Rare Nuclearities in Ni(II) Cluster Chemistry: An Unprecedented {Ni12} Nanosized Cage from the Use of N-Naphthalidene-2-Amino-5-Chlorobenzoic Acid
Perlepe, Panagiota S.; Pantelis, Konstantinos N.; Cunha-Silva, Luís; Bekiari, Vlasoula; Escuer, Albert; Stamatatos, Theocharis C.; Inorganics 8 (2020) 32–; doi:10.3390/inorganics8050032

data_1558192
_publ_section_title
;
 Rare Nuclearities in Ni(II) Cluster Chemistry: An Unprecedented {Ni12}
 Nanosized Cage from the Use of N-Naphthalidene-2-Amino-5-Chlorobenzoic
 Acid
;
_journal_issue                   5
_journal_name_full               Inorganics
_journal_page_first              32
_journal_paper_doi               10.3390/inorganics8050032
_journal_volume                  8
_journal_year                    2020
_chemical_formula_moiety         'C133 H101 Cl5 I2 N9 Ni12 O35, I'
_chemical_formula_sum            'C133 H101 Cl5 I3 N9 Ni12 O35'
_chemical_formula_weight         3647.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             '20 November 2018'
_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_cell_angle_alpha                115.783(4)
_cell_angle_beta                 92.992(5)
_cell_angle_gamma                106.118(5)
_cell_formula_units_Z            2
_cell_length_a                   19.422(2)
_cell_length_b                   22.654(3)
_cell_length_c                   25.321(3)
_cell_measurement_reflns_used    8263
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.48
_cell_volume                     9443(2)
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            134933
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.648
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.786
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3644
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.613
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1787
_refine_ls_number_reflns         32481
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0872
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+102.1290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23114
_reflns_number_total             32481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CIF-complex_1.cif
_cod_data_source_block           pp295a_sq
_cod_database_code               1558192
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.695
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              78451
_shelx_hkl_checksum              50438
_shelx_fab_checksum              56057