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_4345300
_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, C13 H18 O2 Ti, Cl4 Fe'
_chemical_formula_sum            'C35 H56 Al Cl6 Fe O10 Ti3'
_chemical_formula_weight         1075.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.212(3)
_cell_length_b                   24.938(7)
_cell_length_c                   27.221(7)
_cell_measurement_reflns_used    7058
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      30.7790
_cell_measurement_theta_min      2.7177
_cell_volume                     8969(4)
_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      95(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37420
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.848
_diffrn_reflns_theta_min         2.843
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.679
_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            blue
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         12430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0300P)^2^+7.6275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9164
_reflns_number_total             12430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02824_si_001.cif
_cod_data_source_block           3
_cod_database_code               4345300
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.646
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              97163
_shelx_hkl_checksum              32849