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_7062643
_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         'C42 H38 O22 Y2, 2(H2 O)'
_chemical_formula_sum            'C42 H42 O24 Y2'
_chemical_formula_weight         1108.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 105.8630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.37330(10)
_cell_length_b                   14.88310(10)
_cell_length_c                   15.43080(10)
_cell_measurement_reflns_used    32049
_cell_measurement_temperature    122.97(10)
_cell_measurement_theta_max      76.5400
_cell_measurement_theta_min      4.2230
_cell_volume                     2291.59(3)
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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     28.00 120.00   0.50    0.05    --   47.64  69.00 -21.00  184
  2  \w     85.00 178.00   0.50    0.05    --  107.11  77.00  60.00  186
  3  \w     91.00 178.00   0.50    0.05    --  107.11  61.00  60.00  174
  4  \w     95.00 178.00   0.50    0.05    --  107.11  45.00  60.00  166
  5  \w     95.00 178.00   0.50    0.05    --  107.11  30.00 120.00  166
  6  \w     88.00 178.00   0.50    0.05    --  107.11  69.00 -21.00  180
  7  \w     94.00 178.00   0.50    0.05    --  107.11  15.00 -90.00  168
  8  \w    124.00 178.00   0.50    0.05    --  107.11  45.00-120.00  108
  9  \w     95.00 178.00   0.50    0.05    --  107.11  45.00 -90.00  166
 10  \w     94.00 178.00   0.50    0.05    --  107.11  15.00 -30.00  168
 11  \w     94.00 178.00   0.50    0.05    --  107.11  15.00  30.00  168
 12  \w     59.00  85.00   0.50    0.05    --  107.11 -94.00 -60.00   52
 13  \w     41.00  74.00   0.50    0.05    --  107.11 -94.00   0.00   66
 14  \w     35.00 106.00   0.50    0.05    --  107.11 -94.00 -90.00  142
 15  \w     35.00 106.00   0.50    0.05    --  107.11 -94.00-150.00  142
 16  \w     34.00  95.00   0.50    0.05    --   47.64-125.00 -30.00  122
 17  \w    -24.00  67.00   0.50    0.05    --   47.64 -69.00-153.00  182
 18  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00 -30.00   68
 19  \w     36.00  70.00   0.50    0.05    --  107.11 -45.00  30.00   68
 20  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00  30.00   68
 21  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00   0.00   68
 22  \w     35.00 127.00   0.50    0.05    --  107.11 -69.00-153.00  184
 23  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00-180.00   68
 24  \w    -27.00  60.00   0.50    0.05    --   47.64 -19.00-180.00  174
 25  \w     36.00  76.00   0.50    0.05    --  107.11 -45.00-120.00   80
 26  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00 -90.00   68
 27  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00 120.00   68
 28  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00  90.00   68
 29  \w    -67.00  25.00   0.50    0.05    --  -47.64  69.00 -21.00  184
 30  \w   -106.00 -13.00   0.50    0.05    --  -86.25  69.00 -21.00  186
 31  \w    -68.00 -11.00   0.50    0.05    --  -86.25  30.00-180.00  114
 32  \w   -159.00 -67.00   0.50    0.05    --  -86.25 -69.00-153.00  184
 33  \w   -120.00 -28.00   0.50    0.05    --  -47.64 -69.00-153.00  184
 34  \w   -161.00 -73.00   0.50    0.05    --  -86.25 -30.00  90.00  176
 35  \w   -158.00 -73.00   0.50    0.05    --  -86.25 -45.00 150.00  170
 36  \w   -159.00 -70.00   0.50    0.05    --  -86.25 -61.00  90.00  178
 37  \w   -120.00 -73.00   0.50    0.05    --  -47.64-125.00  30.00   94
 38  \w   -120.00 -73.00   0.50    0.05    --  -47.64-125.00   0.00   94
 39  \w   -120.00 -73.00   0.50    0.05    --  -47.64-125.00-120.00   94
 40  \w   -120.00 -73.00   0.50    0.05    --  -47.64-125.00-180.00   94
;
_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      0.0790024000
_diffrn_orient_matrix_UB_12      -0.0034353000
_diffrn_orient_matrix_UB_13      -0.0712285000
_diffrn_orient_matrix_UB_21      -0.0814515000
_diffrn_orient_matrix_UB_22      0.0804191000
_diffrn_orient_matrix_UB_23      -0.0493259000
_diffrn_orient_matrix_UB_31      0.1047387000
_diffrn_orient_matrix_UB_32      0.0650531000
_diffrn_orient_matrix_UB_33      0.0571141000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42965
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.897
_diffrn_reflns_theta_min         4.207
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70159
_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            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0402P)^2^+1.7667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4729
_reflns_number_total             4773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02735j2.cif
_cod_data_source_block           jo289_b2
_cod_depositor_comments
'Adding full bibliography for 7062632--7062650.cif.'
_cod_database_code               7062643
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Y C H O'
_shelx_estimated_absorpt_t_max   0.616
_shelx_estimated_absorpt_t_min   0.521
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Free rotating group:
 O12(H12A,H12B)
1.b Rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
1.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C10(H10A), C20(H20), C14(H14), C3(H3), C6(H6), C7(H7), C17(H17),
 C11(H11A), C13(H13), C18(H18), C4(H4)
1.d Idealised tetrahedral OH refined as rotating group:
 O10(H10), O9(H9), O11(H11)
;
_shelx_res_checksum              34911
_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 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.806