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_7039613
_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
;  
C15 H24 Cu F3 N6 O5 S, C F3 O3 S, 0.67(H2 O) 
;
_chemical_formula_sum            'C16 H25.34 Cu F6 N6 O8.67 S2'
_chemical_formula_weight         682.15
_chemical_name_common
;
[L2Cu(HOCH3)][O3SCF3]2
;
_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           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-05-05 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                93.3069(14)
_cell_angle_beta                 103.0089(16)
_cell_angle_gamma                107.1032(17)
_cell_formula_units_Z            2
_cell_length_a                   8.30645(16)
_cell_length_b                   12.6697(2)
_cell_length_c                   13.6657(2)
_cell_measurement_reflns_used    15940
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      30.9810
_cell_measurement_theta_min      3.8050
_cell_volume                     1327.40(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      100.0(6)
_diffrn_detector_area_resol_mean 10.2836
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -5.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1621   57.0000    0.0000 95

  2 omega  -17.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1621   77.0000  120.0000 98

  3 omega   -2.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1621   77.0000 -180.0000 39

  4 omega  -28.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1621  -77.0000   90.0000 26

  5 omega  -50.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1621  -57.0000 -150.0000 95

  6 omega  -90.00  -13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.8496  -57.0000   60.0000 77

  7 omega  -45.00   58.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.8496   57.0000   90.0000 103

  8 omega  -58.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1621  -57.0000  -90.0000 104

  9 omega  -63.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1621  -77.0000 -180.0000 113

 10 omega  -13.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1621   57.0000 -120.0000 103

 11 omega  -58.00   17.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.1621  -57.0000    0.0000 75

;
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34182
_diffrn_reflns_theta_full        29.20
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 SCALE3 ABSPACK.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             695.4
_exptl_crystal_recrystallization_method
'vapor diffussion of ether into methanol'
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.718
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7190
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+3.4100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                6645
_reflns_number_total             7190
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6dt01955b2.cif
_cod_data_source_block           cag238lta_6
_cod_depositor_comments
'Adding full bibliography for 7039610--7039615.cif.'
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_formula_sum
;
 C16 H25.34 Cu F6 N6 O8.67 S2
;
_cod_database_code               7039613