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_7062642
_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 H42 Ho2 O24, 10(H2 O)'
_chemical_formula_sum            'C42 H62 Ho2 O34'
_chemical_formula_weight         1440.77
_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                90.5010(10)
_cell_angle_beta                 101.7230(10)
_cell_angle_gamma                105.3020(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8167(2)
_cell_length_b                   11.3009(2)
_cell_length_c                   11.45320(10)
_cell_measurement_reflns_used    22764
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      77.0560
_cell_measurement_theta_min      3.9530
_cell_volume                     1319.33(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (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      123.00(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 0.979
_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     35.00 121.00   0.50    0.05    --   47.82  35.00  61.00  172
  2  \w     33.00 119.00   0.50    0.05    --   47.82  57.00 150.00  172
  3  \w     25.00 118.00   0.50    0.05    --   47.82  77.00-150.00  186
  4  \w     95.00 178.00   0.50    0.05    --  107.75 125.00 -60.00  166
  5  \w     95.00 178.00   0.50    0.05    --  107.75 125.00 -90.00  166
  6  \w     95.00 178.00   0.50    0.05    --  107.75 125.00-120.00  166
  7  \w     94.00 178.00   0.50    0.05    --  107.75  15.00-120.00  168
  8  \w     35.00 131.00   0.50    0.05    --  107.75 -77.00-120.00  192
  9  \w     95.00 178.00   0.50    0.05    --  107.75  35.00  61.00  166
 10  \w     94.00 178.00   0.50    0.05    --  107.75  15.00  30.00  168
 11  \w     36.00  76.00   0.50    0.05    --  107.75 -45.00  30.00   80
 12  \w     36.00  76.00   0.50    0.05    --  107.75 -45.00   0.00   80
 13  \w     36.00  76.00   0.50    0.05    --  107.75 -45.00 -60.00   80
 14  \w     33.00  66.00   0.50    0.05    --  107.75 -30.00 -60.00   66
 15  \w     34.00  68.00   0.50    0.05    --  107.75 -35.00 -96.00   68
 16  \w     36.00  76.00   0.50    0.05    --  107.75 -45.00-120.00   80
 17  \w    -25.00  61.00   0.50    0.05    --   47.82 -35.00 -96.00  172
 18  \w    -23.00  63.00   0.50    0.05    --   47.82 -57.00  30.00  172
 19  \w     33.00  66.00   0.50    0.05    --  107.75 -30.00   0.00   66
 20  \w     33.00  66.00   0.50    0.05    --  107.75 -30.00  60.00   66
 21  \w     33.00  66.00   0.50    0.05    --  107.75 -30.00 150.00   66
 22  \w     35.00 106.00   0.50    0.05    --  107.75 -94.00  60.00  142
 23  \w     35.00 106.00   0.50    0.05    --  107.75 -94.00  30.00  142
 24  \w     35.00 112.00   0.50    0.05    --  107.75-125.00 150.00  154
 25  \w     35.00 106.00   0.50    0.05    --  107.75 -94.00   0.00  142
 26  \w     35.00 106.00   0.50    0.05    --  107.75 -94.00 -60.00  142
 27  \w     35.00 106.00   0.50    0.05    --  107.75 -94.00-150.00  142
 28  \w     35.00 112.00   0.50    0.05    --  107.75-125.00-150.00  154
 29  \w     35.00 106.00   0.50    0.05    --  107.75 -96.00-179.32  142
 30  \w     35.00 106.00   0.50    0.05    --  107.75 -94.00-120.00  142
 31  \w     35.00 106.00   0.50    0.05    --  107.75 -94.00 -30.00  142
 32  \w     35.00 106.00   0.50    0.05    --  107.75 -94.00  90.00  142
 33  \w     35.00 106.00   0.50    0.05    --  107.75 -94.00 150.00  142
 34  \w    -85.00 -13.00   0.50    0.05    --  -47.82 125.00 150.00  144
 35  \w    -86.00 -13.00   0.50    0.05    --  -86.25 125.00  90.00  146
 36  \w    -60.00  26.00   0.50    0.05    --  -47.82  35.00  61.00  172
 37  \w    -70.00 -13.00   0.50    0.05    --  -86.25  35.00  61.00  114
 38  \w   -121.00 -35.00   0.50    0.05    --  -47.82 -35.00 -96.00  172
 39  \w   -160.00 -73.00   0.50    0.05    --  -86.25 -35.00 -96.00  174
 40  \w   -119.00 -73.00   0.50    0.05    --  -47.82-125.00-150.00   92
 41  \w   -119.00 -73.00   0.50    0.05    --  -47.82-125.00-120.00   92
 42  \w   -119.00 -25.00   0.50    0.05    --  -47.82 -77.00  30.00  188
;
_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      -0.0083322000
_diffrn_orient_matrix_UB_12      0.1206527000
_diffrn_orient_matrix_UB_13      -0.0585583000
_diffrn_orient_matrix_UB_21      -0.1412745000
_diffrn_orient_matrix_UB_22      -0.0215878000
_diffrn_orient_matrix_UB_23      0.0183366000
_diffrn_orient_matrix_UB_31      0.0530269000
_diffrn_orient_matrix_UB_32      0.0709878000
_diffrn_orient_matrix_UB_33      0.1232435000
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26548
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.475
_diffrn_reflns_theta_min         3.951
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (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    1.813
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5499
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+2.0072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5470
_reflns_number_total             5499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02735j2.cif
_cod_data_source_block           jo264_b1
_cod_depositor_comments
'Adding full bibliography for 7062632--7062650.cif.'
_cod_database_code               7062642
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ho C H O'
_shelx_estimated_absorpt_t_max   0.505
_shelx_estimated_absorpt_t_min   0.404
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Restrained distances
 H13A-H14A
 2.2 with sigma of 0.02
2.a Free rotating group:
 O16(H16A,H16B), O13(H13A,H13B), O15(H15A,H15B), O17(H17A,H17B), O14(H14A,H14B)
2.b Rotating group:
 O11(H11A,H11B), O10(H10A,H10B), O12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C13(H13), C17(H17), C7(H7A), C20(H20), C10(H10), C3(H3), C4(H4),
 C11(H11), C6(H6), C14(H14), C18(H18)
2.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O7(H7), O9(H9)
;
_shelx_res_checksum              40261
_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 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.691