The Redox Chemistry of [Co6C(CO)15](2-): A Synthetic Route to New Co-Carbide Carbonyl Clusters.
Ciabatti, Iacopo; Femoni, Cristina; Hayatifar, Mohammad; Iapalucci, Maria Carmela; Longoni, Giuliano; Pinzino, Calogero; Solmi, Matilde Valeria; Zacchini, Stefano; Inorganic chemistry 53 (2014) 3818–; doi:10.1021/ic500161e

data_4337979
_publ_section_title
;
 The Redox Chemistry of [Co6C(CO)15](2-): A Synthetic Route to New
 Co-Carbide Carbonyl Clusters.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3818
_journal_paper_doi               10.1021/ic500161e
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C35.5 H17 Cl Co11 N O23'
_chemical_formula_weight         1509.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.6090(10)
_cell_angle_beta                 95.4510(10)
_cell_angle_gamma                110.2430(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6783(7)
_cell_length_b                   14.6091(9)
_cell_length_c                   15.2432(16)
_cell_measurement_reflns_used    8727
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.9235
_cell_measurement_theta_min      2.3405
_cell_volume                     2339.5(3)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'SCHAKAL99 (Keller, 1999)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0225
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22545
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    3.930
_exptl_absorpt_correction_T_max  0.6499
_exptl_absorpt_correction_T_min  0.5222
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.0742 (selected reflections only, before parameter refinement)
 R(int) = 0.0371 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1470
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.363
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         8209
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1424P)^2^+11.2947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2249
_reflns_number_gt                6634
_reflns_number_total             8209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500161e_si_001.cif
_cod_data_source_block           7_[TMBA][Co11C2(CO)23]0.5CH2Cl2
_cod_depositor_comments
'Adding full bibliography for 4337973--4337985.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C35.50 H17 Cl Co11 N O23'
_cod_database_code               4337979