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_4307826
_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         'C68 H92 Hf O5 P2'
_chemical_formula_sum            'C68 H92 Hf O5 P2'
_chemical_formula_weight         1229.85
_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                67.765(6)
_cell_angle_beta                 75.820(7)
_cell_angle_gamma                81.975(8)
_cell_formula_units_Z            2
_cell_length_a                   13.328(5)
_cell_length_b                   15.052(6)
_cell_length_c                   18.924(7)
_cell_measurement_reflns_used    871
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.6
_cell_measurement_theta_min      2.2
_cell_volume                     3402(2)
_computing_cell_refinement       'APEX2 v1.0-22'
_computing_data_collection       'APEX2 v1.0-22 (Bruker, 2004)'
_computing_data_reduction        'APEX2 v1.0-22'
_computing_molecular_graphics    'SHELXTL 5.1'
_computing_publication_material  'SHELXTL 5.1'
_computing_structure_refinement  'SHELXTL 5.1'
_computing_structure_solution    'SHELXTL 5.1 (Sheldrick, 1998)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1650
_diffrn_reflns_av_sigmaI/netI    0.4684
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18831
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.19
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_T_max  0.8545
_exptl_absorpt_correction_T_min  0.8545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.710
_refine_diff_density_min         -1.714
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.0073(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   0.836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         11839
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.2569
_refine_ls_R_factor_gt           0.0829
_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^)+(0.0878P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.2352
_reflns_number_gt                3438
_reflns_number_total             11839
_reflns_threshold_expression     I>2\s
_cod_data_source_file            ic062314esi20061204_093854.cif
_cod_data_source_block           ync248
_cod_database_code               4307826