Phenol Reduces Nitrite to NO at Copper(II): Role of a Proton-Responsive Outer Coordination Sphere in Phenol Oxidation.
Mondal, Aditesh; Reddy, Kiran P.; Bertke, Jeffery A.; Kundu, Subrata; Journal of the American Chemical Society 142 (2020) 1726–1730; doi:10.1021/jacs.9b11597

data_4133965
_publ_contact_author             'Subrata Kundu'
_publ_section_title
;
 Phenol Reduces Nitrite to NO at Copper(II): Role of a Proton-Responsive
 Outer Coordination Sphere in Phenol Oxidation.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1726
_journal_page_last               1730
_journal_paper_doi               10.1021/jacs.9b11597
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C33 H45 Cu N6 O5, Cl O4, 0.174(H2 O)'
_chemical_formula_sum            'C33 H45.35 Cl Cu N6 O9.17'
_chemical_formula_weight         771.87
_chemical_name_common            '[mC]Cu(O2N)(ClO4)'
_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     intrinsic
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                112.421(4)
_cell_angle_beta                 110.003(5)
_cell_angle_gamma                96.959(5)
_cell_formula_units_Z            2
_cell_length_a                   12.2345(19)
_cell_length_b                   12.3329(18)
_cell_length_c                   13.275(2)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.50
_cell_volume                     1665.3(4)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
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_computing_structure_refinement  'SHELX-2018-3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker APEX ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25117
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.504
_diffrn_reflns_theta_min         2.510
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             809
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         6862
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0328P)^2^+1.0276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6036
_reflns_number_total             6862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11597_si_002.cif
_cod_data_source_block           AM29F
_cod_depositor_comments
'Adding full bibliography for 4133963--4133966.cif.'
_cod_database_code               4133965
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              5438
_shelx_hkl_checksum              63354