Nitric Oxide Oxidatively Nitrosylates Ni(I) and Cu(I) C-Organonitroso Adducts
Stefan Wiese; Pooja Kapoor; Kamille D. Williams; Timothy H. Warren; Journal of the American Chemical Society 131 (2009) 18105–18111; doi:10.1021/ja903550n

data_4105460
_publ_contact_author             'Timothy H. Warren'
_publ_contact_author_email       thw@georgetown.edu
_publ_section_title
;
 Nitric Oxide Oxidatively Nitrosylates Ni(I) and Cu(I) C-Organonitroso
 Adducts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18105
_journal_page_last               18111
_journal_paper_doi               10.1021/ja903550n
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C52 H64 Cu2 N5 O1.5'
_chemical_formula_weight         910.16
_chemical_name_common            '{[Me2NN]Cu}2(m-h2:h1-ONAr) + 0.5 ether'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.64(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.714(11)
_cell_length_b                   11.670(2)
_cell_length_c                   23.333(5)
_cell_measurement_reflns_used    4332
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.446
_cell_measurement_theta_min      2.285
_cell_volume                     9705(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics
'ORTEP-3 for Windows; Ferrugia L J (1997), J. Appl. Cryst. 30, 565'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_sigmaI/netI    0.1035
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22490
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.795
_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            black
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.00077(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         8547
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+5.2269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2053
_reflns_number_gt                5689
_reflns_number_total             8547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903550n_si_004.cif
_cod_data_source_block           cmpd_2a_{[Me2NN]Cu}2(m-h2:h1-ONAr)
_cod_original_formula_sum        'C52 H64 Cu2 N5 O1.50'
_cod_database_code               4105460