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_1561025
_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         'C29 H40 Ca I2 N2 O6 Zn, C4 H8 O'
_chemical_formula_sum            'C33 H48 Ca I2 N2 O7 Zn'
_chemical_formula_weight         943.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.9060(2)
_cell_length_b                   14.3422(2)
_cell_length_c                   37.8508(5)
_cell_measurement_reflns_used    11162
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.713
_cell_measurement_theta_min      4.545
_cell_volume                     7549.06(18)
_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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            28061
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.166
_diffrn_reflns_theta_min         3.945
_exptl_absorpt_coefficient_mu    15.309
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.09491
_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    1.661
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.605
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7815
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+3.3617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6911
_reflns_number_total             7815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00238d2.cif
_cod_data_source_block           009CKW17
_cod_depositor_comments
'Adding full bibliography for 1561024--1561035.cif.'
_cod_database_code               1561025
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.580
_shelx_estimated_absorpt_t_min   0.114
_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
{C27A, C27B}
{C29A, C29B}
3. Restrained distances
 C22A-O5 \\sim C22B-O5 \\sim C25A-O5 \\sim C25B-O5
 with sigma of 0.02
 C25A-C24A \\sim C22A-C23A \\sim C25B-C24B \\sim C22B-C23B
 with sigma of 0.02
 C24A-C23A \\sim C24B-C23B
 with sigma of 0.02
 C23A-C25A \\sim C22A-C24A \\sim C23B-C25B \\sim C22B-C24B
 with sigma of 0.02
 C24A-O5 \\sim C23A-O5 \\sim C24B-O5 \\sim C23B-O5
 with sigma of 0.02
 O7A-C90A \\sim O7A-C93A \\sim O7B-C90B \\sim O7B-C93B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C25A \\sim C24A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C25B \\sim C24B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C90B \\sim C90A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C91B \\sim C91A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C92B \\sim C92A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C93B \\sim C93A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C27A) = Uanis(C27B)
Uanis(C29A) = Uanis(C29B)
5. Rigid body (RIGU) restrains
 O7A, C90A, C91A, C92A, C93A, O7B, C90B, C91B, C92B, C93B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22A, C23A, C24A, C25A, C22B, C23B, C24B, C25B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O7A, C90A, C91A, C92A, C93A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O7A, C90A, C91A, C92A, C93A}
{O7A, C90A, C91A, C92A, C93A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O7B, C90B, C91B, C92B, C93B}
7. Others
 Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(C29B)=Sof(H29C)=
 Sof(H29D)=Sof(C28B)=Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C29A)=Sof(H29A)=
 Sof(H29B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=FVAR(1)
 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(2)
 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(2)
 Sof(O7B)=Sof(C90B)=Sof(H90C)=Sof(H90D)=Sof(C91B)=Sof(H91C)=Sof(H91D)=
 Sof(C92B)=Sof(H92C)=Sof(H92D)=Sof(C93B)=Sof(H93C)=Sof(H93D)=1-FVAR(3)
 Sof(O7A)=Sof(C90A)=Sof(H90A)=Sof(H90B)=Sof(C91A)=Sof(H91A)=Sof(H91B)=
 Sof(C92A)=Sof(H92A)=Sof(H92B)=Sof(C93A)=Sof(H93A)=Sof(H93B)=FVAR(3)
8.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C26(H26A,H26B), C26(H26C,H26D), C27A(H27A,H27B),
 C29A(H29A,H29B), C28A(H28A,H28B), C27B(H27C,H27D), C29B(H29C,H29D), C28B(H28C,
 H28D), C22A(H22A,H22B), C23A(H23A,H23B), C24A(H24A,H24B), C25A(H25A,H25B),
 C22B(H22C,H22D), C23B(H23C,H23D), C24B(H24C,H24D), C25B(H25C,H25D), C90A(H90A,
 H90B), C91A(H91A,H91B), C92A(H92A,H92B), C93A(H93A,H93B), C90B(H90C,H90D),
 C91B(H91C,H91D), C92B(H92C,H92D), C93B(H93C,H93D)
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              62303
_shelx_hkl_checksum              18209
_olex2_submission_original_sample_id 009CKW17
_olex2_submission_special_instructions 'No special instructions were received'