Synthesis of titanium and zirconium complexes supported by a p-terphenoxide ligand and their reactions with N2, CO2 and CS2
Takashi Kurogi; Yutaka Ishida; Hiroyuki Kawaguchi; Chem.Commun. 49 (2013) 11755–; doi:10.1039/c3cc47284a

data_7110137
_publ_section_title
;
 Synthesis of titanium and zirconium complexes supported by a
 p-terphenoxide ligand and their reactions with N2, CO2 and CS2
;
_journal_name_full               Chem.Commun.
_journal_page_first              11755
_journal_paper_doi               10.1039/c3cc47284a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C66 H80 O6 S4 Zr2, 4(C7 H8)'
_chemical_formula_sum            'C94 H112 O6 S4 Zr2'
_chemical_formula_weight         1648.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.889(15)
_cell_angle_beta                 80.28(2)
_cell_angle_gamma                80.586(14)
_cell_formula_units_Z            1
_cell_length_a                   9.498(3)
_cell_length_b                   14.156(5)
_cell_length_c                   16.469(5)
_cell_measurement_reflns_used    5127
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4468
_cell_measurement_theta_min      3.0006
_cell_volume                     2115.0(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Saturn CCD (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_sigmaI/netI    0.1033
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26318
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.9247
_exptl_absorpt_correction_T_min  0.9247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         9639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+3.0523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1901
_reflns_number_gt                6469
_reflns_number_total             9639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47284a.txt
_cod_data_source_block           {[(C6H4)(ArO)2Zr]2(C2S4)(thf)2}4(toluene)
_cod_original_cell_volume        2114.9(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110137