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_4337977
_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            'C41 H40 Co11 N2 O23'
_chemical_formula_weight         1576.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   45.530(13)
_cell_length_b                   9.782(3)
_cell_length_c                   12.033(3)
_cell_measurement_reflns_used    1569
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.4165
_cell_measurement_theta_min      2.463
_cell_volume                     5359(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      296(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.1167
_diffrn_reflns_av_unetI/netI     0.1235
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10395
_diffrn_reflns_theta_full        22.72
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    3.388
_exptl_absorpt_correction_T_max  0.6866
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1291 (selected reflections only, before parameter refinement)
 R(int) = 0.0619 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3124
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         5852
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0869
_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^)+(0.1547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2148
_refine_ls_wR_factor_ref         0.2467
_reflns_number_gt                4011
_reflns_number_total             5852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500161e_si_001.cif
_cod_data_source_block           5_[TEA]2[Co11C2(CO)23]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/rss-feeds/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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4337973--4337985.cif.
;
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               4337977