Interesting chemical and physical features in the products of the reactions between trivalent lanthanoids and a tetradentate Schiff base derived from cyclohexane-1,2-diamine
Mylonas-Margaritis, Ioannis; Lada, Zoi G.; Kitos, Alexandros; Maniaki, Diamantoula; Skordi, Katerina; Tasiopoulos, Anastasios; Bekiari, Vlasoula; Escuer, Albert; Mayans, Julia; Nastopoulos, Vasilis; Bakalbassis, Evangelos; Papaioannou, Dionissios A.; Perlepes, Spyros; Dalton Transactions  (2023) –; doi:10.1039/D3DT00817G

data_7713022
_publ_section_title
;
 Interesting chemical and physical features in the products of the
 reactions between trivalent lanthanoids and a tetradentate Schiff base
 derived from cyclohexane-1,2-diamine
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00817G
_journal_year                    2023
_chemical_formula_moiety         'C23 H32 N5 O12 Sm'
_chemical_formula_sum            'C23 H32 N5 O12 Sm'
_chemical_formula_weight         720.88
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-03-04 deposited with the CCDC.	2023-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                72.600(4)
_cell_angle_beta                 82.703(4)
_cell_angle_gamma                73.013(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0397(4)
_cell_length_b                   10.8222(6)
_cell_length_c                   15.4002(7)
_cell_measurement_reflns_used    4667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8170
_cell_measurement_theta_min      3.9130
_cell_volume                     1373.63(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics
'PLATON v.270519 (Spek, 2009); MERCURY v.2020.3.0 (Macrae et al. 2020)'
_computing_publication_material
'WINGX v.2018.3 (Farrugia, 2012); OLEX2 v.1.3.0 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4223
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova with Atlas CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11005
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.308
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.209
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             726
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/dichloromethane'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5937
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0180P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5234
_reflns_number_total             5937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00817g2.cif
_cod_data_source_block           3_xrp110
_cod_database_code               7713022
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.679
_shelx_estimated_absorpt_t_max   0.793
_shelx_res_checksum              34084
_shelx_hkl_checksum              27108