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_1561032
_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, C4 H6 O, C4 H8 O'
_chemical_formula_sum            'C33 H46 I2 N2 O7 Zn2'
_chemical_formula_weight         967.26
_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             2021-01-18
_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                 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(2)
_cell_measurement_theta_max      75.766
_cell_measurement_theta_min      4.206
_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_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 0.990
_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  0.0489
_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
_exptl_absorpt_coefficient_mu    14.803
_exptl_absorpt_correction_T_max  1
_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    1.705
_exptl_crystal_description       rod
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.119
_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      1.023
_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^)+(0.0787P)^2^+0.5650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1136
_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_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1561024--1561035.cif.'
_cod_database_code               1561032
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.525
_shelx_estimated_absorpt_t_min   0.119
_olex2_refinement_description
;
1. Shared sites
{C2B, C2A}
{H3AA, H3BB}
{C4B, C4A}
{C22B, C22A}
{C25A, C25B}
2. Others
 Fixed Uiso: H1A(0.058) H1B(0.058) H1C(0.058) H3(0.047) H4(0.059) H5(0.047)
 H8(0.036) H9A(0.043) H9B(0.043) H11A(0.06) H11B(0.06) H11C(0.06) H12A(0.066)
 H12B(0.066) H12C(0.066) H13A(0.047) H13B(0.047) H14(0.039) H16(0.046)
 H17(0.054) H18(0.043) H2AA(0.109) H2AB(0.109) H3AA(0.099) H3AB(0.099)
 H4AA(0.163) H4AB(0.163) H2BA(0.109) H2BB(0.109) H3BA(0.099) H3BB(0.099)
 H4BA(0.163) H4BB(0.163) H1CA(0.116) H1CB(0.116) H2CA(0.082) H2CB(0.082)
 H3CA(0.076) H3CB(0.076) H4CA(0.07) H4CB(0.07) H1DA(0.156) H1DB(0.156)
 H2DA(0.156) H2DB(0.156) H3DA(0.076) H3DB(0.076) H4DA(0.076) H4DB(0.076)
 H22A(0.053) H22B(0.053) H23A(0.077) H23B(0.077) H24A(0.065) H24B(0.065)
 H25A(0.059) H25B(0.059) H22C(0.053) H22D(0.053) H23C(0.077) H23D(0.077)
 H24C(0.065) H24D(0.065) H25C(0.059) H25D(0.059) H21A(0.082) H21B(0.082)
 H21C(0.082)
 Fixed X: H1A(0.776994) H1B(0.710357) H1C(0.782337) H3(0.809559) H4(0.808826)
 H5(0.623048) H8(0.415115) H9A(0.13188) H9B(0.242167) H11A(0.271517)
 H11B(0.244709) H11C(0.154164) H12A(-0.006586) H12B(0.113141) H12C(-0.006128)
 H13A(-0.049826) H13B(-0.043001) H14(-0.080262) H16(-0.157177) H17(-0.149171)
 H18(0.021003) H2AA(0.837959) H2AB(0.693182) H3AA(0.910987) H3AB(0.764293)
 H4AA(0.789733) H4AB(0.9144) H2BA(0.797067) H2BB(0.700458) H3BA(0.965724)
 H3BB(0.913474) H4BA(0.769957) H4BB(0.890413) H1CA(0.305503) H1CB(0.432338)
 H2CA(0.256846) H2CB(0.37018) H3CA(0.508819) H3CB(0.382304) H4CA(0.562697)
 H4CB(0.415936) H1DA(0.359636) H1DB(0.26945) H2DA(0.50494) H2DB(0.379425)
 H3DA(0.460687) H3DB(0.58889) H4DA(0.367253) H4DB(0.513511) H22A(0.243139)
 H22B(0.19261) H23A(0.230026) H23B(0.342819) H24A(0.463731) H24B(0.362884)
 H25A(0.508575) H25B(0.551911) H22C(0.26732) H22D(0.186372) H23C(0.230003)
 H23D(0.262889) H24C(0.460548) H24D(0.446965) H25C(0.479077) H25D(0.564779)
 H21A(0.240153) H21B(0.315545) H21C(0.16272)
 Fixed Y: H1A(0.58113) H1B(0.550938) H1C(0.491674) H3(0.522763) H4(0.474479)
 H5(0.425279) H8(0.382419) H9A(0.392908) H9B(0.331533) H11A(0.21887)
 H11B(0.268802) H11C(0.196844) H12A(0.279124) H12B(0.220824) H12C(0.20545)
 H13A(0.285737) H13B(0.363523) H14(0.324155) H16(0.346026) H17(0.402282)
 H18(0.485572) H2AA(0.768491) H2AB(0.737637) H3AA(0.648107) H3AB(0.616426)
 H4AA(0.575903) H4AB(0.629307) H2BA(0.7784) H2BB(0.704969) H3BA(0.706486)
 H3BB(0.647173) H4BA(0.587658) H4BB(0.604373) H1CA(0.801857) H1CB(0.827249)
 H2CA(0.715174) H2CB(0.750892) H3CA(0.65735) H3CB(0.610475) H4CA(0.65042)
 H4CB(0.636764) H1DA(0.795868) H1DB(0.7348) H2DA(0.800389) H2DB(0.777685)
 H3DA(0.660419) H3DB(0.684398) H4DA(0.607748) H4DB(0.599444) H22A(0.652345)
 H22B(0.640945) H23A(0.769479) H23B(0.765291) H24A(0.775073) H24B(0.724236)
 H25A(0.630032) H25B(0.66998) H22C(0.675925) H22D(0.628163) H23C(0.768338)
 H23D(0.707199) H24C(0.775406) H24D(0.758126) H25C(0.644388) H25D(0.651015)
 H21A(0.510224) H21B(0.583729) H21C(0.587705)
 Fixed Z: H1A(0.804214) H1B(0.671431) H1C(0.768939) H3(0.993343) H4(1.202371)
 H5(1.276082) H8(1.249726) H9A(1.22929) H9B(1.269277) H11A(1.111446)
 H11B(0.984143) H11C(1.011154) H12A(1.268812) H12B(1.279001) H12C(1.17728)
 H13A(0.997106) H13B(1.078338) H14(0.812533) H16(0.608479) H17(0.407428)
 H18(0.367067) H2AA(0.295732) H2AB(0.266179) H3AA(0.283791) H3AB(0.262367)
 H4AA(0.46842) H4AB(0.497466) H2BA(0.276593) H2BB(0.275297) H3BA(0.394527)
 H3BB(0.283448) H4BA(0.417671) H4BB(0.519069) H1CA(0.057683) H1CB(0.14318)
 H2CA(0.198566) H2CB(0.293405) H3CA(0.249424) H3CB(0.196076) H4CA(0.047588)
 H4CB(-0.006397) H1DA(0.264082) H1DB(0.185142) H2DA(0.112114) H2DB(0.020425)
 H3DA(-0.008505) H3DB(0.078087) H4DA(0.157047) H4DB(0.216262) H22A(0.82884)
 H22B(0.681331) H23A(0.675452) H23B(0.788824) H24A(0.614135) H24B(0.526022)
 H25A(0.580642) H25B(0.715483) H22C(0.828648) H22D(0.717773) H23C(0.665937)
 H23D(0.556341) H24C(0.610681) H24D(0.761018) H25C(0.563417) H25D(0.697378)
 H21A(0.347572) H21B(0.406513) H21C(0.373464)
;
_shelx_res_checksum              538
_shelx_hkl_checksum              57312
_olex2_submission_special_instructions 'No special instructions were received'