Synthesis and catalytic activity of single-site group V alkoxide complexes for the ring-opening polymerization of ε-caprolactone.
Peprah, Frank; Tarantola, Grace E.; Plaman, Alyson S.; Vu, Emily L.; Huynh, Alyssa B.; Durr, Christopher B.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7073–7080; doi:10.1039/d4dt00422a

data_7715606
_publ_section_title
;
 Synthesis and catalytic activity of single-site group V alkoxide
 complexes for the ring-opening polymerization of &#x3b5;-caprolactone.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7073
_journal_page_last               7080
_journal_paper_doi               10.1039/d4dt00422a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C20 H22 N O5 Ta'
_chemical_formula_sum            'C20 H22 N O5 Ta'
_chemical_formula_weight         537.33
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-08
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1648(2)
_cell_length_b                   7.73010(10)
_cell_length_c                   16.3269(2)
_cell_measurement_reflns_used    14791
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.8430
_cell_measurement_theta_min      2.7070
_cell_volume                     1904.19(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (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            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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     23.00 108.00   0.50    0.20    --   41.95  54.00  30.00  170
  2  \w     23.00 108.00   0.50    0.20    --   41.95  54.00 120.00  170
  3  \w     23.00 108.00   0.50    0.20    --   41.95  54.00  60.00  170
  4  \w     23.00 108.00   0.50    0.20    --   41.95  54.00 -60.00  170
  5  \w     23.00 108.00   0.50    0.20    --   41.95  54.00-180.00  170
  6  \w     23.00 108.00   0.50    0.20    --   41.95  54.00-150.00  170
  7  \w     23.00 108.00   0.50    0.20    --   41.95  54.00-120.00  170
  8  \w     23.00 108.00   0.50    0.20    --   41.95  54.00 -30.00  170
  9  \w     23.00 108.00   0.50    0.20    --   41.95  54.00 150.00  170
 10  \w    -33.00  24.00   0.50    0.20    --   41.95 -11.00   0.00  114
 11  \w    -33.00  24.00   0.50    0.20    --   41.95 -11.00 120.00  114
 12  \w    -23.00  48.00   0.50    0.20    --   41.95 -43.00-180.00  142
 13  \w     77.00 152.00   0.50    0.40    --   93.72  17.00  30.00  150
 14  \w     84.00 165.00   0.50    0.40    --   93.72  97.00-133.00  162
 15  \w     97.00 162.00   0.50    0.40    --   93.72  68.00 -90.00  130
 16  \w     19.00  99.00   0.50    0.20    --   41.95-138.00-150.00  160
 17  \w     19.00  99.00   0.50    0.20    --   41.95-138.00  60.00  160
 18  \w    -28.00  75.00   0.50    0.20    --   41.95 -97.00 119.00  206
 19  \w     21.00 107.00   0.50    0.40    --   93.72 -97.00 119.00  172
 20  \w     26.00  83.00   0.50    0.40    --   93.72 -68.00 120.00  114
 21  \w     28.00  57.00   0.50    0.40    --   93.72 -50.00 150.00   58
 22  \w     28.00  57.00   0.50    0.40    --   93.72 -50.00 120.00   58
 23  \w     28.00  57.00   0.50    0.40    --   93.72 -50.00 -90.00   58
 24  \w     28.00  57.00   0.50    0.40    --   93.72 -50.00-120.00   58
 25  \w    -24.00  32.00   0.50    0.20    --  -42.26  11.00-150.00  112
 26  \w    -83.00 -26.00   0.50    0.40    --  -94.03  68.00-120.00  114
 27  \w    -83.00 -26.00   0.50    0.40    --  -94.03  68.00-150.00  114
 28  \w    -83.00 -26.00   0.50    0.40    --  -94.03  68.00-180.00  114
 29  \w    -48.00  24.00   0.50    0.20    --  -42.26  43.00-120.00  144
 30  \w    -57.00 -28.00   0.50    0.40    --  -94.03  50.00-180.00   58
 31  \w    -57.00 -28.00   0.50    0.40    --  -94.03  50.00-120.00   58
 32  \w    -68.00 -27.00   0.50    0.40    --  -94.03  59.00 -30.00   82
 33  \w    -57.00 -28.00   0.50    0.40    --  -94.03  50.00  30.00   58
 34  \w    -24.00  32.00   0.50    0.20    --  -42.26  11.00 150.00  112
 35  \w    -68.00 -27.00   0.50    0.40    --  -94.03  59.00  90.00   82
 36  \w   -160.00 -77.00   0.50    0.40    --  -94.03 -50.00 -60.00  166
 37  \w   -161.00 -97.00   0.50    0.40    --  -94.03 -68.00-150.00  128
 38  \w   -160.00 -87.00   0.50    0.40    --  -94.03 -59.00-180.00  146
 39  \w    -75.00  29.00   0.50    0.20    --  -42.26  97.00-133.00  208
 40  \w   -106.00 -22.00   0.50    0.40    --  -94.03  97.00-133.00  168
 41  \w   -161.00 -97.00   0.50    0.40    --  -94.03 -68.00 150.00  128
 42  \w   -167.00 -84.00   0.50    0.40    --  -94.03 -97.00 119.00  166
 43  \w   -109.00 -79.00   0.50    0.20    --  -42.26-138.00 -30.00   60
 44  \w   -109.00 -79.00   0.50    0.20    --  -42.26-138.00 -90.00   60
 45  \w   -109.00 -79.00   0.50    0.20    --  -42.26-138.00-150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0177952000
_diffrn_orient_matrix_UB_12      -0.1863880000
_diffrn_orient_matrix_UB_13      0.0307529000
_diffrn_orient_matrix_UB_21      -0.0699741000
_diffrn_orient_matrix_UB_22      0.0218446000
_diffrn_orient_matrix_UB_23      0.0614018000
_diffrn_orient_matrix_UB_31      -0.0722154000
_diffrn_orient_matrix_UB_32      -0.0671224000
_diffrn_orient_matrix_UB_33      -0.0653845000
_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  0.0365
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19529
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.932
_diffrn_reflns_theta_min         3.792
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.924
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+2.8587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3278
_reflns_number_total             3443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           C-2
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_database_code               7715606
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ta N O C H'
_shelx_estimated_absorpt_t_max   0.515
_shelx_estimated_absorpt_t_min   0.208
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C14(H14), C15(H15), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              19521
_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 2.142
_oxdiff_exptl_absorpt_empirical_full_min 0.623