Selective synthesis of the [Ni36Co8C8(CO)48]6- octa-carbide carbonyl cluster by thermal decomposition of the [H2Ni22Co6C6(CO)36]4- hexa-carbide.
Ciabatti, Iacopo; Fabrizi de Biani, Fabrizia; Femoni, Cristina; Iapalucci, Maria Carmela; Longoni, Giuliano; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 42 (2013) 9662–9670; doi:10.1039/c3dt50710f

data_7023095
_publ_section_title
;
 Selective synthesis of the [Ni36Co8C8(CO)48]6- octa-carbide carbonyl
 cluster by thermal decomposition of the [H2Ni22Co6C6(CO)36]4-
 hexa-carbide.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9662
_journal_page_last               9670
_journal_paper_doi               10.1039/c3dt50710f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C131 H126 Co8 N6 Ni36 O53'
_chemical_formula_weight         5217.38
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 90.012(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.324(8)
_cell_length_b                   17.491(6)
_cell_length_c                   23.175(8)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.741
_cell_measurement_theta_min      2.237
_cell_volume                     8644(5)
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1778
_diffrn_reflns_av_sigmaI/netI    0.1238
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78617
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    4.628
_exptl_absorpt_correction_T_max  0.5635
_exptl_absorpt_correction_T_min  0.4292
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Data were corrected for Lorentz polarisation and absorption
effects (empirical absorption corrections SADABS)
R(int) = 0.1707 (selected reflections only, before parameter refinement)
R(int) = 0.0884 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5204
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.182
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         15264
_refine_ls_number_restraints     980
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1777
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1119P)^2^+47.0041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2467
_reflns_number_gt                7940
_reflns_number_total             15264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50710f.txt
_cod_data_source_block           p21nx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7023095