Cluster-Bound Nitriles Do Not Click with Organic Azides: Unexpected Formation of Imino Complexes of the [Re6(μ3-Se)8]2+ Core-Containing Clusters
Xiaoyan Tu; Ethan Boroson; Huong Truong; Alvaro Muñoz-Castro; Ramiro Arratia-Pérez; Gary, S. Nichol; Zhiping Zheng; Inorganic Chemistry 49 (2010) 380–382; doi:10.1021/ic902251z

data_4314617
_publ_contact_author             'Dr Zhiping Zheng'
_publ_contact_author_email       zhiping@email.arizona.edu
_publ_contact_author_fax         '+1 520 626 6495'
_publ_contact_author_phone       '+1 520 626 6495'
_publ_section_title
;
 Cluster-Bound Nitriles Do Not Click with Organic Azides: Unexpected
 Formation of Imino Complexes of the [Re6(\m3-Se)8]2+ Core-Containing
 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              380
_journal_page_last               382
_journal_paper_doi               10.1021/ic902251z
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C38 H84 N P5 Re6 Se8 2+, 2 C24 H20 B -, C7 H8'
_chemical_formula_sum            'C93 H132 B2 N P5 Re6 Se8'
_chemical_formula_weight         3189.35
_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                96.744(2)
_cell_angle_beta                 92.112(2)
_cell_angle_gamma                91.052(2)
_cell_formula_units_Z            2
_cell_length_a                   16.870(2)
_cell_length_b                   17.192(2)
_cell_length_c                   17.913(2)
_cell_measurement_reflns_used    5201
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.79
_cell_volume                     5154.5(10)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube with Miracol optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35633
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    9.961
_exptl_absorpt_correction_T_max  0.6203
_exptl_absorpt_correction_T_min  0.2986
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3010
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.421
_refine_diff_density_min         -3.198
_refine_diff_density_rms         0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         19336
_refine_ls_number_restraints     609
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.0812
_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^)+(0.1084P)^2^+132.3695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2572
_reflns_number_gt                9183
_reflns_number_total             19336
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic902251z_si_002.cif
_cod_data_source_block           Complex3
_cod_original_cell_volume        5154.6(12)
_cod_database_code               4314617