A N3S(thioether)-Ligated Cu(II)-Superoxo with Enhanced Reactivity.
Kim, Sunghee; Lee, Jung Yoon; Cowley, Ryan E.; Ginsbach, Jake W.; Siegler, Maxime A.; Solomon, Edward I.; Karlin, Kenneth D.; Journal of the American Chemical Society 137 (2015) 2796–2799; doi:10.1021/ja511504n

data_4123467
_publ_section_title
;
 A N3S(thioether)-Ligated Cu(II)-Superoxo with Enhanced Reactivity.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2796
_journal_page_last               2799
_journal_paper_doi               10.1021/ja511504n
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H35 Cu N7 O, 2(Cl O4)'
_chemical_formula_sum            'C24 H35 Cl2 Cu N7 O9'
_chemical_formula_weight         700.03
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_symmetry_space_group_name_Hall  'P 65'
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_cell_angle_gamma                120
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_cell_measurement_reflns_used    13864
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      72.03
_cell_measurement_theta_min      3.36
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19557
_diffrn_reflns_point_group_measured_fraction_full 0.817
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.821
_diffrn_reflns_theta_min         3.391
_exptl_absorpt_coefficient_mu    3.240
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.486
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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            green
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       rod
_exptl_crystal_F_000             2178
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 1614 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.013(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         4703
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+1.2738P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.568
_reflns_Friedel_fraction_full    0.624
_reflns_Friedel_fraction_max     0.599
_reflns_number_gt                4565
_reflns_number_total             4703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja511504n_si_002.cif
_cod_data_source_block           xs0399a
_cod_depositor_comments
'Adding full bibliography for 4123467--4123469.cif.'
_cod_original_cell_volume        4458.52(13)
_cod_database_code               4123467
_shelxl_version_number           2013-2
_shelx_res_checksum              31732
_shelx_hkl_checksum              88453