Synthesis, characterization and magnetic properties of halogenated tetranuclear cubane-like nickel(ii) complexes
Aryaeifar, Mahnaz; Rudbari, Hadi Amiri; Moreno-Pineda, Eufemio; Cuevas-Vicario, José V.; Paul, Sagar; Schulze, Michael; Wernsdorfer, Wolfgang; Lloret, Francisco; Moini, Nakisa; Blacque, Olivier; New Journal of Chemistry 48 (2024) 3603–3613; doi:10.1039/D3NJ05585J

data_7063073
_publ_section_title
;
 Synthesis, characterization and magnetic properties of halogenated
 tetranuclear cubane-like nickel(ii) complexes
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3603
_journal_page_last               3613
_journal_paper_doi               10.1039/D3NJ05585J
_journal_volume                  48
_journal_year                    2024
_chemical_formula_sum            'C36 H40 Br4 Cl4 Ni4 O16'
_chemical_formula_weight         1424.96
_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-2016/6
_audit_update_record
;
2024-01-18 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.952(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1504(12)
_cell_length_b                   18.4070(14)
_cell_length_c                   15.3957(12)
_cell_measurement_reflns_used    8553
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      2.82
_cell_volume                     4859.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL (Sheldrick, 2015a)'
_diffrn_ambient_temperature      302(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            93557
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.848
_exptl_absorpt_coefficient_mu    5.099
_exptl_absorpt_correction_T_max  0.412
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.00048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         8553
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+58.0739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5603
_reflns_number_total             8553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj05585j2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7063073
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.207
_shelx_estimated_absorpt_t_max   0.268
_shelx_res_checksum              62110