Ti-Mo heterobimetallic thiacalix[4]arene complex containing an unusual alpha-agostic micro2-eta5:eta2-cyclopentadienyl ligand.
Takemoto, Shin; Tanaka, Shinpei; Mizobe, Yasushi; Hidai, Masanobu; Chemical communications (Cambridge, England)  (2004) 838–839; doi:10.1039/b316972c

data_7102553
_publ_section_title
;
 Ti-Mo heterobimetallic thiacalix[4]arene complex containing an unusual
 alpha-agostic micro2-eta5:eta2-cyclopentadienyl ligand.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              838
_journal_page_last               839
_journal_paper_doi               10.1039/b316972c
_journal_year                    2004
_chemical_formula_sum            'C64 H75 Mo O4 P2 S4 Ti'
_chemical_formula_weight         1242.33
_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                   23.430(10)
_cell_length_b                   23.594(11)
_cell_length_c                   22.051(9)
_cell_measurement_temperature    293(2)
_cell_volume                     12190(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.2589
_diffrn_reflns_av_sigmaI/netI    0.1572
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70858
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.01
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.9721
_exptl_absorpt_correction_T_min  0.8945
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5192
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         10290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.2346
_refine_ls_R_factor_gt           0.1726
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+195.0306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2641
_refine_ls_wR_factor_ref         0.2878
_reflns_number_gt                6753
_reflns_number_total             10290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b316972c.txt
_cod_data_source_block
'[TC4A-(O)4Ti(mu2-eta5:eta1-C5H5)MoH(PMe2Ph)2](4)'
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               7102553