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_7062644
_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 H15 O9 Y, H2 O'
_chemical_formula_sum            'C21 H17 O10 Y'
_chemical_formula_weight         518.26
_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
_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                92.421(2)
_cell_angle_beta                 97.081(2)
_cell_angle_gamma                101.336(2)
_cell_formula_units_Z            2
_cell_length_a                   5.29940(10)
_cell_length_b                   12.1464(2)
_cell_length_c                   17.0480(3)
_cell_measurement_reflns_used    11330
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.5600
_cell_measurement_theta_min      3.7080
_cell_volume                     1065.25(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      123.01(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 0.965
_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     33.00 104.00   0.50    0.05    --   47.64  57.00 150.00  142
  2  \w     95.00 178.00   0.50    0.05    --  107.11  45.00   0.00  166
  3  \w     94.00 178.00   0.50    0.05    --  107.11  15.00 -30.00  168
  4  \w     25.00 120.00   0.50    0.05    --   47.64  77.00-120.00  190
  5  \w    -60.00  28.00   0.50    0.05    --  -47.64  19.00 -30.00  176
  6  \w    -68.00 -11.00   0.50    0.05    --  -86.25  30.00  60.00  114
  7  \w    -78.00 -14.00   0.50    0.05    --  -86.25  45.00-180.00  128
  8  \w     41.00 102.00   0.50    0.05    --   47.64-137.00 -58.00  122
  9  \w     35.00 112.00   0.50    0.05    --  107.11-125.00-150.00  154
 10  \w     41.00 121.00   0.50    0.05    --  107.11-137.00 -58.00  160
 11  \w     35.00 109.00   0.50    0.05    --  107.11-113.00 -25.99  148
 12  \w     35.00 106.00   0.50    0.05    --  107.11 -98.00  28.62  142
 13  \w     39.00 117.00   0.50    0.05    --  107.11-133.00 118.00  156
 14  \w     35.00 106.00   0.50    0.05    --  107.11 -94.00 150.00  142
 15  \w     39.00 100.00   0.50    0.05    --   47.64-133.00 118.00  122
 16  \w     35.00 106.00   0.50    0.05    --  107.11 -94.00  30.00  142
 17  \w     35.00 106.00   0.50    0.05    --  107.11 -94.00 -90.00  142
 18  \w     35.00 106.00   0.50    0.05    --  107.11 -94.00-180.00  142
 19  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00  60.00   68
 20  \w     36.00  76.00   0.50    0.05    --  107.11 -45.00  90.00   80
 21  \w     36.00  76.00   0.50    0.05    --  107.11 -45.00 150.00   80
 22  \w    -24.00  63.00   0.50    0.05    --   47.64 -57.00 120.00  174
 23  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00  30.00   68
 24  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00 150.00   68
 25  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00   0.00   68
 26  \w    -25.00  61.00   0.50    0.05    --   47.64 -38.00-120.00  172
 27  \w     32.00  66.00   0.50    0.05    --  107.11 -30.00-150.00   68
 28  \w     36.00  76.00   0.50    0.05    --  107.11 -45.00 -90.00   80
 29  \w     87.00 178.00   0.50    0.05    --  107.11 137.00   4.00  182
 30  \w     95.00 178.00   0.50    0.05    --  107.11 125.00-150.00  166
 31  \w     90.00 178.00   0.50    0.05    --  107.11 133.00-172.00  176
 32  \w    -92.00 -17.00   0.50    0.05    --  -86.25 133.00-172.00  150
 33  \w    -91.00 -17.00   0.50    0.05    --  -47.64 133.00-172.00  148
 34  \w    -95.00 -19.00   0.50    0.05    --  -47.64 137.00   4.00  152
 35  \w    -95.00 -19.00   0.50    0.05    --  -86.25 137.00   4.00  152
 36  \w   -120.00 -73.00   0.50    0.05    --  -47.64-125.00-120.00   94
 37  \w   -120.00 -66.00   0.50    0.05    --  -47.64-137.00 -58.00  108
 38  \w   -159.00 -66.00   0.50    0.05    --  -86.25-137.00 -58.00  186
 39  \w   -120.00 -68.00   0.50    0.05    --  -47.64-133.00 118.00  104
 40  \w   -159.00 -68.00   0.50    0.05    --  -86.25-133.00 118.00  182
;
_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      -0.0843759000
_diffrn_orient_matrix_UB_12      -0.0654360000
_diffrn_orient_matrix_UB_13      -0.0814415000
_diffrn_orient_matrix_UB_21      -0.0848377000
_diffrn_orient_matrix_UB_22      -0.1090874000
_diffrn_orient_matrix_UB_23      0.0411961000
_diffrn_orient_matrix_UB_31      -0.2742333000
_diffrn_orient_matrix_UB_32      0.0250932000
_diffrn_orient_matrix_UB_33      -0.0010629000
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.160
_diffrn_reflns_theta_min         3.720
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63700
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0761P)^2^+0.1001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4115
_reflns_number_total             4365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02735j2.cif
_cod_data_source_block           jo289_a2
_cod_depositor_comments
'Adding full bibliography for 7062632--7062650.cif.'
_cod_database_code               7062644
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Y C H O'
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.354
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Free rotating group:
 O10(H10A,H10B)
1.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C21(H21), C20(H20), C10(H10), C17(H17), C13(H13), C3(H3A),
  C18(H18), C7(H7), C6(H6A), C4(H4)
1.c Idealised tetrahedral OH refined as rotating group:
 O6(H6), O3(H3), O9(H9)
;
_shelx_res_checksum              86813
_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 1.558
_oxdiff_exptl_absorpt_empirical_full_min 0.635