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_7715603
_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         'C18 H28 N O5 Ta'
_chemical_formula_sum            'C18 H28 N O5 Ta'
_chemical_formula_weight         519.36
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                 98.4290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.4758(4)
_cell_length_b                   8.11590(10)
_cell_length_c                   16.0060(3)
_cell_measurement_reflns_used    25075
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.8310
_cell_measurement_theta_min      2.9130
_cell_volume                     3916.14(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.989
_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    -30.00  74.00   0.50    0.20    --   41.95 -96.00-140.00  208
  2  \w    -75.00  30.00   0.50    0.20    --  -42.26  96.00 -31.00  210
  3  \w     22.00 106.00   0.50    0.60    --   93.72 -96.00-140.00  168
  4  \w   -166.00 -83.00   0.50    0.60    --  -94.03 -96.00-140.00  166
  5  \w     22.00  56.00   0.50    0.20    --   41.95  58.00-137.86   68
  6  \w    -24.00  37.00   0.50    0.20    --   41.95 -32.00-180.00  122
  7  \w    -24.00  37.00   0.50    0.20    --   41.95 -32.00 -60.00  122
  8  \w    -28.00  28.00   0.50    0.20    --   41.95 -21.00-120.00  112
  9  \w    -23.00  48.00   0.50    0.20    --   41.95 -43.00-120.00  142
 10  \w     21.00  48.00   0.50    0.20    --   41.95  61.00 107.89   54
 11  \w     23.00  66.00   0.50    0.20    --   41.95  56.00  71.49   86
 12  \w    -28.00  28.00   0.50    0.20    --   41.95 -21.00   0.00  112
 13  \w     22.00  50.00   0.50    0.20    --   41.95  60.00 150.30   56
 14  \w    -48.00  24.00   0.50    0.20    --  -42.26  43.00  60.00  144
 15  \w   -100.00 -19.00   0.50    0.20    --  -42.26 138.00 120.00  162
 16  \w   -108.00 -24.00   0.50    0.20    --  -42.26 -54.00  30.00  168
 17  \w    -24.00  32.00   0.50    0.20    --  -42.26  11.00-180.00  112
 18  \w   -109.00 -79.00   0.50    0.20    --  -42.26-138.00   0.00   60
 19  \w    -60.00 -23.00   0.50    0.20    --  -42.26 -57.00  65.97   74
 20  \w    -53.00 -22.00   0.50    0.20    --  -42.26 -59.00-140.66   62
 21  \w   -109.00 -79.00   0.50    0.20    --  -42.26-138.00 -30.00   60
 22  \w    -53.00 -22.00   0.50    0.20    --  -42.26 -59.00 -94.14   62
 23  \w    -53.00 -22.00   0.50    0.20    --  -42.26 -59.00-170.19   62
 24  \w    -37.00  24.00   0.50    0.20    --  -42.26  32.00 120.00  122
 25  \w    -24.00  32.00   0.50    0.20    --  -42.26  11.00 -90.00  112
 26  \w     28.00  57.00   0.50    0.60    --   93.72 -50.00  90.00   58
 27  \w     28.00 109.00   0.50    0.60    --   93.72-117.00 -30.00  162
 28  \w     28.00 109.00   0.50    0.60    --   93.72-117.00  60.00  162
 29  \w     79.00 160.00   0.50    0.60    --   93.72  42.00 -60.00  162
 30  \w     92.00 159.00   0.50    0.60    --   93.72 117.00 -60.00  134
 31  \w     79.00 160.00   0.50    0.60    --   93.72  42.00 -90.00  162
 32  \w     28.00  57.00   0.50    0.60    --   93.72 -50.00-180.00   58
 33  \w     27.00 127.00   0.50    0.60    --   93.72-145.00 -90.00  200
 34  \w     26.00  83.00   0.50    0.60    --   93.72 -68.00-120.00  114
 35  \w     28.00 109.00   0.50    0.60    --   93.72-117.00  30.00  162
 36  \w     28.00 109.00   0.50    0.60    --   93.72-117.00-180.00  162
 37  \w     28.00  57.00   0.50    0.60    --   93.72 -50.00  60.00   58
 38  \w     84.00 166.00   0.50    0.60    --   93.72  96.00 -31.00  164
 39  \w     26.00  83.00   0.50    0.60    --   93.72 -68.00   0.00  114
 40  \w    -57.00 -28.00   0.50    0.60    --  -94.03  50.00-120.00   58
 41  \w   -160.00 -77.00   0.50    0.60    --  -94.03 -50.00 150.00  166
 42  \w   -162.00-101.00   0.50    0.60    --  -94.03 -77.00  30.00  122
 43  \w   -159.00 -92.00   0.50    0.60    --  -94.03-117.00 -90.00  134
 44  \w   -160.00 -83.00   0.50    0.60    --  -94.03 -33.00  90.00  154
 45  \w    -68.00 -27.00   0.50    0.60    --  -94.03  59.00 120.00   82
 46  \w   -160.00 -83.00   0.50    0.60    --  -94.03 -33.00  60.00  154
 47  \w   -109.00 -29.00   0.50    0.60    --  -94.03 117.00-150.00  160
 48  \w   -160.00 -77.00   0.50    0.60    --  -94.03 -50.00-120.00  166
 49  \w   -162.00-101.00   0.50    0.60    --  -94.03 -77.00-180.00  122
 50  \w   -160.00 -77.00   0.50    0.60    --  -94.03 -50.00 120.00  166
 51  \w    -57.00 -28.00   0.50    0.60    --  -94.03  50.00 -30.00   58
 52  \w    -83.00 -26.00   0.50    0.60    --  -94.03  68.00 -30.00  114
 53  \w   -161.00 -97.00   0.50    0.60    --  -94.03 -68.00  90.00  128
 54  \w   -105.00 -25.00   0.50    0.60    --  -94.03  77.00-120.00  160
 55  \w    -57.00 -28.00   0.50    0.60    --  -94.03  50.00 -60.00   58
 56  \w   -106.00 -22.00   0.50    0.60    --  -94.03  96.00 -31.00  168
 57  \w     21.00  48.00   0.50    0.20    --   41.95  61.00  28.62   54
 58  \w     22.00  56.00   0.50    0.20    --   41.95  58.00 174.84   68
 59  \w     21.00  48.00   0.50    0.20    --   41.95  61.00  83.34   54
 60  \w     27.00 108.00   0.50    0.20    --   41.95  43.00 120.00  162
 61  \w     22.00  50.00   0.50    0.20    --   41.95  60.00-171.12   56
 62  \w     21.00  48.00   0.50    0.20    --   41.95  61.00-132.68   54
 63  \w     31.00 108.00   0.50    0.20    --   41.95  32.00 -90.00  154
 64  \w     23.00  66.00   0.50    0.20    --   41.95  56.00-107.21   86
 65  \w    -56.00 -22.00   0.50    0.20    --  -42.26 -58.00 174.35   68
 66  \w    -48.00 -22.00   0.50    0.20    --  -42.26 -61.00 -34.90   52
 67  \w   -109.00 -31.00   0.50    0.20    --  -42.26 -32.00 -30.00  156
 68  \w    -48.00 -22.00   0.50    0.20    --  -42.26 -61.00 -76.14   52
 69  \w    -53.00 -22.00   0.50    0.20    --  -42.26 -59.00 -57.64   62
 70  \w    -60.00 -23.00   0.50    0.20    --  -42.26 -57.00-115.49   74
 71  \w   -109.00 -27.00   0.50    0.20    --  -42.26 -43.00 -60.00  164
 72  \w    -79.00   4.00   0.50    0.20    --  -42.26 104.00 120.00  166
 73  \w   -109.00 -24.00   0.50    0.20    --  -42.26 -53.00 164.36  170
 74  \w    -60.00 -23.00   0.50    0.20    --  -42.26 -57.00 108.18   74
 75  \w     76.00 160.00   0.50    0.60    --   93.72  50.00 -30.00  168
 76  \w     87.00 161.00   0.50    0.60    --   93.72  59.00-150.00  148
 77  \w   -160.00 -75.00   0.50    0.60    --  -94.03 -55.00  74.76  170
 78  \w   -160.00 -75.00   0.50    0.60    --  -94.03 -54.00  -0.46  170
 79  \w   -160.00 -75.00   0.50    0.60    --  -94.03 -56.00-172.41  170
 80  \w   -161.00 -75.00   0.50    0.60    --  -94.03-145.00 -30.00  172
 81  \w   -160.00 -77.00   0.50    0.60    --  -94.03 -50.00  30.00  166
;
_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      -0.0464630000
_diffrn_orient_matrix_UB_12      0.0124645000
_diffrn_orient_matrix_UB_13      0.0265898000
_diffrn_orient_matrix_UB_21      -0.0101350000
_diffrn_orient_matrix_UB_22      -0.1777100000
_diffrn_orient_matrix_UB_23      -0.0306941000
_diffrn_orient_matrix_UB_31      0.0187367000
_diffrn_orient_matrix_UB_32      -0.0650766000
_diffrn_orient_matrix_UB_33      0.0884997000
_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  0.0651
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35982
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.387
_diffrn_reflns_theta_min         2.932
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50974
_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    1.762
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.073
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 2592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.047(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6422
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0436P)^2^+16.3483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    0.808
_reflns_Friedel_fraction_max     0.797
_reflns_number_gt                6186
_reflns_number_total             6422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           I-2
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_database_code               7715603
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ta O N C H'
_shelx_estimated_absorpt_t_max   0.512
_shelx_estimated_absorpt_t_min   0.242
_reflns_odcompleteness_completeness 100.00
_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:
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C31(H31A,H31B), C33(H33A,
 H33B), C35(H35A,H35B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C20(H20), C21(H21), C23(H23), C27(H27)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              8316
_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 1.911
_oxdiff_exptl_absorpt_empirical_full_min 0.577