Two Ni/Ce complexes based on bicompartmental ligands with field supported slow magnetic relaxation
Krešáková, Lenka; Litecká, Miroslava; Oyarzabal, Itziar; Titiš, Ján; Červeňáková, Michaela; Hillard, Elizabeth A.; Robert, Jerome; Černák, Juraj; New Journal of Chemistry 48 (2024) 17750–17760; doi:10.1039/D4NJ03545C

data_7063475
_publ_section_title
;
 Two Ni/Ce complexes based on bicompartmental ligands with field supported
 slow magnetic relaxation
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17750
_journal_page_last               17760
_journal_paper_doi               10.1039/D4NJ03545C
_journal_volume                  48
_journal_year                    2024
_chemical_formula_sum            'C21 H28 Ce N5 Ni O15'
_chemical_formula_weight         789.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-09-23 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.8440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.87460(10)
_cell_length_b                   16.0480(2)
_cell_length_c                   10.07710(10)
_cell_measurement_reflns_used    13395
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.4630
_cell_measurement_theta_min      2.7630
_cell_volume                     1434.43(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13419
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         77.891
_diffrn_reflns_theta_min         4.390
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    13.635
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (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    1.827
_exptl_crystal_description       block
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.210
_refine_diff_density_max         3.225
_refine_diff_density_min         -2.320
_refine_diff_density_rms         0.204
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.

 The final difference map contained 
 high peaks (highest of 3.22 e per A3) 
 and high holes (highest of -2.32 e per A3);
 these are situated near the Ce1 and Ni1 atoms. 

;
_refine_ls_abs_structure_Flack   0.017(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5473
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0621
_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^)+(0.1448P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.843
_reflns_number_gt                5445
_reflns_number_total             5473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03545c2.cif
_cod_data_source_block           Structure2-lk17b
_cod_depositor_comments
'Adding full bibliography for 7063474--7063475.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7063475
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.062
_shelx_estimated_absorpt_t_max   0.162
_shelx_res_checksum              45544
_shelx_hkl_checksum              23025