Synthesis and Reactivity of Dialkyl Lutetium Complexes Supported by a Novel Bis(phosphinimine)carbazole Pincer Ligand
Johnson, Kevin R. D.; Hayes, Paul G.; Organometallics 28 (2009) 6352–; doi:10.1021/om900731x

data_4070338
_publ_section_title
;
 Synthesis and Reactivity of Dialkyl Lutetium Complexes Supported by a
 Novel Bis(phosphinimine)carbazole Pincer Ligand
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6352
_journal_paper_doi               10.1021/om900731x
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C56 H53 N3 P2, 2(C6 H6)'
_chemical_formula_sum            'C68 H65 N3 P2'
_chemical_formula_weight         986.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                77.5770(10)
_cell_angle_beta                 80.3780(10)
_cell_angle_gamma                78.8940(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9413(6)
_cell_length_b                   16.6229(12)
_cell_length_c                   19.4273(14)
_cell_measurement_reflns_used    5883
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2743.2(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33540
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.82
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS: (Sheldrick 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         9677
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+1.4561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                7085
_reflns_number_total             9677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900731x_si_002.cif
_cod_data_source_block           ph09022
_cod_database_code               4070338