Diels−Alder Reactions of Benzyne with Indenyl and Fluorenyl Ruthenium Complexes
Luo, Shuang; Zhao, Xi; Mu, Bin; Song, Haibin; Xu, Shansheng; Wang, Baiquan; Organometallics 28 (2009) 4602–; doi:10.1021/om9003303

data_4069638
_publ_section_title
;
 Diels&#x2212;Alder Reactions of Benzyne with Indenyl and Fluorenyl
 Ruthenium Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4602
_journal_paper_doi               10.1021/om9003303
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C25 H18'
_chemical_formula_sum            'C25 H18'
_chemical_formula_weight         318.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.33(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.696(17)
_cell_length_b                   17.44(2)
_cell_length_c                   18.75(3)
_cell_measurement_reflns_used    2397
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      1.6
_cell_volume                     3356(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40873
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.9845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0127(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0659P)^2^+0.5839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                6402
_reflns_number_total             7741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9003303_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3356(8)
_cod_database_code               4069638