Ni-Cu tetracarbide carbonyls with vacant Ni(CO) fragments as borderline compounds between molecular and quasi-molecular clusters.
Bernardi, Alessandro; Ciabatti, Iacopo; Femoni, Cristina; Iapalucci, Maria Carmela; Longoni, Giuliano; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 42 (2013) 407–421; doi:10.1039/c2dt31719b

data_7020701
_publ_section_title
;
 Ni-Cu tetracarbide carbonyls with vacant Ni(CO) fragments as borderline
 compounds between molecular and quasi-molecular clusters.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              407
_journal_page_last               421
_journal_paper_doi               10.1039/c2dt31719b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C85.65 H76 Cu2 N8 Ni29.65 O33.66'
_chemical_formula_weight         3624.01
_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                89.4140(10)
_cell_angle_beta                 89.1030(10)
_cell_angle_gamma                62.4730(10)
_cell_formula_units_Z            2
_cell_length_a                   14.2042(9)
_cell_length_b                   14.8781(10)
_cell_length_c                   28.1762(18)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.396
_cell_measurement_theta_min      2.1555
_cell_volume                     5279.7(6)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            50273
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    5.613
_exptl_absorpt_correction_T_max  0.5290
_exptl_absorpt_correction_T_min  0.4152
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Data were corrected for Lorentz polarisation and absorption
effects (empirical absorption correction SADABS)
R(int) = 0.0923 (selected reflections only, before parameter refinement)
R(int) = 0.0323 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3607
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.745
_refine_diff_density_min         -2.009
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1476
_refine_ls_number_reflns         18579
_refine_ls_number_restraints     634
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0312P)^2^+25.7316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                13152
_reflns_number_total             18579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31719b.txt
_cod_data_source_block           ni30cutmba4_p-1
_cod_original_cell_volume        5279.8(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7020701