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_7062641
_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 Ho2 O22, 2(H2 O)'
_chemical_formula_sum            'C42 H42 Ho2 O24'
_chemical_formula_weight         1260.61
_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
_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                 105.8910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3692(3)
_cell_length_b                   14.8578(5)
_cell_length_c                   15.4168(5)
_cell_measurement_reflns_used    12995
_cell_measurement_temperature    123.00(13)
_cell_measurement_theta_max      77.1480
_cell_measurement_theta_min      4.2410
_cell_volume                     2284.40(13)
_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      123.00(13)
_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 0.984
_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    -82.00  -1.00   0.50    0.05    --  -47.64 110.00 -73.00  162
  2  \w     23.00  87.00   0.50    0.05    --   47.64-110.00-168.00  128
  3  \w    -82.00 -13.00   0.50    0.20    --  -86.25 110.00 -73.00  138
  4  \w   -159.00 -82.00   0.50    0.20    --  -86.25-110.00-168.00  154
  5  \w    103.00 178.00   0.50    0.20    --  107.75 110.00 -73.00  150
  6  \w     35.00 108.00   0.50    0.20    --  107.75-110.00-168.00  146
  7  \w   -120.00 -73.00   0.50    0.05    --  -47.64-125.00-120.00   94
  8  \w   -120.00 -73.00   0.50    0.05    --  -47.64-125.00  90.00   94
  9  \w   -120.00 -73.00   0.50    0.05    --  -47.64-125.00 -30.00   94
 10  \w   -120.00 -73.00   0.50    0.05    --  -47.64-125.00   0.00   94
 11  \w    -25.00  61.00   0.50    0.05    --   47.64 -38.00-120.00  172
 12  \w     36.00  76.00   0.50    0.20    --  107.75 -45.00   0.00   80
 13  \w     35.00 127.00   0.50    0.20    --  107.75 -77.00-150.00  184
 14  \w     40.00  66.00   0.50    0.20    --  107.75 -30.00 -60.00   52
 15  \w     35.00 106.00   0.50    0.20    --  107.75 -94.00 -30.00  142
 16  \w     36.00  62.00   0.50    0.20    --  107.75 -30.00  60.00   52
 17  \w     39.00  65.00   0.50    0.20    --  107.75 -30.00-150.00   52
 18  \w     38.00  68.00   0.50    0.20    --  107.75 -94.00-150.00   60
 19  \w     75.00 104.00   0.50    0.20    --  107.75 -94.00-150.00   58
 20  \w     33.00  59.00   0.50    0.20    --  107.75 -30.00  30.00   52
 21  \w     38.00  63.00   0.50    0.20    --  107.75 -45.00  60.00   50
 22  \w     36.00 115.00   0.50    0.20    --  107.75 -77.00 -30.00  158
 23  \w     34.00  66.00   0.50    0.20    --  107.75 -30.00-120.00   64
 24  \w     44.00  76.00   0.50    0.20    --  107.75 -45.00  90.00   64
 25  \w     35.00  63.00   0.50    0.20    --  107.75 -30.00  90.00   56
 26  \w     36.00  71.00   0.50    0.20    --  107.75 -45.00-150.00   70
 27  \w     46.00 106.00   0.50    0.20    --  107.75 -94.00 120.00  120
 28  \w     38.00  63.00   0.50    0.20    --  107.75 -30.00-180.00   50
 29  \w     36.00  62.00   0.50    0.20    --  107.75-125.00-180.00   52
 30  \w     64.00  90.00   0.50    0.20    --  107.75-125.00-180.00   52
 31  \w     36.00  68.00   0.50    0.20    --  107.75 -45.00  30.00   64
 32  \w     42.00  84.00   0.50    0.20    --  107.75 -94.00-120.00   84
 33  \w     33.00  65.00   0.50    0.20    --  107.75 -30.00 -30.00   64
;
_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      -0.0437087000
_diffrn_orient_matrix_UB_12      0.0518918000
_diffrn_orient_matrix_UB_13      -0.0898607000
_diffrn_orient_matrix_UB_21      -0.0119254000
_diffrn_orient_matrix_UB_22      0.0869542000
_diffrn_orient_matrix_UB_23      0.0517365000
_diffrn_orient_matrix_UB_31      0.1475504000
_diffrn_orient_matrix_UB_32      0.0223840000
_diffrn_orient_matrix_UB_33      0.0072684000
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24375
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.406
_diffrn_reflns_theta_min         4.212
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66077
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+2.0426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4485
_reflns_number_total             4773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02735j2.cif
_cod_data_source_block           jo281_a1
_cod_depositor_comments
'Adding full bibliography for 7062632--7062650.cif.'
_cod_database_code               7062641
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ho C H O'
_shelx_estimated_absorpt_t_max   0.272
_shelx_estimated_absorpt_t_min   0.101
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
1.b Aromatic/amide H refined with riding coordinates:
 C10(H10A), C14(H14), C13(H13), C21(H21), C7(H7), C17(H17), C18(H18), C11(H11),
  C3(H3), C6(H6), C20(H20), C4(H4)
1.c Tetrahedral OH refined with riding coordinates:
 O9(H9)
1.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_shelx_res_checksum              66684
_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 2.760
_oxdiff_exptl_absorpt_empirical_full_min 0.729