Synthesis and characterisation of an enantiomerically pure scandium pentadienyl complex and its application in the polymerisation of rac-lactide
Münster, Katharina; Raeder, Jan; Walter, Marc D.; Dalton Transactions  (2022) –; doi:10.1039/D1DT03920B

data_7709135
_publ_section_title
;
 Synthesis and characterisation of an enantiomerically pure scandium
 pentadienyl complex and its application in the polymerisation of
 rac-lactide
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03920B
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H52 N O Sc Si2'
_chemical_formula_sum            'C27 H52 N O Sc Si2'
_chemical_formula_weight         507.83
_chemical_melting_point          361
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-11-18 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2101(2)
_cell_length_b                   13.2214(2)
_cell_length_c                   22.7451(4)
_cell_measurement_reflns_used    12648
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.9510
_cell_measurement_theta_min      3.9260
_cell_volume                     3070.40(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.982
_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     27.00 119.00   0.50    1.50    --   48.41  80.00  70.00  184
  2  \w     98.00 178.00   0.50    6.00    --  105.75  30.00   0.00  160
  3  \w     84.00 178.00   0.50    6.00    --  105.75  80.00  70.00  188
  4  \w     92.00 178.00   0.50    6.00    --  105.75  61.00  30.00  172
  5  \w     74.00 119.00   0.50    1.50    --   48.41 125.00 -90.00   90
  6  \w     41.00 120.00   0.50    1.50    --   48.41  38.00-150.00  158
  7  \w     34.00 128.00   0.50    6.00    --  105.75 -80.00 -53.00  188
  8  \w     28.00 119.00   0.50    1.50    --   48.41  77.00-150.00  182
  9  \w     28.00 119.00   0.50    1.50    --   48.41  77.00 -60.00  182
 10  \w    -70.00  24.00   0.50    1.50    --  -48.41  80.00  70.00  188
 11  \w    -73.00 -34.00   0.50    6.00    -- -105.75  61.00-150.00   78
 12  \w   -107.00 -34.00   0.50    6.00    -- -105.75  77.00 -90.00  146
 13  \w   -128.00 -34.00   0.50    6.00    -- -105.75  80.00  70.00  188
 14  \w    -73.00 -34.00   0.50    6.00    -- -105.75  61.00 150.00   78
 15  \w   -177.00 -84.00   0.50    6.00    -- -105.75 -80.00 -53.00  186
 16  \w   -177.00 -97.00   0.50    6.00    -- -105.75 -30.00 120.00  160
 17  \w   -177.00 -85.00   0.50    6.00    -- -105.75 -77.00  30.00  184
 18  \w   -177.00 -91.00   0.50    6.00    -- -105.75 -61.00 -30.00  172
 19  \w   -177.00 -96.00   0.50    6.00    -- -105.75 -45.00-180.00  162
 20  \w   -177.00 -97.00   0.50    6.00    -- -105.75 -30.00-150.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0767281000
_diffrn_orient_matrix_UB_12      0.0187868000
_diffrn_orient_matrix_UB_13      0.0572832000
_diffrn_orient_matrix_UB_21      0.0129369000
_diffrn_orient_matrix_UB_22      -0.1149751000
_diffrn_orient_matrix_UB_23      0.0090833000
_diffrn_orient_matrix_UB_31      0.1292512000
_diffrn_orient_matrix_UB_32      0.0004267000
_diffrn_orient_matrix_UB_33      -0.0350191000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35213
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.593
_diffrn_reflns_theta_min         3.867
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1112
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 2393 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         6316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0532P)^2^+0.8099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                5893
_reflns_number_total             6316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03920b2.cif
_cod_data_source_block           km36ra
_cod_database_code               7709135
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H52 N1 O1 Si2 Sc1'
_chemical_oxdiff_usercomment     'n-Hexane, -30 degC'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C9(H9), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C23(H23A,H23B), C6(H6A,H6B), C8(H8A,H8B), C13(H13A,H13B),
 C21(H21A,H21B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C12(H12A,H12B,H12C), C17(H17A,H17B,H17C), C25(H25A,H25B,
 H25C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C14(H14A,
 H14B,H14C), C26(H26A,H26B,H26C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              95129
_shelx_hkl_checksum              71378
_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 1.505
_oxdiff_exptl_absorpt_empirical_full_min 0.722