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_7110136
_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         'C73 H85 O10 Zr2, 2.5(C4 H8 O)'
_chemical_formula_sum            'C83 H105 O12.5 Zr2'
_chemical_formula_weight         1485.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.8792(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.785(2)
_cell_length_b                   14.4383(19)
_cell_length_c                   29.830(4)
_cell_measurement_reflns_used    11744
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      3.0477
_cell_volume                     7619.6(17)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0992
_diffrn_reflns_av_unetI/netI     0.0946
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            92813
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_min         3.048
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.9900
_exptl_absorpt_correction_T_min  0.9705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             3132
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
;
_refine_diff_density_max         1.579
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         17461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0934
_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^)+(0.1460P)^2^+16.7935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11882
_reflns_number_total             17461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc47284a.txt
_cod_data_source_block           (C6H4)2(CO2)(ArO)4Zr2(thf)4]2.5(thf)
_cod_original_cell_volume        7619.7(17)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C83 H105 O12.50 Zr2'
_cod_database_code               7110136
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.990