Intramolecular Hydrogen Bonding Enhances Stability and Reactivity of Mononuclear Cupric Superoxide Complexes.
Bhadra, Mayukh; Lee, Jung Yoon C.; Cowley, Ryan E.; Kim, Sunghee; Siegler, Maxime A.; Solomon, Edward I.; Karlin, Kenneth D.; Journal of the American Chemical Society 140 (2018) 9042–9045; doi:10.1021/jacs.8b04671

data_4132529
_publ_section_title
;
 Intramolecular Hydrogen Bonding Enhances Stability and Reactivity of
 Mononuclear Cupric Superoxide Complexes.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9042
_journal_page_last               9045
_journal_paper_doi               10.1021/jacs.8b04671
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C25 H20 Cu1 F5 N8, C F3 S O3, 0.5(H2 O)'
_chemical_formula_sum            'C26 H21 Cu F8 N8 O3.5 S'
_chemical_formula_weight         749.11
_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
_cell_angle_alpha                113.519(2)
_cell_angle_beta                 94.289(2)
_cell_angle_gamma                95.9659(17)
_cell_formula_units_Z            16
_cell_length_a                   16.9714(4)
_cell_length_b                   25.4865(5)
_cell_length_c                   30.1352(7)
_cell_measurement_reflns_used    19045
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.99
_cell_measurement_theta_min      2.62
_cell_volume                     11790.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0818
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            139082
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.899
_diffrn_reflns_theta_min         1.911
_exptl_absorpt_coefficient_mu    2.609
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       'thick needle'
_exptl_crystal_F_000             6048
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.083
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4032
_refine_ls_number_reflns         46079
_refine_ls_number_restraints     3066
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0910P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28292
_reflns_number_total             46079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04671_si_004.cif
_cod_data_source_block           F5BA_CuII_N3_OTf
_cod_original_formula_sum        'C26 H21 Cu F8 N8 O3.50 S'
_cod_database_code               4132529
_oxdiff_exptl_absorpt_empirical_full_min 0.808
_oxdiff_exptl_absorpt_empirical_full_max 1.269
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2014-3
_shelx_res_checksum              81658
_shelx_hkl_checksum              77738