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_7133343
_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         'C44 H76 N4 Si4 Yb, C6 H14'
_chemical_formula_sum            'C50 H90 N4 Si4 Yb'
_chemical_formula_weight         1032.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-26 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.0881(4)
_cell_length_b                   22.6537(4)
_cell_length_c                   26.9902(6)
_cell_measurement_reflns_used    19637
_cell_measurement_temperature    173.0(2)
_cell_measurement_theta_max      29.8760
_cell_measurement_theta_min      2.0850
_cell_volume                     11059.6(4)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.800
_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    -66.00 -16.00   0.50   14.00    --    4.31 -10.00 -69.00  100
  2  \w      3.00  77.00   0.50   14.00    --    4.31  38.00-150.00  148
  3  \w    -17.00  34.00   0.50   14.00    --    4.31 -99.00  30.00  102
;
_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      -0.0048200000
_diffrn_orient_matrix_UB_12      -0.0199072000
_diffrn_orient_matrix_UB_13      -0.0200472000
_diffrn_orient_matrix_UB_21      -0.0015926000
_diffrn_orient_matrix_UB_22      0.0241084000
_diffrn_orient_matrix_UB_23      -0.0167247000
_diffrn_orient_matrix_UB_31      0.0388716000
_diffrn_orient_matrix_UB_32      -0.0015066000
_diffrn_orient_matrix_UB_33      -0.0031397000
_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  0.0644
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.800
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            68006
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.800
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.169
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62692
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         14315
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+35.9259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9880
_reflns_number_total             14315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03009e2.cif
_cod_data_source_block           xc-2-83_auto
_cod_depositor_comments
'Adding full bibliography for 7133340--7133344.cif.'
_cod_database_code               7133343
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Yb Si'
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.447
_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. Restrained distances
 N2-C53 \\sim N2-C9
 with sigma of 0.02
 C53-C51 \\sim C9-C8
 with sigma of 0.02
 N2-C51 \\sim N2-C8
 with sigma of 0.04
 N3-C53 \\sim N3-C9
 with sigma of 0.04
 N2-C9 \\sim N2-C53
 with sigma of 0.02
 C8-C9 \\sim C51-C53
 with sigma of 0.02
 N3-C51 \\sim N3-C8
 with sigma of 0.02
 N4-C01M \\sim N4-C6
 with sigma of 0.02
 C01M-C7 \\sim C6-C52
 with sigma of 0.02
 N4-C7 \\sim N4-C52
 with sigma of 0.04
 N3-C01M \\sim N3-C6
 with sigma of 0.04
 N3-C7 \\sim N3-C52
 with sigma of 0.02
 C6-C52 \\sim C7-C01M
 with sigma of 0.02
 N4-C6 \\sim N4-C01M
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C51 \\sim C53: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C9 \\sim C8: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C7 \\sim C01M: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C6 \\sim C52: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C51) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C01M) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C8)=Sof(H8A)=Sof(H8B)=1-FVAR(1)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C51)=Sof(H51A)=Sof(H51B)=FVAR(1)
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C6)=Sof(H6A)=Sof(H6B)=1-FVAR(2)
 Sof(C01M)=Sof(H01A)=Sof(H01B)=Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C27(H27), C19(H19), C22(H22)
5.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C49(H,HA), C51(H51A,H51B), C48(HE,HF), C47(HG,HH), C46(HI,HJ),
  C01M(H01A,H01B), C7(H7A,H7B), C9(H9A,H9B), C8(H8A,H8B), C52(H52A,H52B),
 C6(H6A,H6B)
5.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C3(H3), C15(H15), C30(H30), C33(H33), C31(H31), C16(H16), C17(H17),
 C32(H32)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C21(H21A,H21B,
 H21C), C42(H42A,H42B,H42C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C12(H12A,
 H12B,H12C), C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C11(H11A,H11B,H11C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C38(H38A,H38B,
 H38C), C5(H5A,H5B,H5C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C50(HB,HC,
 HD), C45(HK,HL,HM)
;
_shelx_res_checksum              58556
_shelx_hkl_checksum              59481
_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 1.499
_oxdiff_exptl_absorpt_empirical_full_min 0.733