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_4125387
_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         'C21 H16 Cl4 Cu F6 N2 O'
_chemical_formula_sum            'C21 H16 Cl4 Cu F6 N2 O'
_chemical_formula_weight         631.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.146(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2563(7)
_cell_length_b                   19.6314(19)
_cell_length_c                   8.5775(8)
_cell_measurement_reflns_used    8711
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.59
_cell_volume                     1221.9(2)
_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      102(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15047
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.422
_diffrn_reflns_theta_min         2.591
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_T_max  0.94820
_exptl_absorpt_correction_T_min  0.79059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2580
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0294P)^2^+2.1579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2267
_reflns_number_total             2580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11332_si_007.cif
_cod_data_source_block           b16064_a
_cod_depositor_comments
'Adding full bibliography for 4125387--4125389.cif.'
_cod_database_code               4125387
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.645
_shelx_estimated_absorpt_t_max   0.909
_shelx_res_checksum              51991
_shelx_hkl_checksum              66789