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_1561035
_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 Br2 Mg2 N2 O6, 2(C4 H8 O)'
_chemical_formula_sum            'C37 H56 Br2 Mg2 N2 O8'
_chemical_formula_weight         865.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 91.6710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7118(2)
_cell_length_b                   20.0019(2)
_cell_length_c                   18.6537(3)
_cell_measurement_reflns_used    12903
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.3540
_cell_measurement_theta_min      4.4170
_cell_volume                     3994.97(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -99.00 -47.00   1.00    2.50    --    0.00 178.00-150.00   52
  2  \w      6.00  35.00   1.00    2.50    --    0.00 -99.00 150.00   29
  3  \w    -79.00 -39.00   1.00    2.50    --    0.00-178.00   0.00   40
  4  \w     -1.00  31.00   1.00   10.00    --  -60.50  15.00 150.00   32
  5  \w     -3.00  34.00   1.00   10.00    --  -60.50  15.00   0.00   37
  6  \w     -3.00  22.00   1.00   10.00    --  -60.50  15.00  60.00   25
  7  \w    -29.00  28.00   1.00   10.00    --  -60.50  45.00  90.00   57
  8  \w      2.00  30.00   1.00   10.00    --  -60.50  15.00  30.00   28
  9  \w    103.00 128.00   1.00   10.00    --   60.50 125.00-150.00   25
 10  \w     98.00 134.00   1.00   10.00    --   60.50 125.00  60.00   36
 11  \w    107.00 152.00   1.00   10.00    --   60.50 125.00  90.00   45
 12  \w    126.00 154.00   1.00   10.00    --   60.50  77.00 -90.00   28
 13  \w     30.00 109.00   1.00   10.00    --   60.50-125.00  60.00   79
 14  \w     25.00  51.00   1.00   20.00    --  121.00 -91.00   0.00   26
 15  \w     30.00  55.00   1.00   20.00    --  121.00 -37.00-120.00   25
 16  \w     57.00 108.00   1.00   20.00    --  121.00-111.00   0.00   51
 17  \w     33.00  85.00   1.00   20.00    --  121.00-111.00 -30.00   52
 18  \w     60.00 108.00   1.00   20.00    --  121.00-111.00  60.00   48
 19  \w     87.00 175.00   1.00   20.00    --  121.00  37.00 120.00   88
 20  \w     37.00  64.00   1.00   20.00    --  121.00 -37.00 -90.00   27
 21  \w     49.00  75.00   1.00   20.00    --  121.00 -50.00  60.00   26
 22  \w     85.00 175.00   1.00   20.00    --  121.00  63.00-180.00   90
 23  \w    114.00 141.00   1.00   20.00    --  121.00 111.00  60.00   27
 24  \w     56.00  82.00   1.00   20.00    --  121.00 -91.00   0.00   26
 25  \w     35.00  64.00   1.00   20.00    --  121.00 -37.00  90.00   29
 26  \w     41.00  72.00   1.00   20.00    --  121.00 -50.00 -30.00   31
 27  \w     38.00  74.00   1.00   20.00    --  121.00 -50.00  30.00   36
 28  \w     95.00 144.00   1.00   20.00    --  121.00  52.00 170.00   49
 29  \w     41.00  66.00   1.00   20.00    --  121.00 -50.00-120.00   25
 30  \w    -17.00  25.00   1.00    2.50    --    0.00 -77.00-120.00   42
 31  \w      9.00  44.00   1.00    2.50    --    0.00 -77.00 -90.00   35
 32  \w    -20.00  14.00   1.00    2.50    --    0.00 -77.00   0.00   34
 33  \w      6.00  31.00   1.00    2.50    --    0.00 -99.00 -60.00   25
 34  \w      6.00  31.00   1.00    2.50    --    0.00 -99.00-180.00   25
 35  \w     16.00  43.00   1.00    2.50    --    0.00 -77.00   0.00   27
 36  \w      6.00  35.00   1.00   10.00    --  -60.50  15.00 -60.00   29
 37  \w    -17.00  10.00   1.00   10.00    --  -60.50  45.00 -90.00   27
 38  \w     -2.00  35.00   1.00   10.00    --  -60.50  15.00-120.00   37
 39  \w     -1.00  27.00   1.00   10.00    --  -60.50  15.00-150.00   28
 40  \w    -78.00 -23.00   1.00   10.00    --  -60.50 125.00 120.00   55
 41  \w      0.00  26.00   1.00   10.00    --  -60.50  15.00 -30.00   26
 42  \w    102.00 128.00   1.00   10.00    --   60.50 125.00-180.00   26
 43  \w    125.00 151.00   1.00   10.00    --   60.50 125.00-150.00   26
 44  \w    109.00 136.00   1.00   10.00    --   60.50 125.00 -90.00   27
 45  \w     29.00  92.00   1.00   10.00    --   60.50-125.00 -90.00   63
 46  \w    117.00 142.00   1.00   10.00    --   60.50 125.00  30.00   25
 47  \w     29.00 108.00   1.00   20.00    --  121.00-111.00-150.00   79
 48  \w     67.00 108.00   1.00   20.00    --  121.00-111.00-120.00   41
 49  \w     30.00  56.00   1.00   20.00    --  121.00 -37.00-150.00   26
 50  \w     79.00 144.00   1.00   20.00    --  121.00 178.00-120.00   65
 51  \w     33.00  90.00   1.00   20.00    --  121.00 -63.00  30.00   57
 52  \w     77.00 106.00   1.00   20.00    --  121.00-111.00-180.00   29
 53  \w     38.00  64.00   1.00   20.00    --  121.00  12.00  90.00   26
 54  \w     69.00 107.00   1.00   20.00    --  121.00-111.00 -60.00   38
 55  \w     35.00  61.00   1.00   20.00    --  121.00-111.00 -60.00   26
 56  \w     40.00  66.00   1.00   20.00    --  121.00 -50.00-180.00   26
 57  \w     56.00  93.00   1.00   20.00    --  121.00-111.00 -90.00   37
 58  \w     38.00  63.00   1.00   20.00    --  121.00 -37.00 150.00   25
 59  \w     82.00 108.00   1.00   20.00    --  121.00-111.00 -30.00   26
 60  \w     32.00  64.00   1.00   20.00    --  121.00 -37.00-180.00   32
 61  \w     67.00 155.00   1.00   20.00    --  121.00  12.00  90.00   88
 62  \w     83.00 101.00   1.00   20.00    --  121.00-111.00  30.00   18
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1387639000
_diffrn_orient_matrix_UB_12      -0.0073276000
_diffrn_orient_matrix_UB_13      -0.0177727000
_diffrn_orient_matrix_UB_21      0.0356424000
_diffrn_orient_matrix_UB_22      0.0486252000
_diffrn_orient_matrix_UB_23      0.0613524000
_diffrn_orient_matrix_UB_31      0.0121411000
_diffrn_orient_matrix_UB_32      -0.0593620000
_diffrn_orient_matrix_UB_33      0.0523925000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35779
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.645
_diffrn_reflns_theta_min         3.240
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.587
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         8364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0692P)^2^+6.8338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6656
_reflns_number_total             8364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00238d2.cif
_cod_data_source_block           012rwfk20
_cod_depositor_comments
'Adding full bibliography for 1561024--1561035.cif.'
_cod_database_code               1561035
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H100Mg2O6N4
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.552
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C13(H13a,H13b), C22(H22a,H22b), C26(H26a,H26b), C27(H27a,H27b),
 C8S(H8Sa,H8Sb), C25(H25a,H25b), C7S(H7Sa,H7Sb), C2S(H2Sa,H2Sb), C5S(H5Sa,H5Sb),
  C9S(H9Sa,H9Sb), C10S(H10a,H10b), C23(H23a,H23b), C29(H29a,H29b), C28(H28a,
 H28b), C24(H24a,H24b), C3S(H3Sa,H3Sb), C4S(H4Sa,H4Sb)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C14(H14), C6(H6), C16(H16), C7(H7), C18(H18), C17(H17)
2.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C21(H21a,H21b,H21c), C11(H11a,H11b,H11c), C1(H1a,H1b,H1c)
;
_shelx_res_checksum              61349
_shelx_hkl_checksum              44484
_ins_header
;
TITL 012RWFK20 in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.711800  20.001906  18.653742  90.0000  91.6714  90.0000
ZERR    4.00   0.000155   0.000239   0.000297   0.0000   0.0014   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O Mg
UNIT 200.00 400.00 16.00 24.00 8.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.1; aver:150.0
TEMP -123
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id 012RWFK20
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.769