Biphenolate Phosphine Complexes of Group 4 Metals
Lan-Chang Liang; Yu-Ning Chang; Hon Man Lee; Inorganic Chemistry 46 (2007) 2666–2673; doi:10.1021/ic062314e

data_4307827
_publ_section_title
;
Biphenolate Phosphine Complexes of Group 4 Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2666
_journal_page_last               2673
_journal_paper_doi               10.1021/ic062314e
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C94 H124 Cl4 O6 P2 Ti2'
_chemical_formula_sum            'C94 H124 Cl4 O6 P2 Ti2'
_chemical_formula_weight         1649.47
_chemical_name_systematic
;
 ?
;
_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                78.436(6)
_cell_angle_beta                 76.747(5)
_cell_angle_gamma                75.310(3)
_cell_formula_units_Z            1
_cell_length_a                   11.2340(8)
_cell_length_b                   13.2667(11)
_cell_length_c                   16.5354(12)
_cell_measurement_reflns_used    29547
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     2293.7(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.2362
_diffrn_reflns_av_sigmaI/netI    0.2497
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26859
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.030(5)
_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   1.068
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.2760
_refine_ls_R_factor_gt           0.1313
_refine_ls_shift/su_max          0.192
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1705P)^2^+1.5140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2970
_refine_ls_wR_factor_ref         0.3855
_reflns_number_gt                3057
_reflns_number_total             7524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062314esi20061204_093933.cif
_cod_data_source_block           5581
_cod_database_code               4307827