Reactivity of a Dititanium Bis(pentalene) Complex toward Heteroallenes and Main-Group Element‒Element Bonds
Kilpatrick, Alexander F. R.; Green, Jennifer C.; Cloke, F. Geoffrey N.; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00791

data_4086897
_publ_section_title
;
 Reactivity of a Dititanium Bis(pentalene) Complex toward Heteroallenes
 and Main-Group Element--Element Bonds
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00791
_journal_year                    2016
_chemical_formula_moiety         'C64 H102  Si4 Te2 Ti2'
_chemical_formula_sum            'C64 H102 Si4 Te2 Ti2'
_chemical_formula_weight         1334.81
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.708(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1208(3)
_cell_length_b                   16.1056(3)
_cell_length_c                   25.6467(5)
_cell_measurement_reflns_used    19146
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.5960
_cell_measurement_theta_min      3.4910
_cell_volume                     7329.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material
;
Olex2 (Dolomanov et al., 2009), ShelXL-2013 (Sheldrick, 2013), Platon (Spek, 2003), and WinGX (Farrugia, 2013)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1033
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39773
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.263
_diffrn_reflns_theta_min         3.260
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.869
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;

Compound 7 contained disordered pentane molecules that could not 
be refined satisfactorily; for this reason, the program SQUEEZE 
was used to mathematically remove the effects of the solvent. 

;
_refine_diff_density_max         3.339
_refine_diff_density_min         -1.689
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         13961
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0578
_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^)+(0.1057P)^2^+5.6362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11632
_reflns_number_total             13961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00791_si_003.cif
_cod_data_source_block           Compound7
_cod_database_code               4086897
_shelx_estimated_absorpt_t_min   0.126
_shelx_estimated_absorpt_t_max   0.270
_shelxl_version_number           2013-3
_shelx_res_checksum              86548
_shelx_hkl_checksum              6270