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_7715604
_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 Nb O5'
_chemical_formula_sum            'C17 H25 Cl N Nb O5'
_chemical_formula_weight         451.74
_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             2022-05-16
_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                 94.0660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4876(2)
_cell_length_b                   13.0436(2)
_cell_length_c                   22.1841(3)
_cell_measurement_reflns_used    16623
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.9320
_cell_measurement_theta_min      3.8950
_cell_volume                     3892.96(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 0.998
_diffrn_measured_fraction_theta_max 0.986
_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     19.00 115.00   0.50    1.00    --   41.95  15.00-154.00  192
  2  \w    -31.00  24.00   0.50    1.00    --   41.95 -15.00  35.00  110
  3  \w     70.00 167.00   0.50    5.00    --   93.72  15.00-154.00  194
  4  \w   -167.00 -73.00   0.50    5.00    --  -94.03 -15.00  35.00  188
  5  \w    -28.00  28.00   0.50    1.00    --   41.95 -21.00-120.00  112
  6  \w     19.00  99.00   0.50    1.00    --   41.95-138.00 -30.00  160
  7  \w     23.00 108.00   0.50    1.00    --   41.95  54.00-150.00  170
  8  \w   -109.00 -79.00   0.50    1.00    --  -42.26-138.00 150.00   60
  9  \w    -28.00  28.00   0.50    1.00    --  -42.26  21.00   0.00  112
 10  \w   -109.00 -79.00   0.50    1.00    --  -42.26-138.00 -90.00   60
 11  \w   -109.00 -79.00   0.50    1.00    --  -42.26-138.00 -30.00   60
 12  \w    -24.00  31.00   0.50    1.00    --  -42.26  15.00-154.00  110
 13  \w   -109.00 -79.00   0.50    1.00    --  -42.26-138.00-120.00   60
 14  \w    -79.00   4.00   0.50    1.00    --  -42.26 104.00-180.00  166
 15  \w   -115.00 -21.00   0.50    1.00    --  -42.26 -15.00  35.00  188
 16  \w   -109.00 -79.00   0.50    1.00    --  -42.26-138.00-180.00   60
 17  \w     28.00  57.00   0.50    5.00    --   93.72 -50.00 -60.00   58
 18  \w     28.00  57.00   0.50    5.00    --   93.72 -50.00-120.00   58
 19  \w   -160.00 -87.00   0.50    5.00    --  -94.03 -59.00   0.00  146
 20  \w    -68.00 -27.00   0.50    5.00    --  -94.03  59.00   0.00   82
 21  \w    -57.00 -28.00   0.50    5.00    --  -94.03  50.00-180.00   58
 22  \w   -109.00 -29.00   0.50    5.00    --  -94.03 117.00 -90.00  160
 23  \w   -109.00 -29.00   0.50    5.00    --  -94.03 117.00-150.00  160
 24  \w   -161.00 -97.00   0.50    5.00    --  -94.03 -68.00 -30.00  128
 25  \w    -68.00 -27.00   0.50    5.00    --  -94.03  59.00-150.00   82
 26  \w   -161.00 -97.00   0.50    5.00    --  -94.03 -68.00 -60.00  128
 27  \w    -57.00 -28.00   0.50    5.00    --  -94.03  50.00  90.00   58
 28  \w    -57.00 -28.00   0.50    5.00    --  -94.03  50.00  30.00   58
 29  \w    -57.00 -28.00   0.50    5.00    --  -94.03  50.00-120.00   58
 30  \w    -68.00 -27.00   0.50    5.00    --  -94.03  59.00 120.00   82
 31  \w    -57.00 -28.00   0.50    5.00    --  -94.03  50.00 -30.00   58
 32  \w   -160.00 -83.00   0.50    5.00    --  -94.03 -33.00   0.00  154
 33  \w   -106.00 -22.00   0.50    5.00    --  -94.03  96.00  90.00  168
 34  \w   -161.00 -99.00   0.50    5.00    --  -94.03 -68.00  90.00  124
 35  \w   -102.00 -37.00   0.50    5.00    --  -94.03  96.00-150.00  130
;
_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      -0.1139528000
_diffrn_orient_matrix_UB_12      0.0113036000
_diffrn_orient_matrix_UB_13      -0.0063551000
_diffrn_orient_matrix_UB_21      -0.0041742000
_diffrn_orient_matrix_UB_22      -0.0191448000
_diffrn_orient_matrix_UB_23      0.0682508000
_diffrn_orient_matrix_UB_31      0.0104536000
_diffrn_orient_matrix_UB_32      0.1160769000
_diffrn_orient_matrix_UB_33      0.0119116000
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29938
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.350
_diffrn_reflns_theta_min         3.722
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.530
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63420
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0386P)^2^+0.9597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6137
_reflns_number_total             7048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           I-3
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_database_code               7715604
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H Nb O N Cl'
_shelx_estimated_absorpt_t_max   0.695
_shelx_estimated_absorpt_t_min   0.403
_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:
 C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C29(H29A,H29B), C31(H31A,
 H31B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C19(H19), C20(H20), C22(H22), C25(H25)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              33427
_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 2.858
_oxdiff_exptl_absorpt_empirical_full_min 0.315