Synthesis and Characterization of {Ni(NO)}10 and {Co(NO)2}10 Complexes Supported by Thiolate Ligands
Andrew G. Tennyson; Shanta Dhar; Stephen J. Lippard; Journal of the American Chemical Society 130 (2008) 15087–15098; doi:10.1021/ja803992y

data_4108632
_publ_section_title
;
 Synthesis and Characterization of {Ni(NO)}10 and {Co(NO)2}10 Complexes
 Supported by Thiolate Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15087
_journal_page_last               15098
_journal_paper_doi               10.1021/ja803992y
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C18 H15 Co3 N6 O6 S3'
_chemical_formula_weight         684.33
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.050(3)
_cell_length_b                   9.0194(15)
_cell_length_c                   32.227(6)
_cell_measurement_temperature    110(2)
_cell_volume                     4955.9(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart CCD Area Detector'
_diffrn_measurement_method       'Phi and omega 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  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            47123
_diffrn_reflns_theta_full        28.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    2.285
_exptl_absorpt_correction_T_max  0.6579
_exptl_absorpt_correction_T_min  0.6579
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       Plates
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+4.3920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                4666
_reflns_number_total             6185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja803992y_si_005.cif
_cod_data_source_block           at20
_cod_original_cell_volume        4955.8(15)
_cod_database_code               4108632