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_1561034
_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         'C33 H48 I N2 Na O7 Zn'
_chemical_formula_sum            'C33 H48 I N2 Na O7 Zn'
_chemical_formula_weight         799.99
_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
_audit_creation_date             2021-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-19 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.002(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0024(5)
_cell_length_b                   10.5844(2)
_cell_length_c                   15.9024(3)
_cell_measurement_reflns_used    8537
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.416
_cell_measurement_theta_min      4.169
_cell_volume                     3534.53(13)
_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_temperature      150.15
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22541
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.055
_diffrn_reflns_theta_min         4.211
_exptl_absorpt_coefficient_mu    8.330
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.47053
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7305
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0570P)^2^+1.9705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6167
_reflns_number_total             7305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00238d2.cif
_cod_data_source_block           063ckw17
_cod_depositor_comments
'Adding full bibliography for 1561024--1561035.cif.'
_cod_database_code               1561034
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.368
_shelx_estimated_absorpt_t_min   0.230
_olex2_refinement_description
;
1. 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
2. Shared sites
{C24A, C24B}
{C30A, C30B}
{C32A, C32B}
3. Restrained distances
 C22A-C23A \\sim C22B-C23B \\sim C23A-C24A \\sim C23B-C24B
 with sigma of 0.02
 C30A-C31A \\sim C30B-C31B \\sim C32A-C31A \\sim C32B-C31B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C24A) = Uanis(C24B)
Uanis(C30A) = Uanis(C30B)
Uanis(C32A) = Uanis(C32B)
Uanis(C23B) = Uanis(C23A)
Uanis(C22A) = Uanis(C22B)
Uanis(C31A) = Uanis(C31B)
5. Rigid body (RIGU) restrains
 C22A, C23A, C24A, C22B, C23B, C24B, C30A, C31A, C32A, C30B, C31B, C32B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(H25C)=Sof(H25D)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=
 Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C23A)=Sof(H23A)=
 Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=FVAR(1)
 Sof(H33C)=Sof(H33D)=Sof(C30B)=Sof(H30C)=Sof(H30D)=Sof(C31B)=Sof(H31C)=
 Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=1-FVAR(2)
 Sof(H33A)=Sof(H33B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(C31A)=Sof(H31A)=
 Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C25(H25A,H25B), C25(H25C,H25D), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C33(H33A,H33B), C33(H33C,H33D),
  C22A(H22A,H22B), C23A(H23A,H23B), C24A(H24A,H24B), C22B(H22C,H22D), C23B(H23C,
 H23D), C24B(H24C,H24D), C30A(H30A,H30B), C31A(H31A,H31B), C32A(H32A,H32B),
 C30B(H30C,H30D), C31B(H31C,H31D), C32B(H32C,H32D)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C14(H14), C16(H16), C17(H17), C18(H18)
7.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              56205
_shelx_hkl_checksum              53397
_olex2_submission_special_instructions 'No special instructions were received'