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_7714511
_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         'C34 H45 N3 O Zn, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C34.5 H46 Cl N3 O Zn'
_chemical_formula_weight         619.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-08
_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                90
_cell_angle_beta                 135.126(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2654(6)
_cell_length_b                   16.8069(3)
_cell_length_c                   21.0819(11)
_cell_measurement_reflns_used    23702
_cell_measurement_temperature    120.01(11)
_cell_measurement_theta_max      28.9070
_cell_measurement_theta_min      3.4570
_cell_volume                     3316.2(6)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.904
_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    -69.00   0.00   1.00   25.00    --  -15.82 124.00 168.00   69
  2  \w    -83.00 -14.00   1.00   25.00    --  -15.82 148.00 -26.00   69
  3  \w     14.00  85.00   1.00   25.00    --   17.54-148.00 -74.00   71
  4  \w      0.00  70.00   1.00   25.00    --   17.54-124.00  89.00   70
  5  \w    -88.00 -39.00   1.00   25.00    --  -15.82-178.00-150.00   49
  6  \w    -85.00   3.00   1.00   25.00    --  -15.82 -38.00 150.00   88
  7  \w    -35.00  53.00   1.00   25.00    --  -15.82  38.00 -30.00   88
  8  \w    -33.00  51.00   1.00   25.00    --  -15.82  57.00 -90.00   84
  9  \w     -9.00  39.00   1.00   25.00    --   17.54  77.00-180.00   48
 10  \w     -9.00  39.00   1.00   25.00    --   17.54  77.00 -30.00   48
 11  \w     -9.00  39.00   1.00   25.00    --   17.54  77.00 150.00   48
 12  \w    -33.00  51.00   1.00   25.00    --  -15.82  57.00 120.00   84
 13  \w    -39.00  11.00   1.00   25.00    --  -15.82 -77.00-150.00   50
 14  \w     -9.00  20.00   1.00   25.00    --   17.54  77.00 120.00   29
 15  \w      1.00  85.00   1.00   25.00    --   17.54  57.00  30.00   84
;
_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      0.0445632000
_diffrn_orient_matrix_UB_12      -0.0265418000
_diffrn_orient_matrix_UB_13      0.0370152000
_diffrn_orient_matrix_UB_21      0.0301785000
_diffrn_orient_matrix_UB_22      0.0326000000
_diffrn_orient_matrix_UB_23      0.0300909000
_diffrn_orient_matrix_UB_31      -0.0533769000
_diffrn_orient_matrix_UB_32      -0.0037062000
_diffrn_orient_matrix_UB_33      -0.0001161000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            72427
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.535
_diffrn_reflns_theta_min         3.320
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82761
_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    1.241
_exptl_crystal_description       plate
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         8388
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0339P)^2^+1.8135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6909
_reflns_number_total             8388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03344a2.cif
_cod_data_source_block           db8-8_reprocessed
_cod_original_cell_volume        3316.2(4)
_cod_original_formula_sum        'C34.50 H46 Cl N3 O Zn'
_cod_database_code               7714511
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn1 N3 O1 C34 H46'
_chemical_oxdiff_usercomment     '@ 120 K '
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.706
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 Zn1-O1 \\sim Zn1-O1A
 with sigma of 0.02
 N3-C31 \\sim N3A-C31A
 with sigma of 0.02
 N3-C30 \\sim N3A-C30A
 with sigma of 0.02
 C31-C32 \\sim C31A-C32A
 with sigma of 0.02
 C33-C34 \\sim C33A-C34A
 with sigma of 0.02
 C33-C32 \\sim C33A-C32A
 with sigma of 0.02
 C30-C34 \\sim C30A-C34A
 with sigma of 0.02
 C30-O1 \\sim C30A-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1A) = Uanis(O1)
Uanis(N3A) = Uanis(N3)
Uanis(C34) = Uanis(C34A)
Uanis(C33) = Uanis(C33A)
Uanis(C32) = Uanis(C32A)
Uanis(C31) = Uanis(C31A)
Uanis(C30) = Uanis(C30A)
4. Others
 Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=
 Sof(C34A)=Sof(H34A)=Sof(N3A)=Sof(O1A)=1-FVAR(1)
 Sof(C30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=
 Sof(H34)=Sof(N3)=Sof(O1)=FVAR(1)
 Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) Cl1(0.5) Cl1A(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
5.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C31(H31),
 C31A(H31A), C32(H32), C32A(H32A), C33(H33), C33A(H33A), C34(H34), C34A(H34A)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              1946
_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 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.832