Cluster Self-Assembly and Anion Binding by Metal Complexes of Non-Innocent Thiazolidinyl-Thiolate Ligands
Riffel, Madeline N.; Siegel, Lukas; Oliver, Allen Grayson; Tsui, Emily Y.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01339H

data_7710456
_publ_section_title
;
 Cluster Self-Assembly and Anion Binding by Metal Complexes of
 Non-Innocent Thiazolidinyl-Thiolate Ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01339H
_journal_year                    2022
_chemical_formula_moiety         'C13 H19 Cl2 Fe N3 S2, C4 H7 O'
_chemical_formula_sum            'C17 H26 Cl2 Fe N3 O S2'
_chemical_formula_weight         479.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-04-20 deposited with the CCDC.	2022-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                79.604(2)
_cell_angle_beta                 83.267(2)
_cell_angle_gamma                81.096(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3772(5)
_cell_length_b                   11.7069(8)
_cell_length_c                   12.7130(8)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    119.99
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.21
_cell_volume                     1062.39(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      119.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36783
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.518
_diffrn_reflns_theta_min         1.635
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6929
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0579 before and 0.0515 after correction.
The Ratio of minimum to maximum transmission is 0.9287.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       Rod
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         6491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.9246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5842
_reflns_number_total             6491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01339h2.cif
_cod_data_source_block           mr_1_231_fecl2l
_cod_database_code               7710456
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.693
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H00E,H00H), C2(H00K,H00L), C10(H00M,H00N), C11(H00I,H00J)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H00D), C6(H00G), C7(H00F), C14(H00R)
2.c Idealised Me refined as rotating group:
 C12(H00A,H00B,H00C), C13(H00O,H00P,H00Q), C16(H00S,H00T,H00U), C17(H00V,H00W,
 H00X)
;
_shelx_res_checksum              67302
_shelx_hkl_checksum              1704
_olex2_submission_special_instructions 'No special instructions were received'