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_7061885
_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         'C15 H15 Nd O9 S3'
_chemical_formula_sum            'C15 H15 Nd O9 S3'
_chemical_formula_weight         579.69
_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             2022-03-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-05 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.78(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.020(3)
_cell_length_b                   12.070(2)
_cell_length_c                   10.720(2)
_cell_measurement_reflns_used    3344
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1909.1(6)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3344
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         1.380
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    3.095
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.807
_refine_diff_density_min         -2.110
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3344
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+8.1129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3203
_reflns_number_total             3344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03556a2.cif
_cod_data_source_block           vv1nd_tw
_cod_depositor_comments
'Adding full bibliography for 7061882--7061892.cif.'
_cod_original_cell_volume        1909.1(7)
_cod_database_code               7061885
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.91957
 0.08043
2. Restrained distances
 S3-C15 \\sim S3A-C13
 with sigma of 0.02
 C4-C3 \\sim C4A-C5
 with sigma of 0.02
 S1A-C3 \\sim S1-C5
 with sigma of 0.02
 C14A-C15 \\sim C14-C13
 with sigma of 0.02
 C9A-C10 \\sim C9-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C9 \\sim C8: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C9A \\sim C10: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(S3) = Uanis(S3A)
Uanis(C4A) = Uanis(C4)
Uanis(S1A) = Uanis(S1)
Uanis(S3A) = Uanis(S3)
Uanis(C14A) = Uanis(C14)
Uanis(C9) = Uanis(C9A)
4. Others
 Sof(S1A)=Sof(H3B)=Sof(H5B)=Sof(C4A)=Sof(H4A)=1-FVAR(1)
 Sof(S1)=Sof(H3A)=Sof(H5A)=Sof(C4)=Sof(H4)=FVAR(1)
 Sof(S3)=Sof(H15A)=Sof(H13A)=Sof(C14)=Sof(H14)=1-FVAR(2)
 Sof(S3A)=Sof(H15)=Sof(H13)=Sof(C14A)=Sof(H14A)=FVAR(2)
 Sof(S2A)=Sof(H8A)=Sof(H10)=Sof(C9A)=Sof(H9AA)=1-FVAR(3)
 Sof(S2)=Sof(H8B)=Sof(H10A)=Sof(C9)=Sof(H9)=FVAR(3)
5.a Free rotating group:
 O8(H8C,H8D), O7(H7A,H7B)
5.b Rotating group:
 O9(H9A,H9B)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C15(H15A), C3(H3A), C3(H3B), C8(H8A), C8(H8B), C13(H13), C13(H13A),
 C10(H10), C10(H10A), C5(H5A), C5(H5B), C9(H9), C14A(H14A), C4(H4), C4A(H4A),
 C14(H14), C9A(H9AA)
;
_shelx_res_checksum              16532
_olex2_submission_special_instructions 'No special instructions were received'