Synthesis, Structure, and Chemistry of New, Mixed Group 14 and 16 Heterocycles: Nucleophile-Induced Ring Contraction of Mesocyclic Dications
Eric Block; Evgeny V. Dikarev; Richard S. Glass; Jin Jin; Bo Li; Xiaojie Li; Shao-Zhong Zhang; Journal of the American Chemical Society 128 (2006) 14949–14961; doi:10.1021/ja065037j

data_4111079
_publ_section_title
;
 Synthesis, Structure, and Chemistry of New, Mixed Group 14 and 16
 Heterocycles: Nucleophile-Induced Ring Contraction of Mesocyclic
 Dications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14949
_journal_page_last               14961
_journal_paper_doi               10.1021/ja065037j
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety
;
 'Rh2 (O2 C C F3)4 Se (C H2)2 Si (C H3)2'
;
_chemical_formula_sum            'C12 H10 F12 O8 Rh2 Se Si'
_chemical_formula_weight         823.07
_chemical_name_systematic
; 
 catena-((3,3-bis-methyl-1,3-selenasiletane)
 -dirhodium(ii)-tetratrifluoroacetate) 
;
_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                65.7790(10)
_cell_angle_beta                 73.4060(10)
_cell_angle_gamma                80.7200(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5735(7)
_cell_length_b                   11.3637(8)
_cell_length_c                   13.0078(9)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      1.77
_cell_volume                     1235.23(15)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide \w exposures'
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10828
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    2.983
_exptl_absorpt_correction_T_max  0.7963
_exptl_absorpt_correction_T_min  0.6632
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.213
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5513
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0436
_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^+6.3287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                4488
_reflns_number_total             5513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065037jsi20060721_015341.cif
_cod_data_source_block           C12H10F12O8Rh2SeSi_45a
_cod_database_code               4111079