Synthesis and Structure of 1-Zirconacyclopent-3-yne Complexes without Substituents Adjacent to the Triple Bond
Noriyuki Suzuki; Naoto Aihara; Hidemichi Takahara; Takaaki Watanabe; Masakazu Iwasaki; Masahiko Saburi; Daisuke Hashizume; Teiji Chihara; Journal of the American Chemical Society 126 (2004) 60–61; doi:10.1021/ja0385742

data_4060214
_publ_contact_author_address
;
    Chemical Analysisi Division, RIKEN, Wako, Saitama, 351-0198, Japan
;
_publ_contact_author_email       ' nsuzuki@postman.riken.go.jp'
_publ_contact_author_fax         ' +81-48-462-4631 '
_publ_contact_author_name        ' Noriyuki Suzuki'
_publ_section_title
;
Synthesis and Structure of 1-Zirconacyclopent-3-yne Complexes without
Substituents Adjacent to the Triple Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              60
_journal_page_last               61
_journal_paper_doi               10.1021/ja0385742
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C27 H33 P Zr2'
_chemical_formula_sum            'C27 H33 P Zr2'
_chemical_formula_weight         570.97
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 105.6613(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5259(2)
_cell_length_b                   33.0858(4)
_cell_length_c                   8.2256(1)
_cell_measurement_reflns_used    72723
_cell_measurement_temperature    200.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      0.6
_cell_volume                     2758.28(7)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9995
_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  0.039
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            44567
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_exptl_crystal_size_rad          ?
_refine_diff_density_max         0.92
_refine_diff_density_min         -1.06
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.707
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     271
_refine_ls_number_reflns         8071
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.0027
_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         0.1316
_reflns_number_gt                7146
_reflns_number_total             8071
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4060214