Synthesis, structure, and corrosion inhibiting properties of REIII 3-thiophenecarboxylate complexes
Vithana, Vidushi P.; Guo, Zhifang; Deacon, Glen B.; Somers, Anthony E.; Junk, Peter C.; New Journal of Chemistry 46 (2022) 19104–19111; doi:10.1039/D2NJ03556A

data_7061892
_publ_section_title
;
 Synthesis, structure, and corrosion inhibiting properties of REIII
 3-thiophenecarboxylate complexes
;
_journal_issue                   40
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19104
_journal_page_last               19111
_journal_paper_doi               10.1039/D2NJ03556A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C30 H26 Er2 O16 S6, H2 O'
_chemical_formula_sum            'C30 H28 Er2 O17 S6'
_chemical_formula_weight         1187.40
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-07-05 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.458(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9187(7)
_cell_length_b                   19.1800(7)
_cell_length_c                   11.0843(7)
_cell_measurement_reflns_used    4315
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1887.8(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36686
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.706
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.866
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4315
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0205P)^2^+0.7553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3667
_reflns_number_total             4315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03556a2.cif
_cod_data_source_block           er1
_cod_depositor_comments
'Adding full bibliography for 7061882--7061892.cif.'
_cod_database_code               7061892
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.532
_shelx_estimated_absorpt_t_min   0.446
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C9-C8 \\sim C9A-C10
 with sigma of 0.02
 C14A-C15 \\sim C14-C13
 with sigma of 0.02
 C5-C4 \\sim C5A-C3
 with sigma of 0.02
3. Rigid bond restraints
 C14, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14A, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C14A \\sim C15: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C14 \\sim C13: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C5A) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(S1) = Uanis(S1A)
Uanis(S2) = Uanis(S2A)
Uanis(S3) = Uanis(S3A)
Uanis(C5A) = Uanis(C5)
Uanis(C14) = Uanis(C14A)
Uanis(C9) = Uanis(C9A)
5. Others
 Sof(S2)=Sof(H10A)=1-FVAR(1)
 Sof(S2A)=Sof(H8AA)=FVAR(1)
 Sof(S3)=Sof(H15A)=1-FVAR(2)
 Sof(S3A)=Sof(H13)=FVAR(2)
 Sof(S1)=Sof(H3A)=1-FVAR(3)
 Sof(S1A)=Sof(H4B)=FVAR(3)
 Sof(H3B)=Sof(C5A)=Sof(H5A)=1-FVAR(4)
 Sof(H4A)=Sof(C5)=Sof(H5)=FVAR(4)
 Sof(H13A)=Sof(C14)=Sof(H14)=1-FVAR(5)
 Sof(H15)=Sof(C14A)=Sof(H14A)=FVAR(5)
 Sof(H10)=Sof(C9A)=Sof(H9A)=1-FVAR(6)
 Sof(H8BB)=Sof(C9)=Sof(H9)=FVAR(6)
 Fixed Sof: O9(0.5) H9B(0.5) H9C(0.5)
6.a Free rotating group:
 O9(H9B,H9C)
6.b Rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4B), C4(H4A), C8(H8AA), C8(H8BB), C10(H10A), C10(H10), C3(H3A), C3(H3B),
 C15(H15A), C15(H15), C13(H13), C13(H13A), C5(H5), C5A(H5A), C14(H14),
 C14A(H14A), C9(H9), C9A(H9A)
;
_shelx_res_checksum              3642
_olex2_submission_special_instructions 'No special instructions were received'