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_1553125
_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         'C18 H25 N S Si Zr'
_chemical_formula_sum            'C18 H25 N S Si Zr'
_chemical_formula_weight         406.76
_chemical_name_systematic
'2,2-bis(\h5-cyclopentadienyl)-3-trimethylsilyl-5-dimethylamino- 1-thia-2-zirconacyclopenta-3,4-diene'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-04-03 deposited with the CCDC.
2015-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.282(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.471(8)
_cell_length_b                   9.164(4)
_cell_length_c                   14.060(7)
_cell_measurement_reflns_used    5166
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.5126
_cell_measurement_theta_min      2.6196
_cell_volume                     1892.8(16)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6977
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         2.620
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 REQAB (Rigaku, 1998)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+4.1127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3344
_reflns_number_total             4168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qo00072f2.cif
_cod_data_source_block           ns253_5a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1553125
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              30518
_shelx_hkl_checksum              86394