Sulfur-containing stable five-membered “cycloallene” complexes: 1-thia-2-zircona- and 1-thia-2-titanacyclopenta-3,4-dienes
Suzuki, Noriyuki; Asada, Takumi; Kawamura, Akiko; Masuyama, Yoshiro; Organic Chemistry Frontiers 2 (2015) 681–; doi:10.1039/C5QO00072F

data_1553126
_publ_section_title
;
 Sulfur-containing stable five-membered &#x201C;cycloallene&#x201D;
 complexes: 1-thia-2-zircona- and 1-thia-2-titanacyclopenta-3,4-dienes
;
_journal_issue                   6
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              681
_journal_paper_doi               10.1039/C5QO00072F
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C8 H17 N S Si'
_chemical_formula_sum            'C8 H17 N S Si'
_chemical_formula_weight         187.37
_chemical_name_systematic
(Z)-N,N-diethyl-3-(tert-butylditrimethylsilyl)prop-2-enethioamide
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-01
_audit_creation_method           'by CrystalStructure 4.1'
_audit_update_record
;
2015-03-02 deposited with the CCDC.
2015-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                92.0278
_cell_angle_beta                 99.0665
_cell_angle_gamma                112.2068
_cell_formula_units_Z            2
_cell_length_a                   6.2605
_cell_length_b                   6.9304
_cell_length_c                   14.4299
_cell_measurement_reflns_used    1574
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.87
_cell_volume                     569.305
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5433
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.192
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             204.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.51
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1994
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1686P)^2^+0.2089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2217
_refine_ls_wR_factor_ref         0.2447
_reflns_d_resolution_high        0.8410
_reflns_number_gt                1549
_reflns_number_total             1994
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5qo00072f2.cif
_cod_data_source_block           ns299KA
_cod_original_cell_volume        569.3065
_cod_database_code               1553126
_shelx_title                     ' KA141129a'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            88.32
_shelx_f_squared_multiplier      1.000