Lanthanoid Coordination Prompts Unusually Distorted Pseudo-Octahedral NiII Coordination in Heterodinuclear Ni-Ln Complexes: Synthesis, Structure and Understanding of Magnetic Behaviour through Experiment and Computation
Dutta, Biswarup; Guizouarn, Thierry; Pointillart, Fabrice; Kotrle, Kamil; Herchel, Radovan; Ray, Debashis; Dalton Transactions  (2023) –; doi:10.1039/D3DT01387A

data_7713326
_publ_section_title
;
 Lanthanoid Coordination Prompts Unusually Distorted Pseudo-Octahedral
 NiII Coordination in Heterodinuclear Ni-Ln Complexes: Synthesis,
 Structure and Understanding of Magnetic Behaviour through Experiment and
 Computation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01387A
_journal_year                    2023
_chemical_formula_moiety         'C30 H28 Er N5 Ni O13 S2, 0.5(O)'
_chemical_formula_sum            'C30 H28 Er N5 Ni O13.5 S2'
_chemical_formula_weight         964.645
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-08 deposited with the CCDC.	2023-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.063(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1700(7)
_cell_length_b                   21.0171(14)
_cell_length_c                   18.8670(12)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      2.369
_cell_volume                     3633.8(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31960
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.425
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    2.998
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1264 before and 0.0447 after correction.
The Ratio of minimum to maximum transmission is 0.6985.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             1916.0
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+3.7661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5473
_reflns_number_total             6412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01387a2.cif
_cod_data_source_block           biswarup_0m_a_CCDC1
_cod_original_formula_sum        'C30 H28 Er N5 Ni O13 S2, 0.5(O)'
_cod_database_code               7713326
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O1W(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C7(H7), C20(H20), C10(H10), C25(H25), C18(H18), C28(H28), C13(H13),
 C19(H19), C3(H3), C11(H11), C5(H5), C4(H4), C12(H12), C27(H27), C26(H26)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C22(H22A,H22B,H22C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              57616
_shelx_hkl_checksum              58916
_olex2_submission_special_instructions 'No special instructions were received'