Yb/Si frustrated Lewis pairs with a labile naphthalenyl bridge.
Xu, Cheng; Zhao, Sixuan; Zhang, Heng; Peng, Qian; Chen, Yaofeng; Chemical communications (Cambridge, England) 60 (2024) 8411–8414; doi:10.1039/d4cc03009e

data_7133344
_publ_section_title
;
 Yb/Si frustrated Lewis pairs with a labile naphthalenyl bridge.
;
_journal_issue                   64
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8411
_journal_page_last               8414
_journal_paper_doi               10.1039/d4cc03009e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C34 H68 N4 S2 Si4 Yb, 0.055[CH3OH]'
_chemical_formula_sum            'C34.06 H68.23 N4 O0.06 S2 Si4 Yb'
_chemical_formula_weight         884.35
_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             2023-12-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-26 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                78.3820(10)
_cell_angle_beta                 69.4360(10)
_cell_angle_gamma                69.691(2)
_cell_formula_units_Z            4
_cell_length_a                   15.4962(3)
_cell_length_b                   17.7037(3)
_cell_length_c                   19.3080(3)
_cell_measurement_reflns_used    52865
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      31.2100
_cell_measurement_theta_min      2.1820
_cell_volume                     4632.04(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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    -17.00  76.00   0.50    2.45    --    3.98  75.00-102.00  186
  2  \w    -18.00  35.00   0.50    2.45    --    3.98 -99.00  90.00  106
  3  \w    -18.00  35.00   0.50    2.45    --    3.98 -99.00   0.00  106
  4  \w    -68.00  25.00   0.50    2.45    --    3.98 -75.00 130.00  186
  5  \w     -6.00  76.00   0.50    2.45    --    3.98  38.00-180.00  164
  6  \w    -18.00  35.00   0.50    2.45    --    3.98 -99.00-180.00  106
  7  \w    -18.00  35.00   0.50    2.45    --    3.98 -99.00-120.00  106
  8  \w    -77.00   9.00   0.50    2.45    --   -4.92 -57.00 -30.00  172
  9  \w    -77.00 -33.00   0.50    2.45    --   -4.92   0.00 -30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0050421000
_diffrn_orient_matrix_UB_12      -0.0276118000
_diffrn_orient_matrix_UB_13      0.0315490000
_diffrn_orient_matrix_UB_21      0.0255612000
_diffrn_orient_matrix_UB_22      0.0218484000
_diffrn_orient_matrix_UB_23      0.0079537000
_diffrn_orient_matrix_UB_31      -0.0441573000
_diffrn_orient_matrix_UB_32      0.0245026000
_diffrn_orient_matrix_UB_33      0.0222170000
_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  0.0799
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            103666
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.139
_diffrn_reflns_theta_min         2.113
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.097
_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     812
_refine_ls_number_reflns         24542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0276P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18944
_reflns_number_total             24542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03009e2.cif
_cod_data_source_block           xc-2-37_auto
_cod_depositor_comments
'Adding full bibliography for 7133340--7133344.cif.'
_cod_database_code               7133344
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Yb Si S'
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.389
_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 Ternary CH refined with riding coordinates:
 C9(H9), C44(H44), C36(H36), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C52(H52A,H52B), C19(H19A,H19B), C18(H18A,H18B), C55(H55A,
 H55B), C21(H21A,H21B), C56(H56A,H56B), C22(H22A,H22B)
2.c Me refined with riding coordinates:
 C54(H54A,H54B,H54C), C51(H51A,H51B,H51C), C57(H57A,H57B,H57C), C24(H24A,H24B,
 H24C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C46(H46A,
 H46B,H46C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C20(H20A,H20B,H20C),
 C58(H58A,H58B,H58C), C10(H10A,H10B,H10C), C28(H28A,H28B,H28C), C31(H31A,H31B,
 H31C), C26(H26A,H26B,H26C), C65(H65A,H65B,H65C), C25(H25A,H25B,H25C), C60(H60A,
 H60B,H60C), C66(H66A,H66B,H66C), C37(H37A,H37B,H37C), C61(H61A,H61B,H61C),
 C3(H3A,H3B,H3C), C45(H45A,H45B,H45C), C59(H59A,H59B,H59C), C028(H02A,H02B,
 H02C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C63(H63A,H63B,H63C), C32(H32A,
 H32B,H32C), C64(H64A,H64B,H64C), C30(H30A,H30B,H30C), C62(H62A,H62B,H62C),
 C35(H35A,H35B,H35C), C1(H1A,H1B,H1C)
2.d Aromatic/amide H refined with riding coordinates:
 C49(H49), C15(H15), C41(H41), C39(H39), C40(H40), C5(H5), C7(H7), C6(H6)
2.e Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 5 electrons were 
found in a volume of 756\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
0.11[CH3OH] per Asymmetric Unit 
which account for 4 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47548
_shelx_hkl_checksum              52629
_shelx_fab_checksum              12536
_platon_squeeze_special_details
;
A solvent mask was calculated and 55 electrons were 
found in a volume of 412\%A^3^ in 6 voids per unit cell. 
This is consistent with the presence of 
0.56[C6H14], 1[], 1[], 0.5[], 1.5[], 0.5[] per Asymmetric Unit 
which account for 56 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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 2.757
_oxdiff_exptl_absorpt_empirical_full_min 0.153