Synthesis, oligomerization and catalytic studies of a redox-active Ni4-cubane: a detailed mechanistic investigation
Kushvaha, Saroj Kumar; Francis, Maria; Kumar, Jayasree; Nag, Ekta; Ravichandran, Prathap; Roy, Sudipta; Chandra Mondal, Kartik; RSC Advances 11 (2021) 22849–22858; doi:10.1039/D1RA03071J

data_7243120
_publ_section_title
;
 Synthesis, oligomerization and catalytic studies of a redox-active
 Ni4-cubane: a detailed mechanistic investigation
;
_journal_issue                   37
_journal_name_full               'RSC Advances'
_journal_page_first              22849
_journal_page_last               22858
_journal_paper_doi               10.1039/D1RA03071J
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C60 H53 Cl N4 Ni4 O12'
_chemical_formula_sum            'C60 H53 Cl N4 Ni4 O12'
_chemical_formula_weight         1292.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-28 deposited with the CCDC.	2021-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.577(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.831(2)
_cell_length_b                   23.697(5)
_cell_length_c                   14.715(3)
_cell_measurement_reflns_used    1340
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.34
_cell_measurement_theta_min      2.77
_cell_volume                     5863.1(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1545
_diffrn_reflns_av_unetI/netI     0.2051
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
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_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.206
_diffrn_reflns_theta_max         25.206
_diffrn_reflns_theta_min         1.630
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       Block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         10269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.1593
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4743
_reflns_number_total             10269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03071j2.cif
_cod_data_source_block           KK5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7243120
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.898
_shelx_res_checksum              67659
_shelx_fab_checksum              67664