Mechanistic studies on the in-situ generation of furoxan ring during the formation of Cu(II) coordination compound from dioxime ligand: Theoretical and experimental study
Bikas, Rahman; Valadbeigi, Younes; Otręba, Marta; Lis, Tadeusz; Inorganica Chimica Acta 510 (2020) 119756–; doi:10.1016/j.ica.2020.119756

data_1564426
_publ_section_title
;
 Mechanistic studies on the in-situ generation of furoxan ring during the
 formation of Cu(II) coordination compound from dioxime ligand:
 Theoretical and experimental study
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119756
_journal_paper_doi               10.1016/j.ica.2020.119756
_journal_volume                  510
_journal_year                    2020
_chemical_formula_moiety         'C12 H8 Cu N6 O8'
_chemical_formula_sum            'C12 H8 Cu N6 O8'
_chemical_formula_weight         427.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.468(3)
_cell_length_b                   14.359(4)
_cell_length_c                   20.227(5)
_cell_measurement_reflns_used    15525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     3040.3(14)
_computing_cell_refinement
'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_data_collection
'CrysAlis CCD; Oxford-Diffraction Poland, 2003'
_computing_data_reduction
'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.579
_diffrn_measurement_device_type
;
Kuma KM4 kappa-geometry diffractometer with a CCD detector
;
_diffrn_measurement_method       /w
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.579
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24177
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.579
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         36.787
_diffrn_reflns_theta_min         3.011
_exptl_absorpt_coefficient_mu    1.500
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.260
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0792P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3669
_reflns_number_total             4412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-510-119751.cif
_cod_data_source_block           b2411a
_cod_database_code               1564426
_shelx_estimated_absorpt_t_min   0.533
_shelx_estimated_absorpt_t_max   0.696
_shelxl_version_number           2013-2
_shelx_res_checksum              60225
_shelx_hkl_checksum              97160