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_7131044
_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 H23 Au Cl O P, C H2 Cl2'
_chemical_formula_sum            'C32 H25 Au Cl3 O P'
_chemical_formula_weight         759.80
_chemical_name_systematic        C32H25AuCl3OP
_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             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                96.709(2)
_cell_angle_beta                 109.916(2)
_cell_angle_gamma                110.821(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8459(10)
_cell_length_b                   12.2003(12)
_cell_length_c                   12.4897(12)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      72.31
_cell_measurement_theta_min      4.03
_cell_volume                     1398.1(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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.960
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18139
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.298
_diffrn_reflns_theta_min         4.027
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.260
_exptl_absorpt_correction_T_max  0.4243
_exptl_absorpt_correction_T_min  0.2383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1125 before and 0.0529 after correction. The Ratio of minimum to maximum transmission is 0.5616. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0354P)^2^+3.1817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5197
_reflns_number_total             5320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05436a2.cif
_cod_data_source_block           eli85_0m_a
_cod_depositor_comments
'Adding full bibliography for 7131043--7131047.cif.'
_cod_database_code               7131044
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.260
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C29(H29), C30(H30), C31(H31)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              25872
_shelx_hkl_checksum              57867
_olex2_submission_original_sample_id Eli85
_olex2_submission_special_instructions 'No special instructions were received'