Biphenolate Phosphine Complexes of Tantalum
Lan-Chang Liang; Liang-Chien Cheng; Tzung-Ling Tsai; Ching-Han Hu; Wen-Hsin Guo; Inorganic Chemistry 48 (2009) 5697–5703; doi:10.1021/ic802125z

data_4302407
_publ_section_title
;
Biphenolate Phosphine Complexes of Tantalum
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5697
_journal_page_last               5703
_journal_paper_doi               10.1021/ic802125z
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C80 H90 O5 P2 Ta1'
_chemical_formula_sum            'C68 H91 O5 P2 Ta'
_chemical_formula_weight         1231.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.896(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9740(15)
_cell_length_b                   31.433(4)
_cell_length_c                   22.293(3)
_cell_measurement_reflns_used    207031
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.037
_cell_volume                     9086(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_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 0.688
_diffrn_measured_fraction_theta_max 0.688
_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  0.1245
_diffrn_reflns_av_sigmaI/netI    0.1714
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29182
_diffrn_reflns_theta_full        25.1
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  1.0475
_exptl_absorpt_correction_T_min  0.6593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    0.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.778
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.213
_refine_ls_extinction_coef       0.0139(9)
_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   1.009
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         13434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1682
_refine_ls_R_factor_gt           0.1116
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1998P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3011
_refine_ls_wR_factor_ref         0.3290
_reflns_number_gt                7350
_reflns_number_total             13434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802125z_si_002_3.cif
_cod_data_source_block           7654
_cod_original_cell_volume        9086.4(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302407