Scandium, Titanium and Vanadium Complexes Supported by PCP-type Pincer Ligands: Synthesis, Structure, and Styrene Polymerization Activity
Zhang, Jiayu; Huang, Wenshuang; Han, Kailing; Song, Guoyong; Hu, Shaowei; Dalton Transactions  (2022) –; doi:10.1039/D2DT01389D

data_7710733
_publ_section_title
;
 Scandium, Titanium and Vanadium Complexes Supported by PCP-type Pincer
 Ligands: Synthesis, Structure, and Styrene Polymerization Activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01389D
_journal_year                    2022
_chemical_formula_sum            'C30 H61 O2 P2 Si2 Ti'
_chemical_formula_weight         619.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-03-24 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1891(2)
_cell_length_b                   13.1418(2)
_cell_length_c                   16.9923(3)
_cell_measurement_reflns_used    12072
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.2450
_cell_measurement_theta_min      4.3230
_cell_volume                     3615.18(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  Rigaku
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13919
_diffrn_reflns_point_group_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.776
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.510
_diffrn_reflns_theta_min         3.363
_exptl_absorpt_coefficient_mu    3.645
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 1995 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(4)
_refine_ls_extinction_coef       0.00059(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5894
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.7806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0703
_reflns_Friedel_coverage         0.566
_reflns_Friedel_fraction_full    0.656
_reflns_Friedel_fraction_max     0.582
_reflns_number_gt                5744
_reflns_number_total             5894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01389d2.cif
_cod_data_source_block           shelx
_cod_database_code               7710733
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              27114
_shelx_hkl_checksum              91367