Pentavalent vs Trivalent Phosphorus-Bridged Ligands. Synthesis and Structural Characterization of Unexpected Group 4 Metal Complexes Incorporating an Indenylide Unit, [σ:σ-iPr2NP(O)(C9H6)(C2B10H10)]M(NR2)2
Wang, Hong; Chan, Hoi-Shan; Xie, Zuowei; Organometallics 25 (2006) 2569–; doi:10.1021/om060082l

data_4075168
_publ_section_title
;
 Pentavalent vs Trivalent Phosphorus-Bridged Ligands. Synthesis and
 Structural Characterization of Unexpected Group 4 Metal Complexes
 Incorporating an Indenylide Unit,
 [\s:\s-iPr2NP(O)(C9H6)(C2B10H10)]M(NR2)2
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2569
_journal_paper_doi               10.1021/om060082l
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C23 H49 B10 N4 O P Ti'
_chemical_formula_weight         584.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.5538(6)
_cell_length_b                   15.3753(6)
_cell_length_c                   28.0020(11)
_cell_measurement_temperature    293(2)
_cell_volume                     6696.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34535
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8533
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+1.9643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                3762
_reflns_number_total             5896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060082lsi20060126_023303.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4075168