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_7715607
_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         'C20 H21 Cl N Nb O6'
_chemical_formula_sum            'C20 H21 Cl N Nb O6'
_chemical_formula_weight         499.74
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-17
_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                115.7499(18)
_cell_angle_beta                 90.3226(17)
_cell_angle_gamma                91.8519(16)
_cell_formula_units_Z            2
_cell_length_a                   7.93594(17)
_cell_length_b                   11.4858(2)
_cell_length_c                   12.4086(2)
_cell_measurement_reflns_used    10697
_cell_measurement_temperature    120.00(16)
_cell_measurement_theta_max      67.9160
_cell_measurement_theta_min      3.9300
_cell_volume                     1017.96(4)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(16)
_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 0.991
_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      2.00  80.00   0.50    2.00    --   41.95-111.00-156.00  156
  2  \w    -80.00  -2.00   0.50    2.00    --  -42.26 111.00 -62.00  156
  3  \w     30.00 109.00   0.50    8.00    --   93.72-111.00-156.00  158
  4  \w     81.00 158.00   0.50    8.00    --   93.72 111.00 -62.00  154
  5  \w   -158.00 -81.00   0.50    8.00    --  -94.03-111.00-156.00  154
  6  \w   -109.00 -30.00   0.50    8.00    --  -94.03 111.00 -62.00  158
  7  \w    -28.00  28.00   0.50    2.00    --   41.95 -21.00 -30.00  112
  8  \w    -24.00  37.00   0.50    2.00    --   41.95 -32.00   0.00  122
  9  \w    -23.00  48.00   0.50    2.00    --   41.95 -43.00-120.00  142
 10  \w    -28.00  28.00   0.50    2.00    --   41.95 -21.00-150.00  112
 11  \w    -15.00  72.00   0.50    2.00    --   41.95 -89.00  30.00  174
 12  \w    -33.00  24.00   0.50    2.00    --   41.95 -11.00 -90.00  114
 13  \w    -64.00  25.00   0.50    2.00    --  -42.26  65.00-120.00  178
 14  \w   -112.00 -29.00   0.50    2.00    --  -42.26 -21.00-150.00  166
 15  \w    -24.00  32.00   0.50    2.00    --  -42.26  11.00-120.00  112
 16  \w   -109.00 -79.00   0.50    2.00    --  -42.26-138.00 -90.00   60
 17  \w    -78.00   4.00   0.50    2.00    --  -42.26 104.00  90.00  164
 18  \w   -112.00 -29.00   0.50    2.00    --  -42.26 -21.00 -90.00  166
 19  \w    -28.00  28.00   0.50    2.00    --  -42.26  21.00-180.00  112
 20  \w     28.00  57.00   0.50    8.00    --   93.72 -50.00 -90.00   58
 21  \w     28.00  57.00   0.50    8.00    --   93.72 -50.00  30.00   58
 22  \w     28.00  57.00   0.50    8.00    --   93.72 -50.00-180.00   58
 23  \w     87.00 161.00   0.50    8.00    --   93.72  59.00  30.00  148
 24  \w     28.00  57.00   0.50    8.00    --   93.72 -50.00-120.00   58
 25  \w     27.00 127.00   0.50    8.00    --   93.72-145.00  90.00  200
 26  \w     99.00 165.00   0.50    8.00    --   93.72  96.00 -30.00  132
 27  \w     28.00  57.00   0.50    8.00    --   93.72 -50.00 -30.00   58
 28  \w     23.00 106.00   0.50    8.00    --   93.72 -96.00-150.00  166
 29  \w     79.00 160.00   0.50    8.00    --   93.72  42.00  60.00  162
 30  \w     27.00 127.00   0.50    8.00    --   93.72-145.00-150.00  200
 31  \w     26.00  83.00   0.50    8.00    --   93.72 -68.00-180.00  114
 32  \w    101.00 162.00   0.50    8.00    --   93.72  77.00  60.00  122
 33  \w     28.00  57.00   0.50    8.00    --   93.72 -50.00-150.00   58
 34  \w   -159.00 -79.00   0.50    8.00    --  -94.03 -42.00-150.00  160
 35  \w   -105.00 -25.00   0.50    8.00    --  -94.03  77.00 -60.00  160
 36  \w   -106.00 -23.00   0.50    8.00    --  -94.03  96.00  60.00  166
 37  \w   -161.00 -97.00   0.50    8.00    --  -94.03 -68.00 -60.00  128
 38  \w    -83.00 -26.00   0.50    8.00    --  -94.03  68.00  60.00  114
 39  \w   -105.00 -25.00   0.50    8.00    --  -94.03  77.00   0.00  160
 40  \w   -163.00-101.00   0.50    8.00    --  -94.03 -87.00   0.00  124
 41  \w    -83.00 -26.00   0.50    8.00    --  -94.03  68.00 -60.00  114
 42  \w   -109.00 -32.00   0.50    8.00    --  -94.03 117.00  60.00  154
 43  \w   -106.00 -23.00   0.50    8.00    --  -94.03  96.00 120.00  166
 44  \w   -161.00 -97.00   0.50    8.00    --  -94.03 -68.00 -30.00  128
 45  \w    -83.00 -26.00   0.50    8.00    --  -94.03  68.00 120.00  114
 46  \w     23.00 108.00   0.50    2.00    --   41.95  54.00   0.00  170
 47  \w     23.00 108.00   0.50    2.00    --   41.95  54.00  60.00  170
 48  \w     23.00 108.00   0.50    2.00    --   41.95  54.00  90.00  170
 49  \w     23.00 108.00   0.50    2.00    --   41.95  54.00 150.00  170
 50  \w     27.00 108.00   0.50    2.00    --   41.95  43.00 -30.00  162
 51  \w     23.00 108.00   0.50    2.00    --   41.95  54.00-150.00  170
 52  \w     23.00 108.00   0.50    2.00    --   41.95  54.00  30.00  170
 53  \w     23.00 108.00   0.50    2.00    --   41.95  54.00 120.00  170
 54  \w   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00-180.00  168
 55  \w   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00   0.00  168
 56  \w   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00 120.00  168
 57  \w   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00-120.00  168
 58  \w   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00-150.00  168
 59  \w     79.00 160.00   0.50    8.00    --   93.72  42.00 120.00  162
 60  \w     76.00 133.00   0.50    8.00    --   93.72  50.00  30.00  114
 61  \w     76.00 160.00   0.50    8.00    --   93.72  50.00 -30.00  168
 62  \w     76.00 160.00   0.50    8.00    --   93.72  50.00 150.00  168
 63  \w     76.00 160.00   0.50    8.00    --   93.72  50.00  90.00  168
 64  \w     76.00 160.00   0.50    8.00    --   93.72  50.00   0.00  168
 65  \w   -161.00 -97.00   0.50    8.00    --  -94.03 -68.00 -90.00  128
 66  \w   -160.00 -77.00   0.50    8.00    --  -94.03 -50.00-120.00  166
 67  \w   -160.00 -77.00   0.50    8.00    --  -94.03 -50.00 -90.00  166
 68  \w   -160.00 -77.00   0.50    8.00    --  -94.03 -50.00-180.00  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      -0.1031547000
_diffrn_orient_matrix_UB_12      0.1230768000
_diffrn_orient_matrix_UB_13      0.0459348000
_diffrn_orient_matrix_UB_21      0.0051392000
_diffrn_orient_matrix_UB_22      0.0071283000
_diffrn_orient_matrix_UB_23      0.1268584000
_diffrn_orient_matrix_UB_31      0.1645433000
_diffrn_orient_matrix_UB_32      0.0837270000
_diffrn_orient_matrix_UB_33      0.0283920000
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19633
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.084
_diffrn_reflns_theta_min         3.956
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.356
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.630
_exptl_crystal_description       needle
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0531P)^2^+1.1394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3393
_reflns_number_total             3682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           C-3OMe
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_original_cell_volume        1017.95(4)
_cod_database_code               7715607
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Nb Cl O N C H'
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.437
_reflns_odcompleteness_completeness 99.94
_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:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C14(H14), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C)
;
_shelx_res_checksum              70519
_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 1.730
_oxdiff_exptl_absorpt_empirical_full_min 0.408