Metal-dependent regioselective homocoupling of stannyl- and alkyl-substituted alkynes on group 4 elements. Formation of unsymmetrical titanacyclopentadienes and symmetrical zircona-cyclopentadienes.
Bando, Masayoshi; Nakajima, Kiyohiko; Song, Zhiyi; Takahashi, Tamotsu; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13912–13915; doi:10.1039/c9dt02759a

data_7700973
_publ_section_title
;
 Metal-dependent regioselective homocoupling of stannyl- and
 alkyl-substituted alkynes on group 4 elements. Formation of unsymmetrical
 titanacyclopentadienes and symmetrical zircona-cyclopentadienes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13912
_journal_page_last               13915
_journal_paper_doi               10.1039/c9dt02759a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C22 H34 Si2 Ti'
_chemical_formula_sum            'C22 H34 Si2 Ti'
_chemical_formula_weight         402.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-08-14 deposited with the CCDC.    2019-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                96.05(2)
_cell_angle_beta                 95.99(2)
_cell_angle_gamma                104.28(2)
_cell_formula_units_Z            2
_cell_length_a                   9.709(5)
_cell_length_b                   10.178(6)
_cell_length_c                   12.212(6)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.10
_cell_volume                     1152.3(11)
_computing_cell_refinement       'RAPID AUTO (Rigaku)'
_computing_data_collection       'RAPID AUTO (Rigaku)'
_computing_data_reduction        'RAPID AUTO (Rigaku)'
_computing_molecular_graphics    'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11429
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         3.094
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.9104
_exptl_absorpt_correction_T_min  0.7960
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         5222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0658P)^2^+0.3013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                4451
_reflns_number_total             5222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02759a2.cif
_cod_data_source_block           tt301
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700973.cif.
;
_cod_original_cell_volume        1152.3(10)
_cod_database_code               7700973
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.796
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              31558