Nucleophilic reactivity of the gold atom in a diarylborylgold(i) complex toward polar multiple bonds.
Suzuki, Akane; Guo, Xueying; Lin, Zhenyang; Yamashita, Makoto; Chemical science 12 (2020) 917–928; doi:10.1039/d0sc05478j

data_1559577
_publ_section_title
;
 Nucleophilic reactivity of the gold atom in a diarylborylgold(i) complex
 toward polar multiple bonds.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              917
_journal_page_last               928
_journal_paper_doi               10.1039/d0sc05478j
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C41 H50 Au B N2'
_chemical_formula_sum            'C41 H50 Au B N2'
_chemical_formula_weight         778.60
_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     dual
_audit_creation_date             2020-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2020-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                72.838(3)
_cell_angle_beta                 89.216(3)
_cell_angle_gamma                74.717(3)
_cell_formula_units_Z            4
_cell_length_a                   10.5714(3)
_cell_length_b                   18.1828(6)
_cell_length_c                   20.5890(9)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      30.4610
_cell_measurement_theta_min      2.0420
_cell_volume                     3638.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.9821
_diffrn_measured_fraction_theta_max 0.9821
_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    -32.00   7.14   0.38   30.00    --   -4.24 -37.00 -60.00  103
  2  \w     30.00  67.62   0.38   30.00    --   -4.24  57.00 -60.00   99
  3  \w    -14.00  20.20   0.38   30.00    --   -4.24 -99.00 120.00   90
  4  \w    -66.00   4.30   0.38   30.00    --   -4.24 -37.00-180.00  185
  5  \w    -19.00  38.00   0.38   30.00    --    5.65 -99.00 150.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0054291000
_diffrn_orient_matrix_UB_12      -0.0134855000
_diffrn_orient_matrix_UB_13      -0.0285777000
_diffrn_orient_matrix_UB_21      -0.0694153000
_diffrn_orient_matrix_UB_22      0.0105680000
_diffrn_orient_matrix_UB_23      0.0008860000
_diffrn_orient_matrix_UB_31      -0.0036902000
_diffrn_orient_matrix_UB_32      0.0388093000
_diffrn_orient_matrix_UB_33      -0.0221106000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.9821
_diffrn_reflns_Laue_measured_fraction_max 0.9821
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21641
_diffrn_reflns_point_group_measured_fraction_full 0.9821
_diffrn_reflns_point_group_measured_fraction_max 0.9821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.065
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-R
_exptl_absorpt_coefficient_mu    4.073
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.76a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.053
_refine_diff_density_max         2.751
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         21641
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0949P)^2^+0.7970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17682
_reflns_number_total             21641
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9967\% 
around [0.91 0.41 0.02] (reciprocal) or [1.00 0.00 -0.00] (direct)
;
_cod_data_source_file            d0sc05478j3.cif
_cod_data_source_block           2
_cod_depositor_comments
;Adding full bibliography for 1559577--1559587.cif.

 Adding full bibliography for 1559577--1559587.cif.
;
_cod_database_code               1559577
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C41 H50Au B N2'
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.620
_diffrn_oxdiff_digest_frames
;
017ffeb1fcd7df8c1e43a2b36eda4767da006271b44
;
_diffrn_oxdiff_digest_hkl
;
01d9778f7bac164176ace4e69714f9ff1ca47f
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5387(7)
 0.4613(7)
2. 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
3. Uiso/Uaniso restraints and constraints
C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B1) = Uanis(C42)
Uanis(B2) = Uanis(C92)
4. Rigid body (RIGU) restrains
 C35, C36, C37, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C43, C44, C45, C46, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C85, C86, C87, C88, C89, C90, C91
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C92, C93, C94, C95, C96, C97, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=1-FVAR(1)
 Sof(C35)=Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(1)
 Sof(C92)=Sof(C93)=Sof(C94)=Sof(H94)=Sof(C95)=Sof(H95)=Sof(C96)=Sof(H96)=
 Sof(C97)=Sof(H97)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=1-FVAR(2)
 Sof(C85)=Sof(C86)=Sof(C87)=Sof(H87)=Sof(C88)=Sof(H88)=Sof(C89)=Sof(H89)=
 Sof(C90)=Sof(H90)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=FVAR(2)
 Sof(H70A)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C74)=Sof(H74A)=Sof(H74B)=
 Sof(H74C)=1-FVAR(3)
 Sof(H70)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C72)=Sof(H72A)=Sof(H72B)=
 Sof(H72C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C58(H58), C61(H61), C70(H70),
 C70(H70A), C75(H75)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39), C40(H40),
  C44(H44), C45(H45), C46(H46), C47(H47), C50(H50), C51(H51), C54(H54),
 C55(H55), C56(H56), C66(H66), C67(H67), C68(H68), C80(H80), C81(H81), C82(H82),
  C83(H83), C87(H87), C88(H88), C89(H89), C90(H90), C94(H94), C95(H95),
 C96(H96), C97(H97)
6.c Fitted hexagon refined as free rotating group:
 C78(C79,C80,C81,C82,C83), C85(C86,C87,C88,C89,C90), C92(C93,C94,C95,C96,C97)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C34(H34A,H34B,H34C), C41(H41A,H41B,H41C), C48(H48A,H48B,H48C),
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,
 H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C84(H84A,H84B,H84C),
 C91(H91A,H91B,H91C), C98(H98A,H98B,H98C)
;
_shelx_res_checksum              19870
_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 1.934
_oxdiff_exptl_absorpt_empirical_full_min 0.345
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2