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_7062647
_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 Er2 O24, 10(H2 O)'
_chemical_formula_sum            'C42 H62 Er2 O34'
_chemical_formula_weight         1445.43
_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                90.5310(10)
_cell_angle_beta                 101.7250(10)
_cell_angle_gamma                105.3210(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8172(2)
_cell_length_b                   11.3109(2)
_cell_length_c                   11.44570(10)
_cell_measurement_reflns_used    22689
_cell_measurement_temperature    123.01(13)
_cell_measurement_theta_max      31.9920
_cell_measurement_theta_min      3.6490
_cell_volume                     1319.51(4)
_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(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.858
_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    -23.00  43.00   0.50    0.60    --    9.15 -99.00-120.00  132
  2  \w     -6.00  82.00   0.50    0.60    --    9.15  57.00-180.00  176
  3  \w    -66.00  21.00   0.50    0.60    --    9.15 -22.00 -45.00  174
  4  \w    -23.00  43.00   0.50    0.60    --    9.15 -99.00  60.00  132
  5  \w    -66.00 -41.00   0.50    0.60    --    9.15 -19.00  30.00   50
  6  \w    -63.00  24.00   0.50    0.60    --    9.15 -57.00 150.00  174
  7  \w     -3.00  85.00   0.50    0.60    --    9.15  22.00 119.00  176
  8  \w    -21.00  67.00   0.50    0.60    --   -8.84  22.00 119.00  176
  9  \w    -23.00  25.00   0.50    0.60    --   -8.84 -99.00 120.00   96
 10  \w    -23.00  25.00   0.50    0.60    --   -8.84 -99.00   0.00   96
 11  \w    -23.00  25.00   0.50    0.60    --   -8.84 -99.00 -60.00   96
 12  \w    -23.00  25.00   0.50    0.60    --   -8.84 -99.00-150.00   96
;
_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      0.0590269000
_diffrn_orient_matrix_UB_12      0.0351540000
_diffrn_orient_matrix_UB_13      -0.0144476000
_diffrn_orient_matrix_UB_21      -0.0274531000
_diffrn_orient_matrix_UB_22      0.0503085000
_diffrn_orient_matrix_UB_23      -0.0108955000
_diffrn_orient_matrix_UB_31      0.0245907000
_diffrn_orient_matrix_UB_32      0.0219031000
_diffrn_orient_matrix_UB_33      0.0607968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36333
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.250
_diffrn_reflns_theta_min         3.644
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73314
_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 pinkish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_description       block
_exptl_crystal_F_000             722
_exptl_crystal_preparation
'Metathesis of 1:3 Er(NO3)3 + NaL in water at 90C for 2h.'
_exptl_crystal_recrystallization_method 'From the reaction mixture.'
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         8024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+0.3824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7476
_reflns_number_total             8024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02735j2.cif
_cod_data_source_block           jo3025_90_a1
_cod_depositor_comments
'Adding full bibliography for 7062632--7062650.cif.'
_cod_database_code               7062647
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Er C H O'
_chemical_oxdiff_usercomment     'Colourless block'
_shelx_estimated_absorpt_t_max   0.686
_shelx_estimated_absorpt_t_min   0.599
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1.a Free rotating group:
 O16(H16A,H16B), O13(H13A,H13B), O15(H15A,H15B), O17(H17A,H17B), O14(H14A,H14B)
1.b Rotating group:
 O11(H11A,H11B), O10(H10A,H10B), O12(H12A,H12B)
1.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)
1.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O7(H7), O9(H9)
;
_shelx_res_checksum              83339
_olex2_exptl_crystal_mounting_method 'Thick hydrocarbon oil'
_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 2.145
_oxdiff_exptl_absorpt_empirical_full_min 0.710