0.071 Uiso 1 1 calc R . .
H19C H 0.1398 0.4724 0.4864 0.071 Uiso 1 1 calc R . .
O20 O 0.5372(2) 0.39781(18) 0.52760(14) 0.0398(4) Uani 1 1 d D . .
H20 H 0.613(4) 0.353(4) 0.554(4) 0.077(13) Uiso 1 1 d D . .
S30 S 0.14060(18) 0.74519(14) 0.30123(11) 0.0499(3) Uani 0.854(4) 1 d PDU A 1
O31 O 0.2658(4) 0.7747(4) 0.2594(3) 0.0811(11) Uani 0.854(4) 1 d PD A 1
O32 O -0.0163(4) 0.6830(5) 0.2189(3) 0.0898(12) Uani 0.854(4) 1 d PD A 1
O33 O 0.1821(4) 0.6820(4) 0.3900(3) 0.0750(9) Uani 0.854(4) 1 d PD A 1
C30 C 0.1330(6) 0.9208(5) 0.3717(4) 0.0705(12) Uani 0.854(4) 1 d PDU A 1
F31 F 0.0200(5) 0.9109(3) 0.4145(4) 0.1019(12) Uani 0.854(4) 1 d PDU A 1
F32 F 0.2720(5) 0.9974(4) 0.4500(3) 0.1086(13) Uani 0.854(4) 1 d PDU A 1
F33 F 0.0924(5) 0.9930(4) 0.2975(5) 0.1078(13) Uani 0.854(4) 1 d PDU A 1
S30' S 0.1704(14) 0.7604(12) 0.2925(10) 0.073(4) Uiso 0.146(4) 1 d PDU A 2
O31' O 0.152(4) 0.795(3) 0.1891(18) 0.116(9) Uiso 0.146(4) 1 d PD A 2
O32' O 0.071(3) 0.6277(18) 0.279(3) 0.107(8) Uiso 0.146(4) 1 d PD A 2
O33' O 0.3303(17) 0.782(2) 0.3651(16) 0.074(5) Uiso 0.146(4) 1 d PD A 2
C30' C 0.093(2) 0.889(2) 0.3656(17) 0.109(10) Uiso 0.146(4) 1 d PDU A 2
F31' F 0.110(3) 0.875(3) 0.4669(16) 0.109(5) Uiso 0.146(4) 1 d PDU A 2
F32' F 0.173(4) 1.0192(18) 0.383(3) 0.112(5) Uiso 0.146(4) 1 d PDU A 2
F33' F -0.048(3) 0.895(3) 0.294(3) 0.151(6) Uiso 0.146(4) 1 d PDU A 2
N40 N 0.5492(6) 0.8091(4) 0.9573(3) 0.0846(10) Uani 1 1 d . . .
C41 C 0.6412(6) 0.9011(5) 0.9592(4) 0.0825(12) Uani 1 1 d . . .
C42 C 0.7534(9) 1.0176(8) 0.9567(7) 0.137(3) Uani 1 1 d . . .
H42A H 0.7643 0.9936 0.8832 0.205 Uiso 1 1 calc R . .
H42B H 0.8588 1.0345 1.0173 0.205 Uiso 1 1 calc R . .
H42C H 0.7131 1.1037 0.9678 0.205 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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
O20 Fe1 O20 76.60(8) . 2_666
O20 Fe1 O8 103.97(8) . .
O20 Fe1 O8 101.79(8) 2_666 .
O20 Fe1 N1 93.18(8) . .
O20 Fe1 N1 169.40(8) 2_666 .
O8 Fe1 N1 77.75(8) . .
O20 Fe1 N14 158.72(9) . .
O20 Fe1 N14 88.38(8) 2_666 .
O8 Fe1 N14 93.70(9) . .
N1 Fe1 N14 102.22(9) . .
O20 Fe1 N11 93.55(8) . .
O20 Fe1 N11 109.25(8) 2_666 .
O8 Fe1 N11 147.17(8) . .
N1 Fe1 N11 73.70(8) . .
N14 Fe1 N11 77.08(8) . .
C6 N1 C2 122.2(2) . .
C6 N1 Fe1 122.06(19) . .
C2 N1 Fe1 115.73(19) . .
N1 C2 C3 120.9(3) . .
N1 C2 C7 112.0(2) . .
C3 C2 C7 127.1(3) . .
C4 C3 C2 117.6(3) . .
C3 C4 C5 121.0(3) . .
C6 C5 C4 118.2(3) . .
N1 C6 C5 120.1(3) . .
N1 C6 C10 112.9(2) . .
C5 C6 C10 127.0(3) . .
O9 C7 O8 124.8(3) . .
O9 C7 C2 120.6(3) . .
O8 C7 C2 114.6(2) . .
C7 O8 Fe1 119.82(18) . .
N11 C10 C6 108.6(2) . .
C19 N11 C10 110.6(2) . .
C19 N11 C12 110.7(2) . .
C10 N11 C12 109.0(2) . .
C19 N11 Fe1 110.65(16) . .
C10 N11 Fe1 107.47(15) . .
C12 N11 Fe1 108.37(15) . .
N11 C12 C13 111.7(2) . .
N14 C13 C18 121.7(3) . .
N14 C13 C12 115.9(2) . .
C18 C13 C12 122.1(3) . .
C13 N14 C15 119.5(2) . .
C13 N14 Fe1 118.70(18) . .
C15 N14 Fe1 121.74(19) . .
N14 C15 C16 121.8(3) . .
C15 C16 C17 118.4(3) . .
C18 C17 C16 120.1(3) . .
C17 C18 C13 118.5(3) . .
Fe1 O20 Fe1 103.40(8) . 2_666
O32 S30 O33 113.7(2) . .
O32 S30 O31 116.2(2) . .
O33 S30 O31 114.5(2) . .
O32 S30 C30 104.3(3) . .
O33 S30 C30 103.4(2) . .
O31 S30 C30 102.3(2) . .
F32 C30 F31 110.9(4) . .
F32 C30 F33 105.8(4) . .
F31 C30 F33 107.3(4) . .
F32 C30 S30 113.1(3) . .
F31 C30 S30 109.4(3) . .
F33 C30 S30 110.2(4) . .
O33' S30' O32' 112.5(17) . .
O33' S30' O31' 114.4(18) . .
O32' S30' O31' 115.9(19) . .
O33' S30' C30' 105.4(9) . .
O32' S30' C30' 103.4(10) . .
O31' S30' C30' 103.6(10) . .
F32' C30' F31' 107(2) . .
F32' C30' F33' 97(2) . .
F31' C30' F33' 121(2) . .
F32' C30' S30' 110.7(13) . .
F31' C30' S30' 110.7(12) . .
F33' C30' S30' 109.5(13) . .
N40 C41 C42 177.5(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O20 1.9664(17) .
Fe1 O20 1.9700(17) 2_666
Fe1 O8 1.9728(19) .
Fe1 N1 2.085(2) .
Fe1 N14 2.111(2) .
Fe1 N11 2.247(2) .
N1 C6 1.328(4) .
N1 C2 1.337(4) .
C2 C3 1.383(4) .
C2 C7 1.506(5) .
C3 C4 1.382(6) .
C4 C5 1.389(5) .
C5 C6 1.388(4) .
C6 C10 1.504(4) .
C7 O9 1.219(4) .
C7 O8 1.296(4) .
C10 N11 1.490(3) .
N11 C19 1.477(4) .
N11 C12 1.491(3) .
C12 C13 1.501(4) .
C13 N14 1.340(4) .
C13 C18 1.382(4) .
N14 C15 1.340(4) .
C15 C16 1.378(5) .
C16 C17 1.380(6) .
C17 C18 1.377(5) .
O20 Fe1 1.9700(17) 2_666
S30 O32 1.406(4) .
S30 O33 1.430(3) .
S30 O31 1.441(3) .
S30 C30 1.796(4) .
C30 F32 1.308(6) .
C30 F31 1.327(5) .
C30 F33 1.338(6) .
S30' O33' 1.397(13) .
S30' O32' 1.429(14) .
S30' O31' 1.449(15) .
S30' C30' 1.780(15) .
C30' F32' 1.319(15) .
C30' F31' 1.335(15) .
C30' F33' 1.337(15) .
N40 C41 1.138(6) .
C41 C42 1.444(9) .
