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_1550929
_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            'C29 H42 Si2 Ti'
_chemical_formula_weight         494.70
_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                 98.8260(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2569(6)
_cell_length_b                   10.8620(4)
_cell_length_c                   18.2070(7)
_cell_measurement_reflns_used    8923
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.26
_cell_volume                     2786.12(19)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25163
_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         27.999
_diffrn_reflns_theta_min         1.694
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6735
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+1.0432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5551
_reflns_number_total             6735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01002e2.cif
_cod_data_source_block           AX1557
_cod_database_code               1550929
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              40264