Polycarbide nickel clusters containing interstitial Ni(eta2-C2)4 and Ni2(micro-eta2-C2)4 acetylide moieties: mimicking the supersaturated Ni-C solutions preceding the catalytic growth of CNTs with the structures of [HNi25(C2)4(CO)32]3- and [Ni22(C2)4(CO)28Cl]3-.
Femoni, Cristina; Iapalucci, Maria Carmela; Longoni, Giuliano; Zacchini, Stefano; Chemical communications (Cambridge, England)  (2008) 3157–3159; doi:10.1039/b803992e

data_7103216
_publ_section_title
;
 Polycarbide nickel clusters containing interstitial Ni(eta2-C2)4 and
 Ni2(micro-eta2-C2)4 acetylide moieties: mimicking the supersaturated
 Ni-C solutions preceding the catalytic growth of CNTs with the
 structures of [HNi25(C2)4(CO)32]3- and [Ni22(C2)4(CO)28Cl]3-.
;
_journal_issue                   27
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3157
_journal_page_last               3159
_journal_paper_doi               10.1039/b803992e
_journal_year                    2008
_chemical_formula_sum            'C61.5 H63 Br0 Cl N3 Ni22 O28.5'
_chemical_formula_weight         2627.22
_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                65.368(2)
_cell_angle_beta                 82.239(2)
_cell_angle_gamma                88.296(2)
_cell_formula_units_Z            4
_cell_length_a                   13.6790(16)
_cell_length_b                   23.876(3)
_cell_length_c                   27.991(3)
_cell_measurement_reflns_used    9103
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.5275
_cell_measurement_theta_min      2.2495
_cell_volume                     8230.1(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_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  0.1012
_diffrn_reflns_av_sigmaI/netI    0.1503
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            77938
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    5.004
_exptl_absorpt_correction_T_max  0.6091
_exptl_absorpt_correction_T_min  0.4197
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5256
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2051
_refine_ls_number_reflns         28968
_refine_ls_number_restraints     553
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1789
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1028P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.2165
_reflns_number_gt                12822
_reflns_number_total             28968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b803992e.txt
_cod_data_source_block           cl
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C61.50 H63 Br0 Cl N3 Ni22 O28.50'
_cod_database_code               7103216