Peroxo and Superoxo Moieties Bound to Copper Ion: Electron-Transfer Equilibrium with a Small Reorganization Energy.
Cao, Rui; Saracini, Claudio; Ginsbach, Jake W.; Kieber-Emmons, Matthew T; Siegler, Maxime A.; Solomon, Edward I.; Fukuzumi, Shunichi; Karlin, Kenneth D.; Journal of the American Chemical Society 138 (2016) 7055–7066; doi:10.1021/jacs.6b02404

data_4130335
_publ_section_title
;
 Peroxo and Superoxo Moieties Bound to Copper Ion: Electron-Transfer
 Equilibrium with a Small Reorganization Energy.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7055
_journal_page_last               7066
_journal_paper_doi               10.1021/jacs.6b02404
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C35 H36.11 Cl Cu2 N6.89 O2.77, 2(F6 Sb), 2(C H2 Cl2)'
_chemical_formula_sum            'C37 H40.11 Cl5 Cu2 F12 N6.89 O2.78 Sb2'
_chemical_formula_weight         1401.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                106.146(2)
_cell_angle_beta                 93.216(2)
_cell_angle_gamma                107.792(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5135(2)
_cell_length_b                   13.8420(3)
_cell_length_c                   20.1911(5)
_cell_measurement_reflns_used    13063
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.12
_cell_volume                     2402.75(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 15.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29451
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.249
_diffrn_reflns_theta_min         2.126
_exptl_absorpt_coefficient_mu    2.354
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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            yellow
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_description       plate
_exptl_crystal_F_000             1371
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         9714
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+2.0098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8386
_reflns_number_total             9714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b02404_si_004.cif
_cod_data_source_block           Cl
_cod_database_code               4130335
_shelx_shelxl_version_number     2014/7
_additional_information_molecular_formula
;
The crystal is a phase mixture, for which the major component
has the nitrato group attached to C17 with an occupancy of 0.886(4).
The minor component being that for which one H atom is attached
to C17 (which was initially the expected ligand).
After tackling the phase mixture problem,
the refinement turned out to be problem free.
;
_shelx_res_checksum              37395
_shelx_hkl_checksum              27647