A New Route to Coordination Complexes of Nitroxyl (HNO) via Insertion Reactions of Nitrosonium Triflate with Transition-Metal Hydrides
Rory Melenkivitz; Joel S. Southern; Gregory L. Hillhouse; Thomas E. Concolino; Louise M. Liable-Sands; Arnold L. Rheingold; Journal of the American Chemical Society 124 (2002) 12068–12069; doi:10.1021/ja0277475

data_4115202
_publ_section_title
;
 A New Route to Coordination Complexes of Nitroxyl (HNO) via Insertion
 Reactions of Nitrosonium Triflate with Transition-Metal Hydrides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12068
_journal_page_last               12069
_journal_paper_doi               10.1021/ja0277475
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C47 H41 F6 N2 O3.5 P3 Re'
_chemical_formula_weight         1082.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.88(2)
_cell_angle_beta                 79.511(14)
_cell_angle_gamma                78.031(10)
_cell_formula_units_Z            2
_cell_length_a                   10.746(2)
_cell_length_b                   13.136(2)
_cell_length_c                   17.475(3)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    261(2)
_cell_measurement_theta_max      12.54
_cell_measurement_theta_min      4.76
_cell_volume                     2297.8(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      261(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8732
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.816
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            light_orange
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                6197
_reflns_number_total             7507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0277475_s2.cif
_cod_data_source_block           hil04
_cod_original_cell_volume        2298.0(8)
_cod_original_formula_sum        'C47 H41 F6 N2 O3.50 P3 Re'
_cod_database_code               4115202