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_7061890
_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 Lu2 O16 S6, H2 O'
_chemical_formula_sum            'C30 H28 Lu2 O17 S6'
_chemical_formula_weight         1202.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-13
_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                 116.308(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8729(3)
_cell_length_b                   19.2032(5)
_cell_length_c                   11.0534(4)
_cell_measurement_reflns_used    14414
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      32.1900
_cell_measurement_theta_min      3.7000
_cell_volume                     1878.57(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.850
_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      4.00  52.00   0.50    0.56    --   -8.90  38.00  60.00   96
  2  \w    -42.00  16.00   0.50    0.56    --    9.22 -87.00  64.00  116
  3  \w    -36.00  21.00   0.50    0.56    --   -8.90  87.00-177.00  114
  4  \w    -42.00  18.00   0.50    0.56    --   -8.90 -87.00  64.00  120
  5  \w    -23.00  24.00   0.50    0.56    --   -8.90 -99.00 -60.00   94
  6  \w    -23.00  24.00   0.50    0.56    --   -8.90 -99.00-120.00   94
  7  \w    -23.00  23.00   0.50    0.56    --   -8.90 -99.00-180.00   92
  8  \w    -22.00  23.00   0.50    0.56    --   -8.90 -99.00-150.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0170704000
_diffrn_orient_matrix_UB_12      -0.0183657000
_diffrn_orient_matrix_UB_13      0.0607282000
_diffrn_orient_matrix_UB_21      -0.0315933000
_diffrn_orient_matrix_UB_22      0.0274683000
_diffrn_orient_matrix_UB_23      0.0221455000
_diffrn_orient_matrix_UB_31      -0.0716713000
_diffrn_orient_matrix_UB_32      -0.0164709000
_diffrn_orient_matrix_UB_33      -0.0307923000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26278
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.145
_diffrn_reflns_theta_min         3.705
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50689
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_description       prism
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.121
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5615
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0172P)^2^+4.1736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4901
_reflns_number_total             5615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03556a2.cif
_cod_data_source_block           mx138_21_auto
_cod_depositor_comments
'Adding full bibliography for 7061882--7061892.cif.'
_cod_database_code               7061890
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Lu S O C H'
_chemical_oxdiff_usercomment     'colourless block'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 C4-C3 \\sim C4A-C5
 with sigma of 0.02
 C14A-C15 \\sim C14-C13
 with sigma of 0.02
 C9-C8 \\sim C9A-C10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(S1A)
Uanis(C4A) = Uanis(C4)
Uanis(C14) = Uanis(C14A)
Uanis(S3) = Uanis(S3A)
Uanis(S2A) = Uanis(S2)
Uanis(C9) = Uanis(C9A)
4. Others
 Sof(S2)=Sof(H10A)=Sof(H8BB)=Sof(C9)=Sof(H9)=1-FVAR(1)
 Sof(S2A)=Sof(H10)=Sof(H8AA)=Sof(C9A)=Sof(H9A)=FVAR(1)
 Sof(S3A)=Sof(H13A)=Sof(H15A)=Sof(C14A)=Sof(H14A)=1-FVAR(2)
 Sof(S3)=Sof(H13)=Sof(H15)=Sof(C14)=Sof(H14)=FVAR(2)
 Sof(S1A)=Sof(H5B)=Sof(H3B)=Sof(C4A)=Sof(H4A)=1-FVAR(3)
 Sof(S1)=Sof(H5A)=Sof(H3A)=Sof(C4)=Sof(H4)=FVAR(3)
 Fixed Sof: O9(0.5) H9B(0.5) H9C(0.5)
5.a Free rotating group:
 O9(H9B,H9C)
5.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10A), C10(H10), C8(H8AA), C8(H8BB), C5(H5A), C5(H5B), C3(H3B), C3(H3A),
 C13(H13A), C13(H13), C15(H15), C15(H15A), C14(H14), C9(H9), C9A(H9A),
 C14A(H14A), C4A(H4A), C4(H4)
;
_shelx_res_checksum              85130
_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 2.696
_oxdiff_exptl_absorpt_empirical_full_min 0.624