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_4068578
_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            'C34 H54 Zr'
_chemical_formula_weight         553.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 100.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.723(2)
_cell_length_b                   13.155(3)
_cell_length_c                   11.469(2)
_cell_measurement_reflns_used    13047
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      1.78
_cell_volume                     1589.5(6)
_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      200(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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22682
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6246
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0182
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                5898
_reflns_number_total             6246
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8009624_si_002.cif
_cod_data_source_block           ks613m
_cod_original_cell_volume        1589.4(5)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4068578