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_7062650
_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         'C62 H46 Dy2 N4 O18, 4(H2 O), 2(C10 H8 N2)'
_chemical_formula_sum            'C82 H70 Dy2 N8 O22'
_chemical_formula_weight         1844.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 113.1660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3138(5)
_cell_length_b                   13.1899(4)
_cell_length_c                   19.1424(6)
_cell_measurement_reflns_used    8103
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.16
_cell_measurement_theta_min      2.56
_cell_volume                     4019.0(2)
_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(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0723
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48794
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.929
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       needle
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.984
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         9227
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0416P)^2^+3.0617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6735
_reflns_number_total             9227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02735j2.cif
_cod_data_source_block           p21n_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7062632--7062650.cif.'
_cod_database_code               7062650
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.552
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N38) = Uanis(C39)
Uanis(C37) = Uanis(N38)
2.a Free rotating group:
 O11(H11A,H11B), O10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7A), C6(H6), C3(H3), C20(H20), C14(H14), C31(H31), C38(H38), C21(H21),
 C22(H22), C30(H30), C29(H29), C28(H28), C10(H10), C11(H11), C13(H13), C23(H23),
  C17(H17), C35(H35), C18(H18), C4(H4), C24(H24), C25(H25), C39(H39), C32(H32),
 C34(H34), C33(H33), C41(H41), C40(H40)
2.c Tetrahedral OH refined with riding coordinates:
 O7(H7)
2.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O8(H8)
;
_shelx_res_checksum              93946
_olex2_submission_special_instructions 'No special instructions were received'