Bimetallic Nickel‒Cobalt Hexacarbido Carbonyl Clusters [H6‒nNi22Co6C6(CO)36]n−(n= 3‒6) Possessing Polyhydride Nature and Their Base-Induced Degradation to the Monoacetylide [Ni9CoC2(CO)16‒x]3‒(x= 0, 1)
Ciabatti, Iacopo; Femoni, Cristina; Iapalucci, Maria Carmela; Longoni, Giuliano; Zacchini, Stefano; Organometallics 31 (2012) 4593–; doi:10.1021/om300412d

data_4078606
_publ_section_title
;
 Bimetallic Nickel--Cobalt Hexacarbido Carbonyl Clusters
 [H6--nNi22Co6C6(CO)36]n&#x2212;(n= 3--6) Possessing Polyhydride Nature
 and Their Base-Induced Degradation to the Monoacetylide
 [Ni9CoC2(CO)16--x]3--(x= 0, 1)
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              4593
_journal_paper_doi               10.1021/om300412d
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C41.29 H60 Co N3 Ni9 O15.3'
_chemical_formula_weight         1430.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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            2
_cell_length_a                   11.9970(11)
_cell_length_b                   12.2347(11)
_cell_length_c                   18.4420(17)
_cell_measurement_reflns_used    9185
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9235
_cell_measurement_theta_min      2.2085
_cell_volume                     2706.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25578
_diffrn_reflns_theta_full        25.59
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    3.414
_exptl_absorpt_correction_T_max  0.7264
_exptl_absorpt_correction_T_min  0.5785
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         2626
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0491P)^2^+2.3819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                2231
_reflns_number_total             2626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300412d_si_001.cif
_cod_data_source_block           pnnm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pnnm
_cod_original_formula_sum        'C41.29 H60 Co N3 Ni9 O15.30'
_cod_database_code               4078606