Zinc 8-aminotrihydroquinolines appended with pendant N-diphenylphosphinoethyl arms as exceptionally active catalysts for the ROP of ε-CL
Cao, Furong; Wang, Yun; Wang, Xing; Zhang, Wenjuan; Solan, Gregory A.; Wang, Rui; Ma, Yanping; Hao, Xiang; Sun, Wen-Hua; Catalysis Science & Technology 12 (2022) 6687–6703; doi:10.1039/D2CY00979J

data_1567777
_publ_section_title
;
 Zinc 8-aminotrihydroquinolines appended with pendant
 N-diphenylphosphinoethyl arms as exceptionally active catalysts for the
 ROP of \e-CL
;
_journal_issue                   22
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              6687
_journal_page_last               6703
_journal_paper_doi               10.1039/D2CY00979J
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C24 H27 Cl2 N2 P Zn'
_chemical_formula_sum            'C24 H27 Cl2 N2 P Zn'
_chemical_formula_weight         510.71
_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             2021-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-06 deposited with the CCDC.	2022-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                109.146(3)
_cell_angle_beta                 112.870(4)
_cell_angle_gamma                91.797(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6677(4)
_cell_length_b                   11.6496(3)
_cell_length_c                   12.2679(5)
_cell_measurement_reflns_used    7495
_cell_measurement_temperature    169.99(11)
_cell_measurement_theta_max      70.0090
_cell_measurement_theta_min      4.1980
_cell_volume                     1182.45(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_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   -124.00 -75.00   0.50    0.05    --  -26.54-125.00 132.00   98
  2  \w   -135.00 -60.00   0.50    0.05    --  -26.54-146.00 -33.00  150
  3  \w     32.00 108.00   0.50    0.05    --   26.54-146.00 -33.00  152
  4  \w   -168.00 -59.00   0.50    0.05    --  -70.34-146.00 -33.00  218
  5  \w   -168.00 -74.00   0.50    0.05    --  -70.34-125.00 132.00  188
  6  \w   -112.00 -13.00   0.50    0.05    --  -70.34 125.00-149.00  198
  7  \w     67.00 152.00   0.50    0.05    --   70.34 146.00  16.00  170
  8  \w     80.00 153.00   0.50    0.05    --   70.34 125.00-149.00  146
  9  \w     19.00 112.00   0.50    0.05    --   70.34-125.00 132.00  186
 10  \w   -168.00 -74.00   0.50    0.05    --  -99.00-125.00 132.00  188
 11  \w   -126.00 -24.00   0.50    0.05    --  -99.00 146.00  16.00  204
 12  \w   -168.00 -59.00   0.50    0.05    --  -99.00-146.00 -33.00  218
 13  \w     31.00 127.00   0.50    0.05    --  114.14-146.00 -33.00  192
 14  \w     19.00 112.00   0.50    0.05    --  114.14-125.00 132.00  186
 15  \w     66.00 169.00   0.50    0.05    --  114.14 146.00  16.00  206
 16  \w    -22.00  54.00   0.50    0.05    --  -26.54  19.00  30.00  152
 17  \w    -19.00   7.00   0.50    0.05    --  -26.54  19.00-180.00   52
 18  \w     -1.00  46.00   0.50    0.05    --  -26.54  19.00 -60.00   94
 19  \w   -131.00 -99.00   0.50    0.05    --  -26.54 -99.00  30.00   64
 20  \w    -10.00  40.00   0.50    0.05    --  -26.54  19.00 -90.00  100
 21  \w     19.00  47.00   0.50    0.05    --  -26.54  19.00-180.00   56
 22  \w    -21.00  12.00   0.50    0.05    --  -70.34  15.00 -30.00   66
 23  \w    -21.00  12.00   0.50    0.05    --  -70.34  15.00  60.00   66
 24  \w    -20.00  12.00   0.50    0.05    --  -70.34  15.00  30.00   64
 25  \w   -163.00 -92.00   0.50    0.05    --  -70.34-111.00 -90.00  142
 26  \w    -31.00  11.00   0.50    0.05    --  -70.34  30.00-180.00   84
 27  \w    -19.00  12.00   0.50    0.05    --  -70.34  15.00   0.00   62
 28  \w    -21.00   5.00   0.50    0.05    --  -70.34  15.00  90.00   52
 29  \w    -43.00 -17.00   0.50    0.05    --  -70.34  45.00-180.00   52
 30  \w    -45.00 -19.00   0.50    0.05    --  -70.34  45.00-150.00   52
 31  \w    -43.00  -6.00   0.50    0.05    --  -70.34  45.00  30.00   74
 32  \w     88.00 153.00   0.50    0.05    --   70.34 111.00  60.00  130
 33  \w    105.00 153.00   0.50    0.05    --   70.34 111.00 -30.00   96
 34  \w    -12.00  28.00   0.50    0.05    --   70.34 -15.00-180.00   80
 35  \w     24.00 103.00   0.50    0.05    --   70.34-111.00 -90.00  158
 36  \w    -33.00   8.00   0.50    0.05    --   70.34 -15.00 150.00   82
 37  \w    -42.00 -17.00   0.50    0.05    --  -99.00  43.00-120.00   50
 38  \w    -43.00 -18.00   0.50    0.05    --  -99.00  43.00 -90.00   50
 39  \w    -45.00 -20.00   0.50    0.05    --  -99.00  43.00-180.00   50
 40  \w   -168.00 -83.00   0.50    0.05    --  -99.00 -89.00  30.00  170
 41  \w    -73.00 -47.00   0.50    0.05    --  -99.00 125.00-149.00   52
 42  \w    -64.00 -30.00   0.50    0.05    --  -99.00  65.00   0.00   68
 43  \w    -44.00 -16.00   0.50    0.05    --  -99.00  43.00 150.00   56
 44  \w     76.00 102.00   0.50    0.05    --  114.14-104.00 -90.00   52
 45  \w     40.00  80.00   0.50    0.05    --  114.14 -65.00-180.00   80
 46  \w     11.00  37.00   0.50    0.05    --  114.14 -65.00-180.00   52
 47  \w     73.00 107.00   0.50    0.05    --  114.14-104.00-180.00   68
 48  \w     15.00  40.00   0.50    0.05    --  114.14 -32.00-150.00   50
 49  \w     93.00 131.00   0.50    0.05    --  114.14 104.00-180.00   76
 50  \w    134.00 162.00   0.50    0.05    --  114.14 104.00 150.00   56
 51  \w     26.00  65.00   0.50    0.05    --  114.14 -54.00  30.00   78
 52  \w     96.00 126.00   0.50    0.05    --  114.14 104.00 150.00   60
 53  \w     82.00 107.00   0.50    0.05    --  114.14-104.00 -30.00   50
 54  \w     12.00  44.00   0.50    0.05    --  114.14-104.00 -30.00   64
 55  \w     15.00 100.00   0.50    0.05    --  114.14 -77.00 120.00  170
 56  \w     16.00  41.00   0.50    0.05    --  114.14 -32.00-180.00   50
 57  \w     73.00 168.00   0.50    0.05    --  114.14 138.00  90.00  190
 58  \w     57.00 109.00   0.50    0.05    --  114.14 -77.00 -30.00  104
 59  \w     14.00  44.00   0.50    0.05    --  114.14 -77.00 -30.00   60
 60  \w     15.00  65.00   0.50    0.05    --  114.14 -54.00-120.00  100
 61  \w     31.00  62.00   0.50    0.05    --  114.14 -65.00 150.00   62
 62  \w     23.00  51.00   0.50    0.05    --  114.14 -43.00 -90.00   56
 63  \w    131.00 156.00   0.50    0.05    --  114.14 138.00  60.00   50
 64  \w     66.00  91.00   0.50    0.05    --  114.14-104.00 150.00   50
 65  \w     13.00  53.00   0.50    0.05    --  114.14-104.00 150.00   80
 66  \w     62.00 100.00   0.50    0.05    --  114.14-104.00  30.00   76
 67  \w     24.00  65.00   0.50    0.05    --  114.14 -54.00-180.00   82
 68  \w    140.00 165.00   0.50    0.05    --  114.14  21.00 150.00   50
 69  \w     20.00  46.00   0.50    0.05    --  114.14-104.00-180.00   52
 70  \w      2.00 135.00   0.50    0.05    --  114.14  21.00 150.00  266
 71  \w     38.00  64.00   0.50    0.05    --  114.14 -54.00   0.00   52
 72  \w     21.00  54.00   0.50    0.05    --  114.14-104.00  30.00   66
 73  \w     13.00  39.00   0.50    0.05    --  114.14-104.00 -90.00   52
 74  \w     15.00  40.00   0.50    0.05    --  114.14 -32.00-120.00   50
 75  \w    129.00 155.00   0.50    0.05    --  114.14 125.00-149.00   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      0.0577251000
_diffrn_orient_matrix_UB_12      0.1403911000
_diffrn_orient_matrix_UB_13      0.0525874000
_diffrn_orient_matrix_UB_21      0.1011342000
_diffrn_orient_matrix_UB_22      -0.0212030000
_diffrn_orient_matrix_UB_23      -0.0731261000
_diffrn_orient_matrix_UB_31      -0.1318356000
_diffrn_orient_matrix_UB_32      0.0105460000
_diffrn_orient_matrix_UB_33      -0.1157448000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12599
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.025
_diffrn_reflns_theta_min         4.086
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0672P)^2^+0.6132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4240
_reflns_number_total             4411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy00979j2.cif
_cod_data_source_block           Zn2
_cod_depositor_comments
'Adding full bibliography for 1567777--1567778.cif.'
_cod_original_cell_volume        1182.45(8)
_cod_database_code               1567777
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Zn P'
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C17(H17), C3(H3), C14(H14), C2(H2A), C23(H23), C21(H21), C16(H16),
 C15(H15), C20(H20), C22(H22), C19(H19)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_shelx_res_checksum              41570
_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 1.574
_oxdiff_exptl_absorpt_empirical_full_min 0.677