Reversible methanol addition to copper Schiff base complexes: a kinetic, structural and spectroscopic study of reactions at azomethine C[double bond, length as m-dash]N bonds.
Zhang, Wuyu; Saraei, Nina; Nie, Hanlin; Vaughn, John R.; Jones, Alexis S.; Mashuta, Mark S.; Buchanan, Robert M.; Grapperhaus, Craig A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15791–15799; doi:10.1039/c6dt01955b

data_7039615
_publ_section_title
;
 Reversible methanol addition to copper Schiff base complexes: a kinetic,
 structural and spectroscopic study of reactions at azomethine C[double
 bond, length as m-dash]N bonds.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15791
_journal_page_last               15799
_journal_paper_doi               10.1039/c6dt01955b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 H16 N6, H2 O'
_chemical_formula_sum            'C12 H18 N6 O'
_chemical_formula_weight         262.32
_chemical_name_common            L1
_chemical_name_systematic
'[([(1-methyl-1H-imidazol-2-yl)methylidene] ({2-[(1-methyl-1H-imidazol-2-yl)methylidene]aminoethyl})amine) (perchlorato)copper(II)]perchlorate'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
<i>CrysAlis PRO</i> (Agilent, 2013) 
Version 1.171.36.32
;
_audit_update_record
;
2016-05-05 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.9045(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.37814(17)
_cell_length_b                   12.2120(2)
_cell_length_c                   11.9164(2)
_cell_measurement_reflns_used    11008
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      30.3410
_cell_measurement_theta_min      4.2070
_cell_volume                     1357.50(4)
_computing_cell_refinement       '<i>CrysAlis PRO</i> (Agilent, 2013)'
_computing_data_collection       '<i>CrysAlis PRO</i> (Agilent, 2013)'
_computing_data_reduction        '<i>CrysAlis PRO</i> (Agilent, 2013)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae<i>et al.</i>, 2006)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.95(10)
_diffrn_detector_area_resol_mean 10.2836
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   -8.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5172   57.0000  -30.0000 94

  2 omega  -11.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5172   77.0000 -180.0000 102

  3 omega   49.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5172   77.0000 -120.0000 44

  4 omega  -10.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5172   77.0000   60.0000 101

  5 omega  -44.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2047   57.0000  -90.0000 104

  6 omega  -44.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2047   57.0000 -180.0000 104

  7 omega  -44.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2047   57.0000    0.0000 104

  8 omega  -44.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2047   57.0000   60.0000 104

  9 omega  -15.00   16.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5172   57.0000 -150.0000 31

 10 omega  -19.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5172   77.0000   90.0000 112

;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0095
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16814
_diffrn_reflns_theta_full        29.56
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 SCALE3 ABSPACK.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.9486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                1755
_reflns_number_total             1902
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6dt01955b2.cif
_cod_data_source_block           cag204lta_last
_cod_depositor_comments
'Adding full bibliography for 7039610--7039615.cif.'
_cod_original_cell_volume        1357.49(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7039615
_solvent_exptl_crystal_recrystallization_method 'water at 4 deg C'