Structures, Interconversions, and Spectroscopy of Iron Carbonyl Clusters with an Interstitial Carbide: Localized Metal Center Reduction by Overall Cluster Oxidation.
Kuppuswamy, Subramaniam; Wofford, Joshua D.; Joseph, Chris; Xie, Zhu-Lin; Ali, Azim K.; Lynch, Vincent M.; Lindahl, Paul A.; Rose, Michael J.; Inorganic chemistry 56 (2017) 5998–6012; doi:10.1021/acs.inorgchem.7b00741

data_4345896
_publ_section_title
;
 Structures, Interconversions, and Spectroscopy of Iron Carbonyl Clusters
 with an Interstitial Carbide: Localized Metal Center Reduction by Overall
 Cluster Oxidation.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5998
_journal_page_last               6012
_journal_paper_doi               10.1021/acs.inorgchem.7b00741
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C15 O14 Fe5 2-, 2 C4 H12 N 1+'
_chemical_formula_sum            'C23 H24 Fe5 N2 O14'
_chemical_formula_weight         831.69
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 96.463(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5579(13)
_cell_length_b                   10.8967(10)
_cell_length_c                   28.9033(16)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2
_cell_measurement_theta_min      4.54
_cell_volume                     6120.6(8)
_computing_cell_refinement
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_collection
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M.'
_computing_structure_solution
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Agilent SuperNova with AtlasS2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1599
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            26965
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.515
_diffrn_reflns_theta_min         3.077
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    19.173
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_description       plates
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.766
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         6220
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1579
_refine_ls_R_factor_gt           0.1104
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1348P)^2^+360.6494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2773
_refine_ls_wR_factor_ref         0.3320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4299
_reflns_number_total             6220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00741_si_002.cif
_cod_data_source_block           4
_cod_original_formula_sum        C23H24Fe5N2O14
_cod_database_code               4345896
_shelx_estimated_absorpt_t_min   0.059
_shelx_estimated_absorpt_t_max   0.597
_shelxl_version_number           2013-4
_shelx_res_checksum              58253
_shelx_hkl_checksum              64712