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_7061883
_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 O9 Pr S3'
_chemical_formula_sum            'C15 H15 O9 Pr S3'
_chemical_formula_weight         576.36
_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             2022-02-15
_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                 100.81(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.059(3)
_cell_length_b                   12.157(2)
_cell_length_c                   10.775(2)
_cell_measurement_reflns_used    5508
_cell_measurement_temperature    190
_cell_measurement_theta_max      71.4640
_cell_measurement_theta_min      4.6800
_cell_volume                     1937.6(6)
_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      190
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, EosS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.870
_diffrn_reflns_theta_min         4.708
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21022
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.309
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3776
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0796P)^2^+1.2035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3377
_reflns_number_total             3776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03556a2.cif
_cod_data_source_block           vvipr_tw
_cod_depositor_comments
'Adding full bibliography for 7061882--7061892.cif.'
_cod_original_cell_volume        1937.5(7)
_cod_database_code               7061883
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.876(3)
 0.124(3)
2. 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
3. Restrained distances
 C14A-C15 \\sim C14-C13
 with sigma of 0.02
 Pr1-H8A \\sim Pr1-H8B
 with sigma of 0.02
 Pr1-H9A \\sim Pr1-H9B
 with sigma of 0.02
4. Rigid bond restraints
 S1, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
S1 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C14A) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(S3) = Uanis(S3A)
Uanis(C14) = Uanis(C14A)
6. Others
 Sof(S3A)=Sof(H13A)=Sof(H15A)=Sof(C14A)=Sof(H14A)=1-FVAR(1)
 Sof(S3)=Sof(H13)=Sof(H15)=Sof(C14)=Sof(H14)=FVAR(1)
7.a Free rotating group:
 O9(H9A,H9B), O8(H8A,H8B)
7.b Rotating group:
 O7(H7A,H7B)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C13(H13A), C13(H13), C8(H8), C15(H15), C15(H15A), C10(H10),
 C9(H9), C3(H3), C14(H14), C14A(H14A)
;
_shelx_res_checksum              60000
_olex2_submission_special_instructions 'No special instructions were received'