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_4132526
_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 H25 Cu N8, Cl O4'
_chemical_formula_sum            'C25 H25 Cl Cu N8 O4'
_chemical_formula_weight         600.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
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_cell_length_a                   9.47238(10)
_cell_length_b                   9.82216(11)
_cell_length_c                   27.9989(3)
_cell_measurement_reflns_used    18128
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      72.04
_cell_measurement_theta_min      3.15
_cell_volume                     2573.32(5)
_computing_cell_refinement
;
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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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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_diffrn_measured_fraction_theta_full 1.000
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_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  0.0276
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_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32629
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.890
_diffrn_reflns_theta_min         3.196
_exptl_absorpt_coefficient_mu    2.576
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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    1.550
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_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         5052
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0399P)^2^+1.2947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4654
_reflns_number_total             5052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04671_si_002.cif
_cod_data_source_block           BA_CuII_N3_ClO4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132526
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              40638
_shelx_hkl_checksum              68947