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_4104027
_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            'C55 H58 N4 P2 Zr'
_chemical_formula_weight         928.21
_chemical_name_systematic
;
 ?
;
_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                 110.034(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8825(14)
_cell_length_b                   23.109(2)
_cell_length_c                   17.1419(18)
_cell_measurement_reflns_used    1432
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17.31
_cell_measurement_theta_min      2.43
_cell_volume                     4794.4(8)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.1628
_diffrn_reflns_av_sigmaI/netI    0.1743
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26697
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.753
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         6171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.753
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                3334
_reflns_number_total             6171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809892a_si_003.cif
_cod_data_source_block           pascal8m
_cod_original_cell_volume        4794.3(9)
_cod_database_code               4104027