Unraveling the origins of catalyst degradation in non-heme iron-based alkane oxidation.
Grau, Michaela; Kyriacou, Andrew; Cabedo Martinez, Fernando; de Wispelaere, Irene M.; White, Andrew J. P.; Britovsek, George J. P.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 17108–17119; doi:10.1039/c4dt02067g

data_7032713
_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         'C44 H36 F12 Fe2 N8 O16 S4, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H42 F12 Fe2 N10 O16 S4'
_chemical_formula_weight         1482.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   25.4174(4)
_cell_length_b                   25.4174(4)
_cell_length_c                   51.8599(7)
_cell_measurement_reflns_used    26758
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.4172
_cell_measurement_theta_min      2.8443
_cell_volume                     29015.1(8)
_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(2)
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            28931
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         31.49
_diffrn_reflns_theta_min         2.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
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            Orange-red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             13536
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
 SQUEEZE suggests 698e/cell = 19.4e/asu
 Solvent = MeCN = C2H3N = 22e.
 1MeCN per asu was used as the solvent present.
 
 From SQUEEZE, atom list low by C2H3N per asu, so UNIT low by
 C72 H108 N36, i.e. C792 H648 N144 O288 F216 S72 Fe36
;
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         9380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                6515
_reflns_number_total             9380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02067g2.cif
_cod_data_source_block           '[Fe(4)(OTf)2]2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' 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      R-3c
_cod_database_code               7032713