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_7039612
_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         'C14 H24 Cl Cu N6 O6, Cl O4'
_chemical_formula_sum            'C14 H24 Cl2 Cu N6 O10'
_chemical_formula_weight         570.83
_chemical_name_common
;
[L2Cu(HOCH3)][ClO4]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           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                90.00
_cell_angle_beta                 104.371(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0049(3)
_cell_length_b                   11.5913(2)
_cell_length_c                   15.1039(4)
_cell_measurement_reflns_used    40630
_cell_measurement_temperature    100.1(6)
_cell_measurement_theta_max      30.4300
_cell_measurement_theta_min      3.6180
_cell_volume                     2205.57(9)
_computing_cell_refinement       '<i>CrysAlis PRO</i> (Agilent, 2010)'
_computing_data_collection       '<i>CrysAlis PRO</i> (Agilent, 2010)'
_computing_data_reduction        '<i>CrysAlis PRO</i> (Agilent, 2010)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material
'PLATON (Spek, 2009) and publCIF (Westrip, 2010)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.1(6)
_diffrn_detector_area_resol_mean 10.2836
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -89.00  -18.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7707  -57.0000 -120.0000 71

  2 omega    9.00   67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832   57.0000  120.0000 58

  3 omega  -43.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -77.0000  150.0000 92

  4 omega  -53.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -77.0000  -60.0000 98

  5 omega  -25.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -77.0000 -150.0000 74

  6 omega  -44.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -77.0000   30.0000 93

  7 omega  -19.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832   77.0000    0.0000 109

  8 omega  -13.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832   57.0000 -150.0000 78

  9 omega  -44.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7707   57.0000    0.0000 103

 10 omega  -93.00   19.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7707  -77.0000  120.0000 112

 11 omega  -44.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7707   57.0000 -120.0000 103

 12 omega  -89.00   15.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7707  -57.0000  -30.0000 104

 13 omega  -93.00   19.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7707  -77.0000 -120.0000 112

 14 omega  -64.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -77.0000   90.0000 113

 15 omega  -64.00  -10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -77.0000  -60.0000 54

 16 omega  -64.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -77.0000 -180.0000 113

;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            83528
_diffrn_reflns_theta_full        28.16
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80854
_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    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1172
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.847
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.355(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         10813
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0475P)^2^+2.9100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                10434
_reflns_number_total             10813
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c6dt01955b2.cif
_cod_data_source_block           rmb73ltb_5
_cod_depositor_comments
'Adding full bibliography for 7039610--7039615.cif.'
_cod_original_sg_symbol_Hall     'P -2yac '
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7039612
_solvent_exptl_crystal_recrystallization_method methanol/ether