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_4337976
_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            'C45.25 H32.5 Cl0.5 Co11 N2 O23'
_chemical_formula_weight         1638.19
_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                106.9450(10)
_cell_angle_beta                 97.0880(10)
_cell_angle_gamma                90.8430(10)
_cell_formula_units_Z            4
_cell_length_a                   9.9820(10)
_cell_length_b                   24.042(2)
_cell_length_c                   24.415(2)
_cell_measurement_reflns_used    7124
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      21.557
_cell_measurement_theta_min      2.2005
_cell_volume                     5554.1(9)
_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 pmega 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  0.0645
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            58138
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    3.297
_exptl_absorpt_correction_T_max  0.6739
_exptl_absorpt_correction_T_min  0.5308
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.0955 (selected reflections only, before parameter refinement)
 R(int) = 0.0486 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3230
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1471
_refine_ls_number_reflns         21727
_refine_ls_number_restraints     543
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                11912
_reflns_number_total             21727
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500161e_si_001.cif
_cod_data_source_block           4_[TMBA]2[Co11C2(CO)23].0.25CH2Cl2
_cod_depositor_comments
'Adding full bibliography for 4337973--4337985.cif.'
_cod_original_cell_volume        5554.2(10)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C45.25 H32.50 Cl0.50 Co11 N2 O23'
_cod_database_code               4337976