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_7061888
_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 Ho2 O16 S6, H2 O'
_chemical_formula_sum            'C30 H28 Ho2 O17 S6'
_chemical_formula_weight         1182.74
_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             2022-01-07
_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                 116.176(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9388(6)
_cell_length_b                   19.2401(11)
_cell_length_c                   11.0949(8)
_cell_measurement_reflns_used    3476
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6250
_cell_measurement_theta_min      3.9380
_cell_volume                     1904.0(2)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0217
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.846
_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     -8.00  23.00   1.00    3.00    --   15.71  77.00 150.00   31
  2  \w     -2.00  24.00   1.00    3.00    --   15.71  77.00 -60.00   26
  3  \w    -84.00  -7.00   1.00    3.00    --  -16.96 -38.00-120.00   77
  4  \w    -42.00  38.00   1.00    3.00    --  -16.96  77.00   0.00   80
;
_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      -0.0087739000
_diffrn_orient_matrix_UB_12      -0.0365332000
_diffrn_orient_matrix_UB_13      -0.0082410000
_diffrn_orient_matrix_UB_21      -0.0431662000
_diffrn_orient_matrix_UB_22      0.0044777000
_diffrn_orient_matrix_UB_23      -0.0701840000
_diffrn_orient_matrix_UB_31      0.0662187000
_diffrn_orient_matrix_UB_32      -0.0018674000
_diffrn_orient_matrix_UB_33      -0.0091018000
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8447
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.178
_diffrn_reflns_theta_min         3.704
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69998
_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    2.063
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.935
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4364
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0208P)^2^+2.9954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3711
_reflns_number_total             4364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03556a2.cif
_cod_data_source_block           2202vv1ho
_cod_depositor_comments
'Adding full bibliography for 7061882--7061892.cif.'
_cod_database_code               7061888
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H12 S3 O6 Ho'
_chemical_oxdiff_usercomment     '  '
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 S1A-C5 \\sim S1-C3
 with sigma of 0.02
 S2A-C10 \\sim S2-C8
 with sigma of 0.02
 C9-C10 \\sim C9A-C8
 with sigma of 0.02
 S3-C15 \\sim S3A-C13
 with sigma of 0.02
 C14-C13 \\sim C14A-C15
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(S1A)
Uanis(C4) = Uanis(C4A)
Uanis(C9A) = Uanis(C9)
Uanis(S2) = Uanis(S2A)
Uanis(C14A) = Uanis(S3A)
Uanis(C14) = Uanis(S3)
Uanis(S3A) = Uanis(S3)
Uanis(C14) = Uanis(C14A)
3. Others
 Sof(C4A)=Sof(H4A)=Sof(H3B)=Sof(H5B)=Sof(S1A)=1-FVAR(1)
 Sof(C4)=Sof(H4)=Sof(H3A)=Sof(H5A)=Sof(S1)=FVAR(1)
 Sof(H8BB)=Sof(H10A)=Sof(S2A)=Sof(C9A)=Sof(H9A)=1-FVAR(2)
 Sof(H8AA)=Sof(H10)=Sof(S2)=Sof(C9)=Sof(H9)=FVAR(2)
 Sof(H15A)=Sof(H13A)=Sof(S3A)=Sof(C14A)=Sof(H14A)=1-FVAR(3)
 Sof(C14)=Sof(H14)=Sof(H15)=Sof(H13)=Sof(S3)=FVAR(3)
 Fixed Sof: O9(0.5) H9B(0.5) H9C(0.5)
4.a Free rotating group:
 O9(H9B,H9C)
4.b Rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C4(H4), C8(H8AA), C8(H8BB), C3(H3B), C3(H3A), C5(H5A), C5(H5B),
 C10(H10A), C10(H10), C9A(H9A), C9(H9), C14(H14), C15(H15), C15(H15A), C13(H13),
  C13(H13A), C14A(H14A)
;
_shelx_res_checksum              10038
_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 1.690
_oxdiff_exptl_absorpt_empirical_full_min 0.796