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_4345892
_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_absolute_configuration ad
_chemical_formula_moiety         '16 C O, 6 Fe, C, 2 C4 H12 N, C4 H8 O'
_chemical_formula_sum            'C29 H32 Fe6 N2 O17'
_chemical_formula_weight         1015.66
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.210(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4065(3)
_cell_length_b                   15.6419(5)
_cell_length_c                   21.1122(7)
_cell_measurement_reflns_used    17700
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.81
_cell_measurement_theta_min      3.80
_cell_volume                     3766.0(2)
_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      133(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Agilent SuperNova Dual source with AtlasS2 detector'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41422
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.434
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.325
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.013(15)
_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     990
_refine_ls_number_reflns         17007
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+2.5408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                15717
_reflns_number_total             17007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00741_si_002.cif
_cod_data_source_block           1a
_cod_database_code               4345892
_shelx_estimated_absorpt_t_min   0.573
_shelx_estimated_absorpt_t_max   0.752
_shelxl_version_number           2013-4
_shelx_res_checksum              76352
_shelx_hkl_checksum              69281