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_7715608
_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         'C17 H25 Cl N O5 Ta'
_chemical_formula_sum            'C17 H25 Cl N O5 Ta'
_chemical_formula_weight         539.78
_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             2022-05-02
_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                 94.0280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.50190(10)
_cell_length_b                   13.0675(2)
_cell_length_c                   22.1817(2)
_cell_measurement_reflns_used    42002
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.0430
_cell_measurement_theta_min      3.8780
_cell_volume                     3903.98(8)
_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 0.998
_diffrn_measured_fraction_theta_max 0.987
_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    -35.00  31.00   0.50    1.00    --   41.95  -6.00 171.00  132
  2  \w   -119.00  15.00   0.50    1.00    --  -42.26  -6.00 171.00  268
  3  \w    -31.00  34.00   0.50    1.00    --  -42.26   6.00 -12.00  130
  4  \w     25.00 170.00   0.50    4.00    --   93.72   6.00 -12.00  290
  5  \w   -171.00 -37.00   0.50    4.00    --  -94.03  -6.00 171.00  268
  6  \w    -27.00 119.00   0.50    1.00    --   41.95   6.00 -12.00  292
  7  \w     22.00  50.00   0.50    1.00    --   41.95  60.00-164.76   56
  8  \w     22.00  53.00   0.50    1.00    --   41.95  59.00 124.55   62
  9  \w     21.00  48.00   0.50    1.00    --   41.95  61.00 130.72   54
 10  \w     22.00  50.00   0.50    1.00    --   41.95  60.00  45.43   56
 11  \w     21.00  48.00   0.50    1.00    --   41.95  61.00  75.53   54
 12  \w     22.00  53.00   0.50    1.00    --   41.95  59.00-173.76   62
 13  \w    -24.00  37.00   0.50    1.00    --   41.95 -32.00 -60.00  122
 14  \w     22.00  50.00   0.50    1.00    --   41.95  60.00 115.84   56
 15  \w     31.00 108.00   0.50    1.00    --   41.95  32.00  60.00  154
 16  \w     19.00  99.00   0.50    1.00    --   41.95-138.00  90.00  160
 17  \w     22.00  50.00   0.50    1.00    --   41.95  60.00  95.89   56
 18  \w     21.00  48.00   0.50    1.00    --   41.95  61.00 104.72   54
 19  \w     21.00  48.00   0.50    1.00    --   41.95  61.00 -17.61   54
 20  \w     21.00  48.00   0.50    1.00    --   41.95  61.00-175.99   54
 21  \w     22.00  53.00   0.50    1.00    --   41.95  59.00 177.15   62
 22  \w     22.00  56.00   0.50    1.00    --   41.95  58.00  65.16   68
 23  \w    -23.00  48.00   0.50    1.00    --   41.95 -43.00 -60.00  142
 24  \w     21.00  48.00   0.50    1.00    --   41.95  61.00  -9.54   54
 25  \w     22.00  50.00   0.50    1.00    --   41.95  60.00-152.37   56
 26  \w     21.00  48.00   0.50    1.00    --   41.95  61.00 102.48   54
 27  \w     23.00 108.00   0.50    1.00    --   41.95  54.00-120.00  170
 28  \w     22.00  53.00   0.50    1.00    --   41.95  59.00 160.14   62
 29  \w     21.00  48.00   0.50    1.00    --   41.95  61.00-143.70   54
 30  \w    -28.00  28.00   0.50    1.00    --   41.95 -21.00-120.00  112
 31  \w     22.00  53.00   0.50    1.00    --   41.95  59.00  79.44   62
 32  \w    -79.00   4.00   0.50    1.00    --  -42.26 104.00 -30.00  166
 33  \w    -50.00 -25.00   0.50    1.00    --  -42.26 -60.00 113.12   50
 34  \w    -50.00 -25.00   0.50    1.00    --  -42.26 -60.00 135.77   50
 35  \w    -47.00  13.00   0.50    1.00    --  -42.26  43.00 120.00  120
 36  \w   -109.00 -81.00   0.50    1.00    --  -42.26-138.00 -30.00   56
 37  \w    -49.00  15.00   0.50    1.00    --  -42.26  -6.00 171.00  128
 38  \w    -50.00 -24.00   0.50    1.00    --  -42.26 -57.00  -1.05   52
 39  \w    -64.00 -29.00   0.50    1.00    --  -42.26 -21.00 120.00   70
 40  \w    -98.00 -73.00   0.50    1.00    --  -42.26 -21.00 120.00   50
 41  \w    -47.00 -22.00   0.50    1.00    --  -42.26 -61.00  51.64   50
 42  \w    -48.00 -22.00   0.50    1.00    --  -42.26 -60.00  63.74   52
 43  \w     28.00  57.00   0.50    4.00    --   93.72 -50.00-150.00   58
 44  \w     77.00 103.00   0.50    4.00    --   93.72  50.00 120.00   52
 45  \w     77.00 103.00   0.50    4.00    --   93.72  50.00  90.00   52
 46  \w     26.00  83.00   0.50    4.00    --   93.72 -68.00 150.00  114
 47  \w     76.00 102.00   0.50    4.00    --   93.72  53.00 135.95   52
 48  \w     76.00 102.00   0.50    4.00    --   93.72  50.00  60.00   52
 49  \w     28.00  57.00   0.50    4.00    --   93.72 -50.00-120.00   58
 50  \w     28.00 105.00   0.50    4.00    --   93.72 -77.00 -60.00  154
 51  \w    -53.00 -28.00   0.50    4.00    --  -94.03  59.00  60.00   50
 52  \w   -154.00-110.00   0.50    4.00    --  -94.03 -54.00  68.52   88
 53  \w   -102.00 -76.00   0.50    4.00    --  -94.03 -53.00  79.44   52
 54  \w    -83.00 -37.00   0.50    4.00    --  -94.03  68.00  90.00   92
 55  \w   -104.00 -75.00   0.50    4.00    --  -94.03 -54.00  12.81   58
 56  \w   -157.00-131.00   0.50    4.00    --  -94.03 -53.00  79.44   52
 57  \w   -159.00-133.00   0.50    4.00    --  -94.03 -54.00  12.81   52
 58  \w   -103.00 -75.00   0.50    4.00    --  -94.03 -54.00 117.80   56
 59  \w   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00  21.88   52
 60  \w   -102.00 -76.00   0.50    4.00    --  -94.03 -55.00  41.90   52
 61  \w   -100.00 -75.00   0.50    4.00    --  -94.03 -54.00  68.52   50
 62  \w   -102.00 -76.00   0.50    4.00    --  -94.03 -56.00 -24.20   52
 63  \w   -102.00 -76.00   0.50    4.00    --  -94.03 -53.00  13.82   52
 64  \w   -100.00 -75.00   0.50    4.00    --  -94.03 -55.00  35.02   50
 65  \w   -153.00-127.00   0.50    4.00    --  -94.03 -55.00  41.90   52
 66  \w   -155.00 -77.00   0.50    4.00    --  -94.03 -50.00  60.00  156
 67  \w    -82.00 -33.00   0.50    4.00    --  -94.03 117.00-120.00   98
 68  \w   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00 138.52   52
 69  \w    -61.00 -29.00   0.50    4.00    --  -94.03 117.00  90.00   64
 70  \w   -100.00 -75.00   0.50    4.00    --  -94.03 -54.00 125.27   50
 71  \w   -108.00 -70.00   0.50    4.00    --  -94.03 117.00  90.00   76
 72  \w   -102.00 -76.00   0.50    4.00    --  -94.03 -52.00  86.17   52
 73  \w   -160.00-135.00   0.50    4.00    --  -94.03 -54.00 125.27   50
 74  \w   -160.00 -75.00   0.50    4.00    --  -94.03 -55.00 105.24  170
 75  \w   -157.00-118.00   0.50    4.00    --  -94.03 -52.00  86.17   78
 76  \w   -114.00 -76.00   0.50    4.00    --  -94.03 -51.00 148.09   76
 77  \w   -160.00 -75.00   0.50    4.00    --  -94.03 -55.00  54.04  170
 78  \w   -159.00-133.00   0.50    4.00    --  -94.03 -51.00 148.09   52
 79  \w   -113.00 -76.00   0.50    4.00    --  -94.03 -56.00  -8.34   74
 80  \w    -57.00 -32.00   0.50    4.00    --  -94.03  50.00  30.00   50
 81  \w   -102.00 -76.00   0.50    4.00    --  -94.03 -54.00   2.21   52
 82  \w   -157.00-131.00   0.50    4.00    --  -94.03 -54.00   2.21   52
 83  \w   -156.00-116.00   0.50    4.00    --  -94.03 -56.00  -8.34   80
 84  \w    -62.00 -26.00   0.50    4.00    --  -94.03  96.00  90.00   72
 85  \w   -106.00 -66.00   0.50    4.00    --  -94.03  96.00  90.00   80
 86  \w    -58.00 -29.00   0.50    4.00    --  -94.03 117.00 -30.00   58
 87  \w   -103.00 -77.00   0.50    4.00    --  -94.03 -53.00   5.12   52
 88  \w   -134.00 -75.00   0.50    4.00    --  -94.03 -54.00 141.32  118
 89  \w   -160.00 -77.00   0.50    4.00    --  -94.03 -54.00 133.25  166
 90  \w   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00  -3.18   52
 91  \w   -103.00 -77.00   0.50    4.00    --  -94.03 -56.00  50.74   52
 92  \w   -101.00 -75.00   0.50    4.00    --  -94.03 117.00 -30.00   52
 93  \w   -115.00 -77.00   0.50    4.00    --  -94.03 -49.00  51.09   76
 94  \w   -103.00 -77.00   0.50    4.00    --  -94.03 -50.00  90.00   52
 95  \w   -102.00 -76.00   0.50    4.00    --  -94.03 -52.00  80.06   52
 96  \w   -103.00 -77.00   0.50    4.00    --  -94.03 -53.00 113.40   52
 97  \w   -103.00 -77.00   0.50    4.00    --  -94.03 -51.00  83.39   52
 98  \w   -103.00 -77.00   0.50    4.00    --  -94.03 -53.00 109.29   52
 99  \w   -100.00 -75.00   0.50    4.00    --  -94.03 -55.00  26.65   50
100  \w   -159.00 -75.00   0.50    4.00    --  -94.03 -54.00 -19.82  168
101  \w   -160.00-107.00   0.50    4.00    --  -94.03 -55.00  21.88  106
102  \w    -56.00 -30.00   0.50    4.00    --  -94.03  50.00 -90.00   52
103  \w   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00  23.92   52
104  \w   -100.00 -75.00   0.50    4.00    --  -94.03 -55.00  -7.88   50
105  \w   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00 146.35   52
106  \w    -55.00 -28.00   0.50    4.00    --  -94.03  50.00-120.00   54
;
_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      -0.1143935000
_diffrn_orient_matrix_UB_12      -0.0016511000
_diffrn_orient_matrix_UB_13      -0.0027940000
_diffrn_orient_matrix_UB_21      -0.0033139000
_diffrn_orient_matrix_UB_22      -0.0095651000
_diffrn_orient_matrix_UB_23      -0.0693292000
_diffrn_orient_matrix_UB_31      0.0019597000
_diffrn_orient_matrix_UB_32      -0.1174257000
_diffrn_orient_matrix_UB_33      0.0056649000
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            64517
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.343
_diffrn_reflns_theta_min         3.720
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.881
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28072
_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    1.837
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.067
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+3.3652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6356
_reflns_number_total             7080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           I-4
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_original_cell_volume        3903.99(8)
_cod_database_code               7715608
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ta N O C H Cl'
_shelx_estimated_absorpt_t_max   0.654
_shelx_estimated_absorpt_t_min   0.271
_reflns_odcompleteness_completeness 99.97
_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:
 C14(H14A,H14B), C29(H29A,H29B), C12(H12A,H12B), C33(H33A,H33B), C31(H31A,
 H31B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C25(H25), C5(H5), C20(H20), C19(H19), C2(H2), C22(H22), C3(H3)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C10(H10A,H10B,H10C), C28(H28A,H28B,
 H28C), C11(H11A,H11B,H11C), C34(H34A,H34B,H34C), C15(H15A,H15B,H15C), C13(H13A,
 H13B,H13C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              75054
_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 3.260
_oxdiff_exptl_absorpt_empirical_full_min 0.626