Synthesis ofansa-Dimethylsilanediyl−dicyclopentadienyl− zirconacyclopent-3-yne, Me2Si(η5-C5H4)2Zr(η4-H2C4H2), and Its Reactions with Ni(0) and B(C6F5)3†
Beweries, Torsten; Bach, Marc A.; Burlakov, Vladimir V.; Arndt, Perdita; Baumann, Wolfgang; Spannenberg, Anke; Rosenthal, Uwe; Organometallics 26 (2007) 241–; doi:10.1021/om0608760

data_4072612
_publ_section_title
;
 Synthesis ofansa-Dimethylsilanediyl&#x2212;dicyclopentadienyl&#x2212;
 zirconacyclopent-3-yne, Me2Si(\h5-C5H4)2Zr(\h4-H2C4H2), and Its Reactions
 with Ni(0) and B(C6F5)3&#x2020;
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              241
_journal_paper_doi               10.1021/om0608760
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C16 H18 Si Zr'
_chemical_formula_weight         329.61
_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                 94.416(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.4537(10)
_cell_length_b                   6.9281(4)
_cell_length_c                   21.0200(11)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    293(2)
_cell_volume                     2969.8(3)
_computing_data_collection       STOE-X-AREA
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE-IPDS II'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36806
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  0.8099
_exptl_absorpt_correction_T_min  0.6995
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                3706
_reflns_number_total             5233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0608760si20060925_072736.cif
_cod_data_source_block           ks553
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4072612