Heterodinuclear catalysts Zn(ii)/M and Mg(ii)/M, where M = Na(i), Ca(ii) or Cd(ii), for phthalic anhydride/cyclohexene oxide ring opening copolymerisation
Deacy, Arron C.; Durr, Christopher B.; Kerr, Ryan W. F.; Williams, Charlotte K.; Catalysis Science & Technology 11 (2021) 3109–3118; doi:10.1039/D1CY00238D

data_1561024
_publ_section_title
;
 Heterodinuclear catalysts Zn(ii)/M and Mg(ii)/M, where M = Na(i), Ca(ii)
 or Cd(ii), for phthalic anhydride/cyclohexene oxide ring opening
 copolymerisation
;
_journal_issue                   9
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3109
_journal_page_last               3118
_journal_paper_doi               10.1039/D1CY00238D
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C25 H32 I2 N2 O5 Zn2, 2(C4 H8 O)'
_chemical_formula_sum            'C33 H48 I2 N2 O7 Zn2'
_chemical_formula_weight         969.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-22 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.802(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3649(2)
_cell_length_b                   17.3850(4)
_cell_length_c                   10.4787(2)
_cell_measurement_reflns_used    8126
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      75.7660
_cell_measurement_theta_min      4.2060
_cell_volume                     1884.04(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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      2.00  43.00   1.00    3.00    --   42.41 -99.00   0.00   41
  2  \w    -42.00  -5.00   1.00    3.00    --  -42.41  38.00 -90.00   37
  3  \w    -47.00  14.00   1.00    3.00    --  -42.41  38.00 -30.00   61
  4  \w    -50.00  30.00   1.00    3.00    --  -42.41  38.00  90.00   80
  5  \w    -99.00 -36.00   1.00    3.00    --  -42.41-178.00  60.00   63
  6  \w    150.00 176.00   1.00   13.00    --  111.00 125.00  60.00   26
  7  \w    144.00 174.00   1.00   13.00    --  111.00  15.00   0.00   30
  8  \w     84.00 109.00   1.00   13.00    --  111.00 -95.00-120.00   25
  9  \w     54.00 103.00   1.00   13.00    --  111.00 -95.00-150.00   49
 10  \w     52.00  88.00   1.00   13.00    --  111.00 -30.00 -90.00   36
 11  \w     49.00  80.00   1.00   13.00    --  111.00 -30.00-150.00   31
 12  \w     40.00  89.00   1.00   13.00    --  111.00 -45.00 -90.00   49
 13  \w     71.00 115.00   1.00   13.00    --  111.00  15.00   0.00   44
 14  \w     53.00  91.00   1.00   13.00    --  111.00 -30.00  60.00   38
 15  \w     43.00 142.00   1.00   13.00    --  111.00 -77.00  60.00   99
 16  \w     39.00  89.00   1.00   13.00    --  111.00 -30.00 120.00   50
 17  \w     40.00  82.00   1.00   13.00    --  111.00 -30.00  30.00   42
 18  \w     42.00  98.00   1.00   13.00    --  111.00 -45.00 -30.00   56
 19  \w     34.00  61.00   1.00   13.00    --  111.00 -95.00-120.00   27
 20  \w    -49.00  27.00   1.00    3.00    --  -42.41  38.00  30.00   76
 21  \w     65.00  92.00   1.00    3.00    --   42.41 178.00-180.00   27
 22  \w     86.00 128.00   1.00    3.00    --   42.41 178.00 -90.00   42
 23  \w     24.00  51.00   1.00    3.00    --   42.41  38.00 -60.00   27
 24  \w     88.00 121.00   1.00    3.00    --   42.41-178.00  90.00   33
 25  \w     78.00 110.00   1.00    3.00    --   42.41  38.00 -60.00   32
 26  \w    148.00 176.00   1.00   13.00    --  111.00  45.00-180.00   28
 27  \w     85.00 153.00   1.00   13.00    --  111.00 -15.00   0.00   68
 28  \w     42.00  92.00   1.00   13.00    --  111.00 -45.00-150.00   50
 29  \w     69.00  96.00   1.00   13.00    --  111.00 -45.00  60.00   27
 30  \w     79.00 121.00   1.00   13.00    --  111.00-125.00  90.00   42
 31  \w     33.00  60.00   1.00   13.00    --  111.00 -15.00   0.00   27
 32  \w     73.00 114.00   1.00   13.00    --  111.00-125.00  30.00   41
 33  \w     80.00 112.00   1.00   13.00    --  111.00-125.00 -30.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0515740000
_diffrn_orient_matrix_UB_12      -0.0239981000
_diffrn_orient_matrix_UB_13      0.1355334000
_diffrn_orient_matrix_UB_21      0.0877533000
_diffrn_orient_matrix_UB_22      0.0716178000
_diffrn_orient_matrix_UB_23      0.0082848000
_diffrn_orient_matrix_UB_31      -0.1085772000
_diffrn_orient_matrix_UB_32      0.0462835000
_diffrn_orient_matrix_UB_33      0.0576652000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15964
_diffrn_reflns_point_group_measured_fraction_full 0.821
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.053
_diffrn_reflns_theta_min         4.228
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.804
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       rod
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.420(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         6252
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0784P)^2^+0.5444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.554
_reflns_Friedel_fraction_full    0.629
_reflns_Friedel_fraction_max     0.588
_reflns_number_gt                5971
_reflns_number_total             6252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00238d2.cif
_cod_data_source_block           070ckw17
_cod_depositor_comments
'Adding full bibliography for 1561024--1561035.cif.'
_cod_database_code               1561024
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C21 H24 I2 N2 O4 Zn1'
_shelx_estimated_absorpt_t_max   0.525
_shelx_estimated_absorpt_t_min   0.119
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.580(7)
 0.420(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{C2A, C2B}
{C4A, C4B}
{C22A, C22B}
{C25A, C25B}
4. Restrained distances
 C2A-C3A \\sim C3A-C4A \\sim C2B-C3B \\sim C3B-C4B
 with sigma of 0.02
 O1C-C1C \\sim O1C-C4C \\sim O1D-C1D \\sim O1D-C4D
 with sigma of 0.02
 C1C-C2C \\sim C2C-C3C \\sim C3C-C4C \\sim C1D-C2D \\sim C2D-C3D \\sim C3D-C4D
 with sigma of 0.02
 O1C-C2C \\sim O1C-C3C \\sim C1C-C3C \\sim C4C-C2C \\sim O1D-C2D \\sim O1D-C3D
\\sim C1D-C3D \\sim C4D-C2D
 with sigma of 0.02
 C22A-C23A \\sim C23A-C24A \\sim C24A-C25A \\sim C22B-C23B \\sim C23B-C24B
\\sim C24B-C25B
 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(C2A) = Uanis(C2B)
Uanis(C4A) = Uanis(C4B)
Uanis(C22A) = Uanis(C22B)
Uanis(C25A) = Uanis(C25B)
Uanis(C23A) = Uanis(C23B)
Uanis(C24A) = Uanis(C24B)
Uanis(C3A) = Uanis(C3B)
Uanis(C4D) = Uanis(C3D)
Uanis(C1D) = Uanis(C2D)
6. Rigid body (RIGU) restrains
 O1C, C1C, C2C, C3C, C4C, O1D, C1D, C2D, C3D, C4D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(H1AC)=Sof(H1AD)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=
 Sof(C4B)=Sof(H4BA)=Sof(H4BB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=FVAR(1)
 Sof(O1D)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(C2D)=Sof(H2DA)=Sof(H2DB)=Sof(C3D)=
 Sof(H3DA)=Sof(H3DB)=Sof(C4D)=Sof(H4DA)=Sof(H4DB)=1-FVAR(2)
 Sof(O1C)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(C2C)=Sof(H2CA)=Sof(H2CB)=Sof(C3C)=
 Sof(H3CA)=Sof(H3CB)=Sof(C4C)=Sof(H4CA)=Sof(H4CB)=FVAR(2)
 Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=
 Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25C)=Sof(H25D)=1-FVAR(3)
 Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=
 Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=Sof(H25B)=FVAR(3)
8.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1A(H1AC,H1AD), C9(H9A,H9B), C13(H13A,H13B), C2A(H2AA,H2AB),
 C3A(H3AA,H3AB), C4A(H4AA,H4AB), C2B(H2BA,H2BB), C3B(H3BA,H3BB), C4B(H4BA,H4BB),
  C1C(H1CA,H1CB), C2C(H2CA,H2CB), C3C(H3CA,H3CB), C4C(H4CA,H4CB), C1D(H1DA,
 H1DB), C2D(H2DA,H2DB), C3D(H3DA,H3DB), C4D(H4DA,H4DB), C22A(H22A,H22B),
 C23A(H23A,H23B), C24A(H24A,H24B), C25A(H25A,H25B), C22B(H22C,H22D), C23B(H23C,
 H23D), C24B(H24C,H24D), C25B(H25C,H25D)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C14(H14), C16(H16), C17(H17), C18(H18)
8.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              9732
_shelx_hkl_checksum              57312
_ins_header
;
TITL 070ckw17 in P2(1) 
REM P2(1) (#4 in standard setting)
CELL 1.54184  10.364916  17.384986  10.478683  90.0000  93.8021  90.0000
ZERR    4.00   0.000229   0.000376   0.000242   0.0000   0.0021   0.0000
LATT -1
SYMM -x, y+1/2,-z 
SFAC C H N O Zn I
UNIT 84.00 96.00 8.00 16.00 4.00 8.00
TREF
HKLF 4
END
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.697
_oxdiff_exptl_absorpt_empirical_full_min 0.642