Experimental and theoretical evidence for low-lying excited states in [Cr6E8(PEt3)6] (E = S, Se, Te) cluster molecules
Bügel, Patrick; Krummenacher, Ivo; Weigend, Florian; Eichhöfer, Andreas; Dalton Transactions  (2022) –; doi:10.1039/D2DT01690G

data_7711214
_publ_section_title
;
 Experimental and theoretical evidence for low-lying excited states in
 [Cr6E8(PEt3)6] (E = S, Se, Te) cluster molecules
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01690G
_journal_year                    2022
_chemical_formula_moiety         '2(C18 H45 Cr3 P3 S4)'
_chemical_formula_sum            'C36 H90 Cr6 P6 S8'
_chemical_formula_weight         1277.37
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-05-12 deposited with the CCDC.	2022-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                88.924(3)
_cell_angle_beta                 87.547(3)
_cell_angle_gamma                72.177(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7892(4)
_cell_length_b                   12.6230(5)
_cell_length_c                   20.2222(7)
_cell_measurement_reflns_used    48794
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      35.25
_cell_measurement_theta_min      1.97
_cell_volume                     2862.26(19)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      180.0
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI Mo'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            65054
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.344
_diffrn_reflns_theta_min         1.977
_diffrn_source                   'Mo GeniX 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Mo
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.584
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Koziskova, J.; Hahn, F.; Richter, J.; Kozisek, J. Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II), Acta Chim. Slov., 2016, 9(2), 136-140.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         23669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17188
_reflns_number_total             23669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01690g2.cif
_cod_data_source_block           p-1
_cod_database_code               7711214
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.693
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B),
 C21(H21A,H21B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B),
  C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              48069
_olex2_submission_special_instructions 'No special instructions were received'