Copper catalysed aerobic oxidation of benzylic alcohols in an imidazole containing N4 ligand framework.
Jain, Rahul; Gibson, Tony J.; Mashuta, Mark S.; Buchanan, Robert M.; Grapperhaus, Craig A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18356–18364; doi:10.1039/c6dt03395d

data_7041063
_publ_section_title
;
 Copper catalysed aerobic oxidation of benzylic alcohols in an imidazole
 containing N4 ligand framework.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18356
_journal_page_last               18364
_journal_paper_doi               10.1039/c6dt03395d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 H20 Cl2 Cu N6 O8'
_chemical_formula_sum            'C12 H20 Cl2 Cu N6 O8'
_chemical_formula_weight         510.78
_chemical_name_common            'L3-Cu[ClO4]2 '
_chemical_name_systematic
;
ligand [(1-methyl-4,5-dihydro-1H-imidazol-2-yl)methyl](2-ethyl)amine]Cu[ClO4]2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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
;
2016-08-29 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.258(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.244(2)
_cell_length_b                   8.1023(10)
_cell_length_c                   13.7251(15)
_cell_measurement_reflns_used    8692
_cell_measurement_temperature    100.05(10)
_cell_measurement_theta_max      30.6430
_cell_measurement_theta_min      3.7450
_cell_volume                     1906.2(4)
_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)'
_computing_structure_refinement  '<i>SHELXL</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.05(10)
_diffrn_detector_area_resol_mean 10.2836
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -11.00   14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9321   77.0000  -90.0000 25

  2 omega  -58.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2446  -57.0000  120.0000 101

  3 omega  -16.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2446   77.0000  -60.0000 105

  4 omega  -45.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9321   57.0000 -120.0000 104

  5 omega  -59.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2446  -57.0000   30.0000 62

;
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19245
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/diethyl ether'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         4656
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0426P)^2^+3.9846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                4176
_reflns_number_total             4656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03395d2.cif
_cod_data_source_block           rmb335ltb
_cod_depositor_comments
'Adding full bibliography for 7041063--7041064.cif.'
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7041063