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_7102552
_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            'C90 H100 O8 S8 Ti2'
_chemical_formula_weight         1662.07
_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                109.90(3)
_cell_angle_beta                 95.721(19)
_cell_angle_gamma                93.84(3)
_cell_formula_units_Z            2
_cell_length_a                   13.483(3)
_cell_length_b                   16.930(8)
_cell_length_c                   20.649(6)
_cell_measurement_temperature    296(2)
_cell_volume                     4384(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1122
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16123
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        -3.95
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.9197
_exptl_absorpt_correction_T_min  0.7271
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.985
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         15406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1496
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1227P)^2^+3.2119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.2249
_reflns_number_gt                8595
_reflns_number_total             15406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b316972c.txt
_cod_data_source_block           '[TC4A-(OH)(O)3TiCp](3)'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7102552