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_4314618
_publ_contact_author             'Dr Gary S. Nichol'
_publ_contact_author_email       gsnichol@email.arizona.edu
_publ_contact_author_fax         '+1 520 621 8407'
_publ_contact_author_phone       '+1 520 621 4168'
_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         'C40 H78 N2 P4 Re6 Se8 2+, 2 Sb F6 -'
_chemical_formula_sum            'C40 H78 F12 N2 P4 Re6 Sb2 Se8'
_chemical_formula_weight         2931.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 115.038(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8376(5)
_cell_length_b                   38.9235(16)
_cell_length_c                   14.7586(6)
_cell_measurement_reflns_used    11872
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      3.32
_cell_volume                     6681.6(5)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 1999)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31139
_diffrn_reflns_theta_full        54.18
_diffrn_reflns_theta_max         54.18
_diffrn_reflns_theta_min         3.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    33.386
_exptl_absorpt_correction_T_max  0.2971
_exptl_absorpt_correction_T_min  0.0226
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.368
_refine_diff_density_min         -1.907
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       0.000015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         8072
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0861P)^2^+40.5412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1407
_reflns_number_gt                7148
_reflns_number_total             8072
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic902251z_si_003.cif
_cod_data_source_block           Complex4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4314618