Synthesis of Co(II)-NO(-) Complexes and Their Reactivity as a Source of Nitroxyl.
Walter, Melody R.; Dzul, Stephen P.; Rodrigues, Andria V.; Stemmler, Timothy L.; Telser, Joshua; Conradie, Jeanet; Ghosh, Abhik; Harrop, Todd C.; Journal of the American Chemical Society 138 (2016) 12459–12471; doi:10.1021/jacs.6b05896

data_4130701
_publ_section_title
;
 Synthesis of Co(II)-NO(-) Complexes and Their Reactivity as a Source of
 Nitroxyl.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12459
_journal_page_last               12471
_journal_paper_doi               10.1021/jacs.6b05896
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C16 H12 Co N5 O'
_chemical_formula_weight         349.24
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                96.3220(10)
_cell_angle_beta                 96.0850(10)
_cell_angle_gamma                98.4760(10)
_cell_formula_units_Z            4
_cell_length_a                   8.7573(7)
_cell_length_b                   9.2971(8)
_cell_length_c                   17.9518(15)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.764
_cell_measurement_theta_min      2.233
_cell_volume                     1425.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART APEX II'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6201
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_T_max  0.8881
_exptl_absorpt_correction_T_min  0.6757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER TWINABS'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.791
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6201
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0804P)^2^+2.1422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                5862
_reflns_number_total             6201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b05896_si_002.cif
_cod_data_source_block           twin5
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4130701