Mesityl Alkyne Substituents for Control of Regiochemistry and Reversibility in Zirconocene Couplings: New Synthetic Strategies for Unsymmetrical Zirconacyclopentadienes and Conjugated Polymers
Adam D. Miller; John F. Tannaci; Samuel A. Johnson; Hyuk Lee; Jennifer L. McBee; T. Don Tilley; Journal of the American Chemical Society 131 (2009) 4917–4927; doi:10.1021/ja809896t

data_4104132
_publ_section_title
;
 Mesityl Alkyne Substituents for Control of Regiochemistry and
 Reversibility in Zirconocene Couplings: New Synthetic Strategies for
 Unsymmetrical Zirconacyclopentadienes and Conjugated Polymers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4917
_journal_page_last               4927
_journal_paper_doi               10.1021/ja809896t
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C38 H46 Zr'
_chemical_formula_sum            'C38 H46 Zr'
_chemical_formula_weight         593.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.786(7)
_cell_length_b                   17.808(6)
_cell_length_c                   8.229(3)
_cell_measurement_reflns_used    924
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      18.64
_cell_measurement_theta_min      3.35
_cell_volume                     3046.0(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1018
_diffrn_reflns_av_sigmaI/netI    0.1564
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10021
_diffrn_reflns_theta_full        22.09
_diffrn_reflns_theta_max         22.09
_diffrn_reflns_theta_min         3.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, 2004'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.708
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         1879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.708
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                900
_reflns_number_total             1879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809896t_si_003.cif
_cod_data_source_block           adam13m
_cod_original_cell_volume        3045.9(17)
_cod_database_code               4104132