Impact of Group 13 Metals on Cp2TiCl2 Reduction and Structural Characterization of Resulting Compounds
Petrus, Rafał; Utko, Józef; Lis, Tadeusz; Sobota, Piotr; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.6b02824

data_4345299
_publ_section_title
;
 Impact of Group 13 Metals on Cp2TiCl2 Reduction and Structural
 Characterization of Resulting Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b02824
_journal_year                    2017
_chemical_formula_moiety
'(C22 H38 Al Cl2 O8 Ti2), 0.5(C3 H8 O2), 2.5(C2 H6 O), Cl'
_chemical_formula_sum            'C28.5 H57 Al Cl3 O11.5 Ti2'
_chemical_formula_weight         812.87
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                75.87(4)
_cell_angle_beta                 80.44(4)
_cell_angle_gamma                73.89(3)
_cell_formula_units_Z            2
_cell_length_a                   11.737(4)
_cell_length_b                   12.398(4)
_cell_length_c                   15.341(6)
_cell_measurement_reflns_used    7342
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      36.6067
_cell_measurement_theta_min      2.8605
_cell_volume                     2068.2(13)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'DIAMOND  (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.481
_diffrn_measurement_device_type  'PX Xcalibur'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.481
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16971
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.481
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         36.692
_diffrn_reflns_theta_min         2.866
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         9890
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.901
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1824P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2341
_refine_ls_wR_factor_ref         0.2610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6086
_reflns_number_total             9890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02824_si_001.cif
_cod_data_source_block           2A
_cod_original_cell_volume        2068.2(14)
_cod_original_formula_sum        'C28.50 H57 Al Cl3 O11.50 Ti2'
_cod_database_code               4345299
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.754
_shelx_estimated_absorpt_t_max   0.870
_shelx_res_checksum              7333
_shelx_hkl_checksum              70434