Sodium cubane and double-cubane aggregates of hybridised salicylaldimines and their transmetallation to nickel for catalytic ethylene oligomerisation
Xiaolu Song; Zhe Wang; Jin Zhao; T. S. Andy Hor; Chem.Commun. 49 (2013) 4992–; doi:10.1039/c3cc40320c

data_7109323
_publ_section_title
;
 Sodium cubane and double-cubane aggregates of hybridised salicylaldimines
 and their transmetallation to nickel for catalytic ethylene
 oligomerisation
;
_journal_name_full               Chem.Commun.
_journal_page_first              4992
_journal_paper_doi               10.1039/c3cc40320c
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C32.5 H32.75 Cl4 N3.25 Ni3 O2.5 S2'
_chemical_formula_weight         890.92
_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                96.290(2)
_cell_angle_beta                 95.839(2)
_cell_angle_gamma                98.850(2)
_cell_formula_units_Z            4
_cell_length_a                   12.2929(14)
_cell_length_b                   13.6662(16)
_cell_length_c                   22.289(3)
_cell_measurement_reflns_used    995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.65
_cell_volume                     3650.7(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48584
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  0.8580
_exptl_absorpt_correction_T_min  0.7429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2008)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1818
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         16709
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+2.7870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                14419
_reflns_number_total             16709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40320c.txt
_cod_data_source_block           b757
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3650.7(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C32.50 H32.75 Cl4 N3.25 Ni3 O2.50 S2'
_cod_database_code               7109323