Simple and versatile selective synthesis of neutral and cationic copper(I) N-heterocyclic carbene complexes using an electrochemical procedure
Benjamin R. M. Lake; Emma K. Bullough; Thomas J. Williams; Adrian C. Whitwood; Marc A. Little; Charlotte E. Willans; Chem.Commun. 48 (2012) 4887–; doi:10.1039/c2cc30862b

data_7107648
_publ_section_title
;
 Simple and versatile selective synthesis of neutral and cationic
 copper(I) N-heterocyclic carbene complexes using an electrochemical
 procedure
;
_journal_name_full               Chem.Commun.
_journal_page_first              4887
_journal_paper_doi               10.1039/c2cc30862b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C42 H36 Br2 Cu2 N4'
_chemical_formula_sum            'C42 H36 Br2 Cu2 N4'
_chemical_formula_weight         883.65
_chemical_name_systematic
;
?
;
_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_creation_date             2011-09-13
_audit_creation_method
;
Olex2 1.1
(compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                69.206(7)
_cell_angle_beta                 82.837(6)
_cell_angle_gamma                69.262(6)
_cell_formula_units_Z            1
_cell_length_a                   9.4581(6)
_cell_length_b                   9.5482(7)
_cell_length_c                   11.2949(10)
_cell_measurement_reflns_used    3571
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      31.2520
_cell_measurement_theta_min      2.9964
_cell_volume                     891.79(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details
;
1 omega -35.00 9.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -23.1156 -84.0000 -133.0000 44

2 omega -20.00 67.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 24.6781 -99.0000 0.0000 87

3 omega 60.00 101.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 24.6781 -178.0000 -180.0000 41

4 omega 4.00 89.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 24.6781 57.0000 -150.0000 85

5 omega -46.00 97.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 24.6781 0.0000 0.0000 143
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0773826000
_diffrn_orient_matrix_UB_12      -0.0281660000
_diffrn_orient_matrix_UB_13      0.0168238000
_diffrn_orient_matrix_UB_21      0.0207234000
_diffrn_orient_matrix_UB_22      -0.0171925000
_diffrn_orient_matrix_UB_23      -0.0571610000
_diffrn_orient_matrix_UB_31      0.0035803000
_diffrn_orient_matrix_UB_32      0.0775774000
_diffrn_orient_matrix_UB_33      -0.0310147000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8485
_diffrn_reflns_theta_full        29.07
_diffrn_reflns_theta_max         31.32
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.470
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dull ? colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.1108
_exptl_crystal_size_min          0.0626
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.6919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                4252
_reflns_number_total             5176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc30862b.txt
_cod_data_source_block           ijsf1115
_cod_original_cell_volume        891.80(12)
_cod_database_code               7107648
_chemical_oxdiff_formula         'C21 H18 Br1 Cu1 N2'
_chemical_oxdiff_usercomment     'Tom's BRML58'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.07