A strong-field pentadentate ligand in iron-based alkane oxidation catalysis and implications for iron(iv) oxo intermediates
Wong, Emma; Jeck, Jonathan; Grau, Michaela; White, Andrew J. P.; Britovsek, George J. P.; Catalysis Science & Technology 3 (2013) 1116–; doi:10.1039/c3cy20823k

data_1556385
_publ_section_title
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 A strong-field pentadentate ligand in iron-based alkane oxidation
 catalysis and implications for iron(iv) oxo intermediates
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_journal_issue                   4
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1116
_journal_paper_doi               10.1039/c3cy20823k
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C46 H42 Fe2 N10 O, C2 H3 N, 4(Cl O4), H2 O'
_chemical_formula_sum            'C48 H47 Cl4 Fe2 N11 O18'
_chemical_formula_weight         1319.47
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/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                 117.208(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4043(8)
_cell_length_b                   38.877(2)
_cell_length_c                   12.3737(10)
_cell_measurement_reflns_used    3077
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.1219
_cell_measurement_theta_min      4.0995
_cell_volume                     5306.9(7)
_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 15.9863
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.731
_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  0.1065
_diffrn_reflns_av_sigmaI/netI    0.1796
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22265
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
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
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plates'
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         10488
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1683
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1703
_reflns_number_gt                5396
_reflns_number_total             10488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cy20823k.txt
_cod_data_source_block           '[{Fe(1)}2O](ClO4)4'
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1556385