Synthesis of disubstituted furans catalysed by [(AuCl)2(μ-bis(phosphino)metallocene)] and Na[BArF24]
Gwinn, Reilly K.; Boggess, Anna E.; Winter, Elizabeth P.; Nataro, Chip; Dalton Transactions  (2022) –; doi:10.1039/D2DT02999E

data_7711547
_publ_section_title
;
 Synthesis of disubstituted furans catalysed by
 [(AuCl)2(\m-bis(phosphino)metallocene)] and Na[BArF24]
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02999E
_journal_year                    2022
_chemical_formula_moiety         'C34 H28 Au2 Cl2 Os P2'
_chemical_formula_sum            'C34 H28 Au2 Cl2 Os P2'
_chemical_formula_weight         1153.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-10-22 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.880(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7482(2)
_cell_length_b                   16.7111(5)
_cell_length_c                   10.6925(3)
_cell_measurement_reflns_used    9378
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.5020
_cell_measurement_theta_min      2.2900
_cell_volume                     1557.49(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.946
_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     85.00 110.00   0.50   12.54    --   20.00  54.00 -53.60   50
  2  \w    -74.00 -14.00   0.50   12.54    --   20.00  54.00   0.00  120
  3  \w     50.00  98.00   0.50   12.54    --   20.00  54.00   0.00   96
  4  \w    -71.00 -35.00   0.50   12.54    --   20.00  54.00-180.00   72
  5  \w    -27.00   3.00   0.50   12.54    --   20.00  54.00-180.00   60
  6  \w      8.00  68.00   0.50   12.54    --   20.00  54.00-180.00  120
  7  \w    -74.00 -15.00   0.50   12.54    --   20.00  54.00 120.00  118
  8  \w     40.00  77.00   0.50   12.54    --   20.00  54.00 120.00   74
  9  \w    -63.00  80.00   0.50   12.54    --   20.00  54.00  30.00  286
 10  \w    -72.00  28.00   0.50   12.54    --   20.00  54.00 -53.60  200
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15974
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.556
_diffrn_reflns_theta_min         2.267
_exptl_absorpt_coefficient_mu    13.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.460
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2;Et2O'
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.412
_exptl_crystal_size_min          0.188
_refine_diff_density_max         2.844
_refine_diff_density_min         -2.059
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         4523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0482P)^2^+0.5030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3940
_reflns_number_total             4523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02999e2.cif
_cod_data_source_block           '[(aucl)2(dppo)]'
_cod_database_code               7711547
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17)
;
_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
;