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_7062636
_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         'C84 H76 O44 Pr4, 4(H2 O)'
_chemical_formula_sum            'C84 H84 O48 Pr4'
_chemical_formula_weight         2425.15
_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                93.1860(10)
_cell_angle_beta                 102.7450(10)
_cell_angle_gamma                105.5620(10)
_cell_formula_units_Z            1
_cell_length_a                   12.0467(3)
_cell_length_b                   14.1840(4)
_cell_length_c                   14.6821(4)
_cell_measurement_reflns_used    7595
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.85
_cell_measurement_theta_min      2.30
_cell_volume                     2339.57(11)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51444
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.068
_diffrn_reflns_theta_min         1.433
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4282
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.849
_refine_diff_density_min         -1.579
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0217(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         13334
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0379P)^2^+0.2115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10968
_reflns_number_total             13334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02735j2.cif
_cod_data_source_block           p1
_cod_depositor_comments
'Adding full bibliography for 7062632--7062650.cif.'
_cod_database_code               7062636
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.674
_olex2_refinement_description
;
1. Restrained distances
 O24-H24A = O24-H24B
 0.85 with sigma of 0.02
 H24A-H24B
 1.34 with sigma of 0.04
 Pr2-H15A \\sim Pr2-H15B
 with sigma of 0.02
2.a Free rotating group:
 O23(H23A,H23B), O15(H15A,H15B)
2.b Rotating group:
 O16(H16A,H16B), O7(H7A,H7B), O8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C24(H24), C14(H14), C6(H6), C11(H11), C34(H34), C39(H39), C31(H31),
 C38(H38), C4(H4), C10(H10), C3(H3), C28(H28), C13(H13), C35(H35), C17(H17A),
 C20(H20A), C32(H32), C25(H25), C18(H18A), C21(H21A), C27(H27), C42(H42),
 C41(H41)
2.d Tetrahedral OH refined with riding coordinates:
 O17(H17), O21(H21)
2.e Idealised tetrahedral OH refined as rotating group:
 O18(H18), O20(H20), O22(H22), O19(H19)
;
_shelx_res_checksum              14845
_olex2_submission_special_instructions 'No special instructions were received'