2-Indenylidene Pincer Complexes of Zirconium and Palladium
Pascal Oulié; Noel Nebra; Nathalie Saffon; Laurent Maron; Blanca Martin-Vaca; Didier Bourissou; Journal of the American Chemical Society 131 (2009) 3493–3498; doi:10.1021/ja809892a

data_4104026
_publ_section_title
;
 2-Indenylidene Pincer Complexes of Zirconium and Palladium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3493
_journal_page_last               3498
_journal_paper_doi               10.1021/ja809892a
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C59 H69 Cl4 N5 P2 Zr'
_chemical_formula_weight         1143.15
_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                94.687(2)
_cell_angle_beta                 103.329(2)
_cell_angle_gamma                91.388(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0482(10)
_cell_length_b                   14.0223(14)
_cell_length_c                   21.011(2)
_cell_measurement_reflns_used    4092
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.08
_cell_measurement_theta_min      2.49
_cell_volume                     2868.2(5)
_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      173(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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19734
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.625121
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         9549
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                6751
_reflns_number_total             9549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809892a_si_002.cif
_cod_data_source_block           pascal5m
_cod_database_code               4104026