Hybrid amino/iminopyridines with auxiliary phosphines enabling active zinc catalysts for the ring-opening polymerization of lactide.
Xue, Xiaopan; Zhu, Dongzhi; Zhang, Wenjuan; Zheng, Tongxin; Wang, Rui; Ma, Yanping; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3388–3399; doi:10.1039/d5dt02857d

data_7720092
_publ_section_title
;
 Hybrid amino/iminopyridines with auxiliary phosphines enabling active
 zinc catalysts for the ring-opening polymerization of lactide.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3388
_journal_page_last               3399
_journal_paper_doi               10.1039/d5dt02857d
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         '2(C32 H36 Cl2 N3 P Zn)'
_chemical_formula_sum            'C64 H72 Cl4 N6 P2 Zn2'
_chemical_formula_weight         1259.75
_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     iterative
_audit_creation_date             2023-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-11-28 deposited with the CCDC.	2026-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                63.087(4)
_cell_angle_beta                 69.006(3)
_cell_angle_gamma                71.911(3)
_cell_formula_units_Z            2
_cell_length_a                   14.1106(5)
_cell_length_b                   15.8409(6)
_cell_length_c                   16.7144(5)
_cell_measurement_reflns_used    17849
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      74.5780
_cell_measurement_theta_min      3.0500
_cell_volume                     3060.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.959
_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     47.00 120.00   0.50    0.34    --   48.81  77.00-150.00  146
  2  \w     90.00 120.00   0.50    0.34    --   48.81 136.00 -93.00   60
  3  \w     99.00 124.00   0.50    0.80    --  101.25 136.00 -93.00   50
  4  \w     88.00 113.00   0.50    0.80    --  101.25 133.00  88.00   50
  5  \w     90.00 173.00   0.50    0.80    --  101.25  57.00 120.00  166
  6  \w     94.00 166.00   0.50    0.80    --  101.25  38.00  30.00  144
  7  \w     97.00 172.00   0.50    0.80    --  101.25  38.00 -90.00  150
  8  \w    -23.00  30.00   0.50    0.34    --   48.81 -19.00-120.00  106
  9  \w     29.00  68.00   0.50    0.80    --  101.25 -57.00-150.00   78
 10  \w     40.00  69.00   0.50    0.80    --  101.25 -57.00-180.00   58
 11  \w     30.00  62.00   0.50    0.80    --  101.25 -57.00  30.00   64
 12  \w    -18.00  17.00   0.50    0.34    --   48.81 -77.00 150.00   70
 13  \w     24.00  65.00   0.50    0.34    --   48.81 -77.00 150.00   82
 14  \w     30.00  68.00   0.50    0.80    --  101.25 -57.00 150.00   76
 15  \w     42.00  83.00   0.50    0.80    --  101.25 -99.00  90.00   82
 16  \w     67.00  94.00   0.50    0.80    --  101.25-133.00  20.00   54
 17  \w     60.00  96.00   0.50    0.34    --   48.81-133.00  20.00   72
 18  \w     55.00  81.00   0.50    0.34    --   48.81-136.00-157.00   52
 19  \w     74.00 116.00   0.50    0.80    --  101.25-136.00-157.00   84
 20  \w     57.00  87.00   0.50    0.80    --  101.25 -99.00-150.00   60
 21  \w     71.00 104.00   0.50    0.80    --  101.25 -99.00-120.00   66
 22  \w     32.00 106.00   0.50    0.80    --  101.25 -99.00  30.00  148
 23  \w   -120.00 -91.00   0.50    0.80    -- -103.25 136.00 -93.00   58
 24  \w   -112.00 -36.00   0.50    0.80    -- -103.25 125.00 -60.00  152
 25  \w    -88.00 -35.00   0.50    0.80    -- -103.25 125.00 -90.00  106
 26  \w   -111.00 -70.00   0.50    0.80    -- -103.25 125.00-150.00   82
 27  \w    -74.00 -48.00   0.50    0.80    -- -103.25 125.00   0.00   52
 28  \w   -109.00 -68.00   0.50    0.80    -- -103.25 117.00  -9.63   82
 29  \w   -111.00 -77.00   0.50    0.80    -- -103.25 125.00   0.00   68
 30  \w   -117.00 -54.00   0.50    0.80    -- -103.25 133.00  88.00  126
 31  \w   -112.00 -36.00   0.50    0.80    -- -103.25 125.00 120.00  152
 32  \w   -102.00 -32.00   0.50    0.80    -- -103.25  77.00 120.00  140
 33  \w    -97.00 -29.00   0.50    0.34    --  -48.81 133.00  88.00  136
 34  \w    -82.00 -56.00   0.50    0.34    --  -48.81 136.00 -93.00   52
 35  \w    -94.00 -32.00   0.50    0.80    -- -103.25  77.00 -60.00  124
 36  \w   -168.00-102.00   0.50    0.80    -- -103.25 -38.00-150.00  132
 37  \w   -161.00-135.00   0.50    0.80    -- -103.25 -67.00 -52.50   52
 38  \w   -165.00 -99.00   0.50    0.80    -- -103.25 -38.00  90.00  132
 39  \w   -118.00 -28.00   0.50    0.34    --  -48.81 -77.00  30.00  180
 40  \w   -165.00 -75.00   0.50    0.80    -- -103.25-125.00  60.00  180
 41  \w   -121.00 -84.00   0.50    0.80    -- -103.25-133.00  20.00   74
 42  \w    -97.00 -70.00   0.50    0.34    --  -48.81-133.00  20.00   54
 43  \w   -120.00 -69.00   0.50    0.34    --  -48.81-136.00-157.00  102
 44  \w   -142.00-116.00   0.50    0.80    -- -103.25-136.00-157.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0554714000
_diffrn_orient_matrix_UB_12      -0.0040349000
_diffrn_orient_matrix_UB_13      -0.0622314000
_diffrn_orient_matrix_UB_21      0.0768169000
_diffrn_orient_matrix_UB_22      0.0558565000
_diffrn_orient_matrix_UB_23      -0.0869836000
_diffrn_orient_matrix_UB_31      0.0717325000
_diffrn_orient_matrix_UB_32      -0.0956487000
_diffrn_orient_matrix_UB_33      -0.0004927000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43961
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.772
_diffrn_reflns_theta_min         3.068
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.407
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         12213
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0466P)^2^+2.9482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10191
_reflns_number_total             12213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02857d2.cif
_cod_data_source_block           Zn4
_cod_depositor_comments
'Adding full bibliography for 7720091--7720092.cif.'
_cod_database_code               7720092
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N P Zn Cl'
_diffrn_oxdiff_digest_frames
;
01924fd2ff719297cfe286b11f51fea346042069e4e
;
_diffrn_oxdiff_digest_hkl
;
01a5af4d0a0fced56650744fb8edb2a0d0fd52
;
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P2A-C53 \\sim P2-C53 \\sim P2A-C59 \\sim P2-C59
 with sigma of 0.02
 C9A-C8 \\sim C9-C8
 with sigma of 0.02
3. Rigid bond restraints
 C9, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
P2 \\sim C53 \\sim C58 \\sim C57 \\sim C59 \\sim C60 \\sim C54 \\sim C64 \\sim
C63 \\sim C55 \\sim C56 \\sim C61 \\sim C51 \\sim C62 \\sim C52 \\sim C51A
\\sim C52A \\sim P2A: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C9A \\sim C8 \\sim C9: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(P2) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C54) \\sim Ueq,
Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C62) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(C51A) \\sim Ueq, Uanis(C52A) \\sim Ueq, Uanis(P2A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9A) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H6B)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=Sof(P2A)=
 1-FVAR(1)
 Sof(P2)=Sof(H6A)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 FVAR(1)
 Sof(H8B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
 Sof(H8A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 N3(H3), N6(H6A), N6(H6B), C40(H40), C8(H8A), C8(H8B)
6.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C19(H19A,H19B), C51(H51A,H51B), C52(H52A,H52B), C51A(H51C,
 H51D), C52A(H52C,H52D)
6.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C6(H6), C36(H36), C4(H4), C37(H37), C12(H12), C44(H44), C5(H5),
 C28(H28), C14(H14), C22(H22), C46(H46), C26(H26), C30(H30), C25(H25), C32(H32),
  C58(H58), C31(H31), C24(H24), C23(H23), C57(H57), C29(H29), C60(H60),
 C54(H54), C64(H64), C63(H63), C55(H55), C56(H56), C61(H61), C62(H62)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C49(H49A,H49B,H49C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C1(H1A,
 H1B,H1C), C9(H9A,H9B,H9C), C41(H41A,H41B,H41C), C9A(H9AA,H9AB,H9AC)
;
_shelx_res_checksum              18602
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.694