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_7715605
_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         'C24 H30 N Nb O5'
_chemical_formula_sum            'C24 H30 N Nb O5'
_chemical_formula_weight         505.40
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-07
_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                 108.275(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.5797(4)
_cell_length_b                   7.4688(2)
_cell_length_c                   31.9583(9)
_cell_measurement_reflns_used    5427
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.8100
_cell_measurement_theta_min      2.8920
_cell_volume                     4664.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_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 2014/5 (Sheldrick, 2014)'
_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 0.994
_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     -4.00  79.00   0.50   10.00    --   41.95-104.00 -39.00  166
  2  \w    -79.00   4.00   0.50   10.00    --  -42.26 104.00  61.00  166
  3  \w     24.00 108.00   0.50   30.00    --   93.72-104.00 -39.00  168
  4  \w     83.00 163.00   0.50   30.00    --   93.72 104.00  61.00  160
  5  \w   -164.00 -83.00   0.50   30.00    --  -94.03-104.00 -39.00  162
  6  \w   -107.00 -24.00   0.50   30.00    --  -94.03 104.00  61.00  166
  7  \w    -24.00  37.00   0.50   10.00    --   41.95 -32.00 -90.00  122
  8  \w    -28.00  28.00   0.50   10.00    --   41.95 -21.00 -30.00  112
  9  \w    -33.00  24.00   0.50   10.00    --   41.95 -11.00  30.00  114
 10  \w    -48.00  24.00   0.50   10.00    --  -42.26  43.00 120.00  144
 11  \w   -109.00 -79.00   0.50   10.00    --  -42.26-138.00  90.00   60
 12  \w   -109.00 -79.00   0.50   10.00    --  -42.26-138.00 -60.00   60
 13  \w   -109.00 -79.00   0.50   10.00    --  -42.26-138.00  60.00   60
 14  \w    -28.00  28.00   0.50   10.00    --  -42.26  21.00-180.00  112
 15  \w    -48.00  24.00   0.50   10.00    --  -42.26  43.00 -60.00  144
 16  \w    -28.00  28.00   0.50   10.00    --  -42.26  21.00  60.00  112
 17  \w     28.00  57.00   0.50   30.00    --   93.72 -50.00 -30.00   58
 18  \w    101.00 162.00   0.50   30.00    --   93.72  77.00  30.00  122
 19  \w    101.00 162.00   0.50   30.00    --   93.72  77.00 -60.00  122
 20  \w     28.00  57.00   0.50   30.00    --   93.72 -50.00   0.00   58
 21  \w     28.00  57.00   0.50   30.00    --   93.72 -50.00 -60.00   58
 22  \w     26.00  83.00   0.50   30.00    --   93.72 -68.00 -60.00  114
 23  \w   -159.00 -92.00   0.50   30.00    --  -94.03-117.00 -60.00  134
 24  \w    -83.00 -26.00   0.50   30.00    --  -94.03  68.00  60.00  114
 25  \w   -109.00 -29.00   0.50   30.00    --  -94.03 117.00 -30.00  160
 26  \w   -153.00 -99.00   0.50   30.00    --  -94.03 -96.00 -60.00  108
 27  \w   -153.00-102.00   0.50   30.00    --  -94.03 -68.00-150.00  102
 28  \w   -129.00 -97.00   0.50   30.00    --  -94.03-117.00-150.00   64
 29  \w   -162.00-102.00   0.50   30.00    --  -94.03 -77.00  30.00  120
 30  \w   -108.00 -34.00   0.50   30.00    --  -94.03 117.00  90.00  148
 31  \w    -57.00 -28.00   0.50   30.00    --  -94.03  50.00 -60.00   58
 32  \w   -123.00 -84.00   0.50   30.00    --  -94.03 -25.00   0.00   78
;
_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      -0.0221262000
_diffrn_orient_matrix_UB_12      0.1946331000
_diffrn_orient_matrix_UB_13      0.0040902000
_diffrn_orient_matrix_UB_21      0.0011054000
_diffrn_orient_matrix_UB_22      0.0390420000
_diffrn_orient_matrix_UB_23      -0.0471194000
_diffrn_orient_matrix_UB_31      -0.0756061000
_diffrn_orient_matrix_UB_32      -0.0563145000
_diffrn_orient_matrix_UB_33      -0.0184633000
_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  0.0609
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            15375
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.982
_diffrn_reflns_theta_min         2.912
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
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    1.439
_exptl_crystal_description       plate
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.053
_refine_diff_density_max         3.166
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0631
_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^)+(0.1241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3329
_reflns_number_total             4223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           C-1tBu
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_database_code               7715605
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ta Cl O N C H'
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.648
_reflns_odcompleteness_completeness 99.91
_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:
 C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C14(H14), 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), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              55246
_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 1.912
_oxdiff_exptl_absorpt_empirical_full_min 0.351