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_7715601
_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 Nb O5'
_chemical_formula_sum            'C18 H28 N Nb O5'
_chemical_formula_weight         431.32
_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             2022-05-16
_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                 98.4580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.4282(3)
_cell_length_b                   8.11400(10)
_cell_length_c                   15.99700(10)
_cell_measurement_reflns_used    28134
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.9400
_cell_measurement_theta_min      2.9270
_cell_volume                     3906.61(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -19.00  77.00   0.50    0.40    --   41.95-101.00 106.00  192
  2  \w    -77.00  19.00   0.50    0.40    --  -42.26 101.00-149.00  192
  3  \w     84.00 165.00   0.50    1.20    --   93.72 101.00-149.00  162
  4  \w     23.00 107.00   0.50    1.20    --   93.72-101.00 106.00  168
  5  \w   -107.00 -23.00   0.50    1.20    --  -94.03 101.00-149.00  168
  6  \w   -165.00 -84.00   0.50    1.20    --  -94.03-101.00 106.00  162
  7  \w     27.00 108.00   0.50    0.40    --   41.95  43.00 150.00  162
  8  \w    -23.00  48.00   0.50    0.40    --   41.95 -43.00 -30.00  142
  9  \w     19.00  99.00   0.50    0.40    --   41.95-138.00  60.00  160
 10  \w    -33.00  24.00   0.50    0.40    --   41.95 -11.00 120.00  114
 11  \w     28.00 112.00   0.50    0.40    --   41.95  21.00  60.00  168
 12  \w    -25.00  68.00   0.50    0.40    --   41.95 -77.00-120.00  186
 13  \w    -33.00  24.00   0.50    0.40    --   41.95 -11.00-180.00  114
 14  \w   -112.00 -29.00   0.50    0.40    --  -42.26 -21.00 -60.00  166
 15  \w    -28.00  28.00   0.50    0.40    --  -42.26  21.00 150.00  112
 16  \w   -109.00 -79.00   0.50    0.40    --  -42.26-138.00  90.00   60
 17  \w   -109.00 -79.00   0.50    0.40    --  -42.26-138.00 150.00   60
 18  \w    -24.00  32.00   0.50    0.40    --  -42.26  11.00 150.00  112
 19  \w   -109.00 -79.00   0.50    0.40    --  -42.26-138.00-120.00   60
 20  \w    -24.00  32.00   0.50    0.40    --  -42.26  11.00 -30.00  112
 21  \w    -37.00  24.00   0.50    0.40    --  -42.26  32.00-150.00  122
 22  \w     28.00 109.00   0.50    1.20    --   93.72-117.00 -90.00  162
 23  \w     28.00  57.00   0.50    1.20    --   93.72 -50.00 150.00   58
 24  \w     83.00 162.00   0.50    1.20    --   93.72  25.00-180.00  158
 25  \w     76.00 160.00   0.50    1.20    --   93.72  50.00  60.00  168
 26  \w     28.00  57.00   0.50    1.20    --   93.72 -50.00 120.00   58
 27  \w     28.00  57.00   0.50    1.20    --   93.72 -50.00-180.00   58
 28  \w     27.00 127.00   0.50    1.20    --   93.72-145.00 120.00  200
 29  \w     25.00 105.00   0.50    1.20    --   93.72 -77.00 120.00  160
 30  \w     28.00  57.00   0.50    1.20    --   93.72 -50.00  90.00   58
 31  \w     79.00 160.00   0.50    1.20    --   93.72  42.00 -30.00  162
 32  \w     26.00  83.00   0.50    1.20    --   93.72 -68.00  90.00  114
 33  \w     28.00 109.00   0.50    1.20    --   93.72-117.00 -60.00  162
 34  \w     92.00 159.00   0.50    1.20    --   93.72 117.00  90.00  134
 35  \w     87.00 161.00   0.50    1.20    --   93.72  59.00-180.00  148
 36  \w    101.00 162.00   0.50    1.20    --   93.72  77.00-120.00  122
 37  \w     97.00 162.00   0.50    1.20    --   93.72  68.00 -30.00  130
 38  \w   -109.00 -29.00   0.50    1.20    --  -94.03 117.00 120.00  160
 39  \w   -162.00-101.00   0.50    1.20    --  -94.03 -77.00-120.00  122
 40  \w    -83.00 -26.00   0.50    1.20    --  -94.03  68.00-150.00  114
 41  \w   -163.00-101.00   0.50    1.20    --  -94.03 -87.00   0.00  124
 42  \w   -161.00 -97.00   0.50    1.20    --  -94.03 -68.00 -30.00  128
 43  \w    -68.00 -27.00   0.50    1.20    --  -94.03  59.00-120.00   82
 44  \w   -160.00 -87.00   0.50    1.20    --  -94.03 -59.00-180.00  146
 45  \w   -106.00 -22.00   0.50    1.20    --  -94.03  96.00  30.00  168
 46  \w   -109.00 -29.00   0.50    1.20    --  -94.03 117.00  30.00  160
 47  \w   -160.00 -87.00   0.50    1.20    --  -94.03 -59.00  60.00  146
 48  \w    -57.00 -28.00   0.50    1.20    --  -94.03  50.00  60.00   58
 49  \w   -159.00 -92.00   0.50    1.20    --  -94.03-117.00 150.00  134
 50  \w   -163.00 -83.00   0.50    1.20    --  -94.03 -25.00   0.00  160
 51  \w     23.00 108.00   0.50    0.40    --   41.95  54.00 120.00  170
 52  \w     23.00 108.00   0.50    0.40    --   41.95  54.00 150.00  170
 53  \w     23.00 108.00   0.50    0.40    --   41.95  54.00-180.00  170
 54  \w     23.00 108.00   0.50    0.40    --   41.95  54.00 -30.00  170
 55  \w     23.00 108.00   0.50    0.40    --   41.95  54.00  90.00  170
 56  \w     23.00 108.00   0.50    0.40    --   41.95  54.00  30.00  170
 57  \w     23.00 108.00   0.50    0.40    --   41.95  54.00-120.00  170
 58  \w     23.00 108.00   0.50    0.40    --   41.95  54.00 -90.00  170
 59  \w     23.00 108.00   0.50    0.40    --   41.95  54.00-150.00  170
 60  \w     23.00 108.00   0.50    0.40    --   41.95  54.00  60.00  170
 61  \w   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00-120.00  168
 62  \w   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00 -60.00  168
 63  \w   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00-150.00  168
 64  \w   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00-180.00  168
 65  \w   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00 -90.00  168
 66  \w     76.00 160.00   0.50    1.20    --   93.72  50.00   0.00  168
 67  \w     28.00  57.00   0.50    1.20    --   93.72 -50.00 -90.00   58
 68  \w     76.00 160.00   0.50    1.20    --   93.72  50.00 -90.00  168
 69  \w     76.00 160.00   0.50    1.20    --   93.72  50.00 120.00  168
 70  \w   -160.00 -77.00   0.50    1.20    --  -94.03 -50.00-150.00  166
 71  \w    -57.00 -28.00   0.50    1.20    --  -94.03  50.00  30.00   58
;
_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      0.0137130000
_diffrn_orient_matrix_UB_12      0.1689148000
_diffrn_orient_matrix_UB_13      -0.0318219000
_diffrn_orient_matrix_UB_21      -0.0070049000
_diffrn_orient_matrix_UB_22      -0.0654212000
_diffrn_orient_matrix_UB_23      -0.0914034000
_diffrn_orient_matrix_UB_31      -0.0487958000
_diffrn_orient_matrix_UB_32      0.0569329000
_diffrn_orient_matrix_UB_33      -0.0108235000
_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  0.0442
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_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       -19
_diffrn_reflns_number            36703
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.942
_diffrn_reflns_theta_min         2.936
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74150
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 2547 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.033(6)
_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     463
_refine_ls_number_reflns         6259
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0546P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    0.765
_reflns_Friedel_fraction_max     0.763
_reflns_number_gt                6106
_reflns_number_total             6259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           I-1
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_database_code               7715601
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N O Nb'
_shelx_estimated_absorpt_t_max   0.744
_shelx_estimated_absorpt_t_min   0.391
_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), C26(H26)
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), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              18306
_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 1.430
_oxdiff_exptl_absorpt_empirical_full_min 0.720