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_4105459
_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            'C50 H59 N5 Ni2 O'
_chemical_formula_weight         863.44
_chemical_name_common            {[Me2NN]Ni}2(m-h2:h2-ONAr)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.517(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.171(3)
_cell_length_b                   13.684(2)
_cell_length_c                   19.160(4)
_cell_measurement_reflns_used    4799
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.432
_cell_measurement_theta_min      2.197
_cell_volume                     4500.4(14)
_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  0.1082
_diffrn_reflns_av_sigmaI/netI    0.1004
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33208
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.834
_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            dark_green
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.00027(14)
_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   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                4901
_reflns_number_total             7909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903550n_si_003.cif
_cod_data_source_block           cmpd_1a_{[Me2NN]Ni}2(m-h2:h2-ONAr)
_cod_original_cell_volume        4500.5(14)
_cod_database_code               4105459