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_4345893
_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         'C17 Fe6 O16, 2(C8 H20 N)'
_chemical_formula_sum            'C33 H40 Fe6 N2 O16'
_chemical_formula_weight         1055.77
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
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_space_group_name_Hall           '-P 4ac 2bc'
_space_group_name_H-M_alt        'P 42/n n m'
_symmetry_space_group_name_Hall  '-P 4ac 2bc'
_symmetry_space_group_name_H-M   'P 42/n n m :2'
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_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_b                   11.7157(4)
_cell_length_c                   16.8663(6)
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_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.4
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_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
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_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M. 2013'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
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'Nonius Kappa CCD with Bruker Apex II detector'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
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_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_min         2.739
_diffrn_source                   'sealed tube'
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_exptl_absorpt_correction_T_min  0.815
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_exptl_absorpt_process_details
;
SADABS. Apex II release 2010, Bruker AXS, Inc.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       prisms
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_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.160
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_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+2.6558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1087
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_reflns_number_gt                1175
_reflns_number_total             1430
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           1b
_cod_original_cell_volume        2315.03(18)
_cod_database_code               4345893
_shelx_estimated_absorpt_t_min   0.605
_shelx_estimated_absorpt_t_max   0.748
_shelxl_version_number           2013-4
_shelx_res_checksum              80785
_shelx_hkl_checksum              70775
_shelx_fab_checksum              73882