NacNac-zinc-pyridonate mediated ε-caprolactone ROP.
Hughes, Jack W. J.; Babula, Dawid J.; Stowers-Veitch, Findlay; Yuan, Kang; Uzelac, Marina; Nichol, Gary S.; Ingleson, Michael J.; Garden, Jennifer A.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt03344a

data_7714510
_publ_section_title
;
 NacNac-zinc-pyridonate mediated &#x3b5;-caprolactone ROP.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt03344a
_journal_year                    2023
_chemical_formula_moiety         'C35 H47 N3 O Zn'
_chemical_formula_sum            'C35 H47 N3 O Zn'
_chemical_formula_weight         591.12
_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             2022-06-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-27 deposited with the CCDC.	2023-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                78.352(2)
_cell_angle_beta                 83.508(2)
_cell_angle_gamma                70.096(2)
_cell_formula_units_Z            4
_cell_length_a                   12.3962(3)
_cell_length_b                   16.5432(4)
_cell_length_c                   17.1649(4)
_cell_measurement_reflns_used    16680
_cell_measurement_temperature    120.0(5)
_cell_measurement_theta_max      25.2800
_cell_measurement_theta_min      3.9140
_cell_volume                     3237.86(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -70.00  -2.00   1.00   20.00    --  -15.82 126.00   2.00   68
  2  \w    -81.00 -14.00   1.00   20.00    --  -15.82 145.00 170.00   67
  3  \w     14.00  83.00   1.00   20.00    --   17.54-145.00 117.00   69
  4  \w      2.00  72.00   1.00   20.00    --   17.54-126.00 -74.00   70
  5  \w     39.00  90.00   1.00   20.00    --   17.54 178.00  60.00   51
  6  \w     -9.00  39.00   1.00   20.00    --   17.54  77.00 150.00   48
  7  \w    -12.00  89.00   1.00   20.00    --   17.54  19.00 -60.00  101
  8  \w     -9.00  39.00   1.00   20.00    --   17.54  77.00   0.00   48
  9  \w    -12.00  89.00   1.00   20.00    --   17.54  19.00-150.00  101
 10  \w      1.00  85.00   1.00   20.00    --   17.54  57.00  90.00   84
 11  \w    -39.00  11.00   1.00   20.00    --  -15.82 -77.00 -30.00   50
 12  \w     -1.00  87.00   1.00   20.00    --   17.54  38.00 -30.00   88
 13  \w      1.00  85.00   1.00   20.00    --   17.54  57.00  30.00   84
 14  \w     -9.00  39.00   1.00   20.00    --   17.54  77.00-120.00   48
 15  \w    -20.00  56.00   1.00   20.00    --   17.54 -99.00   0.00   76
 16  \w    -50.00  34.00   1.00   20.00    --   17.54 -57.00-120.00   84
 17  \w    -20.00  56.00   1.00   20.00    --   17.54 -99.00-150.00   76
 18  \w    -50.00  34.00   1.00   20.00    --   17.54 -57.00 150.00   84
 19  \w    -20.00  22.00   1.00   20.00    --   17.54 -99.00  30.00   42
 20  \w    -20.00  56.00   1.00   20.00    --   17.54 -99.00 150.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0335975000
_diffrn_orient_matrix_UB_12      -0.0147033000
_diffrn_orient_matrix_UB_13      0.0340613000
_diffrn_orient_matrix_UB_21      0.0506952000
_diffrn_orient_matrix_UB_22      -0.0114476000
_diffrn_orient_matrix_UB_23      -0.0248064000
_diffrn_orient_matrix_UB_31      0.0036173000
_diffrn_orient_matrix_UB_32      0.0423994000
_diffrn_orient_matrix_UB_33      -0.0029560000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1119
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19098
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.375
_diffrn_reflns_theta_min         3.272
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method
'Crystallised from hexanes by cooling to -27 C.'
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         19098
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0459P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11599
_reflns_number_total             19098
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9192\% 
 around [1.00 0.00 -0.00] (reciprocal) or [0.97 -0.24 -0.03] (direct)
;
_cod_data_source_file            d3dt03344a2.cif
_cod_data_source_block           db39b_reprocess_twin1_hklf4
_cod_database_code               7714510
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn1 N3 O1 C35 H47'
_chemical_oxdiff_usercomment     '120 K'
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.730
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8736
 0.1264
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 C27, C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C29: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
C12 \\sim C13 \\sim C14: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C47(H47), C50(H50), C59(H59), C62(H62)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31),
 C32(H32), C33(H33), C37(H37), C43(H43), C44(H44), C45(H45), C55(H55), C56(H56),
  C57(H57), C67(H67), C68(H68), C69(H69)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              37540
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on MITEGEN holder in oil'
_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 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.795
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2