Synthesis and Characterization of Chiral Group 4 Metallocene Alkyne Complexes: (η5-menthyl-C5H4)2M(η2-Me3SiC2SiMe3), M = Ti, Zr⊥
Klahn, Marcus; Baumann, Wolfgang; Arndt, Perdita; Burlakov, Vladimir V.; Schareina, Thomas; Spannenberg, Anke; Rosenthal, Uwe; Organometallics 28 (2009) 915–; doi:10.1021/om8009624

data_4068576
_publ_section_title
;
 Synthesis and Characterization of Chiral Group 4 Metallocene Alkyne
 Complexes: (\h5-menthyl-C5H4)2M(\h2-Me3SiC2SiMe3), M = Ti, Zr&#x22A5;
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_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              915
_journal_paper_doi               10.1021/om8009624
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C38 H64 Si2 Ti'
_chemical_formula_weight         624.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 121.43(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.750(3)
_cell_length_b                   9.6744(19)
_cell_length_c                   15.032(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      4
_cell_volume                     1954.4(9)
_computing_cell_refinement       STOE-CELL
_computing_data_collection       STOE-EXPOSE
_computing_data_reduction        STOE-INTEGRATE
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE-IPDS I'
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6030
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3476
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                2972
_reflns_number_total             3476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8009624_si_002.cif
_cod_data_source_block           ks536m
_cod_original_cell_volume        1954.6(7)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4068576