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_7132351
_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         'C30 H43 O Y'
_chemical_formula_sum            'C30 H43 O Y'
_chemical_formula_weight         508.55
_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   geom
_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
;
2023-08-31 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.699(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4266(2)
_cell_length_b                   17.1628(3)
_cell_length_c                   16.8285(3)
_cell_measurement_reflns_used    16390
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.7180
_cell_measurement_theta_min      3.4140
_cell_volume                     2656.03(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_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 0.821
_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    -73.00 -46.00   0.50   11.59    --   -4.69 -32.00 132.00   54
  2  \w    -17.00  45.00   0.50   11.59    --   -4.69  32.00 -68.00  124
  3  \w    -26.00   0.00   0.50   11.59    --   -4.69  77.00   0.00   52
  4  \w     12.00  69.00   0.50   11.59    --   -4.69  24.00 -38.60  114
  5  \w    -30.00   5.00   0.50   11.59    --   -4.69 -32.00 132.00   70
  6  \w    -26.00  -1.00   0.50   11.59    --   -4.69  77.00-150.00   50
  7  \w    -15.00  20.00   0.50   11.59    --    5.47 -57.00-120.00   70
  8  \w     -7.00  18.00   0.50   11.59    --    5.47  37.00-150.00   50
  9  \w     13.00  39.00   0.50   11.59    --    5.47 -99.00 120.00   52
 10  \w     40.00  71.00   0.50   11.59    --    5.47   0.00-120.00   62
 11  \w     13.00  39.00   0.50   11.59    --    5.47 -99.00  90.00   52
;
_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      -0.0097174000
_diffrn_orient_matrix_UB_12      -0.0146980000
_diffrn_orient_matrix_UB_13      0.0378290000
_diffrn_orient_matrix_UB_21      -0.0734152000
_diffrn_orient_matrix_UB_22      -0.0091138000
_diffrn_orient_matrix_UB_23      -0.0180733000
_diffrn_orient_matrix_UB_31      0.0216337000
_diffrn_orient_matrix_UB_32      -0.0375209000
_diffrn_orient_matrix_UB_33      -0.0104560000
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32939
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.842
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0242P)^2^+2.4052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5975
_reflns_number_total             6862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04520j2.cif
_cod_data_source_block           erp-ii-124_hex_final
_cod_database_code               7132351
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         YC30H43O
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.416
_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:
 C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C25(H25), C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,
 H16C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C7(H7A,H7B,
 H7C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              55702
_shelx_hkl_checksum              4366
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.775
_oxdiff_exptl_absorpt_empirical_full_min 0.787