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_7710736
_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_moiety         'C32 H57 P2 Si2 Ti'
_chemical_formula_sum            'C32 H57 P2 Si2 Ti'
_chemical_formula_weight         607.79
_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_date             2022-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-25 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                   16.1352(2)
_cell_length_b                   13.17667(18)
_cell_length_c                   17.2700(3)
_cell_measurement_reflns_used    10628
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2460
_cell_measurement_theta_min      4.3020
_cell_volume                     3671.74(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  25.00   0.50    0.10    --   46.95 -23.00-154.00  104
  2  \w    -21.00  12.00   0.50    0.10    --   46.95 -19.00 -30.00   66
  3  \w    -15.00  28.00   0.50    0.10    --   46.95 -19.00  60.00   86
  4  \w     95.00 162.00   0.50    0.50    --  104.75  23.00  10.00  134
  5  \w    -57.00 -32.00   0.50    0.50    -- -102.00  61.00 -60.00   50
  6  \w   -109.00 -32.00   0.50    0.50    -- -102.00 101.00 172.00  154
  7  \w   -116.00 -59.00   0.50    0.50    -- -102.00-144.00-177.00  114
  8  \w   -116.00 -78.00   0.50    0.10    --  -46.95-125.00 -60.00   76
  9  \w     60.00  90.00   0.50    0.10    --   46.95-125.00 -60.00   60
 10  \w     43.00  93.00   0.50    0.50    --  104.75 -77.00  90.00  100
 11  \w     36.00  72.00   0.50    0.50    --  104.75 -61.00 120.00   72
 12  \w     38.00  69.00   0.50    0.50    --  104.75 -61.00 -30.00   62
 13  \w     47.00  72.00   0.50    0.50    --  104.75 -61.00 -60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0830583000
_diffrn_orient_matrix_UB_12      -0.0107509000
_diffrn_orient_matrix_UB_13      0.0431897000
_diffrn_orient_matrix_UB_21      0.0465805000
_diffrn_orient_matrix_UB_22      0.0337748000
_diffrn_orient_matrix_UB_23      -0.0734250000
_diffrn_orient_matrix_UB_31      -0.0061051000
_diffrn_orient_matrix_UB_32      0.1115076000
_diffrn_orient_matrix_UB_33      0.0264149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13581
_diffrn_reflns_point_group_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.437
_diffrn_reflns_theta_min         3.354
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 2021 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6009
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+1.2290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1257
_reflns_Friedel_coverage         0.571
_reflns_Friedel_fraction_full    0.662
_reflns_Friedel_fraction_max     0.588
_reflns_number_gt                5838
_reflns_number_total             6009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01389d2.cif
_cod_data_source_block           exp_3918
_cod_original_cell_volume        3671.75(9)
_cod_database_code               7710736
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H  P Ti Si'
_diffrn_oxdiff_digest_frames
;
01ca102ad8e7877c90162d2f76ee1b6e9b00104edfb
;
_diffrn_oxdiff_digest_hkl
;
01a03a7c38b437d160dd0a3be3fbfd4073df9f
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              5458
_shelx_hkl_checksum              47084
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.836
_oxdiff_exptl_absorpt_empirical_full_min 0.598