Pnictogen bonding at the service of gold catalysis: the case of a phosphinostiborane gold complex.
Zhou, Benyu; Bedajna, Shantabh; Gabbaï, François P; Chemical communications (Cambridge, England) 60 (2023) 192–195; doi:10.1039/d3cc04942f

data_7132357
_publ_section_title
;
 Pnictogen bonding at the service of gold catalysis: the case of a
 phosphinostiborane gold complex.
;
_journal_issue                   2
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              192
_journal_page_last               195
_journal_paper_doi               10.1039/d3cc04942f
_journal_volume                  60
_journal_year                    2023
_chemical_formula_moiety         'C47 H48 O P Sb'
_chemical_formula_sum            'C47 H48 O P Sb'
_chemical_formula_weight         781.57
_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
_audit_creation_date             2023-09-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-03 deposited with the CCDC.	2023-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.786(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.478(2)
_cell_length_b                   18.488(2)
_cell_length_c                   12.2139(16)
_cell_measurement_reflns_used    9385
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      28.985
_cell_measurement_theta_min      2.501
_cell_volume                     3877.0(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            93220
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.156
_diffrn_reflns_theta_min         2.179
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.4833
_exptl_absorpt_correction_T_min  0.4365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1061 before and 0.0915 after correction.
The Ratio of minimum to maximum transmission is 0.9032.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10438
_refine_ls_number_restraints     351
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0094P)^2^+8.3255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7638
_reflns_number_total             10438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04942f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7132357--7132360.cif.'
_cod_original_cell_volume        3877.2(9)
_cod_database_code               7132357
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.852
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Sb1A-C4 \\sim Sb1-C5
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.02 within 2A
C36A \\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.02 within 2A
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41: within 2A with sigma of
0.003 and sigma for terminal atoms of 0.02 within 2A
C42A \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim C47A \\sim C42 \\sim C43
\\sim C44 \\sim C45 \\sim C46 \\sim C47: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
P1A \\sim P1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C30A \\sim C31A
\\sim C32A \\sim C33A \\sim C34A \\sim C35A: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.02 within 2A
4. Same fragment restrains
{Sb1, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35} sigma for
1-2: 0.02, 1-3: 0.04
as in
{Sb1A, C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A, C35A}
{P1, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47} sigma for 1-2:
0.005, 1-3: 0.01
as in
{P1A, C36A, C37A, C38A, C39A, C40A, C41A, C42A, C43A, C44A, C45A, C46A, C47A}
5. Others
 Sof(P1A)=Sof(C36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=
 Sof(H39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(C43A)=
 Sof(H43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=
 Sof(C47A)=Sof(H47A)=Sof(Sb1A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=
 Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=
 Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=1-FVAR(1)
 Sof(P1)=Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(C43)=Sof(H43)=Sof(C44)=
 Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(Sb1)=
 Sof(C24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=
 Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=
 Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C37A(H37A), C38A(H38A), C39A(H39A), C40A(H40A), C41A(H41A), C43A(H43A),
 C44A(H44A), C45A(H45A), C46A(H46A), C47A(H47A), C25A(H25A), C26A(H26A),
 C27A(H27A), C28A(H28A), C29A(H29A), C31A(H31A), C32A(H32A), C33A(H33A),
 C34A(H34A), C35A(H35A), C8(H8), C3(H3), C6(H6), C1(H1), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
  C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35)
6.b Fitted hexagon refined as free rotating group:
 C36A(C37A,C38A,C39A,C40A,C41A), C42A(C43A,C44A,C45A,C46A,C47A), C24A(C25A,
 C26A,C27A,C28A,C29A), C30A(C31A,C32A,C33A,C34A,C35A), C36(C37,C38,C39,C40,C41),
  C42(C43,C44,C45,C46,C47), C24(C25,C26,C27,C28,C29), C30(C31,C32,C33,C34,C35)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C19(H19A,H19B,
 H19C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C)
;
_shelx_res_checksum              55764
_shelx_hkl_checksum              25054
_olex2_submission_special_instructions 'No special instructions were received'