4-Hydroxybenzoato-rare earth(iii) complexes – syntheses, a structural goldmine from coordination diversity and improved corrosion inhibition behaviour
Moon, Josh; Guo, Zhifang; Beaumont, Owen A.; Hamilton, Sophie; Bousrez, Guillaume; Mottram, Eleanor; Wang, Jun; Somers, Anthony E.; Deacon, Glen B.; Junk, Peter C.; New Journal of Chemistry 47 (2023) 16843–16854; doi:10.1039/D3NJ02735J

data_7062633
_publ_section_title
;
 4-Hydroxybenzoato-rare earth(iii) complexes -- syntheses, a structural
 goldmine from coordination diversity and improved corrosion inhibition
 behaviour
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16843
_journal_page_last               16854
_journal_paper_doi               10.1039/D3NJ02735J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C21 H19 Ce O11, 3(H2 O)'
_chemical_formula_sum            'C21 H25 Ce O14'
_chemical_formula_weight         641.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-04-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                104.267(3)
_cell_angle_beta                 93.474(3)
_cell_angle_gamma                96.567(2)
_cell_formula_units_Z            2
_cell_length_a                   6.36120(10)
_cell_length_b                   10.0317(2)
_cell_length_c                   19.6952(9)
_cell_measurement_reflns_used    12088
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      77.0760
_cell_measurement_theta_min      4.5400
_cell_volume                     1204.91(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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     89.00 178.00   0.50    0.15    --  107.75 134.00 109.00  178
  2  \w     88.00 178.00   0.50    0.15    --  107.75 136.00 -71.00  180
  3  \w     95.00 178.00   0.50    0.15    --  107.75 125.00-120.00  166
  4  \w     95.00 178.00   0.50    0.15    --  107.75 125.00-180.00  166
  5  \w    -60.00  28.00   0.50    0.06    --  -47.64  19.00  30.00  176
  6  \w    -94.00 -19.00   0.50    0.06    --  -47.64 136.00 -71.00  150
  7  \w    -94.00 -19.00   0.50    0.15    --  -86.25 136.00 -71.00  150
  8  \w    -92.00 -18.00   0.50    0.06    --  -47.64 134.00 109.00  148
  9  \w     41.00 101.00   0.50    0.06    --   47.64-136.00-136.00  120
 10  \w     -1.00  81.00   0.50    0.06    --   47.64 -99.00-150.00  164
 11  \w     41.00 120.00   0.50    0.15    --  107.75-136.00-136.00  158
 12  \w     35.00 112.00   0.50    0.15    --  107.75-125.00 -60.00  154
 13  \w     35.00 112.00   0.50    0.15    --  107.75-125.00   0.00  154
 14  \w     39.00 119.00   0.50    0.15    --  107.75-134.00  42.00  160
 15  \w     35.00 112.00   0.50    0.15    --  107.75-125.00 150.00  154
 16  \w     76.00 101.00   0.50    0.15    --  107.75 -94.00  60.00   50
 17  \w     35.00 107.00   0.50    0.15    --  107.75-104.00  64.40  144
 18  \w     39.00 100.00   0.50    0.06    --   47.64-134.00  42.00  122
 19  \w     35.00 106.00   0.50    0.15    --  107.75 -94.00-180.00  142
 20  \w     71.00 102.00   0.50    0.15    --  107.75 -94.00-150.00   62
 21  \w     37.00  68.00   0.50    0.15    --  107.75 -94.00-150.00   62
 22  \w     35.00  68.00   0.50    0.15    --  107.75 -94.00-120.00   66
 23  \w     74.00 106.00   0.50    0.15    --  107.75 -94.00-120.00   64
 24  \w     35.00 131.00   0.50    0.15    --  107.75 -77.00 -30.00  192
 25  \w     35.00 124.00   0.50    0.15    --  107.75 -61.00-150.00  178
 26  \w     36.00  76.00   0.50    0.15    --  107.75 -45.00-120.00   80
 27  \w     33.00  66.00   0.50    0.15    --  107.75 -30.00-180.00   66
 28  \w     33.00  66.00   0.50    0.15    --  107.75 -30.00 -90.00   66
 29  \w     36.00  66.00   0.50    0.15    --  107.75 -30.00-120.00   60
 30  \w     36.00  76.00   0.50    0.15    --  107.75 -45.00 -60.00   80
 31  \w     33.00  66.00   0.50    0.15    --  107.75 -30.00 -30.00   66
 32  \w     33.00  66.00   0.50    0.15    --  107.75 -30.00  30.00   66
 33  \w     33.00 122.00   0.50    0.15    --  107.75 -15.00 -30.00  178
 34  \w     33.00 122.00   0.50    0.15    --  107.75 -15.00  60.00  178
 35  \w     33.00  64.00   0.50    0.15    --  107.75 -30.00  90.00   62
 36  \w     47.00  74.00   0.50    0.15    --  107.75 -45.00 120.00   54
 37  \w     38.00  64.00   0.50    0.15    --  107.75 -30.00 150.00   52
 38  \w   -120.00 -25.00   0.50    0.06    --  -47.64 -77.00  60.00  190
 39  \w   -158.00 -73.00   0.50    0.15    --  -86.25 -45.00  90.00  170
 40  \w   -158.00 -73.00   0.50    0.15    --  -86.25 -45.00  30.00  170
 41  \w   -120.00 -73.00   0.50    0.06    --  -47.64-125.00  90.00   94
 42  \w   -120.00 -68.00   0.50    0.06    --  -47.64-134.00  42.00  104
 43  \w   -159.00 -68.00   0.50    0.15    --  -86.25-134.00  42.00  182
 44  \w   -120.00 -66.00   0.50    0.06    --  -47.64-136.00-136.00  108
 45  \w   -159.00 -66.00   0.50    0.15    --  -86.25-136.00-136.00  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2080914000
_diffrn_orient_matrix_UB_12      0.0587707000
_diffrn_orient_matrix_UB_13      0.0193006000
_diffrn_orient_matrix_UB_21      0.0752594000
_diffrn_orient_matrix_UB_22      0.0290401000
_diffrn_orient_matrix_UB_23      0.0787185000
_diffrn_orient_matrix_UB_31      0.1047484000
_diffrn_orient_matrix_UB_32      0.1458353000
_diffrn_orient_matrix_UB_33      -0.0007464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4963
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.359
_diffrn_reflns_theta_min         4.584
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       prism
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         13.258
_refine_diff_density_min         -4.594
_refine_diff_density_rms         0.488
_refine_ls_extinction_coef       0.0031(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.358
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4963
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.356
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.1128
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2826
_refine_ls_wR_factor_ref         0.2855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4705
_reflns_number_total             4963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02735j2.cif
_cod_data_source_block           jo204ce_a2_tw
_cod_depositor_comments
'Adding full bibliography for 7062632--7062650.cif.'
_cod_database_code               7062633
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ce C H O'
_shelx_estimated_absorpt_t_max   0.311
_shelx_estimated_absorpt_t_min   0.150
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6287
 0.3713
2. Restrained distances
 H14B_$2-H9
 2.2 with sigma of 0.02
 H9-H14A_$2
 2.2 with sigma of 0.02
 H14B-H6
 2.2 with sigma of 0.02
 H14A-H6
 2.2 with sigma of 0.02
 H14B_$3-H11B
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16 \\sim C15: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C17 \\sim C16 \\sim C21 \\sim C15: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
4.a Free rotating group:
 O14(H14A,H14B), O13(H13A,H13B), O11(H11A,H11B)
4.b Rotating group:
 O10(H10A,H10B), O12(H12A,H12B)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C11(H11), C6(H6A), C17(H17), C21(H21), C14(H14), C3(H3A),
 C13(H13), C4(H4), C20(H20), C18(H18)
4.d Idealised tetrahedral OH refined as rotating group:
 O6(H6), O3(H3), O9(H9)
;
_shelx_res_checksum              34781
_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 2.726
_oxdiff_exptl_absorpt_empirical_full_min 0.417