Coordination properties of N,N′-bis(5-methylsalicylidene)-2-hydroxy-1,3-propanediamine with d- and f-electron ions: crystal structure, stability in solution, spectroscopic and spectroelectrochemical studies
Kaczmarek, Malgorzata T.; Skrobanska, Monika; Zabiszak, Michal; Wałęsa-Chorab, Monika; Kubicki, Maciej; Jastrzab, Renata; RSC Advances 8 (2018) 30994–; doi:10.1039/C8RA03565B

data_7231496
_publ_section_title
;
 Coordination properties of
 N,N&#x2032;-bis(5-methylsalicylidene)-2-hydroxy-1,3-propanediamine with
 d- and f-electron ions: crystal structure, stability in solution,
 spectroscopic and spectroelectrochemical studies
;
_journal_issue                   54
_journal_name_full               'RSC Advances'
_journal_page_first              30994
_journal_paper_doi               10.1039/C8RA03565B
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C22 H26 Cu2 N2 O6, C H4 O'
_chemical_formula_sum            'C23 H30 Cu2 N2 O7'
_chemical_formula_weight         573.57
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-08-21 deposited with the CCDC.
2018-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.548(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4733(4)
_cell_length_b                   9.9490(2)
_cell_length_c                   15.8181(6)
_cell_measurement_reflns_used    3602
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      26.3420
_cell_measurement_theta_min      3.3640
_cell_volume                     2401.37(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.34a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.34a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.34a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '/w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9312
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         3.319
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0337P)^2^+0.8695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3958
_reflns_number_total             4604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra03565b2.cif
_cod_data_source_block           1
_cod_database_code               7231496
_shelxl_version_number           2013-4
_shelx_res_checksum              51224