Selective Tin-Carbon Bond Cleavage Reactions of Trimethylstannylzirconocene Dichloride with Electrophiles
Xu Cheng; Carla Slebodnick; Paul A. Deck; Damon R. Billodeaux; Frank R. Fronczek; Inorganic Chemistry 39 (2000) 4921–4926; doi:10.1021/ic991461s

data_4321490
_publ_contact_author_address
; Department of Chemistry
  Virginia Tech
  Blacksburg, Virginia 24061-0212
;
_publ_contact_author_email       pdeck@vt.edu
_publ_contact_author_fax         540-231-3255
_publ_contact_author_name        'Paul A. Deck'
_publ_contact_author_phone       540-231-3493
_publ_section_title
;
 Selective Tin-Carbon Bond Cleavage Reactions of
 Trimethylstannylzirconocene Dichloride with Electrophiles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4921
_journal_page_last               4926
_journal_paper_doi               10.1021/ic991461s
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C11 H12 Br4 Sn Zr, C4 H8 O'
_chemical_formula_sum            'C15 H20 Br4 O Sn Zr'
_chemical_formula_weight         745.86
_chemical_name_common            '(Br2MeSnCp)CpZrBr2 Sn-THF adduct'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.5120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.6230(2)
_cell_length_b                   8.3330(2)
_cell_length_c                   11.9970(4)
_cell_measurement_reflns_used    42481
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      0.998
_cell_volume                     2012.74(9)
_computing_cell_refinement
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.079
_diffrn_reflns_av_sigmaI/netI    0.058
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29435
_diffrn_reflns_theta_full        35.03
_diffrn_reflns_theta_max         35.03
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    9.698
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995) '
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.204
_refine_diff_density_min         -1.528
_refine_diff_density_rms         0.306
_refine_ls_extinction_coef       0.0034(2)
_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   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         8855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+12.5418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                7507
_reflns_number_total             8855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991461s_1.cif
_cod_data_source_block           Complex4
_cod_original_cell_volume        2012.74(8)
_cod_database_code               4321490