A cationic gold-fluorenyl complex with a dative Au → C+ bond: synthesis, structure, and carbophilic reactivity
Litle, Elishua D.; Gabbaï, François P.; Chemical Communications 59 (2023) 603–606; doi:10.1039/D2CC05436A

data_7131045
_publ_section_title
;
 A cationic gold-fluorenyl complex with a dative Au \\rightarrow C+ bond:
 synthesis, structure, and carbophilic reactivity
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              603
_journal_page_last               606
_journal_paper_doi               10.1039/D2CC05436A
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C31 H22 Au Cl2 P'
_chemical_formula_sum            'C31 H22 Au Cl2 P'
_chemical_formula_weight         693.32
_chemical_name_systematic        C31H22AuCl2P
_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
_audit_creation_date             2022-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-12 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.629(2)
_cell_length_b                   19.046(4)
_cell_length_c                   28.172(7)
_cell_measurement_reflns_used    8571
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      68.487
_cell_measurement_theta_min      3.138
_cell_volume                     5167(2)
_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  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57508
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.567
_diffrn_reflns_theta_min         3.137
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.326
_exptl_absorpt_correction_T_max  0.4215
_exptl_absorpt_correction_T_min  0.1489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1616 before and 0.0907 after correction. The Ratio of minimum to maximum transmission is 0.3521. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.136
_refine_diff_density_max         2.099
_refine_diff_density_min         -2.206
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4726
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+42.3095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3946
_reflns_number_total             4726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05436a2.cif
_cod_data_source_block           eli93_0m_a
_cod_depositor_comments
'Adding full bibliography for 7131043--7131047.cif.'
_cod_original_cell_volume        5166(2)
_cod_database_code               7131045
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C20 \\sim C21A \\sim C22A \\sim C23 \\sim C24A \\sim C25A: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.004 within 2A
Uanis(C26') = Uanis(C26)
3. Others
 Sof(C26')=1-FVAR(1)
 Sof(C26)=FVAR(1)
 Sof(C31')=Sof(H31')=1-FVAR(2)
 Sof(C31)=Sof(H31)=FVAR(2)
 Sof(C30')=Sof(H30')=1-FVAR(3)
 Sof(C30)=Sof(H30)=FVAR(3)
 Sof(C29')=Sof(H29')=1-FVAR(4)
 Sof(C29)=Sof(H29)=FVAR(4)
 Sof(C28')=Sof(H28')=1-FVAR(5)
 Sof(C28)=Sof(H28)=FVAR(5)
 Sof(C27')=Sof(H27')=1-FVAR(6)
 Sof(C27)=Sof(H27)=FVAR(6)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C16(H16),
 C17(H17), C18(H18), C19(H19), C27(H27), C31(H31), C30(H30), C29(H29), C28(H28),
  C27'(H27'), C28'(H28'), C29'(H29'), C30'(H30'), C31'(H31'), C25A(H25A),
 C24A(H24A), C23(H23), C22A(H22A), C21A(H21A)
4.b Fitted hexagon refined as free rotating group:
 C27(C26,C31,C30,C29,C28), C20(C25A,C24A,C23,C22A,C21A)
;
_shelx_res_checksum              80271
_shelx_hkl_checksum              15500
_olex2_submission_original_sample_id Eli93
_olex2_submission_special_instructions 'No special instructions were received'