Synthesis and structural analysis of aryloxo-modified trinuclear half-titanocenes, and their use as catalyst precursors for ethylene polymerisation
Yan, Qing; Tsutsumi, Ken; Nomura, Kotohiro; RSC Adv. 7 (2017) 41345–; doi:10.1039/C7RA07581B

data_7228989
_publ_section_title
;
 Synthesis and structural analysis of aryloxo-modified trinuclear
 half-titanocenes, and their use as catalyst precursors for ethylene
 polymerisation
;
_journal_issue                   66
_journal_name_full               'RSC Adv.'
_journal_page_first              41345
_journal_paper_doi               10.1039/C7RA07581B
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C75 H111 Cl6 N O3 Ti3'
_chemical_formula_sum            'C75 H111 Cl6 N O3 Ti3'
_chemical_formula_weight         1431.12
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-05-12 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.814(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.5836(9)
_cell_length_b                   22.4075(10)
_cell_length_c                   21.6663(10)
_cell_measurement_reflns_used    8223
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.92
_cell_measurement_theta_min      1.84
_cell_volume                     8506.5(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            89388
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.599
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3040.00
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     793
_refine_ls_number_reflns         19531
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1099P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.2209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10706
_reflns_number_total             19531
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7ra07581b2.cif
_cod_data_source_block           Ti5
_cod_database_code               7228989
_shelx_res_checksum              37026