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_4345894
_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         'C65 H40 Fe6 O16 P2'
_chemical_formula_sum            'C65 H40 Fe6 O16 P2'
_chemical_formula_weight         1474.01
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.209(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0889(16)
_cell_length_b                   14.517(2)
_cell_length_c                   18.902(3)
_cell_measurement_reflns_used    5503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      1.000000
_cell_measurement_theta_min      0.705017
_cell_volume                     2984.8(8)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 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      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33022
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.014
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  0.8735
_exptl_absorpt_correction_T_min  0.7374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            PURPLE
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.518(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         10481
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0490P)^2^+3.4009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10050
_reflns_number_total             10481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00741_si_002.cif
_cod_data_source_block           1c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/current/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4345894
_shelx_estimated_absorpt_t_min   0.737
_shelx_estimated_absorpt_t_max   0.873
_shelxl_version_number           2013-4
_shelx_res_checksum              1140
_shelx_hkl_checksum              88077