Probing the electronic structure of a copper(II) complex with a ligand derived from a rare metal ion-assisted, crossed-aldol reaction of acetone with di-2-pyridyl ketone by cw- and pulse-EPR spectroscopy
Perlepes, Spyros P.; Lada, Zoi G.; Sanakis, Yiannis; Raptopoulou, Catherine P.; Psycharis, Vassilis; Mitrikas, George; Dalton Trans.  (2017) –; doi:10.1039/C7DT01785E

data_7043193
_publ_section_title
;
 Probing the electronic structure of a copper(II) complex with a ligand
 derived from a rare metal ion-assisted, crossed-aldol reaction of acetone
 with di-2-pyridyl ketone by cw- and pulse-EPR spectroscopy
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01785E
_journal_year                    2017
_chemical_formula_sum            'C28 H32 Cu N6 O12'
_chemical_formula_weight         708.13
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-05-04 deposited with the CCDC.
2017-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.4360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.63550(10)
_cell_length_b                   19.7062(4)
_cell_length_c                   10.2494(2)
_cell_measurement_reflns_used    10645
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      71.72
_cell_measurement_theta_min      6.69
_cell_volume                     1516.68(5)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  'publCIF J.Appl.Cryst. 2010, 43, 920'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13760
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.972
_diffrn_reflns_theta_min         7.052
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         2653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0455P)^2^+0.7495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2338
_reflns_number_total             2653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01785e2.cif
_cod_data_source_block           shelxl
_cod_database_code               7043193
_shelxl_version_number           2014/6
_shelx_res_checksum              54853