Reaction of 1-Zirconacyclopent-3-yne with "Zirconocene": Synthesis and Structure of Bimetallic 1,2,3-Butatriene Complexes
Suzuki, Noriyuki; Watanabe, Takaaki; Iwasaki, Masakazu; Chihara, Teiji; Organometallics 24 (2005) 2065–2069; doi:10.1021/om049288h

data_1100828
_publ_section_title
;
 Reaction of 1-Zirconacyclopent-3-yne with "Zirconocene":
 Synthesis and Structure of Bimetallic 1,2,3-Butatriene Complexes
;
_journal_coden_ASTM              ORGND7
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2065
_journal_page_last               2069
_journal_paper_doi               10.1021/om049288h
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C14 H14 Zr'
_chemical_formula_sum            'C14 H14 Zr'
_chemical_formula_weight         273.48
_chemical_melting_point          ?
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_cell_angle_alpha                90
_cell_angle_beta                 91.525(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1150(4)
_cell_length_b                   9.2921(3)
_cell_length_c                   9.9839(2)
_cell_measurement_reflns_used    13461
_cell_measurement_temperature    113.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.0
_cell_volume                     1123.52(5)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9550
_diffrn_measured_fraction_theta_max 0.9550
_diffrn_measurement_device_type  'Rigaku RAXIS-CS Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3688
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_refine_diff_density_max         0.38
_refine_diff_density_min         -1.18
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-8'
_refine_ls_abs_structure_Flack   0.43(5)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    ?
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2965
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.0022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                2780
_reflns_number_total             1573
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_duplicate_entry             4060460
_cod_database_code               1100828