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_4104134
_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         593.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.700(5)
_cell_angle_beta                 80.995(5)
_cell_angle_gamma                79.982(6)
_cell_formula_units_Z            2
_cell_length_a                   8.350(3)
_cell_length_b                   11.514(4)
_cell_length_c                   17.134(7)
_cell_measurement_reflns_used    1346
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      19.1
_cell_measurement_theta_min      3.29
_cell_volume                     1554.0(10)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.1064
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10070
_diffrn_reflns_theta_full        23.39
_diffrn_reflns_theta_max         23.39
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, 2004'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0707P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                2984
_reflns_number_total             4431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809896t_si_005.cif
_cod_data_source_block           adam14s
_cod_database_code               4104134