Synthesis and Complexation of a New Tripodal Tetradentate Ligand, a Silyl Ligand Tethered with Three Thioether Moieties
Takeda, Nobuhiro; Watanabe, Daisuke; Nakamura, Tetsu; Unno, Masafumi; Organometallics 29 (2010) 2839–; doi:10.1021/om100255p

data_4066030
_publ_section_title
;
 Synthesis and Complexation of a New Tripodal Tetradentate Ligand, a Silyl
 Ligand Tethered with Three Thioether Moieties
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2839
_journal_paper_doi               10.1021/om100255p
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C33 H46 S3 Si'
_chemical_formula_weight         566.97
_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                77.746(3)
_cell_angle_beta                 74.587(3)
_cell_angle_gamma                83.570(4)
_cell_formula_units_Z            4
_cell_length_a                   11.6359(2)
_cell_length_b                   15.8805(5)
_cell_length_c                   19.5216(5)
_cell_measurement_reflns_used    17829
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.2812
_cell_measurement_theta_min      2.6280
_cell_volume                     3392.39(16)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device
;
RAXIS conversion
;
_diffrn_measurement_method       dtprofit.ref
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23394
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.9732
_exptl_absorpt_correction_T_min  0.8756
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         11820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0833
_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^)+(0.0000P)^2^+11.6169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                11584
_reflns_number_total             11820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100255p_si_001.cif
_cod_data_source_block           sihstbu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3392.39(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066030