Geometric and Electronic Structure of [{Cu(MeAN)}2(μ-η2:η2(O22-))]2+ with an Unusually Long O-O Bond: O-O Bond Weakening vs Activation for Reductive Cleavage
Ga Young Park; Munzarin F. Qayyum; Julia Woertink; Keith O. Hodgson; Britt Hedman; Amy A. Narducci Sarjeant; Edward I. Solomon; Kenneth D. Karlin; Journal of the American Chemical Society 134 (2012) 8513–8524; doi:10.1021/ja300674m

data_4117950
_publ_section_title
;
 Geometric and Electronic Structure of [{Cu(MeAN)}2(\m-\h2:\h2(O22-))]2+
 with an Unusually Long O-O Bond: O-O Bond Weakening vs Activation for
 Reductive Cleavage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8513
_journal_page_last               8524
_journal_paper_doi               10.1021/ja300674m
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C22 H54 Cu2 N6 O2, 2(C3 H6 O), 2 (F6 Sb)'
_chemical_formula_sum            'C28 H66 Cu2 F12 N6 O4 Sb2'
_chemical_formula_weight         1149.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.149(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.3759(2)
_cell_length_b                   21.4090(5)
_cell_length_c                   12.8492(3)
_cell_measurement_reflns_used    13165
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      31.02
_cell_measurement_theta_min      3.66
_cell_volume                     2201.68(10)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_solution    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21845
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    2.255
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
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            purple
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4304
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0339P)^2^+5.2309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                3570
_reflns_number_total             4304
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja300674m_si_002.cif
_cod_data_source_block           x0410a
_cod_database_code               4117950