New Systematic Route to Mixed-Valence Triiron Clusters Derived from Dinuclear Models of the Active Site of [Fe–Fe]-Hydrogenases
Beaume, Laetitia; Clémancey, Martin; Blondin, Geneviève; Greco, Claudio; Pétillon, François Y.; Schollhammer, Philippe; Talarmin, Jean; Organometallics 33 (2014) 6290–; doi:10.1021/om5010594

data_4084652
_publ_section_title
;
 New Systematic Route to Mixed-Valence Triiron Clusters Derived from
 Dinuclear Models of the Active Site of [Fe--Fe]-Hydrogenases
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6290
_journal_paper_doi               10.1021/om5010594
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
;
        C43 H41 Fe3 N O5 P2 S4, C H2 Cl2
;
_chemical_formula_sum            'C44 H43 Cl2 Fe3 N O5 P2 S4'
_chemical_formula_weight         1094.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-04T11:26:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.143(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2436(6)
_cell_length_b                   22.8649(11)
_cell_length_c                   15.4358(9)
_cell_measurement_radiation      'Mo K\a'
_cell_measurement_reflns_used    4938
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.52
_cell_volume                     4586.1(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics
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        ORTEP3 for Windows (Farrugia, 1997)
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_computing_publication_material
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        WinGX (Farrugia, 1999)
        PLATON (Spek, 1990-2003)
        enCIFer (Allen et al., 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0516943967
_diffrn_orient_matrix_UB_12      -0.0050596308
_diffrn_orient_matrix_UB_13      0.0212960555
_diffrn_orient_matrix_UB_21      0.014279323
_diffrn_orient_matrix_UB_22      0.0276820586
_diffrn_orient_matrix_UB_23      -0.0145638561
_diffrn_orient_matrix_UB_31      -0.0102094652
_diffrn_orient_matrix_UB_32      0.013064923
_diffrn_orient_matrix_UB_33      0.0390732368
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.1137
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40478
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
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            red
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
        truncated hexagonal prism, axis [1 0 0]
;
_exptl_crystal_F_000             2240
_exptl_crystal_recrystallization_method
;
from solution in dichloromethane in freezer, 
by slow diffusion of pentane
;
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         11377
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                6318
_reflns_number_total             11377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5010594_si_002.cif
_cod_data_source_block           lb105-a0
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/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 4084652.cif.

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4084652