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_1567778
_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         'C29 H29 Cl2 N2 P Zn'
_chemical_formula_sum            'C29 H29 Cl2 N2 P Zn'
_chemical_formula_weight         572.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 101.4970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.59830(10)
_cell_length_b                   11.35930(10)
_cell_length_c                   16.43550(10)
_cell_measurement_reflns_used    15454
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.1930
_cell_measurement_theta_min      2.7720
_cell_volume                     2670.76(4)
_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      170.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_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    -38.00  -5.00   0.50    0.05    --  -47.20  91.00 -55.00   66
  2  \w    -22.00  73.00   0.50    0.05    --   47.20 -91.00-169.00  190
  3  \w   -146.00-121.00   0.50    0.05    --  -99.00 -91.00-169.00   50
  4  \w   -116.00 -79.00   0.50    0.05    --  -99.00 -91.00-169.00   74
  5  \w   -104.00 -27.00   0.50    0.05    --  -99.00  91.00 -55.00  154
  6  \w     31.00 103.00   0.50    0.05    --  103.25 -91.00-169.00  144
  7  \w   -120.00 -77.00   0.50    0.05    --  -47.20-125.00 150.00   86
  8  \w   -118.00 -76.00   0.50    0.05    --  -47.20-125.00 -90.00   84
  9  \w     -2.00  23.00   0.50    0.05    --  -47.20  38.00 150.00   50
 10  \w    -33.00  -8.00   0.50    0.05    --  -47.20  38.00 150.00   50
 11  \w    -23.00  28.00   0.50    0.05    --  -47.20  19.00  60.00  102
 12  \w    -67.00 -29.00   0.50    0.05    --  -99.00  61.00 150.00   76
 13  \w    -65.00 -28.00   0.50    0.05    --  -99.00  61.00 120.00   74
 14  \w   -111.00 -86.00   0.50    0.05    --  -99.00 -30.00 150.00   50
 15  \w    -77.00 -26.00   0.50    0.05    --  -99.00  77.00 -60.00  102
 16  \w    -66.00 -40.00   0.50    0.05    --  -99.00  61.00 -90.00   52
 17  \w    -96.00 -39.00   0.50    0.05    --  -99.00  77.00 150.00  114
 18  \w   -166.00-122.00   0.50    0.05    --  -99.00 -30.00 150.00   88
 19  \w     32.00  60.00   0.50    0.05    --  103.25 -61.00-150.00   56
 20  \w     78.00 104.00   0.50    0.05    --  103.25 -77.00  60.00   52
 21  \w     31.00  64.00   0.50    0.05    --  103.25 -77.00  60.00   66
 22  \w     95.00 168.00   0.50    0.05    --  103.25  45.00 -90.00  146
 23  \w     39.00  72.00   0.50    0.05    --  103.25 -61.00-180.00   66
 24  \w    126.00 166.00   0.50    0.05    --  103.25  45.00-120.00   80
 25  \w     31.00  56.00   0.50    0.05    --  103.25 -61.00   0.00   50
 26  \w    103.00 128.00   0.50    0.05    --  103.25  91.00 -55.00   50
;
_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      0.0293601000
_diffrn_orient_matrix_UB_12      0.0483266000
_diffrn_orient_matrix_UB_13      -0.0785706000
_diffrn_orient_matrix_UB_21      -0.0550131000
_diffrn_orient_matrix_UB_22      0.1140148000
_diffrn_orient_matrix_UB_23      0.0070596000
_diffrn_orient_matrix_UB_31      0.0877718000
_diffrn_orient_matrix_UB_32      0.0554292000
_diffrn_orient_matrix_UB_33      0.0540573000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19525
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.559
_diffrn_reflns_theta_min         3.701
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.837
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42568
_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    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.067
_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     316
_refine_ls_number_reflns         5281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0342
_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^)+(0.0575P)^2^+1.3498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4958
_reflns_number_total             5281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy00979j2.cif
_cod_data_source_block           Zn5
_cod_depositor_comments
'Adding full bibliography for 1567777--1567778.cif.'
_cod_database_code               1567778
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N P Cl Zn'
_reflns_odcompleteness_completeness 99.96
_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
2.a Ternary CH refined with riding coordinates:
 N2(H2), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C10(H10A,H10B), C7(H7A,H7B), C11(H11A,H11B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C25(H25), C3(H3), C23(H23), C2(H2A), C29(H29), C17(H17), C15(H15),
 C21(H21), C14(H14), C22(H22), C26(H26), C16(H16), C19(H19), C20(H20), C28(H28),
  C27(H27)
;
_shelx_res_checksum              7572
_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 1.603
_oxdiff_exptl_absorpt_empirical_full_min 0.635