Rare nuclearities in Ni(ii) cluster chemistry: a Ni11 cage from the first use of N-salicylidene-2-amino-5-chlorobenzoic acid in metal cluster chemistry
Athanasopoulou, Angeliki A.; Raptopoulou, Catherine P.; Escuer, Albert; Stamatatos, Theocharis C.; RSC Adv. 4 (2014) 12680–; doi:10.1039/C4RA00738G

data_7235508
_publ_section_title
;
 Rare nuclearities in Ni(ii) cluster chemistry: a Ni11 cage from the first
 use of N-salicylidene-2-amino-5-chlorobenzoic acid in metal cluster
 chemistry
;
_journal_issue                   25
_journal_name_full               'RSC Adv.'
_journal_page_first              12680
_journal_paper_doi               10.1039/C4RA00738G
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C133 H159.5 Cl5 N12.5 Ni11 O37.5'
_chemical_formula_weight         3356.29
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 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                 114.718(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.090(3)
_cell_length_b                   22.251(2)
_cell_length_c                   28.725(3)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.37
_cell_volume                     15728(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            466517
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             6952
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.637
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1814
_refine_ls_number_reflns         27654
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+83.1893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                22644
_reflns_number_total             27654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra00738g2.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C133 H159.50 Cl5 N12.50 Ni11 O37.50'
_cod_database_code               7235508