1-Titanacyclobuta-2,3-diene – an Elusive Four-membered Cyclic Allene
Reiß, Fabian; Reiß, Melanie; Bresien, Jonas; Spannenberg, Anke; Jiao, Haijun; Baumann, Wolfgang; Arndt, Perdita; Beweries, Torsten; Chemical Science  (2019) –; doi:10.1039/C9SC01002E

data_1550930
_publ_section_title
;
 1-Titanacyclobuta-2,3-diene -- an Elusive Four-membered Cyclic Allene
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01002E
_journal_year                    2019
_chemical_formula_sum            'C22 H28 Si2'
_chemical_formula_weight         348.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.59(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.485(2)
_cell_length_b                   9.6273(19)
_cell_length_c                   19.737(4)
_cell_measurement_reflns_used    664
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      2.07
_cell_volume                     2137.8(7)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2012)'
_computing_data_reduction        X-AREA
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36201
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         1.903
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'LANA (Stoe & Cie, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         5154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3064
_reflns_number_total             5154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01002e2.cif
_cod_data_source_block           ks1463
_cod_original_cell_volume        2137.7(8)
_cod_database_code               1550930
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              64789