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_7061884
_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 Ce O9 S3'
_chemical_formula_sum            'C15 H15 Ce O9 S3'
_chemical_formula_weight         575.57
_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             2022-01-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-05 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.769(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0999(6)
_cell_length_b                   12.1722(4)
_cell_length_c                   10.8103(3)
_cell_measurement_reflns_used    4237
_cell_measurement_temperature    190.0
_cell_measurement_theta_max      28.7930
_cell_measurement_theta_min      3.9690
_cell_volume                     1951.93(12)
_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_temperature      190.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0217
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.862
_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      2.00  46.00   1.00    8.00    --   15.71  19.00-180.00   44
  2  \w     -3.00  38.00   1.00    8.00    --   15.71  77.00 -30.00   41
  3  \w    -10.00  15.00   1.00    8.00    --   15.71  77.00 -90.00   25
  4  \w    -43.00  39.00   1.00    8.00    --  -16.96  77.00   0.00   82
  5  \w    -84.00   0.00   1.00    8.00    --  -16.96 -57.00-150.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, EosS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0416259000
_diffrn_orient_matrix_UB_12      0.0270193000
_diffrn_orient_matrix_UB_13      0.0215130000
_diffrn_orient_matrix_UB_21      0.0217402000
_diffrn_orient_matrix_UB_22      -0.0516657000
_diffrn_orient_matrix_UB_23      0.0115187000
_diffrn_orient_matrix_UB_31      0.0088772000
_diffrn_orient_matrix_UB_32      -0.0002438000
_diffrn_orient_matrix_UB_33      -0.0621577000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11030
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.227
_diffrn_reflns_theta_min         3.216
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78734
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4592
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0322P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3740
_reflns_number_total             4592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03556a2.cif
_cod_data_source_block           2200vvice
_cod_depositor_comments
'Adding full bibliography for 7061882--7061892.cif.'
_cod_database_code               7061884
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H12 S3 O6 Ce'
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.412
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 C14A-C15 \\sim C14-C13
 with sigma of 0.02
 S2A-C13 \\sim S2-C15
 with sigma of 0.02
 Ce1-H8A \\sim Ce1-H8B
 with sigma of 0.02
 Ce1-H7A \\sim Ce1-H7B
 with sigma of 0.02
 C4A-C3 \\sim C4-C5
 with sigma of 0.02
 S1-C3 \\sim S4A-C5
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C14A)
Uanis(S2A) = Uanis(S2)
Uanis(C4A) = Uanis(C4)
Uanis(S1) = Uanis(S4A)
3. Others
 Sof(S2A)=Sof(H15A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=1-FVAR(1)
 Sof(S2)=Sof(H15)=Sof(H13)=Sof(C14)=Sof(H14)=FVAR(1)
 Sof(S4A)=Sof(H5B)=Sof(H3B)=Sof(C4A)=Sof(H4A)=1-FVAR(2)
 Sof(S1)=Sof(H5A)=Sof(H3A)=Sof(C4)=Sof(H4)=FVAR(2)
4.a Free rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
4.b Rotating group:
 O9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C8(H8), C5(H5B), C5(H5A), C9(H9), C15(H15), C15(H15A), C13(H13A),
 C13(H13), C3(H3A), C3(H3B), C14(H14), C14A(H14A), C4(H4), C4A(H4A)
;
_shelx_res_checksum              25777
_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 1.186
_oxdiff_exptl_absorpt_empirical_full_min 0.812