Copper(II) Activation of Nitrite: Nitrosation of Nucleophiles and Generation of NO by Thiols.
Kundu, Subrata; Kim, William Y.; Bertke, Jeffery A.; Warren, Timothy H.; Journal of the American Chemical Society 139 (2017) 1045–1048; doi:10.1021/jacs.6b11332

data_4125389
_publ_contact_author             'Timothy H. Warren'
_publ_section_title
;
 Copper(II) Activation of Nitrite: Nitrosation of Nucleophiles and
 Generation of NO by Thiols.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1045
_journal_page_last               1048
_journal_paper_doi               10.1021/jacs.6b11332
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C39 H37 Cl4 Cu F6 N2 S2'
_chemical_formula_sum            'C39 H37 Cl4 Cu F6 N2 S2'
_chemical_formula_weight         917.16
_chemical_name_systematic        '[Cl2NNF6]Cu(tBuBnSSBntBu)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9172(11)
_cell_length_b                   17.5654(10)
_cell_length_c                   25.9568(15)
_cell_measurement_reflns_used    9738
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.145
_cell_measurement_theta_min      2.258
_cell_volume                     8169.2(8)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4 (Bruker, 2014) 
;
_computing_molecular_graphics    'SHELXTL v2014-4 (Bruker, 2014)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            103316
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.187
_diffrn_reflns_theta_min         2.258
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.290
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         11009
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0265P)^2^+6.0587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9048
_reflns_number_total             11009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11332_si_004.cif
_cod_data_source_block           tryPbca
_cod_depositor_comments
'Adding full bibliography for 4125387--4125389.cif.'
_cod_database_code               4125389
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.673
_shelx_estimated_absorpt_t_max   0.769
_shelx_res_checksum              31947
_shelx_hkl_checksum              52465