Copper(I)/O2 Chemistry with Imidazole Containing Tripodal Tetradentate Ligands Leading to μ-1,2-Peroxo-Dicopper(II) Species
Yunho Lee; Ga Young Park; Heather R. Lucas; Peter L. Vajda; Kaliappan Kamaraj; Michael A. Vance; Ashley E. Milligan; Julia S. Woertink; Maxime A. Siegler; Amy A. Narducci Sarjeant; Lev N. Zakharov; Arnold L. Rheingold; Edward I. Solomon; Kenneth D. Karlin; Inorganic Chemistry 48 (2009) 11297–11309; doi:10.1021/ic9017695

data_4303750
_publ_section_title
;
Copper(I)/O2 Chemistry with Imidazole Containing Tripodal Tetradentate
Ligands Leading to \m-1,2-Peroxo-Dicopper(II) Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11297
_journal_page_last               11309
_journal_paper_doi               10.1021/ic9017695
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C19 H22 Cl Cu N6 O4, Cl O4'
_chemical_formula_sum            'C19 H22 Cl2 Cu N6 O8'
_chemical_formula_weight         596.87
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.916(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2773(19)
_cell_length_b                   10.9131(16)
_cell_length_c                   15.564(4)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.84
_cell_measurement_theta_min      3.92
_cell_volume                     2372.8(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS_97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            12930
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.92
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.10 beta (release 25.09.2003 CrysAlis171 VC++)
(compiled Sep 25 2003,17:01:25)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4134
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                3158
_reflns_number_total             4134
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic9017695_si_001_2.cif
_cod_data_source_block           2c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4303750