Isolation of an organometallic yttrium bismuth cluster and elucidation of its electronic structure.
Pugliese, Elizabeth R.; Benner, Florian; Demir, Selvan; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc04520j

data_7132350
_publ_section_title
;
 Isolation of an organometallic yttrium bismuth cluster and elucidation of
 its electronic structure.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc04520j
_journal_year                    2023
_chemical_formula_moiety         'C52 H94 Bi6 K2 O8 Y2'
_chemical_formula_sum            'C52 H94 Bi6 K2 O8 Y2'
_chemical_formula_weight         2357.17
_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             2023-08-28
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-10-31 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.961(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3252(3)
_cell_length_b                   16.7323(5)
_cell_length_c                   15.4540(5)
_cell_measurement_reflns_used    13310
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      25.1600
_cell_measurement_theta_min      2.2100
_cell_volume                     3382.78(17)
_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 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(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 0.997
_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    -18.00  14.00   0.50   90.00    --   -5.49  57.00 -30.00   64
  2  \w    -28.00  -1.00   0.50   90.00    --   -5.49  77.00 -90.00   54
  3  \w    -11.00  14.00   0.50   90.00    --   -5.49  57.00-120.00   50
  4  \w    -15.00  14.00   0.50   90.00    --   -5.49  57.00-180.00   58
  5  \w    -28.00  -1.00   0.50   90.00    --   -5.49  77.00-150.00   54
  6  \w    -15.00  10.00   0.50   90.00    --    5.10 -57.00-150.00   50
  7  \w      4.00  32.00   0.50   90.00    --    5.10 -95.00 -39.00   56
  8  \w    -19.00  15.00   0.50   90.00    --   -5.49  57.00 120.00   68
  9  \w      0.00  27.00   0.50   90.00    --    5.10 -77.00  60.00   54
 10  \w     13.00  38.00   0.50   90.00    --    5.10 -99.00 120.00   50
 11  \w      0.00  28.00   0.50   90.00    --    5.10 -77.00 150.00   56
 12  \w    -25.00  26.00   0.50   90.00    --   -5.49 -95.00 -39.00  102
;
_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      0.0240192000
_diffrn_orient_matrix_UB_12      -0.0379656000
_diffrn_orient_matrix_UB_13      0.0038943000
_diffrn_orient_matrix_UB_21      -0.0282437000
_diffrn_orient_matrix_UB_22      -0.0108760000
_diffrn_orient_matrix_UB_23      -0.0420215000
_diffrn_orient_matrix_UB_31      0.0395743000
_diffrn_orient_matrix_UB_32      0.0153933000
_diffrn_orient_matrix_UB_33      -0.0201236000
_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  0.0575
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32621
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.216
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    17.407
_exptl_absorpt_correction_T_max  0.04468
_exptl_absorpt_correction_T_min  0.02608
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.314
_exptl_crystal_description       sphere
_exptl_crystal_F_000             2168
_exptl_crystal_recrystallization_method 'Used as recieved'
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.077
_exptl_crystal_size_rad          0.069
_refine_diff_density_max         1.754
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         6102
_refine_ls_number_restraints     1107
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0840P)^2^+4.3400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4693
_reflns_number_total             6102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04520j2.cif
_cod_data_source_block           erp-1-36_110620
_cod_original_cell_volume        3382.79(17)
_cod_database_code               7132350
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20Y2Bi6K2O8
_shelx_estimated_absorpt_t_max   0.348
_shelx_estimated_absorpt_t_min   0.126
_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. Restrained distances
 C3A-C2A \\sim C2B-C3B \\sim C2B-C1B \\sim C1A-C2A \\sim C1A-C5A \\sim C1B-C5B
\\sim C5A-C4A \\sim C4B-C5B
 \\sim C4A-C3A \\sim C4B-C3B
 with sigma of 0.02
 O3B-C19B \\sim O3A-C19A \\sim O3A-C22A \\sim O3B-C22B \\sim O2B-C18B \\sim
O2B-C15B \\sim O2A-C15A ~
 O2A-C18A \\sim O1A-C14A \\sim O1B-C14B \\sim O1A-C11A \\sim O1B-C11B
 with sigma of 0.02
 C12A-C11A \\sim C12B-C11B \\sim C13A-C12A \\sim C13B-C12B \\sim C13A-C14A
\\sim C13B-C14B \\sim C18B-
 C17B \\sim C15A-C16A \\sim C16B-C15B \\sim C17B-C16B \\sim C18A-C17A \\sim
C17A-C16A \\sim C19A-C20A ~
 C19B-C20B \\sim C20B-C21B \\sim C20A-C21A \\sim C21A-C22A \\sim C21B-C22B
\\sim C24B-C23B \\sim C24A-
 C23A \\sim C24B-C25B \\sim C25A-C24A \\sim C25B-C26B \\sim C25A-C26A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B \\sim
C16B \\sim C17B \\sim C18B \\sim C19B \\sim C20B \\sim C21B \\sim C22B \\sim
C23B \\sim C24B \\sim C25B \\sim C26B \\sim C1A \\sim C2A \\sim C3A \\sim C4A
\\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim
C12A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim
C19A \\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim
C26A: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
within 2A
O1B \\sim O2B \\sim O3B \\sim O4B \\sim O1A \\sim O2A \\sim O3A \\sim O4A:
within 2A with sigma of 0.0002 and sigma for terminal atoms of 0.004 within 2A
Uanis(C20A) = Uanis(C20B)
Uanis(C19A) = Uanis(C19B)
Uanis(K1A) = Uanis(K1B)
Uanis(O4A) = Uanis(O1B)
Uanis(O4B) = Uanis(O2A)
4. Others
 Fixed Sof: Bi1B(0.5) Bi2B(0.5) Bi3B(0.5) Y1B(0.5) K1B(0.5) O1B(0.5) O2B(0.5)
 O3B(0.5) O4B(0.5) C1B(0.5) C2B(0.5) C3B(0.5) C4B(0.5) C5B(0.5) C6B(0.5)
 H6BA(0.5) H6BB(0.5) H6BC(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C8B(0.5)
 H8BA(0.5) H8BB(0.5) H8BC(0.5) C9B(0.5) H9BA(0.5) H9BB(0.5) H9BC(0.5) C10B(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) C11B(0.5) H11A(0.5) H11B(0.5) C12B(0.5)
 H12A(0.5) H12B(0.5) C13B(0.5) H13A(0.5) H13B(0.5) C14B(0.5) H14A(0.5)
 H14B(0.5) C15B(0.5) H15A(0.5) H15B(0.5) C16B(0.5) H16A(0.5) H16B(0.5)
 C17B(0.5) H17A(0.5) H17B(0.5) C18B(0.5) H18A(0.5) H18B(0.5) C19B(0.5)
 H19A(0.5) H19B(0.5) C20B(0.5) H20A(0.5) H20B(0.5) C21B(0.5) H21A(0.5)
 H21B(0.5) C22B(0.5) H22A(0.5) H22B(0.5) C23B(0.5) H23A(0.5) H23B(0.5)
 C24B(0.5) H24A(0.5) H24B(0.5) C25B(0.5) H25A(0.5) H25B(0.5) C26B(0.5)
 H26A(0.5) H26B(0.5) Bi1A(0.5) Bi2A(0.5) Bi3A(0.5) Y1A(0.5) K1A(0.5) O1A(0.5)
 O2A(0.5) O3A(0.5) O4A(0.5) C1A(0.5) C2A(0.5) C3A(0.5) C4A(0.5) C5A(0.5)
 C6A(0.5) H6AA(0.5) H6AB(0.5) H6AC(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5)
 C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5)
 C10A(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C11A(0.5) H11C(0.5) H11D(0.5)
 C12A(0.5) H12C(0.5) H12D(0.5) C13A(0.5) H13C(0.5) H13D(0.5) C14A(0.5)
 H14C(0.5) H14D(0.5) C15A(0.5) H15C(0.5) H15D(0.5) C16A(0.5) H16C(0.5)
 H16D(0.5) C17A(0.5) H17C(0.5) H17D(0.5) C18A(0.5) H18C(0.5) H18D(0.5)
 C19A(0.5) H19C(0.5) H19D(0.5) C20A(0.5) H20C(0.5) H20D(0.5) C21A(0.5)
 H21C(0.5) H21D(0.5) C22A(0.5) H22C(0.5) H22D(0.5) C23A(0.5) H23C(0.5)
 H23D(0.5) C24A(0.5) H24C(0.5) H24D(0.5) C25A(0.5) H25C(0.5) H25D(0.5)
 C26A(0.5) H26C(0.5) H26D(0.5)
5.a Riding coordinates:
 C18B(H18A,H18B), C19B(H19A,H19B), C22B(H22A,H22B), C23B(H23A,H23B), C11A(H11C,
 H11D), C26A(H26C,H26D)
5.b Secondary CH2 refined with riding coordinates:
 C11B(H11A,H11B), C12B(H12A,H12B), C13B(H13A,H13B), C14B(H14A,H14B), C15B(H15A,
 H15B), C16B(H16A,H16B), C17B(H17A,H17B), C20B(H20A,H20B), C21B(H21A,H21B),
 C24B(H24A,H24B), C25B(H25A,H25B), C26B(H26A,H26B), C12A(H12C,H12D), C13A(H13C,
 H13D), C14A(H14C,H14D), C15A(H15C,H15D), C16A(H16C,H16D), C17A(H17C,H17D),
 C18A(H18C,H18D), C19A(H19C,H19D), C20A(H20C,H20D), C21A(H21C,H21D), C22A(H22C,
 H22D), C23A(H23C,H23D), C24A(H24C,H24D), C25A(H25C,H25D)
5.c Idealised Me refined as rotating group:
 C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,
 H9BC), C10B(H10A,H10B,H10C), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC),
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              41321
_shelx_hkl_checksum              46776
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_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 2.851
_oxdiff_exptl_absorpt_empirical_full_min 0.463