Migratory Insertion of Hydrogen Isocyanide in the Pentacyano(methyl)cobaltate(III) Anion
Pauli Kofod; Pernille Harris; Sine Larsen; Inorganic Chemistry 42 (2003) 244–249; doi:10.1021/ic020353u

data_4312859
_publ_section_title
;
 Migratory Insertion of Hydrogen Isocyanide in the
 Pentacyano(methyl)cobaltate(III) Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              244
_journal_page_last               249
_journal_paper_doi               10.1021/ic020353u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'N0.5 C4 H10, As C24 H20, Co0.5 N2.5 C3 H1.5'
_chemical_formula_sum            'C31 H31.5 As Co0.5 N3'
_chemical_formula_weight         550.48
_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                65.01(2)
_cell_angle_beta                 82.11(2)
_cell_angle_gamma                73.36(2)
_cell_formula_units_Z            2
_cell_length_a                   10.724(2)
_cell_length_b                   11.070(2)
_cell_length_c                   12.923(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      20.50
_cell_measurement_theta_min      17.93
_cell_volume                     1332.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16006
_diffrn_reflns_theta_full        32.46
_diffrn_reflns_theta_max         32.46
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        3.4
_diffrn_standards_interval_time  155.7
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.601
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         9626
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0502P)^2^+0.6809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                8194
_reflns_number_total             9626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020353u.cif
_cod_data_source_block           nyfix
_cod_original_formula_sum        'C31 H31.5 As1 Co0.5 N3'
_cod_database_code               4312859