Isolation and reactivity of a gold(I) hydroxytrifluoroborate complex stabilized by anion-π<sup>+</sup> interactions.
Zhou, Jiliang; Litle, Elishua D.; Gabbaï, François P; Chemical communications (Cambridge, England) 57 (2021) 10154–10157; doi:10.1039/d1cc04105c

data_7128904
_publ_section_title
;
 Isolation and reactivity of a gold(I) hydroxytrifluoroborate complex
 stabilized by anion-\p<sup>+</sup> interactions.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10154
_journal_page_last               10157
_journal_paper_doi               10.1039/d1cc04105c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C40 H31 Au B F3 O3 P, 0.53(C6 H4 F2), 0.47(C6 H14), B F4'
_chemical_formula_sum            'C46 H39.7 Au B2 F8.06 O3 P'
_chemical_formula_weight         1043.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-09 deposited with the CCDC.	2021-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.643(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.170(3)
_cell_length_b                   10.7619(10)
_cell_length_c                   25.281(3)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.64
_cell_volume                     8135.5(15)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0601
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            117359
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         1.977
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.736
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_correction_T_min  0.3155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1088 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.6393.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       plate
_exptl_crystal_F_000             4130
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.038
_refine_diff_density_min         -1.978
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10526
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0385P)^2^+95.0255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8948
_reflns_number_total             10526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04105c2.cif
_cod_data_source_block           5-BF4
_cod_depositor_comments
'Adding full bibliography for 7128901--7128904.cif.'
_cod_original_cell_volume        8135.4(13)
_cod_original_formula_sum        'C46 H39.70 Au B2 F8.06 O3 P'
_cod_database_code               7128904
_shelxl_version_number           2014-3
_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, All O(H) groups
2. Restrained distances
 O3-H3
 0.87 with sigma of 0.01
 B1-H3
 1.941327 with sigma of 0.02
 Au1-H3
 2.68079 with sigma of 0.02
 C7S-C8S \\sim C8S-C9S
 with sigma of 0.005
 C9S-C10S \\sim C8S-C9S
 with sigma of 0.005
 C9S-C10S \\sim C10S-C11S
 with sigma of 0.005
 C10S-C11S \\sim C11S-C12S
 with sigma of 0.005
 C1S-F1S \\sim C2S-F2S
 with sigma of 0.005
 C6S-F1S \\sim C3S-F2S
 with sigma of 0.005
3. Restrained planarity
 F1S, F2S, C1S, C2S, C3S, C4S, C5S, C6S
 with sigma of 0.1
4. Rigid bond restraints
 F1S, F2S, C1S, C2S, C3S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F4, F5, F6, F7, B2
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C7S, C8S, C9S, C10S, C11S, C12S
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
5. Uiso/Uaniso restraints and constraints
F1S \\sim F2S \\sim C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
F4 \\sim F5 \\sim F6 \\sim F7 \\sim B2: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C7S \\sim C8S \\sim C9S \\sim C10S \\sim C11S \\sim C12S: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
6. Others
 Fixed Sof: F1S(0.53) F2S(0.53) C1S(0.53) C2S(0.53) C3S(0.53) H3S(0.53)
 C4S(0.53) H4S(0.53) C5S(0.53) H5S(0.53) C6S(0.53) H6S(0.53) C7S(0.47)
 H7SA(0.47) H7SB(0.47) H7SC(0.47) C8S(0.47) H8SA(0.47) H8SB(0.47) C9S(0.47)
 H9SA(0.47) H9SB(0.47) C10S(0.47) H10A(0.47) H10B(0.47) C11S(0.47) H11A(0.47)
 H11B(0.47) C12S(0.47) H12A(0.47) H12B(0.47) H12C(0.47)
7.a Secondary CH2 refined with riding coordinates:
 C8S(H8SA,H8SB), C9S(H9SA,H9SB), C10S(H10A,H10B), C11S(H11A,H11B)
7.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C34(H34), C3(H3A), C2(H2), C4(H4), C11(H11), C18(H18), C27(H27),
 C19(H19), C12(H12), C33(H33), C31(H31), C36(H36), C39(H39), C38(H38), C37(H37),
  C30(H30), C26(H26), C20(H20), C21(H21), C25(H25), C24(H24), C40(H40),
 C32(H32), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
7.c Fitted hexagon refined as free rotating group:
 C1S(C2S,C3S,C4S,C5S,C6S)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7S(H7SA,H7SB,H7SC), C12S(H12A,H12B,H12C)
;
_shelx_res_checksum              65019
_olex2_submission_special_instructions 'No special instructions were received'