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_1561027
_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         'C63 H72 Mg3 N6 O12'
_chemical_formula_sum            'C63 H72 Mg3 N6 O12'
_chemical_formula_weight         1178.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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            4
_cell_length_a                   26.6385(5)
_cell_length_b                   12.1506(2)
_cell_length_c                   18.5863(3)
_cell_measurement_reflns_used    11925
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.895
_cell_measurement_theta_min      3.269
_cell_volume                     6015.90(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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0605
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38599
_diffrn_reflns_point_group_measured_fraction_full 0.827
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.091
_diffrn_reflns_theta_min         3.318
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.70743
_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    1.301
_exptl_crystal_description       plate
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 2985 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         10130
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0695P)^2^+1.7386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.567
_reflns_Friedel_fraction_full    0.641
_reflns_Friedel_fraction_max     0.602
_reflns_number_gt                9223
_reflns_number_total             10130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00238d2.cif
_cod_data_source_block           045ckw17
_cod_depositor_comments
'Adding full bibliography for 1561024--1561035.cif.'
_cod_database_code               1561027
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.823
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O12-C63A \\sim O12-C63B
 with sigma of 0.02
3. Others
 Sof(C63B)=Sof(H63D)=Sof(H63E)=Sof(H63F)=1-FVAR(1)
 Sof(C63A)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C29(H29A,H29B), C31(H31A,H31B), C50(H50A,H50B),
 C52(H52A,H52B)
4.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C63A(H63A,H63B,H63C), C63B(H63D,H63E,H63F)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C15(H15),
 C24(H24), C25(H25), C26(H26), C28(H28), C32(H32), C34(H34), C35(H35), C36(H36),
  C45(H45), C46(H46), C47(H47), C49(H49), C53(H53), C55(H55), C56(H56), C57(H57)
;
_shelx_res_checksum              70492
_shelx_hkl_checksum              51509
_olex2_submission_special_instructions 'No special instructions were received'